High-Temperature Oxidation of Heavy Boron-Doped Diamond Electrodes: Microstructural and Electrochemical Performance Modification
Abstract
:1. Introduction
2. Materials and Methods
3. Results and Discussion
3.1. Electron Transfer through High-Temperature-Treated BDD Interface
3.2. High-Temperature Oxidation Influence on BDD Physico-Chemical Properties
3.3. Reversibility of the High-Temperature BDD Surface Oxidation
4. Conclusions
- ✓
- hindered charge transfer kinetics, demonstrated by the decrease in peak current on CV scans when comparing to the as-prepared BDDs, a feature observed even at the shortest treatment duration;
- ✓
- the modification of BDD microstructure and the appearance of small and shallow etch pits throughout the diamond surface, damaging diamond structure at prolonged treatments;
- ✓
- the disappearance of the spectral component, located at approximately 283.2 eV, and originating from surface sp2-carbon in XPS;
- ✓
- the bimodal character of BDD conductivity observed by SRRM with a gradual increase in the share of low conductivity areas, dependent on the BDD crystallographic structure.
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Parameter | Untreated | High-Temperature Treatment | |||
---|---|---|---|---|---|
3 min | 10 min | 30 min | 90 min | ||
iA/mA | 0.44 | 0.29 | 0.16 | 0.20 | 0.16 |
iA/iC/- | 0.97 | 1.14 | 1.33 | 1.45 | 1.43 |
ΔE/V | 0.35 | 0.31 | 0.39 | 1.04 | 0.72 |
k0/cm/s | 3.58 × 10−3 | 1.96 × 10−3 | 1.94 × 10−3 | 1.78 × 10−3 | 1.91 × 10−3 |
Parameter | Untreated | High-Temperature Treatment | |||
---|---|---|---|---|---|
3 min | 10 min | 30 min | 90 min | ||
Mean Sa/nm | 55.1374 | 55.860 | 51.4811 | 54.4982 | 36.3451 |
Mean Rs/Ω | 0.1505 | 0.7993 | 1.6417 | 13.0889 | 16.1148 |
Chemical State | BE/eV | Untreated | High-Temperature Treatment | ||||
---|---|---|---|---|---|---|---|
3 min | 10 min | 30 min | 90 min | ||||
C1s | C-C sp2 | 283.2 | 2.1 | 2.4 | 2.9 | 1.8 | 1.5 |
C-C(1) | 284.2 | 83.5 | 23.1 | 23.7 | 24.4 | 25.3 | |
C-C(2) | 284.9 | 8.7 | 49.2 | 30.3 | 23.9 | 20.8 | |
C-OH | 285.6 | 4.8 | 15.8 | 31.6 | 35.6 | 36.8 | |
>C=O | 287.0 | 0.6 | 7.4 | 6.6 | 6.4 | 6.5 | |
COOH | 288.7 | 0.3 | 2.1 | 4.9 | 7.9 | 9.1 |
Parameter | Untreated | High-Temperature Treated and Rehydrogenated | |||
---|---|---|---|---|---|
3 min | 10 min | 30 min | 90 min | ||
iA/mA | 0.44 | 0.39 | 0.26 | 0.29 | 0.24 |
iA/iC/- | 0.97 | 1.00 | 1.19 | 0.88 | 1.06 |
ΔE/V | 0.35 | 0.22 | 0.50 | 0.55 | 0.20 |
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Ryl, J.; Cieslik, M.; Zielinski, A.; Ficek, M.; Dec, B.; Darowicki, K.; Bogdanowicz, R. High-Temperature Oxidation of Heavy Boron-Doped Diamond Electrodes: Microstructural and Electrochemical Performance Modification. Materials 2020, 13, 964. https://doi.org/10.3390/ma13040964
Ryl J, Cieslik M, Zielinski A, Ficek M, Dec B, Darowicki K, Bogdanowicz R. High-Temperature Oxidation of Heavy Boron-Doped Diamond Electrodes: Microstructural and Electrochemical Performance Modification. Materials. 2020; 13(4):964. https://doi.org/10.3390/ma13040964
Chicago/Turabian StyleRyl, Jacek, Mateusz Cieslik, Artur Zielinski, Mateusz Ficek, Bartlomiej Dec, Kazimierz Darowicki, and Robert Bogdanowicz. 2020. "High-Temperature Oxidation of Heavy Boron-Doped Diamond Electrodes: Microstructural and Electrochemical Performance Modification" Materials 13, no. 4: 964. https://doi.org/10.3390/ma13040964