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 FULL PAPERS
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5 A. Raafik, S. Aralekallu, S. Varhade, 5
6 Z. M. Bhat, A. R. Kottaichamy, 6
M. C. Devendrachari, M. Gautam,

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8 M. O. Thotiyl*........................... 1700337 8
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A Redox-Active Electrochemical
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1
2 A Redox-Active Electrochemical Decoder 1
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Pramod Gaikwad, Mahavir Misal, Siddhi Khaire, Abdul Raafik, Shambhulinga Aralekallu, 5
6 Swapnil Varhade, Zahid Manzoor Bhat, Alagar Raja Kottaichamy, Mruthyunjayachari 6

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8 Chattanahalli Devendrachari, Manu Gautam, and Musthafa Ottakam Thotiyl* 8
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11 HIGH logic is chemically reversible which 11
12 In communication systems, transmission of data between different locations is governed by hydronium ion concen- 12
13 requires encoders for encryption and decoders for decrypting encoded data. trations surrounding the redox-active 13
14 In modern digital devices, these functions are performed by transistors from electrode/electrolyte interface, thereby 14

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15 demonstrating extended cyclability over 15
their distinct logic levels. It is demonstrated that a redox-active interface
16 2000 cycles without any external voltage 16
17 with twin interfacial states can decrypt encoded information through electro- bias. It should be noted that the operation 17
18 chemical means; consequently, it can function as an electrochemical decoder of the redox switch in the logic HIGH and 18
19 in memory devices. The redox-active half-cell electrode/electrolyte interface of LOW states is analogues to a battery or a 19
20 the device furnishes bistable conducting and nonconducting states providing supercapacitor in the open circuit state or 20
21 shorted configuration.[12–19] 21
the logic HIGH and logic LOW levels of operation, respectively. The logic
22 22

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23 HIGH level of operation is prompted by self-charge injection into the redox- 23
24 active polymeric backbone which is confirmed by quartz crystal microbalance, 24
2. Results and Discussion
25 galvanostatic intermittent titration technique, and spectroelectrochemistry. A 25
26 single cathodic interface allows bistable interfacial chemistry; consequently, The electrochemical system consists of 26
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27 ‘n’ cell combination can process second possibilities demonstrating the four complete cells (Scheme 1). Alu- 27
28 minum (Al) was selected as the nega- 28
power of electrochemical interface in decoding encoded information.
29 tive half-cell due to its negative reduction 29
30 potential and redox active and con- 30
31 ducting polypyrrole (PPy) was chosen as 31
32 1. Introduction the positive electrode due to its positive formal potential, cur- 32
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33 rent versus potential curves (Figure S1, Supporting Informa- 33

34 In communication systems like networking, telecommu- tion). These half-cell electrodes were immersed in sulfuric 34
35 nication etc., encryption and decryption of the data require acid electrolytes because of the stability of Al in the presence 35
36 encoders and decoders, respectively.[1–4] Encoders usually con- of sulfate anions and doped and conducting states at the 36
37 vert the analog data to digital and its primary role is to com- polymeric interface.[20–23] In proposed decoder the combina- 37
38 press larger data into smaller outputs.[5–8] On the other hand, tion of both half-cells provides the necessary logic levels of 38
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39 decoders perform the opposite function by converting the operation (Scheme 1). A single cell provides binary voltage 39
40 digital encrypted data to analog outputs with the ability to levels, with a voltage HIGH (1) level and a voltage LOW (0) 40
41 convert single inputs into multiple outputs. Transistor-based level at the output. These two levels depend upon circuit 41
42 circuit elements with distinct logic levels are the fundamental shorting and open circuit between the electrodes of the half- 42
43 circuit elements in such applications.[9–11] Here we show an cells. The operation of the decoder is shown in Scheme 1 43
44 electrochemical interface with distinct logic levels derived along with the truth table in Table S1 (Supporting Information). 44
45 from their well-defined conducting and nonconducting states The distinct bistable states provided by the cathodic interface 45
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46 that can provide multiple outputs for an input signal thereby allowed two distinct possibilities therefore four cells can have 46
47 decrypting the information. We show that the logic LOW and 24 (16) possibilities (truth table, Table S1, Supporting Informa- 47
48 logic HIGH levels of the redox-active interface can process tion), allowing the cell combinations to handle multiple outputs 48
49 information by electrochemical means, therefore can function with lesser number of input switches. These demonstrate that 49
50 as an electrochemical decoder in memory devices. The active electrochemical interface can decode the information thereby 50
51 functioning as an electrochemical decoder. 51
52 The cyclability of the switch crucially depends upon the 52
P. Gaikwad, M. Misal, S. Khaire, A. Raafik, S. Aralekallu, S. Varhade,
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Z. M. Bhat, A. R. Kottaichamy, M. C. Devendrachari, M. Gautam, redox-active PPy cathode and its chemical reversibility as
54 M. O. Thotiyl Al anode is in excess. The cyclic voltammogram (Figure S1, 54
55 Department of Chemistry and Center for Energy Science Supporting Information) and the polarization (Figure 1a) 55
56 Indian Institute of Science Education and Research (IISER) Pune clearly demonstrate a transition from nonconducting to con- 56
Q2 Dr. Homi Bhabha Road, Pashan, Pune 411008, India
57 E-mail: musthafa@iiserpune.ac.in
ducting state which is well known for redox-active conducting 57
58 polymers.[24,25] The maximum power available from such a 58
59 DOI: 10.1002/admt.201700337 cell is ≈0.37 mW cm−2 with respect to the cathode (Figure 1a), 59

Adv. Mater. Technol. 2018, 1700337 1700337  (1 of 7) © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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1 any voltage bias is investigated by short-cir- 1

2 cuiting the cathode with negative electrode 2
3 for 20 s and then relaxing the system to the 3

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4 open circuit (Figure 1b). As shown, after 4
5 the fall time (tf) or the time required for the 5
6 signal to fall from its 90% to its 10% value, 6

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7 the rise time (tr) or the time required for 7
8 the signal to rise from its 10% to 90% value 8
9 is ≈100 s. These suggest that the redox-active 9
10 polymer can self-recover to its conducting 10
11 form which is governed by the sur- 11
12 rounding media as reported by others.[26–31] 12
13 It is well known that the redox energy of the 13
14 redox-active polymers can be tuned by the 14

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15 medium in which they are housed and acidic 15
16 pH can chemically reverse the polymer from 16
17 its nonconducting to conducting form.[26–31] 17
18 Therefore during tf period a transition from 18
19 conducting to nonconducting form should 19
20 occur and during the tr period, the polymer 20
21 Scheme 1. Schematic illustration of redox-active electrochemical decoder. M1 is metallic should recover to its conducting state which 21
22 aluminum anode and P2 is a polypyrrole cathode immersed in acidic solution. in turn is governed by the medium in which 22

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23 they are housed. These transitions are fur- 23
24 suggesting the performance is limited by the cathode. However ther investigated by UV–vis spectroscopy and galvanostatic dis- 24
25 the power levels can be amplified by increasing the amounts of charge curves (Figure 1c; Figure S2, Supporting Information). 25
26 PPy cathode on the current collector. As there is no voltage input UV–vis spectra clearly demonstrate the shifting of the absorp- 26
27
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to revitalize the cathode, its chemical reversibility is crucially tion band from longer to shorter wavelength on short circuit 27
28 dependent on the self-charge injection kinetics. The chemical which is indicative of conducting to nonconducting transition. 28
29 reversibility from nonconducting to conducting state without It is to be noted that as prepared polymer samples were in the 29
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Figure 1.  a) Polarization curves for Al-PPy electrochemical decoder by ramping the current till the cell voltage drops to 0 V, b) rise time (tr) measure-
57 ments of Al-PPy decoder in 1 m H2SO4, c) UV–vis spectra of redox-active polymeric interface of the electrochemical decoder at different tr intervals and 57
58 d) electrochemical impedance spectra of Al-PPy electrochemical decoder at tr different periods. The impedance spectra were collected at 0 V versus 58
59 OCV in the frequency range of 100 kHz to 10 mHz with 10 mV peak to peak AC amplitude. 59

Adv. Mater. Technol. 2018, 1700337 1700337  (2 of 7) © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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1 conducting state, scanning electron microscopy (SEM) and changing rapidly with time. We note that the electrochemical 1
2 energy dispersive X-ray spectroscopy (EDS) (Figure S3, Sup- system proposed here has a slow switching speed compared to 2
3 porting Information). EDS clearly demonstrates the presence of existing systems, however the system at hand can be modified 3

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4 chloride dopant (Figure S3b, Supporting Information), demon- to achieve a lower switching time by tailoring the logic levels 4
5 strating as synthesized polymer is in the conducting form. On of the electrochemical switch. By changing the upper threshold 5
6 relaxing the short circuit, in shorter time tr scale (≈200 s), the (HIGH) level to 60% (Figure S5 and Table S3, Supporting Infor- 6

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7 polymer recovered to its conducting state noticeably, however on mation), a switching time of ≈15 s can be achieved. This kind 7
8 longer tr time scale (≈1000 s), the self-recovery was significant. of redox-active electrochemical decoder system would be appli- 8
9 Galvanostatic discharge after the first discharge with a shorter cable for telecommunication network, video game remote con- 9
10 tr time scale (≈200 s) furnished ≈80% of its first discharge trol, one way traffic counting, electrochemical keyboard, weight 10
11 capacity, however on longer tr scale (≈1000 s) it could recover control, etc. This electrochemical decoder can be a potential 11
12 to >90% of its first discharge capacity. This is further sup- candidate for applications where the operating speed is below 12
13 ported by electrochemical impedance spectroscopy (Figure 1d), ≈240 cycles per hour. 13
14 where the diameter of the semi-circle reflecting the charge Galvanostatic intermittent titration technique (GITT) and 14

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15 transfer resistance increased during tf period and decreased quartz crystal microbalance (QCM) techniques were further 15
16 during the tr period (Figure S4, Table S2, Supporting Informa- used to evaluate these aspects (Figure 2). As shown in Figure 2a, 16
17 tion). All these demonstrate a conducting to nonconducting the relaxation voltage (after the iR drop) on the removal of cur- 17
18 transition in the redox-active conducting polymeric half-cell on rent pulse is regained to ≈85% of its value after 60 min and 18
19 circuit shorting and its chemical reversal to conducting state it was sustainable for several cycles. The QCM data during 19
20 on relaxing the short circuit. In essence the proposed electro- tr period demonstrate a decrease in frequency with a simul- 20
21 chemical decoder is a self-charging battery (induced by charge taneous increase in mass with respect to tf period.[32,33] The 21
22 injection into the polymer) with a distinct power output, there- resistance profile demonstrated an increase during the tf period 22

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23 fore it does not need any external switching power to attain the (due to the transition from conducting to nonconducting state) 23
24 logic high level. Nonetheless the switching speed of the device and its reversal during the tr period (due to the transition from 24
25 during the relaxation to logic high level is controlled by the nonconducting to conducting state). These confirm that PPy 25
26 kinetics of self-charge injection which is controlled by the con- possesses distinct bistable states and it can self-recover to its 26
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27 ducting polymer electrode and the nature of the injecting anion. conducting state which in turn is governed by the surrounding 27
28 The switching speed is important in applications where input is medium. The long term cyclability of the redox switch for 28
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Figure 2.  a) Galvanostatic intermittent titration technique of Al-PPy electrochemical decoder on continuous cycling. A current of 200 µA cm−2 was
57 applied for 5 min and the system was relaxed to its open circuit (at zero current) for 1 h. b) Frequency shift versus time plots, corresponding c) mass 57
58 change versus time plots and d) resistance versus time plots. A current pulse of 200 µA cm−2 was applied for 5 min and the system was allowed to 58
59 relax to its open circuit during quartz crystal microbalance studies. 59

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Figure 3.  a) Cycling studies of Al-PPy-based redox decoder for 2000 cycles at constant tr = 200 s and tf = 20 s, b) the relaxation voltage for a fixed
tr versus cycle number, c) rise time for a fixed voltage versus cycle number and d) digital photograph of electrochemical decoder.
27
28 28
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30 2000 cycles is shown in Figure 3a demonstrating decent cycla- 3. Conclusion 30
31 bility with sufficient stability. The voltage attained after relaxa- 31
32 tion in the time limit employed, Figure 3b demonstrates a slight We have demonstrated a redox-active electrochemical decoder 32
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33 voltage decline during cycling; however it maintained ≈90% of based on negative metallic and positive polymeric half-cell elec- 33
34 its voltage with respect to first cycle. The relaxation time for trodes whose bistable logic levels can decrypt encoded infor- 34
35 attaining a fixed voltage demonstrates an opposite trend during mation. The distinct bistable states provided by the cathodic 35
36 cycling with an increase from ≈100 to ≈140 s at the end of interface allowed two distinct possibilities; therefore, n cells 36
37 2000 cycles (Figure 3c). The decrease in cell voltage with a could process 2n possibilities. The bistable chemistry at the 37
38 concomitant increase relaxation time could be due to repeated cathodic interface is confirmed to be a transition from con- 38
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39 swelling and contraction of the polymer during repeated doping ducting to nonconducting during the tf period and its reversal 39
40 and de-doping processes. These kinds of volume expansion and during the tr period is solvent assisted. The decoder demon- 40
41 contraction of the cathode may lead to crack in the polymer strated extended cyclability over 2000 with decent stability at 41
42 with its ultimate delamination in the long run.[34,35] Other pos- respective interfaces. 42
43 sibility could be the surface passivation of Al in H2SO4.[36,37] 43
44 A single cell has two possibilities and therefore the number 44
45 of possibilities with n cells will be 2n. There are 16 possibilities 45
4. Experimental Section
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46 with four cells in series as demonstrated in Table S1 (Supporting 46

47 Information) suggesting 16 characters can be processed elec- Materials and Methods: Pyrrole, HCl, H2SO4, and ferric chloride 47
48 trochemically with the help of four complete cells (Figure 3d; (FeCl3) were obtained from Sigma Aldrich India. Monomer was distilled 48
49 Figure S6, Supporting Information) indicating that it can prior to the polymerization reaction. 49
Synthesis of Polymers and Fabrication of Electrochemical Decoder:
50 handle multiple outputs with lesser number of input switches. Polypyrrole conducting polymer was prepared by using, monomer
50
51 This demonstrates its function as an electrochemical decoder. (1 g of pyrrole) was dissolved in 1 m HCl (80 mL) solution.[38–40] To the 51 Q4
52 The operation of the decoder is explained in the Experimental monomer solution ferric chloride in water was added drop by drop with 52
53 Section and a four-cell combination can process 16 characters. vigorous stirring for 24 h. The product collected by filtration was washed 53
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54 This is demonstrated in Video S1 (Supporting Information) thoroughly with acid and plenty of water and then dried in vacuum oven 54
55 where the short circuiting of the half-cell electrodes triggered for 15 h. Slurry was made by dispersing polypyrrole in isopropyl alcohol 55
with 5 wt% PTFE and then it was coated on substrate of titanium nitride
56 the logic LOW level and on relaxing, the surrounding solu- 56
current collector for decoder fabrication and performance evaluation.
57 tion governed the attainment of active HIGH logic, Video S1 Al negative electrode (4 × 1 cm) and PPy positive electrode (4 × 1 cm) 57
58 (Supporting Information), thereby decoding the information were housed in acidic medium to make the electrochemical decoder as 58
59 electrochemically. shown in Scheme 1. 59

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1 Characterization: SEIKO-EG&G QCM922A was used to carry out EQCM Supporting Information 1
2 measurements in four-cell electrochemical decoder system using PPy 2
covered Au coated quartz crystal as the resonating crystal (8.95 MHz). Supporting Information is available from the Wiley Online Library or
3 3
During the relaxation period at zero current and discharge period from the author.

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4 at 200 µA cm−2, the frequency and mass changes were monitored.
4
5 Surface morphology and elemental composition of PPy cathode was 5
6 monitored by JSM-5300LV (Japan) SEM. Transmittance of the PPy 6
Acknowledgements

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7 electrode in the UV–vis region before and after use in electrochemical 7
8 decoder was monitored by a VMP-300 Biologic machine. In a two- M.O.T. acknowledges financial assistance from DST-SERB, MHRD and 8
9 electrode electrochemical decoder system, GITT measurements were DST-Nanomission, India. 9
carried out by applying a relaxation period for 1 h and a discharge
10 10
current of 200 µA cm−2 for 5 min. Nyquist plots were obtained
11 for the PPy electrode in the frequency range of 100 kHz to 10 mHz 11
12 at 0 V versus Open- circuit voltage (OCV). A 10 mV peak to peak Conflict of Interest 12
13 AC excitation signal was employed for exciting the interface. A The authors declare no conflict of interest. 13
14 VMP-300 Biologic electrochemical workstation was used to obtain 14

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15 electrochemical information. 15
Device Fabrication and Operation of Electrochemical Decoder: Redox-
16 16
active polymer-based electrochemical decoder was fabricated by using Keywords 17
17 four electrochemical switches. Each switch has made with aluminum
18 as an anode and PPy as a cathode. The standard reduction potential of communication systems, conducting polymer, electrochemical decoder, 18
19 aluminum was −1.65 V and the calculated formal potential of polypyrrole memory device, potentiometric device 19
20 was 0.2 V versus Ag/AgCl (3 m KCl). Therefore the total cell voltage 20
should be ≈1.8 V but practically the obtained voltage was ≈1.2 V possibly Received: November 17, 2017
21 Revised: December 19, 2017
21
22 because of the losses at the anode. In this electrochemical decoder, 22

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single polyacrylic compartments for fixing the half-cell electrodes were Published online:
23 used. Electrochemical decoder provides bistable voltage levels (HIGH/
23
24 LOW) at the output and these levels depend upon circuit shorting and 24
25 open circuit between the half-cell electrodes (Scheme 1). 25
26 Initially, the half-cell electrodes were immersed in H2SO4 (1 m) [1] C. Paola, B. Giacomo, B. Vincenzo, Angew. Chem. 2009, 121, 8668. 26
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27 electrolyte solution and the electromotive force was generated due [2] A. Grunnet-Jepsen, A. E. Johnson, E. S. Maniloff, T. W. Mossburg, 27
28 to the different redox potentials of the half-cells. The voltage across M. J. Munroe, J. N. Sweetser, Electron. Lett. 1999, 35, 1096. 28
Al-PPy cell was ≈1.2 V initially due to the conducting form of PPy half- [3] N. Wada, G. Cincotti, S. Yoshima, N. Kataoka, K. Kitayama, J. Lightwave
29 29
cell as shown in Scheme 1. This is taken as the logic “HIGH” level Technol. 2006, 24, 0733.
30 of electrochemical decoder (Scheme 1). By pushing the substrate 30
[4] N. Kock, Decis. Support Syst. 2007, 44, 175.
31 platform of the redox decoder, the spring connecting the electrodes 31
[5] W. Bender, D. Gruhl, N. Morimoto, A. Lu, IBM Syst. J. 1996, 35, 313.
32 got shorted, forcing the reduction of cathodic interface. This 32
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[6] G. J. Sullivan, T. Weigand, Proc. IEEE 2005, 93, 18.

33 prompted the transition of conducting to nonconducting form at the 33
[7] P. H. Ang, P. A. Ruetz, D. Auld, IEEE Spectrum 1991, 28, 16.
34 polymeric interface and the voltage fell to 0 V. This was taken as the 34
[8] C. Chrysafis, A. Ortega, IEEE Trans. Image Process. 2000, 9, 378.
logic “LOW” level of electrochemical decoder (Scheme 1). By using
35 [9] P. Agnihotri, P. Dhakras, J. U. Lee, Nano Lett. 2016, 16, 4355. 35
four electrochemical cells (4-bit), 16 combinations of analog voltage
36 levels were made. These analog levels acted as an input address [10] M. J. Rozenberg, I. H. Inoue, M. J. Sanchez, Phys. Rev. Lett. 2004, 36
37 for electrochemical decoder. For these corresponding addresses, 92, 178302. 37
38 alphanumeric output was printed onto the liquid crystal display (LCD) [11] K. Kim, S. Gaba, D. Wheeler, J. M. Cruz-Albrecht, T. Hussain, 38
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39 and seven segment display. N. Srinivasa, W. Lu, Nano Lett. 2012, 12, 389. 39
40 When a force was applied on one of the electrochemical cell say on “A” [12] J. Borghetti, G. S. Snider, P. J. Kuekes, J. J. Yang, D. R. Stewart, 40
(put weights on substrate platform of “A”) and simultaneously released R. S. Williams, Nature 2010, 464, 873.
41 41
the forces on electrochemical cells B, C, and D, the electrochemical cell [13] H. G. Jung, J. Hassoun, J. B. Park, Y. K. Sun, B. Scrosati, Nat. Chem.
42 A would be shorted as a result of compression of springs attached to the 2012, 4, 579.
42
43 electrodes. The voltage for the cell decreased toward 0 V. On the other [14] Y. Chen, S. A. Freunberger, Z. Peng, O. Fontaine, P. G. Bruce, Nat. 43
44 hand, in switch B, C, and D, redox-active conducting polymer remained Chem. 2013, 5, 489. 44
45 in the conducting state leading to the logic HIGH level (1.2 V). This [15] Y. Wang, Y. Xia, Adv. Mater. 2013, 25, 5336. 45
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46 condition was taken as the logic A = 0 (0 V), B = 1 (1.2 V), C = 1 (1.2 V), [16] C. Arbizzani, M. Mastragostino, L. Meneghello, R. Paraventi, Adv. 46
47 and D = 1 (1.2 V). This was considered as the input address (0111) Mater. 1996, 8, 4. 47
(Table S1, Supporting Information). The redox-active potential outputs [17] A. L. M. Reddy, P. Chumyim, S. R. Jadhav, G. John, P. M. Ajayan,
48 48
were given to analog input of Arduino Uno board (Microcontroller Sci. Rep. 2012, 2, 960.
49 Atmega328). Microcontroller is an integrated circuit (IC) component 49
50 [18] V. G. Anju, R. Manjunatha, P. M. Austeria, S. Sampath, J. Mater. 50
useful to automatically control the device. The programs written in
Chem. A 2016, 4, 5258.
51 “C” language was uploaded into the microcontroller. Microcontroller 51
[19] H. Cheng, K. Scott, Electrochim. Acta 2014, 116, 51.
52 has an inbuilt comparator and comparator is an electronic device, 52
which can compare electrochemical signal. According to the program, [20] Y. Zhai, Y. Dou, D. Zhai, P. F. Fulvio, R. T. Mayes, S. Dai, Adv. Mater.
53 53
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microcontroller compared the output signals of electrochemical cells 2011, 23, 4828.
54 [21] X. Xia, D. Chao, X. Qi, Q. Xiong, Y. Zhang, J. Tu, H. Zhang, H. Fan, 54
and also declared the electrochemical input address (0111). The in-built
55 comparator compared these inputs and corresponding numerical output J. Nano Lett. 2013, 13, 4562. 55 Q5
56 “8” was shown on LCD as well as on seven segment display. Figure S6 [22] R. T. Foley, T. H. Nguyen, J. Electrochem. Soc. 1982, 129, 464. 56
57 (Supporting Information) shows block diagram, electrochemical switch [23] R. Mukkabla, M. Deepa, A. K. Srivastava, RSC Adv. 2015, 5, 99164. 57
58 assembly, and circuit diagram and hardware system for electrochemical [24] D. P. Dubal, S. H. Lee, J. G. Kim, W. B. Kim, C. D. Lokhande, 58
59 decoder. J. Mater. Chem. 2012, 22, 3044. 59

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