Comparative Study on Quantitation of Phase Component and Phase Composition of HfB2-SiC-HfC Ceramics

doi:10.15541/jim20140058

Abstract

Abstract:

Phase component and phase composition of two pressureless-sintered HfB₂-SiC-HfC ultra-high temperature ceramic samples were quantitatively analyzed. The results obtained by two different methods were compared. The phase component and phase composition for HfB₂, SiC and HfC phases are in consistence, suggesting that the two methods respectively based on X-ray diffraction (XRD) and scanning electron microscope (SEM) are both applicable to the phase quantification for ceramic composites. Trace WB phase was also detected and further quantified by the backscattered electron (BSE) method. XRD-K value method was successfully extended to quantify the low-solution phase components. Quantitative results of stable W solute levels in HfB₂ and HfC phases in both samples, which were prepared with different milling media and WC contents, indicate that the liquid phase plays a key role in the reactive-densification process. The loss of W by the SiC milling makes Si₃N₄ to be more suitable milling medium.

Key words: UHTCs, XRD, SEM, quantitative analysis, milling media

CLC Number:

TQ174

HU Dong-Li, XING Juan-Juan, ZHENG Qiang, GU Hui, NI De-Wei, ZHANG Guo-Jun. Comparative Study on Quantitation of Phase Component and Phase Composition of HfB₂-SiC-HfC Ceramics[J]. Journal of Inorganic Materials, 2014, 29(10): 1105-1109.

Figures/Tables 6

References 20

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Phase	R. C. P. / nm			I. S. R.
Phase		HSW5-N	HSW10-C	HSW5-N	HSW10-C
HfB₂	a	0.31374(2)	0.31372(2)	5263996	3613367
HfB₂	c	0.34678(3)	0.34675(2)	5263996	3613367
SiC	a	0.30816(4)	0.3080(4)	43397	45603.5
SiC	c	1.5106(8)	1.510(2)	43397	45603.5
HfC	a	0.45899(2)	0.45866(3)	246251	416280

Phase	R. C. P. / nm			I. S. R.
Phase		HSW5-N	HSW10-C	HSW5-N	HSW10-C
HfB₂	a	0.31374(2)	0.31372(2)	5263996	3613367
HfB₂	c	0.34678(3)	0.34675(2)	5263996	3613367
SiC	a	0.30816(4)	0.3080(4)	43397	45603.5
SiC	c	1.5106(8)	1.510(2)	43397	45603.5
HfC	a	0.45899(2)	0.45866(3)	246251	416280

Sample	Method	M _{Solute level}(M=W, Hf) / mol%
Sample	Method	Hf(W)B₂	Hf(W)C	W(Hf)B
HSW5-N	XRD	3.77	12.10	-
HSW5-N	SEM	3.79±0.89	13.62±0.81	6.38±1.96
HSW10-C	XRD	3.93	13.24	-
HSW10-C	SEM	3.74±1.09	14.26±0.69	6.47±1.74

Sample	Method	M _{Solute level}(M=W, Hf) / mol%
Sample	Method	Hf(W)B₂	Hf(W)C	W(Hf)B
HSW5-N	XRD	3.77	12.10	-
HSW5-N	SEM	3.79±0.89	13.62±0.81	6.38±1.96
HSW10-C	XRD	3.93	13.24	-
HSW10-C	SEM	3.74±1.09	14.26±0.69	6.47±1.74

Sample	Method	Phase component / vol%
Sample	Method	HfB₂	SiC	HfC	WB
HSW5-N	XRD	75.2	22.3	2.5	0
HSW5-N	SEM	75.8±1.3	20.6±1.7	3.0±0.3	0.6±0.2
HSW10-C	XRD	65.0	29.6	5.4	0
HSW10-C	SEM	67.0±5.0	27.0±4.7	5.3±0.8	0.7±0.5

Comparative Study on Quantitation of Phase Component and Phase Composition of HfB₂-SiC-HfC Ceramics

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Phase	HSW5-N / mol%		HSW10-C / mol%
Phase	Theoretical	SEM	Theoretical	SEM
HfB₂	94.8	94.5	90.1	90.1
WC	5.2	-	9.9	-
HfC	-	4.5	-	8.5
WB	-	1.0	-	1.4
W (sum)	5.2	5.1	9.9	5.9

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