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Preparation method for as-cast lead or lead alloy EBSD sample

A lead alloy and sample technology, applied in the field of EBSD sample preparation, can solve the problems of incomplete display, unable to display grains, small grain size, etc., and achieve the effect of less passes, real sample structure and high calibration rate.

Active Publication Date: 2014-07-09
GRIMAT ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The grain size of the deformed and deformed recrystallized lead and lead alloy samples is small, and the shape of each grain can be clearly displayed by metallographic microscopy / scanning electron microscopy / EBSD technology and the average grain size of the sample can be accurately estimated However, the grain size of as-cast lead and lead alloys is relatively large, and a complete grain cannot be displayed at the minimum magnification, resulting in the inability to fully display the shape of each grain and accurately estimate the as-cast lead and lead alloy samples. The average grain size of

Method used

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  • Preparation method for as-cast lead or lead alloy EBSD sample
  • Preparation method for as-cast lead or lead alloy EBSD sample
  • Preparation method for as-cast lead or lead alloy EBSD sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Cut a sample from the cast pure lead ingot, and the sample is processed as follows:

[0033] a. Manual grinding: use 800# Al 2 o 3 Water sandpaper is used to polish the surface to be tested of the cast pure lead sample until the surface to be tested is smooth;

[0034] b. Chemical polishing 1: Add H dropwise on the surface of the pure lead sample to be tested with a rubber dropper 2 o 2 and CH 3 COOH volume ratio is 0.8:1 chemical polishing solution I, rinse with deionized water while adding dropwise, until no black / gray product is generated on the surface of the sample to be tested;

[0035] c. Chemical polishing 2: drop H on the surface to be tested of the cast lead sample treated in step b with a rubber dropper 2 o 2 and CH 3 Chemical polishing solution II with a volume ratio of COOH of 0.1:0.9, rinse with deionized water for 0.5 min while adding it dropwise, to make the surface of the sample to be tested bright;

[0036] d. Erosion: Add citric acid and ammon...

Embodiment 2

[0038] Cut a sample from the ingot of as-cast Pb-0.6%Ag alloy (in this as-cast lead-silver alloy sample, the content of Ag is 0.6% by weight, and the balance is Pb), and the sample is processed as follows:

[0039] a. Manual grinding: use 800# Al 2 o 3 Water sandpaper is used to polish the surface to be tested of the as-cast Pb-0.6%Ag alloy sample until the surface to be tested is flat;

[0040] b. Chemical polishing 1: Add H dropwise on the surface of the cast Pb-0.6% Ag sample to be tested with a rubber dropper 2 o 2 and CH 3 COOH volume ratio is 1.2:0.8 chemical polishing solution I, rinse with deionized water while adding dropwise, until no black / gray product is generated on the surface of the sample to be tested;

[0041] c. Chemical polishing 2: Add H dropwise on the surface to be tested of the cast Pb-0.6%Ag sample treated in step b with a dropper 2 o 2 and CH 3 Chemical polishing solution II with a volume ratio of COOH of 0.05:0.95, rinse with deionized water fo...

Embodiment 3

[0044] From the as-cast Pb-0.2%Ag-0.08%Ca-0.05%Sr alloy ingot (in this cast lead-silver-calcium-strontium alloy sample, the content of Ag is 0.2% by weight, the content of Ca is 0.08% by weight, and the content of Sr is 0.05% by weight, and the balance is Pb), a sample is cut out, and the sample is processed as follows:

[0045] a. Manual grinding: use 800# Al 2 o 3 Water sandpaper is used to grind the surface to be tested of the cast lead-silver-calcium-strontium alloy sample until the surface to be tested is flat;

[0046] b. Chemical polishing 1: Add H dropwise on the surface of the cast Pb-0.2%Ag-0.08%Ca-0.05%Sr alloy sample to be tested with a rubber dropper 2 o 2 and CH 3 COOH volume ratio is 0.8:1.2 chemical polishing solution I, rinse with deionized water while adding dropwise, until no black / gray product is generated on the surface of the sample to be tested;

[0047] c. Chemical polishing 2: Use a rubber dropper to drop H on the surface to be tested of the cast ...

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Abstract

The invention relates to a preparation method for an as-cast lead or lead alloy EBSD (electron back-scattered diffraction) sample. The method includes: manual polishing: using waterproof abrasive paper to polish a to-be-tested surface of the as-cast lead or lead alloy sample; chemical polishing 1: adding a chemical polishing solution composed of H2O2 and CH3COOH in a volume ratio of 0.8-1.2:0.8-1.2 to the to-be-tested surface dropwise; chemical polishing 2: then adding a chemical polishing solution composed of H2O2 and CH3COOH in a volume ratio of 0.05-0.2:0.8-0.95 to the to-be-tested surface dropwise; erosion: covering the sample surface by an erosion solution composed of citric acid, ammonium molybdate and deionized water in a weight ratio of 10-20:6-12:60-150, then soaking the sample in alcohol for 5-10 seconds, then taking the sample out and blowing it dry, thus obtaining the sample that can display Kikuchi lines through the electron back-scattered diffraction technology. The sample preparation method is simple in operation, and the prepared sample has real texture and a high back-scattered electron diffraction pattern calibration rate.

Description

technical field [0001] The invention relates to the technical field of EBSD (electron backscattering diffraction analysis technology) sample preparation, in particular to a method for preparing cast lead / lead alloy EBSD samples. Background technique [0002] Due to the low hardness of lead, lead and its alloys are very soft, and will deform under low pressure. When using traditional methods to prepare metallographic samples of lead and lead alloys, large surface flow and deformation will occur during grinding and polishing. , if the deformed layer is not completely removed, the real tissue will be covered, resulting in false images, which will bring difficulties to the preparation of metallographic samples. During the grinding process, the embedding of abrasive grains on the surface of the sample should be avoided as much as possible, so as to obtain the real tissue. The grain size of the deformed and deformed recrystallized lead and lead alloy samples is small, and the sha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/32C23F3/06
Inventor 袁学韬吕旭东雷扬华志强王磊李弢
Owner GRIMAT ENG INST CO LTD
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