MEV Journal of Mechatronics, Electrical Power, and Vehicular Technology 12 (2021) 45-50 Journal of Mechatronics, Electrical Power, and Vehicular Technology e-ISSN: 2088-6985 p-ISSN: 2087-3379 mev.lipi.go.id doi: https://dx.doi.org/10.14203/j.mev.2021.v12.45-50 2088-6985 / 2087-3379 ©2021 Research Centre for Electrical Power and Mechatronics - Indonesian Institute of Sciences (RCEPM LIPI). This is an open access article under the CC BY-NC-SA license (https://creativecommons.org/licenses/by-nc-sa/4.0/). MEV is Sinta 1 Journal (https://sinta.ristekbrin.go.id/journals/detail?id=814) accredited by Ministry of Research & Technology, Republic Indonesia. Phosphate ion sensor fabrication based on conductive polymer polypyrrole film coatings in doped phosphate using thick film technology Nofriyani a, *, Robeth Viktoria Manurung b, Aminuddin Debataraja c, Indra Dwisaputra a a Electrical Engineering Department, Politeknik Manufaktur Negeri Bangka Belitung Kawasan Industri Air Katung Sungailiat Bangka, Bangka-Belitung, 33211 Indonesia b Research Center for Electronics and Telecommunications, Indonesian Institute of Sciences Jl. Cisitu, Sangkuriang, Bandung, West Java, 40135 Indonesia c Electrical Engineering Department, Politeknik Negeri Jakarta Jl. Prof. DR. G.A. Siwabessy, Kukusan, Beji, Depok, West Java, 16424 Indonesia Received 15 April 2021; Accepted 26 June 2021; Published online 31 July 2021 Abstract This study describes the development of chemical sensors to detect polypyrrole (PPy) based phosphate sensors in doped di-ammonium hydrogen phosphate (DAP) with thick film technology (TFT). Manufacturing screen-printed carbon electrode (SPCE) with thick film uses alumina substrate provided a more portable, miniature, inexpensive, and reduced use of samples and reagents. Polymer polypyrrole and di-ammonium hydrogen phosphate as sensitive membranes are electrodeposition on carbon electrodes. Characterization has been conducted to see the electrode morphology in scanning electron microscopy (SEM) test, which showed that sensitive material particles were distributed evenly on the surface of the sample and spherical. The energy dispersive spectroscopy (EDS) experiment results showed the atomic composition respectively carbon 86.95 %, nitrogen 6.94 %, oxygen 5.9 %, and phosphate 0.21 %, which were exposed to the electrode. The performance test of electrodes with a phosphate standard solution has proceeded at a concentration between 5 to 100 mg/l, which is measured using the galvanostatic method. The voltage range was from 0.252 to 0.957 V with R2 at approximately 90.265 %. The results of sensor performance were concluded that the electrode was able to detect phosphate ions. ©2021 Research Centre for Electrical Power and Mechatronics - Indonesian Institute of Sciences. This is an open access article under the CC BY-NC-SA license (https://creativecommons.org/licenses/by-nc-sa/4.0/). Keywords: carbon electrode; electropolimerization; phosphate; polymer polypyrrole; thick film. I. Introduction Excessive use of fertilizers on agricultural land causes the risk of environmental pollution, degradation of soil structure, and decreased groundwater levels. Monitoring and analysis of precision farming soil are needed to monitor the main nutrient contents such as nitrogen (N), phosphate (P), or potassium (K) on agricultural land before farming activities are carried out [1]. Therefore, instrumentation devices are needed to detect nutrient content on agricultural soil. In previous studies, sensor design and fabrication studies for precision farming. Sensor terminology is strongly influenced by the substrate, the conductivity of the electrode, and the sensitive material [2]. Microelectromechanical system (MEMS) technology is carried out to miniaturize the sensor, portable size, and reduce the consumption of the sample and reagent integrated into one piece of substrate. The substrate used for the phosphate sensor is a polyester film, polyvinyl chloride (PVC), filter paper, and carbon fiber [3][4][5]. The materials used for electrodes are gold paste, silver, cobalt, black carbon nanoparticles, graphite, and lead [6][7][8]. Sensitive polymer polypyrrole (PPy) membrane has been used for biosensors, electrochemical sensors, protein sensors, glucose biosensors, clofibric acid sensors, non-enzyme sensors, and nitrate selectivity sensors [9][10][11]. * Corresponding Author. Tel: +62-823-3729-1941 E-mail address: nofriyani03@gmail.com https://dx.doi.org/10.14203/j.mev.2021.v12.45-50 http://u.lipi.go.id/1436264155 http://u.lipi.go.id/1434164106 https://mev.lipi.go.id/mev/index https://dx.doi.org/10.14203/j.mev.2021.v12.45-50 https://creativecommons.org/licenses/by-nc-sa/4.0/ https://sinta.ristekbrin.go.id/journals/detail?id=814 https://crossmark.crossref.org/dialog/?doi=10.14203/j.mev.2021.v12.45-50&domain=pdf https://creativecommons.org/licenses/by-nc-sa/4.0/ Nofriyani et al. / Journal of Mechatronics, Electrical Power, and Vehicular Technology 12 (2021) 45-50 46 According to the previous literature, this study will be carried out on the development of phosphate ion sensor fabrication of thick film technology. Sensitive membrane sensors based on polymer polypyrrole (PPy) film layer are doped with a solution of di-ammonium hydrogen phosphate (DAP) on a carbon electrode screened-printing onto the aluminum substrate. The study was conducted to improve the performance of electrodes to detect phosphate ions in precision farming. This research focuses on the sensitive membrane used. It is printed on carbon electrodes using an alumina substrate with PPy membrane and DAP using thick-film technology. The phosphate ion sensor consists of three electrodes, the working electrode, the counter electrode, and the reference electrode. This study focuses on fabricating precision farming sensors that are specifically aimed to detect ion phosphate nutrients. The morphological characteristics testing and composition of electrode material were conducted using SEM and EDS [12]. The electrode performance testing is implemented to obtain a good sensor performance (sensitivity, limit detection, response time, and linearity). II. Materials and Methods A. Equipment and reagent Supporting equipment are used in this study are screen printing, screen maker machine, printing machine, firing machine, oven, stative, beaker glass, micropipette, magnetic stirrer, nitrogen tube, power supply, Accumet solid-state half cell ISE (Fisherbrand), multimeters (SANWA PC-550), computers, SEM and EDS (SU3500). Materials used in this study are alumina substrate (Al2O3), silver | silver chloride (Ag | AgCl) conductor paste (Ferro), platinized carbon paste (C2000511D1), protective film, ulana 133, ulano film, deionized water with 17 MΩ resi st i vi ties, 98 % grade pyrrole reagent (Aldrich), ammonium hydrogen phosphate (Merck), aluminum oxide (Merck), phosphate standard solution (Merck), and potassium chloride (KCL). B. Fabrication of electrode The electrode design is needed to determine the pattern, dimensions, and electrode layout that use thick film technology with a screen-printing technique that aims to determine the effect of the path width on the sensor sensitivity. The Electrode design is made by using Corel draw software. The thick film technology process consists of screen making, electrode printing, drying, firing, pin installation, and packaging. As the first stages, the reference electrode and conjunction pad are printed on the alumina substrate using paste (Ag | AgCl). Then it was dried in an oven to minimize the liquid that is bound to the electrode. The process is continued by gradually firing with a temperature of 0 to 800 °C for 30 minutes in a furnace firing sinters machine. The next stage is printing the working electrodes and counter electrodes using platinized carbon paste, then dried material with a temperature of 0 to 120 °C for 15 minutes to bind the exposed carbon to the alumina substrate. Then the packaging is carried out, so the electrodes are ready to use. The configuration of electrodes fabrication stages is shown in Figure 1. C. Electrodeposition of polypyrrole doped DAP Electrodeposition of pyrrole doped with DAP onto carbon was performed by an electrochemical process. In the first step, polypyrrole must be purified with powdered alumina oxide in a dark room to remove the substances that were oxidized with the air. Amperometric used as a constant voltage source for electrodeposition. The initial polymerization solution consisted of PPy (C4H4NH) [1M] doped with a solution of DAP ((NH4)2HPO4) [0.1M] dissolved with deionized water. The electrodeposition with the amperometric method is implemented by adjusting the constant voltage source of 1 V connected to the carbon electrode and the platinum plate anode so that an oxidation reaction occurs to the sensitive membrane solution by flowing purging with nitrogen gas experiment. The deposition of the carbon electrode is executed for 30 minutes by measuring the changes in current during the electropolymerization process. Freshly prepare electrodeposition sample, the electrode then must be immersed in a solution ((NH4)2HPO4) [0.01M] for 24 hours in a dark room. D. Testing performance sensor Sensor performance testing was conducted using a potentiostat to control the electrodes and measure the experiment electroanalytical (Figure 2). The previous research on measurement electrodes used the amperometric method [4]. The galvanostatic was used as a constant current source set at 0.7 V, with a resistance of 10 kΩ as input to get the response output voltage. The Electrodes are connected to the conditioning signal circuit, and then it is dipped into a phosphate standard solution (PO4 3-) with a concentration of 5 mg/l, 25 mg/l, 50 mg/l, and 100 mg/l. The multimeter is connected to the sensor output to measure the output voltage, while the acquisition data is transferred to the computer. The testing is repeated five times in 10 minutes for each of test sample. Figure 1. Screen printing electrode Nofriyani et al. / Journal of Mechatronics, Electrical Power, and Vehicular Technology 12 (2021) 45-50 47 III. Results and Discussions A. Electrodes of sensor The Phosphate sensor consists of three electrodes, the working electrode, the reference electrode, and the counter electrode. On 50 × 50 mm substrate alumina, the reference electrode was printed with a size of 21.21 × 3.5 mm and the conjunction pad sized on 3.95 × 1.5 mm. The Carbon electrodes in a comb shape were sized on 21.31 × 2.28 mm. The electrode Prototype to detect the phosphate fabricated ion by using thick-film technology is shown in Figure 3. B. The morphological and composition material testing The morphological characteristics testing was implemented by the scanning electron microscope (SEM) method. The 'before and after' of carbon electrode morphology is being coated with a polymer-sensitive polypyrrole membrane which is doped with ((NH4)2 HPO4) solution is shown in Figure 4. The differences of topographic surface in the before and after electrodes electropolymerization can be seen according to the morphological testing using SEM. The analyzed surface polypyrrole has using SEM to observe the morphology of ion- sensitive membrane [13]. The coated surface of the sensitive membrane is more evenly distributed than before. The particles have significantly shown dissimilar. The Polymerized electrodes were seen at a magnification of 20,000 secondary electrons with 10 kV. The morphology sample with a size of 2 µm showed that spherical particles were distributed evenly on the electrode surface. After that, energy dispersive spectroscopy (EDS) was tested (shown in Table 1) to determine the atom composition at the electropolymerized electrodes. The EDS results showed the composition of atoms, namely carbon at 86.95 %, Nitrogen at 6.94 %, oxygen at 5.9 %, and phosphate at 0.21 %. Based on the percentage, the phosphate atomic elements are greatly small because they are comparable with the concentration of the used solution ((NH4)2HPO4) of 0.1 mol/l. C. Electrodeposition testing Measurement of current response by amperometric method on electrodeposition shows the occurrence of PPy and DAP as sensitive membrane coating on carbon electrodes. The Electrode electrodeposition experiment is shown in Figure 5. The Current measurement results for 30 minutes showed the output current response in the range of 0.03 to 0.2 mA with the presence of a stable current change during electropolymerization. In addition, there was an accretion of sensitive membranes on carbon electrodes. Figure 2. Testing performance sensor Reference Electrode Working Electrode Cou nter Electrode Alu mina Subs trate Pad Figure 3. Prototype electrode (a) (b) Figure 4. SEM photograph. (a) Electrode carbon before electropolimerization; (b) Electrode carbon and PPy after electropolimerization Nofriyani et al. / Journal of Mechatronics, Electrical Power, and Vehicular Technology 12 (2021) 45-50 48 D. Electrode stability The reference electrode of the Ag | AgCl testing was implemented to see the stability of the electrode performance. As a result, the electrode has been the stability of the reference electrode [13]. The testing is executed by comparing the reference electrodes with commercial, which is tested in a KCl [3M] solution. The average voltage of the reference electrode test obtained the output at 6.8 to 7.4 mV. The reference electrode experiment is shown in Figure 6. The test is executed for 30 minutes. The experiment shows that the reference electrode voltage is relatively stable. E. Sensor performance testing The output response of performance ion sensor using phosphate solution concentration is 0.252 V to 0.957 V, which indicates that the higher the phosphate concentration is detected, the output voltage is increased. The peak intensity was increased with the increasing phosphate concentration shows the sensor's better response with different concentrations of phosphate [6]. The discussed research has been shown the limit of detection ion phosphate based on different conductive electrodes [6][7][14]. This study's limit of detection ion phosphate is 5 mg/l with a linear range of 5 to 100 mg/l phosphate solution. The result of the output voltage chart to the solution concentration obtained a sensitivity of 0.008 V for every addition concentration and regression value (R2 = 90.265 %) which shows a linear response. Furthermore, measurement performance at the phosphate sensor resulted has shown that response linear [13][15]. Therefore, the output voltage at the electrode test can be used as a sensor to detect phosphate ions. The output response sensor performance of the average voltage from the electrode is shown in Figure 7. Improvement is achieved result compared to previous research, the analytic parameter sensor phosphate detection is shown Table 2. Table 1. Result of EDS electrodes experiment Element Element Composition Weight percent (wt. %) Atomic percent (at. %) Data error (%)* Net interpret element The pure element standard (K-Ratio) Atomic number corection (Z) Atomic number corection (A) Secondary fluorescence correctiion (F) C K 84.10 86.9 3.5 24.95 0.680 1.01 0.80 1 N K 7.82 6.9 25.1 28.40 0.005 0.98 0.06 1 O K 7.59 5.9 17.8 68.90 0.007 0.96 0.09 1 P K 0.53 0.2 4.2 56.80 0.004 0.82 0.98 1 *Data error is comparison both eZAF (standardless- based correction factor nation) and P/B (peak to background ratio element) method Figure 5. Output response of electrodeposition electrodes 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0.10 0.11 0.12 0.13 0.14 0.15 0.16 0.17 0.18 0.19 0.20 0.21 00 :0 0. 0 00 :4 5. 5 01 :3 1. 0 02 :1 6. 5 03 :0 2. 0 03 :4 7. 5 04 :3 3. 0 05 :1 8. 5 06 :0 4. 0 06 :4 9. 5 07 :3 5. 0 08 :2 0. 5 09 :0 6. 0 09 :5 1. 5 10 :3 7. 0 11 :2 2. 5 12 :0 8. 0 12 :5 3. 5 13 :3 9. 0 14 :2 4. 5 15 :1 0. 0 15 :5 5. 5 16 :4 1. 0 17 :2 6. 5 18 :1 2. 0 18 :5 7. 5 19 :4 3. 0 20 :2 8. 5 21 :1 4. 0 21 :5 9. 5 22 :4 5. 0 23 :3 0. 5 24 :1 6. 0 25 :0 1. 5 25 :4 7. 0 26 :3 2. 5 27 :1 8. 0 28 :0 3. 5 28 :4 9. 0 29 :3 4. 5 Cu rr en t ( I) m A Time (minutes) Figure 6. Output response stability reference electrode 6.8 6.9 7 7.1 7.2 7.3 7.4 7.5 0 5 10 15 20 25 30 vo lta ge (m V) time (minutes) Nofriyani et al. / Journal of Mechatronics, Electrical Power, and Vehicular Technology 12 (2021) 45-50 49 IV. Conclusion Sensitive membrane coating that uses polymer polypyrrole doped with di-ammonium phosphate was successfully implemented using the electropolymerization method. The occurrence of electropolymerization is shown by the output current flowing in the electrode ranging from 0.2 to 0.03 mA. The sensitive membrane layer in the SEM test shows that it is evenly distributed on the surface of the electrode and spherical. According to the EDS test, it showed the percentage of each atom those are carbon (C) 86.95 %, nitrogen (N) 6.94 %, oxygen (O) 5.9 %, and phosphate (P) 0.21 %. The stability test of reference versus commercial electrodes shows a stable voltage output in the range of 6.8 to 7.4 mV. The performance testing at a concentration of 5 to 100 mg/l phosphate standard solution - shows the output voltage ranges from 0.252 V to 0.957 V, with a sensitivity of 0.008 V for every addition concentration and linear regression performance of sensor ion phosphate (R2 = 90.267 %). According to the testing, as the results, the electrode is capable of detecting the phosphate ion. Acknowledgment The author would like to say thank you very much to the researcher at the Research Center for Electronics and Telecommunication, Indonesian Institute of Sciences (LIPI), Bandung for supporting all of these study activities. Declarations Author contribution Norfriyani contributed as the main contributor of this paper. All authors read and approved the final paper. Funding statement This research did not receive any specific grant from funding agencies in the public, commercial, or not-for- profit sectors. Conflict of interest The authors declare no known conflict of financial interest or personal relationships that could have appeared to influence the work reported in this paper. Additional information Reprints and permission information is available at https://mev.lipi.go.id/. 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Materials and Methods A. Equipment and reagent B. Fabrication of electrode C. Electrodeposition of polypyrrole doped DAP D. Testing performance sensor III. Results and Discussions A. Electrodes of sensor B. The morphological and composition material testing C. Electrodeposition testing D. Electrode stability E. Sensor performance testing IV. Conclusion Acknowledgment Declarations Author contribution Funding statement Conflict of interest Additional information References