The Application Of EBSD In Materials Research

The present work is carried out with the Electron Backscatter Diffraction (EBSD) analysis system of the Center of Analysis & Measurement of Zhejiang University, which is composed of Field Emission Scanning Electron Microscopy (FESEM SIRION100, FEI Incorporated, Holand) and EBSD analysis apparatus (TSL Incorporated, USA).The operation parameters of EBSD system are summarized as following: the accelerating voltage 30 kv, the work distance 10.0 mm, the vacuum degree more than 5×10-5 Torr, the spot size 6.0. The operation process of EBSD is prescribed as followings: (1) samples preparation; (2) the relative position of the microscope, sample and diffraction instrument are calibrated by the standard sample, and the SEM system is adjusted to normal state; (3) sample installation; (4) the analysis area is determinated under SEM image field, the analyzed area of the sample is focused to the same position as the calibrated point of the standard sample; (5)setting up the system conditions and collecting the EBSP; (6) the collected patterns is indexed by PC; (7) the data is saved.There are various preparation methods for EBSD samples and the following methods are employed by the literatures review: the common mechanical polishing method and the electro-polishing method. For metallic materials the chemical polishing or electro-polishing method is used to remove the deformation layer. Ion-sputter thinning can remove the deformation layer of metal materials and nonmetallic materials caused by a process. For some powder materials with regular crystalline form, their smooth crystal plane can be analyzed directly.The bulk materials with good electro-conductivity, e.g. single crystal Si wafers, pure iron sheet, are analyzed by EBSD in the present work. The experimental result is accordant with the known result, which indicates the feasibility of the processing parameters, operating procedures and preparation of samples proposed in the present paper. The objective of development of EBSD analysis technique is achieved.At present, EBSD is seldom used to analyze these powder materials with fine crystalline grain and nanosized materials. An attempt is carried out to analyze the powder materials with fine crystalline grain by EBSD. Microcrystalline PbTiO3 is investigated by EBSD, and then analyzed by X-ray diffraction. Experimental results of EBSD are accordant with that of XRD, which illuminates that surface EBSD analysis technique is feasible to determine crystal structure and orientation of powder material with new structure.The crystal structure and orientation of ZnO whisker and Ag nanorod are determined through EBSD analysis technique in the present investigation, respectively. The repeating test results appears good consistency.