CN113340698A - Etchant for zirconium alloy metallographic structure observation and method for preparing zirconium alloy metallographic sample - Google Patents
Etchant for zirconium alloy metallographic structure observation and method for preparing zirconium alloy metallographic sample Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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Abstract
An erosion agent for zirconium alloy metallographic structure observation and a method for preparing a zirconium alloy metallographic specimen belong to the field of metallographic preparation. The invention aims to solve the problem that the prior metallographic etching technology cannot obtain clear zirconium alloy grain boundaries. The erosion liquid consists of the following components: 20ml to 60ml of nitric acid, 10ml to 20ml of hydrofluoric acid, 10ml to 20ml of oxalic acid and 20ml to 60ml of distilled water. After the erosion of the metallographic specimen for 40-60 s by using the erosion solution, in order to make the metallographic phase clearer, the metallographic specimen is placed on an electric hot plate according to a metallographic thermopainting method, is placed in air and is rapidly heated to 400 ℃, and is kept for 8-15 minutes. The metallographic etchant in the method has simple preparation process and convenient preparation of metallographic samples, and can clearly observe the distribution of crystal boundaries and second phases of the zirconium alloy.
Description
Technical Field
The invention relates to an erosion agent for zirconium alloy metallographic structure observation and a method for preparing a zirconium alloy metallographic specimen, belonging to the field of metallographic preparation.
Background
Zirconium is a rare metal with an atomic number of 40, an average atomic mass of 91 and a density of 6.49g/cm3. The alloyed zirconium has the advantages of high mechanical strength, good ductility and processability, and corrosion resistance at high temperature, and is widely applied to the fields of nuclear industry, medical instruments and the like. In addition, the zirconium alloy has the advantages of low thermal neutron absorption cross section, excellent corrosion resistance, excellent high-temperature mechanical property and the like, and is a core structure material which is most widely applied including a nuclear power reactor fuel rod cladding material.
In the research and application of zirconium alloy, the microstructure type of the zirconium alloy needs to be observed and analyzed frequently, and then the components, the processing and the heat treatment process of the zirconium alloy are adjusted in time according to the analysis result; further, after welding of zirconium alloy, it is also necessary to analyze the structure of the welded joint to investigate the cause of the change in the properties. However, zirconium alloys have good corrosion resistance, and deep corrosion is often used in metallographic corrosion, which causes severe relief on the metallographic surface, which is not conducive to optical analysis, and the grain boundaries are difficult to distinguish.
Chinese patent CN111778507A discloses a metallographic etchant for zirconium alloy, which uses 8-12% hydrofluoric acid solution, 40-50% nitric acid solution, 4-8% hydrochloric acid solution and the balance water. And (3) dipping absorbent cotton into corrosive liquid to wipe the surface of the metallographic specimen for 20-30 times, flushing the corrosive liquid with water, and carrying out metallographic observation. By using the method, the metallographic structure picture of the zirconium alloy without recrystallization in thermal deformation can be clearly obtained, but the metallographic observation of the recrystallized isometric crystal has certain difficulty.
Chinese patent CN102998162A discloses a metallographic corrosion method for zirconium alloy, the volume ratio of which is H2O2:HF:H2Metallography of solution with O-0.8-1.2: 1:2Wiping the sample, removing the surface oxide film, and using the volume ratio of H2O2:HF:H2And chemically etching the solution with the O being 0.8-1.2:2:17 for 40-50 s, and cleaning and dehydrating to obtain the metallographic sample. The method is not easy to control the corrosion depth during corrosion, and imaging under an optical microscope has certain difficulty.
In addition to conventional chemical etching methods, electrolytic etching is also frequently used during metallographic etching of zirconium alloys. However, the parameters of the electrolytic polishing require a lot of experimental investigation, and the corrosion quality is not stable enough and is not easy to be mastered. And the perchloric acid solution needed by the electrolytic polishing solution has strong oxidizing property and corrosiveness, and has the danger of causing combustion and explosion when contacting or mixing with organic matters, reducing agents, inflammable substances and the like.
Disclosure of Invention
The invention provides an etchant for observing a metallographic structure of a zirconium alloy and a method for preparing a metallographic sample, which improve the quality of the metallographic preparation speed of the zirconium alloy and ensure the reliability of deep study on the microstructure.
The technical solution for realizing the effect of the invention is as follows: a method for preparing a metallographic specimen of zirconium alloy. The method comprises the following specific steps:
(1) pretreatment: pre-cleaning a metallographic sample, soaking the sample in a beaker filled with acetone, and placing the beaker in an ultrasonic cleaning machine for cleaning for more than 10 minutes to remove oil stains on the surface of the sample; after the surface of the sample is smooth, using metallographic abrasive paper to perform rough grinding, fine grinding and polishing on the metallographic sample in sequence, wherein the granularity grade of the abrasive paper is as follows: 240# → 400# → 600# → 800# → 1000# → 1200# → 1500# → 2000# → 2500 #; when pre-grinding is carried out, the higher-number abrasive paper is required to be replaced when the scratches on the surface of the sample are uniform and the directions are consistent, and the grinding direction is vertical to the previous direction; after the sample is pre-ground, mechanically polishing by adopting polishing pastes of W2.5 and W1.5, then cleaning residual oil stain, gravel and residual polishing paste on the surface of the metallographic specimen by using an ultrasonic cleaning machine, and drying by using cold air;
(2) chemical erosion: preparing a metallographic erosion solution, wherein the specific components comprise nitric acid, hydrofluoric acid, oxalic acid and distilled water in a volume ratio of 2-6:1-2:1-2: 2-6; dipping the solution by using a cotton ball for degreasing, and lightly wiping the surface of the sample for 40-60 s until the surface of the sample is bright like a mirror surface; among them, since the HF solution reacts with glass, a plastic container is used for the prepared solution.
(3) Cleaning: after chemical corrosion, a small amount of corrosion liquid is remained on the surface of the metallographic specimen, and in order to prevent excessive corrosion, the metallographic specimen needs to be washed for 30-50 s by running water;
(4) oxidation by a thermal dyeing method: and (3) dehydrating the cleaned metallographic specimen, placing the metallographic specimen on a constant-temperature electric hot plate, setting the temperature to be 350-400 ℃, carrying out oxidation for 8-15 minutes, taking out the metallographic specimen after the surface color of the metallographic specimen changes from bright white to yellow, and cooling the metallographic specimen to carry out metallographic observation.
Compared with the prior art, the invention has the advantages that: the preparation method of the metallographic erosion solution of the zirconium alloy is provided, and oxidation is performed by combining a thermal dyeing method, so that the prepared zirconium alloy is clear in metallographic structure and good in repeatability, can be applied to zirconium alloys in different processing and heat treatment states, and is favorable for analyzing the microstructure and the second phase of the zirconium alloy; the used heating oxidation equipment is simple, the technical requirements on the equipment and operators are not high, and the method is suitable for preparing the metallographic sample of the zirconium alloy in an analytical laboratory.
Drawings
FIG. 1 is a microstructure of a metallographic specimen of a recrystallized and annealed zirconium alloy according to example 1 of the present invention;
FIG. 2 is a microstructure diagram of a metallographic specimen of a recrystallized and annealed zirconium alloy in example 2 of the present invention;
FIG. 3 is a microstructure diagram of a metallographic zirconium sample in a heat affected zone of pressure resistance welding in example 3 of the present invention;
FIG. 4 is a microstructure of a metallographic specimen according to a comparative example of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
In this example, a recrystallized and annealed Zr-4 alloy bar was taken, a metallographic specimen of a zirconium alloy was prepared and observed as follows, and the metallographic microstructure thereof is shown in fig. 1.
1. Sampling and cleaning: pre-cleaning a metallographic sample, soaking the metallographic sample in a beaker filled with acetone, and placing the beaker in an ultrasonic cleaning machine to remove oil stains on the surface of the sample.
2. Coarse grinding-fine grinding: after the surface of the sample is smooth, using metallographic abrasive paper to perform rough grinding, fine grinding and polishing on the metallographic sample in sequence, wherein the granularity grade of the abrasive paper is as follows: 240# → 400# → 600# → 800# → 1000# → 1200# → 1500# → 2000# → 2500 #. When the pre-grinding is carried out, the sand paper with higher number needs to be replaced when scratches on the surface of the sample are uniform and the direction is consistent, and the grinding direction is vertical to the prior direction. After the sample is pre-ground, mechanically polishing by adopting polishing pastes of W2.5 and W1.5, and cleaning residual oil stain, gravel and residual polishing paste on the surface of the metallographic specimen by using an ultrasonic cleaning machine and drying by using cold air.
3. Chemical erosion: preparing metallographic etching solution with specific components of HNO according to volume ratio3:HF:H2C2O4：H2O40: 10:10: 40. And (5) dipping the solution by using a cotton wool ball, and lightly wiping the surface of the sample for 60s until the surface of the sample is bright like a mirror surface.
4. Cleaning: after the chemical corrosion, a small amount of corrosive liquid remains on the surface of the metallographic specimen, and the metallographic specimen needs to be washed for 50 seconds by running water to prevent excessive corrosion.
5. Oxidation by a thermal dyeing method: and (3) dehydrating the cleaned metallographic specimen, placing the metallographic specimen on a constant-temperature electric hot plate, setting the temperature to be 400 ℃, carrying out oxidation for 10 minutes, taking out the metallographic specimen after the surface color of the metallographic specimen is changed from bright white to yellow, and carrying out metallographic observation.
Example 2
In this example, a recrystallized and annealed Zr-4 alloy bar was taken, a metallographic specimen of a zirconium alloy was prepared and observed as follows, and the metallographic microstructure thereof is shown in fig. 2.
1. Sampling and cleaning: pre-cleaning a metallographic sample, soaking the metallographic sample in a beaker filled with acetone, and placing the beaker in an ultrasonic cleaning machine to remove oil stains on the surface of the sample.
2. Coarse grinding-fine grinding: after the surface of the sample is smooth, using metallographic abrasive paper to perform rough grinding, fine grinding and polishing on the metallographic sample in sequence, wherein the granularity grade of the abrasive paper is as follows: 240# → 400# → 600# → 800# → 1000# → 1200# → 1500# → 2000# → 2500 #. When the pre-grinding is carried out, the sand paper with higher number needs to be replaced when scratches on the surface of the sample are uniform and the direction is consistent, and the grinding direction is vertical to the prior direction. After the sample is pre-ground, mechanically polishing by adopting polishing pastes of W2.5 and W1.5, and cleaning residual oil stain, gravel and residual polishing paste on the surface of the metallographic specimen by using an ultrasonic cleaning machine and drying by using cold air.
3. Chemical erosion: preparing metallographic etching solution with specific components of HNO according to volume ratio3:HF:H2C2O4：H2O40: 10:10: 40. And (4) dipping the solution by using a cotton wool ball, and lightly wiping the surface of the sample for 40s until the surface of the sample is bright like a mirror surface.
4. Cleaning: after the chemical corrosion, a small amount of corrosive liquid remains on the surface of the metallographic specimen, and the metallographic specimen needs to be washed for 50 seconds by running water to prevent excessive corrosion.
5. Oxidation by a thermal dyeing method: and (3) dehydrating the cleaned metallographic specimen, placing the metallographic specimen on a constant-temperature electric hot plate, setting the temperature to be 350 ℃, carrying out oxidation for 10 minutes, taking out the metallographic specimen after the surface color of the metallographic specimen is changed from bright white to yellow, and carrying out metallographic observation.
Example 3
Pressure resistance welding is carried out on two Zr-4 alloy bars to obtain a welded joint, a zirconium alloy metallographic sample is prepared according to the following process, the microstructure of a welding heat affected zone is observed, and the metallographic microstructure is shown in figure 3.
1. Sampling and cleaning: pre-cleaning a metallographic sample, soaking the metallographic sample in a beaker filled with acetone, and placing the beaker in an ultrasonic cleaning machine to remove oil stains on the surface of the sample.
2. Coarse grinding-fine grinding: after the surface of the sample is smooth, using metallographic abrasive paper to perform rough grinding, fine grinding and polishing on the metallographic sample in sequence, wherein the granularity grade of the abrasive paper is as follows: 240# → 400# → 600# → 800# → 1000# → 1200# → 1500# → 2000# → 2500 #. When the pre-grinding is carried out, the sand paper with higher number needs to be replaced when scratches on the surface of the sample are uniform and the direction is consistent, and the grinding direction is vertical to the prior direction. After the sample is pre-ground, mechanically polishing by adopting polishing pastes of W2.5 and W1.5, and cleaning residual oil stain, gravel and residual polishing paste on the surface of the metallographic specimen by using an ultrasonic cleaning machine and drying by using cold air.
3. Chemical erosion: preparing metallographic etching solution with specific components of HNO according to volume ratio3:HF:H2C2O4：H2O35: 15:15: 35. And (4) dipping the solution by using a cotton wool ball, and lightly wiping the surface of the sample for 40s until the surface of the sample is bright like a mirror surface.
4. Cleaning: after the chemical corrosion, a small amount of corrosive liquid remains on the surface of the metallographic specimen, and the metallographic specimen needs to be washed for 50 seconds by running water to prevent excessive corrosion.
5. Oxidation by a thermal dyeing method: and (3) dehydrating the cleaned metallographic specimen, placing the metallographic specimen on a constant-temperature electric hot plate, setting the temperature to be 350 ℃, carrying out oxidation for 10 minutes, taking out the metallographic specimen after the surface color of the metallographic specimen is changed from bright white to yellow, and carrying out metallographic observation.
Comparative example
In this example, a recrystallized and annealed Zr-4 alloy bar (same as examples 1 and 2) was taken, a metallographic specimen of a zirconium alloy was prepared and observed as follows, and the metallographic microstructure thereof is shown in fig. 4.
1. Sampling and cleaning: pre-cleaning a metallographic sample, soaking the metallographic sample in a beaker filled with acetone, and placing the beaker in an ultrasonic cleaning machine to remove oil stains on the surface of the sample.
2. Coarse grinding-fine grinding: after the surface of the sample is smooth, using metallographic abrasive paper to perform rough grinding, fine grinding and polishing on the metallographic sample in sequence, wherein the granularity grade of the abrasive paper is as follows: 240# → 400# → 600# → 800# → 1000# → 1200# → 1500# → 2000# → 2500 #. When the pre-grinding is carried out, the sand paper with higher number needs to be replaced when scratches on the surface of the sample are uniform and the direction is consistent, and the grinding direction is vertical to the prior direction. After the sample is pre-ground, mechanically polishing by adopting polishing pastes of W2.5 and W1.5, and cleaning residual oil stain, gravel and residual polishing paste on the surface of the metallographic specimen by using an ultrasonic cleaning machine and drying by using cold air.
3. Chemical erosion: preparation of goldThe specific components of the phase erosion solution are HNO according to volume ratio3:HF:H2C2O4：H2O40: 10:10: 40. And (5) dipping the solution by using a cotton wool ball, and lightly wiping the surface of the sample for 60s until the surface of the sample is bright like a mirror surface.
4. Cleaning: after the chemical corrosion, a small amount of corrosive liquid remains on the surface of the metallographic specimen, and the metallographic specimen needs to be washed for 50 seconds by running water to prevent excessive corrosion.
As is apparent from the examples and fig. 1-3 and the comparative example and fig. 4, the microstructure prepared by the metallographic preparation method of the zirconium alloy of the present invention has clear grains and grain boundaries, and the second phase intermetallic compound dispersed in the matrix is also clearly visible, so that grain size evaluation and microstructure analysis can be performed.
Claims (4)
1. A method for preparing a metallographic specimen of a zirconium alloy is characterized by comprising the following specific steps:
(1) pretreatment: pre-cleaning a metallographic sample, soaking the sample in a beaker filled with acetone, and placing the beaker in an ultrasonic cleaning machine for cleaning for more than 10 minutes to remove oil stains on the surface of the sample; after the surface of the sample is smooth, using metallographic abrasive paper to perform rough grinding, fine grinding and polishing on the metallographic sample in sequence, wherein the granularity grade of the abrasive paper is as follows: 240# → 400# → 600# → 800# → 1000# → 1200# → 1500# → 2000# → 2500 #; after the sample is pre-ground, mechanically polishing by adopting polishing pastes of W2.5 and W1.5, then cleaning residual oil stain, gravel and residual polishing paste on the surface of the metallographic specimen by using an ultrasonic cleaning machine, and drying by using cold air;
(2) chemical erosion: preparing a metallographic erosion solution, wherein the specific components comprise nitric acid, hydrofluoric acid, oxalic acid and distilled water in a volume ratio of 2-6:1-2:1-2: 2-6; dipping the solution by using a cotton ball for degreasing, and lightly wiping the surface of the sample for 40-60 s until the surface of the sample is bright like a mirror surface; wherein, the HF solution reacts with the glass, so the prepared solution needs to use a plastic container;
(3) cleaning: after chemical corrosion, a small amount of corrosion liquid is remained on the surface of the metallographic specimen, and in order to prevent excessive corrosion, the metallographic specimen needs to be washed for 30-50 s by running water;
(4) oxidation by a thermal dyeing method: and (3) dehydrating the cleaned metallographic specimen, placing the metallographic specimen on a constant-temperature electric hot plate, setting the temperature to be 350-400 ℃, carrying out oxidation for 8-15 minutes, taking out the metallographic specimen after the surface color of the metallographic specimen changes from bright white to yellow, and cooling the metallographic specimen to carry out metallographic observation.
2. The method for preparing a metallographic specimen of a zirconium alloy according to claim 1, wherein the pre-grinding in step (1) is performed by replacing a higher-grade abrasive paper when the scratches on the surface of the metallographic specimen are uniform and the direction of the scratches is consistent, and the grinding direction is perpendicular to the direction of the scratches of the previous abrasive paper.
3. A method of preparing a metallographic specimen of a zirconium alloy according to claim 1, characterised in that said zirconium alloy is a Zr-4 alloy.
4. The etchant for observing the metallographic structure of the zirconium alloy is characterized in that a metallographic etchant solution comprises nitric acid, hydrofluoric acid, oxalic acid and distilled water in a volume ratio of 2-6:1-2:1-2: 2-6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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