A TEM study of nanostructures and interfaces in the hot-press sintered ZrB2–SiC–Si3N4 composites

Vladimir Bazhin; Aleksander Nikolaev; Valeria Esthefania Quiroz Cabascango; Changjin Shao; Genrih Davletov; Tatyana Gizatullina; Vadim Fetisov

doi:10.53063/synsint.2023.34165

Vladimir Bazhin ¹
Aleksander Nikolaev ²
Valeria Esthefania Quiroz Cabascango ³
Changjin Shao ⁴
Genrih Davletov ²
Tatyana Gizatullina ²
Vadim Fetisov ²

¹ Department of Metallurgy, Empress Catherine II Saint Petersburg Mining University, Saint Petersburg, Russia
² Department of Petroleum Engineering, Empress Catherine II Saint Petersburg Mining University, Saint Petersburg, Russia
³ Independent Researcher, Quito, Ecuador
⁴ Department of Petroleum Engineering, China University of Petroleum-Beijing 18, Fuxue Road, Changping District, Beijing 102249, China

https://doi.org/10.53063/synsint.2023.34165

Abstract

A fully dense ZrB₂–30 vol% SiC composite containing 5 wt% Si₃N₄ and 4 wt% phenolic resin (1.6 wt% carbon) was sintered using the hot-pressing route under the external pressure of 10 MPa at 1900 ºC for 2 h. The microstructural evolution and interfacial phenomena were scrutinized using advanced microscopy facilities such as high-resolution transmission electron microscopy (HRTEM) and field emission scanning electron microscopy (FESEM). The FESEM images showed the ZrB₂ and SiC grains without any evidence of Si₃N₄. The formation of the hexagonal BN (hBN) phase was proven in the sintered composite. The hBN nanosheets had a graphite-like morphology with an average thickness of 20 nm. This phase has a perpendicular orientation to the pressure direction and prevents abnormal ZrB₂ grain growth. Two types of ZrB₂/SiC interfaces were detected, which exhibited an amorphous phase along with the grain boundary and a clean/smooth interface, resulting from the Si₃N₄ addition. HRTEM and inverse fast Fourier transform (IFFT) observations disclosed that the d-spacing value in the ZrB₂ grain (0.335 nm) is higher than those reported in the literature. Furthermore, it was found that the exerted pressure during the sintering distorted atomic planes. The presence of numerous dislocations within the ZrB₂ grains confirmed dislocation creep as the main densification mechanism.

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Keywords: ZrB2–SiC ceramics, Si3N4 additive, Hot-pressing, Interface, Microstructure, Dislocation

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