Morrison, Daniel; (2001) Liquid mediated solid-state metathesis reactions. Doctoral thesis (Ph.D.), University College London.

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Abstract

A variety of metathetical reactions have been carried out in a liquid medium to explore the variety and depth of such reactions. A comparison with the similar solid-state reactions gives a clear indication of the differences and similarities between the two alternate routes. The fact that these reactions go to completion at all is interesting in that the conditions employed are very mild and do not employ any "forcing" means to induce reaction. Main group and transition metal sulphide, selenide and telluride and transition metal phosphide, arsenide and antimonide binary and ternary compounds were synthesised and characterised. An in-depth investigation into the synthesis and characterisation of the chalcopyrite CuInE2 (E = S, Se, Te) family of ternary compounds has also been carried out with a specific focus on liquid variation, reaction duration and temperature and annealing treatment. Solid-state metathesis synthesis of CuInE2 was also carried out for comparison purposes. The main conclusions drawn from the use of the liquid-mediated metathesis methodology are that the reactions, for the most part, go to completion and produce single-phase products. Reactions require a much lower temperature and take much longer to go to completion as compared with the solid-state metathesis method. The majority of the products are X-ray amorphous before being subjected to annealing, and crystallinity can be induced under relatively mild conditions and with good control of crystallinity level. Product particle size is significantly reduced both before and after annealing.

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