CONTENTS Volume 199, March 2013 Flexible deposition of TiO 2 electrodes for photocatalytic applications: Modulation of the crystal phase as a function of the layer thickness C. Tealdi, E. Quartarone, P. Galinetto, M.S. Grandi and P. Mustarelli page 1 C-AFM images (2 2 mm 2 ) of TiO 2 thin films deposited at 750 1C with different thicknesses: (a) 50 nm [Z=40 nm]; (b) 100 nm [Z=60 nm]; (c) 400 nm [Z=120 nm]. Temperature-dependent Raman scattering study on Cs 4 W 11 O 35 and Rb 4 W 11 O 35 systems K. Pereira da Silva, J. Santos Coelho, M. Maczka, W. Paraguassu, P.T.C. Freire, J. Mendes Filho and J. Hanuza page 7 Valence Balanced Hexagonal Bronzes obtained by partial substitu- tion of the tungsten atoms in the A x WO 3 structure by atoms with lower valence state. These materials undergo a number of phase transitions and display ferroelectric or anti-ferroelectric properties associated with reversible dipole orientations arising from displacements of tungsten atoms from the center of the WO 6 octahedral units. In the present work we report mainly results of temperature Raman scattering experiment on Cs 4 W 11 O 35 and Rb 4 W 11 O 35 hexatungstates in the 30–295 K temperature range. Synthesis of hollow spherical tantalum oxide nanoparticles and their photocatalytic activity for hydrogen production Sen Lin, Lei Shi, Hisao Yoshida, Mingrun Li and Xiaodong Zou page 15 TEM images of the as-prepared HSTaO show that a major portion of the material consists of hollow sphere-like nanoparticles with particle sizes ranging from 50–200 nm in diameter. Crystal structure modeling, electrical and thermal characterization of triple molybdates RbCrTi 0.5 (MoO 4 ) 3 (R=Fe, Cr) Sesegma G. Dorzhieva, Bair G. Bazarov, Alexey K. Subanakov and Jibzema G. Bazarova page 21 Crystal structure of RbRTi 0.5 (MoO 4 ) 3 (R=Fe, Cr) along c-axis. Abstracted/indexed in BioEngineering Abstracts, Chemical Abstracts, Coal Abstracts, Current Contents/Physics, Chemical, & Earth Sciences, Engineering Index, Research Alert, SCISEARCH, Science Abstracts, and Science Citation Index. Also covered in the abstract and citation database SciVerse SCOPUS s . Full text available on SciVerse ScienceDirect s . Continued
Transcript
CONTENTS
Volume 199, March 2013
Abstracted/& Earth Sccovered in
indexed in BioEngineering Abstracts, Chemical Abstracts, Coal Abstracts, Current Contents/Physics, Chemical,iences, Engineering Index, Research Alert, SCISEARCH, Science Abstracts, and Science Citation Index. Alsothe abstract and citation database SciVerse SCOPUSs. Full text available on SciVerse ScienceDirects.
Flexible deposition of TiO2 electrodes for photocatalytic
applications: Modulation of the crystal phase as a function of
the layer thickness
C. Tealdi, E. Quartarone, P. Galinetto, M.S. Grandi andP. Mustarellipage 1
C-AFM images (2� 2 mm2) of TiO2 thin films deposited at 750 1Cwith different thicknesses: (a) 50 nm [Z=40 nm]; (b) 100 nm[Z=60 nm]; (c) 400 nm [Z=120 nm].
Temperature-dependent Raman scattering study on
Cs4W11O35 and Rb4W11O35 systems
K. Pereira da Silva, J. Santos Coelho, M. Maczka, W.Paraguassu, P.T.C. Freire, J. Mendes Filho and J. Hanuzapage 7
Valence Balanced Hexagonal Bronzes obtained by partial substitu-tion of the tungsten atoms in the AxWO3 structure by atomswith lower valence state. These materials undergo a number ofphase transitions and display ferroelectric or anti-ferroelectricproperties associated with reversible dipole orientations arisingfrom displacements of tungsten atoms from the centerof the WO6 octahedral units. In the present work we reportmainly results of temperature Raman scattering experiment onCs4W11O35 and Rb4W11O35 hexatungstates in the 30–295 Ktemperature range.
Synthesis of hollow spherical tantalum oxide nanoparticles
and their photocatalytic activity for hydrogen production
Sen Lin, Lei Shi, Hisao Yoshida, Mingrun Li andXiaodong Zoupage 15
TEM images of the as-prepared HSTaO show that a major portionof the material consists of hollow sphere-like nanoparticles withparticle sizes ranging from 50–200 nm in diameter.
Crystal structure modeling, electrical and thermal
characterization of triple molybdates RbCrTi0.5(MoO4)3(R=Fe, Cr)
Sesegma G. Dorzhieva, Bair G. Bazarov, Alexey K.Subanakov and Jibzema G. Bazarovapage 21
Crystal structure of RbRTi0.5(MoO4)3 (R=Fe, Cr) along c-axis.
Continued
Theoretical study of phase stability, magnetization and
lattice vibrations of Fe23CB6 structure with Cr23C6 prototype
Pair potentials based on ab initio calculations and on the lattice-inversion method have been used to calculate the structuralproperties of a new compound Fe23CB6. The results show thatFe23CB6 possess the Cr23C6 prototype of structure, and the carbonsatoms are positioned at 4a sites in Fe23CB6 compound. Thecalculated lattice constants are similar to observed results fromliteratures. Further, the stability of the structure is furtherconfirmed through molecular dynamic simulations at differenttemperatures. In addition, we have calculated the magneticmoments of Fe22NiB6, Fe23C6, Fe23B6 and Fe23CB6 compounds.Furthermore, the phonon densities of states (DOS) of thesecomplex compounds are evaluated for the first time.
Influence of the network modifier on the characteristics of
MSnO3 (M=Sr and Ca) thin films synthesized by chemical
solution deposition
M.C.F. Alves, R.M.M. Marinho, G.P. Casali, M. Siu-Li,S. Deputier, M. Guilloux-Viry, A.G. Souza, E. Longo, I.T.Weber, I.M.G. Santos and V. Bouquetpage 34
The morphology of films on sapphire substrate was stronglyinfluenced by the network modifier.
Tuning structural topologies of five photoluminescent Cd(II)
coordination polymers through modifying the substitute
With different substituted groups in the organic ligands, five compoundsexhibit five distinct framework structures. The results reveal a newapproach toward tuning structural topologies of coordination polymersthrough modifying the substitute groups in organic ligands.
Influence of post-treatment temperature of TNTa
photoelectrodes on photoelectrochemical properties and
Photophysical chemistry processes and the degradation of 4-NP onTNTa photoelectrodes was showed in the graphical. The overallscheme of TNTa photoelectrodes (A) movement of photoelectrons andholes without bias potentials; (B) movement of photoelectrons andholes at applied bias potentials; the local enlargement of the part inblack open circle of (A) showed the mixed crystal effect. The numberrefers (1) transmission process of photoelectrons and holes; (2)Recombination process of photoelectrons and holes; Arrow representmove direction of photoelectons. A-anatase TiO2, R-rutile TiO2.
Novel bismuth oxophosphate halides [Bi8O8][BiO2](PO4)2X(X=Cl, Br) based on oxocentered 2D blocks and their
relationships to the Aurivillius phases
Michael S. Kozin, Almaz Aliev, Marie Colmont, OlivierMentre, Oleg I. Siidra and Sergey V. Krivovichevpage 56
The scheme of the formation of ([O8Bi8][O2Bi])7þ oxocentered
block in the structures of [Bi8O8][BiO2](PO4)2X (X ¼ Cl, Br)(designations: OBi4 tetrahedra – red, OBi3 triangles – green).
Crystal structure of Li4ZnTeO6 and revision of Li3Cu2SbO6
V.B. Nalbandyan, M. Avdeev and M.A. Evstigneevapage 62
Crystal structure of Li4ZnTeO6: a polyhedral presentation.
b-HfCuGe—A new polymorph of HfCuGe with a novel
structure type
Leslie M. Schoop, Jared M. Allred, Ni Ni, D. Hirai,Julia Krez, Michael Schwall, Huiwen Ji, Mazhar N. Aliand R.J. Cavapage 66
Crystal structure of b-HfCuGe (right) and the coordination of thedifferent atoms in b-HfCuGe (left).
Solid solutions of platinum(II) and palladium(II) oxalato-
Solid solutions of platinum(II) and palladium(II) oxalato-complexsalt as precursors of nanoalloys.
Continued
Evolutionary search for BiInS3 crystal structure and
predicting its second-order nonlinear optical property
Chen-sheng Lin, Wen-dan Cheng, Zhong-zhen Luo andGuo-liang Chaipage 78
The most stable P21 structure (left) and the meta-stable Pnmastructure (right) for BiInS3 crystal predicted by ab initioevolutionary algorithm.
The composite structure of mixed t-(Ag, Cu)xV2O5
bronzes—Evidence for T dependant guest-species ordering
and mobility
Wilfred Hermes, Mickael Dolle, Patrick Rozier and SvenLidinpage 84
Overview of the structure of t1-[AgCu]0.92V2O5. Note how Cu ions(brown) are modulated in the direction of the columns only whilethe silver ions (green) are displaced in all directions.
Investigation on the thermoelectric properties of
nanostructured Cr1�xTixSi2S. Karuppaiah, M. Beaudhuin and R. Viennoispage 90
Power factor for CrSi2 and Cr1�xTixSi2 for x=0.03, 0.06, 0.1, 0.15.We see that the optimum is obtained for 10% Ti doping. If wecompare it with the power factor of CrSi2 it is increased by a factor2 at 800 K.
Characteristic features of the structural properties, phase
transitions, and ferroelastic properties in LiK1�xRbxSO4
(x=0, 0.2, and 1) crystals
Ae Ran Lim, Ho Hyoun Kim and Moohee Leepage 96
We report a systematic nuclear magnetic resonance (NMR) studyof alkaline ions in LiK1�xRbxSO4 (x=0, 0.2, and 1) crystals,which was performed to investigate the effects of the randomdistribution of the Rb substitutional cation on the sequence ofphase transitions.
Structural and magnetic investigation of Fe3þ and Mg2þ
substitution into the trigonal bipyramidal site of InGaCuO4
Rosa Grajczyk, Romain Berthelot, Sean Muir, A.W.Sleight and M.A. Subramanianpage 102
Solid solutions of InGa1�xFexCuO4, InFeCu1�xMgxO4 andInGa1�xFexCu1�xMgxO4 have been synthesized and analyzed withpowder X-ray and neutron diffraction, and DC magnetismmeasurements. The influence of the trigonal bipyramidal site hasbeen investigated through cation substitutions of ionic radiisimilarities and electronic configuration differences.
The preferential growth of ZnS on ZnO nanorods
Haridas Kumarakuru and David Chernspage 109
TEM image comparison of ZnS surface decoration on ZnOnanorod (a) after 15 min sulphidation shows a relatively uniformdeposit on the (0001) end facet, (b) 30 min sulphidation shows amore extensive reaction on the (0001) facet which gives amushroom-like appearance of the nanorod and (c) 60 minsulphidation shows the end cap partially detached and a voidedregion underneath. The presumed growth direction is arrowed(based on the lack of reaction at the other end).
Novel light-conversion hybrids of SBA-16 functionalized with
rare earth (Eu3þ
, Nd3þ
, Yb3þ
) complexes of modified 2-
methyl-9-hydroxyphenalenone and 1,10-phenanthroline
Yan-Jing Gu, Bing Yan and Xiao-Fei Qiaopage 116
Novel rare earth complex-functionalized mesoporous SBA-16-typehybrid materials, which show novel light conversion properties, aresynthesized by the co-condensation of modified 2-methyl-9-hydro-xyphenalenone and tetraethoxysilane with a second ligand, 1,10-phenanthroline.
Phase homology in new layered mixed Li, M (M=Mg, Cu,
Cd, Pb, Bi) bismuth oxophosphates and oxoarsenates
M.S. Kozin, M. Colmont, D. Endara, A. Aliev, M. Huve,O.I. Siidra, S.V. Krivovichev and O. Mentrepage 123
Two new bismuth oxophosphate compounds were isolated. Theyboth enhance infinite [Bi2O2]
2þ layers associated to (BiO)þ
dimmers surrounded by interlayer blocks build on XO4 (X=P,As), LiOx and MOy connected entities. Here the insertion oflithium drastically changed the classical topology observed inrelated Aurivillius compounds.
A series of inorganic aggregates composed of [MnV13O38]7�
polyoxoanions and transition metal cations
Qing Lan, Huaqiao Tan, Ding Liu and Enbo Wangpage 129
Three new extended solid frameworks based on [MnV13O38]7� have
been synthesized. In these compounds, two bi-supported{M2(H2O)10(MnV13O38)} units are connected by a Kþ ions toform the polyoxoanion {K[M2(H2O)5MnV13O38]2}
4�.
Formation processes of high-dimensional Mo–O frameworks
phase structural conversions under restricted dehydration
conditions
Kazuo Eda, Tatsuya Koduka, Yuichi Iriki and M. StanleyWhittinghampage 134
Seven structural phases with Mo–O framework structures ofvarious dimensionalities were found. Two phases having 0Dframework structures were formed in the mother solution. Theremaining five phases were obtained when the two phases wereaged in resin, indicating that the high-dimensional (1D and 2D)Mo–O frameworks of the compound were formed under restricteddehydration conditions such as in resin. There were two differentconversion routes respectively originating from the two phasesformed in the mother solution. The phase sequences in the routesshowed snapshots concerning the formation processes of the high-dimensional frameworks.
Tetragonal-antiprismatic coordination of transition metals in
intermetallic compounds: x1-Mn6Ga29 and its structural
relationships
Iryna Antonyshyn, Yurii Prots, Irene Margiolaki, MarcusPeter Schmidt, Olga Zhak, Stepan Oryshchyn and YuriGrinpage 141
o1-Mn6Ga29 was synthesised applying the high-temperaturecentrifugation-aided filtration technique. The crystal structurewas determined using diffraction data collected from a twinnedspecimen: a new prototype, space group P1; a=6.3114(2) A,b=9.9557(3) A, c=18.920(1) A, a=90.473(1)1, b=90.847(1)1,g=90.396(1)1. The basic building unit of the structure is themonocapped distorted tetragonal antiprism [MnGa8þ 1]. Theseantiprisms condense into pairs by sharing their pseudo-quadraticfaces and are interconnected via common apexes and edges to forma 3D framework.
A first-principles study on chromium sesquioxide, Cr2O3
C. Wessel and R. Dronskowskipage 149
A theoretical high-pressure study on chromium sesquioxideindicates that Cr2O3 is likely to adopt the Rh2O3(II) structuretype at high pressure, and the latter structure appears as aminimum on the potential energy surface.
Continued
Crystal structure and oxygen content of the double
perovskites GdBaCo2�xFexO6�d
D.S. Tsvetkov, I.L. Ivanov and A.Yu. Zuevpage 154
Lattice parameters of GdBaCo2�xFexO6�d (x ¼ 0.4; 0.6) vs.temperature in air.
Nickel segment-length dependent magnetic properties of
Au–Ni–Au nanowires at low temperature fabricated by
electrochemical deposition
S. Ishrat, K. Maaz, Kyu Joon Lee, Myung-Hwa Jung andGil-Ho Kimpage 160
Segmented Au–Ni–Au nanowires fabricated by electrochemicaldeposition. Coercivity and saturation magnetization as a functionof Ni segment length (l) at 300 K and 2 K.
Glucose-assisted hydrothermal preparation and catalytic
performance of porous LaFeO3 for toluene combustion
Kemeng Ji, Hongxing Dai, Jiguang Deng, Liyun Song,Shaohua Xie and Wen Hanpage 164
Porous LaFeO3 is prepared by the glucose-assisted hydrothermalmethod. The good catalytic performance of porous LaFeO3 fortoluene combustion is ascribed to high surface area and Oads
concentration and good reducibility.
The system Ta–V–Si: Thermodynamic modeling
P. Broz, A.U. Khan, H. Niu, X.-Q. Chen, D. Li, J. Vrestal,J. Bursik and P. Roglpage 171
Calculated phase diagram of the Ta–V–Si system at 1500 1C.
New cubic superstructure of titanium monoxide with double
structure imperfection
A.I. Gusevpage 181
A cubic (space group Pm3m) model of new Ti5O5 (Ti5’O5&=Ti90’18O90&18) ordered phase of nonstoichiometric titaniummonoxide TixOz with double structure imperfection.
Xinsong Lin, Stanislav S. Stoyko and Arthur Marpage 189
LaZn2As3 contains defect fluorite slabs that are built from edge-sharing ZnAs4 tetrahedra and that stack in a different way than inCeZn2As3 or PrZn2As3.
Simulation of the growth kinetics of boride layers formed on
Fe during gas boriding in H2-BCl3 atmosphere
M. Kulka, N. Makuch, A. Pertek and L. Ma"dzinskipage 196
JBFeB, JB
Fe2B, JBFe—diffusion fluxes, CB,Fe/Fe2B
, CB,Fe2B/Fe, CB,FeB/Fe2B
and CB,s/FeB—boron contents at the interfaces Fe/Fe2B/FeB and atthe surface, dxFeB, dYFe2B
energy of borides, t—boriding time, T—absolute temperature,R—gas constant tXFeB=0—time needed for the total elimination ofFeB phase, gas boriding—diffusion process in H2-BCI3 atmosphereproviding the two-phase boride layers, diffusion annealing—thesecond stage of process in which the single phase boride layer isobtained.
Solvothermal synthesis, characterization and magnetic
properties of a-Fe2O3 and Fe3O4 flower-like hollow
microspheres
Jing-San Xu, Ying-Jie Zhu and Feng Chenpage 204
Flower-like hollow microspheres of a-Fe2O3 and Fe3O4 have beenprepared by a solvothermal combined with precursor heattreatment method. a-Fe2O3 hollow microspheres exhibit a highcoercivity value of 2738 Oe, and Fe3O4 hollow microspheres have asaturation magnetization of 58.3 emu g�1.
Characterisation, phase stability and surface chemical
properties of photocatalytic active Zr and Y co-doped
anatase TiO2 nanoparticles
Andreas Mattsson, Christian Lejon, Snejana Bakardjieva,Vaclav Stengl and Lars Osterlundpage 212
Phase transition of Y and Zr co-doped anatase TiO2 andprecipitation of ZrTiO4 as well as photocatalytic degradation offormic acid.
Synthesis, characterization, and photocatalytic properties of
BiOBr catalyst
Yan Wang, Zhuqing Shi, Caimei Fan, Xiaowen Wang,Xiaogang Hao and Yongqing Chipage 224
The photocatalytic property and structural morphology of the as-prepared BiOBr semiconductor using a facile hydrolysis methodfor the photocatalytic degradation of organics in water.
Assembly of Cu/Ag-quinoxaline-polyoxotungstate hybrids:
Influence of Keggin and Wells–Dawson polyanions on the
Four new POMs-based hybrids have been synthesized and theresults indicate that Keggin and Wells–Dawson polyanions play animportant role in the assembly of hybrids.
Re-examination of ‘‘Pb3TeO6’’: Determination of its correct
composition as Pb5TeO8
Christine Artner and Matthias Weilpage 240
The unprecedented [O4Pb10] unit in Pb5TeO8.
Continued
Color Point Tuning by Partial Ba2þ Substitution of Ca2þ in
(Ca1�xBax)3(PO4)2 Phosphor for White Light Emitting
With the Ba2þ content increasing, the emission peak of (Ca1�xBax)3(PO4)2: Eu2þ shifts from 447 to 550 nm, and the chromaticitycoordinates shifted from (0.2037, 0.3026) to (0.3295, 0.4638).
Syntheses and crystal structures of three barium uranium
sulfides
Adel Mesbah and James A. Iberspage 253
View of the structure of Ba3.69US6 down [1 0 1].
Influence of KOH-activated graphite nanofibers on the
electrochemical behavior of Pt–Ru nanoparticle catalysts for
fuel cells
Seul-Yi Lee, Byung-Ju Kim and Soo-Jin Parkpage 258
This is described that the CV data of the Pt–Ru/KOH-activatedGNFs catalysts in 0.5 M H2SO4 containing 1.0 M CH3OH. Thismeans the electrochemical activity increased with increasingchemical activation temperature up to K900-GNFs, and thendecreased.
Study of the pseudo-ternary Ag2S–As2S3–HgI2 vitreous
system
R. Boidin, D. Le Coq, A. Cuisset, F. Hindle, J.-B.Brubach, K. Michel and E. Bychkovpage 264
Glass-forming region of the pseudo-ternary Ag2S–As2S3–HgI2system. Emphasis on the evolution of conductivity properties,glass transition temperature, and far-infrared transmission of theA-series glasses (Ag2S)50�x/2 (As2S3)50�x/2 (HgI2)x is shown.
Controlled synthesis of nitrogen-doped binary and ternary
TiO2 nanostructures with enhanced visible-light catalytic
activity
Ligang Gai, Qinghu Mei, Xiuquan Duan, Haihui Jiang,Guowei Zhou, Yan Tian and Xifeng Lupage 271
TiO2 nanostructures bearing binary and/or ternary polymorphs,nitrogen doping, and one-dimensional anatase phase can becontrollably synthesized through a hydrazine-mediated solvother-mal approach, yielding TiO2 photocatalysts with good photo-stability and enhanced visible-light photoactivity as compared toDegussa P25 and the undoped counterpart.
Facile fabrication of N-doped TiO2 nanocatalyst with
superior performance under visible light irradiation
Jie Fu, Yanlong Tian, Binbin Chang, Fengna Xi andXiaoping Dongpage 280
Solid-state calcining of titanate nanotube with NH4Cl leads to theformation of N-doped TiO2 nanocatalyst, which shows anenhanced photocatalytic activity under visible light.
Solvothermal syntheses, crystal structures, and properties of
new mercury(II)–thioantimonates(III) and a mixed-valent
Mercury thioantimonates(III) and thioantimonate(III,V) weresolvothermally prepared, and a new coordination mode for theSb2S5 subunit are observed in the mercury thioantimonates(III).
Particle size effects on the magnetic and phonon properties of
multiferroic CoCr2O4
Maciej Ptak, Miros"aw Maczka, Krzysztof Hermanowicz,Adam Pikul and Jerzy Hanuzapage 295
TEM image of CoCr2O4 annealed at 700 1C (left panel) andhistogram showing the particle size distribution (right panel).
Versatile frameworks constructed from divalent metals with
4,40-methylenedibenzoic acid and imidazole derivative
ligands: Syntheses, crystal structures and physical properties
Guang-Xiang Liu, Xiao-Feng Wang and Hong Zhoupage 305
Seven new complexes were obtained by the reactions of 4,40-methylenedibenzoic acid and several ancillary ligands with metalnitrate. The structural differences indicate that the differentcoordination modes of DBA anion, auxiliary N-donor ligandsand metal ions play important roles in the formation of the finalframework structures. Moreover, their physical properties werealso investigated.
Preparation of nanoporous titania spherical nanoparticles
Kota Shiba, Soh Sato, Takayuki Matsushita and MakotoOgawapage 317
0 200 300 400 600 800
Calcination temperature/ °C
Amorphous Anatase Rutile
Well-defined titania–octadecylamine hybrid spherical particles wereprepared as precursors for nanoporous titania particles. Thenanoporous structure was varied by calcination and the mechanismwas proposed: titania wall shrank to expand pore size (2.2–3.3nm)at calcination up to 3001C and crystal phase transition (300–8001C)resulted in broader pore size distribution.
Structural investigation of a-LaZr2F11 by coupling X-ray
powder diffraction, 19F solid state NMR and DFT
calculations
Charlotte Martineau, Christophe Legein, Monique Body,Olivier Peron, Brigitte Boulard and Franck Fayonpage 326
19F 2D DQ-SQ MAS (64 kHz) NMR correlation spectrum of a-LaZ2F11 recorded at a magnetic field of 17.6 T. The projectionof the 2D spectrum onto the 19F SQ dimension is shown on topwith resonance assignment. Perspective views of trigonal mono-caped ZrF7
3� prisms (blue) and of square-based Archimedes anti-prisms LaF8
5� (yellow).
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Thermal recovery and lattice expansion of self-irradiated
U0.80Am0.20O2�x, an in situ high temperature x-ray
diffraction study
D. Prieur, G. Pagliosa, J. Spino, R. Caciuffo, J. Somersand R. Eloirdipage 334
Lattice parameter recovery at room temperature as a function ofthe annealing temperature. Differential of U0.80Am0.20O2�x latticeparameters measured at room temperature as a function of theannealing temperature.
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Fabrication of superhydrophobic surfaces via CaCO3
mineralization mediated by poly(glutamic acid)
Heng Cao, Jinrong Yao and Zhengzhong Shaopage 338
The superhydrophobic surfaces with the controllable micro- andnanostructure could be constructed in one-step via polypeptidemediated in situ mineralization of CaCO3 combined with chemicalmodification.
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