Research ArticlePreparation, Physicochemical Characterization, andMicrorobotics Applications of Polyvinyl Chloride- (PVC-) BasedPANI/PEDOT: PSS/ZrP Composite Cation-Exchange Membrane
Mohd Imran Ahamed,1 Inamuddin ,2,3,4 Abdullah M. Asiri,2,3 Mohammad Luqman,5
and Lutfullah1
1Department of Chemistry, Faculty of Science, Aligarh Muslim University, Aligarh 202002, Uttar Pradesh, India2Chemistry Department, Faculty of Science, King Abdulaziz University, Jeddah 21589, Saudi Arabia3Centre of Excellence for Advanced Materials Research, King Abdulaziz University, Jeddah 21589, Saudi Arabia4Advanced Functional Materials Laboratory, Department of Applied Chemistry, Faculty of Engineering and Technology,Aligarh Muslim University, Aligarh 202002, India5Chemical Engineering Department, College of Engineering, Taibah University, Yanbu Albahr 41911, Saudi Arabia
Poly(3,4-ethylene dioxythiophene): polystyrene sulfonate (PEDOT: PSS) zirconium(IV) phosphate (ZrP) based ionomericmembrane was prepared by a solution-casting method. Subsequently, aniline polymerization was carried out on the surface of themembrane by oxidative chemical polymerization. It was characterized by thermogravimetric analysis/differential thermalanalysis/differential thermogravimetry (TGA/DTA/DTG), scanning electron microscopy (SEM), X-ray diffraction (XRD), energydispersive X-ray (EDX) analysis, and Fourier-transform infrared (FTIR) spectroscopy. )e membrane was also characterized byion-exchange properties. )e tip displacement investigation of the ionomeric membrane was also carried out. )e outcomesdemonstrated that the manufactured ionomeric membrane could produce generative strengths (tip powers), and consequentlycreate good displacement. In this manner, the proposed ionomeric membrane was found proper for bending movement actuatorthat will give a successful and promising stage for smaller-scale mechanical applications.
1. Introduction
Traditionally, ionic polymer metal composites (IPMCs)emerged as potential materials for electric stimulus re-sponsive actuators when subjected to a lower voltage(e.g., 1–5V) due to various properties including theirprominent mechanical flexibility, lighter weight, low-powerrequirement, easy processing, precise sensing ability, andlarge dynamic deformation. )ese properties are very usefulin different robotic applications including microgrippers,fish, artificial muscles [1–5]. Commonly, an IPMC com-prises an ionomeric membrane (e.g., Nafion) coveredwith metal (e.g., Pt or Au) as an electrode at both sides ofthe membrane and water as the inward medium for the
separation of metal cation, which can produce plain visiblemovement as a result of the movement of cations and watermolecules under a suitable connected voltage [6–10]. Highcost, tedious electroless plating of metal, spillage from thedamaged permeable surface, electrolysis, high dissipationrate of water molecules under connected voltage, and hys-teresis are some serious drawbacks which affect the per-formance of IPMCs [11–13]. Much attention is focusedaround the globe in recent years to develop some distinctclass of speciality materials having the capability of trans-forming electrical energy into mechanical work to utilize inthe multidimensional area of microrobotics [14]. Monomersof thiophene, pyrrole, aniline, and their derivatives [15–17]with excellent response rates during potential cycling
HindawiAdvances in Materials Science and EngineeringVolume 2019, Article ID 4764198, 11 pageshttps://doi.org/10.1155/2019/4764198
experiments are mostly utilized for the preparation ofelectrically conducting polymers (ECPs) [18]. Polyaniline(PANI) is of particular interest electrically conductingpolymer because it can be prepared by both chemical andelectrochemical routes and is thermally, chemically, andenvironmentally stable in air and aqueous media [19, 20].PANI has negligible film-forming capability; thus, despitehaving excellent electrical conducting property, it is com-bined with other similar materials where these materials arerequired in the form of films/membranes. )ese days,poly(3,4-ethylene dioxythiophene):polystyrene sulfonate(PEDOT:PSS) is developed as one of the most encouraging,viable, and effective electrically conducting polymers withvarious applications in different rising fields such as elec-trically conducting and antistatic coatings, sensors, capac-itors as well as thermoelectric materials due to its cost-effectiveness, low surface roughness, mechanical flexibility,high electrical conductivity, and high work function [21–24].Electrically conducting polymers have different preferences,for example, simple preparation, cost adequacy, and greatelectrical conductivity, thus possessing various emergingapplications in nanoactuators and artificial muscles [25]. Foractuation purpose, composite ionomeric membranes de-veloped by using ion-exchange material in a polymer binder(polyvinyl chloride; PVC) could be effectively utilized asthese membranes have several remarkable properties as aresult of combination of properties of inorganic exchangerand organic polymer such as film-forming capability,enhanced electrical and ion exchange/conductivity ca-pacity, mechanical stability and flexibility, and water-retention capacity [26–28]. In the quest for providingan effective alternative (in terms of cost and properties) totraditional actuation materials (e.g., Nafion), we propose,in this study, PANI/PVC-PEDOT: PSS-ZrP-based com-posite cation-exchange membranes to be utilized formicrorobotic applications. )ere is always a need to havevarious options in selecting a material based on thespecific need. A few alternatives to Nafion-based actuationmaterials have been reported where tip displacement issignificantly higher than that based on the Nafion [25].)ese materials have been produced using time-consuming electroless-plating methods using expensivenoble metals for providing electrical conductivity to themembrane. Herein, we propose a cost-effective alternativemethod where there is no need for plating the membranewith expensive noble metals, but by PANI itself, thusreducing the cost in comparison to not only that based onNafion [25] but also Inamuddin et al. [29] and SPVA-Py[30]. Additional advantages of this material are that thebinding of PVC with composite ion exchange materialPEDOT: PSS-ZrP provides a mechanically stable com-posite cation-exchange membrane, whereas ion exchangepolymer PEDOT: PSS works as a semiconductor under anapplied voltage. However, to enhance the electrical con-ductivity, PANI was coated on the surface of the com-posite ion-exchange membrane. )ese materials areexpected to be employed where the need for bendingdisplacement is medium to low, similar or a bit better thanthat based on Nafion.
2. Experimental
2.1.Materials. )eprimary reagents utilized were zirconiumoxychloride octahydrate (ZrOCl2·8H2O), hydrochloricacid (HCl), potassium persulphate (K2S2O8), and dioctylphthalate (C6H4(CO2C8H17)2) (Central Drug House, India),orthophosphoric acid (H3PO4), tetrahydrofuran (C4H8O),liquor ammonia solution (NH4OH), aniline (C6H5NH2)(Fischer Scientific, India), nitric acid (HNO3) (E-Merck,India), poly(3,4-ethylene dioxythiophene):polystyrene sul-fonate (PEDOT:PSS) 1.3 wt.% dispersion in H2O, (Sigma-Aldrich, India), and polyvinyl chloride (Otto Chemicals,India). Every one of the chemicals and reagents was ofanalytical reagent grade and utilized as such.
2.3. Synthesis of the Composite Cation Exchanger. )ecomposite ionomer of PEDOT: PSS-Zr-P was developed asrevealed by Mohammad et al. [31]. )e IEC was determinedafter converting the dried granules into H+ ion form asdiscussed elsewhere [29].
2.4. Membrane Preparation and Coating of Polyaniline.Coetzee and Benson [32] technique was taken after for thereadiness of the composite cation-exchange membrane ofPANI/PVC-PEDOT: PSS-ZrP. )e composite ionomericmaterial was ground well to a fine powder. Polyvinyl chloride(PVC) powder was dissolved in 10ml of tetrahydrofuran(THF) and 1 g of powdered composite ionomer, and 50 μL ofdioctyl phthalate was included and blended completely withthe assistance of magnetic stirrer [33]. )e resultant materialwas carefully poured into a glass-casting ring (diameter10mm) laying on a glass plate. )e ring was left for moderatevanishing of THF. )e film, after total evaporation of THF,was put into a beaker containing 20ml of 10% aniline and20ml of 0.1M potassium persulphate (K2S2O8) and stirredutilizing a stirrer beneath 10°C for 60minutes. Subsequently,the beaker containing the membrane was kept underneath10°C in an icebox for 24 h.)emembrane was taken out fromthe beaker, washed with demineralised water (DMW) toevacuate traces of surface unbound polyaniline (PANI), anddried in an electric oven kept up at 45± 0.5°C.)e membranewas put away in a desiccator to conduct further experiments.
2.5. Characterization. )e ion-exchange capacity (IEC), theproton conductivity, water uptake (by mass), and water loss(by mass) properties of the PANI/PVC-PEDOT: PSS-ZrP
2 Advances in Materials Science and Engineering
composite ionomeric membrane was determined as re-ported by Inamuddin et al. [11].
2.6. Electromechanical Study. For portraying the electro-mechanical parameters of the PANI/PVC-PEDOT: PSS-ZrPcomposite membrane, a testing setup is outlined as shown inFigure 1 where the PANI/PVC-PEDOT: PSS-ZrP compositemembrane actuator in a cantilever mode is clasped in aholder which is mounted on the steel-based table. An inputcommand in terms of voltage (0–3.5V DC) is sent throughcomputer-controlled digital analogue card (DAC), minia-turized scale controller, and computerized power supply.)e current rating 50–200mA was required for enacting themembrane which was given by utilizing a specially designedamplifier circuit. )e copper tapes were put on both surfacesof the membrane for conductivity and current supplyneeded during actuation. A laser displacement sensor wasutilized as a feedback framework for measuring the tipdislodging position of the actuator. A converter (Make:Adam) was likewise utilized for changing over the in-formation from RS-485 to RS-232 convention which wasassociated with a computer (PC) port. )e information wasgathered by Docklight V1.8 programming through RS-232port in a PC. A PC code utilizing C programming dialect wascomposed where the sampling rate (20 tests for each second)was settled in the software for controlling the layer.
2.7. Force Measurement. A high-accuracy load cell wasutilized for measuring the load of the PANI/PVC-PEDOT:PSS-ZrP membrane actuator. )e voltage was measuredutilizing multimeter while the composite membrane was inoperation.
3. Results and Discussion
)e PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane possessed a significant ion-exchangecapacity of 1.23meq·g−1 of the dry membrane and fur-thermore, has a proton conductivity of 8.83×10−6 S cm−1(Table 1). )e higher water take-up of the PANI/PVC-PEDOT: PSS-ZrP ionomeric membrane might be becauseof good IEC and proton conductivity of the membranewhich may come about the quick movement of hydratedcations towards cathode by producing an ideal pressuretowards the anode, responsible for actuation (Figure 2). )ehigher water take-up promotes for the execution of com-posite cation-exchange membrane. )e water take-up limitof PANI/PVC-PEDOT: PSS-ZrP composite cation-exchangemembrane at 25± 3°C was subject to time as it incrementswith the expansion of drenching time up to 16h, and afterthat, saturation was built up (Figure 2). )e percent watertake-up at 25± 3°C with inundation time 16 h was found10.7%. )e percent water take-up of the composite cation-exchange membrane PEDOT: PSS-ZrP was recorded 8.16%at 45°C. )e outcomes explain that only 2.54% of water-holding limit of the membrane was lost at 45°C (Figure 3).
)e superb water-retention capacity even at raisedtemperature might be because of the presence of more
dynamic thermally broadened PO42− sites on the composite
ionomeric membrane.)e high water take-up of composite-cation exchange membrane even at elevated temperaturemay likewise encourage the movement of hydrated cationeven if there should be an occurrence of high temperatureprompting to the good actuation. )e water loss of thepremeasured PANI/PVC-PEDOT: PSS-ZrP compositecation-exchange membrane was determined by applying anelectric voltage of 3V at time interims i.e., 3, 6, 9, and 12min.Water loss of the composite cation-exchange membrane wasobserved to be dependent to the time of applying voltage, asit increments with increment in time of connected voltage,and water loss up to 2.41% was seen subsequent to applyingan electric voltage of 3V for a period of 12min (Figure 4).
)e water loss from the composite membrane may comeabout because of the water spillage from the damaged surface.)is is the reason behind the shorter existence of IPMCs. )eelectrical property of PANI/PVC-PEDOT: PSS-ZrP com-posite cation-exchange membrane was investigated by utiliz-ing potentiostatic cyclic voltammetry. )e speedy movementof the hydrated cations in the composite membrane, in view ofthe connected electrical voltage, with the decay profile of waterbecause of electrolysis mirrors the state of I-V hysteresiscurves. It was observed that there was no critical voltage dropand the slant of the I-V curve for composite cation-exchangemembrane was altogether high [13], recommending the quickmovement of hydrated cations and moderate dissipation ofwater (Figure 5). )e current density of PANI-PEDOT-Zr-Pcomposite cation-exchange membrane was assessed by ap-plying a voltage of 3.5 and found subject to connected voltageas it increments with increment in connected voltage as shownin Figure 6.)e elemental composition acquired by the energydispersive X-ray (EDX) examination is introduced in Table 2.)e presence of chemical constituents (C, O, Zr, P, N, and Cl)in the EDX spectrum in respective ratios confirms the for-mation of PANI/PVC-PEDOT: PSS-ZrP composite ion-exchange membrane (Figure 7). )e X-ray diffraction pat-tern of PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane showed little pinnacles of 2θ values,recommending the indistinct nature of the composite cation-exchange membrane (Figure 8). )e FTIR spectrum of PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange mem-brane (Figure 9) affirms presence of the–OH stretching ofexternal water molecules (3434 cm−1) [34], metal oxygen bond(Zr-O) (609 and 518 cm−1) [35], ionic phosphate (1074 cm−1)[36], C�O stretching (1730 cm−1) [37], lattice (internal) water(1636 cm−1) [38], whereas a sharp peak at 2927 cm−1 deals withthe C-H stretching mode for polyvinyl chloride [39].
)e thermogram of the PANI/PVC-PEDOT: PSS-ZrPcomposite cation-exchange membrane (Figure 10) indicatedgood thermal stability as it helds 51% of mass at 600°C.When the hybrid cation-exchange membrane was heated upto 101°C, only 5.54% weight reduction was watched which isascribed because of the evacuation of outer water moleculesjoined to the surface of composite cation-exchange mem-brane. Further heating up to 200°C came about 9.96% weightreduction which might be because of the evacuation of astrongly coordinated water molecule from the compositecation-exchange membrane [40]. A mass loss of 17.7% was
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Feedback system
+
–
Actuator
I/P command
Controller
DAC card
DisplacementsensorDigital power supply
Customised control system
Computer
Figure 1: Sketch for testing the bending of PANI/PVC-PEDOT: PSS-ZrP actuator.
Table 1: Composition, IEC, and PC of the PANI/PVC-PEDOT: PSS-ZrP composite ionomer membrane.
S. No.Membrane composition
PANI-PEDOTZrP (mg)
PVC(mg)
Plasticizer(μL)
THF(ml)
�ickness(mm)
IEC(meq g−1 of dry membrane)
Protonconductivity (S cm−1)
M-1 1000 200 50 10 0.161 1.23 8.83×10−6
–
+
Fixed anion
Mobile
Water
–
–
–
–
–
–
–
–
+
+
+
+
+
+
+
+
+
– –
–
––
–
+
+ +
+
+
+
––
+
+
+–Before actuation A�er immersion in water
A�er actuation
– –
–
––
–
+ +
++
+
––
+ +
–
+
–
+
–
+
–
+
+
+ Hydrated cation
Movement of hydrated cation
Figure 2: Bending mechanism of PANI/PVC-PEDOT: PSS-ZrP membrane.
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related while heating the membrane up to 250°C because ofphysical transitions such as crystallization occurring duringheating [41]. As temperature increases up to 329°C, 7.6%weight loss was observed which corresponds to the releaseand deterioration of organic polymer PEDOT: PSS [42]. �econversion of the phosphate group into pyrophosphategroup is accompanied with 1.98% weight loss up to 399°C[43]. Another 5.77% weight reduction observed whileheating is proceeded up to 600°C which was related to thedeterioration of organic polymer polyvinyl chloride [44].�e DTA curve demonstrated two sharp peaks at 330 and
500°C which a�rmed the transitions associated in TGAanalysis. �e almost horizontal curve beyond 600°C repre-sented the formation of oxides [40].
00
2
4
6
8
10
12
4 8 12Time (h)
Wat
er u
ptak
e (%
)
16 20 24
Water uptake at 25 ± 3°CWater uptake at 45°C
Figure 3: Water uptake of PANI/PVC-PEDOT: PSS-ZrPmembrane.
Wat
er lo
ss (%
)
Time (min)
0
0.5
1
1.5
2
2.5
0 3 6 9 12
Figure 4: Water loss from PANI/PVC-PEDOT: PSS-ZrPmembrane.
1 1.5 2 2.5 3 3.5 40.5
1
1.5
2
2.5
3
Potential (volt)
Curr
ent d
ensit
y (A
/cm
2 )
×10–5
Figure 6: LSV of PANI/PVC-PEDOT: PSS-ZrP membrane.
Figure 9: FTIR spectrum of PANI/PVC-PEDOT: PSS-ZrP membrane.
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Temperature (°C)140012001000800600400200
DTA
µV
80.0
60.0
40.0
20.0
0.0
–20.0
–40.0
–60.0
–80.0
–100.0
–120.0
–140.0
TG (%
)
150.0
140.0
130.0
120.0
110.0
100.0
90.0
80.0
70.0
60.0
50.0
DTG
(mg/
min
)
0.50
0.00
–0.50
–1.00
–1.50
–2.00
–2.50
–3.00
20°C99.97%
101°C94.43%
200°C84.77%
399°C57.42%
500°C54.99% 599°C
51.65%801°C50.52%
1001°C49.92%
1200°C49.98%
1446°C49.9%
231°C0.52 mg/min
310°C0.20 mg/min 535°C
0.05 mg/min
329°C59.4%250°C
67.0%
330°C20.5 µV
–579 mJ/mg
DTADTGTG
Figure 10: Simultaneous TGA/DTA/DTG curves of PANI/PVC-PEDOT: PSS-ZrP membrane.
(a) (b)
Figure 11: Continued.
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Scanning electron microscopic pictures of the PANI/PVC-PEDOT: PSS-ZrP composite membrane before andafter applying an electrical voltage of 3.5V are shown inFigures 11(a) and 11(b). )e fresh composite membranehas smooth surface morphology with no sort of spaces,while in the wake of applying voltage, surface morphologyof the composite membrane became slightly rough, and avery thin rupture was noticeable on the surface of themembrane which is responsible for the lesser degree ofwater loss. Along these lines, it was watched that in thewake of applying the voltage, the hybrid membrane had ingeneral very little influence. SEMmicrophotographs shownin Figures 11(c) and 11(d) portray the cross-sectionalimages of the fresh PANI/PVC-PEDOT: PSS-ZrP com-posite cation-exchange membrane which demonstratedthat the PEDOT: PSS-ZrP composite ion-exchanger par-ticles are profoundly embedded in the framework ofpolyvinyl chloride. )e denser collection of cation-exchanger particles in the composite cation-exchangemembrane resulted in the compact granular filling whichwas responsible for the lesser degree of water loss from thehybrid cation-exchange membrane. )is is because of thefact that the dense aggregation obstructs in the path of flowof water molecules.
Whenever voltage (0–3.5V DC) was connected to themembrane through a customized control framework, the tipdisplacement was controlled through PC interface as aninput command and the composite membrane twisted at aconnected voltage (0–3.5V DC). )e size of the membrane(30mm length × 10mm width × 0.16mm thickness) is cutfor experimentation purpose. In the wake of applying thevoltages, the twisting deflection pictures were taken atvarious voltages as demonstrated in Figure 12. A few timestests were produced and information was likewise gatheredas given in Table 3. )e average values at correspondingvoltages were plotted in Figure 13. It is conceived that the
greatest deflection was achieved up to 14.5mm at 3.5V withthe steady-state behaviour. It was likewise watched thatwhen the voltage was in off mode, the PANI/PVC-PEDOT:PSS-ZrP membrane did not return in a similar way, and ithighlights some error in deflection (0.5mm). For avoidingthis deflection error, a proportional-derivative (PD) con-trol system was applied in the controller where the PDcontroller gains were tuned in the controller by setting afrequency. For force characteristic of PANI-PEDOT-ZrPactuator, the membrane was clamped with overload cell.)e experimental data were collected as given in Table 4. Byusing the probability distribution method, the standarddeviation was calculated as 0.1353 when the mean value was0.2019. By using normal distribution function, the re-peatability of PANI/PVC-PEDOT: PSS-ZrP actuator wasfound to be 99.03%. Amicrogripper was developed as shownin Figure 14. By holding the object, these PANI-PEDOT-ZrPbased membranes demonstrate the capability of smallerscale automated applications.
4. Conclusion
In this paper, a PANI/PVC-PEDOT: PSS-ZrP compositecation-exchange membrane was prepared by solutioncasting technique with a specific end goal to use in smallerscale microrobotic applications. )is composite cation-exchange membrane showed good ion exchange capacityand proton conductivity with faster actuation capability.From the experimental results, it was assumed that thismaterial has great water take-up limit and a lesser measure ofwater misfortune under connected voltage. Additionally, thetip relocation parameters showed quick actuation. )us, thePANI/PVC-PEDOT: PSS-ZrP composite exchange mem-brane could be effectively utilized for actuation purpose,which will open a new path of prospects in a very dynamicand rapidly emerging field of microrobotics.
(c) (d)
Figure 11: SEM microphotographs of PANI/PVC-PEDOT: PSS-ZrP. (a) Image at a magnification of 500× before actuation. (b) Image at amagnification of 500× after actuation. (c) Cross-sectional image at a magnification of 150× before actuation. (d) Cross-sectional image at amagnification of 150× after actuation.
8 Advances in Materials Science and Engineering
(a) (b) (c) (d)
(e) (f ) (g) (h)
Figure 12: Experimental deflection response of PANI/PVC-PEDOT: PSS-ZrP at different voltages (0–3.5V): (a) 0V, (b) 0.5V, (c) 1.0V, (d)1.5V, (e) 2.0 V, (f ) 2.5V, (g) 3.0 V, and (h) 3.5 V.
Table 3: Experimental deflection data of the PANI/PVC-PEDOT: PSS-ZrP membrane with applied voltages.
)e data used to support the findings of this study areavailable from the corresponding author upon request.
Conflicts of Interest
)e authors declare that they have no conflicts of interest.
Acknowledgments
)e authors are thankful to the Department of AppliedChemistry, Aligarh Muslim University, India, for providingresearch facilities. )e authors are also thankful to CSIR-CMERI, Durgapur, India, for carrying out the electrome-chanical characterization and demonstration of the IPMC-based microrobotic system at DMS/Microrobotics Labora-tory, CSIR-CMERI, Durgapur, India.
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–4 –3 –2 –1 0 1 2 3 4–15
–10
–5
0
5
10
15X: 3.5Y: 14.5
Voltage (V)
Def
lect
ion
(mm
)
X: –3.5Y: –14.5
Forward behavior of PANI/PVC-PEDOT: PSS-ZrP membraneReverse behavior of PANI/PVC-PEDOT: PSS-ZrP membrane
Figure 13: Deflection characteristics of PANI/PVC-PEDOT: PSS-ZrP actuator.
PANI/PVC-PEDOT:PSS-ZrP-based
gripper
Figure 14: A prototype of PANI/PVC-PEDOT: PSS-ZrP-basedmicrogripping system.
Table 4: Experimental force data of the PANI/PVC-PEDOT: PSS-ZrP actuator.
Voltage(V)
Force data in mN Average forcedata (Fd) in mNFd1 Fd2 Fd3 Fd4 Fd4
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