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Synthesis and properties of transition metal carbides
Nedvědová Šolcová, Pavlína ; Tyrpekl, Václav (advisor) ; Zákutná, Dominika (referee)
This master thesis is a follow-up of my bachelor's project, where the goal was to prepare high entropy carbide (HEC), namely (Ti, Zr, Hf, Nb, Ta)C, by the sol-gel method followed by carbothermal reduction using spark plasma sintering facility (SPS). In this work, the first aim is to substitute SPS with ultra-fast high-temperature sintering (UHS) for the same HEC, (Ti, Zr, Hf, Nb, Ta)C. The advantages of UHS compared to SPS are a thousand times lower consumption of electricity and simpler set-up. The second aim is the adaptation of the synthesis for the preparation of HEC of different compositions, (Cr, Mn, Fe, Co, Ni)C. The third aim is the testing of the presented sol-gel technique on the production of borides, while the initial experiments were focused on boro- carbothermal reduction. Keywords: high entropy carbides, high entropy borides, transition metals, carbothermal reduction, high-temperature ceramics, sol-gel method
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Nonconventional synthesis of high entropy carbides
Šolcová, Pavlína ; Tyrpekl, Václav (advisor) ; Havlíček, David (referee)
This thesis aimed to streamline the method of the preparation of high entropy carbides. The simplification of synthesis and expends reduction were achieved using sol-gel method instead of using commercial starting powders. As precursors of transition metals, the chlorides (TiCl3, TaCl4, HfCl4 a NbCl5) and chlor-oxide (ZrOCl2) were used. The source of carbon was citric acid. All reactants were mixed in solution and dried to gel. The pyrolysis at 800 řC afterwards leads to creation of the amorphous carbon, which embedded the transition metal oxide nanoparticles. The carbothermal synthesis was completed in Spark plasma sintering device at 1400 řC, 1600 řřC and 1900 řC. Formation of high entropy carbide phase was achieved at 1600řC, which is almost 400 řC less than previously reported in literature. Intermediate and final products were characterized with powder X-Ray diffraction, scanning electron microscopy and products, in addition, were characterized with transmission electron microscopy and elements mapping. Key words: high entropy carbides, carbothermal reduction, high temperature ceramics, sol-gel method,
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