Pressure and Temperature Calibrations of End-Loaded Piston-Cylinder 19 mm Outer Diameter Sample Assembly
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摘要: 在高温高压实验中，样品所处位置的压强、温度及样品腔温度分布情况对实验结果分析十分重要，因此使用高温高压实验装置前需对所用组装进行压强和温度标定。针对双向活塞圆筒装置19 mm外径样品组装，进行了压强与温度标定。利用氯化钠（NaCl）在高压下的熔化曲线对压强进行标定，当下油缸油压出现大幅度下降时，样品腔内的NaCl发生熔化，将此时热电偶测量的温度与文献报道的NaCl在高压下的熔化曲线进行比较，确定样品腔内的实际压强。压强标定结果显示，实际压强与目标压强满足线性关系。采用双热电偶法对19 mm外径样品组装样品腔的中部和上部进行测温，发现样品腔中心温度高于样品腔上部温度，温度梯度随温度升高而增大，随压强升高而减小。在二次加压升温时，样品腔内的温度梯度高于第一次加压升温实验测量结果。所得压强和温度标定结果对今后使用19 mm外径样品组装开展高温高压实验研究具有参考价值和指导意义。Abstract: In the high-temperature and high-pressure experiments, it is essential to know the pressure and temperature of sample as well as the temperature distribution inside sample chamber. Therefore, it is necessary to calibrate the pressure and temperature of the experimental assembly before using the high-temperature and high-pressure experimental device. Here we carried out the pressure and temperature calibrations experiments on 19 mm outer diameter sample assembly of the end-loaded piston-cylinder apparatus. We calibrated the pressure of sample chamber by using the melting curve of sodium chloride (NaCl) under high pressure. When the oil pressure of the oil cylinder drops significantly, the NaCl in the sample chamber melts; according to the temperature measured by the thermocouple at this time and the comparison of the melting curve of NaCl under high pressure published by the predecessors, the real pressure in the sample chamber was determined. The pressure calibration results show that there is a linear relationship between the real pressure and the nominal pressure. The double thermocouple method was used to measure the temperature in the center and upper part of the 19 mm outer diameter sample assembly chamber. It was found that the temperature in the center of the sample chamber was higher than the temperature in the upper part of the sample chamber. In addition, the temperature gradient in the sample chamber increases with increasing temperature and decreases with increasing pressure. The temperature gradient in the sample chamber during the second stage pressurization and heating is higher than the temperature gradient in the sample chamber of the first stage pressurization and heating experiment. The pressure and temperature calibration results obtained in this study are of reference value and guiding significance for future high-temperature and high-pressure experimental study using 19 mm outer diameter sample assembly.
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Key words:
- end-loaded piston-cylinder /
- pressure /
- temperature /
- calibration
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图 1 19 mm外径样品组装的压强标定(a) 和温度标定(b) 的结构平面图
Figure 1. Schematic cross sections of 19 mm outer diameter sample assembly for pressure (a) and temperature (b) calibrations
图 2 下油缸油压（pL）与实测温度（T）的关系
Figure 2. Relationship between oil pressure of lower cylinder (pL) and measured temperature (T)
图 4 实际压强（pR）与目标压强（pN）的关系
Figure 4. Relationship between the real pressure (pR) and the nominal pressure (pN)
图 5 （a）样品腔上部温度（T1）和样品腔中心温度（T2）；（b）样品腔中心与上部的温度差值（ΔT）（首次升压至目标压强的温度标定结果）
Figure 5. (a) Temperature above the sample chamber (T1) and temperature in the center of the sample chamber (T2); (b) temperature difference between the center and the upper part of the sample chamber (ΔT) (temperature calibration results of the first stage to the nominal pressure)
图 6 样品腔中心与上部的温度差值（ΔT）
Figure 6. Temperature difference between the center andthe upper part of the sample chamber (ΔT)
表 1 压强标定实验方案
Table 1. Pressure calibration experiment scheme
No. pN/GPa pL/psi pU/psi TN/℃ t/min P1 1.5 1 692 4 078 1 200 40 P2 1.2 1 354 3 262 1 100 40 P3 0.9 1 015 2 447 1 050 40 
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表 2 温度标定实验方案
Table 2. Temperature calibration experiment scheme
pN/GPa Temperature/℃ First program Second program Third program Fourth program Fifth program Sixth program 1.5 200 400 600 800 1 000 1 200 1.2 200 400 600 800 1 000 1 200 0.9 200 400 600 800 1 000 1 200
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