Oxygen Measurement in Cuprate Superconductors Using the Dissolved Oxygen/Chlorine Method
Abstract
:1. Introduction
Type | Method | Weight | Error | Time | Merit | Demerit |
---|---|---|---|---|---|---|
Physical analysis | Thermogravimetric analysis (TGA) [9] | 0.1 mg | 0.1% | 1 h | High accuracy | Cannot ascertain the precise oxygen content. |
X-ray Photoelectron Spectroscopy (XPS) [10] | 1 μg | >10% | 1 h | The depth profile can be determined. | Sensitive to the surface Lacks precision | |
Auger Electron Spectroscopy (AES) [10] | 1 μg | ~10% | 1 h | The depth profile can be determined. | Sensitive to the surface Lacks precision | |
Oxygen Analyzer [11] | 1 g | ~10% | 10 min | Simple measuring | Requires a large sample Limited accuracy | |
Chemical analysis | Coulometric [12] | 50 mg | 0.1% | 1 h | Minor error Automatic measurement | Long measurement time |
Iodometric [13] | 50 mg | 0.1% | 1 h | Simple measuring | Long measurement time |
2. Experimental
2.1. Preparation
2.2. XRD
2.3. Iodometric Titration Method
2.4. Dissolved Oxygen Method
m(CuO1+z) = w(CuO1+z)/M(CuO1+z) mO2 = Δc V/MO2 1:z/2 = m(CuO1+z):mO2 = w(CuO1+z)/M(CuO1+z):Δc V/MO2 Δc V/MO2 = (z/2) × w(CuO1+z)/M(CuO1+z) |
2.5. DO Method with Differential Equation Correction
2.6. DO/Cl Method with DE Correction
2.7. Effect of Different Acidic Solutions in the DO/Cl Method with DE Correction
3. Results and Discussion
3.1. XRD Analysis
3.2. Iodometric Titration Method Results as a Standard
3.3. DO Method Analysis
3.4. DO Method with DE Correction
3.5. Comparison of DO Method with DE Correction and Iodometric Titration Method for Oxygen Content in Bi2Sr2−xLaxCuOy
3.6. Comparison of DO/Cl Method with DE Correction and Iodometric Titration Method for Oxygen Content in Bi2Sr2−xLaxCuOy
3.7. Effect of Acidic Solutions on DO/Cl Method with DE Correction
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Target | Cu |
Voltage | 40 kV |
Current | 20 mA |
Scan axis | 2θ/θ |
Sampling angle | 0.02° |
Scan speed | 5°/min |
Scanning range | 3°~60° |
Cumulative number | 1 time |
Divergence slit width | 1/2° |
Scattering slit width | 8.0 mm |
Receiving slit width | Open |
La Content (x) | Iodometric | |
---|---|---|
Cu Valance (v) | Oxygen Content (y) | |
x = 0 | 2.383 | 6.191 |
x = 0.2 | 2.459 | 6.330 |
x = 0.4 | 2.466 | 6.433 |
x = 0.6 | 2.460 | 6.530 |
x = 1 | 2.331 | 6.666 |
La Content (x) | Iodometric | DO Method | DO Method with DE Correction | DO/Cl Method with DE Correction | ||||
---|---|---|---|---|---|---|---|---|
Cu Valance (v) | Oxygen Content (y) | Cu Valance (v) | Oxygen Content (y) | Cu Valance (v) | Oxygen Content (y) | Cu Valance (v) | Oxygen Content (y) | |
x = 0 | 2.383 | 6.191 | 2.056 | 6.028 | 2.101 | 6.050 | 2.387 | 6.193 |
x = 0.2 | 2.459 | 6.330 | 2.070 | 6.135 | 2.162 | 6.181 | 2.451 | 6.325 |
x = 0.4 | 2.466 | 6.433 | 2.038 | 6.219 | 2.190 | 6.295 | 2.469 | 6.434 |
x = 0.6 | 2.460 | 6.530 | 2.020 | 6.310 | 2.142 | 6.371 | 2.444 | 6.522 |
x = 1 | 2.331 | 6.666 | 2.010 | 6.505 | 2.017 | 6.509 | 2.329 | 6.665 |
La Content (x) | Iodometric | DO/Cl Method (in HCl) | DO/Cl Method (in H2SO4) | DO/Cl Method (in HNO3) | ||||
---|---|---|---|---|---|---|---|---|
Cu Valance (v) | Oxygen Content (y) | Cu Valance (v) | Oxygen Content (y) | Cu Valance (v) | Oxygen Content (y) | Cu Valance (v) | Oxygen Content (y) | |
x = 0 | 2.383 | 6.191 | 2.387 | 6.193 | 2.104 | 6.052 | 2.061 | 6.031 |
x = 0.2 | 2.459 | 6.330 | 2.451 | 6.325 | 2.106 | 6.153 | 2.051 | 6.125 |
x = 0.4 | 2.466 | 6.433 | 2.469 | 6.434 | 2.109 | 6.254 | 2.046 | 6.223 |
x = 0.6 | 2.460 | 6.530 | 2.444 | 6.522 | 2.102 | 6.351 | 2.056 | 6.328 |
x = 1 | 2.331 | 6.666 | 2.329 | 6.665 | 2.036 | 6.518 | 2.032 | 6.516 |
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Wei, Y.; Yan, C.; Kambe, S. Oxygen Measurement in Cuprate Superconductors Using the Dissolved Oxygen/Chlorine Method. Technologies 2024, 12, 115. https://doi.org/10.3390/technologies12070115
Wei Y, Yan C, Kambe S. Oxygen Measurement in Cuprate Superconductors Using the Dissolved Oxygen/Chlorine Method. Technologies. 2024; 12(7):115. https://doi.org/10.3390/technologies12070115
Chicago/Turabian StyleWei, Yuliang, Chengcheng Yan, and Shiro Kambe. 2024. "Oxygen Measurement in Cuprate Superconductors Using the Dissolved Oxygen/Chlorine Method" Technologies 12, no. 7: 115. https://doi.org/10.3390/technologies12070115