透射模式电子背散射衍射技术在纳米材料研究中的应用

doi:10.15541/jim20140065

无机材料学报 ›› 2015, Vol. 30 ›› Issue (8): 833-837.DOI: 10.15541/jim20140065

透射模式电子背散射衍射技术在纳米材料研究中的应用

刘紫微, 华佳捷, 林初城, 姜彩芬, 曾毅

(中国科学院上海硅酸盐研究所, 上海200050)

收稿日期:2015-01-29 修回日期:2015-03-20 出版日期:2015-08-20 网络出版日期:2015-07-21
作者简介:刘紫微(1981–), 女, 硕士, 工程师. E-mail: ziweiliu@mail.sic.ac.cn
基金资助:
科技部国际合作专项(2013DFG52290);中国科学院上海硅酸盐研究所科技创新重点项目(Y37ZC4141G);上海市无机非金属材料分析测试表征专业技术服务平台(14DZ2292900)Fund of International Science & Technology Cooperation Project of China (2013DFG52290);Science & Technology Innovation Key Project of Shanghai Institute of Ceramics (Y37ZC4141G);Shanghai Technical platform for Testing and Characterization on Inorganic Materials (14DZ2292900)

Application of Transmission Electron Backscattered Diffraction in Nanomaterials Research

LIU Zi-Wei, HUA Jia-Jie, LIN Chu-Cheng, JIANG Cai-Fen, ZENG Yi

(Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China)

Received:2015-01-29 Revised:2015-03-20 Published:2015-08-20 Online:2015-07-21
About author:LIU Zi-Wei. E-mail: ziweiliu@mail.sic.ac.cn

摘要/Abstract

摘要：

为了提高电子背散射衍射技术的空间分辨率, 使之能够对纳米尺度的晶粒或超细粉末进行相鉴定和取向分析, 本研究通过自主设计的透射模式电子背散射衍射技术的样品台, 及调整EBSD探头位置及角度, 收集到清晰、完整的透射电子菊池衍射花样。研究了减薄块体样品厚度对透射电子菊池衍射花样的影响, 对减薄氧化锆涂层样品进行了t-EBSD面分布分析, 其结果的平均角度偏差(MAD)值仅为0.38, 成功鉴定出小于30 nm尺度的纳米氧化锆涂层立方相; 将超声分散后的纳米TiO₂粉体滴在铜网上, 采用t-EBSD对纳米颗粒进行点分析, 成功鉴定了锐钛矿相和金红石相TiO₂, 其中纳米锐钛矿TiO₂粉体的最小尺寸为20 nm左右, 使得扫描电镜中相鉴定的最小分辨率从目前的约100 nm提高到小于30 nm, 大大拓展了电子背散射衍射技术在纳米材料研究中的应用范围。

关键词: 透射模式电子背散射衍射, 高分辨率, 相鉴定, 纳米材料

Abstract:

To improve the spatial resolution of electron backscatter diffraction technique, by which phase identification and orientation analysis of the nano scale grain or ultrafine powders can be achieved, a special specimen holder for transmission electron backscatter diffraction techniques (t-EBSD) accompanied by adjusting position and angle of EBSD detector, was newly designed. The new sample holder could fix the STEM samples, enabling clear TEM Kikuchi diffraction patterns to be successfully collected by EBSD detector. Then the effect of sample thickness on Kikuchi diffraction pattern was investigated. Based on the newly designed holder, the t-EBSD mapping of zirconia coating was acquired with the mean angle deviation (MAD) at only 0.38, successfully identified the cubic phase of less than 30 nm zirconia coating. Put the ultrasonic dispersed TiO₂ powder on copper mesh, the point analysis of t-EBSD could identify the anatase and the rutile of TiO₂, distinguishing minimum size of anatase phase TiO₂less than 20 nm. Therefore, the minimum resolution of phase identification in scanning electron microscopy is improved from about 100 nm to less than 30 nm, demonstrating the electron backscatter diffraction technology a very promising way in nano materials research.

Key words: transmission electron backscattered diffraction, high resolution, phase identification, nanometer materials

中图分类号:

TN16

刘紫微, 华佳捷, 林初城, 姜彩芬, 曾毅. 透射模式电子背散射衍射技术在纳米材料研究中的应用[J]. 无机材料学报, 2015, 30(8): 833-837.

LIU Zi-Wei, HUA Jia-Jie, LIN Chu-Cheng, JIANG Cai-Fen, ZENG Yi. Application of Transmission Electron Backscattered Diffraction in Nanomaterials Research[J]. Journal of Inorganic Materials, 2015, 30(8): 833-837.

图/表 7

图1 SEM中EBSD与t-EBSD的样品放置示意图

Fig. 1 Schematic diagram of sample position laid in SEM EBSD and t-EBSD model (a) EBSD; (b) t-EBSD

图2 单晶硅样品中采用蒙特卡洛模拟得到的电子扩展范围(30 kV)

Fig. 2 Monte Carlo simulations of scattering trajectories for monocrystallinesilicon (Beam energy = 30 kV) (a) EBSD; (b) t-EBSD

图3 减薄SiC/BN复相陶瓷的STEM表征结果及其对应各点的t-EBSD花样

Fig. 3 STEM morphology of SiC/BN compound by ion milling and the corresponding t-EBSD Kikuchi patterns

图4 氧化锆涂层的t-EBSD表征结果

Fig. 4 t-EBSD characterization of zirconium oxide coating (a) Grain band contrast; (b) Phase map of zirconium oxide; c: t-EBSD of grain orientation

图5 t-EBSD菊池花样与数据库晶体结构信息匹配程度

Fig. 5 Matching degree of T-EBSD kikuchi patterns and crystalline structure information in database

图6 表征区域小晶粒统计

Fig. 6 Characterization of small grains (a) Grain size distribution in the coating; (b) Distribution of zirconia crystal grains between 30-100 nm

图7 氧化钛纳米粉体的SEM表征结果及其对应氧化钛纳米粉体单颗粒t-EBSD菊池花样

Fig. 7 SEM image of nano-titanium oxide powder and corresponding t-EBSD kikuchi patterns of nano-titanium oxide powder

参考文献 14

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透射模式电子背散射衍射技术在纳米材料研究中的应用

Application of Transmission Electron Backscattered Diffraction in Nanomaterials Research

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