CN114689411A - Preparation method of Zr-4 alloy welding metallographic sample - Google Patents
Preparation method of Zr-4 alloy welding metallographic sample Download PDFInfo
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- CN114689411A CN114689411A CN202011590677.7A CN202011590677A CN114689411A CN 114689411 A CN114689411 A CN 114689411A CN 202011590677 A CN202011590677 A CN 202011590677A CN 114689411 A CN114689411 A CN 114689411A
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- sample
- alloy welding
- metallographic sample
- preparation
- alloy
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 25
- 239000000956 alloy Substances 0.000 title claims abstract description 25
- 238000003466 welding Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005498 polishing Methods 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 244000137852 Petrea volubilis Species 0.000 claims abstract 2
- 238000000227 grinding Methods 0.000 claims description 12
- 229920000742 Cotton Polymers 0.000 claims description 4
- 239000000243 solution Substances 0.000 description 8
- 229910001093 Zr alloy Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 229910052770 Uranium Inorganic materials 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- CMDGQTVYVAKDNA-UHFFFAOYSA-N propane-1,2,3-triol;hydrate Chemical compound O.OCC(O)CO CMDGQTVYVAKDNA-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of metallographic sample preparation, and particularly relates to a preparation method of a Zr-4 alloy welding metallographic sample. The surface of a metallographic sample welded by the Zr-4 alloy is polished by water sand paper, and then nitric acid with volume ratio: hydrofluoric acid: glycerol 9: 2: and (10) carrying out chemical polishing by using the chemical polishing solution until the surface of the sample is bright and has no scratch. By adopting the method, the weld joint structure displayed by the polished Zr-4 alloy welding metallographic sample is clear, and the authenticity and the reproducibility are realized.
Description
Technical Field
The invention belongs to the technical field of metallographic sample preparation, and particularly relates to a preparation method of a Zr-4 alloy welding metallographic sample.
Background
Zirconium has excellent nuclear properties and has a thermal neutron absorption cross-section of only 0.18X 10-28m2Second to beryllium (0.009X 10)-28m2) And magnesium (0.06X 10)-28m2) 0.22X 10 of pure aluminum-28m2And (4) approaching. The thermal neutron absorption cross section of zirconium alloys such as Zr-2, Zr-4, Zr-1Nb, etc. is only (0.20-0.24) x 10-28m2It is the consideration of neutron economy that has promoted the research and development of zirconium alloy. The zirconium alloy is used as the structural material of the nuclear reactor instead of stainless steel, so that the uranium burnup can be saved by about 1/2. The zirconium and uranium have good compatibility, the zirconium alloy has good corrosion resistance in high-temperature and high-pressure water and steam at the temperature of 300-400 ℃, and has quite good neutron irradiation resistance in the reactor. The zirconium alloy also has moderate mechanicsPerformance and good processability. And thus has been commonly used as a fuel cladding and structural material for nuclear power water-cooled reactors. In China, a plurality of documents mention that corrosion solutions of zirconium alloy microstructure are mixed solutions of nitric acid, hydrofluoric acid and water, and in actual work, the corrosion solution is found to be a mixed solution of nitric acid: hydrofluoric acid: water 9: 2: the 9 (volume ratio) mixed solution has violent chemical reaction when being used for chemical polishing, and is easy to be polished during the polishing process to generate black spots on the surface of a sample, thereby causing false images. Therefore, proposals for improving the chemical polishing liquid have been made.
Disclosure of Invention
The invention aims to provide a preparation method of a metallographic sample for Zr-4 alloy welding, which comprises the following steps of mixing the following raw materials: hydrofluoric acid: water 9: 2: 9 (volume ratio) is improved so that the chemical reaction is slower in use and the false appearance of black spots is not generated.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a Zr-4 alloy welding metallographic sample comprises the steps of polishing the surface of a Zr-4 alloy welding metallographic sample by using waterproof abrasive paper, and then adopting nitric acid with a volume ratio of: hydrofluoric acid: glycerol 9: 2: and (10) carrying out chemical polishing by using the chemical polishing solution until the surface of the sample is bright and has no scratch.
The test specimens were cut longitudinally 1/2 with a wire-cut electrical discharge machine prior to grinding.
And grinding the longitudinal section of the sample by using 1200# SiC waterproof abrasive paper until the number of 2500# SiC waterproof abrasive paper, rotating the sample by 90 degrees every time when the number of 2500# SiC waterproof abrasive paper is replaced, and grinding the scratch of the previous pass.
And (5) polishing by using absorbent cotton.
The beneficial effects obtained by the invention are as follows:
a preparation method of a Zr-4 alloy welding metallographic sample comprises the following steps of: hydrofluoric acid: water (volume ratio) 9: 2: 9 (volume ratio) is changed into glycerol, so that the intensity of chemical reaction is reduced, and black spots are not easy to throw. By adopting the method, the weld joint structure displayed by the polished Zr-4 alloy welding metallographic sample can be clear, and the authenticity and the reproducibility are realized. The technology provides reliable detection guarantee for the test and production of the Zr-4 alloy welding process.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The invention aims to establish a preparation method of a metallographic sample of a Zr-4 alloy welding sample, wherein the Zr-4 alloy welding sample is ground and corroded in different passes, and the displayed microstructure has authenticity and reproducibility.
The technical scheme for realizing the purpose of the invention is as follows: the surface of a Zr-4 alloy welding sample is roughly ground by using No. 1200 waterproof abrasive paper to No. 2500 waterproof abrasive paper, and then nitric acid is adopted: hydrofluoric acid: glycerol 9: 2: and (3) performing chemical polishing by using 10 (volume ratio) of chemical polishing solution until the surface of the sample is bright and has no scratch.
The preparation method of the Zr-4 alloy welding metallographic phase sample comprises the following steps:
(1) cutting a sample: the weld sample was cut in the longitudinal direction 1/2 with a wire electric discharge machine.
(2) Coarse grinding: and grinding the longitudinal section of the sample by using 1200# SiC waterproof abrasive paper until the number of 2500# SiC waterproof abrasive paper, rotating the sample by 90 degrees every time when the number of 2500# SiC waterproof abrasive paper is replaced, and grinding the scratch of the previous pass.
(3) Polishing: wiping and polishing the coarsely ground sample by absorbent cotton soaked with chemical polishing solution, wherein the polishing solution is as follows: nitric acid: hydrofluoric acid: glycerol 9: 2: 10 (volume ratio) until the surface of the sample is bright and has no scratch.
The preparation method of the Zr-4 alloy welding metallographic phase sample comprises the following steps:
(1) cutting a sample: the weld sample was cut in the longitudinal direction 1/2 with a wire electric discharge machine.
(2) Coarse grinding: and grinding the longitudinal section of the sample by using 1200# SiC waterproof abrasive paper until the number of 2500# SiC waterproof abrasive paper, rotating the sample by 90 degrees every time when the number of 2500# SiC waterproof abrasive paper is replaced, and grinding the scratch of the previous pass.
(3) Polishing: wiping and polishing the coarsely ground sample by absorbent cotton soaked with chemical polishing solution, wherein the chemical polishing solution is nitric acid: hydrofluoric acid: glycerol 9: 2: 10 (volume ratio) until the surface of the sample is bright and has no scratch.
The invention discloses a preparation method of a Zr-4 alloy welding metallographic sample, which comprises the following steps of: hydrofluoric acid: water 9: 2: 9 (volume ratio) is changed into glycerol, and the ratio is increased, wherein the ratio of nitric acid: hydrofluoric acid: glycerol water ═ 9: 2: 10 (volume ratio), reduces the violent chemical reaction, and is not easy to throw to generate black spots. By adopting the method, the weld joint structure displayed by the polished Zr-4 alloy welding metallographic sample can be clear, and the authenticity and the reproducibility are realized. The technology provides reliable detection guarantee for the test and production of the Zr-4 alloy welding process.
Claims (4)
1. A preparation method of a Zr-4 alloy welding metallographic sample is characterized by comprising the following steps: the surface of a metallographic sample welded by the Zr-4 alloy is polished by water sand paper, and then nitric acid with volume ratio: hydrofluoric acid: glycerol 9: 2: and (10) carrying out chemical polishing by using the chemical polishing solution until the surface of the sample is bright and has no scratch.
2. The method for preparing the Zr-4 alloy welding metallographic sample according to claim 1, wherein the method comprises the following steps: the test specimens were cut longitudinally 1/2 with a wire-cut electrical discharge machine prior to grinding.
3. The method for preparing the Zr-4 alloy welding metallographic sample according to claim 2, wherein the method comprises the following steps: and grinding the longitudinal section of the sample by using 1200# SiC waterproof abrasive paper until the number of 2500# SiC waterproof abrasive paper, rotating the sample by 90 degrees every time when the number of 2500# SiC waterproof abrasive paper is replaced, and grinding the scratch of the previous pass.
4. The method for preparing the Zr-4 alloy welding metallographic sample according to claim 1, wherein the method comprises the following steps: and (5) polishing by using absorbent cotton.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011590677.7A CN114689411A (en) | 2020-12-29 | 2020-12-29 | Preparation method of Zr-4 alloy welding metallographic sample |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011590677.7A CN114689411A (en) | 2020-12-29 | 2020-12-29 | Preparation method of Zr-4 alloy welding metallographic sample |
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| Publication Number | Publication Date |
|---|---|
| CN114689411A true CN114689411A (en) | 2022-07-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011590677.7A Pending CN114689411A (en) | 2020-12-29 | 2020-12-29 | Preparation method of Zr-4 alloy welding metallographic sample |
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| Country | Link |
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| CN (1) | CN114689411A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115094422A (en) * | 2022-04-24 | 2022-09-23 | 西安西部新锆科技股份有限公司 | Beta-phase corrosive agent for zirconium/zirconium alloy, preparation method and corrosion method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB754188A (en) * | 1953-12-28 | 1956-08-01 | Gen Electric | Improvements relating to the surface finishing of zirconium and alloys thereof |
| JPS63195299A (en) * | 1987-02-09 | 1988-08-12 | Mitsubishi Metal Corp | Electrolytic solution for electropolishing zirconium and zirconium alloy |
| JPH07166280A (en) * | 1993-12-13 | 1995-06-27 | Sumitomo Metal Ind Ltd | Highly corrosion resistant zirconium alloy |
| CN104535394A (en) * | 2015-01-19 | 2015-04-22 | 湖南大学 | Preparation method of metallographic samples of zirconium and zirconium alloy |
-
2020
- 2020-12-29 CN CN202011590677.7A patent/CN114689411A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB754188A (en) * | 1953-12-28 | 1956-08-01 | Gen Electric | Improvements relating to the surface finishing of zirconium and alloys thereof |
| JPS63195299A (en) * | 1987-02-09 | 1988-08-12 | Mitsubishi Metal Corp | Electrolytic solution for electropolishing zirconium and zirconium alloy |
| JPH07166280A (en) * | 1993-12-13 | 1995-06-27 | Sumitomo Metal Ind Ltd | Highly corrosion resistant zirconium alloy |
| CN104535394A (en) * | 2015-01-19 | 2015-04-22 | 湖南大学 | Preparation method of metallographic samples of zirconium and zirconium alloy |
Non-Patent Citations (1)
| Title |
|---|
| 兰光友 等: "Zr-4合金包壳氢化样件的制备", 热加工工艺, vol. 45, no. 18, 30 September 2016 (2016-09-30), pages 87 - 89 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115094422A (en) * | 2022-04-24 | 2022-09-23 | 西安西部新锆科技股份有限公司 | Beta-phase corrosive agent for zirconium/zirconium alloy, preparation method and corrosion method thereof |
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