EBSD sample making method

A vacuum and in-equipment technology, applied in the field of EBSD sample preparation, can solve the problems of long sample preparation time for EBSD samples, long sample preparation time, difficult to achieve the expected effect, etc., to shorten the sample preparation process and time, and the sample preparation success rate. Stable and improved sample preparation efficiency

Inactive Publication Date: 2019-01-25
CENT IRON & STEEL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, in the prior art, in order to reduce the surface stress, three methods of mechanical polishing, electrolytic polishing and ion polishing are usually used for sample preparation. Polishing takes a long time to prepare samples. Different processes are used for different materials, and the success rate of sample preparation cannot be guaranteed. Electropolishing takes a short time to prepare samples, but it is not suitable for all materials. The adjustment range of process parameters for different materials is large. In addition, different electrolytic polishing solutions need to be equipped, and there are many variables in the sample preparation process. It is cumbersome to adjust the voltage, polishing time, temperature, and electrolyte selection; ion polishing has a good sample preparation effect, but it takes a long time and is expensive. Ion polishing where polishing and mechanical polishing are not enough
[0005] Therefore, for the subsequent stress relief of the sample, the sample preparation often lasts for a long time, but it is often difficult to achieve the expected effect, resulting in a long sample preparation time and relatively high cost for the EBSD sample, but the sample preparation success rate is low, and at the same time Calibration rate is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] For low carbon steel Q345, heat up to 1350°C for 2 minutes and then anneal and cool at 128°C / min. The specific process is as follows:

[0065] Process the low-carbon steel plate produced in industry into a cylindrical sample of Φ6×4mm. To test the upper surface of the cylinder, it is necessary to grind the upper surface with sandpaper of different grain sizes. The last step is to use no less than 1000# sandpaper to grind the sample. Mechanical polishing, using a polishing agent with a particle size of 1 μm. After polishing, ensure that the surface has no obvious scratches, and then put the sample into a beaker filled with acetone for ultrasonic cleaning for 20 minutes. After cleaning, polish again to ensure that the surface is bright and free of foreign matter.

[0066] After successful sample preparation, the sample is placed in an alumina crucible and placed in a heat treatment furnace in a high-temperature laser confocal device that can be vacuumed and ventilated. V...

Embodiment 2

[0070] For low carbon steel Q345, heat up to 1150°C for 2 minutes and then anneal and cool at 300°C / min. The specific process is as follows:

[0071] Process the low-carbon steel plate produced in industry into a cylindrical sample of Φ6×4mm. To test the upper surface of the cylinder, it is necessary to grind the upper surface with sandpaper of different grain sizes. The last step is to use no less than 1000# sandpaper to grind the sample. Mechanical polishing, using a polishing agent with a particle size of 1 μm. After polishing, ensure that the surface has no obvious scratches, and then put the sample into a beaker filled with acetone for ultrasonic cleaning for 20 minutes. After cleaning, polish again to ensure that the surface is bright and free of foreign matter.

[0072] After successful sample preparation, the sample is placed in an alumina crucible and placed in a heat treatment furnace in a high-temperature laser confocal device that can be vacuumed and ventilated. V...

Embodiment 3

[0076] For low carbon steel Q345, heat up to 950°C for 2 minutes and then anneal and cool at 300°C / min. The specific process is as follows:

[0077] Process the low-carbon steel plate produced in industry into a cylindrical sample of Φ6×4mm. To test the upper surface of the cylinder, it is necessary to grind the upper surface with sandpaper of different grain sizes. The last step is to use no less than 1000# sandpaper to grind the sample. Mechanical polishing, using a polishing agent with a particle size of 1 μm. After polishing, ensure that the surface has no obvious scratches, and then put the sample into a beaker filled with acetone for ultrasonic cleaning for 20 minutes. After cleaning, polish again to ensure that the surface is bright and free of foreign matter.

[0078] After the sample preparation is successful, the sample is placed in an alumina crucible and placed in a heat treatment furnace in a high-temperature laser confocal device that can be vacuumed and ventilat...

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Abstract

The invention provides an EBSD sample making method. The method includes: sample making, wherein a preset-size test is made from sample raw-material, and a to-be-tested surface of the test sample is polished; and heat processing, wherein the test sample after sample making completion is placed in vacuum airtight equipment capable of temperature control, heat processing is carried out according topreset technology, and the sample is used for an EBSD test after heat processing completion. Through the method, a sample making process and time can be shortened, sample making costs can be reduced,sample making efficiency can be improved, calibration rates of IPF graphs in EBSD tests can be significantly improved at the same time, and a highest calibration rate can reach 99%.

Description

technical field [0001] The invention belongs to the technical field of metal material microstructure analysis and testing, in particular to an EBSD sample preparation method. Background technique [0002] Electron backscatter diffraction (EBSD) technology is to install a set of EBSD acquisition hardware and analysis system in the SEM, so that the micro-area crystal structure and orientation information of the sample can be analyzed in the SEM, and the micro-area crystal structure and orientation information can be compared with the corresponding to the microstructure. Compared with the research method of analyzing the microscopic crystal structure and orientation information of materials in TEM, the analysis area of ​​EBSD technology is large, and the number of grains obtained is large. It has become an effective analysis method for fast and efficient quantitative statistical research on the microstructure and texture of materials. It has a wide range of applications, inclu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/20008
CPCG01N23/2005
Inventor 张淑兰王昌曹文全董瀚王辉
Owner CENT IRON & STEEL RES INST
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