Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

High-Entropy Diborides – Silicon Carbide Composites by Reactive and Non-reactive Spark Plasma Sintering: A Comparative Study

Version 1 : Received: 21 December 2023 / Approved: 22 December 2023 / Online: 22 December 2023 (07:11:43 CET)

A peer-reviewed article of this Preprint also exists.

Pakhomova, E.; Cao, G.; Orrù, R.; Garroni, S.; Ferro, P.; Licheri, R. High-Entropy Diborides—Silicon Carbide Composites by Reactive and Non-Reactive Spark Plasma Sintering: A Comparative Study. Materials 2024, 17, 718. Pakhomova, E.; Cao, G.; Orrù, R.; Garroni, S.; Ferro, P.; Licheri, R. High-Entropy Diborides—Silicon Carbide Composites by Reactive and Non-Reactive Spark Plasma Sintering: A Comparative Study. Materials 2024, 17, 718.

Abstract

The Reactive Spark Plasma Sintering (R-SPS) method is compared in this work with the two-steps SHS-SPS route, based on combination of the Self-propagating High-temperature Synthesis (SHS) with the SPS process, for the fabrication of dense (Hf0.2Mo0.2Ti0.2Ta0.2Nb0.2)B2-SiC and (Hf0.2Mo0.2Ti0.2Ta0.2Zr0.2)B2-SiC ceramics. A multiphasic and inhomogeneous product, containing various borides, is obtained at 2000°C/20min by R-SPS, from transition metals, B4C and Si. In contrast, if the same precursors are first reacted by SHS, and then processed by SPS under the optimized condition of 1800°C/20min, the desired ceramics are successfully attained. Both High-Entropy-Boride/SiC products display densities > 97%, uniform microstructures and contained only small amounts of residual oxides (<2.4 wt.%). The presence of SiC makes the sintering temperature milder, i.e. 150°C below to that needed by the corresponding additive-free system. Fracture toughness is also markedly improved, particularly when considering the Nb-containing system processed at 1800°C/20min, whereas KIC progressively decreases (from 7.35 to 5.36 MPa m1/2) as the SPS conditions become more severe. SiC addition is found to inhibit the volatilization of metal oxides like MoO3 formed during oxidation experiments, thus avoiding mass loss in the ceramics. The benefits above also likely take advantage of the fact that the two composite constituents are synthesized in parallel, according to the SHS-SPS approach, rather than being produced separately and combined subsequently, so that strong interfaces between them are formed.

Keywords

high-entropy borides; silicon carbide; spark plasma sintering; self-propagating high-temperature synthesis; resistance to oxidation; fracture toughness

Subject

Chemistry and Materials Science, Ceramics and Composites

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