Research ArticleFe-TiO2 Nanoparticles Synthesized by Green Chemistry forPotential Application in Waste Water Photocatalytic Treatment
Ricardo A Solano 1 Adriana P Herrera 1 David Maestre2 and Ana Cremades 2
1School of Engineering Nanomaterials and Computer Aided Process Engineering Research Group University of Cartagena130015 Cartagena Colombia
2School of Physical Sciences Department of Materials Physics Universidad Complutense de Madrid 28040 Madrid Spain
Correspondence should be addressed to Adriana P Herrera aherrerab2unicartagenaeduco
Received 2 August 2018 Revised 1 December 2018 Accepted 5 December 2018 Published 20 January 2019
Academic Editor Marco Rossi
Copyright copy 2019 Ricardo A Solano et al (is is an open access article distributed under the Creative Commons AttributionLicense which permits unrestricted use distribution and reproduction in any medium provided the original work isproperly cited
Anatase TiO2 nanoparticles doped with iron ions have been synthesized via the green chemistry method using aqueous extract oflemongrass (Cymbopogon citratus) obtained from Soxhlet extraction and doped by wet impregnation(e TiO2 anatase phase hasbeen doped with Fe3+ (005 0075 and 01 Fe3+ Ti molar ratio) at 550degC and 350degC respectively (e scanning electron mi-croscopy with energy-dispersive X-ray (SEM-EDS) shows nanoparticle clusters and efficiencies of impregnations between 665and 584 depending on the theoretical dopant amount (e electron transmission microscopy (TEM) reveals final particle sizesranging between 7 and 26 nm depending on the presence or not of the dopant (e cathodoluminescence (CL) and photo-luminescence (PL) studies of the doped and undoped nanoparticles show a luminescence signal attributed to surface oxygenvacancies (visible CL emission 380ndash700 nm and PL emission 350ndash800 nm) additionally a decrease in emission intensity isobserved due the inhibition of the recombination of the photogenerated electron-holes pairs moreover nanopowders wereanalyzed by UV-Vis spectrophotometry of diffuse reflectance and the absorption edge of the Fe-TiO2 in comparison to undopedTiO2 is extended greatly toward the visible light (e six bands (A1g + 2B1g + 3Eg) found by Raman spectroscopy and the x-raydiffraction pattern (XRD) confirm that synthesized TiO2 is only anatase phase which is commonly used as a catalyst in waste watertreatment specifically in heterogeneous photocatalytic processes
1 Introduction
Solar energy is a renewable resource and its efficient uti-lization in controlling environmental pollutions by usingphotocatalytic materials is one of the main goals of modernscience and engineering [1ndash4] Owing to exceptional andappropriate properties including nontoxic excellentchemical stability strong ultraviolet (UV) absorption andwide band gap energy (anatase 32 eV and rutile 34 eV)titanium dioxide (TiO2) is a recognized metal oxide semi-conductor which could be extensively applied to diverseapplications Hence the utilization of sustainable luminousenergy like visible light or sunlight is limited because TiO2can only be excited by ultraviolet light (wavelength lowerthan 387 nm) which occupies only 3ndash5 of the entire solarspectrum [5ndash11] It is also known that high recombination of
activated electron-hole pair of TiO2 is still its major draw-back that causes the restriction of practical applications inparticular solar harvesting aspect [10 12 13] (us manyapproaches have been devoted to improve the light responseof TiO2 in the visible light region For instance nonmetaldoping (B C N S and F) metal doping (Fe Co and La)and codoping (Fe and N B and C) [14ndash25]
(ere are current research studies focusing on the use ofplant extracts for the green synthesis of different types ofnanomaterials because the phytochemicals present in thesenatural extracts participate as capping agents or templatesfor the stabilization of crystalline phases and size control ofthe nanoparticles produced [26ndash32] Recently a mixture ofrutile with impurities for anatase phase has been preparedvia green synthesis using M citrifolia leaves extract by thehydrothermal method with calcination temperature 400degC
HindawiJournal of NanotechnologyVolume 2019 Article ID 4571848 11 pageshttpsdoiorg10115520194571848
(e green synthesized compound has a tetragonal structurewhen characterized by XRD and the evaluated averagecrystalline size was 10 nm also the surface morphology ofTiO2 nanoparticles obtained via green synthesis was ob-served as high uniform quasi-spherical shape morphology[33] Furthermore Rajiv et al [34] biosynthesized TiO2nanoparticles (NPs) using the Momordica charantia leafaqueous extract as a reducing and stabilizing agent andthese nanoparticles were applied in the in vitro antimalarialactivity against Plasmodium falciparum and the resultssuggest that the synthesized TiO2 NPs may be employed todevelop newer and safer agents for malaria control In asimilar study Goutam et al [35] prepared green titaniumdioxide NPs using leaf extract of the biodiesel plant Jatrophacurcas L and evaluated its performance for the photo-catalytic treatment of TWW after the secondary (biological)treatment process achieving 8226 and 7648 of CODand Cr removal respectively in a parabolic trough reactor(PTR) Also Jegadeeswaran et al [36] proposed a novelgreen synthesis of AgTiO2 nanocomposites of anatase phaseand average particles size of 2574 nm from Padina tetra-stromatica extract
Accordingly the present work is focused on the study ofthe synthesis and structural characterization of the Fe-dopedTiO2 nanoparticles prepared by green synthesis (e mainaim is to determine the effect of the introduction of thedoping elements in the optical physicochemical structuraland morphological properties Nanostructured TiO2 anatasedoped with different Fe Ti molar ratios were successfullysynthesized (e prepared samples were characterized byphotoluminescence cathodoluminescence UV-Vis spec-trophotometry of diffuse reflectance Raman spectroscopyXRD SEM-EDS and TEM-SAED
2 Materials and Methods
21 Materials Fresh lemongrass plant leaves (Cymbopogoncitratus) were collected from Cartagena Colombia Tita-nium(IV) isopropoxide (C12H28O4Ti) solution (95) andiron(III) chloride hexahydrate (98 purity) were purchasedfrom Alfa Aesarreg and Panreac respectively All reactionswere carried out using ACS Reagent chemicals
22 Lemongrass Leaf Extract Preparation (e lemongrassleaves were washed with griffin water (en they were driedfor six hours in an air circulation oven at 60degC (Esco Iso-thermreg OFA 32-8) and crushed using a manual mill (edried and crushed biomass (100 g) was placed in cloth bagsand subjected to a solvent extraction process using a Soxhletextractor for 6 h in approximately 500mL of distilled water[37 38] (e extract was stored in the refrigerator at 4degCFurther this extract was used to synthesize TiO2 nano-particles [33] (e extraction-concentration was performedusing the technique solid-phase microextraction (SPME)monitoring in vapor phase (HS) using a fiber of fused silicacoated with PDMSDVB of thickness 65micrometers(PDMSDVB-65 pm) (e chromatographic analysis wascarried out in an AT 6890 Series Plus gas chromatograph
(Agilent Technologies Palo Alto California USA) coupledto a selective mass detector (Agilent Technologies MSD5973) operated in the scanning complete radio frequencymode (full scan) (e column used in the analysis was DB-5MS (5 phenyl-poly (methylsiloxane) 60m times 025mm times
025m) (e injection was done in the split mode (30 1)with the SPME device
23 Green Synthesis of Fe-TiO2 Nanoparticles In a typicalexperiment the reaction was carried out in a 250mL beakerwhich was introduced in an ultrasound processor (ultrasonicprocessor WiseClean WUC-A06H 60Hz) Twenty millili-ters of the precursor agent (titanium isopropoxide) wasadded to 100mL of the aqueous extract of lemongrasscontained in a burette at a rate of 1mLmiddotsminus1 additionally thereaction lasted approximately 30 minutes with constantagitation making use of a stirring rod [18 33] (e nano-particles were washed with 70 vol ethanol and finally withdistilled water using separation by centrifugation (universalcentrifuge PLC-012E) for 15min at 5000 rpm (e synthe-sized titanium dioxide nanoparticles were calcined at 550degCfor 3 hours in a (ermo Scientific FB1415M-1450 W-5060Hz muffle [39]
24Characterization CLmeasurements were performed inHitachi S2500 SEM at room temperatures using aHamamatsu photonic multichannel analyzer PMA-12 withexcitation voltage of 25 kV HORIBA Jobin Yvon LabRAMHR800 UV-Vis used the Olympus BX41 confocal micro-scope was used in photoluminescence (PL) and Ramanmeasurements PL spectra have been acquired with a325 nm He-Cd laser using the lowest laser intensity (01 I0)to avoid the anatase to rutile phase transformation duringthe PL acquisition morever a filter D1 hole 850 μmspectrometer 327199 nm and times40 objective were used forthe photoluminescence study while micro-Raman spectroscopyhas been performed using a red He-Ne laser of 633 nmwavelength (e UV-Vis absorption studies of the pho-tocatalysts were conducted on UV-Vis diffuse reflectancespectrophotometer ((ermo Scientific EVOLUTION-600)with BaSO4 as reference(e samples were studied by X-raydiffraction (XRD) using a Panalytical XrsquoPert Pro Alpha1instrument which is equipped with a primary fastXrsquoCelerator detector operating at 45 kV and 40mA andfitted with a primary curved Ge 111 monochromator toobtain CuKα1 radiation (λ 15406 A) Data were collectedat 2θ between 10deg and 90deg with a step size of 004degmiddotsminus1 SEMmicrographs and energy-dispersive X-ray spectroscopy(EDS) maps were obtained in a Leica 440 SEM coupled toBruker AXS XFlash Detector 4010 Investigation of particlemorphology of Fe3+-doped TiO2 samples was performed ona JEM 2100HT JEOL transmission electron microscope(TEM) provided with 200 kV emission gun beam currentof 1086 μA and equipped with diffraction mode (cameralength of 300mm) for selected area electron diffraction(SAED) (e samples were prepared by ultrasonic dis-persing of the powders as slurry in 2-propanol and de-posited in TEM grids
2 Journal of Nanotechnology
3 Results and Discussion
31 Lemongrass Leaf Composition e lemongrass plant isformed by a variety of chemical components with higherpredominance terpenes and terpenoids associated with al-dehydes alcohols and ketones [40] To guarantee the for-mation of the titanium dioxide nanoparticles it is necessarythat the extract of the lemongrass plant has phytochemicalcomponents that guarantee the reduction of the titanium(IV) isopropoxide precursor [41] Figure 1 shows thechromatogram obtained for the lemongrass sample epresumptive identishycation of the compounds registered insolid sample was their mass spectra (EI 70 eV) using theAdams and Wiley databases In Table 1 appear the pre-sumptive identishycation and relative quantity () of thecomponents present in lemongrass solid sample analyzed byGC-MS operated in the full-scan mode of radio frequencyIn order to guarantee the formation of TiO2 nanoparticleswith sizes of less than 20 nm it is necessary that the extract ofthe lemongrass leaves has phytochemical components thatact as surfactants and stabilizers that prevent excessive ag-glomeration of the nanoparticulate material formed duringthe synthesis [33 35 41ndash47] as proposed in the mechanismshown in Figure 2 However it is possible to synthesize TiO2powders through the complete hydrolysis of the used pre-cursor (titanium isopropoxide) through the direct contact ofthe titanium source with water [45 48] with the disad-vantage that it does not present alternatives to control thestages of nucleation and growth that are carried out in theprocess of production of nanoparticles in solution [49]
32 XRD e XRD pattern synthesized TiO2 nanoparticlesusing the leaf extract of the lemongrass plant (Cymbopogoncitratus) is depicted in Figure 3e ten distinct peaks at 2θ 2561deg 378deg 3810deg 4847deg 5424deg 5536deg 6299deg 6920deg7059deg and 7547deg in the XRD pattern of Fe3+-doped TiO2and undoped nanopowders are consistent with anatase(101) (103) (004) (200) (105) (211) (204) (116) (220) and(107) lattice planes (JCPDS No 21-1272) e dicentractionpeaks corresponding to rutile phase only appeared inDegussa (Evonik) P-25 at 2θ 2758deg 3630deg and 5442deg canbe attributed to (110) (101) and (211) planes of rutile TiO2(JCPDS Card No 21-1276) e sharpness of peaks and theabsence of unidentishyed peaks conshyrmed the crystalline andhigh purity of nanoparticles prepared e average crys-talline size of TiO2 nanoparticles was calculated usingDebyendashScherrerrsquos equation [33]
D Kλ
β cos θ (1)
whereD is the average crystal size in A λ is the wavelength ofthe X-ray radiation (15406 A) K is the dimensionless shapefactor (09) β is the line width at half-maximum intensity(FWHM) in radians and θ is Braggrsquos angle in degrees [35]
e average crystalline size was estimated from theFWHMof the TiO2main peak (2θ 2561deg) of XRD patternswhich corresponds to the plane (101)e average crystallinesize was around 10 nm for the prepared nanomaterials Iron
(Fe+3) can conveniently integrate into the matrix of TiO2owing its atomic radius of 069 A which is almost equal toTi+4 atomic radius of 0745 A [50] However no reduction incrystalline size is observed which is attributed to nano-particles growth in the calcination process of the wet im-pregnation at 350degC for 3 h Table 2 summarizes the resultsobtained for the diameter by DebyendashScherrerrsquos equation
33 Raman Spectroscopy Micro-Raman spectroscopy hasbeen carried out for further analysis of the structural phasesof pure and Fe-doped TiO2 NPs as shown in Figure 4Anatase phase of titanium dioxide has six Raman activemodes A1g + 2B1g + 3Eg at 144 cmminus1 (Eg) 197 cmminus1 (Eg)399 cmminus1 (B1g) 516 cmminus1 (A1g + B1g) and 639 cmminus1 (Eg)which were identishyed on the Raman spectra of all thesamples under discussion [51] It has been shown that anypeak associated with iron oxide are not observed even with ahighly doped sample is means that Raman spectral ob-servations are in good agreement with the XRD resultsMoreover Fe-doped TiO2 NPs retained the anatase struc-ture which indicates that the Fe+3 dopants are successfullyincorporated into the TiO2 framework replacing Ti+4 cat-ions However it has been observed that the Raman band at144 cmminus1 (inset in Figure 4) tends to shift to a higher Ramanintensity as the amount of the Fe dopant increases
18 20 22 24 26 28 30 32 34 36 380
20000
40000
60000
80000
100000
120000
372533700631191
3088429847
2931924461
24145
19835
Abu
ndan
ce
Time (min)
19585
Figure 1 GC-MS chromatogram for lemongrass leaves
Table 1 Presumptive identishycation and relative quantity () of thecomponents present in lemongrass biomass
tR (min) Tentative identishycation Relative quantity ()1959 6-Methyl-5-hepten-2-one 1491984 β-Myrcene 4452415 NI compound M+ 150 162446 NI compound M+ 150 272932 NI compound M+ 154 722985 Neral 903088 Geranial 1223119 NI compound M+ 150 293701 NI 203725 NIa 29aUnidentishyed compound
Journal of Nanotechnology 3
Generally it has been accepted that shifts in the Raman peakoccur because of changes in the structure particle size thenature of defects and so on [52]
34 Cathodoluminescence (CL) and Photoluminescence (PL)e spectra of the cathodoluminescence detector andphotoluminescence obtained for all prepared materials areshown in Figures 5 and 6 respectively For both cases in theemission (visible spectrum 380ndash700 nm) of all samplesstudied clearly identishyed the presence of a broadbandaround the 500ndash550 nm which is due to the existence ofsurface states and the self-trapped excites in the anatasephase
(a)
TiO2
(b)
H3C CH3
CH3O
CH3
CH3
CH3
O
Ti O
O
O
O
H3C CH3
CH3
CH3
H3C CH3
H3C
H3C
+
8H2O
O+ HH
CH3
CH3
OH++4 H 4 HO-
TiOO
4Ti OH
OH
HO
OH
Ti OH
OH
HO
OH
+ H2O
(c)
Figure 2 (a) Complete hydrolysis of the precursor (b) condensation (c) encapsulationstabilization by the phytochemicals present in theaqueous extract of lemongrass (6-methyl-5-hepten-2-ona neral and geranial)
20 30 40 50 60
FeTi = 01
FeTi = 0075
FeTi = 005
FeTi = 0
Inte
nsity
(au
)
2θ (deg)
P-25
Figure 3 XRD spectra of TiO2 and Fe-TiO2 with dicenterent Fe3+ Timolar ratio calcined at 550degC for 3 h
Table 2 Particle size obtained for the diameter by DebyendashScherrerrsquos equation
Sample Particle size (DebyendashScherrerrsquos equation) (nm)P-25 1972Fe Ti 0 937Fe Ti 005 1033Fe Ti 0075 1013Fe Ti 01 991
200 400 6000
5000
10000
15000
20000
25000
P-25FeTi = 0FeTi = 005
FeTi = 0075FeTi = 01
639Eg(3)
516A1g + B1g(2)
399B1g
197Eg(2)Ra
man
inte
nsity
Raman shift (cmndash1)
144Eg(1)
70 140 2100
8000
16000
Figure 4 Raman spectra of TiO2 and Fe-TiO2 with dicenterent Fe3+ Ti molar ratios
4 Journal of Nanotechnology
Also it is evident the existence of a shoulder 600ndash650 nm related to the oxygen vacancies in the involvedphase similar to what was reported by several authors[53 54] On the other hand it is noticeable that there isdicenterence in the intensity of the luminescence whichindicates inhibition of the recombination of the electronhole pairs photogenerated by the ions of Fe3+ e in-tensity of Fe-TiO2 is lower than that of pure TiO2 whichsuggests that electron-hollow recombination is muchlower and the ecentectiveness of separation is much highere decrease in the rate of recombination implies thata large number of electrons and photogenerated gapsare involved in the photochemical transformationwhich coincides with the reported by other researchers[9 22 39 52 55]
35 TEM-SAED e surface morphology and particle size(size distribution) of the pure (Fe Ti 0) and Fe-doped TiO2(Fe Ti 01) photocatalyst were further analyzed by TEM asshown in Figures 7(a) and 7(b) respectively
It is evident from these images that the synthesizednanoparticles were agglomerated and their shapes werequasi-nanospheres this corresponds to the results re-ported by several authors in research related to the greensynthesis of TiO2 by the use of aqueous extracts of leaves[33ndash35] Also it can be seen that particles have a small sizebut are perfectly crystalline in nature e TEM results arein close agreement with the average crystallite size ob-tained from the XRD pattern e average particle sizeincreases for Fe Ti 01 as compared to pure TiO2 whichis attributed to nanoparticles growth in the calcinationprocess of the wet impregnation at 350degC for 3 h estructural information obtained from SAED (Figure 8)pattern shows the polycrystalline nature of Fe-TiO2nanoparticles (Fe Ti 01) which is indicated by the(101) (004) (200) and (105) planes of the anatase phasesimilar to that reported by Ali et al [52] e interplanarspace was determined through Equation (2) where h kand l are the Miller indexes a and c are the networkparameters for a tetragonal structure (anatase) and a 37852 bne c 95139 and d(hkl) is the interplanar dis-tance value in A [9 17]
1d2(hkl)
h2 + k2
a2+l2
c2 (2)
36 SEM-EDS e SEM micrographs and EDS analysis ofthe pure (P-25 and Fe Ti 0) and Fe-doped TiO2 (Fe Ti 005 Fe Ti 0075 and Fe Ti 01) photocatalyst aredepicted in Figures 9(a)ndash9(e) respectively Pure andFe3+-doped TiO2 are ultrashyne so they are coupled andagglomerate due to the high surface energy [50] ismeans that the green synthesis method can lead to thecreation of the product with agglomerates in themicrometric scale for which irregular forms are ob-served similar to what was reported by Arabi et al [31]for the green synthesis of TiO2 using the extract of Mooseand yme
e compositional analysis shows the separate peak oftitanium (Ti 4508 keV) iron (Fe 6398 keV) oxygen (O0523 keV) and other elements as Na Ca Si Cl and Kwhich come from the water used in the synthesis process[56] Table 3 shows the atomic percentages obtained for eachelement by EDS in addition to the impregnation elaquocienciesachieved for all prepared samples
37 UV-Vis DRS e UV-Vis dicentuse renotectance spectra ofthe pure TiO2 and Fe-TiO2 samples are shown in Figure 10e absorption is enhanced in the visible light region whenFe is doped into TiO2 e Fe-TiO2 samples exhibit ab-sorption in both the UV and visible light regions Obviouslythe dicentuse renotectance spectra of all the Fe-TiO2 nano-structures exhibit increased absorption in the visible light
300 400 500 600 700 800 900
FeTi = 01
FeTi = 0075
FeTi = 005
CL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 5 CL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
400 500 600 700 800
FeTi = 01
FeTi = 0075
FeTi = 005
PL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 6 PL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
Journal of Nanotechnology 5
range also this increase is more evident by increasing therelationship molar Fe Ti which is induced by the electrontransition from Fe 3d orbitals to TiO2 conduction band (CB)from the O 2p TiO2 valence band (VB) generating a con-siderable decrease in the band gap energy of TiO2 [18] Insummary doping Fe3+ causes structural defects of crystallattice to introduce impurity or defect energy level andinduces the local states below the conduction band edge andthen results in this redshift and narrows the band gap [20]Although doping of the Fe ions in the TiO2 does not modifythe position of the valence band edge of the TiO2 it in-troduces new energy levels (Fe3+Fe4+) of the transition Feions into the band gap of the TiO2
(e direct band gap energy (Eg) was calculated using thefollowing Tauc plot as given in the following equation which
is derived assuming a direct transition between the edge ofthe valence band and conduction
(αhv)1n A hvminusEg1113872 1113873 (3)
where h] is the photon energy a is the absorption coefficientand A is an energy-dependent constant and known as theband tailing parameter Another constant is n which isknown as power factor of the transition mode of thematerials
(e values of n for direct indirect direct forbidden andindirect forbidden transitions are 12 2 32 and 3 re-spectively (e pure anatase and Degussa P-25 TiO2 used inthis research are considered as direct band gap materials[57 58] (erefore the value of n was taken 12 to plot thegraph (αh])2 versus h] as shown in Figure 11 It is observed a
6 8 10 12 14 16 18 20 220
5
10
15
20
Cou
nts
Diameter (nm)
Average 13nmSD 2542
(a)
Cou
nts
10 12 14 16 18 20 22 24 26 280
5
10
15
20
Diameter (nm)
Average 15nmSD 3057
(b)
Figure 7 TEM images and particle size distribution of (a) Fe Ti 0 and (b) Fe Ti 0
2nmndash1
(101)(004)
(200)
(105)
(a)
(101)(004)
(200)
(105)
2nmndash1
(b)
Figure 8 SAED pattern of (a) pure TiO2 and (b) Fe-TiO2 nanoparticles (Fe Ti 01)
6 Journal of Nanotechnology
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Coun
ts (e
V)
Energy (keV)
Ti
Ti
O
P-25
(a)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
KK
O
Ti
Ti
Fe Ti = 0
(b)Co
unts
(eV
)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
Na Cl K
Ti
FeCa
Fe Ti = 005
(c)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Cl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 0075
(d)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
2500
SiCl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 01
(e)
Figure 9 SEM micrographs and EDS spectrum of (a) P-25 TiO2 (b) Fe Ti 0 (c) Fe Ti 005 (d) Fe Ti 0075 and (e) Fe Ti 01magnishycation 150x
Journal of Nanotechnology 7
reduction of 1 eV for the material Fe Ti 01 in comparisonwith the pure TiO2 (Fe Ti 0) synthesized by the meth-odology of green chemistry assisted by ultrasound whichwould allow to use more elaquociently the solar radiation inheterogeneous photocatalytic processes for the degradationof organic pollutants ese results relate to several recentresearch focused on the doping of titanium dioxide with Fe3+ions [56 59ndash61] Moradi et al [18] observed the decreaseof the band gap with the increase of the relationship molar
Fe Ti in catalysts of TiO2 doped with Fe3+ using thetechnique sol-gel
4 Conclusions
In summary TiO2 (anatase phase only) doped with a dif-ferent molar ratio Fe3+ Ti was successfully prepared viagreen synthesis (using the leaves extract of lemongrass plantleaves) assisted ultrasound method followed by calcinatione average crystalline size calculated by XRD pattern wasbetween 937 to 1033 for the TiO2 (Fe Ti 0) and TiO2 (Fe Ti 005) samples respectively e scanning electronmicroscopy with energy-dispersive X-ray (SEM-EDS) showsnanoparticles clusters and elaquociencies of impregnationsbetween 665 and 584 depending on the theoretical dopantamount From PL and CL studies it was conshyrmed thatdoping of Fe (III) ions into TiO2 matrix leads to the in-hibition of recombination of charge carriers thereby en-hancing photochemical quantum elaquociency From UV-VisDRS analysis a reduction of 1 eV was observed for thematerial Fe Ti 01 in comparison with the pure TiO2 (Fe Ti 0) synthesized by the methodology of green chemistryassisted by ultrasound which would allow to use more ef-shyciently the solar radiation in heterogeneous photocatalyticprocesses for the degradation of organic pollutants
Data Availability
e data used to support the shyndings of this study areavailable from the corresponding author upon request
Conflicts of Interest
e authors declare that there are no connoticts of interestregarding the publication of this paper
Acknowledgments
e authors greatly acknowledge the shynancial support fromUniversity de Cartagena (International Internship 201701735) and the Colombian Administrative Department ofScience Technology and Innovation (Colciencias YoungResearchers Program 2017) e authors would also like tothank the Electronic Nanomaterials Physics Research groupof Universidad Complutense de Madrid for providing thefacility of all the equipment used in this research
References
[1] Q Deng Y Liu K Mu et al ldquoPreparation and character-ization of F-modishyed C-TiO2 and its photocatalytic
200 300 400 500 600 700 800
00
02
04
06
08
10
12
Abs
orba
nce (
au)
Wavelength (nm)
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
Figure 10 Typical UV-Vis spectra of bare TiO2 and Fe-TiO2
20 25 30 35 40
0
5
10
15
20
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
(Ahv
)2 (cm
ndash1middoteV
)2
hv (eV)
Figure 11 Tauc plot analysis of bare TiO2 and Fe-TiO2
Sample Ti (atm) O (atm) Fe (atm) Impregnation elaquociency ()P-25 3773 plusmn 17 6227 plusmn 399 mdash mdashFe Ti 0 3777 plusmn 18 5915 plusmn 352 mdash mdashFe Ti 005 3908 plusmn 18 5963 plusmn 357 130 plusmn 01 6653Fe Ti 0075 3732 plusmn 19 6112 plusmn 356 156 plusmn 02 5573Fe Ti 01 4059 plusmn 20 5705 plusmn 351 237 plusmn 02 5838
8 Journal of Nanotechnology
propertiesrdquo Physica Status Solidi (A) vol 212 no 3pp 691ndash697 2015
[2] K S Prasad A Patra G Shruthi and S Chandan ldquoAqueousextract of Saraca indica leaves in the synthesis of copper oxidenanoparticles finding a way towards going greenrdquo Journal ofNanotechnology vol 2017 Article ID 7502610 6 pages 2017
[3] X Wang X Cheng X Yu and X Quan ldquoStudy on surface-enhanced Raman scattering substrate based on titanium oxidenanorods coated with gold nanoparticlesrdquo Journal of Nano-technology vol 2018 Article ID 9602480 9 pages 2018
[4] W Sangchay ldquoWO3-doped TiO2 coating on charcoal acti-vated with increase photocatalytic and antibacterial propertiessynthesized bymicrowave-assisted sol-gel methodrdquo Journal ofNanotechnology vol 2017 Article ID 7902930 7 pages 2017
[5] W Chakhari J Ben Naceur S Ben Taieb I Ben Assaker andR Chtourou ldquoFe-doped TiO2 nanorods with enhancedelectrochemical properties as efficient photoanode materialsrdquoJournal of Alloys and Compounds vol 708 pp 862ndash870 2017
[6] T Kaur A Sraw R K Wanchoo and A P ToorldquoVisiblendashlight induced photocatalytic degradation of fungi-cide with Fe and Si doped TiO2 nanoparticlesrdquo MaterialsToday Proceedings vol 3 no 2 pp 354ndash361 2016
[7] Maulidiyah T Azis A T Nurwahidah D Wibowo andM Nurdin ldquoPhotoelectrocatalyst of Fe co-doped N-TiO2Tinanotubes pesticide degradation of thiamethoxam underUVndashvisible lightsrdquo Environmental Nanotechnology Moni-toring amp Management vol 8 pp 103ndash111 2017
[8] Q Wang R Jin M Zhang and S Gao ldquoSolvothermalpreparation of Fe-doped TiO2 nanotube arrays for en-hancement in visible light induced photoelectrochemicalperformancerdquo Journal of Alloys and Compounds vol 690pp 139ndash144 2017
[9] C W Soo J C Juan C W Lai S B A Hamid andR M Yusop ldquoFe-doped mesoporous anatase-brookite titaniain the solar-light-induced photodegradation of Reactive Black5 dyerdquo Journal of the Taiwan Institute of Chemical Engineersvol 68 pp 153ndash161 2016
[10] WMekprasart S Suphankij T Tangcharoen A Simpraditpanand W Pecharapa ldquoModification of dye-sensitized solar cellworking electrode using TiO2 nanoparticleN-doped TiO2nanofiber compositesrdquo Physica Status Solidi (A) vol 211 no 8pp 1745ndash1751 2014
[11] Z Wu Z-K Zhang D-Z Guo Y-J Xing and G-M ZhangldquoTitanium oxide nanospheres preparation characterizationand wide-spectral absorptionrdquo Physica Status Solidi (A)vol 209 no 10 pp 2020ndash2026 2012
[12] K Kalantari M Kalbasi M Sohrabi and S J RoyaeeldquoEnhancing the photocatalytic oxidation of dibenzothiopheneusing visible light responsive Fe and N co-doped TiO2nanoparticlesrdquo Ceramics International vol 43 no 1pp 973ndash981 2017
[13] S Larumbe M Monge and C Gomez-Polo ldquoComparativestudy of (N Fe) doped TiO2 photocatalystsrdquo Applied SurfaceScience vol 327 pp 490ndash497 2015
[14] P Huo Z Lu HWang et al ldquoEnhanced photodegradation ofantibiotics solution under visible light with Fe2+Fe3+
immobilized on TiO2fly-ash cenospheres by using ions im-printing technologyrdquo Chemical Engineering Journal vol 172no 2-3 pp 615ndash622 2011
[15] E Marquez Brazon C Piccirillo I S Moreira andP M L Castro ldquoPhotodegradation of pharmaceutical per-sistent pollutants using hydroxyapatite-based materialsrdquoJournal of Environmental Management vol 182 pp 486ndash4952016
[16] L Schlur S Begin-Colin P Gilliot et al ldquoEffect of ball-millingand Fe-Al-doping on the structural aspect and visible lightphotocatalytic activity of TiO2 towards Escherichia coli bac-teria abatementrdquo Materials Science and Engineering Cvol 38 no 1 pp 11ndash19 2014
[17] M Yeganeh N Shahtahmasebi A Kompany et al ldquo(emagnetic characterization of Fe doped TiO2 semiconductingoxide nanoparticles synthesized by solndashgel methodrdquo PhysicaB Condensed Matter vol 511 pp 89ndash98 2017
[18] H Moradi A Eshaghi S R Hosseini and K Ghani ldquoFab-rication of Fe-doped TiO2 nanoparticles and investigation ofphotocatalytic decolorization of reactive red 198 under visiblelight irradiationrdquo Ultrasonics Sonochemistry vol 32pp 314ndash319 2016
[19] M Pazoki M Parsa and R Farhadpour ldquoRemoval of thehormones dexamethasone (DXM) by Ag doped on TiO2photocatalysisrdquo Journal of Environmental Chemical Engi-neering vol 4 no 4 pp 4426ndash4434 2016
[20] Q Wang C Yang G Zhang L Hu and P Wang ldquoPho-tocatalytic Fe-doped TiO2PSF composite UF membranescharacterization and performance on BPA removal undervisible-light irradiationrdquo Chemical Engineering Journalvol 319 pp 39ndash47 2017
[21] N C Birben C S Uyguner-Demirel S S Kavurmaci et alldquoApplication of Fe-doped TiO2 specimens for the solarphotocatalytic degradation of humic acidrdquo Catalysis Todayvol 281 pp 78ndash84 2017
[22] S A Ahmed ldquoFerromagnetism in Cr- Fe- and Ni-dopedTiO2 samplesrdquo Journal of Magnetism and Magnetic Materialsvol 442 pp 152ndash157 2017
[23] Y Sui Q Liu T Jiang and Y Guo ldquoSynthesis of nano-TiO2photocatalysts with tunable Fe doping concentration from Ti-bearing tailingsrdquo Applied Surface Science vol 428pp 1149ndash1158 2018
[24] V Moradi M B G Jun A Blackburn and R A HerringldquoSignificant improvement in visible light photocatalytic ac-tivity of Fe doped TiO2 using an acid treatment processrdquoApplied Surface Science vol 427 pp 791ndash799 2018
[25] E Craciun L Predoana I Atkinson et al ldquoFe3+-doped TiO2nanopowders for photocatalytic mineralization of oxalic acidunder solar light irradiationrdquo Journal of Photochemistry andPhotobiology A Chemistry vol 356 pp 18ndash28 2018
[26] M Zare K Namratha M S (akur and K ByrappaldquoBiocompatibility assessment and photocatalytic activity ofbio-hydrothermal synthesis of ZnO nanoparticles by Dymusvulgaris leaf extractrdquo Materials Research Bulletin vol 109pp 49ndash59 2019
[27] S Shalini R Balasundaraprabhu T Satish Kumar et alldquoEnhanced performance of sodium doped TiO2 nanorodsbased dye sensitized solar cells sensitized with extract frompetals of Hibiscus sabdariffa (Roselle)rdquo Materials Lettersvol 221 pp 192ndash195 2018
[28] A A Kashale K P Gattu K Ghule et al ldquoBiomediated greensynthesis of TiO2 nanoparticles for lithium ion battery ap-plicationrdquo Composites Part B Engineering vol 99 pp 297ndash304 2016
[29] S Shalini N Prabavathy R Balasundaraprabhu et alldquoStudies on DSSC encompassing flower shaped assembly ofNa-doped TiO2 nanorods sensitized with extract from petalsof Kigelia africanardquo Optik vol 155 pp 334ndash343 2018
[30] S Subhapriya and P Gomathipriya ldquoGreen synthesis of ti-tanium dioxide (TiO2) nanoparticles by Trigonella foenum-graecum extract and its antimicrobial propertiesrdquo MicrobialPathogenesis vol 116 pp 215ndash220 2018
Journal of Nanotechnology 9
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
(e green synthesized compound has a tetragonal structurewhen characterized by XRD and the evaluated averagecrystalline size was 10 nm also the surface morphology ofTiO2 nanoparticles obtained via green synthesis was ob-served as high uniform quasi-spherical shape morphology[33] Furthermore Rajiv et al [34] biosynthesized TiO2nanoparticles (NPs) using the Momordica charantia leafaqueous extract as a reducing and stabilizing agent andthese nanoparticles were applied in the in vitro antimalarialactivity against Plasmodium falciparum and the resultssuggest that the synthesized TiO2 NPs may be employed todevelop newer and safer agents for malaria control In asimilar study Goutam et al [35] prepared green titaniumdioxide NPs using leaf extract of the biodiesel plant Jatrophacurcas L and evaluated its performance for the photo-catalytic treatment of TWW after the secondary (biological)treatment process achieving 8226 and 7648 of CODand Cr removal respectively in a parabolic trough reactor(PTR) Also Jegadeeswaran et al [36] proposed a novelgreen synthesis of AgTiO2 nanocomposites of anatase phaseand average particles size of 2574 nm from Padina tetra-stromatica extract
Accordingly the present work is focused on the study ofthe synthesis and structural characterization of the Fe-dopedTiO2 nanoparticles prepared by green synthesis (e mainaim is to determine the effect of the introduction of thedoping elements in the optical physicochemical structuraland morphological properties Nanostructured TiO2 anatasedoped with different Fe Ti molar ratios were successfullysynthesized (e prepared samples were characterized byphotoluminescence cathodoluminescence UV-Vis spec-trophotometry of diffuse reflectance Raman spectroscopyXRD SEM-EDS and TEM-SAED
2 Materials and Methods
21 Materials Fresh lemongrass plant leaves (Cymbopogoncitratus) were collected from Cartagena Colombia Tita-nium(IV) isopropoxide (C12H28O4Ti) solution (95) andiron(III) chloride hexahydrate (98 purity) were purchasedfrom Alfa Aesarreg and Panreac respectively All reactionswere carried out using ACS Reagent chemicals
22 Lemongrass Leaf Extract Preparation (e lemongrassleaves were washed with griffin water (en they were driedfor six hours in an air circulation oven at 60degC (Esco Iso-thermreg OFA 32-8) and crushed using a manual mill (edried and crushed biomass (100 g) was placed in cloth bagsand subjected to a solvent extraction process using a Soxhletextractor for 6 h in approximately 500mL of distilled water[37 38] (e extract was stored in the refrigerator at 4degCFurther this extract was used to synthesize TiO2 nano-particles [33] (e extraction-concentration was performedusing the technique solid-phase microextraction (SPME)monitoring in vapor phase (HS) using a fiber of fused silicacoated with PDMSDVB of thickness 65micrometers(PDMSDVB-65 pm) (e chromatographic analysis wascarried out in an AT 6890 Series Plus gas chromatograph
(Agilent Technologies Palo Alto California USA) coupledto a selective mass detector (Agilent Technologies MSD5973) operated in the scanning complete radio frequencymode (full scan) (e column used in the analysis was DB-5MS (5 phenyl-poly (methylsiloxane) 60m times 025mm times
025m) (e injection was done in the split mode (30 1)with the SPME device
23 Green Synthesis of Fe-TiO2 Nanoparticles In a typicalexperiment the reaction was carried out in a 250mL beakerwhich was introduced in an ultrasound processor (ultrasonicprocessor WiseClean WUC-A06H 60Hz) Twenty millili-ters of the precursor agent (titanium isopropoxide) wasadded to 100mL of the aqueous extract of lemongrasscontained in a burette at a rate of 1mLmiddotsminus1 additionally thereaction lasted approximately 30 minutes with constantagitation making use of a stirring rod [18 33] (e nano-particles were washed with 70 vol ethanol and finally withdistilled water using separation by centrifugation (universalcentrifuge PLC-012E) for 15min at 5000 rpm (e synthe-sized titanium dioxide nanoparticles were calcined at 550degCfor 3 hours in a (ermo Scientific FB1415M-1450 W-5060Hz muffle [39]
24Characterization CLmeasurements were performed inHitachi S2500 SEM at room temperatures using aHamamatsu photonic multichannel analyzer PMA-12 withexcitation voltage of 25 kV HORIBA Jobin Yvon LabRAMHR800 UV-Vis used the Olympus BX41 confocal micro-scope was used in photoluminescence (PL) and Ramanmeasurements PL spectra have been acquired with a325 nm He-Cd laser using the lowest laser intensity (01 I0)to avoid the anatase to rutile phase transformation duringthe PL acquisition morever a filter D1 hole 850 μmspectrometer 327199 nm and times40 objective were used forthe photoluminescence study while micro-Raman spectroscopyhas been performed using a red He-Ne laser of 633 nmwavelength (e UV-Vis absorption studies of the pho-tocatalysts were conducted on UV-Vis diffuse reflectancespectrophotometer ((ermo Scientific EVOLUTION-600)with BaSO4 as reference(e samples were studied by X-raydiffraction (XRD) using a Panalytical XrsquoPert Pro Alpha1instrument which is equipped with a primary fastXrsquoCelerator detector operating at 45 kV and 40mA andfitted with a primary curved Ge 111 monochromator toobtain CuKα1 radiation (λ 15406 A) Data were collectedat 2θ between 10deg and 90deg with a step size of 004degmiddotsminus1 SEMmicrographs and energy-dispersive X-ray spectroscopy(EDS) maps were obtained in a Leica 440 SEM coupled toBruker AXS XFlash Detector 4010 Investigation of particlemorphology of Fe3+-doped TiO2 samples was performed ona JEM 2100HT JEOL transmission electron microscope(TEM) provided with 200 kV emission gun beam currentof 1086 μA and equipped with diffraction mode (cameralength of 300mm) for selected area electron diffraction(SAED) (e samples were prepared by ultrasonic dis-persing of the powders as slurry in 2-propanol and de-posited in TEM grids
2 Journal of Nanotechnology
3 Results and Discussion
31 Lemongrass Leaf Composition e lemongrass plant isformed by a variety of chemical components with higherpredominance terpenes and terpenoids associated with al-dehydes alcohols and ketones [40] To guarantee the for-mation of the titanium dioxide nanoparticles it is necessarythat the extract of the lemongrass plant has phytochemicalcomponents that guarantee the reduction of the titanium(IV) isopropoxide precursor [41] Figure 1 shows thechromatogram obtained for the lemongrass sample epresumptive identishycation of the compounds registered insolid sample was their mass spectra (EI 70 eV) using theAdams and Wiley databases In Table 1 appear the pre-sumptive identishycation and relative quantity () of thecomponents present in lemongrass solid sample analyzed byGC-MS operated in the full-scan mode of radio frequencyIn order to guarantee the formation of TiO2 nanoparticleswith sizes of less than 20 nm it is necessary that the extract ofthe lemongrass leaves has phytochemical components thatact as surfactants and stabilizers that prevent excessive ag-glomeration of the nanoparticulate material formed duringthe synthesis [33 35 41ndash47] as proposed in the mechanismshown in Figure 2 However it is possible to synthesize TiO2powders through the complete hydrolysis of the used pre-cursor (titanium isopropoxide) through the direct contact ofthe titanium source with water [45 48] with the disad-vantage that it does not present alternatives to control thestages of nucleation and growth that are carried out in theprocess of production of nanoparticles in solution [49]
32 XRD e XRD pattern synthesized TiO2 nanoparticlesusing the leaf extract of the lemongrass plant (Cymbopogoncitratus) is depicted in Figure 3e ten distinct peaks at 2θ 2561deg 378deg 3810deg 4847deg 5424deg 5536deg 6299deg 6920deg7059deg and 7547deg in the XRD pattern of Fe3+-doped TiO2and undoped nanopowders are consistent with anatase(101) (103) (004) (200) (105) (211) (204) (116) (220) and(107) lattice planes (JCPDS No 21-1272) e dicentractionpeaks corresponding to rutile phase only appeared inDegussa (Evonik) P-25 at 2θ 2758deg 3630deg and 5442deg canbe attributed to (110) (101) and (211) planes of rutile TiO2(JCPDS Card No 21-1276) e sharpness of peaks and theabsence of unidentishyed peaks conshyrmed the crystalline andhigh purity of nanoparticles prepared e average crys-talline size of TiO2 nanoparticles was calculated usingDebyendashScherrerrsquos equation [33]
D Kλ
β cos θ (1)
whereD is the average crystal size in A λ is the wavelength ofthe X-ray radiation (15406 A) K is the dimensionless shapefactor (09) β is the line width at half-maximum intensity(FWHM) in radians and θ is Braggrsquos angle in degrees [35]
e average crystalline size was estimated from theFWHMof the TiO2main peak (2θ 2561deg) of XRD patternswhich corresponds to the plane (101)e average crystallinesize was around 10 nm for the prepared nanomaterials Iron
(Fe+3) can conveniently integrate into the matrix of TiO2owing its atomic radius of 069 A which is almost equal toTi+4 atomic radius of 0745 A [50] However no reduction incrystalline size is observed which is attributed to nano-particles growth in the calcination process of the wet im-pregnation at 350degC for 3 h Table 2 summarizes the resultsobtained for the diameter by DebyendashScherrerrsquos equation
33 Raman Spectroscopy Micro-Raman spectroscopy hasbeen carried out for further analysis of the structural phasesof pure and Fe-doped TiO2 NPs as shown in Figure 4Anatase phase of titanium dioxide has six Raman activemodes A1g + 2B1g + 3Eg at 144 cmminus1 (Eg) 197 cmminus1 (Eg)399 cmminus1 (B1g) 516 cmminus1 (A1g + B1g) and 639 cmminus1 (Eg)which were identishyed on the Raman spectra of all thesamples under discussion [51] It has been shown that anypeak associated with iron oxide are not observed even with ahighly doped sample is means that Raman spectral ob-servations are in good agreement with the XRD resultsMoreover Fe-doped TiO2 NPs retained the anatase struc-ture which indicates that the Fe+3 dopants are successfullyincorporated into the TiO2 framework replacing Ti+4 cat-ions However it has been observed that the Raman band at144 cmminus1 (inset in Figure 4) tends to shift to a higher Ramanintensity as the amount of the Fe dopant increases
18 20 22 24 26 28 30 32 34 36 380
20000
40000
60000
80000
100000
120000
372533700631191
3088429847
2931924461
24145
19835
Abu
ndan
ce
Time (min)
19585
Figure 1 GC-MS chromatogram for lemongrass leaves
Table 1 Presumptive identishycation and relative quantity () of thecomponents present in lemongrass biomass
tR (min) Tentative identishycation Relative quantity ()1959 6-Methyl-5-hepten-2-one 1491984 β-Myrcene 4452415 NI compound M+ 150 162446 NI compound M+ 150 272932 NI compound M+ 154 722985 Neral 903088 Geranial 1223119 NI compound M+ 150 293701 NI 203725 NIa 29aUnidentishyed compound
Journal of Nanotechnology 3
Generally it has been accepted that shifts in the Raman peakoccur because of changes in the structure particle size thenature of defects and so on [52]
34 Cathodoluminescence (CL) and Photoluminescence (PL)e spectra of the cathodoluminescence detector andphotoluminescence obtained for all prepared materials areshown in Figures 5 and 6 respectively For both cases in theemission (visible spectrum 380ndash700 nm) of all samplesstudied clearly identishyed the presence of a broadbandaround the 500ndash550 nm which is due to the existence ofsurface states and the self-trapped excites in the anatasephase
(a)
TiO2
(b)
H3C CH3
CH3O
CH3
CH3
CH3
O
Ti O
O
O
O
H3C CH3
CH3
CH3
H3C CH3
H3C
H3C
+
8H2O
O+ HH
CH3
CH3
OH++4 H 4 HO-
TiOO
4Ti OH
OH
HO
OH
Ti OH
OH
HO
OH
+ H2O
(c)
Figure 2 (a) Complete hydrolysis of the precursor (b) condensation (c) encapsulationstabilization by the phytochemicals present in theaqueous extract of lemongrass (6-methyl-5-hepten-2-ona neral and geranial)
20 30 40 50 60
FeTi = 01
FeTi = 0075
FeTi = 005
FeTi = 0
Inte
nsity
(au
)
2θ (deg)
P-25
Figure 3 XRD spectra of TiO2 and Fe-TiO2 with dicenterent Fe3+ Timolar ratio calcined at 550degC for 3 h
Table 2 Particle size obtained for the diameter by DebyendashScherrerrsquos equation
Sample Particle size (DebyendashScherrerrsquos equation) (nm)P-25 1972Fe Ti 0 937Fe Ti 005 1033Fe Ti 0075 1013Fe Ti 01 991
200 400 6000
5000
10000
15000
20000
25000
P-25FeTi = 0FeTi = 005
FeTi = 0075FeTi = 01
639Eg(3)
516A1g + B1g(2)
399B1g
197Eg(2)Ra
man
inte
nsity
Raman shift (cmndash1)
144Eg(1)
70 140 2100
8000
16000
Figure 4 Raman spectra of TiO2 and Fe-TiO2 with dicenterent Fe3+ Ti molar ratios
4 Journal of Nanotechnology
Also it is evident the existence of a shoulder 600ndash650 nm related to the oxygen vacancies in the involvedphase similar to what was reported by several authors[53 54] On the other hand it is noticeable that there isdicenterence in the intensity of the luminescence whichindicates inhibition of the recombination of the electronhole pairs photogenerated by the ions of Fe3+ e in-tensity of Fe-TiO2 is lower than that of pure TiO2 whichsuggests that electron-hollow recombination is muchlower and the ecentectiveness of separation is much highere decrease in the rate of recombination implies thata large number of electrons and photogenerated gapsare involved in the photochemical transformationwhich coincides with the reported by other researchers[9 22 39 52 55]
35 TEM-SAED e surface morphology and particle size(size distribution) of the pure (Fe Ti 0) and Fe-doped TiO2(Fe Ti 01) photocatalyst were further analyzed by TEM asshown in Figures 7(a) and 7(b) respectively
It is evident from these images that the synthesizednanoparticles were agglomerated and their shapes werequasi-nanospheres this corresponds to the results re-ported by several authors in research related to the greensynthesis of TiO2 by the use of aqueous extracts of leaves[33ndash35] Also it can be seen that particles have a small sizebut are perfectly crystalline in nature e TEM results arein close agreement with the average crystallite size ob-tained from the XRD pattern e average particle sizeincreases for Fe Ti 01 as compared to pure TiO2 whichis attributed to nanoparticles growth in the calcinationprocess of the wet impregnation at 350degC for 3 h estructural information obtained from SAED (Figure 8)pattern shows the polycrystalline nature of Fe-TiO2nanoparticles (Fe Ti 01) which is indicated by the(101) (004) (200) and (105) planes of the anatase phasesimilar to that reported by Ali et al [52] e interplanarspace was determined through Equation (2) where h kand l are the Miller indexes a and c are the networkparameters for a tetragonal structure (anatase) and a 37852 bne c 95139 and d(hkl) is the interplanar dis-tance value in A [9 17]
1d2(hkl)
h2 + k2
a2+l2
c2 (2)
36 SEM-EDS e SEM micrographs and EDS analysis ofthe pure (P-25 and Fe Ti 0) and Fe-doped TiO2 (Fe Ti 005 Fe Ti 0075 and Fe Ti 01) photocatalyst aredepicted in Figures 9(a)ndash9(e) respectively Pure andFe3+-doped TiO2 are ultrashyne so they are coupled andagglomerate due to the high surface energy [50] ismeans that the green synthesis method can lead to thecreation of the product with agglomerates in themicrometric scale for which irregular forms are ob-served similar to what was reported by Arabi et al [31]for the green synthesis of TiO2 using the extract of Mooseand yme
e compositional analysis shows the separate peak oftitanium (Ti 4508 keV) iron (Fe 6398 keV) oxygen (O0523 keV) and other elements as Na Ca Si Cl and Kwhich come from the water used in the synthesis process[56] Table 3 shows the atomic percentages obtained for eachelement by EDS in addition to the impregnation elaquocienciesachieved for all prepared samples
37 UV-Vis DRS e UV-Vis dicentuse renotectance spectra ofthe pure TiO2 and Fe-TiO2 samples are shown in Figure 10e absorption is enhanced in the visible light region whenFe is doped into TiO2 e Fe-TiO2 samples exhibit ab-sorption in both the UV and visible light regions Obviouslythe dicentuse renotectance spectra of all the Fe-TiO2 nano-structures exhibit increased absorption in the visible light
300 400 500 600 700 800 900
FeTi = 01
FeTi = 0075
FeTi = 005
CL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 5 CL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
400 500 600 700 800
FeTi = 01
FeTi = 0075
FeTi = 005
PL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 6 PL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
Journal of Nanotechnology 5
range also this increase is more evident by increasing therelationship molar Fe Ti which is induced by the electrontransition from Fe 3d orbitals to TiO2 conduction band (CB)from the O 2p TiO2 valence band (VB) generating a con-siderable decrease in the band gap energy of TiO2 [18] Insummary doping Fe3+ causes structural defects of crystallattice to introduce impurity or defect energy level andinduces the local states below the conduction band edge andthen results in this redshift and narrows the band gap [20]Although doping of the Fe ions in the TiO2 does not modifythe position of the valence band edge of the TiO2 it in-troduces new energy levels (Fe3+Fe4+) of the transition Feions into the band gap of the TiO2
(e direct band gap energy (Eg) was calculated using thefollowing Tauc plot as given in the following equation which
is derived assuming a direct transition between the edge ofthe valence band and conduction
(αhv)1n A hvminusEg1113872 1113873 (3)
where h] is the photon energy a is the absorption coefficientand A is an energy-dependent constant and known as theband tailing parameter Another constant is n which isknown as power factor of the transition mode of thematerials
(e values of n for direct indirect direct forbidden andindirect forbidden transitions are 12 2 32 and 3 re-spectively (e pure anatase and Degussa P-25 TiO2 used inthis research are considered as direct band gap materials[57 58] (erefore the value of n was taken 12 to plot thegraph (αh])2 versus h] as shown in Figure 11 It is observed a
6 8 10 12 14 16 18 20 220
5
10
15
20
Cou
nts
Diameter (nm)
Average 13nmSD 2542
(a)
Cou
nts
10 12 14 16 18 20 22 24 26 280
5
10
15
20
Diameter (nm)
Average 15nmSD 3057
(b)
Figure 7 TEM images and particle size distribution of (a) Fe Ti 0 and (b) Fe Ti 0
2nmndash1
(101)(004)
(200)
(105)
(a)
(101)(004)
(200)
(105)
2nmndash1
(b)
Figure 8 SAED pattern of (a) pure TiO2 and (b) Fe-TiO2 nanoparticles (Fe Ti 01)
6 Journal of Nanotechnology
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Coun
ts (e
V)
Energy (keV)
Ti
Ti
O
P-25
(a)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
KK
O
Ti
Ti
Fe Ti = 0
(b)Co
unts
(eV
)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
Na Cl K
Ti
FeCa
Fe Ti = 005
(c)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Cl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 0075
(d)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
2500
SiCl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 01
(e)
Figure 9 SEM micrographs and EDS spectrum of (a) P-25 TiO2 (b) Fe Ti 0 (c) Fe Ti 005 (d) Fe Ti 0075 and (e) Fe Ti 01magnishycation 150x
Journal of Nanotechnology 7
reduction of 1 eV for the material Fe Ti 01 in comparisonwith the pure TiO2 (Fe Ti 0) synthesized by the meth-odology of green chemistry assisted by ultrasound whichwould allow to use more elaquociently the solar radiation inheterogeneous photocatalytic processes for the degradationof organic pollutants ese results relate to several recentresearch focused on the doping of titanium dioxide with Fe3+ions [56 59ndash61] Moradi et al [18] observed the decreaseof the band gap with the increase of the relationship molar
Fe Ti in catalysts of TiO2 doped with Fe3+ using thetechnique sol-gel
4 Conclusions
In summary TiO2 (anatase phase only) doped with a dif-ferent molar ratio Fe3+ Ti was successfully prepared viagreen synthesis (using the leaves extract of lemongrass plantleaves) assisted ultrasound method followed by calcinatione average crystalline size calculated by XRD pattern wasbetween 937 to 1033 for the TiO2 (Fe Ti 0) and TiO2 (Fe Ti 005) samples respectively e scanning electronmicroscopy with energy-dispersive X-ray (SEM-EDS) showsnanoparticles clusters and elaquociencies of impregnationsbetween 665 and 584 depending on the theoretical dopantamount From PL and CL studies it was conshyrmed thatdoping of Fe (III) ions into TiO2 matrix leads to the in-hibition of recombination of charge carriers thereby en-hancing photochemical quantum elaquociency From UV-VisDRS analysis a reduction of 1 eV was observed for thematerial Fe Ti 01 in comparison with the pure TiO2 (Fe Ti 0) synthesized by the methodology of green chemistryassisted by ultrasound which would allow to use more ef-shyciently the solar radiation in heterogeneous photocatalyticprocesses for the degradation of organic pollutants
Data Availability
e data used to support the shyndings of this study areavailable from the corresponding author upon request
Conflicts of Interest
e authors declare that there are no connoticts of interestregarding the publication of this paper
Acknowledgments
e authors greatly acknowledge the shynancial support fromUniversity de Cartagena (International Internship 201701735) and the Colombian Administrative Department ofScience Technology and Innovation (Colciencias YoungResearchers Program 2017) e authors would also like tothank the Electronic Nanomaterials Physics Research groupof Universidad Complutense de Madrid for providing thefacility of all the equipment used in this research
References
[1] Q Deng Y Liu K Mu et al ldquoPreparation and character-ization of F-modishyed C-TiO2 and its photocatalytic
200 300 400 500 600 700 800
00
02
04
06
08
10
12
Abs
orba
nce (
au)
Wavelength (nm)
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
Figure 10 Typical UV-Vis spectra of bare TiO2 and Fe-TiO2
20 25 30 35 40
0
5
10
15
20
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
(Ahv
)2 (cm
ndash1middoteV
)2
hv (eV)
Figure 11 Tauc plot analysis of bare TiO2 and Fe-TiO2
Sample Ti (atm) O (atm) Fe (atm) Impregnation elaquociency ()P-25 3773 plusmn 17 6227 plusmn 399 mdash mdashFe Ti 0 3777 plusmn 18 5915 plusmn 352 mdash mdashFe Ti 005 3908 plusmn 18 5963 plusmn 357 130 plusmn 01 6653Fe Ti 0075 3732 plusmn 19 6112 plusmn 356 156 plusmn 02 5573Fe Ti 01 4059 plusmn 20 5705 plusmn 351 237 plusmn 02 5838
8 Journal of Nanotechnology
propertiesrdquo Physica Status Solidi (A) vol 212 no 3pp 691ndash697 2015
[2] K S Prasad A Patra G Shruthi and S Chandan ldquoAqueousextract of Saraca indica leaves in the synthesis of copper oxidenanoparticles finding a way towards going greenrdquo Journal ofNanotechnology vol 2017 Article ID 7502610 6 pages 2017
[3] X Wang X Cheng X Yu and X Quan ldquoStudy on surface-enhanced Raman scattering substrate based on titanium oxidenanorods coated with gold nanoparticlesrdquo Journal of Nano-technology vol 2018 Article ID 9602480 9 pages 2018
[4] W Sangchay ldquoWO3-doped TiO2 coating on charcoal acti-vated with increase photocatalytic and antibacterial propertiessynthesized bymicrowave-assisted sol-gel methodrdquo Journal ofNanotechnology vol 2017 Article ID 7902930 7 pages 2017
[5] W Chakhari J Ben Naceur S Ben Taieb I Ben Assaker andR Chtourou ldquoFe-doped TiO2 nanorods with enhancedelectrochemical properties as efficient photoanode materialsrdquoJournal of Alloys and Compounds vol 708 pp 862ndash870 2017
[6] T Kaur A Sraw R K Wanchoo and A P ToorldquoVisiblendashlight induced photocatalytic degradation of fungi-cide with Fe and Si doped TiO2 nanoparticlesrdquo MaterialsToday Proceedings vol 3 no 2 pp 354ndash361 2016
[7] Maulidiyah T Azis A T Nurwahidah D Wibowo andM Nurdin ldquoPhotoelectrocatalyst of Fe co-doped N-TiO2Tinanotubes pesticide degradation of thiamethoxam underUVndashvisible lightsrdquo Environmental Nanotechnology Moni-toring amp Management vol 8 pp 103ndash111 2017
[8] Q Wang R Jin M Zhang and S Gao ldquoSolvothermalpreparation of Fe-doped TiO2 nanotube arrays for en-hancement in visible light induced photoelectrochemicalperformancerdquo Journal of Alloys and Compounds vol 690pp 139ndash144 2017
[9] C W Soo J C Juan C W Lai S B A Hamid andR M Yusop ldquoFe-doped mesoporous anatase-brookite titaniain the solar-light-induced photodegradation of Reactive Black5 dyerdquo Journal of the Taiwan Institute of Chemical Engineersvol 68 pp 153ndash161 2016
[10] WMekprasart S Suphankij T Tangcharoen A Simpraditpanand W Pecharapa ldquoModification of dye-sensitized solar cellworking electrode using TiO2 nanoparticleN-doped TiO2nanofiber compositesrdquo Physica Status Solidi (A) vol 211 no 8pp 1745ndash1751 2014
[11] Z Wu Z-K Zhang D-Z Guo Y-J Xing and G-M ZhangldquoTitanium oxide nanospheres preparation characterizationand wide-spectral absorptionrdquo Physica Status Solidi (A)vol 209 no 10 pp 2020ndash2026 2012
[12] K Kalantari M Kalbasi M Sohrabi and S J RoyaeeldquoEnhancing the photocatalytic oxidation of dibenzothiopheneusing visible light responsive Fe and N co-doped TiO2nanoparticlesrdquo Ceramics International vol 43 no 1pp 973ndash981 2017
[13] S Larumbe M Monge and C Gomez-Polo ldquoComparativestudy of (N Fe) doped TiO2 photocatalystsrdquo Applied SurfaceScience vol 327 pp 490ndash497 2015
[14] P Huo Z Lu HWang et al ldquoEnhanced photodegradation ofantibiotics solution under visible light with Fe2+Fe3+
immobilized on TiO2fly-ash cenospheres by using ions im-printing technologyrdquo Chemical Engineering Journal vol 172no 2-3 pp 615ndash622 2011
[15] E Marquez Brazon C Piccirillo I S Moreira andP M L Castro ldquoPhotodegradation of pharmaceutical per-sistent pollutants using hydroxyapatite-based materialsrdquoJournal of Environmental Management vol 182 pp 486ndash4952016
[16] L Schlur S Begin-Colin P Gilliot et al ldquoEffect of ball-millingand Fe-Al-doping on the structural aspect and visible lightphotocatalytic activity of TiO2 towards Escherichia coli bac-teria abatementrdquo Materials Science and Engineering Cvol 38 no 1 pp 11ndash19 2014
[17] M Yeganeh N Shahtahmasebi A Kompany et al ldquo(emagnetic characterization of Fe doped TiO2 semiconductingoxide nanoparticles synthesized by solndashgel methodrdquo PhysicaB Condensed Matter vol 511 pp 89ndash98 2017
[18] H Moradi A Eshaghi S R Hosseini and K Ghani ldquoFab-rication of Fe-doped TiO2 nanoparticles and investigation ofphotocatalytic decolorization of reactive red 198 under visiblelight irradiationrdquo Ultrasonics Sonochemistry vol 32pp 314ndash319 2016
[19] M Pazoki M Parsa and R Farhadpour ldquoRemoval of thehormones dexamethasone (DXM) by Ag doped on TiO2photocatalysisrdquo Journal of Environmental Chemical Engi-neering vol 4 no 4 pp 4426ndash4434 2016
[20] Q Wang C Yang G Zhang L Hu and P Wang ldquoPho-tocatalytic Fe-doped TiO2PSF composite UF membranescharacterization and performance on BPA removal undervisible-light irradiationrdquo Chemical Engineering Journalvol 319 pp 39ndash47 2017
[21] N C Birben C S Uyguner-Demirel S S Kavurmaci et alldquoApplication of Fe-doped TiO2 specimens for the solarphotocatalytic degradation of humic acidrdquo Catalysis Todayvol 281 pp 78ndash84 2017
[22] S A Ahmed ldquoFerromagnetism in Cr- Fe- and Ni-dopedTiO2 samplesrdquo Journal of Magnetism and Magnetic Materialsvol 442 pp 152ndash157 2017
[23] Y Sui Q Liu T Jiang and Y Guo ldquoSynthesis of nano-TiO2photocatalysts with tunable Fe doping concentration from Ti-bearing tailingsrdquo Applied Surface Science vol 428pp 1149ndash1158 2018
[24] V Moradi M B G Jun A Blackburn and R A HerringldquoSignificant improvement in visible light photocatalytic ac-tivity of Fe doped TiO2 using an acid treatment processrdquoApplied Surface Science vol 427 pp 791ndash799 2018
[25] E Craciun L Predoana I Atkinson et al ldquoFe3+-doped TiO2nanopowders for photocatalytic mineralization of oxalic acidunder solar light irradiationrdquo Journal of Photochemistry andPhotobiology A Chemistry vol 356 pp 18ndash28 2018
[26] M Zare K Namratha M S (akur and K ByrappaldquoBiocompatibility assessment and photocatalytic activity ofbio-hydrothermal synthesis of ZnO nanoparticles by Dymusvulgaris leaf extractrdquo Materials Research Bulletin vol 109pp 49ndash59 2019
[27] S Shalini R Balasundaraprabhu T Satish Kumar et alldquoEnhanced performance of sodium doped TiO2 nanorodsbased dye sensitized solar cells sensitized with extract frompetals of Hibiscus sabdariffa (Roselle)rdquo Materials Lettersvol 221 pp 192ndash195 2018
[28] A A Kashale K P Gattu K Ghule et al ldquoBiomediated greensynthesis of TiO2 nanoparticles for lithium ion battery ap-plicationrdquo Composites Part B Engineering vol 99 pp 297ndash304 2016
[29] S Shalini N Prabavathy R Balasundaraprabhu et alldquoStudies on DSSC encompassing flower shaped assembly ofNa-doped TiO2 nanorods sensitized with extract from petalsof Kigelia africanardquo Optik vol 155 pp 334ndash343 2018
[30] S Subhapriya and P Gomathipriya ldquoGreen synthesis of ti-tanium dioxide (TiO2) nanoparticles by Trigonella foenum-graecum extract and its antimicrobial propertiesrdquo MicrobialPathogenesis vol 116 pp 215ndash220 2018
Journal of Nanotechnology 9
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
31 Lemongrass Leaf Composition e lemongrass plant isformed by a variety of chemical components with higherpredominance terpenes and terpenoids associated with al-dehydes alcohols and ketones [40] To guarantee the for-mation of the titanium dioxide nanoparticles it is necessarythat the extract of the lemongrass plant has phytochemicalcomponents that guarantee the reduction of the titanium(IV) isopropoxide precursor [41] Figure 1 shows thechromatogram obtained for the lemongrass sample epresumptive identishycation of the compounds registered insolid sample was their mass spectra (EI 70 eV) using theAdams and Wiley databases In Table 1 appear the pre-sumptive identishycation and relative quantity () of thecomponents present in lemongrass solid sample analyzed byGC-MS operated in the full-scan mode of radio frequencyIn order to guarantee the formation of TiO2 nanoparticleswith sizes of less than 20 nm it is necessary that the extract ofthe lemongrass leaves has phytochemical components thatact as surfactants and stabilizers that prevent excessive ag-glomeration of the nanoparticulate material formed duringthe synthesis [33 35 41ndash47] as proposed in the mechanismshown in Figure 2 However it is possible to synthesize TiO2powders through the complete hydrolysis of the used pre-cursor (titanium isopropoxide) through the direct contact ofthe titanium source with water [45 48] with the disad-vantage that it does not present alternatives to control thestages of nucleation and growth that are carried out in theprocess of production of nanoparticles in solution [49]
32 XRD e XRD pattern synthesized TiO2 nanoparticlesusing the leaf extract of the lemongrass plant (Cymbopogoncitratus) is depicted in Figure 3e ten distinct peaks at 2θ 2561deg 378deg 3810deg 4847deg 5424deg 5536deg 6299deg 6920deg7059deg and 7547deg in the XRD pattern of Fe3+-doped TiO2and undoped nanopowders are consistent with anatase(101) (103) (004) (200) (105) (211) (204) (116) (220) and(107) lattice planes (JCPDS No 21-1272) e dicentractionpeaks corresponding to rutile phase only appeared inDegussa (Evonik) P-25 at 2θ 2758deg 3630deg and 5442deg canbe attributed to (110) (101) and (211) planes of rutile TiO2(JCPDS Card No 21-1276) e sharpness of peaks and theabsence of unidentishyed peaks conshyrmed the crystalline andhigh purity of nanoparticles prepared e average crys-talline size of TiO2 nanoparticles was calculated usingDebyendashScherrerrsquos equation [33]
D Kλ
β cos θ (1)
whereD is the average crystal size in A λ is the wavelength ofthe X-ray radiation (15406 A) K is the dimensionless shapefactor (09) β is the line width at half-maximum intensity(FWHM) in radians and θ is Braggrsquos angle in degrees [35]
e average crystalline size was estimated from theFWHMof the TiO2main peak (2θ 2561deg) of XRD patternswhich corresponds to the plane (101)e average crystallinesize was around 10 nm for the prepared nanomaterials Iron
(Fe+3) can conveniently integrate into the matrix of TiO2owing its atomic radius of 069 A which is almost equal toTi+4 atomic radius of 0745 A [50] However no reduction incrystalline size is observed which is attributed to nano-particles growth in the calcination process of the wet im-pregnation at 350degC for 3 h Table 2 summarizes the resultsobtained for the diameter by DebyendashScherrerrsquos equation
33 Raman Spectroscopy Micro-Raman spectroscopy hasbeen carried out for further analysis of the structural phasesof pure and Fe-doped TiO2 NPs as shown in Figure 4Anatase phase of titanium dioxide has six Raman activemodes A1g + 2B1g + 3Eg at 144 cmminus1 (Eg) 197 cmminus1 (Eg)399 cmminus1 (B1g) 516 cmminus1 (A1g + B1g) and 639 cmminus1 (Eg)which were identishyed on the Raman spectra of all thesamples under discussion [51] It has been shown that anypeak associated with iron oxide are not observed even with ahighly doped sample is means that Raman spectral ob-servations are in good agreement with the XRD resultsMoreover Fe-doped TiO2 NPs retained the anatase struc-ture which indicates that the Fe+3 dopants are successfullyincorporated into the TiO2 framework replacing Ti+4 cat-ions However it has been observed that the Raman band at144 cmminus1 (inset in Figure 4) tends to shift to a higher Ramanintensity as the amount of the Fe dopant increases
18 20 22 24 26 28 30 32 34 36 380
20000
40000
60000
80000
100000
120000
372533700631191
3088429847
2931924461
24145
19835
Abu
ndan
ce
Time (min)
19585
Figure 1 GC-MS chromatogram for lemongrass leaves
Table 1 Presumptive identishycation and relative quantity () of thecomponents present in lemongrass biomass
tR (min) Tentative identishycation Relative quantity ()1959 6-Methyl-5-hepten-2-one 1491984 β-Myrcene 4452415 NI compound M+ 150 162446 NI compound M+ 150 272932 NI compound M+ 154 722985 Neral 903088 Geranial 1223119 NI compound M+ 150 293701 NI 203725 NIa 29aUnidentishyed compound
Journal of Nanotechnology 3
Generally it has been accepted that shifts in the Raman peakoccur because of changes in the structure particle size thenature of defects and so on [52]
34 Cathodoluminescence (CL) and Photoluminescence (PL)e spectra of the cathodoluminescence detector andphotoluminescence obtained for all prepared materials areshown in Figures 5 and 6 respectively For both cases in theemission (visible spectrum 380ndash700 nm) of all samplesstudied clearly identishyed the presence of a broadbandaround the 500ndash550 nm which is due to the existence ofsurface states and the self-trapped excites in the anatasephase
(a)
TiO2
(b)
H3C CH3
CH3O
CH3
CH3
CH3
O
Ti O
O
O
O
H3C CH3
CH3
CH3
H3C CH3
H3C
H3C
+
8H2O
O+ HH
CH3
CH3
OH++4 H 4 HO-
TiOO
4Ti OH
OH
HO
OH
Ti OH
OH
HO
OH
+ H2O
(c)
Figure 2 (a) Complete hydrolysis of the precursor (b) condensation (c) encapsulationstabilization by the phytochemicals present in theaqueous extract of lemongrass (6-methyl-5-hepten-2-ona neral and geranial)
20 30 40 50 60
FeTi = 01
FeTi = 0075
FeTi = 005
FeTi = 0
Inte
nsity
(au
)
2θ (deg)
P-25
Figure 3 XRD spectra of TiO2 and Fe-TiO2 with dicenterent Fe3+ Timolar ratio calcined at 550degC for 3 h
Table 2 Particle size obtained for the diameter by DebyendashScherrerrsquos equation
Sample Particle size (DebyendashScherrerrsquos equation) (nm)P-25 1972Fe Ti 0 937Fe Ti 005 1033Fe Ti 0075 1013Fe Ti 01 991
200 400 6000
5000
10000
15000
20000
25000
P-25FeTi = 0FeTi = 005
FeTi = 0075FeTi = 01
639Eg(3)
516A1g + B1g(2)
399B1g
197Eg(2)Ra
man
inte
nsity
Raman shift (cmndash1)
144Eg(1)
70 140 2100
8000
16000
Figure 4 Raman spectra of TiO2 and Fe-TiO2 with dicenterent Fe3+ Ti molar ratios
4 Journal of Nanotechnology
Also it is evident the existence of a shoulder 600ndash650 nm related to the oxygen vacancies in the involvedphase similar to what was reported by several authors[53 54] On the other hand it is noticeable that there isdicenterence in the intensity of the luminescence whichindicates inhibition of the recombination of the electronhole pairs photogenerated by the ions of Fe3+ e in-tensity of Fe-TiO2 is lower than that of pure TiO2 whichsuggests that electron-hollow recombination is muchlower and the ecentectiveness of separation is much highere decrease in the rate of recombination implies thata large number of electrons and photogenerated gapsare involved in the photochemical transformationwhich coincides with the reported by other researchers[9 22 39 52 55]
35 TEM-SAED e surface morphology and particle size(size distribution) of the pure (Fe Ti 0) and Fe-doped TiO2(Fe Ti 01) photocatalyst were further analyzed by TEM asshown in Figures 7(a) and 7(b) respectively
It is evident from these images that the synthesizednanoparticles were agglomerated and their shapes werequasi-nanospheres this corresponds to the results re-ported by several authors in research related to the greensynthesis of TiO2 by the use of aqueous extracts of leaves[33ndash35] Also it can be seen that particles have a small sizebut are perfectly crystalline in nature e TEM results arein close agreement with the average crystallite size ob-tained from the XRD pattern e average particle sizeincreases for Fe Ti 01 as compared to pure TiO2 whichis attributed to nanoparticles growth in the calcinationprocess of the wet impregnation at 350degC for 3 h estructural information obtained from SAED (Figure 8)pattern shows the polycrystalline nature of Fe-TiO2nanoparticles (Fe Ti 01) which is indicated by the(101) (004) (200) and (105) planes of the anatase phasesimilar to that reported by Ali et al [52] e interplanarspace was determined through Equation (2) where h kand l are the Miller indexes a and c are the networkparameters for a tetragonal structure (anatase) and a 37852 bne c 95139 and d(hkl) is the interplanar dis-tance value in A [9 17]
1d2(hkl)
h2 + k2
a2+l2
c2 (2)
36 SEM-EDS e SEM micrographs and EDS analysis ofthe pure (P-25 and Fe Ti 0) and Fe-doped TiO2 (Fe Ti 005 Fe Ti 0075 and Fe Ti 01) photocatalyst aredepicted in Figures 9(a)ndash9(e) respectively Pure andFe3+-doped TiO2 are ultrashyne so they are coupled andagglomerate due to the high surface energy [50] ismeans that the green synthesis method can lead to thecreation of the product with agglomerates in themicrometric scale for which irregular forms are ob-served similar to what was reported by Arabi et al [31]for the green synthesis of TiO2 using the extract of Mooseand yme
e compositional analysis shows the separate peak oftitanium (Ti 4508 keV) iron (Fe 6398 keV) oxygen (O0523 keV) and other elements as Na Ca Si Cl and Kwhich come from the water used in the synthesis process[56] Table 3 shows the atomic percentages obtained for eachelement by EDS in addition to the impregnation elaquocienciesachieved for all prepared samples
37 UV-Vis DRS e UV-Vis dicentuse renotectance spectra ofthe pure TiO2 and Fe-TiO2 samples are shown in Figure 10e absorption is enhanced in the visible light region whenFe is doped into TiO2 e Fe-TiO2 samples exhibit ab-sorption in both the UV and visible light regions Obviouslythe dicentuse renotectance spectra of all the Fe-TiO2 nano-structures exhibit increased absorption in the visible light
300 400 500 600 700 800 900
FeTi = 01
FeTi = 0075
FeTi = 005
CL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 5 CL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
400 500 600 700 800
FeTi = 01
FeTi = 0075
FeTi = 005
PL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 6 PL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
Journal of Nanotechnology 5
range also this increase is more evident by increasing therelationship molar Fe Ti which is induced by the electrontransition from Fe 3d orbitals to TiO2 conduction band (CB)from the O 2p TiO2 valence band (VB) generating a con-siderable decrease in the band gap energy of TiO2 [18] Insummary doping Fe3+ causes structural defects of crystallattice to introduce impurity or defect energy level andinduces the local states below the conduction band edge andthen results in this redshift and narrows the band gap [20]Although doping of the Fe ions in the TiO2 does not modifythe position of the valence band edge of the TiO2 it in-troduces new energy levels (Fe3+Fe4+) of the transition Feions into the band gap of the TiO2
(e direct band gap energy (Eg) was calculated using thefollowing Tauc plot as given in the following equation which
is derived assuming a direct transition between the edge ofthe valence band and conduction
(αhv)1n A hvminusEg1113872 1113873 (3)
where h] is the photon energy a is the absorption coefficientand A is an energy-dependent constant and known as theband tailing parameter Another constant is n which isknown as power factor of the transition mode of thematerials
(e values of n for direct indirect direct forbidden andindirect forbidden transitions are 12 2 32 and 3 re-spectively (e pure anatase and Degussa P-25 TiO2 used inthis research are considered as direct band gap materials[57 58] (erefore the value of n was taken 12 to plot thegraph (αh])2 versus h] as shown in Figure 11 It is observed a
6 8 10 12 14 16 18 20 220
5
10
15
20
Cou
nts
Diameter (nm)
Average 13nmSD 2542
(a)
Cou
nts
10 12 14 16 18 20 22 24 26 280
5
10
15
20
Diameter (nm)
Average 15nmSD 3057
(b)
Figure 7 TEM images and particle size distribution of (a) Fe Ti 0 and (b) Fe Ti 0
2nmndash1
(101)(004)
(200)
(105)
(a)
(101)(004)
(200)
(105)
2nmndash1
(b)
Figure 8 SAED pattern of (a) pure TiO2 and (b) Fe-TiO2 nanoparticles (Fe Ti 01)
6 Journal of Nanotechnology
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Coun
ts (e
V)
Energy (keV)
Ti
Ti
O
P-25
(a)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
KK
O
Ti
Ti
Fe Ti = 0
(b)Co
unts
(eV
)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
Na Cl K
Ti
FeCa
Fe Ti = 005
(c)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Cl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 0075
(d)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
2500
SiCl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 01
(e)
Figure 9 SEM micrographs and EDS spectrum of (a) P-25 TiO2 (b) Fe Ti 0 (c) Fe Ti 005 (d) Fe Ti 0075 and (e) Fe Ti 01magnishycation 150x
Journal of Nanotechnology 7
reduction of 1 eV for the material Fe Ti 01 in comparisonwith the pure TiO2 (Fe Ti 0) synthesized by the meth-odology of green chemistry assisted by ultrasound whichwould allow to use more elaquociently the solar radiation inheterogeneous photocatalytic processes for the degradationof organic pollutants ese results relate to several recentresearch focused on the doping of titanium dioxide with Fe3+ions [56 59ndash61] Moradi et al [18] observed the decreaseof the band gap with the increase of the relationship molar
Fe Ti in catalysts of TiO2 doped with Fe3+ using thetechnique sol-gel
4 Conclusions
In summary TiO2 (anatase phase only) doped with a dif-ferent molar ratio Fe3+ Ti was successfully prepared viagreen synthesis (using the leaves extract of lemongrass plantleaves) assisted ultrasound method followed by calcinatione average crystalline size calculated by XRD pattern wasbetween 937 to 1033 for the TiO2 (Fe Ti 0) and TiO2 (Fe Ti 005) samples respectively e scanning electronmicroscopy with energy-dispersive X-ray (SEM-EDS) showsnanoparticles clusters and elaquociencies of impregnationsbetween 665 and 584 depending on the theoretical dopantamount From PL and CL studies it was conshyrmed thatdoping of Fe (III) ions into TiO2 matrix leads to the in-hibition of recombination of charge carriers thereby en-hancing photochemical quantum elaquociency From UV-VisDRS analysis a reduction of 1 eV was observed for thematerial Fe Ti 01 in comparison with the pure TiO2 (Fe Ti 0) synthesized by the methodology of green chemistryassisted by ultrasound which would allow to use more ef-shyciently the solar radiation in heterogeneous photocatalyticprocesses for the degradation of organic pollutants
Data Availability
e data used to support the shyndings of this study areavailable from the corresponding author upon request
Conflicts of Interest
e authors declare that there are no connoticts of interestregarding the publication of this paper
Acknowledgments
e authors greatly acknowledge the shynancial support fromUniversity de Cartagena (International Internship 201701735) and the Colombian Administrative Department ofScience Technology and Innovation (Colciencias YoungResearchers Program 2017) e authors would also like tothank the Electronic Nanomaterials Physics Research groupof Universidad Complutense de Madrid for providing thefacility of all the equipment used in this research
References
[1] Q Deng Y Liu K Mu et al ldquoPreparation and character-ization of F-modishyed C-TiO2 and its photocatalytic
200 300 400 500 600 700 800
00
02
04
06
08
10
12
Abs
orba
nce (
au)
Wavelength (nm)
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
Figure 10 Typical UV-Vis spectra of bare TiO2 and Fe-TiO2
20 25 30 35 40
0
5
10
15
20
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
(Ahv
)2 (cm
ndash1middoteV
)2
hv (eV)
Figure 11 Tauc plot analysis of bare TiO2 and Fe-TiO2
Sample Ti (atm) O (atm) Fe (atm) Impregnation elaquociency ()P-25 3773 plusmn 17 6227 plusmn 399 mdash mdashFe Ti 0 3777 plusmn 18 5915 plusmn 352 mdash mdashFe Ti 005 3908 plusmn 18 5963 plusmn 357 130 plusmn 01 6653Fe Ti 0075 3732 plusmn 19 6112 plusmn 356 156 plusmn 02 5573Fe Ti 01 4059 plusmn 20 5705 plusmn 351 237 plusmn 02 5838
8 Journal of Nanotechnology
propertiesrdquo Physica Status Solidi (A) vol 212 no 3pp 691ndash697 2015
[2] K S Prasad A Patra G Shruthi and S Chandan ldquoAqueousextract of Saraca indica leaves in the synthesis of copper oxidenanoparticles finding a way towards going greenrdquo Journal ofNanotechnology vol 2017 Article ID 7502610 6 pages 2017
[3] X Wang X Cheng X Yu and X Quan ldquoStudy on surface-enhanced Raman scattering substrate based on titanium oxidenanorods coated with gold nanoparticlesrdquo Journal of Nano-technology vol 2018 Article ID 9602480 9 pages 2018
[4] W Sangchay ldquoWO3-doped TiO2 coating on charcoal acti-vated with increase photocatalytic and antibacterial propertiessynthesized bymicrowave-assisted sol-gel methodrdquo Journal ofNanotechnology vol 2017 Article ID 7902930 7 pages 2017
[5] W Chakhari J Ben Naceur S Ben Taieb I Ben Assaker andR Chtourou ldquoFe-doped TiO2 nanorods with enhancedelectrochemical properties as efficient photoanode materialsrdquoJournal of Alloys and Compounds vol 708 pp 862ndash870 2017
[6] T Kaur A Sraw R K Wanchoo and A P ToorldquoVisiblendashlight induced photocatalytic degradation of fungi-cide with Fe and Si doped TiO2 nanoparticlesrdquo MaterialsToday Proceedings vol 3 no 2 pp 354ndash361 2016
[7] Maulidiyah T Azis A T Nurwahidah D Wibowo andM Nurdin ldquoPhotoelectrocatalyst of Fe co-doped N-TiO2Tinanotubes pesticide degradation of thiamethoxam underUVndashvisible lightsrdquo Environmental Nanotechnology Moni-toring amp Management vol 8 pp 103ndash111 2017
[8] Q Wang R Jin M Zhang and S Gao ldquoSolvothermalpreparation of Fe-doped TiO2 nanotube arrays for en-hancement in visible light induced photoelectrochemicalperformancerdquo Journal of Alloys and Compounds vol 690pp 139ndash144 2017
[9] C W Soo J C Juan C W Lai S B A Hamid andR M Yusop ldquoFe-doped mesoporous anatase-brookite titaniain the solar-light-induced photodegradation of Reactive Black5 dyerdquo Journal of the Taiwan Institute of Chemical Engineersvol 68 pp 153ndash161 2016
[10] WMekprasart S Suphankij T Tangcharoen A Simpraditpanand W Pecharapa ldquoModification of dye-sensitized solar cellworking electrode using TiO2 nanoparticleN-doped TiO2nanofiber compositesrdquo Physica Status Solidi (A) vol 211 no 8pp 1745ndash1751 2014
[11] Z Wu Z-K Zhang D-Z Guo Y-J Xing and G-M ZhangldquoTitanium oxide nanospheres preparation characterizationand wide-spectral absorptionrdquo Physica Status Solidi (A)vol 209 no 10 pp 2020ndash2026 2012
[12] K Kalantari M Kalbasi M Sohrabi and S J RoyaeeldquoEnhancing the photocatalytic oxidation of dibenzothiopheneusing visible light responsive Fe and N co-doped TiO2nanoparticlesrdquo Ceramics International vol 43 no 1pp 973ndash981 2017
[13] S Larumbe M Monge and C Gomez-Polo ldquoComparativestudy of (N Fe) doped TiO2 photocatalystsrdquo Applied SurfaceScience vol 327 pp 490ndash497 2015
[14] P Huo Z Lu HWang et al ldquoEnhanced photodegradation ofantibiotics solution under visible light with Fe2+Fe3+
immobilized on TiO2fly-ash cenospheres by using ions im-printing technologyrdquo Chemical Engineering Journal vol 172no 2-3 pp 615ndash622 2011
[15] E Marquez Brazon C Piccirillo I S Moreira andP M L Castro ldquoPhotodegradation of pharmaceutical per-sistent pollutants using hydroxyapatite-based materialsrdquoJournal of Environmental Management vol 182 pp 486ndash4952016
[16] L Schlur S Begin-Colin P Gilliot et al ldquoEffect of ball-millingand Fe-Al-doping on the structural aspect and visible lightphotocatalytic activity of TiO2 towards Escherichia coli bac-teria abatementrdquo Materials Science and Engineering Cvol 38 no 1 pp 11ndash19 2014
[17] M Yeganeh N Shahtahmasebi A Kompany et al ldquo(emagnetic characterization of Fe doped TiO2 semiconductingoxide nanoparticles synthesized by solndashgel methodrdquo PhysicaB Condensed Matter vol 511 pp 89ndash98 2017
[18] H Moradi A Eshaghi S R Hosseini and K Ghani ldquoFab-rication of Fe-doped TiO2 nanoparticles and investigation ofphotocatalytic decolorization of reactive red 198 under visiblelight irradiationrdquo Ultrasonics Sonochemistry vol 32pp 314ndash319 2016
[19] M Pazoki M Parsa and R Farhadpour ldquoRemoval of thehormones dexamethasone (DXM) by Ag doped on TiO2photocatalysisrdquo Journal of Environmental Chemical Engi-neering vol 4 no 4 pp 4426ndash4434 2016
[20] Q Wang C Yang G Zhang L Hu and P Wang ldquoPho-tocatalytic Fe-doped TiO2PSF composite UF membranescharacterization and performance on BPA removal undervisible-light irradiationrdquo Chemical Engineering Journalvol 319 pp 39ndash47 2017
[21] N C Birben C S Uyguner-Demirel S S Kavurmaci et alldquoApplication of Fe-doped TiO2 specimens for the solarphotocatalytic degradation of humic acidrdquo Catalysis Todayvol 281 pp 78ndash84 2017
[22] S A Ahmed ldquoFerromagnetism in Cr- Fe- and Ni-dopedTiO2 samplesrdquo Journal of Magnetism and Magnetic Materialsvol 442 pp 152ndash157 2017
[23] Y Sui Q Liu T Jiang and Y Guo ldquoSynthesis of nano-TiO2photocatalysts with tunable Fe doping concentration from Ti-bearing tailingsrdquo Applied Surface Science vol 428pp 1149ndash1158 2018
[24] V Moradi M B G Jun A Blackburn and R A HerringldquoSignificant improvement in visible light photocatalytic ac-tivity of Fe doped TiO2 using an acid treatment processrdquoApplied Surface Science vol 427 pp 791ndash799 2018
[25] E Craciun L Predoana I Atkinson et al ldquoFe3+-doped TiO2nanopowders for photocatalytic mineralization of oxalic acidunder solar light irradiationrdquo Journal of Photochemistry andPhotobiology A Chemistry vol 356 pp 18ndash28 2018
[26] M Zare K Namratha M S (akur and K ByrappaldquoBiocompatibility assessment and photocatalytic activity ofbio-hydrothermal synthesis of ZnO nanoparticles by Dymusvulgaris leaf extractrdquo Materials Research Bulletin vol 109pp 49ndash59 2019
[27] S Shalini R Balasundaraprabhu T Satish Kumar et alldquoEnhanced performance of sodium doped TiO2 nanorodsbased dye sensitized solar cells sensitized with extract frompetals of Hibiscus sabdariffa (Roselle)rdquo Materials Lettersvol 221 pp 192ndash195 2018
[28] A A Kashale K P Gattu K Ghule et al ldquoBiomediated greensynthesis of TiO2 nanoparticles for lithium ion battery ap-plicationrdquo Composites Part B Engineering vol 99 pp 297ndash304 2016
[29] S Shalini N Prabavathy R Balasundaraprabhu et alldquoStudies on DSSC encompassing flower shaped assembly ofNa-doped TiO2 nanorods sensitized with extract from petalsof Kigelia africanardquo Optik vol 155 pp 334ndash343 2018
[30] S Subhapriya and P Gomathipriya ldquoGreen synthesis of ti-tanium dioxide (TiO2) nanoparticles by Trigonella foenum-graecum extract and its antimicrobial propertiesrdquo MicrobialPathogenesis vol 116 pp 215ndash220 2018
Journal of Nanotechnology 9
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
Generally it has been accepted that shifts in the Raman peakoccur because of changes in the structure particle size thenature of defects and so on [52]
34 Cathodoluminescence (CL) and Photoluminescence (PL)e spectra of the cathodoluminescence detector andphotoluminescence obtained for all prepared materials areshown in Figures 5 and 6 respectively For both cases in theemission (visible spectrum 380ndash700 nm) of all samplesstudied clearly identishyed the presence of a broadbandaround the 500ndash550 nm which is due to the existence ofsurface states and the self-trapped excites in the anatasephase
(a)
TiO2
(b)
H3C CH3
CH3O
CH3
CH3
CH3
O
Ti O
O
O
O
H3C CH3
CH3
CH3
H3C CH3
H3C
H3C
+
8H2O
O+ HH
CH3
CH3
OH++4 H 4 HO-
TiOO
4Ti OH
OH
HO
OH
Ti OH
OH
HO
OH
+ H2O
(c)
Figure 2 (a) Complete hydrolysis of the precursor (b) condensation (c) encapsulationstabilization by the phytochemicals present in theaqueous extract of lemongrass (6-methyl-5-hepten-2-ona neral and geranial)
20 30 40 50 60
FeTi = 01
FeTi = 0075
FeTi = 005
FeTi = 0
Inte
nsity
(au
)
2θ (deg)
P-25
Figure 3 XRD spectra of TiO2 and Fe-TiO2 with dicenterent Fe3+ Timolar ratio calcined at 550degC for 3 h
Table 2 Particle size obtained for the diameter by DebyendashScherrerrsquos equation
Sample Particle size (DebyendashScherrerrsquos equation) (nm)P-25 1972Fe Ti 0 937Fe Ti 005 1033Fe Ti 0075 1013Fe Ti 01 991
200 400 6000
5000
10000
15000
20000
25000
P-25FeTi = 0FeTi = 005
FeTi = 0075FeTi = 01
639Eg(3)
516A1g + B1g(2)
399B1g
197Eg(2)Ra
man
inte
nsity
Raman shift (cmndash1)
144Eg(1)
70 140 2100
8000
16000
Figure 4 Raman spectra of TiO2 and Fe-TiO2 with dicenterent Fe3+ Ti molar ratios
4 Journal of Nanotechnology
Also it is evident the existence of a shoulder 600ndash650 nm related to the oxygen vacancies in the involvedphase similar to what was reported by several authors[53 54] On the other hand it is noticeable that there isdicenterence in the intensity of the luminescence whichindicates inhibition of the recombination of the electronhole pairs photogenerated by the ions of Fe3+ e in-tensity of Fe-TiO2 is lower than that of pure TiO2 whichsuggests that electron-hollow recombination is muchlower and the ecentectiveness of separation is much highere decrease in the rate of recombination implies thata large number of electrons and photogenerated gapsare involved in the photochemical transformationwhich coincides with the reported by other researchers[9 22 39 52 55]
35 TEM-SAED e surface morphology and particle size(size distribution) of the pure (Fe Ti 0) and Fe-doped TiO2(Fe Ti 01) photocatalyst were further analyzed by TEM asshown in Figures 7(a) and 7(b) respectively
It is evident from these images that the synthesizednanoparticles were agglomerated and their shapes werequasi-nanospheres this corresponds to the results re-ported by several authors in research related to the greensynthesis of TiO2 by the use of aqueous extracts of leaves[33ndash35] Also it can be seen that particles have a small sizebut are perfectly crystalline in nature e TEM results arein close agreement with the average crystallite size ob-tained from the XRD pattern e average particle sizeincreases for Fe Ti 01 as compared to pure TiO2 whichis attributed to nanoparticles growth in the calcinationprocess of the wet impregnation at 350degC for 3 h estructural information obtained from SAED (Figure 8)pattern shows the polycrystalline nature of Fe-TiO2nanoparticles (Fe Ti 01) which is indicated by the(101) (004) (200) and (105) planes of the anatase phasesimilar to that reported by Ali et al [52] e interplanarspace was determined through Equation (2) where h kand l are the Miller indexes a and c are the networkparameters for a tetragonal structure (anatase) and a 37852 bne c 95139 and d(hkl) is the interplanar dis-tance value in A [9 17]
1d2(hkl)
h2 + k2
a2+l2
c2 (2)
36 SEM-EDS e SEM micrographs and EDS analysis ofthe pure (P-25 and Fe Ti 0) and Fe-doped TiO2 (Fe Ti 005 Fe Ti 0075 and Fe Ti 01) photocatalyst aredepicted in Figures 9(a)ndash9(e) respectively Pure andFe3+-doped TiO2 are ultrashyne so they are coupled andagglomerate due to the high surface energy [50] ismeans that the green synthesis method can lead to thecreation of the product with agglomerates in themicrometric scale for which irregular forms are ob-served similar to what was reported by Arabi et al [31]for the green synthesis of TiO2 using the extract of Mooseand yme
e compositional analysis shows the separate peak oftitanium (Ti 4508 keV) iron (Fe 6398 keV) oxygen (O0523 keV) and other elements as Na Ca Si Cl and Kwhich come from the water used in the synthesis process[56] Table 3 shows the atomic percentages obtained for eachelement by EDS in addition to the impregnation elaquocienciesachieved for all prepared samples
37 UV-Vis DRS e UV-Vis dicentuse renotectance spectra ofthe pure TiO2 and Fe-TiO2 samples are shown in Figure 10e absorption is enhanced in the visible light region whenFe is doped into TiO2 e Fe-TiO2 samples exhibit ab-sorption in both the UV and visible light regions Obviouslythe dicentuse renotectance spectra of all the Fe-TiO2 nano-structures exhibit increased absorption in the visible light
300 400 500 600 700 800 900
FeTi = 01
FeTi = 0075
FeTi = 005
CL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 5 CL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
400 500 600 700 800
FeTi = 01
FeTi = 0075
FeTi = 005
PL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 6 PL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
Journal of Nanotechnology 5
range also this increase is more evident by increasing therelationship molar Fe Ti which is induced by the electrontransition from Fe 3d orbitals to TiO2 conduction band (CB)from the O 2p TiO2 valence band (VB) generating a con-siderable decrease in the band gap energy of TiO2 [18] Insummary doping Fe3+ causes structural defects of crystallattice to introduce impurity or defect energy level andinduces the local states below the conduction band edge andthen results in this redshift and narrows the band gap [20]Although doping of the Fe ions in the TiO2 does not modifythe position of the valence band edge of the TiO2 it in-troduces new energy levels (Fe3+Fe4+) of the transition Feions into the band gap of the TiO2
(e direct band gap energy (Eg) was calculated using thefollowing Tauc plot as given in the following equation which
is derived assuming a direct transition between the edge ofthe valence band and conduction
(αhv)1n A hvminusEg1113872 1113873 (3)
where h] is the photon energy a is the absorption coefficientand A is an energy-dependent constant and known as theband tailing parameter Another constant is n which isknown as power factor of the transition mode of thematerials
(e values of n for direct indirect direct forbidden andindirect forbidden transitions are 12 2 32 and 3 re-spectively (e pure anatase and Degussa P-25 TiO2 used inthis research are considered as direct band gap materials[57 58] (erefore the value of n was taken 12 to plot thegraph (αh])2 versus h] as shown in Figure 11 It is observed a
6 8 10 12 14 16 18 20 220
5
10
15
20
Cou
nts
Diameter (nm)
Average 13nmSD 2542
(a)
Cou
nts
10 12 14 16 18 20 22 24 26 280
5
10
15
20
Diameter (nm)
Average 15nmSD 3057
(b)
Figure 7 TEM images and particle size distribution of (a) Fe Ti 0 and (b) Fe Ti 0
2nmndash1
(101)(004)
(200)
(105)
(a)
(101)(004)
(200)
(105)
2nmndash1
(b)
Figure 8 SAED pattern of (a) pure TiO2 and (b) Fe-TiO2 nanoparticles (Fe Ti 01)
6 Journal of Nanotechnology
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Coun
ts (e
V)
Energy (keV)
Ti
Ti
O
P-25
(a)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
KK
O
Ti
Ti
Fe Ti = 0
(b)Co
unts
(eV
)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
Na Cl K
Ti
FeCa
Fe Ti = 005
(c)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Cl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 0075
(d)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
2500
SiCl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 01
(e)
Figure 9 SEM micrographs and EDS spectrum of (a) P-25 TiO2 (b) Fe Ti 0 (c) Fe Ti 005 (d) Fe Ti 0075 and (e) Fe Ti 01magnishycation 150x
Journal of Nanotechnology 7
reduction of 1 eV for the material Fe Ti 01 in comparisonwith the pure TiO2 (Fe Ti 0) synthesized by the meth-odology of green chemistry assisted by ultrasound whichwould allow to use more elaquociently the solar radiation inheterogeneous photocatalytic processes for the degradationof organic pollutants ese results relate to several recentresearch focused on the doping of titanium dioxide with Fe3+ions [56 59ndash61] Moradi et al [18] observed the decreaseof the band gap with the increase of the relationship molar
Fe Ti in catalysts of TiO2 doped with Fe3+ using thetechnique sol-gel
4 Conclusions
In summary TiO2 (anatase phase only) doped with a dif-ferent molar ratio Fe3+ Ti was successfully prepared viagreen synthesis (using the leaves extract of lemongrass plantleaves) assisted ultrasound method followed by calcinatione average crystalline size calculated by XRD pattern wasbetween 937 to 1033 for the TiO2 (Fe Ti 0) and TiO2 (Fe Ti 005) samples respectively e scanning electronmicroscopy with energy-dispersive X-ray (SEM-EDS) showsnanoparticles clusters and elaquociencies of impregnationsbetween 665 and 584 depending on the theoretical dopantamount From PL and CL studies it was conshyrmed thatdoping of Fe (III) ions into TiO2 matrix leads to the in-hibition of recombination of charge carriers thereby en-hancing photochemical quantum elaquociency From UV-VisDRS analysis a reduction of 1 eV was observed for thematerial Fe Ti 01 in comparison with the pure TiO2 (Fe Ti 0) synthesized by the methodology of green chemistryassisted by ultrasound which would allow to use more ef-shyciently the solar radiation in heterogeneous photocatalyticprocesses for the degradation of organic pollutants
Data Availability
e data used to support the shyndings of this study areavailable from the corresponding author upon request
Conflicts of Interest
e authors declare that there are no connoticts of interestregarding the publication of this paper
Acknowledgments
e authors greatly acknowledge the shynancial support fromUniversity de Cartagena (International Internship 201701735) and the Colombian Administrative Department ofScience Technology and Innovation (Colciencias YoungResearchers Program 2017) e authors would also like tothank the Electronic Nanomaterials Physics Research groupof Universidad Complutense de Madrid for providing thefacility of all the equipment used in this research
References
[1] Q Deng Y Liu K Mu et al ldquoPreparation and character-ization of F-modishyed C-TiO2 and its photocatalytic
200 300 400 500 600 700 800
00
02
04
06
08
10
12
Abs
orba
nce (
au)
Wavelength (nm)
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
Figure 10 Typical UV-Vis spectra of bare TiO2 and Fe-TiO2
20 25 30 35 40
0
5
10
15
20
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
(Ahv
)2 (cm
ndash1middoteV
)2
hv (eV)
Figure 11 Tauc plot analysis of bare TiO2 and Fe-TiO2
Sample Ti (atm) O (atm) Fe (atm) Impregnation elaquociency ()P-25 3773 plusmn 17 6227 plusmn 399 mdash mdashFe Ti 0 3777 plusmn 18 5915 plusmn 352 mdash mdashFe Ti 005 3908 plusmn 18 5963 plusmn 357 130 plusmn 01 6653Fe Ti 0075 3732 plusmn 19 6112 plusmn 356 156 plusmn 02 5573Fe Ti 01 4059 plusmn 20 5705 plusmn 351 237 plusmn 02 5838
8 Journal of Nanotechnology
propertiesrdquo Physica Status Solidi (A) vol 212 no 3pp 691ndash697 2015
[2] K S Prasad A Patra G Shruthi and S Chandan ldquoAqueousextract of Saraca indica leaves in the synthesis of copper oxidenanoparticles finding a way towards going greenrdquo Journal ofNanotechnology vol 2017 Article ID 7502610 6 pages 2017
[3] X Wang X Cheng X Yu and X Quan ldquoStudy on surface-enhanced Raman scattering substrate based on titanium oxidenanorods coated with gold nanoparticlesrdquo Journal of Nano-technology vol 2018 Article ID 9602480 9 pages 2018
[4] W Sangchay ldquoWO3-doped TiO2 coating on charcoal acti-vated with increase photocatalytic and antibacterial propertiessynthesized bymicrowave-assisted sol-gel methodrdquo Journal ofNanotechnology vol 2017 Article ID 7902930 7 pages 2017
[5] W Chakhari J Ben Naceur S Ben Taieb I Ben Assaker andR Chtourou ldquoFe-doped TiO2 nanorods with enhancedelectrochemical properties as efficient photoanode materialsrdquoJournal of Alloys and Compounds vol 708 pp 862ndash870 2017
[6] T Kaur A Sraw R K Wanchoo and A P ToorldquoVisiblendashlight induced photocatalytic degradation of fungi-cide with Fe and Si doped TiO2 nanoparticlesrdquo MaterialsToday Proceedings vol 3 no 2 pp 354ndash361 2016
[7] Maulidiyah T Azis A T Nurwahidah D Wibowo andM Nurdin ldquoPhotoelectrocatalyst of Fe co-doped N-TiO2Tinanotubes pesticide degradation of thiamethoxam underUVndashvisible lightsrdquo Environmental Nanotechnology Moni-toring amp Management vol 8 pp 103ndash111 2017
[8] Q Wang R Jin M Zhang and S Gao ldquoSolvothermalpreparation of Fe-doped TiO2 nanotube arrays for en-hancement in visible light induced photoelectrochemicalperformancerdquo Journal of Alloys and Compounds vol 690pp 139ndash144 2017
[9] C W Soo J C Juan C W Lai S B A Hamid andR M Yusop ldquoFe-doped mesoporous anatase-brookite titaniain the solar-light-induced photodegradation of Reactive Black5 dyerdquo Journal of the Taiwan Institute of Chemical Engineersvol 68 pp 153ndash161 2016
[10] WMekprasart S Suphankij T Tangcharoen A Simpraditpanand W Pecharapa ldquoModification of dye-sensitized solar cellworking electrode using TiO2 nanoparticleN-doped TiO2nanofiber compositesrdquo Physica Status Solidi (A) vol 211 no 8pp 1745ndash1751 2014
[11] Z Wu Z-K Zhang D-Z Guo Y-J Xing and G-M ZhangldquoTitanium oxide nanospheres preparation characterizationand wide-spectral absorptionrdquo Physica Status Solidi (A)vol 209 no 10 pp 2020ndash2026 2012
[12] K Kalantari M Kalbasi M Sohrabi and S J RoyaeeldquoEnhancing the photocatalytic oxidation of dibenzothiopheneusing visible light responsive Fe and N co-doped TiO2nanoparticlesrdquo Ceramics International vol 43 no 1pp 973ndash981 2017
[13] S Larumbe M Monge and C Gomez-Polo ldquoComparativestudy of (N Fe) doped TiO2 photocatalystsrdquo Applied SurfaceScience vol 327 pp 490ndash497 2015
[14] P Huo Z Lu HWang et al ldquoEnhanced photodegradation ofantibiotics solution under visible light with Fe2+Fe3+
immobilized on TiO2fly-ash cenospheres by using ions im-printing technologyrdquo Chemical Engineering Journal vol 172no 2-3 pp 615ndash622 2011
[15] E Marquez Brazon C Piccirillo I S Moreira andP M L Castro ldquoPhotodegradation of pharmaceutical per-sistent pollutants using hydroxyapatite-based materialsrdquoJournal of Environmental Management vol 182 pp 486ndash4952016
[16] L Schlur S Begin-Colin P Gilliot et al ldquoEffect of ball-millingand Fe-Al-doping on the structural aspect and visible lightphotocatalytic activity of TiO2 towards Escherichia coli bac-teria abatementrdquo Materials Science and Engineering Cvol 38 no 1 pp 11ndash19 2014
[17] M Yeganeh N Shahtahmasebi A Kompany et al ldquo(emagnetic characterization of Fe doped TiO2 semiconductingoxide nanoparticles synthesized by solndashgel methodrdquo PhysicaB Condensed Matter vol 511 pp 89ndash98 2017
[18] H Moradi A Eshaghi S R Hosseini and K Ghani ldquoFab-rication of Fe-doped TiO2 nanoparticles and investigation ofphotocatalytic decolorization of reactive red 198 under visiblelight irradiationrdquo Ultrasonics Sonochemistry vol 32pp 314ndash319 2016
[19] M Pazoki M Parsa and R Farhadpour ldquoRemoval of thehormones dexamethasone (DXM) by Ag doped on TiO2photocatalysisrdquo Journal of Environmental Chemical Engi-neering vol 4 no 4 pp 4426ndash4434 2016
[20] Q Wang C Yang G Zhang L Hu and P Wang ldquoPho-tocatalytic Fe-doped TiO2PSF composite UF membranescharacterization and performance on BPA removal undervisible-light irradiationrdquo Chemical Engineering Journalvol 319 pp 39ndash47 2017
[21] N C Birben C S Uyguner-Demirel S S Kavurmaci et alldquoApplication of Fe-doped TiO2 specimens for the solarphotocatalytic degradation of humic acidrdquo Catalysis Todayvol 281 pp 78ndash84 2017
[22] S A Ahmed ldquoFerromagnetism in Cr- Fe- and Ni-dopedTiO2 samplesrdquo Journal of Magnetism and Magnetic Materialsvol 442 pp 152ndash157 2017
[23] Y Sui Q Liu T Jiang and Y Guo ldquoSynthesis of nano-TiO2photocatalysts with tunable Fe doping concentration from Ti-bearing tailingsrdquo Applied Surface Science vol 428pp 1149ndash1158 2018
[24] V Moradi M B G Jun A Blackburn and R A HerringldquoSignificant improvement in visible light photocatalytic ac-tivity of Fe doped TiO2 using an acid treatment processrdquoApplied Surface Science vol 427 pp 791ndash799 2018
[25] E Craciun L Predoana I Atkinson et al ldquoFe3+-doped TiO2nanopowders for photocatalytic mineralization of oxalic acidunder solar light irradiationrdquo Journal of Photochemistry andPhotobiology A Chemistry vol 356 pp 18ndash28 2018
[26] M Zare K Namratha M S (akur and K ByrappaldquoBiocompatibility assessment and photocatalytic activity ofbio-hydrothermal synthesis of ZnO nanoparticles by Dymusvulgaris leaf extractrdquo Materials Research Bulletin vol 109pp 49ndash59 2019
[27] S Shalini R Balasundaraprabhu T Satish Kumar et alldquoEnhanced performance of sodium doped TiO2 nanorodsbased dye sensitized solar cells sensitized with extract frompetals of Hibiscus sabdariffa (Roselle)rdquo Materials Lettersvol 221 pp 192ndash195 2018
[28] A A Kashale K P Gattu K Ghule et al ldquoBiomediated greensynthesis of TiO2 nanoparticles for lithium ion battery ap-plicationrdquo Composites Part B Engineering vol 99 pp 297ndash304 2016
[29] S Shalini N Prabavathy R Balasundaraprabhu et alldquoStudies on DSSC encompassing flower shaped assembly ofNa-doped TiO2 nanorods sensitized with extract from petalsof Kigelia africanardquo Optik vol 155 pp 334ndash343 2018
[30] S Subhapriya and P Gomathipriya ldquoGreen synthesis of ti-tanium dioxide (TiO2) nanoparticles by Trigonella foenum-graecum extract and its antimicrobial propertiesrdquo MicrobialPathogenesis vol 116 pp 215ndash220 2018
Journal of Nanotechnology 9
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
Also it is evident the existence of a shoulder 600ndash650 nm related to the oxygen vacancies in the involvedphase similar to what was reported by several authors[53 54] On the other hand it is noticeable that there isdicenterence in the intensity of the luminescence whichindicates inhibition of the recombination of the electronhole pairs photogenerated by the ions of Fe3+ e in-tensity of Fe-TiO2 is lower than that of pure TiO2 whichsuggests that electron-hollow recombination is muchlower and the ecentectiveness of separation is much highere decrease in the rate of recombination implies thata large number of electrons and photogenerated gapsare involved in the photochemical transformationwhich coincides with the reported by other researchers[9 22 39 52 55]
35 TEM-SAED e surface morphology and particle size(size distribution) of the pure (Fe Ti 0) and Fe-doped TiO2(Fe Ti 01) photocatalyst were further analyzed by TEM asshown in Figures 7(a) and 7(b) respectively
It is evident from these images that the synthesizednanoparticles were agglomerated and their shapes werequasi-nanospheres this corresponds to the results re-ported by several authors in research related to the greensynthesis of TiO2 by the use of aqueous extracts of leaves[33ndash35] Also it can be seen that particles have a small sizebut are perfectly crystalline in nature e TEM results arein close agreement with the average crystallite size ob-tained from the XRD pattern e average particle sizeincreases for Fe Ti 01 as compared to pure TiO2 whichis attributed to nanoparticles growth in the calcinationprocess of the wet impregnation at 350degC for 3 h estructural information obtained from SAED (Figure 8)pattern shows the polycrystalline nature of Fe-TiO2nanoparticles (Fe Ti 01) which is indicated by the(101) (004) (200) and (105) planes of the anatase phasesimilar to that reported by Ali et al [52] e interplanarspace was determined through Equation (2) where h kand l are the Miller indexes a and c are the networkparameters for a tetragonal structure (anatase) and a 37852 bne c 95139 and d(hkl) is the interplanar dis-tance value in A [9 17]
1d2(hkl)
h2 + k2
a2+l2
c2 (2)
36 SEM-EDS e SEM micrographs and EDS analysis ofthe pure (P-25 and Fe Ti 0) and Fe-doped TiO2 (Fe Ti 005 Fe Ti 0075 and Fe Ti 01) photocatalyst aredepicted in Figures 9(a)ndash9(e) respectively Pure andFe3+-doped TiO2 are ultrashyne so they are coupled andagglomerate due to the high surface energy [50] ismeans that the green synthesis method can lead to thecreation of the product with agglomerates in themicrometric scale for which irregular forms are ob-served similar to what was reported by Arabi et al [31]for the green synthesis of TiO2 using the extract of Mooseand yme
e compositional analysis shows the separate peak oftitanium (Ti 4508 keV) iron (Fe 6398 keV) oxygen (O0523 keV) and other elements as Na Ca Si Cl and Kwhich come from the water used in the synthesis process[56] Table 3 shows the atomic percentages obtained for eachelement by EDS in addition to the impregnation elaquocienciesachieved for all prepared samples
37 UV-Vis DRS e UV-Vis dicentuse renotectance spectra ofthe pure TiO2 and Fe-TiO2 samples are shown in Figure 10e absorption is enhanced in the visible light region whenFe is doped into TiO2 e Fe-TiO2 samples exhibit ab-sorption in both the UV and visible light regions Obviouslythe dicentuse renotectance spectra of all the Fe-TiO2 nano-structures exhibit increased absorption in the visible light
300 400 500 600 700 800 900
FeTi = 01
FeTi = 0075
FeTi = 005
CL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 5 CL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
400 500 600 700 800
FeTi = 01
FeTi = 0075
FeTi = 005
PL in
tens
ity (a
u)
Wavelength (nm)
P-25
FeTi = 0
Figure 6 PL measurements of TiO2 and Fe-TiO2 with dicenterentFe3+ Ti molar ratios
Journal of Nanotechnology 5
range also this increase is more evident by increasing therelationship molar Fe Ti which is induced by the electrontransition from Fe 3d orbitals to TiO2 conduction band (CB)from the O 2p TiO2 valence band (VB) generating a con-siderable decrease in the band gap energy of TiO2 [18] Insummary doping Fe3+ causes structural defects of crystallattice to introduce impurity or defect energy level andinduces the local states below the conduction band edge andthen results in this redshift and narrows the band gap [20]Although doping of the Fe ions in the TiO2 does not modifythe position of the valence band edge of the TiO2 it in-troduces new energy levels (Fe3+Fe4+) of the transition Feions into the band gap of the TiO2
(e direct band gap energy (Eg) was calculated using thefollowing Tauc plot as given in the following equation which
is derived assuming a direct transition between the edge ofthe valence band and conduction
(αhv)1n A hvminusEg1113872 1113873 (3)
where h] is the photon energy a is the absorption coefficientand A is an energy-dependent constant and known as theband tailing parameter Another constant is n which isknown as power factor of the transition mode of thematerials
(e values of n for direct indirect direct forbidden andindirect forbidden transitions are 12 2 32 and 3 re-spectively (e pure anatase and Degussa P-25 TiO2 used inthis research are considered as direct band gap materials[57 58] (erefore the value of n was taken 12 to plot thegraph (αh])2 versus h] as shown in Figure 11 It is observed a
6 8 10 12 14 16 18 20 220
5
10
15
20
Cou
nts
Diameter (nm)
Average 13nmSD 2542
(a)
Cou
nts
10 12 14 16 18 20 22 24 26 280
5
10
15
20
Diameter (nm)
Average 15nmSD 3057
(b)
Figure 7 TEM images and particle size distribution of (a) Fe Ti 0 and (b) Fe Ti 0
2nmndash1
(101)(004)
(200)
(105)
(a)
(101)(004)
(200)
(105)
2nmndash1
(b)
Figure 8 SAED pattern of (a) pure TiO2 and (b) Fe-TiO2 nanoparticles (Fe Ti 01)
6 Journal of Nanotechnology
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Coun
ts (e
V)
Energy (keV)
Ti
Ti
O
P-25
(a)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
KK
O
Ti
Ti
Fe Ti = 0
(b)Co
unts
(eV
)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
Na Cl K
Ti
FeCa
Fe Ti = 005
(c)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Cl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 0075
(d)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
2500
SiCl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 01
(e)
Figure 9 SEM micrographs and EDS spectrum of (a) P-25 TiO2 (b) Fe Ti 0 (c) Fe Ti 005 (d) Fe Ti 0075 and (e) Fe Ti 01magnishycation 150x
Journal of Nanotechnology 7
reduction of 1 eV for the material Fe Ti 01 in comparisonwith the pure TiO2 (Fe Ti 0) synthesized by the meth-odology of green chemistry assisted by ultrasound whichwould allow to use more elaquociently the solar radiation inheterogeneous photocatalytic processes for the degradationof organic pollutants ese results relate to several recentresearch focused on the doping of titanium dioxide with Fe3+ions [56 59ndash61] Moradi et al [18] observed the decreaseof the band gap with the increase of the relationship molar
Fe Ti in catalysts of TiO2 doped with Fe3+ using thetechnique sol-gel
4 Conclusions
In summary TiO2 (anatase phase only) doped with a dif-ferent molar ratio Fe3+ Ti was successfully prepared viagreen synthesis (using the leaves extract of lemongrass plantleaves) assisted ultrasound method followed by calcinatione average crystalline size calculated by XRD pattern wasbetween 937 to 1033 for the TiO2 (Fe Ti 0) and TiO2 (Fe Ti 005) samples respectively e scanning electronmicroscopy with energy-dispersive X-ray (SEM-EDS) showsnanoparticles clusters and elaquociencies of impregnationsbetween 665 and 584 depending on the theoretical dopantamount From PL and CL studies it was conshyrmed thatdoping of Fe (III) ions into TiO2 matrix leads to the in-hibition of recombination of charge carriers thereby en-hancing photochemical quantum elaquociency From UV-VisDRS analysis a reduction of 1 eV was observed for thematerial Fe Ti 01 in comparison with the pure TiO2 (Fe Ti 0) synthesized by the methodology of green chemistryassisted by ultrasound which would allow to use more ef-shyciently the solar radiation in heterogeneous photocatalyticprocesses for the degradation of organic pollutants
Data Availability
e data used to support the shyndings of this study areavailable from the corresponding author upon request
Conflicts of Interest
e authors declare that there are no connoticts of interestregarding the publication of this paper
Acknowledgments
e authors greatly acknowledge the shynancial support fromUniversity de Cartagena (International Internship 201701735) and the Colombian Administrative Department ofScience Technology and Innovation (Colciencias YoungResearchers Program 2017) e authors would also like tothank the Electronic Nanomaterials Physics Research groupof Universidad Complutense de Madrid for providing thefacility of all the equipment used in this research
References
[1] Q Deng Y Liu K Mu et al ldquoPreparation and character-ization of F-modishyed C-TiO2 and its photocatalytic
200 300 400 500 600 700 800
00
02
04
06
08
10
12
Abs
orba
nce (
au)
Wavelength (nm)
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
Figure 10 Typical UV-Vis spectra of bare TiO2 and Fe-TiO2
20 25 30 35 40
0
5
10
15
20
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
(Ahv
)2 (cm
ndash1middoteV
)2
hv (eV)
Figure 11 Tauc plot analysis of bare TiO2 and Fe-TiO2
Sample Ti (atm) O (atm) Fe (atm) Impregnation elaquociency ()P-25 3773 plusmn 17 6227 plusmn 399 mdash mdashFe Ti 0 3777 plusmn 18 5915 plusmn 352 mdash mdashFe Ti 005 3908 plusmn 18 5963 plusmn 357 130 plusmn 01 6653Fe Ti 0075 3732 plusmn 19 6112 plusmn 356 156 plusmn 02 5573Fe Ti 01 4059 plusmn 20 5705 plusmn 351 237 plusmn 02 5838
8 Journal of Nanotechnology
propertiesrdquo Physica Status Solidi (A) vol 212 no 3pp 691ndash697 2015
[2] K S Prasad A Patra G Shruthi and S Chandan ldquoAqueousextract of Saraca indica leaves in the synthesis of copper oxidenanoparticles finding a way towards going greenrdquo Journal ofNanotechnology vol 2017 Article ID 7502610 6 pages 2017
[3] X Wang X Cheng X Yu and X Quan ldquoStudy on surface-enhanced Raman scattering substrate based on titanium oxidenanorods coated with gold nanoparticlesrdquo Journal of Nano-technology vol 2018 Article ID 9602480 9 pages 2018
[4] W Sangchay ldquoWO3-doped TiO2 coating on charcoal acti-vated with increase photocatalytic and antibacterial propertiessynthesized bymicrowave-assisted sol-gel methodrdquo Journal ofNanotechnology vol 2017 Article ID 7902930 7 pages 2017
[5] W Chakhari J Ben Naceur S Ben Taieb I Ben Assaker andR Chtourou ldquoFe-doped TiO2 nanorods with enhancedelectrochemical properties as efficient photoanode materialsrdquoJournal of Alloys and Compounds vol 708 pp 862ndash870 2017
[6] T Kaur A Sraw R K Wanchoo and A P ToorldquoVisiblendashlight induced photocatalytic degradation of fungi-cide with Fe and Si doped TiO2 nanoparticlesrdquo MaterialsToday Proceedings vol 3 no 2 pp 354ndash361 2016
[7] Maulidiyah T Azis A T Nurwahidah D Wibowo andM Nurdin ldquoPhotoelectrocatalyst of Fe co-doped N-TiO2Tinanotubes pesticide degradation of thiamethoxam underUVndashvisible lightsrdquo Environmental Nanotechnology Moni-toring amp Management vol 8 pp 103ndash111 2017
[8] Q Wang R Jin M Zhang and S Gao ldquoSolvothermalpreparation of Fe-doped TiO2 nanotube arrays for en-hancement in visible light induced photoelectrochemicalperformancerdquo Journal of Alloys and Compounds vol 690pp 139ndash144 2017
[9] C W Soo J C Juan C W Lai S B A Hamid andR M Yusop ldquoFe-doped mesoporous anatase-brookite titaniain the solar-light-induced photodegradation of Reactive Black5 dyerdquo Journal of the Taiwan Institute of Chemical Engineersvol 68 pp 153ndash161 2016
[10] WMekprasart S Suphankij T Tangcharoen A Simpraditpanand W Pecharapa ldquoModification of dye-sensitized solar cellworking electrode using TiO2 nanoparticleN-doped TiO2nanofiber compositesrdquo Physica Status Solidi (A) vol 211 no 8pp 1745ndash1751 2014
[11] Z Wu Z-K Zhang D-Z Guo Y-J Xing and G-M ZhangldquoTitanium oxide nanospheres preparation characterizationand wide-spectral absorptionrdquo Physica Status Solidi (A)vol 209 no 10 pp 2020ndash2026 2012
[12] K Kalantari M Kalbasi M Sohrabi and S J RoyaeeldquoEnhancing the photocatalytic oxidation of dibenzothiopheneusing visible light responsive Fe and N co-doped TiO2nanoparticlesrdquo Ceramics International vol 43 no 1pp 973ndash981 2017
[13] S Larumbe M Monge and C Gomez-Polo ldquoComparativestudy of (N Fe) doped TiO2 photocatalystsrdquo Applied SurfaceScience vol 327 pp 490ndash497 2015
[14] P Huo Z Lu HWang et al ldquoEnhanced photodegradation ofantibiotics solution under visible light with Fe2+Fe3+
immobilized on TiO2fly-ash cenospheres by using ions im-printing technologyrdquo Chemical Engineering Journal vol 172no 2-3 pp 615ndash622 2011
[15] E Marquez Brazon C Piccirillo I S Moreira andP M L Castro ldquoPhotodegradation of pharmaceutical per-sistent pollutants using hydroxyapatite-based materialsrdquoJournal of Environmental Management vol 182 pp 486ndash4952016
[16] L Schlur S Begin-Colin P Gilliot et al ldquoEffect of ball-millingand Fe-Al-doping on the structural aspect and visible lightphotocatalytic activity of TiO2 towards Escherichia coli bac-teria abatementrdquo Materials Science and Engineering Cvol 38 no 1 pp 11ndash19 2014
[17] M Yeganeh N Shahtahmasebi A Kompany et al ldquo(emagnetic characterization of Fe doped TiO2 semiconductingoxide nanoparticles synthesized by solndashgel methodrdquo PhysicaB Condensed Matter vol 511 pp 89ndash98 2017
[18] H Moradi A Eshaghi S R Hosseini and K Ghani ldquoFab-rication of Fe-doped TiO2 nanoparticles and investigation ofphotocatalytic decolorization of reactive red 198 under visiblelight irradiationrdquo Ultrasonics Sonochemistry vol 32pp 314ndash319 2016
[19] M Pazoki M Parsa and R Farhadpour ldquoRemoval of thehormones dexamethasone (DXM) by Ag doped on TiO2photocatalysisrdquo Journal of Environmental Chemical Engi-neering vol 4 no 4 pp 4426ndash4434 2016
[20] Q Wang C Yang G Zhang L Hu and P Wang ldquoPho-tocatalytic Fe-doped TiO2PSF composite UF membranescharacterization and performance on BPA removal undervisible-light irradiationrdquo Chemical Engineering Journalvol 319 pp 39ndash47 2017
[21] N C Birben C S Uyguner-Demirel S S Kavurmaci et alldquoApplication of Fe-doped TiO2 specimens for the solarphotocatalytic degradation of humic acidrdquo Catalysis Todayvol 281 pp 78ndash84 2017
[22] S A Ahmed ldquoFerromagnetism in Cr- Fe- and Ni-dopedTiO2 samplesrdquo Journal of Magnetism and Magnetic Materialsvol 442 pp 152ndash157 2017
[23] Y Sui Q Liu T Jiang and Y Guo ldquoSynthesis of nano-TiO2photocatalysts with tunable Fe doping concentration from Ti-bearing tailingsrdquo Applied Surface Science vol 428pp 1149ndash1158 2018
[24] V Moradi M B G Jun A Blackburn and R A HerringldquoSignificant improvement in visible light photocatalytic ac-tivity of Fe doped TiO2 using an acid treatment processrdquoApplied Surface Science vol 427 pp 791ndash799 2018
[25] E Craciun L Predoana I Atkinson et al ldquoFe3+-doped TiO2nanopowders for photocatalytic mineralization of oxalic acidunder solar light irradiationrdquo Journal of Photochemistry andPhotobiology A Chemistry vol 356 pp 18ndash28 2018
[26] M Zare K Namratha M S (akur and K ByrappaldquoBiocompatibility assessment and photocatalytic activity ofbio-hydrothermal synthesis of ZnO nanoparticles by Dymusvulgaris leaf extractrdquo Materials Research Bulletin vol 109pp 49ndash59 2019
[27] S Shalini R Balasundaraprabhu T Satish Kumar et alldquoEnhanced performance of sodium doped TiO2 nanorodsbased dye sensitized solar cells sensitized with extract frompetals of Hibiscus sabdariffa (Roselle)rdquo Materials Lettersvol 221 pp 192ndash195 2018
[28] A A Kashale K P Gattu K Ghule et al ldquoBiomediated greensynthesis of TiO2 nanoparticles for lithium ion battery ap-plicationrdquo Composites Part B Engineering vol 99 pp 297ndash304 2016
[29] S Shalini N Prabavathy R Balasundaraprabhu et alldquoStudies on DSSC encompassing flower shaped assembly ofNa-doped TiO2 nanorods sensitized with extract from petalsof Kigelia africanardquo Optik vol 155 pp 334ndash343 2018
[30] S Subhapriya and P Gomathipriya ldquoGreen synthesis of ti-tanium dioxide (TiO2) nanoparticles by Trigonella foenum-graecum extract and its antimicrobial propertiesrdquo MicrobialPathogenesis vol 116 pp 215ndash220 2018
Journal of Nanotechnology 9
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
range also this increase is more evident by increasing therelationship molar Fe Ti which is induced by the electrontransition from Fe 3d orbitals to TiO2 conduction band (CB)from the O 2p TiO2 valence band (VB) generating a con-siderable decrease in the band gap energy of TiO2 [18] Insummary doping Fe3+ causes structural defects of crystallattice to introduce impurity or defect energy level andinduces the local states below the conduction band edge andthen results in this redshift and narrows the band gap [20]Although doping of the Fe ions in the TiO2 does not modifythe position of the valence band edge of the TiO2 it in-troduces new energy levels (Fe3+Fe4+) of the transition Feions into the band gap of the TiO2
(e direct band gap energy (Eg) was calculated using thefollowing Tauc plot as given in the following equation which
is derived assuming a direct transition between the edge ofthe valence band and conduction
(αhv)1n A hvminusEg1113872 1113873 (3)
where h] is the photon energy a is the absorption coefficientand A is an energy-dependent constant and known as theband tailing parameter Another constant is n which isknown as power factor of the transition mode of thematerials
(e values of n for direct indirect direct forbidden andindirect forbidden transitions are 12 2 32 and 3 re-spectively (e pure anatase and Degussa P-25 TiO2 used inthis research are considered as direct band gap materials[57 58] (erefore the value of n was taken 12 to plot thegraph (αh])2 versus h] as shown in Figure 11 It is observed a
6 8 10 12 14 16 18 20 220
5
10
15
20
Cou
nts
Diameter (nm)
Average 13nmSD 2542
(a)
Cou
nts
10 12 14 16 18 20 22 24 26 280
5
10
15
20
Diameter (nm)
Average 15nmSD 3057
(b)
Figure 7 TEM images and particle size distribution of (a) Fe Ti 0 and (b) Fe Ti 0
2nmndash1
(101)(004)
(200)
(105)
(a)
(101)(004)
(200)
(105)
2nmndash1
(b)
Figure 8 SAED pattern of (a) pure TiO2 and (b) Fe-TiO2 nanoparticles (Fe Ti 01)
6 Journal of Nanotechnology
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Coun
ts (e
V)
Energy (keV)
Ti
Ti
O
P-25
(a)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
KK
O
Ti
Ti
Fe Ti = 0
(b)Co
unts
(eV
)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Energy (keV)
Na Cl K
Ti
FeCa
Fe Ti = 005
(c)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
Cl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 0075
(d)
Coun
ts (e
V)
0 1 2 3 4 5 6 7 8 9 100
500
1000
1500
2000
2500
SiCl K Ca
Ti
Energy (keV)
Fe
Fe Ti = 01
(e)
Figure 9 SEM micrographs and EDS spectrum of (a) P-25 TiO2 (b) Fe Ti 0 (c) Fe Ti 005 (d) Fe Ti 0075 and (e) Fe Ti 01magnishycation 150x
Journal of Nanotechnology 7
reduction of 1 eV for the material Fe Ti 01 in comparisonwith the pure TiO2 (Fe Ti 0) synthesized by the meth-odology of green chemistry assisted by ultrasound whichwould allow to use more elaquociently the solar radiation inheterogeneous photocatalytic processes for the degradationof organic pollutants ese results relate to several recentresearch focused on the doping of titanium dioxide with Fe3+ions [56 59ndash61] Moradi et al [18] observed the decreaseof the band gap with the increase of the relationship molar
Fe Ti in catalysts of TiO2 doped with Fe3+ using thetechnique sol-gel
4 Conclusions
In summary TiO2 (anatase phase only) doped with a dif-ferent molar ratio Fe3+ Ti was successfully prepared viagreen synthesis (using the leaves extract of lemongrass plantleaves) assisted ultrasound method followed by calcinatione average crystalline size calculated by XRD pattern wasbetween 937 to 1033 for the TiO2 (Fe Ti 0) and TiO2 (Fe Ti 005) samples respectively e scanning electronmicroscopy with energy-dispersive X-ray (SEM-EDS) showsnanoparticles clusters and elaquociencies of impregnationsbetween 665 and 584 depending on the theoretical dopantamount From PL and CL studies it was conshyrmed thatdoping of Fe (III) ions into TiO2 matrix leads to the in-hibition of recombination of charge carriers thereby en-hancing photochemical quantum elaquociency From UV-VisDRS analysis a reduction of 1 eV was observed for thematerial Fe Ti 01 in comparison with the pure TiO2 (Fe Ti 0) synthesized by the methodology of green chemistryassisted by ultrasound which would allow to use more ef-shyciently the solar radiation in heterogeneous photocatalyticprocesses for the degradation of organic pollutants
Data Availability
e data used to support the shyndings of this study areavailable from the corresponding author upon request
Conflicts of Interest
e authors declare that there are no connoticts of interestregarding the publication of this paper
Acknowledgments
e authors greatly acknowledge the shynancial support fromUniversity de Cartagena (International Internship 201701735) and the Colombian Administrative Department ofScience Technology and Innovation (Colciencias YoungResearchers Program 2017) e authors would also like tothank the Electronic Nanomaterials Physics Research groupof Universidad Complutense de Madrid for providing thefacility of all the equipment used in this research
References
[1] Q Deng Y Liu K Mu et al ldquoPreparation and character-ization of F-modishyed C-TiO2 and its photocatalytic
200 300 400 500 600 700 800
00
02
04
06
08
10
12
Abs
orba
nce (
au)
Wavelength (nm)
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
Figure 10 Typical UV-Vis spectra of bare TiO2 and Fe-TiO2
20 25 30 35 40
0
5
10
15
20
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
(Ahv
)2 (cm
ndash1middoteV
)2
hv (eV)
Figure 11 Tauc plot analysis of bare TiO2 and Fe-TiO2
Sample Ti (atm) O (atm) Fe (atm) Impregnation elaquociency ()P-25 3773 plusmn 17 6227 plusmn 399 mdash mdashFe Ti 0 3777 plusmn 18 5915 plusmn 352 mdash mdashFe Ti 005 3908 plusmn 18 5963 plusmn 357 130 plusmn 01 6653Fe Ti 0075 3732 plusmn 19 6112 plusmn 356 156 plusmn 02 5573Fe Ti 01 4059 plusmn 20 5705 plusmn 351 237 plusmn 02 5838
8 Journal of Nanotechnology
propertiesrdquo Physica Status Solidi (A) vol 212 no 3pp 691ndash697 2015
[2] K S Prasad A Patra G Shruthi and S Chandan ldquoAqueousextract of Saraca indica leaves in the synthesis of copper oxidenanoparticles finding a way towards going greenrdquo Journal ofNanotechnology vol 2017 Article ID 7502610 6 pages 2017
[3] X Wang X Cheng X Yu and X Quan ldquoStudy on surface-enhanced Raman scattering substrate based on titanium oxidenanorods coated with gold nanoparticlesrdquo Journal of Nano-technology vol 2018 Article ID 9602480 9 pages 2018
[4] W Sangchay ldquoWO3-doped TiO2 coating on charcoal acti-vated with increase photocatalytic and antibacterial propertiessynthesized bymicrowave-assisted sol-gel methodrdquo Journal ofNanotechnology vol 2017 Article ID 7902930 7 pages 2017
[5] W Chakhari J Ben Naceur S Ben Taieb I Ben Assaker andR Chtourou ldquoFe-doped TiO2 nanorods with enhancedelectrochemical properties as efficient photoanode materialsrdquoJournal of Alloys and Compounds vol 708 pp 862ndash870 2017
[6] T Kaur A Sraw R K Wanchoo and A P ToorldquoVisiblendashlight induced photocatalytic degradation of fungi-cide with Fe and Si doped TiO2 nanoparticlesrdquo MaterialsToday Proceedings vol 3 no 2 pp 354ndash361 2016
[7] Maulidiyah T Azis A T Nurwahidah D Wibowo andM Nurdin ldquoPhotoelectrocatalyst of Fe co-doped N-TiO2Tinanotubes pesticide degradation of thiamethoxam underUVndashvisible lightsrdquo Environmental Nanotechnology Moni-toring amp Management vol 8 pp 103ndash111 2017
[8] Q Wang R Jin M Zhang and S Gao ldquoSolvothermalpreparation of Fe-doped TiO2 nanotube arrays for en-hancement in visible light induced photoelectrochemicalperformancerdquo Journal of Alloys and Compounds vol 690pp 139ndash144 2017
[9] C W Soo J C Juan C W Lai S B A Hamid andR M Yusop ldquoFe-doped mesoporous anatase-brookite titaniain the solar-light-induced photodegradation of Reactive Black5 dyerdquo Journal of the Taiwan Institute of Chemical Engineersvol 68 pp 153ndash161 2016
[10] WMekprasart S Suphankij T Tangcharoen A Simpraditpanand W Pecharapa ldquoModification of dye-sensitized solar cellworking electrode using TiO2 nanoparticleN-doped TiO2nanofiber compositesrdquo Physica Status Solidi (A) vol 211 no 8pp 1745ndash1751 2014
[11] Z Wu Z-K Zhang D-Z Guo Y-J Xing and G-M ZhangldquoTitanium oxide nanospheres preparation characterizationand wide-spectral absorptionrdquo Physica Status Solidi (A)vol 209 no 10 pp 2020ndash2026 2012
[12] K Kalantari M Kalbasi M Sohrabi and S J RoyaeeldquoEnhancing the photocatalytic oxidation of dibenzothiopheneusing visible light responsive Fe and N co-doped TiO2nanoparticlesrdquo Ceramics International vol 43 no 1pp 973ndash981 2017
[13] S Larumbe M Monge and C Gomez-Polo ldquoComparativestudy of (N Fe) doped TiO2 photocatalystsrdquo Applied SurfaceScience vol 327 pp 490ndash497 2015
[14] P Huo Z Lu HWang et al ldquoEnhanced photodegradation ofantibiotics solution under visible light with Fe2+Fe3+
immobilized on TiO2fly-ash cenospheres by using ions im-printing technologyrdquo Chemical Engineering Journal vol 172no 2-3 pp 615ndash622 2011
[15] E Marquez Brazon C Piccirillo I S Moreira andP M L Castro ldquoPhotodegradation of pharmaceutical per-sistent pollutants using hydroxyapatite-based materialsrdquoJournal of Environmental Management vol 182 pp 486ndash4952016
[16] L Schlur S Begin-Colin P Gilliot et al ldquoEffect of ball-millingand Fe-Al-doping on the structural aspect and visible lightphotocatalytic activity of TiO2 towards Escherichia coli bac-teria abatementrdquo Materials Science and Engineering Cvol 38 no 1 pp 11ndash19 2014
[17] M Yeganeh N Shahtahmasebi A Kompany et al ldquo(emagnetic characterization of Fe doped TiO2 semiconductingoxide nanoparticles synthesized by solndashgel methodrdquo PhysicaB Condensed Matter vol 511 pp 89ndash98 2017
[18] H Moradi A Eshaghi S R Hosseini and K Ghani ldquoFab-rication of Fe-doped TiO2 nanoparticles and investigation ofphotocatalytic decolorization of reactive red 198 under visiblelight irradiationrdquo Ultrasonics Sonochemistry vol 32pp 314ndash319 2016
[19] M Pazoki M Parsa and R Farhadpour ldquoRemoval of thehormones dexamethasone (DXM) by Ag doped on TiO2photocatalysisrdquo Journal of Environmental Chemical Engi-neering vol 4 no 4 pp 4426ndash4434 2016
[20] Q Wang C Yang G Zhang L Hu and P Wang ldquoPho-tocatalytic Fe-doped TiO2PSF composite UF membranescharacterization and performance on BPA removal undervisible-light irradiationrdquo Chemical Engineering Journalvol 319 pp 39ndash47 2017
[21] N C Birben C S Uyguner-Demirel S S Kavurmaci et alldquoApplication of Fe-doped TiO2 specimens for the solarphotocatalytic degradation of humic acidrdquo Catalysis Todayvol 281 pp 78ndash84 2017
[22] S A Ahmed ldquoFerromagnetism in Cr- Fe- and Ni-dopedTiO2 samplesrdquo Journal of Magnetism and Magnetic Materialsvol 442 pp 152ndash157 2017
[23] Y Sui Q Liu T Jiang and Y Guo ldquoSynthesis of nano-TiO2photocatalysts with tunable Fe doping concentration from Ti-bearing tailingsrdquo Applied Surface Science vol 428pp 1149ndash1158 2018
[24] V Moradi M B G Jun A Blackburn and R A HerringldquoSignificant improvement in visible light photocatalytic ac-tivity of Fe doped TiO2 using an acid treatment processrdquoApplied Surface Science vol 427 pp 791ndash799 2018
[25] E Craciun L Predoana I Atkinson et al ldquoFe3+-doped TiO2nanopowders for photocatalytic mineralization of oxalic acidunder solar light irradiationrdquo Journal of Photochemistry andPhotobiology A Chemistry vol 356 pp 18ndash28 2018
[26] M Zare K Namratha M S (akur and K ByrappaldquoBiocompatibility assessment and photocatalytic activity ofbio-hydrothermal synthesis of ZnO nanoparticles by Dymusvulgaris leaf extractrdquo Materials Research Bulletin vol 109pp 49ndash59 2019
[27] S Shalini R Balasundaraprabhu T Satish Kumar et alldquoEnhanced performance of sodium doped TiO2 nanorodsbased dye sensitized solar cells sensitized with extract frompetals of Hibiscus sabdariffa (Roselle)rdquo Materials Lettersvol 221 pp 192ndash195 2018
[28] A A Kashale K P Gattu K Ghule et al ldquoBiomediated greensynthesis of TiO2 nanoparticles for lithium ion battery ap-plicationrdquo Composites Part B Engineering vol 99 pp 297ndash304 2016
[29] S Shalini N Prabavathy R Balasundaraprabhu et alldquoStudies on DSSC encompassing flower shaped assembly ofNa-doped TiO2 nanorods sensitized with extract from petalsof Kigelia africanardquo Optik vol 155 pp 334ndash343 2018
[30] S Subhapriya and P Gomathipriya ldquoGreen synthesis of ti-tanium dioxide (TiO2) nanoparticles by Trigonella foenum-graecum extract and its antimicrobial propertiesrdquo MicrobialPathogenesis vol 116 pp 215ndash220 2018
Journal of Nanotechnology 9
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
Figure 9 SEM micrographs and EDS spectrum of (a) P-25 TiO2 (b) Fe Ti 0 (c) Fe Ti 005 (d) Fe Ti 0075 and (e) Fe Ti 01magnishycation 150x
Journal of Nanotechnology 7
reduction of 1 eV for the material Fe Ti 01 in comparisonwith the pure TiO2 (Fe Ti 0) synthesized by the meth-odology of green chemistry assisted by ultrasound whichwould allow to use more elaquociently the solar radiation inheterogeneous photocatalytic processes for the degradationof organic pollutants ese results relate to several recentresearch focused on the doping of titanium dioxide with Fe3+ions [56 59ndash61] Moradi et al [18] observed the decreaseof the band gap with the increase of the relationship molar
Fe Ti in catalysts of TiO2 doped with Fe3+ using thetechnique sol-gel
4 Conclusions
In summary TiO2 (anatase phase only) doped with a dif-ferent molar ratio Fe3+ Ti was successfully prepared viagreen synthesis (using the leaves extract of lemongrass plantleaves) assisted ultrasound method followed by calcinatione average crystalline size calculated by XRD pattern wasbetween 937 to 1033 for the TiO2 (Fe Ti 0) and TiO2 (Fe Ti 005) samples respectively e scanning electronmicroscopy with energy-dispersive X-ray (SEM-EDS) showsnanoparticles clusters and elaquociencies of impregnationsbetween 665 and 584 depending on the theoretical dopantamount From PL and CL studies it was conshyrmed thatdoping of Fe (III) ions into TiO2 matrix leads to the in-hibition of recombination of charge carriers thereby en-hancing photochemical quantum elaquociency From UV-VisDRS analysis a reduction of 1 eV was observed for thematerial Fe Ti 01 in comparison with the pure TiO2 (Fe Ti 0) synthesized by the methodology of green chemistryassisted by ultrasound which would allow to use more ef-shyciently the solar radiation in heterogeneous photocatalyticprocesses for the degradation of organic pollutants
Data Availability
e data used to support the shyndings of this study areavailable from the corresponding author upon request
Conflicts of Interest
e authors declare that there are no connoticts of interestregarding the publication of this paper
Acknowledgments
e authors greatly acknowledge the shynancial support fromUniversity de Cartagena (International Internship 201701735) and the Colombian Administrative Department ofScience Technology and Innovation (Colciencias YoungResearchers Program 2017) e authors would also like tothank the Electronic Nanomaterials Physics Research groupof Universidad Complutense de Madrid for providing thefacility of all the equipment used in this research
References
[1] Q Deng Y Liu K Mu et al ldquoPreparation and character-ization of F-modishyed C-TiO2 and its photocatalytic
200 300 400 500 600 700 800
00
02
04
06
08
10
12
Abs
orba
nce (
au)
Wavelength (nm)
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
Figure 10 Typical UV-Vis spectra of bare TiO2 and Fe-TiO2
20 25 30 35 40
0
5
10
15
20
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
(Ahv
)2 (cm
ndash1middoteV
)2
hv (eV)
Figure 11 Tauc plot analysis of bare TiO2 and Fe-TiO2
Sample Ti (atm) O (atm) Fe (atm) Impregnation elaquociency ()P-25 3773 plusmn 17 6227 plusmn 399 mdash mdashFe Ti 0 3777 plusmn 18 5915 plusmn 352 mdash mdashFe Ti 005 3908 plusmn 18 5963 plusmn 357 130 plusmn 01 6653Fe Ti 0075 3732 plusmn 19 6112 plusmn 356 156 plusmn 02 5573Fe Ti 01 4059 plusmn 20 5705 plusmn 351 237 plusmn 02 5838
8 Journal of Nanotechnology
propertiesrdquo Physica Status Solidi (A) vol 212 no 3pp 691ndash697 2015
[2] K S Prasad A Patra G Shruthi and S Chandan ldquoAqueousextract of Saraca indica leaves in the synthesis of copper oxidenanoparticles finding a way towards going greenrdquo Journal ofNanotechnology vol 2017 Article ID 7502610 6 pages 2017
[3] X Wang X Cheng X Yu and X Quan ldquoStudy on surface-enhanced Raman scattering substrate based on titanium oxidenanorods coated with gold nanoparticlesrdquo Journal of Nano-technology vol 2018 Article ID 9602480 9 pages 2018
[4] W Sangchay ldquoWO3-doped TiO2 coating on charcoal acti-vated with increase photocatalytic and antibacterial propertiessynthesized bymicrowave-assisted sol-gel methodrdquo Journal ofNanotechnology vol 2017 Article ID 7902930 7 pages 2017
[5] W Chakhari J Ben Naceur S Ben Taieb I Ben Assaker andR Chtourou ldquoFe-doped TiO2 nanorods with enhancedelectrochemical properties as efficient photoanode materialsrdquoJournal of Alloys and Compounds vol 708 pp 862ndash870 2017
[6] T Kaur A Sraw R K Wanchoo and A P ToorldquoVisiblendashlight induced photocatalytic degradation of fungi-cide with Fe and Si doped TiO2 nanoparticlesrdquo MaterialsToday Proceedings vol 3 no 2 pp 354ndash361 2016
[7] Maulidiyah T Azis A T Nurwahidah D Wibowo andM Nurdin ldquoPhotoelectrocatalyst of Fe co-doped N-TiO2Tinanotubes pesticide degradation of thiamethoxam underUVndashvisible lightsrdquo Environmental Nanotechnology Moni-toring amp Management vol 8 pp 103ndash111 2017
[8] Q Wang R Jin M Zhang and S Gao ldquoSolvothermalpreparation of Fe-doped TiO2 nanotube arrays for en-hancement in visible light induced photoelectrochemicalperformancerdquo Journal of Alloys and Compounds vol 690pp 139ndash144 2017
[9] C W Soo J C Juan C W Lai S B A Hamid andR M Yusop ldquoFe-doped mesoporous anatase-brookite titaniain the solar-light-induced photodegradation of Reactive Black5 dyerdquo Journal of the Taiwan Institute of Chemical Engineersvol 68 pp 153ndash161 2016
[10] WMekprasart S Suphankij T Tangcharoen A Simpraditpanand W Pecharapa ldquoModification of dye-sensitized solar cellworking electrode using TiO2 nanoparticleN-doped TiO2nanofiber compositesrdquo Physica Status Solidi (A) vol 211 no 8pp 1745ndash1751 2014
[11] Z Wu Z-K Zhang D-Z Guo Y-J Xing and G-M ZhangldquoTitanium oxide nanospheres preparation characterizationand wide-spectral absorptionrdquo Physica Status Solidi (A)vol 209 no 10 pp 2020ndash2026 2012
[12] K Kalantari M Kalbasi M Sohrabi and S J RoyaeeldquoEnhancing the photocatalytic oxidation of dibenzothiopheneusing visible light responsive Fe and N co-doped TiO2nanoparticlesrdquo Ceramics International vol 43 no 1pp 973ndash981 2017
[13] S Larumbe M Monge and C Gomez-Polo ldquoComparativestudy of (N Fe) doped TiO2 photocatalystsrdquo Applied SurfaceScience vol 327 pp 490ndash497 2015
[14] P Huo Z Lu HWang et al ldquoEnhanced photodegradation ofantibiotics solution under visible light with Fe2+Fe3+
immobilized on TiO2fly-ash cenospheres by using ions im-printing technologyrdquo Chemical Engineering Journal vol 172no 2-3 pp 615ndash622 2011
[15] E Marquez Brazon C Piccirillo I S Moreira andP M L Castro ldquoPhotodegradation of pharmaceutical per-sistent pollutants using hydroxyapatite-based materialsrdquoJournal of Environmental Management vol 182 pp 486ndash4952016
[16] L Schlur S Begin-Colin P Gilliot et al ldquoEffect of ball-millingand Fe-Al-doping on the structural aspect and visible lightphotocatalytic activity of TiO2 towards Escherichia coli bac-teria abatementrdquo Materials Science and Engineering Cvol 38 no 1 pp 11ndash19 2014
[17] M Yeganeh N Shahtahmasebi A Kompany et al ldquo(emagnetic characterization of Fe doped TiO2 semiconductingoxide nanoparticles synthesized by solndashgel methodrdquo PhysicaB Condensed Matter vol 511 pp 89ndash98 2017
[18] H Moradi A Eshaghi S R Hosseini and K Ghani ldquoFab-rication of Fe-doped TiO2 nanoparticles and investigation ofphotocatalytic decolorization of reactive red 198 under visiblelight irradiationrdquo Ultrasonics Sonochemistry vol 32pp 314ndash319 2016
[19] M Pazoki M Parsa and R Farhadpour ldquoRemoval of thehormones dexamethasone (DXM) by Ag doped on TiO2photocatalysisrdquo Journal of Environmental Chemical Engi-neering vol 4 no 4 pp 4426ndash4434 2016
[20] Q Wang C Yang G Zhang L Hu and P Wang ldquoPho-tocatalytic Fe-doped TiO2PSF composite UF membranescharacterization and performance on BPA removal undervisible-light irradiationrdquo Chemical Engineering Journalvol 319 pp 39ndash47 2017
[21] N C Birben C S Uyguner-Demirel S S Kavurmaci et alldquoApplication of Fe-doped TiO2 specimens for the solarphotocatalytic degradation of humic acidrdquo Catalysis Todayvol 281 pp 78ndash84 2017
[22] S A Ahmed ldquoFerromagnetism in Cr- Fe- and Ni-dopedTiO2 samplesrdquo Journal of Magnetism and Magnetic Materialsvol 442 pp 152ndash157 2017
[23] Y Sui Q Liu T Jiang and Y Guo ldquoSynthesis of nano-TiO2photocatalysts with tunable Fe doping concentration from Ti-bearing tailingsrdquo Applied Surface Science vol 428pp 1149ndash1158 2018
[24] V Moradi M B G Jun A Blackburn and R A HerringldquoSignificant improvement in visible light photocatalytic ac-tivity of Fe doped TiO2 using an acid treatment processrdquoApplied Surface Science vol 427 pp 791ndash799 2018
[25] E Craciun L Predoana I Atkinson et al ldquoFe3+-doped TiO2nanopowders for photocatalytic mineralization of oxalic acidunder solar light irradiationrdquo Journal of Photochemistry andPhotobiology A Chemistry vol 356 pp 18ndash28 2018
[26] M Zare K Namratha M S (akur and K ByrappaldquoBiocompatibility assessment and photocatalytic activity ofbio-hydrothermal synthesis of ZnO nanoparticles by Dymusvulgaris leaf extractrdquo Materials Research Bulletin vol 109pp 49ndash59 2019
[27] S Shalini R Balasundaraprabhu T Satish Kumar et alldquoEnhanced performance of sodium doped TiO2 nanorodsbased dye sensitized solar cells sensitized with extract frompetals of Hibiscus sabdariffa (Roselle)rdquo Materials Lettersvol 221 pp 192ndash195 2018
[28] A A Kashale K P Gattu K Ghule et al ldquoBiomediated greensynthesis of TiO2 nanoparticles for lithium ion battery ap-plicationrdquo Composites Part B Engineering vol 99 pp 297ndash304 2016
[29] S Shalini N Prabavathy R Balasundaraprabhu et alldquoStudies on DSSC encompassing flower shaped assembly ofNa-doped TiO2 nanorods sensitized with extract from petalsof Kigelia africanardquo Optik vol 155 pp 334ndash343 2018
[30] S Subhapriya and P Gomathipriya ldquoGreen synthesis of ti-tanium dioxide (TiO2) nanoparticles by Trigonella foenum-graecum extract and its antimicrobial propertiesrdquo MicrobialPathogenesis vol 116 pp 215ndash220 2018
Journal of Nanotechnology 9
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
reduction of 1 eV for the material Fe Ti 01 in comparisonwith the pure TiO2 (Fe Ti 0) synthesized by the meth-odology of green chemistry assisted by ultrasound whichwould allow to use more elaquociently the solar radiation inheterogeneous photocatalytic processes for the degradationof organic pollutants ese results relate to several recentresearch focused on the doping of titanium dioxide with Fe3+ions [56 59ndash61] Moradi et al [18] observed the decreaseof the band gap with the increase of the relationship molar
Fe Ti in catalysts of TiO2 doped with Fe3+ using thetechnique sol-gel
4 Conclusions
In summary TiO2 (anatase phase only) doped with a dif-ferent molar ratio Fe3+ Ti was successfully prepared viagreen synthesis (using the leaves extract of lemongrass plantleaves) assisted ultrasound method followed by calcinatione average crystalline size calculated by XRD pattern wasbetween 937 to 1033 for the TiO2 (Fe Ti 0) and TiO2 (Fe Ti 005) samples respectively e scanning electronmicroscopy with energy-dispersive X-ray (SEM-EDS) showsnanoparticles clusters and elaquociencies of impregnationsbetween 665 and 584 depending on the theoretical dopantamount From PL and CL studies it was conshyrmed thatdoping of Fe (III) ions into TiO2 matrix leads to the in-hibition of recombination of charge carriers thereby en-hancing photochemical quantum elaquociency From UV-VisDRS analysis a reduction of 1 eV was observed for thematerial Fe Ti 01 in comparison with the pure TiO2 (Fe Ti 0) synthesized by the methodology of green chemistryassisted by ultrasound which would allow to use more ef-shyciently the solar radiation in heterogeneous photocatalyticprocesses for the degradation of organic pollutants
Data Availability
e data used to support the shyndings of this study areavailable from the corresponding author upon request
Conflicts of Interest
e authors declare that there are no connoticts of interestregarding the publication of this paper
Acknowledgments
e authors greatly acknowledge the shynancial support fromUniversity de Cartagena (International Internship 201701735) and the Colombian Administrative Department ofScience Technology and Innovation (Colciencias YoungResearchers Program 2017) e authors would also like tothank the Electronic Nanomaterials Physics Research groupof Universidad Complutense de Madrid for providing thefacility of all the equipment used in this research
References
[1] Q Deng Y Liu K Mu et al ldquoPreparation and character-ization of F-modishyed C-TiO2 and its photocatalytic
200 300 400 500 600 700 800
00
02
04
06
08
10
12
Abs
orba
nce (
au)
Wavelength (nm)
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
Figure 10 Typical UV-Vis spectra of bare TiO2 and Fe-TiO2
20 25 30 35 40
0
5
10
15
20
FeTi = 01FeTi = 0075
FeTi = 005FeTi = 0
(Ahv
)2 (cm
ndash1middoteV
)2
hv (eV)
Figure 11 Tauc plot analysis of bare TiO2 and Fe-TiO2
Sample Ti (atm) O (atm) Fe (atm) Impregnation elaquociency ()P-25 3773 plusmn 17 6227 plusmn 399 mdash mdashFe Ti 0 3777 plusmn 18 5915 plusmn 352 mdash mdashFe Ti 005 3908 plusmn 18 5963 plusmn 357 130 plusmn 01 6653Fe Ti 0075 3732 plusmn 19 6112 plusmn 356 156 plusmn 02 5573Fe Ti 01 4059 plusmn 20 5705 plusmn 351 237 plusmn 02 5838
8 Journal of Nanotechnology
propertiesrdquo Physica Status Solidi (A) vol 212 no 3pp 691ndash697 2015
[2] K S Prasad A Patra G Shruthi and S Chandan ldquoAqueousextract of Saraca indica leaves in the synthesis of copper oxidenanoparticles finding a way towards going greenrdquo Journal ofNanotechnology vol 2017 Article ID 7502610 6 pages 2017
[3] X Wang X Cheng X Yu and X Quan ldquoStudy on surface-enhanced Raman scattering substrate based on titanium oxidenanorods coated with gold nanoparticlesrdquo Journal of Nano-technology vol 2018 Article ID 9602480 9 pages 2018
[4] W Sangchay ldquoWO3-doped TiO2 coating on charcoal acti-vated with increase photocatalytic and antibacterial propertiessynthesized bymicrowave-assisted sol-gel methodrdquo Journal ofNanotechnology vol 2017 Article ID 7902930 7 pages 2017
[5] W Chakhari J Ben Naceur S Ben Taieb I Ben Assaker andR Chtourou ldquoFe-doped TiO2 nanorods with enhancedelectrochemical properties as efficient photoanode materialsrdquoJournal of Alloys and Compounds vol 708 pp 862ndash870 2017
[6] T Kaur A Sraw R K Wanchoo and A P ToorldquoVisiblendashlight induced photocatalytic degradation of fungi-cide with Fe and Si doped TiO2 nanoparticlesrdquo MaterialsToday Proceedings vol 3 no 2 pp 354ndash361 2016
[7] Maulidiyah T Azis A T Nurwahidah D Wibowo andM Nurdin ldquoPhotoelectrocatalyst of Fe co-doped N-TiO2Tinanotubes pesticide degradation of thiamethoxam underUVndashvisible lightsrdquo Environmental Nanotechnology Moni-toring amp Management vol 8 pp 103ndash111 2017
[8] Q Wang R Jin M Zhang and S Gao ldquoSolvothermalpreparation of Fe-doped TiO2 nanotube arrays for en-hancement in visible light induced photoelectrochemicalperformancerdquo Journal of Alloys and Compounds vol 690pp 139ndash144 2017
[9] C W Soo J C Juan C W Lai S B A Hamid andR M Yusop ldquoFe-doped mesoporous anatase-brookite titaniain the solar-light-induced photodegradation of Reactive Black5 dyerdquo Journal of the Taiwan Institute of Chemical Engineersvol 68 pp 153ndash161 2016
[10] WMekprasart S Suphankij T Tangcharoen A Simpraditpanand W Pecharapa ldquoModification of dye-sensitized solar cellworking electrode using TiO2 nanoparticleN-doped TiO2nanofiber compositesrdquo Physica Status Solidi (A) vol 211 no 8pp 1745ndash1751 2014
[11] Z Wu Z-K Zhang D-Z Guo Y-J Xing and G-M ZhangldquoTitanium oxide nanospheres preparation characterizationand wide-spectral absorptionrdquo Physica Status Solidi (A)vol 209 no 10 pp 2020ndash2026 2012
[12] K Kalantari M Kalbasi M Sohrabi and S J RoyaeeldquoEnhancing the photocatalytic oxidation of dibenzothiopheneusing visible light responsive Fe and N co-doped TiO2nanoparticlesrdquo Ceramics International vol 43 no 1pp 973ndash981 2017
[13] S Larumbe M Monge and C Gomez-Polo ldquoComparativestudy of (N Fe) doped TiO2 photocatalystsrdquo Applied SurfaceScience vol 327 pp 490ndash497 2015
[14] P Huo Z Lu HWang et al ldquoEnhanced photodegradation ofantibiotics solution under visible light with Fe2+Fe3+
immobilized on TiO2fly-ash cenospheres by using ions im-printing technologyrdquo Chemical Engineering Journal vol 172no 2-3 pp 615ndash622 2011
[15] E Marquez Brazon C Piccirillo I S Moreira andP M L Castro ldquoPhotodegradation of pharmaceutical per-sistent pollutants using hydroxyapatite-based materialsrdquoJournal of Environmental Management vol 182 pp 486ndash4952016
[16] L Schlur S Begin-Colin P Gilliot et al ldquoEffect of ball-millingand Fe-Al-doping on the structural aspect and visible lightphotocatalytic activity of TiO2 towards Escherichia coli bac-teria abatementrdquo Materials Science and Engineering Cvol 38 no 1 pp 11ndash19 2014
[17] M Yeganeh N Shahtahmasebi A Kompany et al ldquo(emagnetic characterization of Fe doped TiO2 semiconductingoxide nanoparticles synthesized by solndashgel methodrdquo PhysicaB Condensed Matter vol 511 pp 89ndash98 2017
[18] H Moradi A Eshaghi S R Hosseini and K Ghani ldquoFab-rication of Fe-doped TiO2 nanoparticles and investigation ofphotocatalytic decolorization of reactive red 198 under visiblelight irradiationrdquo Ultrasonics Sonochemistry vol 32pp 314ndash319 2016
[19] M Pazoki M Parsa and R Farhadpour ldquoRemoval of thehormones dexamethasone (DXM) by Ag doped on TiO2photocatalysisrdquo Journal of Environmental Chemical Engi-neering vol 4 no 4 pp 4426ndash4434 2016
[20] Q Wang C Yang G Zhang L Hu and P Wang ldquoPho-tocatalytic Fe-doped TiO2PSF composite UF membranescharacterization and performance on BPA removal undervisible-light irradiationrdquo Chemical Engineering Journalvol 319 pp 39ndash47 2017
[21] N C Birben C S Uyguner-Demirel S S Kavurmaci et alldquoApplication of Fe-doped TiO2 specimens for the solarphotocatalytic degradation of humic acidrdquo Catalysis Todayvol 281 pp 78ndash84 2017
[22] S A Ahmed ldquoFerromagnetism in Cr- Fe- and Ni-dopedTiO2 samplesrdquo Journal of Magnetism and Magnetic Materialsvol 442 pp 152ndash157 2017
[23] Y Sui Q Liu T Jiang and Y Guo ldquoSynthesis of nano-TiO2photocatalysts with tunable Fe doping concentration from Ti-bearing tailingsrdquo Applied Surface Science vol 428pp 1149ndash1158 2018
[24] V Moradi M B G Jun A Blackburn and R A HerringldquoSignificant improvement in visible light photocatalytic ac-tivity of Fe doped TiO2 using an acid treatment processrdquoApplied Surface Science vol 427 pp 791ndash799 2018
[25] E Craciun L Predoana I Atkinson et al ldquoFe3+-doped TiO2nanopowders for photocatalytic mineralization of oxalic acidunder solar light irradiationrdquo Journal of Photochemistry andPhotobiology A Chemistry vol 356 pp 18ndash28 2018
[26] M Zare K Namratha M S (akur and K ByrappaldquoBiocompatibility assessment and photocatalytic activity ofbio-hydrothermal synthesis of ZnO nanoparticles by Dymusvulgaris leaf extractrdquo Materials Research Bulletin vol 109pp 49ndash59 2019
[27] S Shalini R Balasundaraprabhu T Satish Kumar et alldquoEnhanced performance of sodium doped TiO2 nanorodsbased dye sensitized solar cells sensitized with extract frompetals of Hibiscus sabdariffa (Roselle)rdquo Materials Lettersvol 221 pp 192ndash195 2018
[28] A A Kashale K P Gattu K Ghule et al ldquoBiomediated greensynthesis of TiO2 nanoparticles for lithium ion battery ap-plicationrdquo Composites Part B Engineering vol 99 pp 297ndash304 2016
[29] S Shalini N Prabavathy R Balasundaraprabhu et alldquoStudies on DSSC encompassing flower shaped assembly ofNa-doped TiO2 nanorods sensitized with extract from petalsof Kigelia africanardquo Optik vol 155 pp 334ndash343 2018
[30] S Subhapriya and P Gomathipriya ldquoGreen synthesis of ti-tanium dioxide (TiO2) nanoparticles by Trigonella foenum-graecum extract and its antimicrobial propertiesrdquo MicrobialPathogenesis vol 116 pp 215ndash220 2018
Journal of Nanotechnology 9
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
propertiesrdquo Physica Status Solidi (A) vol 212 no 3pp 691ndash697 2015
[2] K S Prasad A Patra G Shruthi and S Chandan ldquoAqueousextract of Saraca indica leaves in the synthesis of copper oxidenanoparticles finding a way towards going greenrdquo Journal ofNanotechnology vol 2017 Article ID 7502610 6 pages 2017
[3] X Wang X Cheng X Yu and X Quan ldquoStudy on surface-enhanced Raman scattering substrate based on titanium oxidenanorods coated with gold nanoparticlesrdquo Journal of Nano-technology vol 2018 Article ID 9602480 9 pages 2018
[4] W Sangchay ldquoWO3-doped TiO2 coating on charcoal acti-vated with increase photocatalytic and antibacterial propertiessynthesized bymicrowave-assisted sol-gel methodrdquo Journal ofNanotechnology vol 2017 Article ID 7902930 7 pages 2017
[5] W Chakhari J Ben Naceur S Ben Taieb I Ben Assaker andR Chtourou ldquoFe-doped TiO2 nanorods with enhancedelectrochemical properties as efficient photoanode materialsrdquoJournal of Alloys and Compounds vol 708 pp 862ndash870 2017
[6] T Kaur A Sraw R K Wanchoo and A P ToorldquoVisiblendashlight induced photocatalytic degradation of fungi-cide with Fe and Si doped TiO2 nanoparticlesrdquo MaterialsToday Proceedings vol 3 no 2 pp 354ndash361 2016
[7] Maulidiyah T Azis A T Nurwahidah D Wibowo andM Nurdin ldquoPhotoelectrocatalyst of Fe co-doped N-TiO2Tinanotubes pesticide degradation of thiamethoxam underUVndashvisible lightsrdquo Environmental Nanotechnology Moni-toring amp Management vol 8 pp 103ndash111 2017
[8] Q Wang R Jin M Zhang and S Gao ldquoSolvothermalpreparation of Fe-doped TiO2 nanotube arrays for en-hancement in visible light induced photoelectrochemicalperformancerdquo Journal of Alloys and Compounds vol 690pp 139ndash144 2017
[9] C W Soo J C Juan C W Lai S B A Hamid andR M Yusop ldquoFe-doped mesoporous anatase-brookite titaniain the solar-light-induced photodegradation of Reactive Black5 dyerdquo Journal of the Taiwan Institute of Chemical Engineersvol 68 pp 153ndash161 2016
[10] WMekprasart S Suphankij T Tangcharoen A Simpraditpanand W Pecharapa ldquoModification of dye-sensitized solar cellworking electrode using TiO2 nanoparticleN-doped TiO2nanofiber compositesrdquo Physica Status Solidi (A) vol 211 no 8pp 1745ndash1751 2014
[11] Z Wu Z-K Zhang D-Z Guo Y-J Xing and G-M ZhangldquoTitanium oxide nanospheres preparation characterizationand wide-spectral absorptionrdquo Physica Status Solidi (A)vol 209 no 10 pp 2020ndash2026 2012
[12] K Kalantari M Kalbasi M Sohrabi and S J RoyaeeldquoEnhancing the photocatalytic oxidation of dibenzothiopheneusing visible light responsive Fe and N co-doped TiO2nanoparticlesrdquo Ceramics International vol 43 no 1pp 973ndash981 2017
[13] S Larumbe M Monge and C Gomez-Polo ldquoComparativestudy of (N Fe) doped TiO2 photocatalystsrdquo Applied SurfaceScience vol 327 pp 490ndash497 2015
[14] P Huo Z Lu HWang et al ldquoEnhanced photodegradation ofantibiotics solution under visible light with Fe2+Fe3+
immobilized on TiO2fly-ash cenospheres by using ions im-printing technologyrdquo Chemical Engineering Journal vol 172no 2-3 pp 615ndash622 2011
[15] E Marquez Brazon C Piccirillo I S Moreira andP M L Castro ldquoPhotodegradation of pharmaceutical per-sistent pollutants using hydroxyapatite-based materialsrdquoJournal of Environmental Management vol 182 pp 486ndash4952016
[16] L Schlur S Begin-Colin P Gilliot et al ldquoEffect of ball-millingand Fe-Al-doping on the structural aspect and visible lightphotocatalytic activity of TiO2 towards Escherichia coli bac-teria abatementrdquo Materials Science and Engineering Cvol 38 no 1 pp 11ndash19 2014
[17] M Yeganeh N Shahtahmasebi A Kompany et al ldquo(emagnetic characterization of Fe doped TiO2 semiconductingoxide nanoparticles synthesized by solndashgel methodrdquo PhysicaB Condensed Matter vol 511 pp 89ndash98 2017
[18] H Moradi A Eshaghi S R Hosseini and K Ghani ldquoFab-rication of Fe-doped TiO2 nanoparticles and investigation ofphotocatalytic decolorization of reactive red 198 under visiblelight irradiationrdquo Ultrasonics Sonochemistry vol 32pp 314ndash319 2016
[19] M Pazoki M Parsa and R Farhadpour ldquoRemoval of thehormones dexamethasone (DXM) by Ag doped on TiO2photocatalysisrdquo Journal of Environmental Chemical Engi-neering vol 4 no 4 pp 4426ndash4434 2016
[20] Q Wang C Yang G Zhang L Hu and P Wang ldquoPho-tocatalytic Fe-doped TiO2PSF composite UF membranescharacterization and performance on BPA removal undervisible-light irradiationrdquo Chemical Engineering Journalvol 319 pp 39ndash47 2017
[21] N C Birben C S Uyguner-Demirel S S Kavurmaci et alldquoApplication of Fe-doped TiO2 specimens for the solarphotocatalytic degradation of humic acidrdquo Catalysis Todayvol 281 pp 78ndash84 2017
[22] S A Ahmed ldquoFerromagnetism in Cr- Fe- and Ni-dopedTiO2 samplesrdquo Journal of Magnetism and Magnetic Materialsvol 442 pp 152ndash157 2017
[23] Y Sui Q Liu T Jiang and Y Guo ldquoSynthesis of nano-TiO2photocatalysts with tunable Fe doping concentration from Ti-bearing tailingsrdquo Applied Surface Science vol 428pp 1149ndash1158 2018
[24] V Moradi M B G Jun A Blackburn and R A HerringldquoSignificant improvement in visible light photocatalytic ac-tivity of Fe doped TiO2 using an acid treatment processrdquoApplied Surface Science vol 427 pp 791ndash799 2018
[25] E Craciun L Predoana I Atkinson et al ldquoFe3+-doped TiO2nanopowders for photocatalytic mineralization of oxalic acidunder solar light irradiationrdquo Journal of Photochemistry andPhotobiology A Chemistry vol 356 pp 18ndash28 2018
[26] M Zare K Namratha M S (akur and K ByrappaldquoBiocompatibility assessment and photocatalytic activity ofbio-hydrothermal synthesis of ZnO nanoparticles by Dymusvulgaris leaf extractrdquo Materials Research Bulletin vol 109pp 49ndash59 2019
[27] S Shalini R Balasundaraprabhu T Satish Kumar et alldquoEnhanced performance of sodium doped TiO2 nanorodsbased dye sensitized solar cells sensitized with extract frompetals of Hibiscus sabdariffa (Roselle)rdquo Materials Lettersvol 221 pp 192ndash195 2018
[28] A A Kashale K P Gattu K Ghule et al ldquoBiomediated greensynthesis of TiO2 nanoparticles for lithium ion battery ap-plicationrdquo Composites Part B Engineering vol 99 pp 297ndash304 2016
[29] S Shalini N Prabavathy R Balasundaraprabhu et alldquoStudies on DSSC encompassing flower shaped assembly ofNa-doped TiO2 nanorods sensitized with extract from petalsof Kigelia africanardquo Optik vol 155 pp 334ndash343 2018
[30] S Subhapriya and P Gomathipriya ldquoGreen synthesis of ti-tanium dioxide (TiO2) nanoparticles by Trigonella foenum-graecum extract and its antimicrobial propertiesrdquo MicrobialPathogenesis vol 116 pp 215ndash220 2018
Journal of Nanotechnology 9
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
[31] N Arabi A Kianvash A Hajalilou and E Abouzari-lotf ldquoAfacile and green synthetic approach toward fabrication ofAlcea- and (yme-stabilized TiO2 nanoparticles for photo-catalytic applicationsrdquo Arabian Journal of Chemistry 2018 Inpress
[32] M Atarod M Nasrollahzadeh and S Mohammad SajadildquoEuphorbia heterophylla leaf extract mediated green synthesisof AgTiO2 nanocomposite and investigation of its excellentcatalytic activity for reduction of variety of dyes in waterrdquoJournal of Colloid and Interface Science vol 462 pp 272ndash2792016
[33] M Sundrarajan K Bama M Bhavani et al ldquoObtaining ti-tanium dioxide nanoparticles with spherical shape and an-timicrobial properties using M citrifolia leaves extract byhydrothermal methodrdquo Journal of Photochemistry and Pho-tobiology B Biology vol 171 pp 117ndash124 2017
[34] P Rajiv C Jayaseelan C Kamaraj S R R Rajasree andR Regina ldquoIn vitro antimalarial activity of synthesized TiO2nanoparticles using Momordica charantia leaf extract againstPlasmodium falciparumrdquo Journal of Applied Biomedicinevol 16 no 4 pp 378ndash386 2018
[35] S P Goutam G Saxena V Singh A K YadavR N Bharagava and K B (apa ldquoGreen synthesis of TiO2nanoparticles using leaf extract of Jatropha curcas L forphotocatalytic degradation of tannery wastewaterrdquo ChemicalEngineering Journal vol 336 pp 386ndash396 2018
[36] P Jegadeeswaran P Rajiv P Vanathi S Rajeshwari andR Venckatesh ldquoA novel green technology synthesis andcharacterization of AgTiO2 nanocomposites using Padinatetrastromatica (seaweed) extractrdquo Materials Letters vol 166pp 137ndash139 2016
[37] B Balakrishnan S Paramasivam and A Arulkumar ldquoEval-uation of the lemongrass plant (Cymbopogon citratus)extracted in different solvents for antioxidant and antibac-terial activity against human pathogensrdquoAsian Pacific Journalof Tropical Disease vol 4 pp S134ndashS139 2014
[38] T S Geetha and N Geetha ldquoPhytochemical screeningquantitative analysis of primary and secondary metabolites ofCymbopogan citratus (DC) stapf Leaves from Kodaikanalhills Tamilnadurdquo International Journal of PharmTech Re-search vol 6 no 2 pp 521ndash529 2014
[39] S Sood A Umar S K Mehta and S K Kansal ldquoHighlyeffective Fe-doped TiO2 nanoparticles photocatalysts forvisible-light driven photocatalytic degradation of toxic or-ganic compoundsrdquo Journal of Colloid and Interface Sciencevol 450 pp 213ndash223 2015
[40] L Venzon L N B Mariano L B Somensi et al ldquoEssential oilof Cymbopogon citratus (lemongrass) and geraniol but notcitral promote gastric healing activity in micerdquo Biomedicineamp Pharmacotherapy vol 98 pp 118ndash124 2018
[41] M Nasrollahzadeh and S M Sajadi ldquoSynthesis and charac-terization of titanium dioxide nanoparticles using Euphorbiaheteradena Jaub root extract and evaluation of their stabilityrdquoCeramics International vol 41 no 10 pp 14435ndash14439 2015
[42] G Rajakumar A A Rahuman B Priyamvada V G KhannaD K Kumar and P J Sujin ldquoEclipta prostrata leaf aqueousextract mediated synthesis of titanium dioxide nanoparticlesrdquoMaterials Letters vol 68 pp 115ndash117 2012
[43] T Santhoshkumar A A Rahuman C Jayaseelan et alldquoGreen synthesis of titanium dioxide nanoparticles usingPsidium guajava extract and its antibacterial and antioxidantpropertiesrdquo Asian Pacific Journal of Tropical Medicine vol 7no 12 pp 968ndash976 2014
[44] V Sivaranjani and P Philominathan ldquoSynthesize of Titaniumdioxide nanoparticles using Moringa oleifera leaves andevaluation of wound healing activityrdquo Wound Medicinevol 12 pp 1ndash5 2016
[45] P Verma and S K Samanta ldquoContinuous ultrasonic stim-ulation based direct green synthesis of pure anatase-TiO2nanoparticles with better separability and reusability forphotocatalytic water decontaminationrdquo Materials ResearchExpress vol 5 no 6 pp 49ndash65 2018
[46] K Logaranjan A J Raiza S C B Gopinath Y Chen andK Pandian ldquoShape- and size-controlled synthesis of silvernanoparticles using Aloe vera plant extract and their anti-microbial activityrdquo Nanoscale Research Letters vol 11 no 1p 520 2016
[47] N K R Bogireddy U Pal L M Gomez and V AgarwalldquoSize controlled green synthesis of gold nanoparticles usingCoffea arabica seed extract and their catalytic performance in4-nitrophenol reductionrdquo RSC Advances vol 8 no 44pp 24819ndash24826 2018
[48] M Kinoshita and Y Shimoyama ldquoPhotocatalytic activity ofmixed-phase titanium oxide synthesized by supercritical sol-gel reactionrdquo Journal of Supercritical Fluids vol 138pp 29ndash35 2018
[49] C M Phan and H M Nguyen ldquoRole of capping agent in wetsynthesis of nanoparticlesrdquo Journal of Physical Chemistry Avol 121 no 17 pp 3213ndash3219 2017
[50] R Ambati and P R Gogate ldquoUltrasound assisted synthesis ofiron doped TiO2 catalystrdquo Ultrasonics sonochemistry vol 40pp 91ndash100 2018
[51] A G Ilie M Scarisoareanu I Morjan E Dutu M Badiceanuand I Mihailescu ldquoPrincipal component analysis of Ramanspectra for TiO2 nanoparticle characterizationrdquo AppliedSurface Science vol 417 pp 93ndash103 2017
[52] T Ali P Tripathi A Azam et al ldquoPhotocatalytic performanceof Fe-doped TiO2 nanoparticles under visible-light irradia-tionrdquo Materials Research Express vol 4 no 1 article 0150222017
[53] M Barberio P Barone V Pingitore and A BonannoldquoOptical properties of TiO2 anatasemdashcarbon nanotubescomposites studied by cathodoluminescence spectroscopyrdquoSuperlattices and Microstructures vol 51 no 1 pp 177ndash1832012
[54] M Enachi M A Stevens-Kalceff A Sarua V Ursaki andI Tiginyanu ldquoDesign of titania nanotube structures by fo-cused laser beam direct writingrdquo Journal of Applied Physicsvol 114 no 23 article 234302 2013
[55] L Lin H Wang W Jiang A R Mkaouar and P XuldquoComparison study on photocatalytic oxidation of pharma-ceuticals by TiO2 -Fe and TiO2 -reduced graphene oxidenanocomposites immobilized on optical fibersrdquo Journal ofHazardous Materials vol 333 pp 162ndash168 2017
[56] M Crisan D Mardare A Ianculescu et al ldquoIron doped TiO2films and their photoactivity in nitrobenzene removal fromwaterrdquo Applied Surface Science vol 455 pp 201ndash215 2018
[57] A J Haider R H ALndashAnbari G R Kadhim andC T Salame ldquoExploring potential environmental applicationsof TiO2 nanoparticlesrdquo Energy Procedia vol 119 pp 332ndash3452017
[58] M K Hossain A A Mortuza S K Sen et al ldquoA comparativestudy on the influence of pure anatase and Degussa-P25 TiO2nanomaterials on the structural and optical properties of dyesensitized solar cell (DSSC) photoanoderdquo Optik vol 171pp 507ndash516 2018
10 Journal of Nanotechnology
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
[59] J Li D Ren Z Wu et al ldquoFlame retardant and visible light-activated Fe-doped TiO2 thin films anchored to wood surfacesfor the photocatalytic degradation of gaseous formaldehyderdquoJournal of Colloid and Interface Science vol 530 pp 78ndash872018
[60] A Akbar A Payan M Fattahi S Jor and B KakavandildquoPhotocatalytic degradation of rhodamine B and real textilewastewater using Fe-doped TiO2 anchored on reduced gra-phene oxide (Fe-TiO2rGO) characterization and feasibility mechanism and pathway studiesrdquo Applied Surface Sciencevol 462 pp 549ndash564 2018
[61] J Shi G Chen G Zeng et al ldquoHydrothermal synthesis ofgraphene wrapped Fe-doped TiO2 nanospheres with highphotocatalysis performancerdquo Ceramics International vol 44no 7 pp 7473ndash7480 2018
Journal of Nanotechnology 11
CorrosionInternational Journal of
Hindawiwwwhindawicom Volume 2018
Advances in
Materials Science and EngineeringHindawiwwwhindawicom Volume 2018
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