High-resolution crystal orientation acquisition method based on scanning electron microscope

A technology of crystal orientation and scanning electron microscopy, which is applied in the field of characterization, can solve problems such as difficult to achieve accurate calibration of nanoscale fine structures, and achieve the effects of convenient operation, reliable technology, and simple equipment

Inactive Publication Date: 2017-03-15
CHONGQING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This means that even if the measurement step size is set to the limit value of its spatial resolu

Method used

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  • High-resolution crystal orientation acquisition method based on scanning electron microscope
  • High-resolution crystal orientation acquisition method based on scanning electron microscope

Examples

Experimental program
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Effect test

Embodiment 1

[0022] 1) Preparation of metal samples for detection

[0023] A metal sample with a thickness of 300 μm was prepared by wire electric discharge cutting; then, the metallographic sandpaper of 200#, 400#, 800#, 1000#, 1500#, 2000# and 2500# was used to grind and thin it step by step to below 90 μm; then Then, at a temperature of -15 °C, in the electrolyte, a double-jet electrolytic instrument was used to perform double-jet thinning electrochemical polishing at a voltage of 10 V for 40 s to prepare a metal sample suitable for detection. Electrolyte, volume fraction is the concentrated perchloric acid of 10% and volume fraction is the mixed solution of absolute ethanol of 90%.

[0024] After treatment, the thickness of the thin area of ​​the prepared metal sample should be 70nm.

[0025] 2) Place the prepared metal sample on the pre-tilted sample stage of the scanning electron microscope and fix it, adjust the inclination angle between the sample and the electron beam to -18°, th...

Embodiment 2

[0027] 1) Preparation of metal samples for detection

[0028] A metal sample with a thickness of 400 μm was prepared by wire electric discharge cutting; then the metallographic sandpaper of 200#, 400#, 800#, 1000#, 1500#, 2000# and 2500# was used to grind and thin it to below 70 μm step by step; then Then, at a temperature of -20 °C, in the electrolyte, a double-jet electrolytic instrument was used to perform double-jet thinning electrochemical polishing at a voltage of 15 V for 60 s to prepare a metal sample suitable for detection. Electrolyte, volume fraction is the concentrated perchloric acid of 12% and volume fraction is the absolute ethanol mixed solution of 88%.

[0029] After treatment, the thin area thickness of the prepared metal sample should be 80nm.

[0030] 2) Place the prepared metal sample on the pre-tilted sample stage of the scanning electron microscope to clamp and fix it, adjust the inclination angle between the sample and the electron beam to -10°, the ac...

Embodiment 3

[0032] 1) Preparation of metal samples for detection

[0033] A metal sample with a thickness of 450 μm was prepared by wire electric discharge cutting; then, the metallographic sandpaper of 200#, 400#, 800#, 1000#, 1500#, 2000# and 2500# was used to grind and thin it step by step to below 70 μm; then Then, at a temperature of -30 °C, in the electrolyte, a double-jet electrolytic instrument was used to perform double-jet thinning electrochemical polishing at a voltage of 20 V for 100 s to prepare a metal sample suitable for detection. Electrolyte, volume fraction is the concentrated perchloric acid of 8% and volume fraction is the absolute ethanol mixed solution of 92%.

[0034] After treatment, the thickness of the thin area of ​​the prepared metal sample should be 60nm.

[0035] 2) Place the prepared metal sample on the pre-tilted sample stage of the scanning electron microscope to clamp and fix it, adjust the inclination angle between the sample and the electron beam to -4...

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Abstract

The invention provides a high-resolution crystal orientation acquisition method based on a scanning electron microscope. The high-resolution crystal orientation acquisition method comprises the following steps: (1) preparing a metal sample with the thickness of 300-500 mu m in a wire cut electrical discharge machining manner; gradually polishing with gold-phase sandpaper to reduce the thickness to be less than 100 mu m; using an automatic twin-jet electropolisher to perform twin-jet electropolishing thickness-reduction for 30-200 seconds at voltage of 10-25 V in electrolyte; and (2) placing the metal sample in a pre-tilt sample stage for clamp fixing, and acquiring parameters at a tilt angle between the sample and an electron beam of 20-0 degrees, an acceleration voltage of 15-30 kV and a working distance of 5-9 mm. The high-resolution crystal orientation acquisition method provided by the invention realizes spatial resolution and angle resolution significantly superior to a conventional backscattered electron diffraction technology in crystal orientation analysis aspect under a scanning electron microscope platform, and further has advantages of being simple in equipment, convenient to operate, technically reliable, high in data acquisition efficiency, easy in processing and analysis, good in repeatability and the like.

Description

technical field [0001] The invention relates to a method for obtaining high-resolution crystal orientation based on a scanning electron microscope. The method is to use a scanning electron microscope to detect a thin area of ​​a metal sample, obtain a sample transmission Kikuchi line pattern, and realize automatic orientation calibration through software. It belongs to the characterization technology field. Background technique [0002] In order to deeply understand the reasons for the changes in the surface properties of materials, it is necessary to have a thorough understanding of the evolution of the surface microstructure and texture, which greatly depends on the test and characterization of the surface. X-ray diffraction (XRD) is sensitive to the crystal structure and orientation of most metal materials, and is often used to determine the phase structure or macroscopic texture changes in the surface layer of the material, but this technique cannot obtain the microstruc...

Claims

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Application Information

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IPC IPC(8): G01N23/22
CPCG01N23/22G01N2223/604
Inventor 柴林江吴昊祝祥辉杨绪盛张朕浩黄灿黄伟九
Owner CHONGQING UNIV OF TECH
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