CN113862767A - Electrolytic corrosion method of austenitic stainless steel and application thereof - Google Patents
Electrolytic corrosion method of austenitic stainless steel and application thereof Download PDFInfo
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- CN113862767A CN113862767A CN202111005918.1A CN202111005918A CN113862767A CN 113862767 A CN113862767 A CN 113862767A CN 202111005918 A CN202111005918 A CN 202111005918A CN 113862767 A CN113862767 A CN 113862767A
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- 229910000963 austenitic stainless steel Inorganic materials 0.000 title claims abstract description 61
- 238000005260 corrosion Methods 0.000 title claims abstract description 50
- 230000007797 corrosion Effects 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 44
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 13
- 239000010935 stainless steel Substances 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 14
- 238000005868 electrolysis reaction Methods 0.000 claims description 12
- 238000000866 electrolytic etching Methods 0.000 claims description 12
- 238000011156 evaluation Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 239000006104 solid solution Substances 0.000 description 12
- 229910001566 austenite Inorganic materials 0.000 description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 238000005530 etching Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- FGHSTPNOXKDLKU-UHFFFAOYSA-N nitric acid;hydrate Chemical compound O.O[N+]([O-])=O FGHSTPNOXKDLKU-UHFFFAOYSA-N 0.000 description 1
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical compound O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/06—Etching of iron or steel
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- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
- G01N15/0227—Investigating particle size or size distribution by optical means using imaging; using holography
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Abstract
The invention relates to an electrolytic corrosion method of austenitic stainless steel and application thereof, relating to the technical field of metallographic detection. The electrolytic corrosion method comprises the following steps: preparing electrolytic corrosion liquid, and preparing a nitric acid aqueous solution with the nitric acid concentration of 7.5-10.0 mol/L; and (3) electrolytic corrosion, namely putting the austenitic stainless steel as an anode and the stainless steel plate as a cathode into the nitric acid aqueous solution for electrolytic corrosion. By adopting the electrolytic corrosion method, the austenitic stainless steel can only show crystal boundaries and does not show twin crystals, and further, the grain structure of the austenitic stainless steel can be clearly, completely and accurately shown.
Description
Technical Field
The invention relates to the technical field of metallographic detection, in particular to an electrolytic corrosion method of austenitic stainless steel and application thereof.
Background
Austenitic stainless steel is stainless steel having an austenitic structure at normal temperature, and is characterized by being nonmagnetic, having high toughness and plasticity, but having low strength. Stainless steel has excellent corrosion resistance, formability, compatibility, toughness in a wide temperature range and the like, so that the stainless steel is widely applied to the industries such as heavy industry, light industry, living goods industry, building decoration and the like.
At present, the structure of austenitic stainless steel after solid solution is displayed, 10% oxalic acid aqueous solution electrolytic corrosion or ferric trichloride hydrochloric acid aqueous solution etching is generally adopted in the industry, the grain structures obtained by the two methods can generate twin crystals, the grain boundaries are incomplete, the twin crystals obviously interfere the measurement and evaluation of the grain size, and the grain size cannot be clearly evaluated if the grain boundaries are incomplete. The prior art mainly aims at the structural details display of austenitic stainless steel after solid solution, and comprehensively analyzes the structural properties; but the evaluation effect on the grain size is not ideal.
Disclosure of Invention
In order to solve the problems, the invention provides an electrolytic corrosion method for austenitic stainless steel, which can effectively inhibit the appearance of twin crystals in an austenitic structure, only shows austenite crystal boundaries, does not show the twin crystals, and can show clear, complete and accurate grain structures of the austenitic stainless steel.
In order to achieve the above object, the present invention provides an electrolytic corrosion method of austenitic stainless steel, comprising the steps of:
preparing an electrolytic corrosion solution: preparing a nitric acid aqueous solution with the nitric acid concentration of 7.5-10.0 mol/L;
electrolytic corrosion: and putting austenitic stainless steel as an anode and a stainless steel plate as a cathode into the nitric acid aqueous solution for electrolytic corrosion.
By adopting the electrolytic corrosion method, the austenitic stainless steel can only show crystal boundaries and does not show twin crystals, and further, the grain structure of the austenitic stainless steel can be clearly, completely and accurately shown.
The inventor finds in earlier studies that, in a metal material used at normal temperature, the finer the crystal grain, the higher the strength and hardness, and the better the plasticity and toughness; however, the strength of the metal material is rather lowered by grain refinement in a high temperature range, and the smaller the grain size of the austenitic stainless steel is, the better the intergranular corrosion resistance is. Meanwhile, the technical specifications of many products specify the required range for the grain size level index, and the measurement of the grain size is very necessary. And because twin crystal is that two parts of a crystal form a mirror symmetry orientation relation along a common crystal plane (namely a specific orientation relation), and the crystal boundary is the interface between crystal grains with the same structure and different orientations, and the crystal grain size is completely different, the crystal boundary needs to be highlighted to inhibit the appearance of twin crystal, so that the austenitic stainless steel only shows the crystal boundary and does not show the twin crystal in order to accurately and effectively evaluate the crystal grain size. In the prior art, the austenitic stainless steel is etched by electrolytic corrosion of 10% oxalic acid aqueous solution or ferric chloride hydrochloric acid aqueous solution, and a satisfactory effect cannot be obtained.
The solid solution austenite structure of the austenitic stainless steel has twin crystals, and the twin crystals are more obvious when the solid solution is more sufficient; in practical tests, twin boundaries can seriously interfere with the measurement of grain size. Therefore, the present inventors have employed a nitric acid aqueous solution having a specific volume concentration in combination with a specific electrolytic voltage, current and electrolytic time to achieve a state in which the nitric acid concentration and the electrolytic voltage are in a mutual combination equilibrium.
In one embodiment, the concentration of nitric acid in the nitric acid aqueous solution is 8.0mol/L to 9.5 mol/L.
By adopting the nitric acid aqueous solution with the volume concentration, the austenite crystal boundary can be fully displayed, twin crystal display can be well inhibited, and the clear and interference-free austenite crystal boundary can be obtained.
In one embodiment, in the electrolytic etching step, the voltage is 1-3V, the current is 0.3-0.5A, and the electrolysis time is 50-70 s.
By adopting the electrolytic corrosion condition, the electrolytic corrosion condition can be cooperated with the nitric acid aqueous solution with the volume concentration, so that austenite crystal boundaries are fully displayed, the display of twin crystal boundaries is well inhibited, and clear and interference-free austenite crystal boundaries are obtained.
In one embodiment, in the step of electrolytic etching, the voltage is 2V, the current is 0.35-0.45A, and the electrolysis time is 60 s.
In one embodiment, in the electrolytic etching step, one surface of the austenitic stainless steel is polished, and the polished surface of the austenitic stainless steel is placed in parallel facing the stainless steel plate.
By adopting the above arrangement, the polished surface of the austenitic stainless steel can be subjected to uniform electrolytic corrosion.
The invention also provides a grain size evaluation method of the austenitic stainless steel, which comprises the following steps:
grain boundary display: taking austenitic stainless steel to be evaluated, and electrolytically corroding the austenitic stainless steel to ensure that the austenitic stainless steel only shows grain boundaries and does not show twin crystals;
grain size evaluation: the grain size of the austenitic stainless steel showing the grain boundaries was evaluated based on the grain boundaries.
By adopting the evaluation method, the grain size of the austenitic stainless steel can be accurately evaluated.
In one embodiment, the austenitic stainless steel to be evaluated is evaluated by the electrolytic corrosion method.
The invention also provides the austenitic stainless steel after electrolytic corrosion obtained by the electrolytic corrosion method.
The invention also provides application of the austenitic stainless steel subjected to electrolytic corrosion in grain size evaluation.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides an electrolytic corrosion method of austenitic stainless steel and application thereof, wherein the electrolytic corrosion method solves the problem that twin crystals interfere with grain size after solid solution of austenitic stainless steel, and solves the problem that the existing etching method can not clearly display grain boundaries; the electrolytic corrosion method can effectively inhibit the appearance of twin crystals in an austenitic structure, only shows an austenitic crystal boundary, does not show the twin crystals, further shows a clear, complete and accurate grain structure of the austenitic stainless steel, greatly improves the working efficiency and accuracy, and provides a basis for the quality evaluation of the austenitic stainless steel material. Meanwhile, the electrolyte in the electrolytic corrosion method is simple and convenient to prepare, the material is easy to obtain, pollution-free, safe to use and capable of being used repeatedly.
Drawings
FIG. 1 is a metallographic structure photograph of example 1;
FIG. 2 is a metallographic structure photograph of comparative example 1;
FIG. 3 is a metallographic structure photograph of comparative example 2;
FIG. 4 is a metallographic structure photograph of comparative example 3;
fig. 5 is a metallographic structure photograph of comparative example 4.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Defining:
the austenitic stainless steel of the invention: which means a stainless steel having an austenitic structure at normal temperature.
Austenite: refers to a non-magnetic solid solution with a small amount of carbon dissolved in gamma-Fe.
Grain boundary: for polycrystalline materials, a narrow region of transition from one crystallographic direction to another separates adjacent grains.
Crystal grain: the entire area surrounded by the grain boundaries. That is, the area within the range of the original grain boundary observed on the two-dimensional surface, or the volume enclosed within the original grain boundary surface on the three-dimensional object, twin interfaces are not considered for the material having twin boundary surfaces.
Twinning: the two parts of one crystal form a mirror symmetry orientation relation along a common crystal plane (namely a specific orientation relation), the two crystals are called twin crystals, and the common crystal plane is called twin crystal plane.
Grain size: refers to a measure representing the size of a grain
The source is as follows:
reagents, materials and equipment used in the present example are all commercially available sources unless otherwise specified; unless otherwise specified, all the experimental methods are routine in the art.
Example 1
Electrolytically corroding the austenitic stainless steel.
1. Preparing an electrolytic corrosion solution: 180ml of nitric acid (65-68% by mass, super pure) is poured into 120ml of water, and after the nitric acid is uniformly stirred by a glass rod, electrolytic corrosion liquid (namely nitric acid water solution with the molar concentration of 8.64-9.12 mol/L) is obtained and poured into an electrolytic tank for later use.
2. Electrolytic corrosion: a solid solution austenitic stainless steel of SA-182F316H was used as a sample, which was polished and subjected to electrolytic corrosion using a stainless steel plate as an anode and a cathode. The electrolysis parameters used were: the voltage is 2V, the current is 0.35-0.45A, and the electrolysis time is 60 s.
Comparative example 1
Electrolytically corroding the austenitic stainless steel.
1. Preparing an electrolytic corrosion solution: preparing 10% oxalic acid water solution as electrolytic corrosion liquid.
2. Electrolytic corrosion: a solid solution austenitic stainless steel made of SA-182F316H was used as a sample, which was ground and polished, and used as an anode and a stainless steel plate as a cathode, and an electrolysis voltage of 6V, a current of 1.2A and an electrolysis time of 60s were carried out.
Comparative example 2
The austenitic stainless steel is etched.
1. Preparing an etching solution: 30g of ferric trichloride, 90ml of hydrochloric acid and 360ml of water are prepared into ferric trichloride hydrochloric acid etching solution.
2. Etching: a solid solution state austenitic stainless steel made of SA-182F316H is used as a sample, and the sample is ground, polished and etched in the etching solution.
Comparative example 3
Electrolytically corroding the austenitic stainless steel.
1. Preparing an electrolytic corrosion solution: preparing a nitric acid aqueous solution with the volume concentration of 30% (namely, a nitric acid aqueous solution with the molar concentration of 6.48-6.84 mol/L) as an electrolytic etching solution.
2. Electrolytic corrosion: a solid solution austenitic stainless steel of SA-182F316H was used as a sample, which was polished and subjected to electrolytic corrosion using a stainless steel plate as an anode and a cathode. The electrolysis parameters adopted by the invention are as follows: the voltage is 2V, the current is 0.35-0.45A, and the electrolysis time is 60 s.
Comparative example 4
Electrolytically corroding the austenitic stainless steel.
1. Preparing an electrolytic corrosion solution: preparing a nitric acid aqueous solution with the volume concentration of 50% (namely, a nitric acid aqueous solution with the molar concentration of 10.8-11.4 mol/L) as an electrolytic etching solution.
2. Electrolytic corrosion: a solid solution austenitic stainless steel of SA-182F316H was used as a sample, which was polished and subjected to electrolytic corrosion using a stainless steel plate as an anode and a cathode. The electrolysis parameters adopted by the invention are as follows: the voltage is 2V, the current is 0.35-0.45A, and the electrolysis time is 60 s.
Examples of the experiments
The austenitic stainless steel after electrolytic corrosion was observed and grain size evaluation was performed.
1. The samples obtained in example 1 and comparative examples 1 to 4 were washed with clean water, dropped with absolute ethyl alcohol, dried with hot air, and then all placed under a microscope of 200X for observation and photographing.
2. The results show that: as shown in figure 1, the sample obtained in the embodiment 1 has clear and complete structure grain boundary after solid solution of austenitic stainless steel, has no twin interference, and can be effectively evaluated in grain size; the sample obtained in comparative example 1 is shown in fig. 2, and the sample obtained in comparative example 2 is shown in fig. 3, both of which have serious twin interference and incomplete grain boundaries, and thus effective grain size evaluation cannot be performed. The sample obtained in the comparative example 3 is shown in fig. 4, twin crystals are inhibited, but austenite crystal boundaries are not completely shown, and the grain boundaries are different in depth; the sample obtained in comparative example 4 is shown in FIG. 5, and twins occur, which interfere with the measurement of the austenite grain boundary.
3. Grain size evaluation: the samples obtained in example 1 were evaluated by a contrast method, an intercept method and an area method in the GBT6394-2017 metal average grain size determination method, and the grain sizes were all 6.5 grades.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. An electrolytic corrosion method of austenitic stainless steel, characterized by comprising the steps of:
preparing an electrolytic corrosion solution: preparing a nitric acid aqueous solution with the nitric acid concentration of 7.5-10.0 mol/L;
electrolytic corrosion: and putting austenitic stainless steel as an anode and a stainless steel plate as a cathode into the nitric acid aqueous solution for electrolytic corrosion.
2. The electrolytic etching method according to claim 1, wherein the concentration of the nitric acid in the aqueous nitric acid solution is 8.0mol/L to 9.5 mol/L.
3. The electrolytic etching method according to claim 1, wherein in the electrolytic etching step, the voltage is 1 to 3V, the current is 0.3 to 0.5A, and the electrolysis time is 50 to 70 s.
4. The electrolytic etching method according to claim 1, wherein in the electrolytic etching step, the voltage is 2V, the current is 0.35-0.45A, and the electrolysis time is 60 s.
5. The electrolytic etching method according to claim 1, wherein in the electrolytic etching step, one surface of the austenitic stainless steel is polished, and the polished surface of the austenitic stainless steel is placed in parallel with facing the stainless steel plate.
6. A method for evaluating grain size of austenitic stainless steel is characterized by comprising the following steps:
grain boundary display: taking austenitic stainless steel to be evaluated, and electrolytically corroding the austenitic stainless steel to ensure that the austenitic stainless steel only shows grain boundaries and does not show twin crystals;
grain size evaluation: the grain size of the austenitic stainless steel showing the grain boundaries was evaluated based on the grain boundaries.
7. The assessment method according to claim 6, wherein the austenitic stainless steel to be assessed is assessed using the electrolytic corrosion method according to any one of claims 1 to 5.
8. An electrolytically corroded austenitic stainless steel obtained by the electrolytic corrosion method according to any one of claims 1 to 5.
9. Use of the electrolytically corroded austenitic stainless steel of claim 8 in grain size evaluation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114561593A (en) * | 2022-03-04 | 2022-05-31 | 马鞍山钢铁股份有限公司 | Steel for long-life high-strength-toughness corrosion-resistant underwater Christmas tree valve body, heat treatment method and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114561593A (en) * | 2022-03-04 | 2022-05-31 | 马鞍山钢铁股份有限公司 | Steel for long-life high-strength-toughness corrosion-resistant underwater Christmas tree valve body, heat treatment method and production method thereof |
| CN114561593B (en) * | 2022-03-04 | 2022-11-08 | 马鞍山钢铁股份有限公司 | Steel for long-life high-strength-toughness corrosion-resistant underwater Christmas tree valve body, heat treatment method and production method thereof |
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