CN102998162A - Preparation method for metallographic sample of zirconium and zirconium alloy microstructures - Google Patents
Preparation method for metallographic sample of zirconium and zirconium alloy microstructures Download PDFInfo
- Publication number
- CN102998162A CN102998162A CN2012105370059A CN201210537005A CN102998162A CN 102998162 A CN102998162 A CN 102998162A CN 2012105370059 A CN2012105370059 A CN 2012105370059A CN 201210537005 A CN201210537005 A CN 201210537005A CN 102998162 A CN102998162 A CN 102998162A
- Authority
- CN
- China
- Prior art keywords
- zirconium
- sample
- grinding
- metallographic
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a preparation method for a metallographic sample of zirconium and zirconium alloy microstructures. The method comprises the following steps of pre-cleaning the metallographic sample; successively performing pre-grinding, rough-grinding and fine-grinding on the metallographic sample after the sample surface is cleaned; preparing a solution according to a volume ratio of H2O2 : HF : H2O of 0.8-1.2 : 1 : 2; wiping the sample surface for 30-40 seconds by using the solution; chemical-etching the sample without a scratch on the surface in a solution with the volume ratio of H2O2 : HF : H2O being 0.8-1.2 : 2 : 17 and with the etching time of 40-50 minutes; cleaning the etched sample; draining water; and performing metallographic observation and grain size evaluation. The microstructure diagrams of the zirconium and zirconium alloy have good effect, clear crystal grains, and are helpful for analysis and the grain size evaluation for the zirconium and zirconium alloy microstructures and intermetallic compound forms. The whole operation process is simple and a procedure is relatively short. The corrosivity for H2O2 solution is lower than that of HNO3, so that the method has small harm to health of an operator; equipment investment can be reduced; the quality and speed for sample preparation are increased; and the method is suitable for the analysis and the grain size evaluation for the zirconium and zirconium alloy microstructures.
Description
Technical field
The present invention relates to a kind of zirconium and zircaloy microstructure metallographic specimen preparation method, belong to Material Field.
Background technology
The reserves of zirconium in the earth's crust are about 0.025%-0.028% (massfraction), and also higher than the reserves of common elements nickel, copper, lead, zinc, the thermal neutron absorption cross section of zircaloy is little, and temperature conductivity is high, mechanical property good, have again good processing characteristics and same UO
2Compatibility is good, especially high-temperature water and high-temperature vapor is also had good etch resistant properties and enough heat resistances, so cladding materials and core structural material that zircaloy is widely used and makes the water-cooled power reactor become the important feature material of nuclear power station.
Zirconium has excellent corrosion resisting property and good thermal conductivity in many organic acids, mineral acid, highly basic and fuse salt, so zirconium and zircaloy also are corrosion resistance structure materials excellent in the chemical engineering.
Zirconium and zircaloy more and more are applied in the petrochemical equipment, its chemical property is active, very easily oxidized in air, form the oxide film of one deck densification, this layer oxide film also is the key point that zircaloy has excellent anticorrosive performance, and it can stop zircaloy to continue to contact with corrosive medium, and then its corrosion stability is increased, and the self-repairing capability of this layer oxide film is very strong, can form at once new oxide film after the Mechanical Crushing.
Because zirconium and zircaloy chemical property are active, the oxide film that the surface forms is very fine and close, adopts conventional metallography preparation step: corase grind-fine grinding-polishing-corrosion-cleaning, dewater, can't reach the purpose of clear observation zirconium and zircaloy micromechanism and tissue.The lot of experiments discovery, the oxide film of zirconium and zircaloy surface compact is strengthened and stablized to traditional polishing step, stops the effect of further bright sample, often through making on the contrary brightness effect decline after the long-time polishing, affected follow-up chemical etching.
The etchant etch is adopted in the sample mechanical buffing to grinding before etch of conventional metallography preparation process need afterwards again.Zirconium and zircaloy as activity very strong metal arranged, especially can react at a terrific speed with oxygen under the moistening external environment at normal temperatures, generate the form compact and stable oxide film of one deck and invest alloy surface, the mechanical buffing of laboratory routine is selected the less diamond abrasive of granularity to dissolve in and is formed suspending liquid in the water.The mechanical buffing mode of this routine prepares successful to most of metal metallographic specimen, but for zirconium and the very strong non-ferrous metal of this activity of zircaloy, can make rapidly the oxide film of its Surface Creation densification, thereby hinders the removal of specimen surface deformation layer.If adopt electropolishing to form the film that one deck has high electrical resistance at original rugged specimen surface by electrolytic buffing attachment shown in Figure 1, the sample bossing is thinner than recessed part, the thinner resistance of film is less, current density is larger, dissolving metal speed is just faster, thereby make bossing gradually smooth, obtain at last smooth even curface.But the method device is complicated, and the time is long, and for specimen size restricted.Feverfew is beautiful, and the mode that Xiao Lin, the people such as Xue Xiangyi adopt mechanical buffing and chemical polishing to combine in document " preparation of zirconium zirconium and microstructure of the alloy and scanning electron microscope analysis sample " prepares the zircaloy metallographic specimen, and the principal ingredient of etchant is HF and HNO
3, this metallography preparation mode long flow path, high to equipment requirement, be unsuitable for microstructure observation and the evaluation of working-yard, and HNO
3Be the severe corrosive solvent, long period of operation is larger to operating personnel's health hazard.
Summary of the invention
This patent is to provide a kind of zirconium and the new metallographic specimen preparation method of zircaloy, improves zirconium and zircaloy metallographic specimen preparation quality and speed, with and the accuracy of microstructure further investigation, and can realize that engineering uses.
The technical solution that realizes the object of the invention effect is: the preparation method of a kind of zirconium and zircaloy metallographic specimen, and its process is as follows:
1 pre-service: metallographic specimen is carried out prerinse, after specimen surface is bright and clean, carry out successively the pre-grinding of metallographic specimen, slightly grind and lappingout;
2 stripings: H by volume
2O
2: HF:H
2O=0.8-1.2:1:2 carries out solution allocation, with this solution in specimen surface wiping about 30-40 second;
3 etches: it is H that the sample of surperficial no marking is placed volume ratio
2O
2: HF:H
2Carry out chemical etching in the solution of O=0.8-1.2:2:17, the etch time is 40-50 second;
Can carry out metallographic observation and grain size evaluation after 4 cleanings, the dehydration.
Prerinse described in the step 1 is to adopt acetone to remove the greasy dirt of specimen surface, and described pre-grinding, corase grind and correct grinding carry out at the abrasive paper for metallograph of 240#, 400# and 600# respectively.
The advantage of patent of the present invention: the zirconium and the zircaloy micro-organization chart that use the said method preparation are respond well, and crystal grain is clear, are conducive to analysis and the grain size evaluation of zirconium and zircaloy microstructure and morphology of intermetallic compound.Whole operating process is easy, and flow process is shorter, H
2O
2The corrosivity of solution is than HNO
3Low, little to operating personnel's health hazard, can reduce equipment investment simultaneously, improve sample quality and speed, be applicable to the evaluation of working-yard zirconium and zircaloy Analysis on Microstructure and grain size.
Description of drawings
Fig. 1 is prior art electrolytic buffing attachment schematic diagram.
Fig. 2 is patent etch principle schematic of the present invention.
Fig. 3 is example of the present invention 1 metallographic specimen micro-organization chart.
Fig. 4 is example of the present invention 2 metallographic specimen micro-organization charts.
Fig. 5 is example of the present invention 3 metallographic specimen micro-organization charts.
Fig. 6 is Comparative Examples metallographic specimen of the present invention micro-organization chart.
Embodiment
Principle Action Specification of the present invention is as follows: by the etchant effect of two kinds of different proportionings, the first etchant can be removed the oxidation deformation layer that the polishing operation stays as early as possible, makes more smooth of surface; The second etchant can evenly immerse the crystal boundary of phase structure fast, very clearly manifests the form of micro structure.
The chemical etching prescription that the described zirconium of patent of the present invention and zircaloy are new is two kinds of etchants with the different proportionings of prescription.Because zirconium and the not corrosion of the reagent of anti-HF of zircaloy, therefore select HF that zircaloy surface compact oxide film is removed, after the dense oxidation film that HF forms zircaloy surface is removed, so that outside the specimen surface high spot was exposed to, these lug boss branches were preferentially by strong oxidising agent H
2O
2Oxidation, the oxide of generation and HF reaction also are removed, and finally obtain the specimen surface of smooth cleaning.Its schematic diagram is called the striping step that zirconium and zircaloy microscopic sample are made as shown in Figure 2.Because after grinding, cut, the deformation layer of specimen surface are more, so improve HF and H
2O
2Proportioning, its proportioning is H
2O
2: HF:H
2O=0.8-1.2:1:2 guarantees that the protrusion of specimen surface is thoroughly removed.
Chemical etching is the sample flour milling etch certain hour in chemical mordant with smooth cleaning, thereby demonstrates the tissue of sample, because atomic arrangement is irregular on the crystal boundary, has higher free energy, so grain boundaries is vulnerable to corrosion and presents chase.When zirconium and zircaloy carry out chemical etching, remove the oxide film of specimen surface by HF, so that H
2O
2Can the etch crystal boundary, thus the crystal boundary of phase structure can evenly be immersed fast at microscopically, very clearly manifest the form of zirconium and zircaloy micro structure.When the selective reagent proportioning, should suitably reduce H
2O
2Relative content, its proportioning is H
2O
2: HF:H
2O=0.8-1.2:2:17 is so that be difficult for the corrosion over-education phenomenon in the chemical corrosion process.
The preparation process that is exclusively used in zirconium and zircaloy metallographic specimen described in the present invention is as follows:
1 cleans: metallographic specimen is carried out prerinse, remove the greasy dirt on surface with acetone, make specimen surface bright and clean;
2 pre-grinding: with sample pre-grinding on the abrasive paper for metallograph of 240#, until the sample cut is till same direction;
3 slightly grind: with sample mechanical lapping on the abrasive paper for metallograph of 400#, grind the grinding perpendicular direction of direction and step 2, until sample cut direction is till same direction;
4 lappingouts: with sample mechanical lapping on the abrasive paper for metallograph of 600#, grind the grinding perpendicular direction of direction and step 3, until the cut direction in the same direction till;
5 stripings: carry out solution allocation, H by following volume ratio
2O
2: HF:H
2O=0.8-1.2:1:2, with this solution in the about 20-40 after second of specimen surface wiping, the very bright cleaning of specimen surface;
6 etches: it is H that the sample of surperficial no marking is placed volume ratio
2O
2: HF:H
2Carry out chemical etching in the solution of O=0.8-1.2:2:17, the etch time is 40-50 second;
Can carry out metallographic observation and grain size evaluation after 7 cleanings, the dehydration.
Embodiment 1:
Prepare the zircaloy metallographic specimen and carry out microstructure observation by the process of being prepared as follows, as shown in Figure 3.
1 cleans: metallographic specimen is carried out prerinse, remove the greasy dirt on surface with acetone, make specimen surface bright and clean;
2 pre-grinding: with sample pre-grinding on the abrasive paper for metallograph of 240#, until the sample cut is till same direction;
3 slightly grind: with sample mechanical lapping on the abrasive paper for metallograph of 400#, grind the grinding perpendicular direction of direction and step 2, until sample cut direction is till same direction;
4 lappingouts: with sample mechanical lapping on the abrasive paper for metallograph of 600#, grind the grinding perpendicular direction of direction and step 3, until the cut direction in the same direction till;
5 stripings: carry out solution allocation, H by following volume ratio
2O
2: HF:H
2O=0.8:1:2.With mentioned solution in the specimen surface wiping approximately after 20 seconds, the very bright cleaning of specimen surface;
6 etches: it is H that the sample of surperficial no marking is placed volume ratio
2O
2: HF:H
2Carry out chemical etching in the solution of O=0.8:2:17, the etch time was 40 seconds;
Can carry out metallographic observation and grain size evaluation after 7 cleanings, the dehydration.
Embodiment 2
Prepare the zircaloy metallographic specimen and carry out microstructure observation by the process of being prepared as follows, as shown in Figure 4.
1 cleans: metallographic specimen is carried out prerinse, remove the greasy dirt on surface with acetone, make specimen surface bright and clean;
2 pre-grinding: with sample pre-grinding on the abrasive paper for metallograph of 240#, until the sample cut is till same direction;
3 slightly grind: with sample mechanical lapping on the abrasive paper for metallograph of 400#, grind the grinding perpendicular direction of direction and step 2, until sample cut direction is till same direction;
4 lappingouts: with sample mechanical lapping on the abrasive paper for metallograph of 600#, grind the grinding perpendicular direction of direction and step 3, until the cut direction in the same direction till;
5 stripings: carry out solution allocation, H by following volume ratio
2O
2: HF:H
2O=1:1:2.With mentioned solution in the specimen surface wiping approximately after 30 seconds, the very bright cleaning of specimen surface;
6 etches: it is H that the sample of surperficial no marking is placed volume ratio
2O
2: HF:H
2Carry out chemical etching in the solution of O=1:2:17, the etch time was 45 seconds;
Can carry out metallographic observation and grain size evaluation after 7 cleanings, the dehydration.
Embodiment 3
Prepare the zircaloy metallographic specimen and carry out microstructure observation by the process of being prepared as follows, as shown in Figure 5.
1 cleans: metallographic specimen is carried out prerinse, remove the greasy dirt on surface with acetone, make specimen surface bright and clean;
2 pre-grinding: with sample pre-grinding on the abrasive paper for metallograph of 240#, until the sample cut is till same direction;
3 slightly grind: with sample mechanical lapping on the abrasive paper for metallograph of 400#, grind the grinding perpendicular direction of direction and step 2, until sample cut direction is till same direction;
4 lappingouts: with sample mechanical lapping on the abrasive paper for metallograph of 600#, grind the grinding perpendicular direction of direction and step 3, until the cut direction in the same direction till;
5 stripings: carry out solution allocation, H by following volume ratio
2O
2: HF:H
2O=1.2:1:2.With mentioned solution in the specimen surface wiping approximately after 40 seconds, the very bright cleaning of specimen surface;
6 etches: it is H that the sample of surperficial no marking is placed volume ratio
2O
2: HF:H
2Carry out chemical etching in the solution of O=1.2:2:17, the etch time was 50 seconds;
Can carry out metallographic observation and grain size evaluation after 7 cleanings, the dehydration.
Comparative Examples:
Prepare the zircaloy metallographic specimen and carry out microstructure observation by the process of being prepared as follows, as shown in Figure 6.
1 cleans: metallographic specimen is carried out prerinse, remove the greasy dirt on surface with acetone, make specimen surface bright and clean;
2 pre-grinding: with sample pre-grinding on the abrasive paper for metallograph of 240#, until the sample cut is till same direction;
3 slightly grind: with sample mechanical lapping on the abrasive paper for metallograph of 400#, grind the grinding perpendicular direction of direction and step 2, until sample cut direction is till same direction;
4 lappingouts: with sample mechanical lapping on the abrasive paper for metallograph of 600#, grind the grinding perpendicular direction of direction and step 3, until the cut direction in the same direction till;
5 mechanical buffinges: at Al
2O
3Add the approximately CrO about 10wt% in the Polishing Powder solution
3Solution, and carry out mechanical buffing;
6 chemical polishings: be HNO in volume ratio with sample after the above-mentioned mechanical buffing
3: HF:H
2Chemical polishing 4min in the solution of O=45:5:50;
7 chemical etchings: it is HNO that the sample after will polishing places volume ratio
3: HF:H
2Carry out chemical etching in the solution of O=45:20:35, the etch time was 60 seconds;
Can carry out metallographic observation and grain size evaluation after 8 cleanings, the dehydration.
From instance graph 3-5 and Comparative Examples Fig. 6, can significantly find out, micro-organization chart's crystal grain rule that zirconium of the present invention and zircaloy metallography preparation method are prepared is clear, disperse is also high-visible in the second-phase intermetallic compound of matrix surface, can carry out grain size evaluation and Analysis on Microstructure, but micro-organization chart's crystal boundary that the metallography preparation method described in the Comparative Examples is prepared is fuzzy, only have individual die can demonstrate complete crystal boundary, therefore the evaluation and the Analysis on Microstructure that are unfavorable for grain size, and consuming time longer, after measured, approximately 10 minutes consuming time of the described preparation method of patent of the present invention, and 45 minutes consuming time of the preparation method described in the Comparative Examples.
Claims (2)
1. a zirconium and zircaloy microstructure metallographic specimen preparation method is characterized in that said method comprising the steps of:
Step 1 pre-service: metallographic specimen is carried out prerinse, after specimen surface is bright and clean, carry out successively the pre-grinding of metallographic specimen, slightly grind and lappingout;
Step 2 striping: H by volume
2O
2: HF:H
2O=0.8-1.2:1:2 carries out solution allocation, with this solution in specimen surface wiping about 30-40 second;
Step 3 etch: it is H that the sample of surperficial no marking is placed volume ratio
2O
2: HF:H
2Carry out chemical etching in the solution of O=0.8-1.2:2:17, the etch time is 40-50 second;
After cleaning, dewater, step 4 can carry out metallographic observation and grain size evaluation.
2. zirconium according to claim 1 and zircaloy microstructure metallographic specimen preparation method, it is characterized in that the prerinse described in the step 1 is to adopt acetone to remove the greasy dirt of specimen surface, described pre-grinding, corase grind and correct grinding carry out at the abrasive paper for metallograph of 240#, 400# and 600# respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105370059A CN102998162A (en) | 2012-12-13 | 2012-12-13 | Preparation method for metallographic sample of zirconium and zirconium alloy microstructures |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105370059A CN102998162A (en) | 2012-12-13 | 2012-12-13 | Preparation method for metallographic sample of zirconium and zirconium alloy microstructures |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102998162A true CN102998162A (en) | 2013-03-27 |
Family
ID=47927015
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105370059A Pending CN102998162A (en) | 2012-12-13 | 2012-12-13 | Preparation method for metallographic sample of zirconium and zirconium alloy microstructures |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102998162A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102809500A (en) * | 2012-05-25 | 2012-12-05 | 中国航空工业集团公司北京航空材料研究院 | Method for rapidly preparing Ni-based superalloy electron backscatter diffraction sample |
| CN103668205A (en) * | 2013-12-04 | 2014-03-26 | 湖南理工学院 | Etchant used for displaying the internal microstructure of Zr-Al-Ni-Cu amorphous alloy |
| CN104535394A (en) * | 2015-01-19 | 2015-04-22 | 湖南大学 | Preparation method of metallographic samples of zirconium and zirconium alloy |
| CN105092580A (en) * | 2015-07-14 | 2015-11-25 | 西部金属材料股份有限公司 | Observation method for industrial pure zirconium microstructure |
| CN106932257A (en) * | 2015-12-30 | 2017-07-07 | 中核北方核燃料元件有限公司 | A kind of uranium zircaloy metallographic engraving method |
| CN107607383A (en) * | 2017-07-26 | 2018-01-19 | 国核锆铪理化检测有限公司 | A kind of zircaloy EBSD preparation method of sample |
| CN107863161A (en) * | 2017-10-31 | 2018-03-30 | 岭澳核电有限公司 | Zirconium alloy cladding surface treatment method and zirconium alloy cladding |
| CN109060857A (en) * | 2018-05-23 | 2018-12-21 | 中国科学院金属研究所 | A kind of zircaloy the second phase corrosive agent and caustic solution |
| CN111118440A (en) * | 2019-03-07 | 2020-05-08 | 苏州微创关节医疗科技有限公司 | Zirconium alloy treatment method and application |
| CN111778507A (en) * | 2020-07-07 | 2020-10-16 | 贵州大学 | Metallographic corrosive liquid and preparation method thereof |
| CN113340698A (en) * | 2021-06-24 | 2021-09-03 | 北京工业大学 | Etchant for zirconium alloy metallographic structure observation and method for preparing zirconium alloy metallographic sample |
| CN114509460A (en) * | 2022-02-18 | 2022-05-17 | 中国核动力研究设计院 | Pretreatment method for zirconium alloy scanning electron microscope sample before neutron irradiation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880881A (en) * | 2010-06-13 | 2010-11-10 | 西南大学 | High aluminum zinc alloy etching agent and use method thereof |
| CN102486994A (en) * | 2010-12-02 | 2012-06-06 | 有研半导体材料股份有限公司 | Silicon wafer cleaning process |
| CN102809500A (en) * | 2012-05-25 | 2012-12-05 | 中国航空工业集团公司北京航空材料研究院 | Method for rapidly preparing Ni-based superalloy electron backscatter diffraction sample |
-
2012
- 2012-12-13 CN CN2012105370059A patent/CN102998162A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880881A (en) * | 2010-06-13 | 2010-11-10 | 西南大学 | High aluminum zinc alloy etching agent and use method thereof |
| CN102486994A (en) * | 2010-12-02 | 2012-06-06 | 有研半导体材料股份有限公司 | Silicon wafer cleaning process |
| CN102809500A (en) * | 2012-05-25 | 2012-12-05 | 中国航空工业集团公司北京航空材料研究院 | Method for rapidly preparing Ni-based superalloy electron backscatter diffraction sample |
Non-Patent Citations (1)
| Title |
|---|
| 白菊丽 等: "锆及锆合金金相及扫描电镜分析样品的制备", 《理化检验-物理分册》, vol. 34, no. 3, 31 March 1998 (1998-03-31) * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102809500A (en) * | 2012-05-25 | 2012-12-05 | 中国航空工业集团公司北京航空材料研究院 | Method for rapidly preparing Ni-based superalloy electron backscatter diffraction sample |
| CN103668205B (en) * | 2013-12-04 | 2018-06-22 | 湖南理工学院 | A kind of corrosive liquid for showing Zr-Al-Ni-Cu non-crystaline amorphous metal internal microstructures |
| CN103668205A (en) * | 2013-12-04 | 2014-03-26 | 湖南理工学院 | Etchant used for displaying the internal microstructure of Zr-Al-Ni-Cu amorphous alloy |
| CN104535394A (en) * | 2015-01-19 | 2015-04-22 | 湖南大学 | Preparation method of metallographic samples of zirconium and zirconium alloy |
| CN105092580A (en) * | 2015-07-14 | 2015-11-25 | 西部金属材料股份有限公司 | Observation method for industrial pure zirconium microstructure |
| CN106932257A (en) * | 2015-12-30 | 2017-07-07 | 中核北方核燃料元件有限公司 | A kind of uranium zircaloy metallographic engraving method |
| CN107607383A (en) * | 2017-07-26 | 2018-01-19 | 国核锆铪理化检测有限公司 | A kind of zircaloy EBSD preparation method of sample |
| CN107863161A (en) * | 2017-10-31 | 2018-03-30 | 岭澳核电有限公司 | Zirconium alloy cladding surface treatment method and zirconium alloy cladding |
| CN109060857A (en) * | 2018-05-23 | 2018-12-21 | 中国科学院金属研究所 | A kind of zircaloy the second phase corrosive agent and caustic solution |
| CN109060857B (en) * | 2018-05-23 | 2021-01-26 | 中国科学院金属研究所 | Zirconium alloy second phase corrosive agent and corrosion method |
| CN111118440A (en) * | 2019-03-07 | 2020-05-08 | 苏州微创关节医疗科技有限公司 | Zirconium alloy treatment method and application |
| CN111118440B (en) * | 2019-03-07 | 2022-03-04 | 苏州微创关节医疗科技有限公司 | Zirconium alloy treatment method and application |
| CN111778507A (en) * | 2020-07-07 | 2020-10-16 | 贵州大学 | Metallographic corrosive liquid and preparation method thereof |
| CN113340698A (en) * | 2021-06-24 | 2021-09-03 | 北京工业大学 | Etchant for zirconium alloy metallographic structure observation and method for preparing zirconium alloy metallographic sample |
| CN114509460A (en) * | 2022-02-18 | 2022-05-17 | 中国核动力研究设计院 | Pretreatment method for zirconium alloy scanning electron microscope sample before neutron irradiation |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102998162A (en) | Preparation method for metallographic sample of zirconium and zirconium alloy microstructures | |
| CN104535394A (en) | Preparation method of metallographic samples of zirconium and zirconium alloy | |
| CN106757299B (en) | A kind of the electrobrightening corrosive agent and its application method of nickel-base alloy metallographic structure | |
| Schuler et al. | Polymer electrolyte water electrolysis: correlating porous transport layer structural properties and performance: Part I. Tomographic analysis of morphology and topology | |
| JP3925867B2 (en) | Method for manufacturing a silicon substrate with a porous layer | |
| CN102383130B (en) | Observation method for metallographic structures of amorphous alloys | |
| CN101368889A (en) | Method for displaying high-strength vessel slab original austenite crystal grain | |
| CN101806684B (en) | Specimen preparation and organization exposure method of metallic phase of zinc and alloy thereof | |
| CN101655426B (en) | Electrochemical metallographic etching method universal for nickel-based alloys | |
| CN103364253B (en) | A kind of bimetal joint interface metallographic structure corrosion reagent and display packing | |
| CN101788413B (en) | Method for preparing lead and lead alloy metallic phase samples and exposing texture | |
| CN109060857B (en) | Zirconium alloy second phase corrosive agent and corrosion method | |
| CN102519776A (en) | Metallographic corrosive, corrosion method for tungsten and display method for metallographic structure of tungsten | |
| CN109459455A (en) | A kind of electrochemical etching method for observing zircaloy nano-second-phase | |
| CN105002498A (en) | GH625 high-temperature alloy metallographic etchant and preparation and application method thereof | |
| CN107462456A (en) | Method for displaying metallographic structure | |
| CN109457245A (en) | A kind of wrought aluminium alloy grain boundary corrosion agent and the preparation method and application thereof for processing state | |
| CN105261491B (en) | A kind of preparation method of the porous nickel nickel compound electric pole piece of flexible nano | |
| CN103900889A (en) | Chemical polishing method for electrical silicon steel EBSD (electron back-scattered diffraction) sample | |
| CN106908302A (en) | A kind of Surface Roughness of Pure Titanium Castings and titanium alloy metallographic specimen mechanical polishing method for making sample | |
| CN104677715A (en) | Method for recording and observing corrosion behavior of magnesium alloy microstructure in situ | |
| Liu et al. | Extrinsic parting limit for dealloying of Cu-Rh | |
| CN103940747A (en) | Method for observing TA7 titanium alloy metallographic structure | |
| CN107957419B (en) | Observation method of industrial pure hafnium metallographic structure | |
| CN106676619A (en) | Method for preparing metal glass nano porous structure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130327 |