碳酸铅在不同传压介质下的高压拉曼研究

阿卜力孜 • 麦提图尔荪; 艾尼瓦尔 • 吾术尔; 谢翠焕; 亓文明

doi:10.11858/gywlxb.20210813

碳酸铅在不同传压介质下的高压拉曼研究

doi: 10.11858/gywlxb.20210813

新疆大学物理科学与技术学院，新疆乌鲁木齐　830046

基金项目: 教育部留学回国人员科研启动基金（60594）

详细信息

作者简介:
阿卜力孜 • 麦提图尔荪（1993－），男，硕士研究生，主要从事矿物质在高压下的稳定性研究.E-mail：1715038477@qq.com

通讯作者:
艾尼瓦尔 • 吾术尔（1974－），男，博士，主要从事高压高温材料制备以及高温高压下地球物质特性研究. E-mail：anwar.hushur@outlook.com

中图分类号: O521.2
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出版历程
- 收稿日期: 2021-06-15
- 修回日期: 2021-07-06

High Pressure Raman Spectroscopic Study of PbCO₃ in Different Pressure Transmitting Medium

School of Physical Science and Technology, Xinjiang University, Urumqi 830046, Xinjiang, China

摘要

摘要: 为研究PbCO₃在高压下的稳定性，利用金刚石对顶砧技术，采用NaCl固体、甲醇-乙醇-水混合液体（16∶3∶1）和甲醇-乙醇混合液体（4∶1）做传压介质，开展了PbCO₃的高压拉曼实验，最高压强分别达到24.5、25.0和67.0 GPa。研究发现，PbCO₃在10、15和30 GPa左右发生相变，在静水压强条件下 ${\rm{CO}}_3^{2-}$ 基团的ν₂-外弯曲振动模出现了软化现象。通过对比得到不同传压介质中PbCO₃的Grüneisen参数γ，发现相变机制略有不同，并且压强对晶格振动的影响比 ${\rm{CO}}_3^{2-}$ 基团的影响大，这是由Pb²⁺―O键的键长较大造成的。在所研究的压强范围内，PbCO₃没有发生分解或非晶化，30.0 GPa以上出现的PbCO₃-Ⅳ相直至67.0 GPa都很稳定。
- PbCO₃ /
- 拉曼光谱 /
- 传压介质 /
- 高压 /
- 相变
Abstract: Using diamond anvil cell (DAC) technique and Raman spectroscopy, we have studied the stability of PbCO₃ at high pressure. Solid NaCl, mixture of methanol-ethanol-water (16∶3∶1) and methanol-ethanol (4∶1) were used as pressure transmitting medium. The highest pressure in this study reached up to 24.5, 25.0 and 67.0 GPa, respectively. It is found that PbCO₃ undergoes three phase transitions at around 10, 15 and 30 GPa, respectively. In addition, the softening of the out of bending vibration mode belonging to ${\rm{CO}}_3^{2-}$ group was observed. By comparison with the Grüneisen parameters ( $\gamma$ ) of PbCO₃ in different pressure-transfer media, the phase transition mechanism is slightly different, and the influence of pressure on lattice vibration is greater than that of ${\rm{CO}}_3^{2-}$ group, which is attributed to the larger distance of the Pb²⁺—O bond. PbCO₃ did not decompose or amorphized in the pressure range of 67.0 GPa, the highest pressure reached in this study. The observed PbCO₃-Ⅳ phase above 30.0 GPa is stable up to 67.0 GPa.
- PbCO₃ /
- Raman spectroscopy /
- pressure-transmitting medium /
- high pressure /
- phase transformation

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图 1 PbCO₃样品的XRD谱与标准谱对比

Figure 1. Comparison of the XRD spectra of PbCO₃with the standard spectra

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图 2 采用NaCl固体传压介质时的PbCO₃高压拉曼光谱

Figure 2. High pressure Raman spectra of PbCO₃ in solid NaCl pressure transmitting medium

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图 3 采用NaCl固体做传压介质时PbCO₃的拉曼峰位移与压强之间的关系（ν₁、ν₂和ν₄分别对应对称拉伸振动模、外弯曲振动模和内弯曲振动模）

Figure 3. Pressure-induced mode shifts of PbCO₃ undergoes the solid NaCl pressure transmitting medium (ν₁, ν₂ and ν₄ are symmetric stretching vibration, out-of-plane bending vibration, and in-plane bending vibration, respectively.)

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图 4 采用甲醇-乙醇-水混合液体作为传压介质时的PbCO₃高压拉曼光谱

Figure 4. High pressure Raman spectra of PbCO₃ in mixture of MEW pressure transmitting medium

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图 5 采用甲醇-乙醇-水混合液体作为传压介质时PbCO₃的拉曼峰位移与压强之间的关系（ν₁、ν₂和ν₄分别对应对称拉伸振动模、外弯曲振动模和内弯曲振动模）

Figure 5. Pressure-induced mode shifts of PbCO₃ undergoes the mixture of MEW pressure transmitting medium (ν₁, ν₂ and ν₄ are symmetric stretching vibration, out-of-plane bending vibrations, and in-plane bending vibration, respectively.)

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图 6 采用甲醇-乙醇混合液体做传压介质时PbCO₃的高压拉曼光谱

Figure 6. High pressure Raman spectra of PbCO₃ in mixture of methanol-ethanol pressure transmitting medium

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图 7 采用甲醇-乙醇混合液体做传压介质时PbCO₃的拉曼峰位移与压强之间的关系（ν₁、ν₂、ν₄分别为对称拉伸振动模、外弯曲振动模和内弯曲振动模）

Figure 7. Pressure-induced mode shifts undergoes the mixture of methanol-ethanol pressure transmitting medium (ν₁, ν₂ and ν₄ are symmetric stretching vibration, out-of-plane bending vibration, and in-plane bending vibration, respectively.)

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表 1 采用NaCl固体做传压介质时PbCO₃-Ⅰ相的拉曼峰对应的位置、dν/dp和 ${{\gamma}}$

Table 1. Raman modes and the values of dν/dp and mode Grüneisen parameters ( ${{\gamma}}$ ) for PbCO₃-Ⅰ phase in solid NaCl pressure transmitting medium

${\nu }{_{\mathrm{i}0}}$ /cm⁻¹	Pressure range/GPa	$\dfrac{\mathrm{d}\nu }{\mathrm{d}p} \Big/({\rm{cm} }{^{-1} }\cdot {\rm{GPa} }{^{-1} })$	$\gamma$
1095.81	0–10.7	2.3( $\pm 0.12$ )	0.1352
842.90	0–10.5	−1.2( $\pm 0.05$ )	−0.0876
686.87	0–10.7	1.4( $\pm 0.04$ )	0.1312
692.78	0–10.7	1.6( $\pm 0.07)$	0.1491
705.85	0–10.7	2.1( $\pm 0.03$ )	0.1907
711.86	0–9.6	1.5( $\pm 0.05$ )	0.1430
116.79	0–10.5	1.1( $\pm 0.04$ )	0.6875
143.79	0–9.5	1.7 $(\pm 0.03)$	0.8219
188.75	0–10.5	3.5 $(\pm 0.04)$	1.4573
173.72	0–10.5	3.8( $\pm 0.06$ )	1.3780
219.50	0–9.8	7.3 $(\pm 0.06)$	2.0950

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表 2 采用NaCl固体做传压介质时PbCO₃-Ⅱ相的拉曼峰对应的位置、dν/dp和 ${{ \gamma }}$

Table 2. Raman modes and the values of dν/dp and mode Grüneisen parameters ( ${{\gamma}}$ ) for PbCO₃-Ⅱ phase in solid NaCl pressure transmitting medium

${\nu }{_{\mathrm{i}0}}$ /cm⁻¹	Pressure range/GPa	$\dfrac{\mathrm{d}\nu }{\mathrm{d}p} \Big/({\rm{cm} }{^{-1} }\cdot {\rm{GPa} }{^{-1} })$	$\gamma$
1147.20	10.7–15.6	2.2( $\pm 0.12$ )	0.0924
1109.28	15.6–16.0	0.7( $\pm 0.06$ )	0.0282
825.75	10.5–15.6	−1.2( $\pm 0.05$ )	−0.0675
858.34	10.5–15.6	−0.9( $\pm 0.04$ )	−0.0471
723.01	10.7–15.6	1.4( $\pm 0.08$ )	0.0991
725.50	10.7–15.6	1.6( $\pm 0.07)$	0.1060
749.32	10.7–15.6	2.1( $\pm 0.03$ )	0.1341
144.56	10.5–15.6	1.1( $\pm 0.04$ )	0.3945
240.83	10.5–15.6	4.6( $\pm 0.07)$	1.3200
229.56	10.5–14.7	3.4 $(\pm 0.03)$	0.2765
223.38	10.5–15.6	1.8 $(\pm 0.04)$	0.4238
354.58	10.5–14.2	8.9( $\pm 0.06$ )	1.7900

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表 3 采用甲醇-乙醇-水混合溶液做传压介质时PbCO₃-Ⅰ相的拉曼峰对应的位置、dν/dp和 ${{\gamma}}$

Table 3. Raman modes and the values of dν/dp and mode Grüneisen parameters ( ${{\gamma}}$ ) for PbCO₃-Ⅰ phase in the mixture of MEW pressure transmitting medium

${\nu }{_{\mathrm{i}0}}$ /cm⁻¹	Pressure range/GPa	$\dfrac{\mathrm{d}\nu }{\mathrm{d}p} \Big/({\rm{cm} }{^{-1} }\cdot {\rm{GPa} }{^{-1} })$	$\gamma$
1094.30	0–10.5	2.2( $\pm0.12$ )	0.1293
839.56	0–10.5	−1.5( $\pm 0.05$ )	−0.1126
687.66	0–10.5	1.5( $\pm 0.04$ )	0.1410
691.93	0–10.5	1.5( $\pm 0.01)$	0.1055
702.07	0–10.5	1.7( $\pm 0.03$ )	0.1177
718.65	0–10.5	2.1( $\pm 0.05$ )	0.1368
116.60	0–10.5	1.1( $\pm 0.04$ )	0.5057
146.73	0–9.5	1.9 $(\pm 0.03)$	0.7115
216.78	0–10.7	6.2 $(\pm 0.04)$	1.8627
236.42	0–10.7	5.8 $(\pm 0.06$ )	1.5516
219.50	0–9.5	8.1 $(\pm 0.06)$	1.7100

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表 4 采用甲醇-乙醇-水混合溶液做传压介质时PbCO₃-Ⅱ相的拉曼峰对应的位置、dν/dp和 ${{\gamma}}$

Table 4. Raman modes and the values of dν/dp and mode Grüneisen parameters ( ${{\gamma}}$ ) for PbCO₃-Ⅱ phase in the mixture of MEW pressure transmitting medium

${\nu }{_{\mathrm{i}0}}$ /cm⁻¹	Pressure range/GPa	$\dfrac{\mathrm{d}\nu }{\mathrm{d}p} \Big/({\rm{cm} }{^{-1} }\cdot {\rm{GPa} }{^{-1} })$	$\gamma$
1177.48	10.5–15.6	3.4( $\pm 0.12$ )	0.0420
1109.79	14.6–24.2	0.6( $\pm 0.06$ )	0.0239
803.90	10.5–15.6	−1.5( $\pm 0.06$ )	−0.0821
847.27	14.6–15.6	−1.1( $\pm 0.04$ )	0.0604
698.60	10.5–15.6	0.5( $\pm 0.04$ )	0.0334
775.90	10.5–15.6	3.5( $\pm 0.07)$	0.2329
798.67	10.5–15.6	3.9( $\pm 0.03$ )	0.2586
148.69	10.5–15.6	1.3( $\pm 0.04$ )	0.5200
181.70	15.6–15.6	1.6( $\pm 0.07)$	0.5290
332.09	10.5–15.6	6.8( $\pm 0.07)$	1.8720
307.06	10.5–15.6	6.8 $(\pm 0.03)$	2.1950
395.80	10.5–15.6	6.4( $\pm 0.06$ )	1.2210

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表 5 采用甲醇-乙醇混合溶液做传压介质时PbCO₃-Ⅰ相的拉曼峰对应的位置、dν/dp和 ${{\gamma}}$

Table 5. Raman modes and the values of dν/dp and mode Grüneisen parameters ( ${{\gamma}}$ ) for PbCO₃-Ⅰ phase in the mixture of methanol-ethanol pressure transmitting medium

${\nu }{_{\mathrm{i}0}}$ /cm⁻¹	Pressure range/GPa	$\dfrac{\mathrm{d}\nu }{\mathrm{d}p} \Big/({\rm{cm} }{^{-1} }\cdot {\rm{GPa} }{^{-1} })$	$\gamma$
1088.20	0–10.0	1.7( $\pm 0.12$ )	0.0990
847.63	0–9.5	−0.8( $\pm 0.06$ )	−0.0589
868.45	0–9.5	−0.7( $\pm 0.04$ )	−0.0503
674.65	0–10.0	0.3( $\pm 0.04$ )	0.0281
690.66	0–9.5	1.5( $\pm 0.07)$	0.1398
692.35	0–9.5	0.9( $\pm 0.03$ )	0.0838
110.70	0–10.0	0.6( $\pm 0.04$ )	0.3673
162.67	0–9.5	3.6( $\pm 0.07)$	1.7964
190.30	0–10.0	3.9 $(\pm 0.03)$	1.6220
192.44	0–7.8	2.4( $\pm 0.06$ )	0.8703
286.00	0–9.5	7.1 $(\pm 0.06)$	2.0378

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表 6 采用甲醇-乙醇混合溶液做传压介质时PbCO₃-Ⅱ相的拉曼峰对应的位置、dν/dp和 ${{\gamma}}$

Table 6. Raman modes and the values of dν/dp and mode Grüneisen parameters ( ${{\gamma}}$ ) for PbCO₃-Ⅱ phase in the mixture of methanol-ethanol pressure transmitting medium

${\nu }{_{\mathrm{i}0}}$ /cm⁻¹	Pressure range/GPa	$\dfrac{\mathrm{d}\nu }{\mathrm{d}p} \Big/({\rm{cm} }{^{-1} }\cdot {\rm{GPa} }{^{-1} })$	$\gamma$
1124.78	10.0–15.4	1.7( $\pm 0.12$ )	0.0710
824.88	10.0–15.4	−0.8( $\pm 0.06$ )	−0.0439
856.89	14.2–29.0	−0.7( $\pm 0.04$ )	0.0367
691.92	10.0–15.4	0.3( $\pm 0.04$ )	0.0200
715.70	10.0–15.4	1.5( $\pm 0.07)$	0.0995
706.60	10.0–15.4	0.9( $\pm 0.03$ )	0.0592
126.19	10.0–15.4	0.6( $\pm 0.04$ )	0.2402
207.51	10.0–15.4	3.6( $\pm 0.07)$	1.1100
178.50	10.0–15.4	3.9 $(\pm 0.03)$	1.0050
248.32	10.0–15.4	2.4( $\pm 0.06$ )	0.5223

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表 7 采用甲醇-乙醇混合溶液做传压介质时PbCO₃-Ⅲ相的拉曼峰对应的位置、dν/dp和 ${{\gamma}}$

Table 7. Raman modes and the values of dν/dp and mode Grüneisen parameters ( ${{\gamma}}$ ) for PbCO₃-Ⅲ phase in the mixture of methanol-ethanol pressure transmitting medium

${\nu }{_{\mathrm{i}0}}$ /cm⁻¹	Pressure range/GPa	$\dfrac{\mathrm{d}\nu }{\mathrm{d}p} \Big/({\rm{cm} }{^{-1} }\cdot {\rm{GPa} }{^{-1} })$	$\gamma$
1278.87	15.4–30.2	2.1( $\pm 0.12$ )	0.2326
1205.66	15.4–30.2	1.3( $\pm 0.03$ )	0.1623
810.95	15.4–30.2	−0.2( $\pm 0.06$ )	−0.0395
845.17	15.4–30.2	−0.2( $\pm 0.04$ )	−0.0390
694.33	15.4–30.2	0.5( $\pm 0.07$ )	0.1018
898.37	15.4–30.2	2.8( $\pm 0.07)$	0.5183
912.60	15.4–30.2	2.6( $\pm 0.03$ )	0.4767
187.60	15.4–30.2	0.8( $\pm 0.04$ )	0.8090
369.96	15.4–30.2	2.2( $\pm 0.07)$	1.2900
280.19	15.4–30.2	2.1( $\pm 0.06)$	1.9164
417.77	15.4–30.2	2.5( $\pm 0.05$ )	1.3500

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表 8 几种碳酸盐矿物质的化学键键长对比

Table 8. Comparison of bond length of several carbonate minerals

Sample	Bond length/Å	c/Å	V/Å³	Reference
PbCO₃	5.176	6.158	270.449	This study
BaCO₃	5.314	6.430	304.200	Ref.[21]
CaCO₃	4.96	5.74	226.70	Ref.[22]
FeCO₃	4.6861(3)	15.362(2)	292.15(5)	Ref.[20]
MgCO₃	4.6255(3)	14.987(2)	277.69(4)	Ref.[19–20]

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参考文献(22)

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碳酸铅在不同传压介质下的高压拉曼研究

doi: 10.11858/gywlxb.20210813

作者简介: 阿卜力孜 • 麦提图尔荪（1993－），男，硕士研究生，主要从事矿物质在高压下的稳定性研究.E-mail：1715038477@qq.com

通讯作者: 艾尼瓦尔 • 吾术尔（1974－），男，博士，主要从事高压高温材料制备以及高温高压下地球物质特性研究. E-mail：anwar.hushur@outlook.com

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High Pressure Raman Spectroscopic Study of PbCO3 in Different Pressure Transmitting Medium

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作者简介:
阿卜力孜 • 麦提图尔荪（1993－），男，硕士研究生，主要从事矿物质在高压下的稳定性研究.E-mail：1715038477@qq.com

通讯作者:
艾尼瓦尔 • 吾术尔（1974－），男，博士，主要从事高压高温材料制备以及高温高压下地球物质特性研究. E-mail：anwar.hushur@outlook.com

High Pressure Raman Spectroscopic Study of PbCO₃ in Different Pressure Transmitting Medium