一种适用于极端高温条件的六面顶压机实验组装

何强; 唐俊杰; 王霏; 刘曦

doi:10.11858/gywlxb.2014.02.003

一种适用于极端高温条件的六面顶压机实验组装

doi: 10.11858/gywlxb.2014.02.003

北京大学地球与空间科学学院，北京 100871

基金项目: 国家自然科学基金(41273072)

详细信息

作者简介:
何强(1986—), 男，博士研究生，主要从事高温高压地球化学实验研究.E-mail:hq_stephen0530@163.com

中图分类号: O521.3
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出版历程
- 收稿日期: 2013-04-16
- 修回日期: 2013-06-23

High Temperature Stable Assembly Designed for Cubic Press

School of Earth and Space Sciences, Peking University, Beijing 100871, China

摘要

摘要: 参考活塞-圆筒高压设备常用的实验组装中热电偶的布局方式，设计了一种适用于极端高温条件的六面顶压机实验组装。在新的实验组装中，热电偶不再横穿石墨加热炉，而是在石墨炉中纵向分布，从石墨炉顶端横向引出。与传统的六面顶压机实验组装相比，这种新组装具有更强的高温稳定性。测试表明：在5 GPa压力下，1 600 ℃时实验组装的稳定性能够保持48 h以上，1 800 ℃时能够保持约30 h，2 000 ℃时能够保持约10 h。温度梯度测试表明，当组装的中心温度为1 454 ℃时，在组装中央4 mm的范围内平均温度梯度仅有27 ℃/mm，低于中心温度的2%。较长的保温时间以及低温度梯度能进一步提高六面顶压机在地球科学研究领域中的应用。
- 六面顶压机 /
- 实验组装设计 /
- 高温稳定性 /
- 热电偶布局
Abstract: Changing the distribution of the thermal couple, a new experimental assembly, which is stable at extremely high temperatures, has been developed for the cubic press.Test experiments showed that at 5 GPa, this new experimental assembly can be stable at 1 600, 1 800 and 2 000 ℃ for more than 48 hours, about 30 h and about 10 h, respectively.Additionally, the temperature gradient in the new experimental assembly is very low:at 1 454 ℃, it is about 27 ℃/mm in the 4 mm long central part of the graphite heater.Long stable duration at extremely high temperatures and low temperature gradient make this new experimetal assembly suitable for the high-pressure experimentation in Geosciences.
- cubic press /
- experimental assembly design /
- high temperature stability /
- thermal couple distribution

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图 1 (a) 六面顶常用实验组装示意图；(b)六面顶新组装示意图

Figure 1. (a) Conventional experimental assembly used on the cubic press; (b) New experimental assembly developed and tested

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图 2 常用组装在不同压力下的温度-功率对应关系

Figure 2. Relation between T and heat power at different pressures for the conventional experimental assembly

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图 3 压力标定结果

Figure 3. Pressure calibrations for the conventional experimental cell and new experimental cell

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图 4 40 MPa油压(5 GPa)下新实验组装在不同温度时的稳定性

Figure 4. Stability of the new experimental assembly at 40 MPa oil pressure (5 GPa) and at different temperatures

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图 5 温度梯度实验中热电偶组装示意图

Figure 5. Thermal couples (T/C-1 and T/C-2) used to measure the temperature gradient in the middle part of the new experimental cell

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图 6 新实验组装在不同压力下的温度梯度(T₂表示石墨炉中心的温度)

Figure 6. Temperature gradient for the middle part of the new experimental assembly at different pressures(T₂ refers to the temperature at the geometric center of the graphite heater)

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表 1 不同温度-压力条件下新实验组装的温度梯度

Table 1. Temperature gradient at different p-T conditions for the new experimental assembly

T₁/(℃)	3 GPa		4 GPa
T₁/(℃)	T₂/(℃)	Temperature gradient/(℃/mm)	T₂/(℃)	Temperature gradient/(℃/mm)
400	412	6.0	415	7.5
600	616	8.0	618	9.0
800	823	11.5	825	12.5
1 000	1 032	16.0	1 032	16.0
1 200	1 244	22.0	1 242	21.0
1 400	1 454	27.0	1 453	26.5
Note:T₂ refers to temperature at the center of the graphite heater while T₁ refers to the temperature 2 mm away from the center.

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表 2 不同材料、尺寸加热器的温度梯度

Table 2. Temperature gradient for heaters of different materials and sizes

Heater	Length/(mm)	OD/(mm)	ID/(mm)	Central thick portion/(mm)	Temperature gradient/(℃/mm)	Data source
Graphite	13.7	3.0	2.6	-	100	Ref.[23]
Graphite	13.7	3.0	2.6	2.3/4.2	-25	Ref.[23]
LaCrO₃	7.2	2.3	1.5	-	200	Ref.[23]
LaCrO₃	7.2	2.0	1.4	-	200	Ref.[23]
Graphite	24.5	5.0	3.5	-	27	This study
Note:(1) Length of the heater in Ref.[23]is calculated based on the size of the octahedron and then subtracted by 1 mm, which is estimated, from the figure given in the reference, for the thickness of the graphite lid; (2) OD:Outer diameter; (3) ID:Inner diameter; (4) Central thick portion is equal to 2.3/4.2 means that ID of the thick portion of the stepped heater is 2.3 mm while the length of this portion is 4.2 mm.

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