CN111979547A - Metallographic corrosive agent for nickel-based alloy and use method thereof - Google Patents
Metallographic corrosive agent for nickel-based alloy and use method thereof Download PDFInfo
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- CN111979547A CN111979547A CN202010663391.0A CN202010663391A CN111979547A CN 111979547 A CN111979547 A CN 111979547A CN 202010663391 A CN202010663391 A CN 202010663391A CN 111979547 A CN111979547 A CN 111979547A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 24
- 239000000956 alloy Substances 0.000 title claims abstract description 23
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 23
- 239000003518 caustics Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims description 16
- 238000005498 polishing Methods 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- 230000003287 optical effect Effects 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229920000742 Cotton Polymers 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- 239000000314 lubricant Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 11
- 230000007797 corrosion Effects 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 5
- 208000027418 Wounds and injury Diseases 0.000 abstract description 4
- 230000006378 damage Effects 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 208000014674 injury Diseases 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract description 2
- 230000009972 noncorrosive effect Effects 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 4
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 241001085205 Prenanthella exigua Species 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- 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
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- Immunology (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
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Abstract
The invention provides a metallographic corrosive agent for nickel-based alloy and a using method thereof, and the technical scheme is as follows: the corrosive agent comprises the following components in percentage by weight: 5g of ferric chloride, 3g of copper chloride, 100ml of 36.5% concentrated hydrochloric acid and 50-100 ml of 95% absolute ethyl alcohol, wherein the content of the absolute ethyl alcohol can be adjusted according to the content of nickel. The beneficial effects are as follows: the invention has simple preparation and easy storage; the invention is non-corrosive strong acid, is not easy to cause personal injury and environmental pollution, is safe and environment-friendly; after the nickel-based high-temperature alloy is corroded by the method, the corrosion effect is good, the metallographic structure is obvious, the grain structure is complete, the condition of non-uniform corrosion or over-corrosion is avoided, and the grain measurement, the metallographic structure analysis, the defect analysis and the like are facilitated.
Description
Technical Field
The invention relates to a metallographic corrosive agent and a method, in particular to a metallographic corrosive agent for nickel-based alloy and a using method.
Background
The nickel-based alloy is an alloy which takes nickel as a matrix, has good high-temperature strength, fatigue resistance, oxidation resistance and corrosion resistance, and has good mechanical properties and processability, and is widely applied to the fields of petrochemical industry, automobiles, aviation, aerospace, nuclear industry, military industry and the like at present.
Because the corrosion resistance is better, the corrosion is more difficult when carrying out metallographic examination, and the commonly used corrosive agent at present includes aqua regia, nitric acid-hydrochloric acid solution etc. but this type of corrosive agent effect is general, and the sample surface corrosion is inhomogeneous simultaneously, and partial region easily forms the over-corrosion, leads to metallographic examination to go on normally, and the corrosive agent such as aqua regia contains volatile strong acid simultaneously, if use and deposit improper probably causes bodily injury and environmental pollution.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the metallographic corrosive agent for the nickel-based alloy and the using method thereof, wherein the metallographic corrosive agent is simple to prepare and easy to store, does not easily cause personal injury and environmental pollution, and is safe and environment-friendly.
The invention provides a metallographic corrosive agent for nickel-based alloy, which has the technical scheme that: the iron chloride, copper chloride, concentrated hydrochloric acid and absolute ethyl alcohol are mixed according to the proportion of 5 g: 3 g: 100 ml: (50-100) ml, wherein the volume percentage concentration of concentrated hydrochloric acid is 36.5%, and the volume percentage concentration of absolute ethyl alcohol is 95%.
Preferably, the preparation method of the metallographic corrosive agent for the nickel-based alloy comprises the following steps:
weighing 5 parts of ferric chloride and 3 parts of copper chloride at room temperature, and putting into a dry and clean beaker; pouring 100ml of concentrated hydrochloric acid which is measured and continuously stirring by using a glass rod; then pouring 50-100 ml of weighed absolute ethyl alcohol, and continuously stirring by using a glass rod until the solid powder is completely dissolved; standing for at least 5 min.
Preferably, the method for using the metallographic corrosive agent for the nickel-based alloy comprises the following steps:
firstly, cutting a metallographic sample from a nickel-based alloy by using a cutting machine, and chamfering each edge of the sample by using a grinding wheel or coarse sand paper;
secondly, grinding the sample by using metallographic waterproof abrasive paper with different particle sizes, and grinding the metallographic sample by using 220-mesh, 400-mesh, 800-mesh and 1000-mesh metallographic waterproof abrasive paper in sequence;
polishing the sample by using a polishing machine, using distilled water as a lubricant, and adding a 2.5-micron diamond polishing spray during polishing; washing the polished surface of the sample with distilled water, then washing with absolute ethyl alcohol, and drying the surface by using a hair drier;
fourthly, using absorbent cotton to dip the nickel-based alloy and then wiping the surface of the sample with a metallographic corrosive agent, and corroding until the surface of the sample becomes black; washing the corroded surface of the sample with distilled water, then washing with absolute ethyl alcohol, and drying the surface by using an electric hair drier; metallographic structure observation was performed using an optical metallographic microscope.
The invention has the beneficial effects that: the invention has simple preparation and easy storage; the invention is non-corrosive strong acid, is not easy to cause personal injury and environmental pollution, is safe and environment-friendly; the nickel-based alloy corroded by the method has the advantages of good corrosion effect, obvious metallographic structure, complete grain structure, no corrosion unevenness or over corrosion, and convenience for grain measurement, metallographic structure analysis, defect analysis and the like.
Drawings
FIG. 1 is a metallographic structure diagram (100X) of a sample of example 1 of the present invention after etching;
FIG. 2 is a metallographic structure graph (400X) after etching in example 1 of the present invention;
FIG. 3 is a metallographic structure graph (100X) obtained after etching in example 2 of the present invention;
FIG. 4 is a metallographic structure graph (400X) showing a corroded structure obtained in example 2 of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1: the metallographic corrosive agent for the K213 nickel-based alloy (the nickel content is about 34-38%) and the using method are as follows:
preparing a corrosive agent: weighing 5g of ferric chloride and 3g of copper chloride at room temperature, and putting into a dry and clean beaker; pouring 100ml of concentrated hydrochloric acid with the volume percentage of 36.5 percent, and continuously stirring by using a glass rod; then 100ml of absolute ethyl alcohol with the volume percentage of 95 percent is poured into the mixture, and the mixture is continuously stirred by a glass rod until the solid powder is completely dissolved; standing for at least 5 min.
Sample preparation: cutting a metallographic specimen from the K213 nickel-based alloy by using a cutting machine; chamfering each side and edge of the sample by using a grinding wheel or coarse sandpaper; grinding the samples by using metallographic waterproof abrasive paper with different particle sizes, and grinding the metallographic samples by using 220-mesh, 400-mesh, 800-mesh and 1000-mesh metallographic waterproof abrasive paper in sequence; polishing the sample by using a polishing machine, using distilled water as a lubricant, and adding a diamond polishing spray with the particle size of 2.5 mu m in the polishing process; washing the polished surface of the sample with distilled water, then washing with absolute ethyl alcohol, and drying the surface by using a hair drier; dipping absorbent cotton in the corrosive agent, wiping the surface of the sample for about 30s, and corroding until the surface of the sample becomes black; washing the corroded surface of the sample with distilled water, then washing with absolute ethyl alcohol, and drying the surface by using an electric hair drier; metallographic structure observation was performed using an optical metallographic microscope.
And (3) metallographic structure observation: taking the corroded sample under an optical microscope to observe a metallographic microstructure; the metallographic structure photograph at a magnification of 100 times is shown in fig. 1, the metallographic structure photograph at a magnification of 400 times is shown in fig. 2, and as can be seen from fig. 1 and 2, the matrix structure (dark color), carbide (bright white color), and the like of the sample can be clearly observed.
Example 2: metallographic etchant for K418 nickel-based alloy (nickel content about 72% to 76%) and method of use are described below.
Preparing a corrosive agent: weighing 5g of ferric chloride and 3g of copper chloride at room temperature, and putting into a dry and clean beaker; pouring 100ml of concentrated hydrochloric acid with the volume percentage of 36.5 percent, and continuously stirring by using a glass rod; then 50ml of absolute ethyl alcohol with the volume percentage of 95 percent is poured into the mixture, and the mixture is continuously stirred by a glass rod until the solid powder is completely dissolved; standing for at least 5 min.
Sample preparation: cutting a metallographic sample of the K418 nickel-based alloy by using a cutting machine; chamfering each side and edge of the sample by using a grinding wheel or coarse sandpaper; grinding the samples by using metallographic waterproof abrasive paper with different particle sizes, and grinding the metallographic samples by using 220-mesh, 400-mesh, 800-mesh and 1000-mesh metallographic waterproof abrasive paper in sequence; polishing the sample by using a polishing machine, using distilled water as a lubricant, and adding a diamond polishing spray with the particle size of 2.5 mu m in the polishing process; washing the polished surface of the sample with distilled water, then washing with absolute ethyl alcohol, and drying the surface by using a hair drier; dipping absorbent cotton with a corrosive agent, wiping the surface of the sample for about 45s, and corroding until the surface of the sample becomes black; washing the corroded surface of the sample with distilled water, then washing with absolute ethyl alcohol, and drying the surface by using an electric hair drier; metallographic structure observation was performed using an optical metallographic microscope.
And (3) metallographic structure observation: taking the corroded sample under an optical microscope to observe a metallographic microstructure; the metallographic structure photograph at a magnification of 100 times is shown in fig. 3, the metallographic structure photograph at a magnification of 400 times is shown in fig. 4, and as can be seen from fig. 3 and 4, the matrix structure (dark color), carbide (bright white color), and the like of the sample can be clearly observed.
The above description is only a few of the preferred embodiments of the present invention, and any person skilled in the art may modify the above-described embodiments or modify them into equivalent ones. Therefore, any simple modifications or equivalent substitutions made in accordance with the technical solution of the present invention are within the scope of the claims of the present invention.
Claims (3)
1. A metallographic corrosive agent for nickel-based alloys is characterized in that: the iron chloride, copper chloride, concentrated hydrochloric acid and absolute ethyl alcohol are mixed according to the proportion of 5 g: 3 g: 100 ml: (50-100) ml, wherein the volume percentage concentration of concentrated hydrochloric acid is 36.5%, and the volume percentage concentration of absolute ethyl alcohol is 95%.
2. The metallographic etchant for nickel-base alloys according to claim 1, characterized by the fact that it is produced by the following method:
weighing 5 parts of ferric chloride and 3 parts of copper chloride at room temperature, and putting into a dry and clean beaker; pouring 100ml of concentrated hydrochloric acid which is measured and continuously stirring by using a glass rod; then pouring 50-100 ml of weighed absolute ethyl alcohol, and continuously stirring by using a glass rod until the solid powder is completely dissolved; standing for at least 5 min.
3. Use of a metallographic etchant for nickel-base alloys according to claim 1 or 2, characterised in that it comprises the following steps:
firstly, cutting a metallographic sample from a nickel-based alloy by using a cutting machine, and chamfering each edge of the sample by using a grinding wheel or coarse sand paper;
secondly, grinding the sample by using metallographic waterproof abrasive paper with different particle sizes, and grinding the metallographic sample by using 220-mesh, 400-mesh, 800-mesh and 1000-mesh metallographic waterproof abrasive paper in sequence;
polishing the sample by using a polishing machine, using distilled water as a lubricant, and adding a 2.5-micron diamond polishing spray during polishing; washing the polished surface of the sample with distilled water, then washing with absolute ethyl alcohol, and drying the surface by using a hair drier;
fourthly, using absorbent cotton to dip the nickel-based alloy and then wiping the surface of the sample with a metallographic corrosive agent, and corroding until the surface of the sample becomes black; washing the corroded surface of the sample with distilled water, then washing with absolute ethyl alcohol, and drying the surface by using an electric hair drier; metallographic structure observation was performed using an optical metallographic microscope.
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| CN202010663391.0A CN111979547A (en) | 2020-07-10 | 2020-07-10 | Metallographic corrosive agent for nickel-based alloy and use method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113640090A (en) * | 2021-08-27 | 2021-11-12 | 北京星航机电装备有限公司 | GH4141 high-temperature alloy metallographic structure corrosive agent and corrosion method |
| CN113758784A (en) * | 2021-09-06 | 2021-12-07 | 湘潭大学 | Metallographic corrosive liquid and corrosive method applied to iron-based matrix nickel-based coating |
| CN114323887A (en) * | 2022-01-11 | 2022-04-12 | 山西太钢不锈钢股份有限公司 | Preparation method and corrosion method of nickel-based alloy metallographic corrosive agent |
| CN114606496A (en) * | 2022-03-28 | 2022-06-10 | 西安热工研究院有限公司 | Metallographic corrosive agent for 800H alloy welded joint sample, preparation method and metallographic display method |
| CN115261862A (en) * | 2022-09-06 | 2022-11-01 | 清华大学 | Corrosive agent for corroding nickel-based single crystal superalloy, corrosion method and device for realizing method |
| CN115753579A (en) * | 2022-11-24 | 2023-03-07 | 江苏隆达超合金股份有限公司 | Nickel-based alloy pipe ferric sulfate intergranular corrosion test method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113640090A (en) * | 2021-08-27 | 2021-11-12 | 北京星航机电装备有限公司 | GH4141 high-temperature alloy metallographic structure corrosive agent and corrosion method |
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| CN113758784A (en) * | 2021-09-06 | 2021-12-07 | 湘潭大学 | Metallographic corrosive liquid and corrosive method applied to iron-based matrix nickel-based coating |
| CN114323887A (en) * | 2022-01-11 | 2022-04-12 | 山西太钢不锈钢股份有限公司 | Preparation method and corrosion method of nickel-based alloy metallographic corrosive agent |
| CN114606496A (en) * | 2022-03-28 | 2022-06-10 | 西安热工研究院有限公司 | Metallographic corrosive agent for 800H alloy welded joint sample, preparation method and metallographic display method |
| CN115261862A (en) * | 2022-09-06 | 2022-11-01 | 清华大学 | Corrosive agent for corroding nickel-based single crystal superalloy, corrosion method and device for realizing method |
| CN115753579A (en) * | 2022-11-24 | 2023-03-07 | 江苏隆达超合金股份有限公司 | Nickel-based alloy pipe ferric sulfate intergranular corrosion test method |
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