Application of Transmission Electron Backscattered Diffraction in Nanomaterials Research

doi:10.15541/jim20140065

Abstract

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

CLC Number:

TN16

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.

Figures/Tables 7

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

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

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

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

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

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

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

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