Microstructure and Oxidation Behavior of ZrB2-SiC Ceramics Fabricated by Tape Casting and Reactive Melt Infiltration

doi:10.15541/jim20240035

Abstract

Abstract:

ZrB₂-based ceramics typically necessitate high temperature and pressure for sintering, whereas ZrB₂-SiC ceramics can be fabricated at 1500 ℃ using the process of reactive melt infiltration with Si. In comparison to the conventional preparation method, reactive synthesis allows for the more facile production of ultra-high temperature ceramics with fine particle size and homogeneous composition. In this work, ZrSi₂, B₄C, and C were used as raw materials to prepare ZrB₂-SiC via combination of tape casting and reactive melt infiltration herein referred to as ZBC ceramics. Control sample of ZrB₂-SiC was also prepared using ZrB₂ and SiC as raw materials through an identical process designated as ZS ceramics. Microscopic analysis of both ceramic groups revealed smaller and more uniformly distributed particles of the ZrB₂ phase in ZBC ceramics compared to the larger particles in ZS ceramics. Both sets of ceramics underwent cyclic oxidation testing in the air at 1600 ℃ for a cumulative duration of 5 cycles, each cycle lasting 2 h. Analysis of the oxidation behavior showed that both ZBC ceramics and ZS ceramics developed a glassy SiO₂-ZrO₂ oxide layer on their surfaces during the oxidation. This layer severed as a barrier against oxygen. In ZBC ceramics, ZrO₂ is finely distributed in SiO₂, whereas in ZS ceramics, larger ZrO₂ particles coexist with glassy SiO₂. The surface oxide layer of ZBC ceramics maintains a dense structure because the well-dispersed ZrO₂ increases the viscosity of glassy SiO₂, preventing its crystallization during the cooling. Conversely, some SiO₂ in the oxide layer of ZS ceramics may crystallize and form a eutectic with ZrO₂, leading to the formation of ZrSiO₄. This leads to cracking of the oxide layer due to differences in thermal expansion coefficients, weakening its barrier effect. An analysis of the oxidation resistance shows that ZBC ceramics exhibit less increase in oxide layer thickness and mass compared to ZS ceramics, suggesting superior oxidation resistance of ZBC ceramics.

Key words: ultra-high temperature ceramic, ZrB₂-SiC, oxidation behavior, reactive melt infiltration

CLC Number:

TQ174

TAN Min, CHEN Xiaowu, YANG Jinshan, ZHANG Xiangyu, KAN Yanmei, ZHOU Haijun, XUE Yudong, DONG Shaoming. Microstructure and Oxidation Behavior of ZrB₂-SiC Ceramics Fabricated by Tape Casting and Reactive Melt Infiltration[J]. Journal of Inorganic Materials, 2024, 39(8): 955-964.

Figures/Tables 12

Fig. 1 Flow chart for the processing of ceramics

Table 1 Raw materials and their molar ratios for ceramics preparation

	ZBC			ZS
Raw materials	ZrSi₂	B₄C	C	ZrB₂	SiC
Molar ratio	2	1	3	1	2

Fig. 2 Microstructure and morphology of ZBC samples (a) XRD patterns of ZBC porous preforms before and after heat treatment; (b) Cross-sectional morphology of ZBC porous preforms after heat treatment; (c) XRD patterns of ceramics after reactive melt infiltration

Fig. 3 Morphologies and corresponding EDS analyses of ZBC ceramics (a-c) Surface; (d-f) Cross section

Fig. 4 Morphologies and corresponding EDS analyses of ZS ceramics (a-c) Surface; (d-f) Cross section

Fig. 5 XRD patterns of ceramics oxidized at 1600 ℃ in the air for different periods (a) ZBC; (b) ZS

Fig. 6 ZrO2-SiO2 binary phase diagram[28]

Fig. 7 Surface morphologies of ZBC ceramics oxidized at 1600 ℃ for different periods (a-c) 2 h; (d-f) 6 h; (g-i) 10 h

Fig. 8 Surface morphologies of ZS ceramics oxidized at 1600 ℃ for different periods (a-c) 2 h; (d-f) 6 h; (g-i) 10 h

Fig. 9 Cross-sectional SEM morphologies of ceramics oxidized at 1600 ℃ for different periods (a, d, g) 2 h; (b, e, h) 6 h; (c, f, i) 10 h

Fig. 10 Thickness of the oxide layer of ceramics oxidized at 1600 ℃ for different periods

Fig. 11 Weight change curves of ZBC and ZS ceramics oxidized at 1600 ℃ for different periods

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Microstructure and Oxidation Behavior of ZrB₂-SiC Ceramics Fabricated by Tape Casting and Reactive Melt Infiltration

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