Quantitative Analysis for Phase Compositions of ZrB2-SiC-ZrC Ultra-High Temperature Ceramic Composites

doi:10.3724/SP.J.1077.2013.12334

Abstract

Abstract:

Three methods were applied and compared to perform quantitative phase analysis of ZrB₂-SiC-ZrC ultra- high temperature ceramic composites: the K value method by powder X-ray diffraction, two SEM methods to combine secondary electron and backscattered electron images, and electron backscatter diffraction and energy dispersive X-ray spectroscope (EDS) mapping. K value method could be applied conveniently and simply, while the two SEM methods could not only be performed quantitative phase analysis but also reveal phase distribution and relationships. Results from the three methods all show significant deviation of phase compositions from the composite designing of reactive sintering, while they are largely consistent with each other. The content of impurity ZrO₂ phase is detected more than 5vol%, and in contrast, the content of secondary ZrC phase is found substantially below the theoretical 5vol% level and even below 1vol% as calculated by the more sensitive K value method. These quantitative phase analysis could provide technical supports to study the true composite microstructure and phase designing.

Key words: ultra-high temperature ceramic composites, quantitative phase analysis, XRD, SEM

CLC Number:

TQ174

ZHENG Qiang, WANG Xian-Hao, XING Juan-Juan, GU Hui, ZHANG Guo-Jun. Quantitative Analysis for Phase Compositions of ZrB₂-SiC-ZrC Ultra-High Temperature Ceramic Composites[J]. Journal of Inorganic Materials, 2013, 28(4): 358-362.

Figures/Tables 6

References 16

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	Strongest reflection, 2θ/(º)	RIR value	Intensity of strongest reflection/(a.u.)	Calculated content/vol%
ZrB₂	41.6	8.10	291841	74.6
β-SiC	35.7	3.53	17294	19.2
ZrC	33.2	9.23	2999	0.6
m-ZrO₂	28.2	4.81	12304	5.6

	Strongest reflection, 2θ/(º)	RIR value	Intensity of strongest reflection/(a.u.)	Calculated content/vol%
ZrB₂	41.6	8.10	291841	74.6
β-SiC	35.7	3.53	17294	19.2
ZrC	33.2	9.23	2999	0.6
m-ZrO₂	28.2	4.81	12304	5.6

	ZrB₂+ZrC/vol%	β-SiC/vol%	m-ZrO₂/vol%
Area 1	72.9	20.0	7.1
Area 2	77.0	17.7	5.3
Area 3	75.9	18.9	5.2
Area 4	75.8	18.3	5.9
Average	75.4±1.7	18.8±1.0	5.8±0.9

	ZrB₂+ZrC/vol%	β-SiC/vol%	m-ZrO₂/vol%
Area 1	72.9	20.0	7.1
Area 2	77.0	17.7	5.3
Area 3	75.9	18.9	5.2
Area 4	75.8	18.3	5.9
Average	75.4±1.7	18.8±1.0	5.8±0.9

	ZrB₂/vol%	ZrC/vol%	β-SiC/vol%	m-ZrO₂/vol%
Theoretical	74.0	5.0	21.0	0
K value method	74.6	0.6	19.2	5.6
SE and BSE method	75.4		18.8	5.8
EBSD and EDS method	73.8	4.0	14.4	7.8

Quantitative Analysis for Phase Compositions of ZrB₂-SiC-ZrC Ultra-High Temperature Ceramic Composites

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