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Zirconium alloy EBSD sample preparation method

A sample preparation and zirconium alloy technology, applied in the preparation of test samples, etc., can solve the problems of complex process, long polishing time, poor effect, etc., and achieve simple and convenient operation, good clarity, and real sample structure Effect

Inactive Publication Date: 2018-01-19
国核锆铪理化检测有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a zirconium alloy EBSD sample preparation method, which solves the problems of complex process, long polishing time and poor effect in the existing sample preparation technology, and is suitable for various zirconium alloys of any shape and size EBSD sample preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0021] A method for preparing a zirconium alloy EBSD sample provided by the invention comprises the steps of: first cutting a zirconium alloy sample block, using 120#, 800# sandpaper to grind the EBSD calibration surface of the sample block in turn, and then using lactic acid solution, nitric acid Solution and hydrofluoric acid solution mixed chemical polishing agent for chemical polishing, specifically use absorbent cotton dipped in chemical polishing solution to wipe the calibration surface of zirconium alloy block EBSD sample for 10s-20s, and finally rinse with water and dry with cold wind to obtain EBSD specimens of zirconium alloys.

[0022] Exemplary, in the chemical polishing agent by volume percentage, the volume percentage of lactic acid solution is 42%-50%, the volume percentage of nitric acid solution is 35%-45%, and the rest is the volume percentage of hydrofluoric acid solution, the above The sum of the volume percentages of the three solutions is 100%.

[0023] ...

Embodiment 1

[0027] A sample was cut from the Zr-3 alloy plate by wire cutting, and the sample was processed as follows:

[0028] First, grind the EBSD calibration surface of the sample block with 120# and 800# sandpaper in turn, and then rinse it with water;

[0029] Then, wipe the EBSD calibration surface of the zirconium sample block with absorbent cotton dipped in a chemical polishing agent for 10 seconds. The chemical polishing agent is a mixture of lactic acid solution, nitric acid solution and hydrofluoric acid solution, wherein lactic acid solution: nitric acid Solution: the volume ratio of hydrofluoric acid solution is 42%: 35%: 23%, and the mass percent of lactic acid in the lactic acid solution is 87%, the mass percent of nitric acid in the nitric acid solution is 66%, the hydrofluoric acid solution in the hydrofluoric acid solution The mass percent of the acid is 45%, all of which are analytically pure;

[0030] Finally, after wiping, quickly rinse with water and dry with cold...

Embodiment 2

[0032] A sample was cut from the Zr-3 alloy plate by wire cutting, and the sample was processed as follows:

[0033] First, grind the EBSD calibration surface of the sample block with 120# and 800# sandpaper in turn, and then rinse it with water;

[0034] Then, use absorbent cotton to dip the EBSD calibration surface of the zirconium sample block to wipe the chemical polishing agent for 20s. The chemical polishing agent is a mixture of lactic acid solution, nitric acid solution and hydrofluoric acid solution, wherein the lactic acid solution: nitric acid Solution: the volume ratio of the hydrofluoric acid solution is 45%: 40%: 15%, and the mass percent of lactic acid in the lactic acid solution is 90%, the mass percent of nitric acid in the nitric acid solution is 68%, and the hydrofluoric acid solution is 68%. The mass percent of the acid is 45%, all of which are analytically pure;

[0035] Finally, after wiping, quickly rinse with water and dry with cold air to obtain the Z...

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Abstract

The invention discloses a zirconium alloy EBSD sample preparation method, which comprises: cutting a zirconium alloy sample block, carrying out chemical polishing by using a chemical polishing agent formed by mixing a lactic acid solution, a nitric acid solution and a hydrofluoric acid solution, rinsing with water, and carrying out blow drying with cold wind to obtain the zirconium alloy EBSD sample. According to the present invention, with the preparation method, the problems of complex process, long polishing time, poor effect and the like of the sample preparation technology in the prior art are solved; the preparation method of the present invention is suitable for the preparation of various zirconium alloy EBSD samples with any shapes and any sizes, has characteristics of less grinding step, simple and convenient chemical polishing operation and rapid and efficient sample preparation, and can be used at the room temperature; and the finally prepared sample has characteristics of real structure and good clarity, wherein the EBSD zirconium calibration rate is more than 90%.

Description

technical field [0001] The invention belongs to the technical field of sample preparation, in particular to a method for preparing a zirconium alloy EBSD sample. Background technique [0002] As a rare metal, zirconium has good corrosion resistance, moderate mechanical properties, and low thermal neutron absorption cross section (zirconium is 0.18×10 -28 piece / m 2 ), so it is widely used in aerospace, military industry, nuclear reaction, atomic energy, chemical industry and other fields. The crystal structure of zirconium is close-packed hexagonal and has strong anisotropy. Zirconium alloy pipes and plates will have a strong texture during processing, which will affect their physical properties. Studying the orientation of zirconium alloys is of great significance for in-depth understanding of the properties of zirconium alloys, and also plays a guiding role in optimizing the processing technology of zirconium alloys. [0003] Compared with the X-ray diffraction (XRD) tec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/32
Inventor 童龙刚卫新民张天广李刚李献军张梦霓佟昕昕陆玉华
Owner 国核锆铪理化检测有限公司
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