On the clathrate form of elemental silicon, Si136:: preparation and characterisation of NaxSi136 (X → 0)

被引:101
作者
Ammar, A
Cros, C
Pouchard, M
Jaussaud, N
Bassat, JM
Villeneuve, G
Duttine, M
Ménétrier, M
Reny, E
机构
[1] Univ Bordeaux 1, CNRS, UPR 9048, Inst Chim Mat Condensee, F-33608 Pessac, France
[2] Univ Bordeaux 3, UMR 5060, IRAMAT, CNRS, F-33607 Pessac, France
[3] Univ Cadi Ayyad, Fac Sci Semlalia, Lab Solide Mineral, Marrakech, Morocco
关键词
silicon; silicon clathrate; NMR spectroscopy; EPR spectroscopy; sodium;
D O I
10.1016/j.solidstatesciences.2004.02.006
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The clathrate form of silicon, Si-136 (otherwise known as Si-34), having a residual sodium content as low as 35 ppm (i.e., x similar to 0.0058 in NaxSi136), has been prepared by thermal decomposition of NaSi under high vacuum, followed by several other treatments under vacuum, and completed by repeated reactions with iodine. The residual amount of sodium has been determined by a combination of analytic and spectroscopic methods involving XRD, electron probe microanalysis, atomic absorption, NMR and EPR. This latter technique proved to be very appropriate to the characterisation of very diluted sodium atoms in such clathrate structure and to the quantitative determination of its residual concentration. (C) 2004 Elsevier SAS. All rights reserved.
引用
收藏
页码:393 / 400
页数:8
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