4.3.1 Synthesis in organic solvents
In contrast to nanocrystalline nitrides and phosphides of the 13th group investigations to prepare nanocrystalline group 13-antimonides in solution are nearly unknown. Chemical preparation methods are largely limited to traditional solid state-chemical methods such as melting of the pure elements or metathesis reactions. Thus, for example, AlSb, GaSb and InSb were prepared by reaction of MI3 (M = Al, Ga, In) with Na3Sb between 550 and 600 °C in autoclaves in the form of microcrystalline powders.
An attractive wet-chemical synthetic method for binary III-V materials in solution was described for the first time in 1989 by Wells et al. Reactions of MCl3 (M = Ga, In) with E(SiMe3)3 (E = P, As) yielded the corresponding nanocrystalline materials. Since then a number of other binary, nanocrystalline materials ME were synthesized according to this procedure. This reaction sequence can be transferred to the synthesis of nanocrystalline GaSb. The reaction of GaCl3 and Sb(SiMe3)3 in organic solvents yielded nanocrystalline GaSb-particles, which show, as a function of the used solvent, different levels of contamination with elemental Sb and Si.
Crystalline GaSb particles were obtained, as was face-centered cubic GaSb (sphalerite type) verified by electron diffraction and X-ray powder diffraction studies. The crystallinity of the GaSb-particles increases with increasing reaction temperature. Electron diffraction images of the GaSb-nanoparticles show Debye-Scherrer rings with d-spacings, which agree very well with literature values. While the level of Si/Cl-contaminations of the material decreases with increasing reaction temperature of the solvent, the size of the particles was found to constantly grows.
All samples show the presence of agglomerates of smaller nanocrystallites. The particle size correlates with the boiling temperature of the solvent. Crystallites were obtained in pentane with a particle size of 10-15 nm, in hexane of 15 nm, in toluene of 25 nm and in xylene of 50 nm. Based on the SEM images the lattice constants of the crystallites were determined. Figure 1 illustrates exemplarily the d-spacings of 0.6 and 3.5 nm, which can be assigned to the planes (100) and (111) in cubic GaSb.
 See for example: a) T. J. Trentler, S. C. Goel, K. M. Hickman, A. M. Viano, M. Y. Chiang, A. M. Beatty, P. C. Gibbons, W. E. Buhro, J. Am. Chem. Soc.1997, 119, 2172; b) J. Jiang, A. K. Schaper, R. Schäfer, T. Hihara, J. A. Becker, Adv. Mater. 1997, 9, 343; c) Y.-D. Li, X.-F. Duan, Y.-T. Qian, L. Yang, M.-R. Ji, C.-W. Li, J. Am. Chem. Soc.1997, 119, 7869; d) Y. Xie, P. Yan, J. Lu, W. Wang, Y. Qian, Chem. Mater. 1999, 11, 2619.
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