Preparation, Physicochemical Characterization, and Microrobotics Applications of Polyvinyl Chloride- (PVC-) Based PANI/PEDOT: PSS/ZrP Composite Cation-Exchange Membrane

Ahamed, Mohd Imran; Inamuddin, undefined; Asiri, Abdullah M.; Luqman, Mohammad; Lutfullah, undefined

doi:https://doi.org/10.1155/2019/4764198

Advances in Materials Science and Engineering

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Abstract Introduction Experimental Results and Discussion Conclusion Data Availability Conflicts of Interest Acknowledgments References Copyright Related Articles

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Advances in Applications of Polymer Nanocomposites

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Research Article | Open Access

Volume 2019 | Article ID 4764198 | https://doi.org/10.1155/2019/4764198

Preparation, Physicochemical Characterization, and Microrobotics Applications of Polyvinyl Chloride- (PVC-) Based PANI/PEDOT: PSS/ZrP Composite Cation-Exchange Membrane

Mohd Imran Ahamed,¹ Inamuddin,^2,3,4Abdullah M. Asiri,^2,3Mohammad Luqman,⁵and Lutfullah¹

Academic Editor: Charles C. Sorrell

Received24 Apr 2018

Revised28 Nov 2018

Accepted01 Jan 2019

Published24 Feb 2019

Abstract

Poly(3,4-ethylene dioxythiophene): polystyrene sulfonate (PEDOT: PSS) zirconium(IV) phosphate (ZrP) based ionomeric membrane was prepared by a solution-casting method. Subsequently, aniline polymerization was carried out on the surface of the membrane by oxidative chemical polymerization. It was characterized by thermogravimetric analysis/differential thermal analysis/differential thermogravimetry (TGA/DTA/DTG), scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray (EDX) analysis, and Fourier-transform infrared (FTIR) spectroscopy. The membrane was also characterized by ion-exchange properties. The tip displacement investigation of the ionomeric membrane was also carried out. The outcomes demonstrated that the manufactured ionomeric membrane could produce generative strengths (tip powers), and consequently create good displacement. In this manner, the proposed ionomeric membrane was found proper for bending movement actuator that 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 responsive actuators when subjected to a lower voltage (e.g., 1–5 V) due to various properties including their prominent mechanical flexibility, lighter weight, low-power requirement, easy processing, precise sensing ability, and large dynamic deformation. These properties are very useful in different robotic applications including microgrippers, fish, artificial muscles [1–5]. Commonly, an IPMC comprises an ionomeric membrane (e.g., Nafion) covered with metal (e.g., Pt or Au) as an electrode at both sides of the membrane and water as the inward medium for the separation of metal cation, which can produce plain visible movement as a result of the movement of cations and water molecules under a suitable connected voltage [6–10]. High cost, tedious electroless plating of metal, spillage from the damaged permeable surface, electrolysis, high dissipation rate of water molecules under connected voltage, and hysteresis are some serious drawbacks which affect the performance of IPMCs [11–13]. Much attention is focused around the globe in recent years to develop some distinct class of speciality materials having the capability of transforming electrical energy into mechanical work to utilize in the multidimensional area of microrobotics [14]. Monomers of thiophene, pyrrole, aniline, and their derivatives [15–17] with excellent response rates during potential cycling experiments are mostly utilized for the preparation of electrically conducting polymers (ECPs) [18]. Polyaniline (PANI) is of particular interest electrically conducting polymer because it can be prepared by both chemical and electrochemical routes and is thermally, chemically, and environmentally stable in air and aqueous media [19, 20]. PANI has negligible film-forming capability; thus, despite having excellent electrical conducting property, it is combined with other similar materials where these materials are required in the form of films/membranes. These days, poly(3,4-ethylene dioxythiophene):polystyrene sulfonate (PEDOT:PSS) is developed as one of the most encouraging, viable, and effective electrically conducting polymers with various applications in different rising fields such as electrically conducting and antistatic coatings, sensors, capacitors 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 great electrical conductivity, thus possessing various emerging applications in nanoactuators and artificial muscles [25]. For actuation purpose, composite ionomeric membranes developed by using ion-exchange material in a polymer binder (polyvinyl chloride; PVC) could be effectively utilized as these membranes have several remarkable properties as a result of combination of properties of inorganic exchanger and organic polymer such as film-forming capability, enhanced electrical and ion exchange/conductivity capacity, mechanical stability and flexibility, and water-retention capacity [26–28]. In the quest for providing an effective alternative (in terms of cost and properties) to traditional actuation materials (e.g., Nafion), we propose, in this study, PANI/PVC-PEDOT: PSS-ZrP-based composite cation-exchange membranes to be utilized for microrobotic applications. There is always a need to have various options in selecting a material based on the specific need. A few alternatives to Nafion-based actuation materials have been reported where tip displacement is significantly higher than that based on the Nafion [25]. These materials have been produced using time-consuming electroless-plating methods using expensive noble metals for providing electrical conductivity to the membrane. Herein, we propose a cost-effective alternative method where there is no need for plating the membrane with expensive noble metals, but by PANI itself, thus reducing the cost in comparison to not only that based on Nafion [25] but also Inamuddin et al. [29] and SPVA-Py [30]. Additional advantages of this material are that the binding of PVC with composite ion exchange material PEDOT: PSS-ZrP provides a mechanically stable composite cation-exchange membrane, whereas ion exchange polymer PEDOT: PSS works as a semiconductor under an applied voltage. However, to enhance the electrical conductivity, PANI was coated on the surface of the composite ion-exchange membrane. These materials are expected to be employed where the need for bending displacement is medium to low, similar or a bit better than that based on Nafion.

2. Experimental

2.1. Materials

The primary reagents utilized were zirconium oxychloride octahydrate (ZrOCl₂·8H₂O), hydrochloric acid (HCl), potassium persulphate (K₂S₂O₈), and dioctyl phthalate (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 sulfonate (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 of analytical reagent grade and utilized as such.

2.2. Instrumentation

An X-ray diffractometer (Miniflex-II, Japan), FTIR spectrometer (Interspec-20, Spectrolab UK), TGA/DTA recorder (EXSTAR, TG/DTA-6300), scanning electron microscope (SEM) (JEOL, JSM-6510 LV, Japan), laser displacement sensor (OADM 20S4460/S14F, Baumer Electronic, Germany), pH meter (Elico LI-120, India), an electric air oven (Jindal Scientific Instrumentation, India), digital electronic balance (Wensar, MAB-220, India), and magnetic stirrer (Labman LMMS-1L4P, India) were used.

2.3. Synthesis of the Composite Cation Exchanger

The composite ionomer of PEDOT: PSS-Zr-P was developed as revealed by Mohammad et al. [31]. The IEC was determined after converting the dried granules into H⁺ ion form as discussed elsewhere [29].

2.4. Membrane Preparation and Coating of Polyaniline

Coetzee and Benson [32] technique was taken after for the readiness of the composite cation-exchange membrane of PANI/PVC-PEDOT: PSS-ZrP. The composite ionomeric material was ground well to a fine powder. Polyvinyl chloride (PVC) powder was dissolved in 10 ml of tetrahydrofuran (THF) and 1 g of powdered composite ionomer, and 50 μL of dioctyl phthalate was included and blended completely with the assistance of magnetic stirrer [33]. The resultant material was carefully poured into a glass-casting ring (diameter 10 mm) laying on a glass plate. The ring was left for moderate vanishing of THF. The film, after total evaporation of THF, was put into a beaker containing 20 ml of 10% aniline and 20 ml of 0.1 M potassium persulphate (K₂S₂O₈) and stirred utilizing a stirrer beneath 10°C for 60 minutes. Subsequently, the beaker containing the membrane was kept underneath 10°C in an icebox for 24 h. The membrane was taken out from the beaker, washed with demineralised water (DMW) to evacuate traces of surface unbound polyaniline (PANI), and dried in an electric oven kept up at 45 ± 0.5°C. The membrane was put away in a desiccator to conduct further experiments.

2.5. Characterization

The ion-exchange capacity (IEC), the proton conductivity, water uptake (by mass), and water loss (by mass) properties of the PANI/PVC-PEDOT: PSS-ZrP composite ionomeric membrane was determined as reported by Inamuddin et al. [11].

2.6. Electromechanical Study

For portraying the electromechanical parameters of the PANI/PVC-PEDOT: PSS-ZrP composite membrane, a testing setup is outlined as shown in Figure 1 where the PANI/PVC-PEDOT: PSS-ZrP composite membrane actuator in a cantilever mode is clasped in a holder which is mounted on the steel-based table. An input command in terms of voltage (0–3.5 V DC) is sent through computer-controlled digital analogue card (DAC), miniaturized scale controller, and computerized power supply. The current rating 50–200 mA was required for enacting the membrane which was given by utilizing a specially designed amplifier circuit. The copper tapes were put on both surfaces of the membrane for conductivity and current supply needed during actuation. A laser displacement sensor was utilized as a feedback framework for measuring the tip dislodging position of the actuator. A converter (Make: Adam) was likewise utilized for changing over the information from RS-485 to RS-232 convention which was associated with a computer (PC) port. The information was gathered by Docklight V1.8 programming through RS-232 port in a PC. A PC code utilizing C programming dialect was composed 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 was utilized for measuring the load of the PANI/PVC-PEDOT: PSS-ZrP membrane actuator. The voltage was measured utilizing multimeter while the composite membrane was in operation.

3. Results and Discussion

The PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane possessed a significant ion-exchange capacity of 1.23 meq·g⁻¹ of the dry membrane and furthermore, has a proton conductivity of 8.83 × 10⁻⁶ S cm⁻¹ (Table 1). The higher water take-up of the PANI/PVC-PEDOT: PSS-ZrP ionomeric membrane might be because of good IEC and proton conductivity of the membrane which may come about the quick movement of hydrated cations towards cathode by producing an ideal pressure towards the anode, responsible for actuation (Figure 2). The higher water take-up promotes for the execution of composite cation-exchange membrane. The water take-up limit of PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane at 25 ± 3°C was subject to time as it increments with the expansion of drenching time up to 16h, and after that, saturation was built up (Figure 2). The percent water take-up at 25 ± 3°C with inundation time 16 h was found 10.7%. The percent water take-up of the composite cation-exchange membrane PEDOT: PSS-ZrP was recorded 8.16% at 45°C. The outcomes explain that only 2.54% of water-holding limit of the membrane was lost at 45°C (Figure 3).

The superb water-retention capacity even at raised temperature might be because of the presence of more dynamic thermally broadened sites on the composite ionomeric membrane. The high water take-up of composite-cation exchange membrane even at elevated temperature may likewise encourage the movement of hydrated cation even if there should be an occurrence of high temperature prompting to the good actuation. The water loss of the premeasured PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane was determined by applying an electric voltage of 3 V at time interims i.e., 3, 6, 9, and 12 min. Water loss of the composite cation-exchange membrane was observed to be dependent to the time of applying voltage, as it increments with increment in time of connected voltage, and water loss up to 2.41% was seen subsequent to applying an electric voltage of 3 V for a period of 12 min (Figure 4).

The water loss from the composite membrane may come about because of the water spillage from the damaged surface. This is the reason behind the shorter existence of IPMCs. The electrical property of PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane was investigated by utilizing potentiostatic cyclic voltammetry. The speedy movement of the hydrated cations in the composite membrane, in view of the connected electrical voltage, with the decay profile of water because of electrolysis mirrors the state of I-V hysteresis curves. It was observed that there was no critical voltage drop and the slant of the I-V curve for composite cation-exchange membrane was altogether high [13], recommending the quick movement of hydrated cations and moderate dissipation of water (Figure 5). The current density of PANI-PEDOT-Zr-P composite cation-exchange membrane was assessed by applying a voltage of 3.5 and found subject to connected voltage as it increments with increment in connected voltage as shown in Figure 6. The elemental composition acquired by the energy dispersive X-ray (EDX) examination is introduced in Table 2. The presence of chemical constituents (C, O, Zr, P, N, and Cl) in the EDX spectrum in respective ratios confirms the formation of PANI/PVC-PEDOT: PSS-ZrP composite ion-exchange membrane (Figure 7). The X-ray diffraction pattern 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). The FTIR spectrum of PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane (Figure 9) affirms presence of the–OH stretching of external 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 with the C-H stretching mode for polyvinyl chloride [39].

The thermogram of the PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane (Figure 10) indicated good thermal stability as it helds 51% of mass at 600°C. When the hybrid cation-exchange membrane was heated up to 101°C, only 5.54% weight reduction was watched which is ascribed because of the evacuation of outer water molecules joined to the surface of composite cation-exchange membrane. Further heating up to 200°C came about 9.96% weight reduction which might be because of the evacuation of a strongly coordinated water molecule from the composite cation-exchange membrane [40]. A mass loss of 17.7% was related while heating the membrane up to 250°C because of physical transitions such as crystallization occurring during heating [41]. As temperature increases up to 329°C, 7.6% weight loss was observed which corresponds to the release and deterioration of organic polymer PEDOT: PSS [42]. The conversion of the phosphate group into pyrophosphate group is accompanied with 1.98% weight loss up to 399°C [43]. Another 5.77% weight reduction observed while heating is proceeded up to 600°C which was related to the deterioration of organic polymer polyvinyl chloride [44]. The DTA curve demonstrated two sharp peaks at 330 and 500°C which affirmed the transitions associated in TGA analysis. The almost horizontal curve beyond 600°C represented the formation of oxides [40].

Scanning electron microscopic pictures of the PANI/PVC-PEDOT: PSS-ZrP composite membrane before and after applying an electrical voltage of 3.5V are shown in Figures 11(a) and 11(b). The fresh composite membrane has smooth surface morphology with no sort of spaces, while in the wake of applying voltage, surface morphology of the composite membrane became slightly rough, and a very thin rupture was noticeable on the surface of the membrane which is responsible for the lesser degree of water loss. Along these lines, it was watched that in the wake of applying the voltage, the hybrid membrane had in general very little influence. SEM microphotographs shown in Figures 11(c) and 11(d) portray the cross-sectional images of the fresh PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane which demonstrated that the PEDOT: PSS-ZrP composite ion-exchanger particles are profoundly embedded in the framework of polyvinyl chloride. The denser collection of cation-exchanger particles in the composite cation-exchange membrane resulted in the compact granular filling which was responsible for the lesser degree of water loss from the hybrid cation-exchange membrane. This is because of the fact that the dense aggregation obstructs in the path of flow of water molecules.

(a)

(b)

(c)

(d)

Whenever voltage (0–3.5 V DC) was connected to the membrane through a customized control framework, the tip displacement was controlled through PC interface as an input command and the composite membrane twisted at a connected voltage (0–3.5 V DC). The size of the membrane (30 mm length × 10 mm width × 0.16 mm thickness) is cut for experimentation purpose. In the wake of applying the voltages, the twisting deflection pictures were taken at various voltages as demonstrated in Figure 12. A few times tests were produced and information was likewise gathered as given in Table 3. The average values at corresponding voltages were plotted in Figure 13. It is conceived that the greatest deflection was achieved up to 14.5 mm at 3.5 V with the steady-state behaviour. It was likewise watched that when the voltage was in off mode, the PANI/PVC-PEDOT: PSS-ZrP membrane did not return in a similar way, and it highlights some error in deflection (0.5 mm). For avoiding this deflection error, a proportional-derivative (PD) control system was applied in the controller where the PD controller gains were tuned in the controller by setting a frequency. For force characteristic of PANI-PEDOT-ZrP actuator, the membrane was clamped with overload cell. The experimental data were collected as given in Table 4. By using the probability distribution method, the standard deviation was calculated as 0.1353 when the mean value was 0.2019. By using normal distribution function, the repeatability of PANI/PVC-PEDOT: PSS-ZrP actuator was found to be 99.03%. A microgripper was developed as shown in Figure 14. By holding the object, these PANI-PEDOT-ZrP based membranes demonstrate the capability of smaller scale automated applications.

(a)

(b)

(c)

(d)

(e)

(f)

(g)

(h)

4. Conclusion

In this paper, a PANI/PVC-PEDOT: PSS-ZrP composite cation-exchange membrane was prepared by solution casting technique with a specific end goal to use in smaller scale microrobotic applications. This composite cation-exchange membrane showed good ion exchange capacity and proton conductivity with faster actuation capability. From the experimental results, it was assumed that this material has great water take-up limit and a lesser measure of water misfortune under connected voltage. Additionally, the tip relocation parameters showed quick actuation. Thus, the PANI/PVC-PEDOT: PSS-ZrP composite exchange membrane could be effectively utilized for actuation purpose, which will open a new path of prospects in a very dynamic and rapidly emerging field of microrobotics.

Data Availability

The data used to support the findings of this study are available from the corresponding author upon request.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Acknowledgments

The authors are thankful to the Department of Applied Chemistry, Aligarh Muslim University, India, for providing research facilities. The authors are also thankful to CSIR-CMERI, Durgapur, India, for carrying out the electromechanical characterization and demonstration of the IPMC-based microrobotic system at DMS/Microrobotics Laboratory, CSIR-CMERI, Durgapur, India.

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Copyright © 2019 Mohd Imran Ahamed et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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