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Content archived on 2022-12-23

Novel ion and mixed conductors for solid state ionic devices : synthesis based on combustion wave and shock wave methods

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This joint research project focuses on the development of new synthesis routes for novel electrode material for rechargeable solid state lithium batteries of the rocking-chair or swing type. Several new techniques for the synthesis of B-C-N compounds have been developed: combustion by external rapid heating, combustion by internal heat - supplying reactants, synthesis in a high-frequency inductive oven, synthesis in a plasma carbon arc, Self-Propagating High-Temperature Synthesis in a large scale reactor. Thermodynamic calculation of B4C and BN synthesis in combustion wave were performed to find optimal conditions for the process. B4C and BN were produced in the combustion regime. Active carbon soot was synthesized using the shock wave technique. The resulting powder is amorphous and has small particle size. Four reactors have been used to produce BC2N: a constant- pressure reactor, a low-pressure reactor, a radio-frequency inductive furnace, and a plasma carbon arc. During these syntheses different types of precursors were used. Several types of carbon including fullerenes (C60, C70) and carbon-containing fullerenes waste, several types of boron and boron-contained compounds were selected to be ingredients of the reactive mixtures. Products of reactions were investigated by XRD and chemical analysis. Resulting products are not B-C-N compounds when synthesized from pure B, C and N. Successful synthesis of BC2N compound was realized by SHS technique in a large scale reactor and by carbon Arc Synthesis. XRD and chemical analysis show that synthesized B-C-N compound is a mixture of BN and BC2N. The following types of analysis were performed to investigate the B-C-N powder: SEM, AFM, DTA, Chemical analysis, Particle size measurements, BET, XRD, and electrochemical, measurements. Electrochemical measurements show that there is a good cycling behaviour of pressed electrodes manufacturing from "BCN-74" material (about 140 cycles at 0.5 mA/cm2 current). Synthesized powders of B-C-N were compacted by different techniques: CUP, HIP and DC in flat (by the shock wave) and cylindrical ( by the detonation wave) configurations. Minimal porosity achieved are: Graphite - 17%(HIP), 19.8%(DC), (B-C-N) - 21.2% (HIP).

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