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Preparation method of metallographic samples of zirconium and zirconium alloy

A technology for metallographic samples and alloys, applied in the field of metallographic sample preparation of zirconium and zirconium alloys, can solve the problems of long-term exploration, easy environmental pollution by waste liquid, strict parameter requirements, etc. High-definition, low-tech effects

Inactive Publication Date: 2015-04-22
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Xu Yuelan, Wang Yang, Guo Hailing and others used a combination of chemical polishing and chemical corrosion to prepare zirconium alloy metallographic samples in the literature "Zirconium and Zirconium Alloy Microstructure Metallographic Preparation Method". The main components are HF and H 2 o 2 , but the test found that this method is only suitable for zirconium alloy samples with coarser grain size (>30μm), and the effect is not ideal for zirconium alloy samples with smaller grain size
[0005] In addition to traditional corrosion, metallographic samples can also be prepared by anodic coating, but because anodic coating is the same as electrolytic polishing, the required equipment is complicated, and the parameters of coating are strict and it takes a long time to explore
The sulfuric acid aqueous solution used for coating is highly corrosive, and the waste liquid produced after the experiment is also very easy to pollute the environment. After coating, polarized light observation is required, which greatly increases the requirements for observation equipment. Suitable for metallographic preparation in general laboratories and construction sites

Method used

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  • Preparation method of metallographic samples of zirconium and zirconium alloy
  • Preparation method of metallographic samples of zirconium and zirconium alloy
  • Preparation method of metallographic samples of zirconium and zirconium alloy

Examples

Experimental program
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Effect test

Embodiment 1

[0029] In this embodiment, the cold-rolled Zr-Sn-Nb-Fe alloy plate in the recrystallization annealed state is taken, and the metallographic sample of the zirconium alloy is prepared and observed according to the following preparation process, as follows: figure 2 Shown:

[0030] a. Sampling and cleaning: Sampling the plate, the size of the sample is 10mm×10mm, and ultrasonically cleaning the sample with acetone to remove surface oil;

[0031] b. Coarse grinding - fine grinding: Grind the cleaned sample on metallographic sandpaper. The grades of the sandpaper used are: 400#→800#→1200#→2000#→3000#. The grinding process requires a balanced force , when replacing sandpaper with different particle sizes, the grinding direction should be 90° to the direction of the wear marks of the previous sandpaper, and the next step should be performed after the previous wear marks are completely eliminated;

[0032] c. Chemical polishing: by volume ratio HF: HNO 3 :H 2 O=10:45:45 is carried...

Embodiment 2

[0036] The Zr-Sn-Nb-Fe alloy was kept at 650°C for 15 hours and quenched in water. The metallographic samples of the zirconium alloy were prepared and observed according to the following preparation process, as shown in image 3 Shown:

[0037] a. Sampling and cleaning: Sampling the plate, the size of the sample is 10mm×10mm, and ultrasonically cleaning the sample with acetone to remove the oil on the surface of the sample;

[0038] b. Coarse grinding - fine grinding: Grind the cleaned sample on metallographic sandpaper. The grades of sandpaper used are: 400#→800#→1200#→2000#→3000#. The grinding process requires a balanced force , when replacing the sandpaper with different particle sizes, the grinding direction should be 90° to the direction of the wear marks of the previous number one sandpaper, and the next step should be performed after the previous wear marks are completely eliminated;

[0039]c. Chemical polishing by volume ratio HF: HNO 3 :H 2 O=10:45:45 is carried o...

Embodiment 3

[0043] The Zr-Sn-Nb-Fe alloy was kept at 800°C for 40 minutes and quenched in water, and the metallographic sample of the zirconium alloy was prepared and observed according to the following preparation process, as shown in Figure 4 Shown:

[0044] a. Sampling and cleaning: Sampling the plate, the size of the sample is 10mm×10mm, and ultrasonically cleaning the sample with acetone to remove surface oil;

[0045] b. Coarse grinding - fine grinding: Grind the cleaned sample on metallographic sandpaper. The grades of the sandpaper used are: 400#→800#→1200#→2000#→3000#. The grinding process requires a balanced force , when replacing sandpaper with different particle sizes, the grinding direction should be 90° to the direction of the wear marks of the previous sandpaper, and the next step should be performed after the previous wear marks are completely eliminated;

[0046] c. Chemical polishing: by volume ratio HF: HNO 3 :H 2 O=10:45:45 is carried out solution preparation, dips...

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Abstract

The invention relates to a preparation method of metallographic samples of zirconium and zirconium alloy. The preparation method comprises the following steps: (a) sample pretreatment, namely sampling a to-be-tested material, ultrasonically cleaning to remove oil stain on the surface of a sample; (b) coarse grinding and fine grinding, namely grinding the sample processed in the step (a) on metallographic sand paper, wherein particle size marks of the utilized sand paper sequentially are 400#, 800#, 1200#, 2000# and 3000#; (3) chemical polishing, namely preparing a solution in a volume ratio that HF to HNO3 to H2O is 10 to 45 to 45, dipping the solution with an absorbent ball, and lightly wiping the surface of the sample with the absorbent ball for several times until the surface of the sample presents a polished surface as bright as a mirror; (d) cleaning, namely lightly wiping the surface of the polished sample in the step (c) by dipping absolute ethyl alcohol with the absorbent ball so as to remove complexes generated by chemical polishing; (e) oxidation cooling, namely dehydrating the cleaned sample, arranging the sample in a constant temperature region of a muffle furnace for oxidation for 2-10 minutes until the color of the surface of the sample is changed from bright white to faint yellow, taking out the sample, cooling, and carrying out metallographic observation and particle size evaluation.

Description

technical field [0001] The invention relates to a method for preparing metallographic samples of zirconium and zirconium alloys, belonging to the field of material detection. Background technique [0002] The content of zirconium in the earth's crust is 220g / t, ranking 20th in terms of abundance, surpassing nickel, zinc, copper, tin, lead and cobalt. Zirconium has excellent nuclear properties, and its thermal neutron absorption cross section is only 0.18×10 -28 m 2 , second only to beryllium (0.009×10 -28 m 2 ) and magnesium (0.06×10 -28 m 2 ), and 0.22×10 of pure aluminum -28 m 2 near. The thermal neutron absorption cross section of zirconium alloys such as Zr-2, Zr-4, Zr-1Nb, etc. is only (0.20~0.24)×10 -28 m 2 . It is precisely because of the consideration of neutron economy that the research and development of zirconium alloys are promoted. Using zirconium alloy instead of stainless steel as the structural material of nuclear reactor can save about 1 / 2 of ura...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
Inventor 张福全马永富周惦武
Owner HUNAN UNIV
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