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Non-hydrolytic sol-gel synthesis of tantalum sulfides.
Non-hydrolytic sol-gel synthesis of tantalum sulfides.
- Source :
- Journal of Sol-Gel Science & Technology; Mar2014, Vol. 69 Issue 3, p596-604, 9p
- Publication Year :
- 2014
-
Abstract
- Non-hydrolytic sol-gel synthesis provides a low temperature solution based approach to solid-state materials. In this work, reactions of TaX (X = F, Cl, Br, I) with the thio-ethers di- tert-butylsulfide and hexamethyldisilathiane were carried out in chloroform or acetonitrile. The influence of synthetic parameters such as temperature, reaction time, starting sulfur to tantalum ratio, and solvent volume were explored, and optimized conditions for the preparation of phase pure crystalline TaS were established. Amorphous powders were recovered for most of the samples, but crystalline 1T- and 3R-TaS modifications could be selectively prepared by heat treatments of the as-recovered precursors at 700 and 800 °C, respectively. The crystallite sizes could be adjusted by tuning the starting sulfur to tantalum ratios, and by choice of solvent. For specific conditions, nanocrystalline 1T-TaS was directly recovered from solution. To our knowledge, this is the first time that crystalline TaS was directly obtained from low temperature solution based routes. [ABSTRACT FROM AUTHOR]
Details
- Language :
- English
- ISSN :
- 09280707
- Volume :
- 69
- Issue :
- 3
- Database :
- Complementary Index
- Journal :
- Journal of Sol-Gel Science & Technology
- Publication Type :
- Academic Journal
- Accession number :
- 94834756
- Full Text :
- https://doi.org/10.1007/s10971-013-3262-8