大腔体压机腔体压强28 GPa的标定方法

葛雨非; 由存; 王星淋; 连敏; 赵鑫宇; 丰丙涛; 马孝慈; 陶强; 胡阔; 刘兆东; 周强; 朱品文

doi:10.11858/gywlxb.20230807

大腔体压机腔体压强28 GPa的标定方法

doi: 10.11858/gywlxb.20230807

吉林大学物理学院, 超硬材料国家重点实验室, 综合极端条件高压科学中心, 吉林长春　130012

基金项目: 国家自然科学基金（11974131）；国家重点研发计划项目（2018YFA0703400）；“综合极端条件实验装置”国家重大科技基础设施项目（发改投资〔2017〕1597号）

详细信息

作者简介:
葛雨非（1994－），男，博士，助理研究员，主要从事高温高压超硬/硬质功能材料制备及物性研究. E-mail：yufeige@jlu.edu.cn

通讯作者:
陶　强（1988－），男，博士，副教授，主要从事高温高压合成新结构以及新型超硬材料研究. E-mail：qiangtao@jlu.edu.cn

朱品文（1972－），男，博士，教授，主要从事高温高压下新型多功能超硬材料的制备与物性研究. E-mail：zhupw@jlu.edu.cn

中图分类号: O521.2; O521.3
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出版历程
- 收稿日期: 2023-12-08
- 修回日期: 2023-12-20
- 录用日期: 2024-01-17
- 刊出日期: 2024-06-03

Pressure Calibration Method of 28 GPa for Large-Volume Press

Synergetic Extreme Condition High-Pressure Science Center, State Key Laboratory of Superhard Materials, College of Physics, Jilin University, Changchun 130012, Jilin, China

摘要

摘要: 在大腔体压机中，一般利用压标物质相变时的电阻变化进行腔体压强标定，但目前仍缺少在22.5～34.5 GPa区间的相变压标物质。地球深部矿物50%MgSiO₃-50%Al₂O₃（En₅₀Cor₅₀）在高温高压下转变为钙钛矿结构，且在27 GPa以上钙钛矿结构MgSiO₃中溶解的Al₂O₃含量随压力升高而增加。为此，选取En₅₀Cor₅₀作为大腔体压机中28 GPa的压标物质进行高压腔体压强的间接标定。首先，利用常用压标物质的相变进行腔体压强标定，得到低压区系统油压-腔体压强的校正曲线（6.0～22.5 GPa）；随后，根据低压区校正曲线及前人对En₅₀Cor₅₀的研究结果，估算28 GPa腔体压强对应的系统油压；将En₅₀Cor₅₀在预估油压、2000 K温度条件下保温3～7 h；最后，利用X射线衍射、拉曼光谱、电子探针等手段对En₅₀Cor₅₀进行测试分析。结果表明：在该条件下成功合成了布里奇曼石，且Al₂O₃的溶解度大于13.7%，对照前人的研究结果，确定样品腔体压强约为29 GPa。该方法成功标定了大腔体压机在28 GPa附近的腔体压强，填补了大腔体压机在该压强范围的标定空白。
- 大腔体压机 /
- 压力标定 /
- 28 GPa /
- 高温高压
Abstract: In the large-volume press (LVP), the pressure calibration for the sample chamber is generally carried out by using phase transitions of specific materials with resistance changes. But there are no suitable materials for pressure calibration in the range of 22.5−34.5 GPa. As we know, the mineral 50 mol%MgSiO₃-50 mol%Al₂O₃ (En₅₀Cor₅₀) systems in deep earth undergo structural transition to perovskite phase under high pressure and high temperature (HPHT) conditions. Moreover, the content of Al₂O₃ dissolved in perovskite MgSiO₃ increases gradually with raised pressure above 27 GPa. Therefore, En₅₀Cor₅₀ was selected as the pressure calibration material for further calibrating 28 GPa in the LVP in this study, and this is an indirect pressure calibration method. First, the low-pressure calibration curve (6.0−22.5 GPa) of system oil pressure versus chamber pressure was obtained by using the phase transitions of different pressure calibration materials. Then, based on the low-pressure calibration curve and previous research results En₅₀Cor₅₀, the estimated system oil pressure corresponding to the 28 GPa of chamber pressure is 65 MPa. At the estimated oil pressure, the En₅₀Cor₅₀ samples were heated to 2000 K and maintained for 3−7 h. The results of X-ray diffraction, Raman, and electron probe measurements indicate that bridgmanite has been successfully synthesized, and the dissolved Al₂O₃ molar fraction is greater than 13.7%. According to the previous research results, the corresponding sample chamber pressure is about 29 GPa. This method successfully calibrated the sample chamber pressure around 28 GPa in the LVP, which fill in the blanks for calibrating this pressure range.
- large-volume press /
- pressure calibration /
- 28 GPa /
- high pressure and high temperature

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图 1 3000 t Kawai型LVP

Figure 1. 3000 t Kawai-type LVP

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图 2 压标物质ZnTe、ZnS、GaAs和GaP的电阻-油压曲线

Figure 2. Electrical resistance-oil pressure curves of pressure calibration materials: ZnTe, ZnS, GaAs and GaP

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图 3 矿物标压实验样品的拉曼光谱(a)和XRD谱(b)

Figure 3. Raman spectra (a) and XRD pattern (b) of pressure calibration mineral sample

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图 4 样品的EDS元素含量分析：(a) 扫描图像，(b) 元素能谱

Figure 4. EDS element content analysis at sample selection point: (a) SEM image; (b) elemental spectrum

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图 5 BSE图像：(a) 保温3 h样品, (b) 保温7 h样品

Figure 5. BSE images: (a) sample held for 3 h; (b) sample held for 7 h

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图 6 2000 K下MgSiO₃-Al₂O₃体系中各相的关系^[12–13]

Figure 6. Phase relations in the MgSiO₃-Al₂O₃ system at 2000 K^[12–13]

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图 7 腔体压强标定曲线

Figure 7. High pressure chamber pressure calibration curve

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表 1 压标材料及其相变压力

Table 1. Pressure calibration materials and their phase transition pressure

Pressure calibration material	Phase transition pressure/GPa
Bi (Ⅰ-Ⅱ)	2.6
Bi (Ⅱ-Ⅲ)	2.7
Tl (Ⅱ-Ⅲ)	3.7
Ba	5.5
ZnTe (Ⅰ-Ⅱ)	6.6
Bi (Ⅲ-Ⅳ)	7.7
ZnTe (Ⅱ-Ⅲ)	8.9−9.5
ZnTe (Ⅲ-Ⅳ)	11.5−13.0
ZnS	15.6
GaAs	18.9
GaP	22.5
Zr	34.5

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表 2 EDS选点测试得到的En₅₀Cor₅₀样品内各成分的摩尔分数

Table 2. Molar fraction of each component obtained by EDS measurement in En₅₀Cor₅₀ sample

Element	Molar fraction/%
Mg	21.67
Si	23.13
Al	7.71
MgO	35.94
SiO₂	49.49
Al₂O₃	14.58

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表 3 EMPA测试的样品内布里奇曼石中各组分的摩尔分数

Table 3. Molar fraction of each component obtained by EMPA in bridgmanite of sample

Composition	Molar fraction/%
MgO	34.67
SiO₂	51.61
Al₂O₃	13.74

下载: 导出CSV

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