Optimising Sodium Borohydride Reduction of Platinum onto Nafion-117 in the Electroless Plating of Ionic Polymer–Metal Composites
Abstract
:1. Introduction
2. Materials and Methods
2.1. IPMC Preparation
2.2. Full Factorial Design for Sodium Borohydride Reduction
2.3. Surface Resistance Measurements
2.4. IPMC Displacement Measurement
2.5. IPMC Blocking Force Measurement
2.6. Scanning Electron Microscopy
3. Results and Discussion
3.1. Concentration
3.2. Stir Time
3.3. Temperature
3.4. Scanning Electron Microscopy Results
3.5. IPMC Performance
4. Limitations and Recommendations
5. Conclusions
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
Appendix A
FF1 | FF2 | FF3 | ||||||
837,545.077 | 2,381,020.195 | 582.518 | 9.979 | 36.336 | 19.905 | 7.03 | 23.759 | 8.632 |
1,934,525.223 | 2,754,967.048 | 4682.585 | 7.927 | 21.9 | 23.526 | 7.927 | 11.611 | 8.898 |
905,504.633 | 2,730,937.747 | 3730.69 | 10.495 | 30.228 | 45.368 | 6.315 | 6.954 | 9.064 |
FF4 | FF5 | FF6 | ||||||
34.263 | 214.228 | 31.932 | 10.336 | 32.989 | 6.436 | 7.278 | 4.138 | 96.579 |
28.979 | 33.535 | 64.008 | 10.044 | 21.962 | 7.183 | 5.43 | 11.311 | 25.654 |
28.316 | 90.202 | 24.116 | 12.933 | 17.517 | 8.518 | 5.944 | 14.772 | 17.937 |
FF7 | FF8 | FF9 | ||||||
13.812 | 18.75 | 45 | 19.445 | 56.283 | 6.472 | 71.68 | 42.175 | 5.351 |
14.589 | 31.509 | 61.746 | 12.511 | 5.913 | 5.948 | 350.506 | 81.694 | 6.706 |
13.892 | 23.394 | 35.287 | 12.746 | 76.687 | 6.408 | 437.834 | 101.935 | 4.782 |
FF10 | FF11 | FF12 | ||||||
99.046 | 2764.726 | 3,635,747.617 | 516.904 | 1584.862 | 7.218 | 36.547 | 19.005 | 5.826 |
362.044 | 2304.978 | 2,772,178.739 | 288,504.969 | 2033.538 | 6.666 | 35.392 | 20.318 | 5.68 |
422.902 | 12,713.805 | 417,848.278 | 122.99 | 3653.969 | 7.253 | 157.38 | 30.79 | 9.615 |
FF13 | FF14 | FF15 | ||||||
32.033 | 95.217 | 31.292 | 19.392 | 13.049 | 6.616 | 60.777 | 16.914 | 4.254 |
30.569 | 59.846 | 25.576 | 29.207 | 10.838 | 5.875 | 551.801 | 11.003 | 3.716 |
26.267 | 476.744 | 25.895 | 26.432 | 9.943 | 6.501 | 22,889.61 | 25.629 | 3.888 |
FF16 | FF17 | FF18 | ||||||
9.299 | 121.47 | 436.187 | 9.408 | 9.609 | 4.044 | 22.689 | 9.609 | 5.961 |
7.392 | 65.903 | 501.895 | 14.065 | 12.293 | 5.383 | 22.764 | 9.395 | 5.686 |
8.202 | 75.451 | 213.183 | 19.014 | 15.709 | 4.661 | 23.048 | 13.137 | 7.263 |
FF19 | FF20 | FF21 | ||||||
8913.456 | 4071.78 | 10,484.77 | 1889.377 | 229.782 | 23.903 | 42.436 | 23.744 | 7.88 |
19,625.522 | 895.949 | 6240.57 | 1965.838 | 320.28 | 15.098 | 22.633 | 15.856 | 6.977 |
4701.204 | 415.075 | 5042.839 | 1485.666 | 1894.301 | 14.203 | 21.931 | 16.185 | 8.274 |
FF22 | FF23 | FF24 | ||||||
6604.527 | 78,888.929 | 108.414 | 30.718 | 14,779.799 | 25,851.422 | 179.526 | 32.61 | 5.494 |
87,029.214 | 86,811.625 | 85.888 | 24.046 | 4073.054 | 28,441.475 | 81.878 | 30.471 | 5.452 |
11,530.769 | 22,689.887 | 37.741 | 31.446 | 1356.76 | 5928.397 | 327.947 | 41.231 | 5.78 |
FF25 | FF26 | FF27 | ||||||
26.312 | 345.196 | 1209.541 | 47.927 | 34.306 | 14.474 | 9.89 | 15.467 | 16.268 |
54.266 | 110.342 | 2756.198 | N/A | 58.453 | 8.885 | 9.27 | 12.178 | 11.348 |
25.589 | 1229.963 | 3058.124 | 129.293 | 64.64 | 13.231 | 9.284 | 14.993 | 28.343 |
Response | Regression Equation |
---|---|
1/Surface Resistance | 0.12132 + 0.00928 Conc._1 + 0.03124 Conc._5 − 0.04052 Conc._10 − 0.02815 Stir Time_20 + 0.00851 Stir Time_40 + 0.01964 Stir Time_60 − 0.08043 Temp._20 + 0.01676 Temp._40 + 0.06367 Temp._60 − 0.00704 Conc.*Stir Time_1 20 + 0.00706 Conc.*Stir Time_1 40 − 0.00002 Conc.*Stir Time_1 60 − 0.01236 Conc.*Stir Time_5 20 − 0.00159 Conc.*Stir Time_5 40 + 0.01395 Conc.*Stir Time_5 60 + 0.01940 Conc.*Stir Time_10 20 − 0.00547 Conc.*Stir Time_10 40 − 0.01393 Conc.*Stir Time_10 60 − 0.01165 Conc.*Temp._1 20 + 0.00286 Conc.*Temp._1 40 + 0.00879 Conc.*Temp._1 60 − 0.01064 Conc.*Temp._5 20 + 0.01985 Conc.*Temp._5 40 − 0.00921 Conc.*Temp._5 60 + 0.02229 Conc.*Temp._10 20 − 0.02271 Conc.*Temp._10 40 + 0.00042 Conc.*Temp._10 60 − 0.00801 Stir Time*Temp._20 20 + 0.00559 Stir Time*Temp._20 40 + 0.00242 Stir Time*Temp._20 60 − 0.01372 Stir Time*Temp._40 20 − 0.02420 Stir Time*Temp._40 40 + 0.03791 Stir Time*Temp._40 60 + 0.02172 Stir Time*Temp._60 20 + 0.01860 Stir Time*Temp._60 40 − 0.04033 Stir Time*Temp._60 60 |
Term | Coef | SE Coef | T-Value | p-Value | VIF |
---|---|---|---|---|---|
Constant | 0.12132 | 0.00434 | 27.94 | 0.000 | |
Conc. | |||||
1 | 0.00928 | 0.00614 | 1.51 | 0.169 | 1.33 |
5 | 0.03124 | 0.00614 | 5.09 | 0.001 | 1.33 |
Stir Time | |||||
20 | −0.02815 | 0.00614 | −4.58 | 0.002 | 1.33 |
40 | 0.00851 | 0.00614 | 1.39 | 0.203 | 1.33 |
Temp. | |||||
20 | −0.08043 | 0.00614 | −13.10 | 0.000 | 1.33 |
40 | 0.01676 | 0.00614 | 2.73 | 0.026 | 1.33 |
Conc.*Stir Time | |||||
1 20 | −0.00704 | 0.00868 | −0.81 | 0.441 | 1.78 |
1 40 | 0.00706 | 0.00868 | 0.81 | 0.440 | 1.78 |
5 20 | −0.01236 | 0.00868 | −1.42 | 0.192 | 1.78 |
5 40 | −0.00159 | 0.00868 | −0.18 | 0.859 | 1.78 |
Conc.*Temp. | |||||
1 20 | −0.01165 | 0.00868 | −1.34 | 0.217 | 1.78 |
1 40 | 0.00286 | 0.00868 | 0.33 | 0.751 | 1.78 |
5 20 | −0.01064 | 0.00868 | −1.23 | 0.255 | 1.78 |
5 40 | 0.01985 | 0.00868 | 2.29 | 0.052 | 1.78 |
Stir Time*Temp. | |||||
20 20 | −0.00801 | 0.00868 | −0.92 | 0.383 | 1.78 |
20 40 | 0.00559 | 0.00868 | 0.64 | 0.538 | 1.78 |
40 20 | −0.01372 | 0.00868 | −1.58 | 0.153 | 1.78 |
40 40 | −0.02420 | 0.00868 | −2.79 | 0.024 | 1.78 |
FF | Conc. (%) | Soak Time (minutes) | Temp. (°C) | Min. Surf. Res. (Ω/square) | Max. Disp. (mm) | Max. Blocking Force (mN) |
---|---|---|---|---|---|---|
1 | 1 | 20 | 20 | 582.52 | 7.71 | 0.052 |
2 | 1 | 20 | 40 | 7.93 | 21.45 | 5.396 |
3 | 1 | 20 | 60 | 6.31 | 14.12 | 1.51 |
4 | 1 | 40 | 20 | 24.12 | 10.34 | 0.895 |
5 | 1 | 40 | 40 | 6.44 | 18.46 | 4.932 |
6 | 1 | 40 | 60 | 4.14 | 19.22 | 0.418 |
7 | 1 | 60 | 20 | 13.81 | 5.13 | 0.6 |
8 | 1 | 60 | 40 | 5.91 | 16.81 | 3.876 |
9 | 1 | 60 | 60 | 4.78 | 12.49 | 3.092 |
10 | 5 | 20 | 20 | 99.05 | 6.83 | 6.277 |
11 | 5 | 20 | 40 | 6.67 | 6.58 | 1.206 |
12 | 5 | 20 | 60 | 5.68 | 12.6 | 7.079 |
13 | 5 | 40 | 20 | 25.58 | 22.16 | 1.377 |
14 | 5 | 40 | 40 | 5.87 | 39.02 | 1.749 |
15 | 5 | 40 | 60 | 3.72 | 31.17 | 1.509 |
16 | 5 | 60 | 20 | 7.39 | 13.06 | 2.545 |
17 | 5 | 60 | 40 | 4.04 | 28.06 | 2.377 |
18 | 5 | 60 | 60 | 5.69 | 24.09 | 1.372 |
19 | 10 | 20 | 20 | 415.08 | 7.26 | 0.313 |
20 | 10 | 20 | 40 | 14.2 | 8.58 | 2.918 |
21 | 10 | 20 | 60 | 6.98 | 59.54 | 3.176 |
22 | 10 | 40 | 20 | 37.74 | 4.32 | 1.618 |
23 | 10 | 40 | 40 | 24.05 | 7.65 | 3.697 |
24 | 10 | 40 | 60 | 5.45 | 20.7 | 3.817 |
25 | 10 | 60 | 20 | 25.59 | 22.74 | 3.389 |
26 | 10 | 60 | 40 | 8.89 | 65.9 | 1.646 |
27 | 10 | 60 | 60 | 9.27 | 48.74 | 3.805 |
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Author (s) | Membrane Size | Reducing Agent | Concentration | Stir Time | Temp., °C |
---|---|---|---|---|---|
Kim et al., 2003 [5] | 5 × 5 cm | NaBH4 1 or LiBH4 2 | 5% | NS 3 | 60 |
Shahinpoor, 2015 [10] | 5 × 5 cm | NaBH4 or LiBH4 | 5% | NS | 40–60 |
Yip et al., 2011 [8] | 50 × 60 mm | NaBH4 | 5 wt% | 6.5 h | 40–60 |
Liu et al., 1992 [11] | 1 in side hexagon | NaBH4 | 0.1 M | 2 h | 50 |
Tian et al., 2021 [12] | 30 × 10 mm | NaBH4 | NS | NS | NS |
Palmre et al., 2014 [13] | 50 × 10 mm | NaBH4 | 0.57 g/L | 2 h | 60 |
Kim et al., 2022 [14] | 0.5 × 2.5 cm | NaBH4 | 0.57 g/L | 2 h | 60 |
Yang et al., 2020 [6] | 10 × 50 mm | NaBH4 | 1% | >30 min | 40–60 |
Oguro et al., 2000 [15] | 30 cm2 | NaBH4 | 5 wt% | 1.5 h | 40–60 |
Xu et al., 2021 [16] | 30 × 29 mm | NaBH4 | 5% | 2 h | NS |
Ma et al., 2020 [17] | 30 × 30 mm | NaBH4 | 5 wt% | 5 h (5 mL added every 30 min 10 times) | 40 |
Rashid et al., 2013 [9] | 15 mm dia. circle | NaBH4 | 10–100 mM | 2 h (replaced every 20 min) | 5, 25, 50 |
Full Factorial Configurations | |||||
---|---|---|---|---|---|
Factor | Unit | Notation | Factor Level | ||
1 | 2 | 3 | |||
Concentration of NaBH4 | % | Conc. | 1 | 5 | 10 |
Stir Time | minutes | ST | 20 | 40 | 60 |
Temperature | °C | Temp. | 20 | 40 | 60 |
FF1 86.7% | FF2 52.5% | FF3 50.6% |
FF4 94.7% | FF5 57.4% | FF6 131.0% |
FF7 54.2% | FF8 108.4% | FF9 122.7% |
FF10 174.6% | FF11 274.4% | FF12 124.9% |
FF13 155.4% | FF14 58.4% | FF15 273.8% |
FF16 110.8% | FF17 47.2% | FF18 53.2% |
FF19 82.1% | FF20 98.0% | FF21 56.9% |
FF22 113.9% | FF23 119.5% | FF24 129.6% |
FF25 115.0% | FF26 80.0% | FF27 39.9% |
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Manaf, E.; Fitzpatrick, D.P.; Higginbotham, C.L.; Lyons, J.G. Optimising Sodium Borohydride Reduction of Platinum onto Nafion-117 in the Electroless Plating of Ionic Polymer–Metal Composites. Actuators 2024, 13, 350. https://doi.org/10.3390/act13090350
Manaf E, Fitzpatrick DP, Higginbotham CL, Lyons JG. Optimising Sodium Borohydride Reduction of Platinum onto Nafion-117 in the Electroless Plating of Ionic Polymer–Metal Composites. Actuators. 2024; 13(9):350. https://doi.org/10.3390/act13090350
Chicago/Turabian StyleManaf, Eyman, Daniel P. Fitzpatrick, Clement L. Higginbotham, and John G. Lyons. 2024. "Optimising Sodium Borohydride Reduction of Platinum onto Nafion-117 in the Electroless Plating of Ionic Polymer–Metal Composites" Actuators 13, no. 9: 350. https://doi.org/10.3390/act13090350