同步辐射高压单晶衍射实验技术

李晓东; 李晖; 李鹏善

doi:10.7498/aps.66.036203

摘要

利用同步辐射光源开展高压X射线衍射（X-ray diffraction，XRD）研究已有近四十年的历史，并且已经取得了非常丰硕的成果.单晶XRD作为高压研究的一部分，在同步辐射装置上的应用也有了接近三十年的历史.近年来，随着同步辐射光学技术以及高压技术、特别是大衍射窗口金刚石对顶砧压腔（diamond anvil cell，DAC）的改进与发展，同步辐射高压单晶衍射实验方法在高压研究中的应用越来越普及.由于能够在压力条件下获得样品在三维空间中的衍射信息分布以及数据具有高信噪比等优势，单晶XRD实验方法不仅可以用于压力条件下的晶体结构解析，如获取晶胞参数、空间群、原子坐标以及原子占位等信息，而且可进一步做晶体电荷密度分析研究，得到更多的化学键、电荷分布及其变化等信息.本文主要介绍同步辐射高压单晶XRD实验方法及相关技术，其中包括单晶XRD实验系统、单晶XRD所用DAC、单晶样品装填以及单晶XRD数据处理等内容.

关键词:

高压 /
单晶 /
同步辐射 /
X射线衍射

Abstract

A lot of great work has been done since the high pressure research carried out on synchrotron radiation facility almost 40 years ago. The history of high pressure single-crystal diffraction research on synchrotron radiation facility has also been more than 20 years. Recently, with the development of synchrotron X-ray optical techniques and high pressure technology, especially the invention and improvement of large opening diamond anvil cell (DAC), high pressure single-crystal X-ray diffraction (HPSXRD) method has become more and more popular in high pressure studies. The HPSXRD can be used to perform structure determination and refinement to obtain the information about lattice parameter, space group, atomic coordinate and site occupation. Compared with powder X-ray diffraction, the HPSXRD can not only obtain the three-dimensional diffraction information of samples, but also have much better signal-to-noise ratio. Furthermore, the HPSXRD data can be used to study the electron density distribution to obtain more information about chemical bonds and electron distribution. In this work, we introduce the HPSXRD method in synchrotron radiation facilities, including the knowledge of single-crystal X-ray diffraction experimental system, DAC for HPSXRD, sample loading, and HPSXRD data processing.

Keywords:

作者及机构信息

1.
中国科学院高能物理研究所多学科中心, 北京 100049;

2.
北京工业大学固体微结构与性能研究所, 北京 100124

通信作者: 李晓东, lixd@ihep.ac.cn

基金项目: 国家自然科学基金（批准号：11274030，11474281）资助的课题.

Authors and contacts

1.
Center for Multi-disciplinary Research, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China;

2.
Institute of Microstructure and Properties of Advanced Materials, Beijing University of Technology, Beijing 100124, China

Corresponding author: Li Xiao-Dong, lixd@ihep.ac.cn

Funds: Project supported by the National Natural Science Foundation of China (Grant Nos. 11274030, 11474281).

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施引文献

[1]	Hemley R J 2000 Annu. Rev. Phys. Chem. 51 763
[2]	Shen G, Mao H K 2017 Rep. Prog. Phys. 80 16101
[3]	Duffy T S 2005 Rep. Prog. Phys. 68 1811
[4]	Huang Q, Yu D, Xu B, Hu W, Ma Y, Wang Y, Zhao Z, Wen B, He J, Liu Z, Tian Y 2014 Nature 510 250
[5]	Wang L, Liu B, Li H, Yang W, Ding Y, Sinogeikin S V, Meng Y, Liu Z, Zeng X C, Mao W L 2012 Science 337 825
[6]	Duan D, Liu Y, Tian F, Li D, Huang X, Zhao Z, Yu H, Liu B, Tian W, Cui T 2014 Sci. Rep. 4 6968
[7]	Ma Y, Eremets M, Oganov A R, Xie Y, Trojan I, Medvedev S, Lyakhov A O, Valle M, Prakapenka V 2009 Nature 458 182
[8]	Sun L, Chen X J, Guo J, Gao P, Huang Q Z, Wang H, Fang M, Chen X, Chen G, Wu Q, Zhang C, Gu D, Dong X, Wang L, Yang K, Li A, Dai X, Mao H, Zhao Z 2012 Nature 483 67
[9]	Kang D, Zhou Y, Yi W, Yang C, Guo J, Shi Y, Zhang S, Wang Z, Zhang C, Jiang S, Li A, Yang K, Wu Q, Zhang G, Sun L, Zhao Z 2015 Nat. Commun. 6 7804
[10]	Zeng Q, Sheng H, Ding Y, Wang L, Yang W, Jiang J Z, Mao W L, Mao H K 2011 Science 332 1404
[11]	Katrusiak A 2008 Acta Crystallogr. Sect. A 64 135
[12]	Katrusiak A 2004 Acta Crystallogr. Sect. A 60 409
[13]	Ballaran T B, Kurnosov A, Trots D 2013 High Press. Res. 33 453
[14]	Loubeyre P, LeToullec R, Hausermann D, Hanfland M, Hemley R J, Mao H K, Finger L W 1996 Nature 383 702
[15]	Mao H K, Jephcoat A P, Hemley R J, Finger L W, Zha C S, Hazen R M, Cox D E 1988 Science 239 1131
[16]	Shen G, Sinogeikin S 2015 Rev. Sci. Instrum. 86 71901
[17]	Ohishi Y, Hirao N, Sata N, Hirose K, Takata M 2008 High Press. Res. 28 163
[18]	Mezouar M, Crichton W A, Bauchau S, Thurel F, Witsch H, Torrecillas F, Blattmann G, Marion P, Dabin Y, Chavanne J, Hignette O, Morawe C, Borel C 2005 J. Synchrotron Radiat. 12 659
[19]	Nowell H, Barnett S A, Christensen K E, Teat S J, Allan D R 2012 J. Synchrotron Radiat. 19 435
[20]	Rothkirch A, Gatta G D, Meyer M, Merkel S, Merlini M, Liermann H P 2013 J. Synchrotron Radiat. 20 711
[21]	Liu J 2016 Chin. Phys. B 25 076106
[22]	Katrusiak A 2004 High-Pressure Crystallography (Dordrecht:Springer Netherlands) pp57-68
[23]	Hammersley A P, Svensson S O, Hanfland M, Fitch A N, Hausermann D 1996 High Press. Res. 14 235
[24]	Dera P, Lavina B, Meng Y, Prakapenka V B 2011 J. Solid State Chem. 184 3040
[25]	Bridgman P W 1937 Proc. Am. Acad. Arts Sci. 71 387
[26]	Jamieson J C, Lawson A W, Nachtrieb N D 1959 Rev. Sci. Instrum. 30 1016
[27]	Weir C E, Lippincott E R, van Valkenburg A, Bunting E N 1959 J. Res. Natl. Bur. Stand. A 63 55
[28]	Piermarini G J, Block S 1975 Rev. Sci. Instrum. 46 973
[29]	Bassett W A, Takahashi T, Stook P W 1967 Rev. Sci. Instrum. 38 37
[30]	Mao H K, Bell P M 1978 Carnegie Inst. Yearb. 77 904
[31]	Huber G, Syassen K, Holzapfel W B 1977 Phys. Rev. B 15 5123
[32]	Merrill L, Bassett W A 1974 Rev. Sci. Instrum. 45 290
[33]	Keller R, Holzapfel W B 1977 Rev. Sci. Instrum. 48 517
[34]	Allan D R, Miletich R, Angel R J 1996 Rev. Sci. Instrum. 67 840
[35]	Mao H K, Bell P M 1980 Carnegie Inst. Yearb. 79 409
[36]	Weir C E, Block S, Piermarini G J 1965 J. Res. Natl. Bur. Stand. C 69 275
[37]	Schiferl D 1977 Rev. Sci. Instrum. 48 24
[38]	Ahsbahs H 1984 Rev. Sci. Instrum. 55 99
[39]	Malinowski M 1987 J. Appl. Crystallogr. 20 379
[40]	Chervin J C, Canny B, Besson J M, Pruzan P 1995 Rev. Sci. Instrum. 66 2595
[41]	Moggach S A, Allan D R, Parsons S, Warren J E 2008 J. Appl. Crystallogr. 41 249
[42]	Bassett W A, Spetzler H, Angel R J, Chen G R, Shen A H, Reichmann H J, Yoneda A 1998 Rev. High Press. Sci. Technol. 7 142
[43]	Boehler R, de Hantsetters K 2004 High Press. Res. 24 391
[44]	Boehler R 2006 Rev. Sci. Instrum. 77 115103
[45]	Ahsbahs H 2004 Z. Fr Krist.-Cryst. Mater. 219 305
[46]	Kantor I, Prakapenka V, Kantor A, Dera P, Kurnosov A, Sinogeikin S, Dubrovinskaia N, Dubrovinsky L 2012 Rev. Sci. Instrum. 83 125102
[47]	Li R 2016 Ph. D. Dissertation (Beijing:Institute of High Energy Physics, Chinese Academy of Sciences) (in Chinese)[李蕊2016博士学位论文(北京:中国科学院高能物理研究所)]
[48]	Miletich R, Allan D R, Kuhs W F 2000 Rev. Mineral. Geochem. 41 445
[49]	Macavei J, Schulz H 1990 Rev. Sci. Instrum. 61 2236
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[51]	Mao H K, Shu J, Fei Y, Hu J, Hemley R J 1996 Phys. Earth Planet. Inter. 96 135
[52]	Lin J F, Shu J, Mao H K, Hemley R J, Shen G 2003 Rev. Sci. Instrum. 74 4732
[53]	Piermarini G J, Block S, Barnett J D 1973 J. Appl. Phys. 44 5377
[54]	Angel R J, Bujak M, Zhao J, Gatta G D, Jacobsen S D 2007 J. Appl. Crystallogr. 40 26
[55]	Shen Y, Kumar R S, Pravica M, Nicol M F 2004 Rev. Sci. Instrum. 75 4450
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[57]	Takemura K, Singh A 2006 Phys. Rev. B 73 224119
[58]	Besson J, Pinceaux J 1979 Science 206 1073
[59]	Dewaele A, Loubeyre P, Mezouar M 2004 Phys. Rev. B 70 94112
[60]	Kenichi T, Sahu P C, Yoshiyasu K, Yasuo T 2001 Rev. Sci. Instrum. 72 3873
[61]	Rivers M, Prakapenka V B, Kubo A, Pullins C, Holl C M, Jacobsen S D 2008 High Press. Res. 28 273
[62]	Zhang L, Meng Y, Dera P, Yang W, Mao W L, Mao H K 2013 Proc. Natl. Acad. Sci. 110 6292
[63]	Křivý I, Gruber B 1976 Acta Crystallogr. A 32 297
[64]	Andrews L C, Bernstein H J 1988 Acta Crystallogr. Sect. A 44 1009
[65]	Steller I, Bolotovsky R, Rossmann M G 1997 J. Appl. Crystallogr. 30 1036
[66]	Rossmann M G 2001 International Tables for Crystallography Volume F:Crystallography of Biological Macromolecules (Dordrecht:Springer Netherlands) pp209-211
[67]	Li H, Li X, He M, Li Y, Liu J, Shen G, Zhang Z 2013 J. Appl. Crystallogr. 46 387
[68]	Dera P, Zhuravlev K, Prakapenka V, Rivers M L, Finkelstein G J, Grubor-Urosevic O, Tschauner O, Clark S M, Downs R T 2013 High Press. Res. 33 466
[69]	Leslie A G W 2001 International Tables for Crystallography Volume F:Crystallography of Biological Macromolecules (Dordrecht:Springer Netherlands) pp212-217
[70]	Holton J M, Frankel K A 2010 Acta Crystallogr. Sect. D 66 393
[71]	Kahn R, Fourme R, Gadet A, Janin J, Dumas C, Andre D 1982 J. Appl. Crystallogr. 15 330
[72]	Mao H K, Xu J, Bell P M 1986 J. Geophys. Res. Solid Earth 91 4673
[73]	Sheldrick G M 2008 Acta Crystallogr. Sect. A 64 112
[74]	Collins D M 1982 Nature 298 49

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