织构化ZrB2-SiC超高温陶瓷中取向关系的EBSD研究

doi:10.15541/jim20170210

无机材料学报 ›› 2018, Vol. 33 ›› Issue (4): 380-384.DOI: 10.15541/jim20170210

所属专题：陶瓷基复合材料

织构化ZrB₂-SiC超高温陶瓷中取向关系的EBSD研究

郑海亚¹, 孟晨曦¹, 胡冬力¹, 顾辉¹, 刘海涛², 张国军^1,3

1. 上海大学材料科学与工程学院, 上海 200444;
2. 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;
3. 东华大学功能材料研究所, 纤维材料改性国家重点实验室, 上海 201620

收稿日期:2017-04-28 修回日期:2017-05-31 出版日期:2018-04-30 网络出版日期:2018-03-27
作者简介:郑海亚(1990-), 男, 硕士. E-mail: zhenghaiya99@163.com
基金资助:
国家自然科学基金重点项目(51532006)

EBSD Analysis for Orientation Relationship of Textured ZrB₂-SiC Ultra-high Temperature Ceramics

ZHENG Hai-Ya¹, MENG Chen-Xi¹, HU Dong-Li¹, GU Hui¹, LIU Hai-Tao¹, ZHANG Guo-Jun^1,3

1. School of Materials Science and Engineering, Shanghai University, Shanghai 200444, China;
2. State Key Laboratory of High Performance Ceramics and Superfine Microstructures, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China;
3. State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, Research Institute of Functional Materials, Donghua University, Shanghai 201620, China

Received:2017-04-28 Revised:2017-05-31 Published:2018-04-30 Online:2018-03-27
About author:ZHENG Hai-Ya. E-mail: zhenghaiya99@163.com
Supported by:
National Natural Science Foundation of China (51532006)

摘要/Abstract

摘要：

以放电等离子体烧结的织构化ZrB₂-SiC复相陶瓷为研究对象, 利用SEM和EDS方法对相组成进行分析。研究发现, 由于初始粉体与杂质之间存在多种反应, 陶瓷中出现相当含量的ZrC新相及少量的ZrO₂、BN相。与利用TEM研究新生成相与主相间取向关系的常规方法相比, SEM中EBSD方法不但能研究该取向关系, 还可同时对大量相界进行研究以获得统计性结果, 从而避免人为选择性。利用该方法, 对ZrB₂与ZrC相间可能存在的三种取向关系(011¯0)||(111)&[21¯1¯0]||[101¯]、(112¯0)||( 2¯02)&[0001]||[111]和(1¯21¯0)||(2 2¯0)&[0001]||[110]进行验证, 确定本实验中所得复相陶瓷中两相间不存在特定取向关系, 从而推断ZrC的成相遵循均匀成核模式, 而非外延成核。

关键词: 织构化超高温陶瓷, 扫描电镜, EBSD, 取向关系

Abstract:

Textured ZrB₂-ZrC ceramics sintered by spark plasma sintering were analyzed. The results obtained by SEM and EDS demonstrate the formation of an amount of resultant ZrC phase and trace level of ZrO₂ and BN phases, due to the various reactions between starting powders and impurities. Compared with conventional methods in which TEM was used to analyze the orientation relationship between the phase and the primary phase, EBSD method in SEM can not only study the orientation relationship, but also study a large number of phase boundaries simultaneously to obtain statistical results, so as to avoid artificial selectivity. By using this method, three orientation relationships that may exist between ZrB₂ and ZrC phases, i.e. (011¯0)||(111)&[21¯1¯0]||[101¯], (112¯0)||(2¯02)&[0001]||[111], and (1¯21¯0)|| (2 2¯0)&[0001]||[110] were checked. It is determined that there is no specific orientation relationship between the two phases in this study, inferring that the ZrC phase formed with a homogeneous nucleation mode rather than an epitaxial nucleation.

Key words: textured ultra-high temperature ceramic, scanning electron microscope, EBSD, orientation relation

中图分类号:

TQ174

郑海亚, 孟晨曦, 胡冬力, 顾辉, 刘海涛, 张国军. 织构化ZrB₂-SiC超高温陶瓷中取向关系的EBSD研究[J]. 无机材料学报, 2018, 33(4): 380-384.

ZHENG Hai-Ya, MENG Chen-Xi, HU Dong-Li, GU Hui, LIU Hai-Tao, ZHANG Guo-Jun. EBSD Analysis for Orientation Relationship of Textured ZrB₂-SiC Ultra-high Temperature Ceramics[J]. Journal of Inorganic Materials, 2018, 33(4): 380-384.

图/表 5

图1 ZS0(a)、ZS10(b)和ZS20(c)三种样品抛光面的SEM照片及各相的能谱曲线(d)

Fig. 1 SEM images of the polished surface for ZS0 (a), ZS10 (b) and ZS20 (c) samples and EDS spectra for different phases formed in the ceramics (d)

图2 ZrB2和ZrC相间三组取向关系的原子模拟图

Fig. 2 Atomic illustration of orientation relationship of ZrB2 and ZrC in plane pair and orientation pair

表1 ZrB2与ZrC相间晶面对和晶向对的错配度

Table 1 Mismatch of plane pair and orientation pair between ZrB2 and ZrC phases

	Mismatch/%
	Plane	Orientation
(011¯0)\|\|(111)	1.27
[21¯1¯0]\|\|[101¯]		4.50
(112¯0)\|\|(2¯02)	4.50
[0001]\|\|[111]		13.10
(1¯21¯0)\|\|( 2¯20)	4.50
[0001]\|\|[110]		6.40

图3 三组晶面对与晶向对的角度差统计图

Fig. 3 Statistics of misorientation in plane pair and orientation pair

图4 ZS10样品中晶面对与晶向对的角度关系

Fig. 4 Relationships of plane pair and orientation pair in ZS10 sample

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织构化ZrB₂-SiC超高温陶瓷中取向关系的EBSD研究

EBSD Analysis for Orientation Relationship of Textured ZrB₂-SiC Ultra-high Temperature Ceramics

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