Walker Type Multi-Anvil Apparatus and Its Applications in Geosciences
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摘要: 高温高压实验是除地球物理和地球化学方法之外, 研究地球深部物质和性质的重要手段之一.多面砧压机是广泛使用的高温高压实验设备, 主要用来研究上地幔温压范围内的实验岩石学和矿物相变动力学等问题.主要介绍中国地质大学(武汉)地球深部研究实验室新引进的Walker型28 GPa多面砧压机的原理和结构、压力标定方法和常用的压力标定材料, 并根据金属铋在2.55和7.7 GPa(25 ℃)的结构相变, 以及石英在3.2 GPa、1 200 ℃向柯石英的转变对多面砧压机18/12装置(八面体传压介质边长/碳化钨截角边长)进行了压力标定, 该装置可实现的最高压力和温度约为8 GPa和2 000 ℃.最后还探讨了高温高压实验在地球科学中的应用.Abstract: High temperature and high pressure (HTHP) experiments is an important approach to study the nature of earth's deep interior. Multi-anvil press is widely used investigating phase transitions and mineral physics under the upper mantle conditions. The pressure calibration of the 18/12 (Octahedron Edge length/Truncated Edge Length) sample assembly for the multi-anvil press installed in China university of geosciences are summarized in this paper. Pressures for the 18/12 assembly were calibrated using phase transitions in bismuth at 2.55 GPa (Ⅰ-Ⅱ), and 7.7 GPa (Ⅲ-Ⅴ) at room temperature, and using quartz /coesite phase transition at 3.2 GPa and 1 200 ℃. This assembly can cover a pressure and temperature range up to 8 GPa and 2 000 ℃. Finally, the applications of HT-HP experiment in geosciences are also briefly discussed.
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图 1 1 000吨多面砧压机walker型高压腔示意
Fig. 1. Cross section of the pressure chamber of 1 000-ton multi-anvil press
图 2 二级压砧组装示意(a)与18/12装置样品组合示意(b)
Fig. 2. The schematic diagram of tungsten carbide assembly (a) and cross section of 18/12 heating assembly
图 3 多面砧压机18/12装置室温压力标定样品组装示意
Fig. 3. Cross section of the 18/12 sample assembly for pressure calibration at room temperature
图 4 室温下压力标定过程中Bi电阻变化曲线
在加载过程中Bi的电阻逐渐减小且在A、B位置有电阻的突变，这是分别是由Bi(Ⅰ-Ⅱ)和Bi(Ⅲ-Ⅴ)相变引起的；卸载过程中在A1点出现了电阻突变，该处电阻突变是由Bi(Ⅱ-Ⅰ)相变造成，由于摩擦力的影响导致同一相变对应的负载在加载和卸载过程中不同
Fig. 4. Typical behavior of the Bi Ⅰ-Ⅱ and Bi Ⅲ-Ⅴ transitions at room temperature. The resistance mutations reflect the structure transitions points of Bi
图 5 高温压力标定实验产物(石英、柯石英)拉曼光谱图
Fig. 5. Raman spectrum of experimental results of pressure calibration at high temperature
图 6 多面砧压机18/12装置压力标定曲线
Fig. 6. Pressure calibration curve of 18/12 assembly obtained at room temperature and high temperature
图 7 橄榄石高压相变和地幔地震波不连续面关系
(a)图中PREM和AK135为地震波速度剖面，pyrolite和piclogite为两种不同的理论地幔岩石成分(据Irifune et al., 2008).橄榄石高压相图据Fei and Bertka(1999)
Fig. 7. High pressure phase diagram of olivine and its bearing in the origin of seismic discontinuities in the mantle
表 1 室温压力标定常用材料及相变类型和压力(Ito, 2007)
Table 1. Some phase transitions as pressure calibrants at room temperature
压力(GPa) 温度(℃) 材料 相变类型 标定方法 文献 2.55 25 Bi Ⅰ → Ⅱ 电阻变化 Bean et al., 1986 7.7 25 Bi Ⅲ → Ⅴ 电阻变化 Bean et al., 1986 15.6 25 ZnS 半导体→导体 电阻变化 Block, 1978 18.3 25 GaAs 半导体→导体 电阻变化 Suzuki et al., 1981 22 25 GaP 半导体→导体 电阻变化 Piermarini and Block, 1975 
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表 2 高温压力标定常用材料及其相变类型和压力(Ito, 2007)
Table 2. Some phase transitions as pressure calibrants at high temperature
压力(GPa) 温度(℃) 材料 相变类型 标定方法 文献 3.2 1 200 SiO2 石英→柯石英 淬火/ 可逆 Bose and Ganguly, 1995 4.8~5.8 800~1 200 Fe2SiO4 α→γ 原位X射线衍射 Yagi et al., 1987 6.2~5.9 900~1 200 CaGeO3 石榴石→钙钛矿 原位X射线衍射 Susaki et al., 1985 8.7~10.1 1 300~1 530 SiO2 柯石英-斯石英 原位X射线衍射 Zhang et al., 1996 12.2~14.3 1 000~1 400 Mg2SiO4 α→β 原位X射线衍射 Morishima et al., 1994 14.2~15.5 1 300~1 600 Mg2SiO4 α→β 原位X射线衍射 Katsura et al., 2004 16.5 1 400 MgSiO3 辉石→β+斯石英 淬火 Gasparik, 1989 15.7→17.4 800~1 000 Mg2SiO4 β→γ 原位X射线衍射 Suzuki et al., 2000 19→20.8 1 200~1 600 Mg2SiO4 β→γ 淬火 Katsura and Ito, 1989 24.8→23.1 1 000~1 600 Mg2SiO4 γ→钙钛矿+方镁石 淬火 Ito and Takahashi, 1989
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表 3 金属铋结构相变引起的体积和电阻的相对改变量及对应的压力(Yoneda and Endo, 1980)
Table 3. Relative changes in volume and resistance of bismuth caused by structure transitions
Bi Ⅰ-Ⅱ Bi Ⅱ-Ⅲ Bi Ⅲ-Ⅴ 体积相对改变量(ΔV/V) 1 0.69% 0.32% 电阻相对改变量(ΔR/R) 1 0.77% 0.23% 对应压力(GPa) 2.55 2.7 7.7
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表 4 高温压力标定实验条件和结果
Table 4. Experimental conditions and results of high temperature pressure calibration
实验编号 负载(psi) 温度(℃) 时间(h) 起始物质 产物 R004 1 400 1 200 1.5 SiO2 柯石英 R006 1 200 1 200 1.5 SiO2 石英 R007 1 300 1 200 1.5 SiO2 柯石英 注：1psi=6.895 kPa.
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