aluminium oxide

Sensors and Actuators A 280 (2018) 114–124

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Sensors and Actuators A: Physical journal homepage: www.elsevier.com/locate/sna

Development of sulfonated poly(vinyl alcohol)/aluminium oxide/graphene based ionic polymer-metal composite (IPMC) actuator Ajahar Khan a,d , Inamuddin a,b,c,∗ , Ravi Kant Jain d , Mohammad Luqman e , Abdullah M. Asiri b,c a Advanced Functional Materials Laboratory, Department of Applied Chemistry, Faculty of Engineering and Technology, Aligarh Muslim University, Aligarh 202002, India b Chemistry Department, Faculty of Science, King Abdulaziz University, Jeddah 21589, Saudi Arabia c Centre of Excellence for Advanced Materials Research (CEAMR), King Abdulaziz University, Jeddah 21589, Saudi Arabia d Surface and Field Robotics Group, CSIR-Central Mechanical Engineering Research Institute, Durgapur 713209, India e Department of Chemistry, School of Advanced Sciences, VIT University, Chennai, Tamil Nadu, India

a r t i c l e

i n f o

Article history: Received 26 February 2018 Received in revised form 21 June 2018 Accepted 13 July 2018 Keywords: Poly(vinyl alcohol) Aluminium oxide Graphene Actuator Ionic polymer-metal composite Film

a b s t r a c t A novel ionic polymer-metal composite (IPMC) actuator based on the ionomeric composite film composed of sulfonated poly(vinyl alcohol)/aluminium oxide/graphene/platinum (SPVA-Al-GR-Pt) was successfully developed. The SPVA-Al-GR films were prepared by solution casting strategy followed by electroding with platinum using electroless plating or chemical reduction method. The SPVA-Al-GR films showed good ion-exchange capacity (1.8 meq g−1 of the dry film) and water uptake (125% at 45 ◦ C for 10 h of drenching time). Moderate solvent (water) loss, good proton conductivity, stability at higher temperatures and electromechanical properties of proposed IPMC actuator places itself as a promising alternative to conventional polymer based IPMC actuators. By building up a small scale holding framework, it was demonstrated that this IPMC actuator can be utilized as a part of miniaturized scale mechanical devices. © 2018 Elsevier B.V. All rights reserved.

1. Introduction Ionic polymer-metal composites (IMPCs) based soft actuators are considered to be one of the most delicate actuation materials, because of their large and fast bending deformation in response to low external electrical stimulus (1–6 V) [1,2]. Recently, IPMCs have attracted increasing interest from researchers and industry engineers because of their quick response, lightweight, adaptable nature, simple control system etc. [3–8]. IPMCs can be utilized as a part of assorted miniaturized devices, for example, biomedical gadgets, smaller than usual or artificial muscles, bio-mimetic robotics, automobiles, and microsensors and switches [2,9–19] attributable to their qualities including large, quick, and delicate bending actuation. A normal IPMC film comprises an ionomeric layer sandwiched between a couple of electrodes mostly Pt or Au. Usually, an ionomeric layer contains mobile ions (e.g. metal cations) and a polar solvent to facilitate ionic mobility. Under-connected

∗ Corresponding author at: Advanced Functional Materials Laboratory, Department of Applied Chemistry, Faculty of Engineering and Technology, Aligarh Muslim University, Aligarh 202002, India. E-mail address: [email protected] (Inamuddin). https://doi.org/10.1016/j.sna.2018.07.027 0924-4247/© 2018 Elsevier B.V. All rights reserved.

electric potential, asymmetric diffusion of cations toward the negatively charged electrode is responsible for the twisting actuation towards positively charged electrode [3,20]. More often, the commercial perfluorinated polymers, for example, Nafion, Flemion, Aciplex and so on are utilized as a result of their high level of proton conductivity and powerful thermo-chemical stabilities arising from their novel perfluorinated structure [1,21]. These industrial ionomers, i.e. polymer electrolytes, have a twostage blend of a steady Teflon spine interweaved with the ionic bunches. The spine structure holds mechanical quality while bunches with ionic groups give the exchange channels to solvated (hydrated) cations. Be that as it may, these conventional actuators have a few downsides as well including very high cost, environmentally unsafe and require steady humidification to counteract the drying of these films [1,22,23]. Thus, a number of non-perfluorinated polymers as a substite of these perfluorinated polymers have been developed [24–29]. Among non-perfluorinated polymers, block copolymers are perceived as promising cutting edge materials for IPMC actuator applications because of their lower cost, mechanical strength, and dimensional stability from solvation to actuation, and magnificent ionic conductivity owing to the efficient microphase-isolated structures. A few of the relevant non-perfluorinated polymers, which can act as

A. Khan et al. / Sensors and Actuators A 280 (2018) 114–124

substitute to the perfluorinated one include sulfonated polystyrene [25], sulfonated styrene/ethylene/butylene based triblock copolymer [26], sulfonated styrene/methylbutylene diblock copolymer, tert-butyl-styrene/ethylene/propylene/styrene/styrene sulfonate penta square copolymer [27,28], Kraton pentablock copolymer [29,30], sulfonated poly(vinyl alcohol)/polpyrrole [31], polyacrylonitrile–Kraton–graphene [32], Kraton/GO/Ag/Pani [33] and thorium(IV) phosphate-polyaniline [34]. The majority of these ionomers bear cation leading polymer layers since cations diffuse speedier than anions with a comparative effective radius. In the present study, a novel non-perfluorinated sulfonated poly(vinyl alcohol), aluminium oxide (Al2 O3 ), graphene and platinum (SPVA-Al-GR-Pt) based IPMC film actuator was developed by solution casting strategy with chemical reduction of Pt on the film surfaces as electrodes. The composite of two or more materials has advantageous and desirable properties which could not possible to be present in the individual material. The configuration of our interest was to develop such polymeric composite material based IPMC film, which can alternate highly expensive, environment non-friendly perfluorinated polymer, beside this having desirable properties and good actuation performance for robotic applications. Herein, a cost-effective non-perfluorinated polymersulfonated poly(vinyl alcohol) was used as base ionomeric material because of its certain advantageous properties such as admirable film forming capacity, easy modification of chemical properties, high ion exchange and water retention capacity and high proton conductivity. Recently, graphene (GR) became a very interesting filler for the composite materials because of its electronic transport properties, excellent electrical conductivity, exceptional thermal and high mechanical strength. Therefore, the incorporation of this two-dimensional carbon nanostructure has been predicted an immense pledge for many potential applications such as nanoelectronics, actuators and sensors, supercapacitors and nanocomposites [35–39]. Thus, the addition of GR to the SPVA can enhance the performance of IPMC [40,41]. The most familiar approach to produce a suitable dielectric material is the addition of inorganic particles to ionomeric composite. Incorporation of inorganic particles such as Al2 O3 in composite results in improved dielectric properties, resistance, thermal stability and conductivity [42]. Thus, the combined chemical and electromechanical properties of composite SPVA, GR, Al2 O3 may improve the mechanical stability, tip displacement and repeatability in the fabricated SPVAAl-GR-Pt IPMC film. Therefore, SPVA-Al-GR-Pt IPMC can afford an easy and worthy way out for realization of the novel actuator, which can show good potential in miniaturized scale robotic system and related applications. 2. Experimental 2.1. Material Poly(vinyl alcohol) (PVA) and hydrochloric acid (HCl-35%); (Central Drug House Pvt. Ltd., India), ammonium hydroxide (NH4 OH-25%); (Merck Specialties Pvt Ltd., India), graphene, aluminium oxide (Al2 O3 ), 4-sulfophthalic acid (HO3 SC6 H3 -1,2(CO2 H)2 -50 wt% aqueous solution); (Sigma-Aldrich Pvt. Ltd., USA), tetraamine platinum(II) chloride monohydrate [Pt(NH3 )4 Cl2 ·H2 O (Crystalline)]; (Alfa Aesar, USA) and sodium borohydride (NaBH4 ); (Thomas Baker Pvt. Ltd., India), were utilized. 2.2. Preparation of the reagent solutions Aqueous solutions of tetraamine platinum(II) chloride monohydrate (0.04 M), NaBH4 (5.0%) and NH4 OH (5.0%) were prepared utilizing demineralised water (DMW). Graphene dispersion was

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made by blending 50 mg of graphene in 20 ml of tetrahydrofuran (THF) with steady mixing up to 6 h at room temperature (25 ± 3 ◦ C). 2.3. Fabrication of films The ionomeric films were fabricated by dissolving almost 3 g of PVA in 75 ml of DMW followed by stirring at 60 ◦ C for 6 h. For sulfonation of prepared homogeneous PVA solution, 3 ml of 4sulfophthalic acid was added with constant stirring for 15 h at 60 ◦ C. To this sulfonated poly(vinyl alcohol) (SPVA) solution, 0.5 g of Al2 O3 powder was added trailed by adding 10 ml suspension of GR with consistent blending for 3 h at 45 ◦ C. From that point onward, the homogeneous composite solution of SPVA, Al2 O3 and GR (SPVA-AlGR) was spread in 4 Petri dishes (100 × 15 mm (S line)) secured with Whatman filter paper (1) for the moderate vanishing of the solvents at 45 ◦ C in an indoor thermostat oven. The film was crosslinked by setting in an indoor thermostat oven at 150 ◦ C for 1 h. Thus, using 3 g of PVA four films of Petri dish sizes were fabricated. Therefore, the exact amount of PVA in one ionomeric polymer film was 0.75 g. 2.4. Water uptake To decide the water uptake (WU) limit of SPVA-Al-GR polymer composite film, the pre-measured film was absorbed by DMW for 6 h. Subsequently, it was grabbed from the DMW and surface was wiped with filter paper, the film was weighed utilizing an advanced digital balance to calculate the weight of water absorbed by the polymer film. The WU of the proposed polymer layer was figured at room temperature (25 ± 3 ◦ C) and 45 ◦ C for the various interim of times e.g. 2, 4, 6, 8, 10 and 20 h. The WU of the polymer layer was calculated using the following formula:

WU =

Wwet − Wdry

Wdry

× 100

(1)

Where Wwet is the weight of water absorbed film and Wdry is the weight of the dry film. 2.5. Ion-exchange capacity The ion-exchange capacity (IEC (meq g−1 )), in general, a measure of the H+ ions released by neutral salts to move through the polymer film was obtained by standard column process. The dried SPVA-Al-GR polymer film (0.25 g) was cut into little pieces and drenched in 1 M HNO3 for 24 h to change into H+ form, trailed by neutralization with refined water, and was dried at 45 ◦ C. The dried SPVA-Al-GR polymer film in the protoned form was stuffed into a glass column. A 1 M NaNO3 as eluent was utilized to elute the protons totally from the column, keeping up a moderate flow rate of 0.5 ml min−1 . A standard (0.1 M) NaOH solution was utilized to titrate the effluent using phenolphthalein as indicator, and the IEC (meq g−1 ) was calculated using following equation: Ion exchange =

Volume

of

capacity NaOH consumed × Molarity Weight of dry film

of

NaOH

(2)

2.6. Electroless plating The SPVA-Al-GR-Pt film based IPMC was created by an electroless plating strategy [30,31]. The entire procedure of plating platinum comprised of the reduction utilizing a strong reductant (NaBH4 ). The SPVA-Al-GR polymer film was at first roughened by gentle sand paper so as to expand the surface regions, trailed by washing with DMW, absorbing in an aqueous solution of 2 M HCl

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and flushing with DMW. The pre-treated film (30 × 10 × 0.11 mm) (Length × width × thickness) (L × W × T) was drenched in 4.5 ml freshly prepared aqueous solution of Pt(NH3 )4 Cl2 .H2 O with the end goal of ion-exchange. Then, 1 ml of ammonium hydroxide (NH4 OH) solution was added. The film was kept in the solution at room temperature for 12 h to exchange from H+ to Pt2+ . After washing with DMW, 1 ml of sodium borohydride (NaBH4 ) solution was added at an interval of 30 min for 7 times. From that point forward, 5 ml of the reducing agent (NaBH4 ) was added to the solution so as to guarantee the entire reduction of Pt inside the polymer film. At long last, the IPMC film was washed with DMW and kept in an aqueous solution of HCl for 1.5 h. 2.7. Proton conductivity Proton conductivity (␴) of the completely hydrated SPVA-AlGR-Pt (1 × 3 cm2 ) IPMC films was obtained at room temperature (25 ± 3 ◦ C) using an impedance analyser (FRA32 M.X), associated with modular potentiostat/galvanostat (Autolab 302 N). The deliberate procedure was completed over a frequency range of 100 KHz under an AC annoyance of 10 mV. The proton conductivity (␴) of IPMC film was figured using the following equation: =

L R×A

(3)

where stands for proton conductivity (S cm−1 ), L for the thickness of the film (cm), R is the resistance (), and A for cross-sectional area of the film (cm2 ). 2.8. Water loss To decide the SPVA-Al-GR-Pt IPMC film’s water loss, the film was first drenched in DMW for 6 h at 45 ◦ C with a specific end goal to ingest water totally before playing out the water loss analysis. The film was grabbed from water; the heaviness of water doused by IPMC film was calculated. The electrical potential was applied with a specific end goal to decide water misfortune. IPMC layer’s water loss was figured at 3, 4 and 5 V for the various interim of time 3, 6, 9 and 12 min and the water loss percent was calculated as: % Water

loss =

m1 − m2 × 100 m1

(4)

where m1 is the mass of water soaked film and m2 is the mass of film after applied potential. 2.9. Characterizations The electrochemical, electromechanical, structural morphology and other characteristic properties of SPVA-Al-GR-Pt-based IPMC films were evaluated via a variety of characterizations. The Fourier transform infrared (FTIR, PerkinElmer SpectrometerUSA) spectra of pristine PVA, GR and SPVA-Al-GR-Pt IPMCs were recorded from 500 to 4000 cm−1 . Scanning electron microscope (SEM Jeol, JSM-6510LV-Japan) was used to observe the surface and the cross-sectional morphologies of SPVA-Al-GR-Pt IPMC films. Energy dispersive X-ray (Oxford instruments INCA, X.act, S.No. 56756, UK) analysis was used to determine the elemental composition on the surface of IPMC film. X-ray diffraction (XRD, Rigaku, Miniflex-II-Japan) with Cu K␣ was utilized to study the structure of composite polymer film. Thermal stability of SPVA-Al-GR-Pt IPMC actuator was studied by a thermogravimetric analyser (TGA, Perkin Elmer, USA) with instrumental TGA pyres 1-HT, at a heating rate of 10 ◦ C min−1 in the N2 atmosphere. To determine the electrical property, cyclic voltammetry (CV) was performed with modular potentiostat/galvanostat (Autolab 302 N) in 0.5 M NaOH solution at a triangular input voltage of ±3.5 V (step of 50 mV s-1 ).

Fig. 1. Water uptake of the SPVA-Al-Gr film at room temperature (25 ± 3 ◦ C) and 45 ◦ C.

The Young’s modulus and tensile strength of SPVA-Al-GR ionomer film was determined by a universal testing machine (Model: H50 KS, Shimadzu Corp.), with the gauge length between the grips were 25 mm under the testing speed of 5 mm min−1 . The electromechanical analyses of the IPMC film was carried out by determining the stepwise bending response along with maximum tip displacement. For load characterization, the IPMC film was clamped in a cantilever configuration and the maximum load carrying capability was determined. The several trials of successive bending responses were conducted and the normal distribution was calculated to confirm the repeatability of SPVA-Al-GR-Pt IPMC actuator. 3. Results and discussion The water uptake (WU) is the characteristic feature of the conventional IPMC actuators, responsible for the deformation of the IPMCs. The performance of IPMC film is supposed to be due to the movement of cations along with the water molecules present in the polymer film, hence WU of a polymer film play vital role in the performance of IPMC actuator [34]. Fig. 1 shows that the water uptake of the SPVA-Al-GR polymer film changed with time in the process of reaching saturated state. It is observed from the Fig. 1 that there was a significant increase in the water uptake at 45 ◦ C. The maximum water uptake capacities of SPVA-Al-GR polymer films at room temperature (RT) (25 ± 3 ◦ C) and 45 ◦ C for 10 h of immersion time were 59 and 125%, respectively. To check the stability of SPVA-Al-GR polymer films towards WU capability, the experiment was repeated for five times at RT and 45 ◦ C. An error bar of WU (Fig. 1) was plotted taking an average of five values. This reveals that there was no significant change in the WU capacity after repetition. This, in turn, confirms the better actuation performance of the fabricated ionomer film [34]. The elevated WU of SPVA-AlGR polymer film supported the hydrophilic nature and ultimately confirm the better performance under an applied potential. The IEC of a polymer film was described by the presence of fixed milli equivalents exchangeable counterparts per gram of polymer film, which are typically the destinations available for proton exchange, and is considered to have an inconceivable association with the proton conductivity. IEC of the SPVA-Al-GR polymer film was found to be 1.8 meq g−1 of the dry film. The high IEC allows more WU and moreover empowers higher amount of particles (Pt) to be significantly settled on both sides of the IPMC film. The greater thickness of Pt particles on the surface of IPMC film signifies the lower resistance and speedier and bigger bowing execution [31,32]. Suitably, the proton conductivity of SPVA-Al-GR-Pt IPMC film was seen to be 1.54 × 10−3 S cm−1 . The high proton conductivity leads


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Fig. 2. SEM micrographs of SPVA-Al-Gr-Pt film before (a, c), after (b, d) applied potential, and a cross-sectional image showing coated layer of Pt electrode (e, f).

to a better execution of the IPMC polymer film by the migration of high amount of protons through the hydrated IPMC film actuator. Fig. 2(a–d) outlines the SEM micrographs of SPVA-Al-GR-Pt IPMC film taken before (a, c), and after (b, d) applying the electrical potential. It can be watched that, before applying the electrical potential, the surface of polymer film deposited with Pt electrodes seem more uniform and smooth than that after it which indicates just a marginally broke and harsh surface with just a couple of cavities (Fig. 2(c, d)). Thus, it was concluded that the loss of solvent (water) from the electrode layer of the proposed IPMC film would be lower. Thus, the natural water loss and electrolysis should be the main considerations for the water misfortune from the proposed IPMC film. Some microcracks are clearly shown on the SPVA-Al-GRPt IPMC film surface as a result of the cracking of the Pt electrode layers during the sample drying before SEM analysis. The crosssectional picture of the SPVA-Al-GR-Pt film was additionally taken to demonstrate the electrode layer on the surfaces of IPMC film (Fig. 2(e), (f)). The EDX analysis of the SPVA-Al-GR-Pt IPMC film surface show the characteristic elemental peaks and composition of carbon, oxygen, sulphur, aluminium and platinum constituting the IPMC film (Fig. 3(a), (b)). The presence of Pt peaks confirms the coating of a metal electrode on the surface of SPVA-Al-GR-Pt-based IPMC film. Fig. 4 shows the water loss from SPVA-Al-GR-Pt film at room temperature, was analyzed as an element of the time. This sol-

vent loss from the SPVA-Al-GR-Pt film may be attributed to the preparation process of the film, surface morphology, electrolysis and natural evaporation. Fig. 4 demonstrates that loss of water from the SPVA-Al-GR-Pt film increases with the increasing applied voltage. The maximum water loss for SPVA-Al-GR-Pt film come to 45% after 12 min upon 5 V of the applied potential. The water loss is the principal figure for a lower performance and shorter lifespan of IPMC actuators [31]. The moderate water loss demonstrates the better execution of SPVA-Al-GR-Pt film actuator with respect to the repeatability. The results demonstrate that after 45% water loss the SPVA-Al-GR-Pt-based IPMC still contain a significant amount of absorbed water (68.75%) requisite for actuation performance because the WU of the fabricated IPMC was 125%. Thus, the fabricated IPMC film confirmed the better performance in comparison to the other reported IPMCs having lower WU [34,43–45]. The FTIR spectra of pristine PVA, SPVA-Al-GR-Pt IPMC film and GR were recorded in the vicinity of 4000 and 500 cm−1 as appeared in Fig. 5. The characteristic strong broadband around ∼3400 cm−1 in all the films, corresponds to stretching vibration of O H, and that at ∼2960 cm−1 could be due to asymmetric −CH2 stretching (Fig. 5(a–c)). By the sulfonation of pure PVA, the intensity of these peaks was enhanced noticeably due to symmetric and asymmetric stretching bands of S O, which generally appear at the same frequency of C O stretching [46]. The absorption at ∼1140 cm−1 for C O S stretching vibration and ∼1240 cm−1 for O S O asymmet-

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Fig. 3. EDX graphs (a, b) of SPVA-Al-GR-Pt IPMC film.

Fig. 6. XRD spectrum of SPVA-Al-Gr-Pt IPMC film. Fig. 4. Water loss of SPVA-Al-Gr-Pt IPMC film at 3, 4 and 5 V.

ric stretching vibration demonstrated that SO3 H was joined on the PVA chain [47]. The reasons behind of no significant change in the intensity of O H band after sulfonation of PVA were: (i) large number of −OH groups were present in the membrane, (ii) each mole of sulfothalic acid consumes two −OH groups of PVA for crosslinking and add one more −OH group due to the occurrence of SO3 H group. The GR characteristic bands are available at ∼1620 cm−1 for C O stretching, ∼1240 cm−1 for C–OH stretching and 1080 cm−1 for C–O of epoxy stretching, separately (Fig. 5(c)) [48].

Fig. 5. FTIR spectra of PVA, GR and SPVA-Al-Gr-Pt film.

The XRD diffraction pattern of SPVA-Al-GR/Pt polymer film appears in Fig. 6 having little peaks of 2␪ values. Generally, when there are crystalline domains in the polymer membrane, the diffraction patterns are sharp with high intensities of peaks, whereas for amorphous nature of polymer membrane the diffraction patterns are broad. Fig. 6 shows that the diffraction pattern of SPVA-Al-GR-Pt film exhibits a typical peak at 2␪ = 20.8◦ due to the presence of poly(vinyl alcohol) [49]. Due to the sulfonation of PVA, the intensity of the characteristic peak of PVA is decreased [49]. The results obtained reveal that there are diffraction peaks of graphite commonly exhibiting at 26.60◦ and 42.20◦ [50,51]. The investigation of this X-ray diffraction spectrum shows an amorphous nature of SPVA-Al-GR-Pt ionomeric polymer film. The thermal stability of SPVA-Al-GR-Pt was an imperative property for its durability during IPMC operation at high temperature. The thermal stability of the SPVA-Al-GR-Pt film was inspected by TGA as appeared in Fig. 7. The first weight reduction of approximately 18% in the initial step happened around 100–200 ◦ C because of the loss of absorbed water. Past this, the second thermal degradation happened over temperature run from 200 to 300 ◦ C, which relates to the degradation of cross-connected polymer chain [52]. The third weight reduction happened between 350 to 550 ◦ C, which should be identified with the degradation of main chain backbone of crosslinked films that could be ascribed to thermal oxidation of PVA. In cyclic voltammetry (CV), a higher current density infers a large migration of ions and additionally a bigger capacitance for large actuation. As appeared in Fig. 8, the cyclic voltammograms


Fig. 7. TGA curve of SPVA-Al-Gr-Pt IPMC film.

Fig. 8. Current-voltage (I–V) hysteresis curve for SPVA-Al-Gr-Pt IPMC film under ±3.5 V triangle voltage input with a scan rate of 50 mV s−1 in 0.5 M NaOH.

of SPVA-Al-GR-Pt IPMC film actuator, which was recorded under a triangular voltage of ±3.5 V with a sweep rate of 50 mV s−1 shows a typical curve pattern, which demonstrates that the current density was relative to the film conductivity. The I–V curve shown in Fig. 8 reveals that the SPVA-Al-GR-Pt IPMC film has a higher value of current density, which proves that Pt electrode layer was uniformly deposited on the surface of IPMC film. Thus, the rate of ionic transfer was higher in SPVA-Al-GR-Pt IPMC required for the bet-

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ter performance of IPMC actuator. The symmetric shape of the CV curve can be assigned to excellent charge distribution in the whole surface region of the IPMC. The high proton conductivity, IEC, and smoothness of the electrode surface are important parameters for the higher current density of IPMC film [30,31]. It is additionally seen from the Fig. 8 that the current density of the proposed IPMC film increases up to 3.5 V, which is responsible for an excellent execution of SPVA-Al-GR-Pt IPMC film as an actuator. To observe the bending/deflection behaviour of SPVA-Al-GR-Ptbased IPMC film, the schematic graph of an experimental testing is shown in Fig. 9. The fabricated IPMC film in a cantilever mode was held in a holder, which was incorporated with a little mounting seat. With a specific end goal to supply the voltage to IPMC film, a personel computer (PC) interfaced modified control framework was utilized which comprises of PC, digital to an analog card (DAC), and miniaturized scale controller. An amplifier was likewise utilized for attaining the best possible voltage e.g. 0–3.5 V dc and current rating (50–200 mA), which was provided to IPMC film for its twisting behaviour. An optical/laser displacement sensor was put before the IPMC for measuring the displacement data with time which additionally fills in as an input gadget for predicting data. At the point, when a voltage signal was sent, a converter was likewise utilized for translating correspondence from RS-485 to RS-232 convention since this sensor gives information in RS-485 and it was additionally interfaced with PC, which peruses in the RS-232 convention. A power supply was likewise utilized for providing the voltage to the customized controller. A program was produced for sending information to the ionomeric film, which was confirmed through Docklight programming and accomplishes the exact twisting/bending behaviour of ionomeric film. The actual testing setup for the ionomeric film appears in Fig. 10. The bidirectional behaviour can likewise be gotten by altering the polarity of the voltage signal. In the wake of sending the proper voltage e.g. 0–3.5 V dc, the twisting of the ionomeric film was accomplished and progressive steps with voltage were as appeared in Fig. 11. Table 1 presents the data from the progressive step of the fabricated IPMC film (30 × 10 × 0.11 mm). In the wake of acquiring the information, the twisting deflection voltage was plotted by utilizing Matlab programming as appeared in Fig. 12. From this figure, it was observed that the maximum tip deflection for the SPVA-Al-GR-Pt IPMC was found to be 19.00 mm, which is fairly comparable with different IPMCs. It was additionally seen that on turning off the voltage, the IPMC film deflection did not accomplish the similar path and it showed the error in deflection up

Fig. 9. Schematic diagrams for the experimental test setup for SPVA-Al-GR-Pt IPMC film.

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Fig. 10. Actual testing setup for SPVA-Al-GR-Pt IPMC film.

Fig. 11. Bending/deflection behaviour of SPVA-Al-GR-Pt IPMC film.

Table 1 Tip deflection data of SPVA-Al-GR-Pt IPMC film. S.No.

Voltage (V)

1 2 3 4 5 6 7 8

0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50

Tip deflection (mm)

Average deflection (mm)

Trial 1

Trial 2

Trial 3

Trial 4

Trial 5

0.00 1.95 5.05 11.00 15.00 16.50 18.10 19.00

0.00 1.85 5.10 11.10 15.20 16.45 18.15 19.25

0.00 2.15 4.90 11.05 14.85 16.60 17.90 19.10

0.00 2.05 4.95 10.95 14.90 16.55 18.00 18.80

0.00 2.00 5.00 10.90 15.05 16.40 17.85 18.85

0.00 2.00 5.00 11.00 15.00 16.50 18.00 19.00

to 1.8 mm. This was adjusted through a proportional derivative (PD) controller by building up an algorithm in a smaller scale controller. A PD control system was used for minimizing the deflection error of proposed IPMC, where the controller bandwidth was set by tuning the frequency. When the frequency in the controller was increased, the time duration of actuation of IPMC decreases and stability also decreases. In order to achieve the fast response of IPMC, by proper tuning of gains in the PD controller the frequency was set. This reveals the steady position between the response time and stability. To observe the driving force capability the SPVA-Al-GR-Pt IPMC film was clamped in a holder in cantilever mode as appeared in Fig. 13. During this observation, the tip of the IPMC film contacted the dish of measuring scale. A low force measuring-cum-weighing


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Fig. 12. Forward and backward deflection of SPVA-Al-GR-Pt IPMC film. Fig. 14. Stress-strain curve of SPVA-Al-GR composite polymer film. Table 3 Mechanical properties of SPVA-Al-GR composite polymer film.

Fig. 13. Testing load setup for SPVA-Al-GR-Pt IPMC film.

scale was utilized for finding the forced quality. It can measure the load between 0.0001–220 g which has a decent accuracy (±1.0 mg) and repeatability (±0.1 mg). The voltage was sent utilizing customized controller and noted through multi-meter in the meantime. The trial data of force behaviour are noted in Table 2. In order to analyze the data, the mean estimation of various force values were taken and the standard deviation (SD) was also calculated utilizing

Membrane

Young’s modulus (MPa)

Ultimate tensile strength (MPa)

Break strain from position (%)

SPVA-Al-GR

265.80

18.01

32.50

MatLab programming. The mechanical stability including Young’s modulus and tensile strength of the SPVA-Al-GR film has a significant effect on the actuation performance. To obtain a stress-strain curve the SPVA-Al-GR composite film (0.11 mm thick and 20 mm width) was fixed into universal testing machine (UTM) with a fixed gauge length of 25 mm. As the film was elongated up to 30 N load the displacement of two endpoints was continuously recorded to attain the strain of the IPMC film. The stress-strain curve of the SPVA-Al-GR film is shown in the Fig. 14 and its mechanical properties are shown in Table 3. The Young’s modulus and ultimate tensile strength of the fabricated ionomeric film were found to be 265.80 MPa and 18.01 MPa, respectively. The stress-strain analysis demonstrates that the SPVA-Al-GR ionomer film provides high mechanical strength and molecular rigidity. The high mechanical strength of the SPVA-Al-GR composite ionomeric polymer film may be due to the addition of GR, which has excellent mechanical strength as well as superior electrical properties. Thus, the combined properties of the SPVA-Al-GR composite could be a better alternative to produce IPMC actuator with the enhanced performance. Moreover, the normal distribution curve was plotted for fabricated IPMC film (Fig. 15). From the analysis of normal distribution curve, the repeatability of the SPVA-Al-GR-Pt IPMC was found to be 99.35%. With a specific end goal to evaluate the appropri-

Table 2 Actuation force of SPVA-Al-GR-Pt IPMC film. F stands for Force in mN. S. No

Voltage (V)

1. 0.00 0.50 2. 3. 1.00 1.50 4. 2.00 5. 2.50 6. 3.00 7. 8. 3.50 Mean Standard Deviation Normal Deviation Repeatability

F1

F2

F3

F4

F5

F (Average)

0.00 0.09 0.19 0.29 0.28 0.47 0.58 0.77

0.00 0.09 0.18 0.30 0.27 0.49 0.61 0.79

0.00 0.10 0.20 0.27 0.31 0.51 0.59 0.79

0.00 0.09 0.19 0.28 0.30 0.48 0.57 0.77

0.00 0.10 0.19 0.31 0.29 0.50 0.57 0.78

0.00 0.09 0.19 0.29 0.29 0.49 0.58 0.78 0.34 0.26 0.64 99.35%

Fig. 15. Normal distribution curve for SPVA-Al-GR-Pt IPMC film.

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Table 4 Comparison of SPVA-Al-GR-Pt based IPMC film with other IPMC films. Parameters

SPVA-Al-GR-Pt

Sulfonated Polyetherimide based IPMC [43]

CNT based IPMC [44]

Nafion based IPMC [45]

Polyacrylonitrile– kraton–graphene based IPMC [32]

Kraton based IPMC [30]

IEC (meq g−1 ) PC (S cm−1 ) WU (%) Tip displacement (mm) Current density (A cm−2 )

1.80 1.54 × 10−3 125.00 19.00 5.40 × 10−3

0.55 1.40 × 10−3 26.40 2.70 5.00 × 10−4

0.71 5.70 × 10−3 25.10 20.00 –

0.98 9.00 × 10−3 16.70 12.00 3.00 × 10−3

1.40 5.26 × 10−3 133.30 18.00 1.60 × 10−4

2.00 1.30 × 10−3 233.00 17.00 2.50 × 10−3

Acknowledgments The authors are thankful to the Department of Applied Chemistry, Aligarh Muslim University, Aligarh, India, for providing research facilities and to the Department of Science and Technology, India, for giving the Young Scientist Award to Dr. Inamuddin (Project No. SR/FT/CS-159/2011).

References

Fig. 16. A prototype of multi SPVA-Al-GR-Pt IPMC film based microgripper.

ateness of SPVA-Al-GR-Pt IPMC film as an actuator, a small scale gripper of this film was developed as appeared in Fig. 16, where fingers based on these IPMCs were incorporated with around wrist. The controlled voltage was sent through a customized control system. It showed that this gripping/holding system was activated by electrical pulse rather than using the conventional motor. This gripping/holding system demonstrates the handling capability for small weight objects, where each IPMC finger controls the misalignment during grasping the object. Use of SPVA-Al-GR-Pt IPMCs in developing the micro gripping system shows its future prospect in robotic applications. The comparison of different properties of SPVA-Al-GR-Pt-based IPMC actuator with the other reported IPMC actuators are given in Table 4.

4. Conclusions In this paper, a novel SPVA-Al-GR-Pt IPMC films using nonperfluorinated polymer composite was developed by simple solution casting strategy with chemical reduction of Pt ions as electrodes. In the wake of building up a composite film, the tests were performed with a focus on the electromechanical properties of SPVA-Al-GR-Pt IPMC film. By the water loss test, it has been shown that moderate water loss of this IPMC after applied potential was responsible for the better performance for the longer term. The SPVA-Al-GR-Pt IPMC film was found to demonstrate an extreme twisting displacement up to 19.00 mm which was very practically identical with other IPMCs for taking care of lightweight articles. A model of small-scale grasping framework utilizing these IPMCs was developed which demonstrates the capability in robotics and different applications.

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Biographies

Dr. Ajahar Khan is working as national postdoctoral fellow funded by Science Engineering and Research Board (SERB), Department of Science and Technology (DST), India at CSIR-CMERI, Durgapur, India. He has worked as a Project Assistant under the DST funded major research project entitled “Development of ionic polymer metal composites based on non-perfluorinated ionomeric materials for robotic actuator, dynamic sensor and artificial muscles application” since January 2013 to September 2015. He received his Doctor of Philosophy (Applied Chemistry) and Masters of Science (Analytical Chemistry) degrees from Aligarh Muslim University (AMU), Aligarh, India in September 2016 and 2012, respectively. He has obtained his B.Sc. degree form M.J.P. Rohilkhand University, Bareilly, India, in 2010. His research interest includes synthesis/development, processing, characterization and applications of polymer/ionomer nanocomposites for artificial muscles, robotics, micro sensors and actuators. Dr. Inamuddin is currently working as Assistant Professor in the Chemistry Department, Faculty of Science, King Abdulaziz University, Jeddah, Saudi Arabia. He is a permanent faculty member (Assistant Professor) at the Department of Applied Chemistry, Aligarh Muslim University, Aligarh, India. He obtained Master of Science degree in Organic Chemistry from Chaudhary Charan Singh (CCS) University, Meerut, India, in 2002. He received his Master of Philosophy and Doctor of Philosophy degrees in Applied Chemistry from Aligarh Muslim University (AMU), Aligarh, India, in 2004 and 2007, respectively. He has extensive research experience in multidisciplinary fields of Analytical Chemistry, Materials Chemistry, and Electrochemistry and, more specifically, Renewable Energy and Environment. He has worked on different research projects as project fellow and senior research fellow funded by University Grants Commission (UGC), Government of India, and Council of Scientific and Industrial Research (CSIR), Government of India. He has received Fast Track Young Scientist Award from the Department of Science and Technology, India, to work in the area of bending actuators and artificial muscles. He has completed four major research projects sanctioned by University Grant Commission, Department of Science and Technology, Council of Scientific and Industrial Research, and Council of Science and Technology, India. He has published 113 research articles in international journals of repute and eighteen book chapters in knowledge-based book editions published by renowned international publishers. He has published twenty-four edited books with Springer, United Kingdom, Elsevier, Nova Science Publishers, Inc. U.S.A., CRC Press Taylor & Francis Asia Pacific, Trans Tech Publications Ltd., Switzerland and Materials Science Forum, U.S.A. He is the member of various editorial boards of the journals and serving as associate editor for journals such as Environmental Chemistry Letter, Applied Water Science, Euro-Mediterranean Journal for Environmental Integration, Springer-Nature, editorial board member for Scientific Reports-Nature and editor for Eurasian Journal of Analytical Chemistry. He has attended as well as chaired sessions in various international and national conferences. He has worked as a Postdoctoral Fellow, leading

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a research team at the Creative Research Initiative Center for Bio-Artificial Muscle, Hanyang University, South Korea, in the field of renewable energy, especially biofuel cells. He has also worked as a Postdoctoral Fellow at the Center of Research Excellence in Renewable Energy, King Fahd University of Petroleum and Minerals, Saudi Arabia, in the field of polymer electrolyte membrane fuel cells and computational fluid dynamics of polymer electrolyte membrane fuel cells. He is a life member of the Journal of the Indian Chemical Society. His research interest includes ion exchange materials, a sensor for heavy metal ions, biofuel cells, supercapacitors and bending actuators. Dr. Ravi Kant Jain received the B.E. in Mechanical Engineering from Barkatullah University Bhopal, India in 1999 and M.Tech. in Mechanical Engineering from MANIT Bhopal, India in 2001. He obtained his Ph.D. in Mechanical Engineering/Micro Robotics from Indian Institute of Technology (IIT) Kanpur, India in 2013. Currently, he is working as Principal Scientist in Information Technology Group at CSIR-Central Mechanical Engineering Research Institute (CMERI), Durgapur, West Bengal, India. Prior to this he has performed his duties as a Senior Scientist and Scientist C in same organization. From 2001 to 2004, he worked a Senior Research Fellow at Research & Development Establishment (Engineers), DRDO, Pune, Maharastra, India. He was one of the recipients of Eminent Engineers and Er. M. P. Baya National Award from The Institution of Engineers (India), Udaipur in 2016 and 2017, respectively. He was awarded IEI Young Engineer Award in Mechanical Engineering of IEI (India) in 2011. He has also received the best paper award in IEEE International Conference organized on the theme “Recent Technologies in Communication and Computing” in Kottayam, India in 2010. In the year 2013, he was the recipient of the best paper presentation at MSC Software India User and honored as Guest of Honor from M/s NI India Pvt. Ltd, Bangalore, India. He is also working as the faculty member of Academy of Scientific and Innovative Research (AcSIR), CSIR-CMERI. He is a member of editorial board, International Journal of Applied Chemistry and Materials Science, Taiwan. He is an active member of The Institution of Engineers (India) and Robotics Society of India. His current research focuses on design and development of ionic polymer metal composite (IPMC)/piezoelectric actuators based micro part handling system for micro manipulation which includes design and development of micro gripper, manipulation system, mathematical analysis, controlling behavior of IPMC and piezoelectric actuators, artificial muscles, flexible and compliant mechanism, robotic system. Dr. Mohammad Luqman has over 9 years of post-PhD experience in teaching, research and administration. He has served as a College Registrar and Advisor to Advisors. He has chaired many university, college, departmental level committees. He has co-edited two books in the field of Ion-Exchange Technology by Springer, and edited a book on Plasticizers with Intech Publishers. He is serving as a Chief Editor to American Chemical Science Journal, and Guest Editor to Special Volume for Advances in Materials Science and Engineering. He has published numerous high quality papers and book chapters. One of his recent papers secured its place at the “Cover Page” of the journal. One another paper was ranked the “First” among the “Top

25 Hottest Articles”, among “All” Chemistry Journals (108 journals) from April to June” during “2008. He is serving as an Adjunct Professor of Chemistry at VIT University Chennai, India. He has served as Assistant Professor of Polymer Science and Engineering, and Chemistry for over 7 years at King Saud University, Saudi Arabia, and A’Sharqiyah, Oman, respectively. He served as a Research Scientist in Samsung Cheil Industries, South Korea, and worked on the development of heat resistant polymers, organic glass, and block copolymers as impact modifiers and compatibilizers for engineering polymers. He served as a post-doctoral fellow at Artificial Muscle Research Center, Konkuk University, Korea. He earned his PhD in the field of Ionomers from Chosun University, South Korea. Dr. Luqman studied extensively the effects of various types of additives/plasticizers on the morphology and dynamic mechanical properties of ionomers. Prof. Abdullah M. Asiri is the Head of the Chemistry Department at King Abdulaziz University (KAU) since October 2009 and he is the founder and the Director of the Center of Excellence for Advanced Materials Research (CEAMR) since 2010 till date. He is the Professor of Organic Photochemistry. He graduated from King Abdulaziz University (KAU) with B.Sc. in Chemistry in 1990 and a Ph.D. from University of Wales, College of Cardiff, U.K. in 1995. His research interest covers color chemistry, synthesis of novel photochromic and thermochromic systems, synthesis of novel coloring matters and dyeing of textiles, materials chemistry, nanochemistry and nanotechnology, polymers and plastics. Prof. Asiri is the principal supervisors of many M.Sc. and Ph.D. theses. He is the main author of ten books of different chemistry disciplines. Prof. Asiri is the Editor-in-Chief of King Abdulaziz University Journal of Science. A major achievement of Prof. Asiri is the discovery of tribochromic compounds, a new class of compounds which change from slightly or colorless to deep colored when subjected to small pressure or when grind. This discovery was introduced to the scientific community as a new terminology published by IUPAC in 2000. This discovery was awarded a patent from European Patent office and from UK patent. Prof. Asiri involved in many committees at the KAU level and on the national level. He took a major role in the advanced materials committee working for KACST to identify the national plan for science and technology in 2007. Prof. Asiri played a major role in advancing the chemistry education and research in KAU. He has been awarded the best researchers from KAU for the past five years. He also awarded the Young Scientist Award from the Saudi Chemical Society in 2009 and also the first prize for the distinction in science from the Saudi Chemical Society in 2012. He also received a recognition certificate from the American Chemical Society (Gulf region Chapter) for the advancement of chemical science in the Kingdome. He received a Scopus certificate for the most publishing scientist in Saudi Arabia in chemistry in 2008. He is also a member of the editorial board of various journals of international repute. He is the Vice- President of Saudi Chemical Society (Western Province Branch). He holds four USA patents, more than one thousand publications in international journals, several book chapters and edited books.