论文部分内容阅读
我们在直径20mm的活塞圆筒容器上建立了高压差热分析方法,经过反复的实验和改进,这一方法已达到很高的灵敏度及测量精度。其要点如下:样品盒用热电偶材料制成,电偶的一个结点就焊在样品盒中心,提高了热信号探测效率;样品量由几百毫克减少到几十毫克,样品在压腔中所占轴向空间减少到约0.5mm,使样品处于等温区内,DTA测量基线变得基本平直;采用平板热电偶,可以充分接收相变潜热,差热信号明显增强。 在高压相图工作中,应用这种方法我们已做了许多成功的实验。
We have established a high-pressure differential thermal analysis method on a piston cylinder of 20mm in diameter. After repeated experiments and improvements, this method has achieved high sensitivity and measurement accuracy. The main points are as follows: The sample box is made of thermocouple material, a junction of the galvanic couple is welded to the center of the sample box to improve the detection efficiency of the heat signal; the sample size is reduced from several hundred milligrams to several ten milligrams; The occupied axial space is reduced to about 0.5mm, so that the sample is in the isothermal zone, and the baseline of the DTA measurement becomes substantially flat. With the flat thermocouple, the latent heat of phase transformation can be fully received, and the differential thermal signal is obviously enhanced. In the work of high-pressure phase diagram, we have done a lot of successful experiments applying this method.