HfB2-SiC-HfC陶瓷相组成与相成分定量分析的对比研究

doi:10.15541/jim20140058

无机材料学报 ›› 2014, Vol. 29 ›› Issue (10): 1105-1109.DOI: 10.15541/jim20140058 CSTR: 32189.14.10.15541/jim20140058

HfB₂-SiC-HfC陶瓷相组成与相成分定量分析的对比研究

胡冬力^1,2, 邢娟娟¹, 郑强³, 顾辉¹, 倪德伟^1,2, 张国军¹

(1. 中国科学院上海硅酸盐研究所, 高性能陶瓷和超微结构国家重点实验室, 上海200050; 2. 中国科学院大学, 北京100049; 3. Max Planck Institute for Chemical Physics of Solids, N?thnitzerStra?e 40, 01187 Dresden, Germany)

收稿日期:2014-02-10 修回日期:2014-03-24 出版日期:2014-10-20 网络出版日期:2014-09-22
作者简介:胡冬力(1986–), 男, 博士. E-mail:dlhu@student.sic.ac.cn
基金资助:
国家自然科学基金(51172255, 51202272)

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

HU Dong-Li^1,2, XING Juan-Juan¹, ZHENG Qiang³, GU Hui¹, NI De-Wei^1,2, ZHANG Guo-Jun¹

(1. State Key Laboratory of High Performance Ceramics and Superfine Microstructures, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China; 2.University of Chinese Academy of Sciences, Beijing 100049, China; 3.Max Planck Institute for Chemical Physics of Solids, N?thnitzerStra?e 40, 01187Dresden, Germany)

Received:2014-02-10 Revised:2014-03-24 Published:2014-10-20 Online:2014-09-22
About author:HU Dong-Li. E-mail:dlhu@student.sic.ac.cn
Supported by:
National Natural Science Foundation of China (51172255, 51202272)

摘要/Abstract

摘要：

以两种不同WC含量、不同球磨介质的无压烧结HfB₂-SiC-HfC超高温陶瓷为研究对象, 对比了两套集成式相组成和相成分定量分析方法, 发现基于X射线衍射和扫描电镜分析的HfB₂、SiC和HfC相组成和固溶度测量结果相互符合, 都适用于复相陶瓷的综合性定量分析。基于扫描电镜的分析还进一步发现和测量出痕量WB相的含量; XRD-K值法被成功应用于测量固溶度低的相组成。两个对比样品的定量分析结果表明: 烧结助剂含量和球磨介质的改变都不影响W在HfB₂和HfC相中的固溶度, 支持了反应致密过程中液相起关键作用的观点; SiC球磨会造成W的损失, 因此Si₃N₄是更合适的球磨介质。

关键词: 超高温陶瓷, X射线衍射, 扫描电镜, 相组成-相成分定量, 球磨介质

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

中图分类号:

TQ174

胡冬力, 邢娟娟, 郑强, 顾辉, 倪德伟, 张国军. HfB₂-SiC-HfC陶瓷相组成与相成分定量分析的对比研究[J]. 无机材料学报, 2014, 29(10): 1105-1109.

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.

图/表 6

参考文献 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

HfB₂-SiC-HfC陶瓷相组成与相成分定量分析的对比研究

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

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参考文献 20

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Metrics

本文评价

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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