CN118360654A - High-nitrogen austenitic stainless steel corrosive and corrosion method - Google Patents

High-nitrogen austenitic stainless steel corrosive and corrosion method Download PDF

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Publication number
CN118360654A
CN118360654A CN202410399788.1A CN202410399788A CN118360654A CN 118360654 A CN118360654 A CN 118360654A CN 202410399788 A CN202410399788 A CN 202410399788A CN 118360654 A CN118360654 A CN 118360654A
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China
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stainless steel
austenitic stainless
polishing
sample
nitrogen austenitic
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CN202410399788.1A
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Inventor
杨晓益
朱章宇
石曜珲
杨书汉
朱轩
李萌蘖
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Abstract

The invention discloses a high-nitrogen austenitic stainless steel corrosive and a corrosion method, wherein the high-nitrogen austenitic stainless steel corrosive is prepared from 3-8% of perchloric acid by volume fraction and 92-97% of alcohol by volume fraction. The invention has the advantages that: the corrosive agent has simple composition, convenient preparation, no pungent smell, easy operation, accurate and controllable corrosion method, stability, high efficiency and good reproducibility. The surface of the sample after corrosion is clean and tidy, no scratch pollution, clear and uniform crystalline phase structure and very good corrosion effect.

Description

High-nitrogen austenitic stainless steel corrosive and corrosion method
Technical Field
The invention relates to the technical field of stainless steel metal corrosive agents, in particular to a high-nitrogen austenitic stainless steel corrosive agent and a corrosion method.
Background
The high-nitrogen austenitic stainless steel is one of new generation advanced steel materials, has excellent mechanical property, corrosion resistance and biocompatibility, and has wide application prospect in the fields of national defense and military industry, nuclear power industry, medical appliances and the like. Nitrogen is added to stainless steel as an important alloying element, which is beneficial to enlarge and stabilize the austenitic phase. Through the synergistic effect with other elements (such as Cr, mn and the like), the strength of the stainless steel is obviously improved, the toughness is not reduced, and the wear resistance and corrosion resistance of the stainless steel are greatly enhanced.
Metallographic detection analysis is an important basic means in the research and development and production process of steel, and is important to grasp microstructure (such as dendrite, precipitated phase, inclusion, microcrack, air hole, grain size and the like) of a product, optimize process parameters and improve product quality. The addition of nitrogen element makes the corrosion resistance of high-nitrogen austenitic stainless steel very excellent, and the conventional stainless steel metallographic corrosive (aqua regia, cuCl 2 solution, etc.) has unsatisfactory corrosion effect, and cannot well show the original austenite grain boundary of high-nitrogen stainless steel. There are few reports on the method of metallographic corrosion of high-nitrogen austenitic stainless steel, and some existing corrosion processes for stainless steel cannot be applied to the metallographic phase of high-nitrogen austenitic stainless steel.
Therefore, a corrosion reagent and a corrosion method suitable for the high-nitrogen austenitic stainless steel are explored, and the corrosion reagent and the corrosion method have important significance for the application of the high-nitrogen austenitic stainless steel.
Disclosure of Invention
The invention aims to provide a high-nitrogen austenitic stainless steel corrosive agent with good corrosion effect and a corrosion method.
In order to solve the technical problems, the invention provides a high-nitrogen austenitic stainless steel corrosive agent which is prepared from 3-8% of perchloric acid by volume fraction and 92-97% of alcohol by volume fraction.
Preferably, the composition is prepared from perchloric acid with the volume fraction of 5% and alcohol with the volume fraction of 95%
Preferably, the N content in the high-nitrogen austenitic stainless steel is more than or equal to 0.45%.
Preferably, the concentration of the perchloric acid is 70-72%.
Preferably, the alcohol is absolute ethanol.
The invention also provides a high-nitrogen austenitic stainless steel corrosion method, which comprises the following steps:
S1, preparing a high-nitrogen austenitic stainless steel corrosive agent: sequentially adding 92 ml-98 ml of alcohol and 2 ml-8 ml of perchloric acid, uniformly stirring, and standing for more than 2 hours;
s2, embedding a sample;
S3, grinding and polishing;
S4, metallographic corrosion: and (3) taking the sample as an anode and connecting the sample with the anode of a power supply, taking platinum as a cathode and connecting the sample with the cathode of the power supply, immersing the sample in the high-nitrogen austenitic stainless steel corrosive liquid prepared in the step (S1), then switching on a direct-current stabilized power supply to corrode the sample until the polished surface of the sample is silver gray, taking out the sample, sequentially flushing the sample with clear water and alcohol, and drying the sample.
The step S2 of embedding the sample comprises the following specific steps: placing the sample in a mosaic machine, and performing cold mosaic by using phenolic resin powder, wherein the mosaic temperature is room temperature and the mosaic time is 15min;
Further, the specific method for grinding and polishing in the step S3 is as follows: sequentially polishing and polishing the detection surface of the sample to be detected by using sand paper until scratches, pits and stains on the surface of the detection surface are removed, so that the surface is smooth and bright, flushing the polished detection surface by using running water, scrubbing by using alcohol and drying;
further, the polishing method comprises the following steps: sequentially polishing with 320 mesh, 600 mesh, 1000 mesh, 1500 mesh, 2000 mesh, 3000 mesh, 5000 mesh and 7000 mesh sand paper under flowing water.
Further, the polishing method comprises the following steps: firstly, carrying out rough polishing by using flocking polishing cloth and diamond polishing paste with the granularity of 5 mu m, and after polishing marks are removed and the polishing mark directions are consistent, carrying out fine polishing by using cashmere polishing cloth and diamond polishing paste with the granularity of 1 mu m until the surface is specular gloss and no polishing mark is observed under an optical microscope.
Further, the power supply in the step S4 is a direct current stabilized power supply, the voltage is 3 v-8 v, and the power-on time is 2S-40S.
The invention has the beneficial effects that:
The high-nitrogen austenitic stainless steel corrosive agent provided by the invention has the advantages of simple composition, convenience in preparation, no pungent smell, easiness in operation, accuracy, controllability, stability, high efficiency and good repeatability. The surface of the sample after corrosion is clean and tidy, no scratch pollution, clear and uniform crystalline phase structure and very good corrosion effect, and has important significance for researching the crystal grain morphology of the high-nitrogen austenitic stainless steel.
Drawings
FIG. 1 is a metallographic structure diagram of a sample obtained by etching in example 4;
FIG. 2 is a metallographic structure of a sample obtained by etching in example 5;
FIG. 3 is a metallographic structure of a sample obtained by etching in example 6;
FIG. 4 is a metallographic diagram of a sample obtained by etching in example 7;
FIG. 5 is a metallographic structure diagram of a sample obtained by etching in comparative example 1;
FIG. 6 is a metallographic structure of a sample obtained by etching in comparative example 2.
Detailed Description
The following describes the embodiments of the present invention further with reference to the drawings. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Example 1
A high-nitrogen austenitic stainless steel corrosive agent is prepared from perchloric acid with the volume fraction of 3% and alcohol with the volume fraction of 97%.
Further, the N content in the high-nitrogen austenitic stainless steel is more than or equal to 0.45%.
Further, the concentration of the perchloric acid is 70-72%.
Further, the alcohol is absolute ethanol.
Example 2
The high nitrogen austenitic stainless steel corrosive agent is prepared by changing the ratio of perchloric acid to alcohol compared with the example 1, specifically, the high nitrogen austenitic stainless steel corrosive agent is prepared by perchloric acid with the volume fraction of 5% and alcohol with the volume fraction of 95%.
Example 3
The high nitrogen austenitic stainless steel corrosive agent is prepared by changing the ratio of perchloric acid to alcohol compared with the example 1, specifically, the high nitrogen austenitic stainless steel corrosive agent is prepared by perchloric acid with the volume fraction of 8% and alcohol with the volume fraction of 92%.
Example 4
A method of corrosion of high nitrogen austenitic stainless steel comprising the steps of:
s1, configuring the high-nitrogen austenitic stainless steel corrosive agent described in the embodiment 1: sequentially adding 97ml of alcohol and 3ml of perchloric acid, uniformly stirring, and standing for more than 2 hours;
S2, embedding a sample: placing a high-nitrogen austenitic stainless steel sample in a inlaying machine, and carrying out cold inlaying by using phenolic resin powder, wherein the inlaying temperature is room temperature and the inlaying time is 15min; the high-nitrogen austenitic stainless steel sample comprises the following specific alloy components in parts by weight: 21% Cr,19% Mn,2% Ni,1% Mo and the balance N;
S3, grinding and polishing: sequentially polishing and polishing the detection surface of the sample to be detected by using sand paper until scratches, pits and stains on the surface of the detection surface are removed, so that the surface is smooth and bright, flushing the polished detection surface by using running water, scrubbing by using alcohol and drying; the polishing method comprises the following steps: sequentially polishing with 320-mesh, 600-mesh, 1000-mesh, 1500-mesh, 2000-mesh, 3000-mesh, 5000-mesh and 7000-mesh sand paper under flowing water; the polishing method comprises the following steps: firstly, carrying out rough polishing by using flocking polishing cloth and diamond polishing paste with the granularity of 5 mu m, and after polishing marks are removed and the polishing mark directions are consistent, carrying out fine polishing by using cashmere polishing cloth and diamond polishing paste with the granularity of 1 mu m until the surface is specular gloss and no polishing mark is observed under an optical microscope;
S4, metallographic corrosion: the sample is used as an anode and is connected with the anode of a power supply, platinum is used as a cathode and is connected with the cathode of the power supply, the sample is immersed into the high-nitrogen austenitic stainless steel corrosive liquid prepared in the step S1, then a direct-current stabilized power supply is connected for corrosion, the sample is taken out until the polished surface of the sample presents silver gray, and the sample is washed with clear water and alcohol in sequence and then dried; the power supply is a direct current stabilized voltage power supply, the voltage is 3v, and the electrifying time is 40s.
The sample corroded by the method is observed under a microscope, and the metallographic structure obtained by observation is shown in fig. 1, so that a part of grain boundaries are corroded.
Example 5
The method of etching high nitrogen austenitic stainless steel was the same as in example 4 except that the etchant prepared in step S1 and the voltage and time of energization in step S4 were different. Specifically, the high nitrogen austenitic stainless steel etchant configured was the high nitrogen austenitic stainless steel etchant described in example 2: sequentially adding 95ml of alcohol and 5ml of perchloric acid, uniformly stirring, and standing for more than 2 hours; the voltage in the step S4 is 5v, and the power-on time is 10S.
The sample corroded by the method is observed under a microscope, and the metallographic structure obtained by observation is shown in figure 2, so that the crystal boundary is clear, complete and uniform, the corrosion effect is good, and the observation is easy.
Example 6
The method of etching high nitrogen austenitic stainless steel was the same as in example 4 except that the etchant prepared in step S1 and the voltage and time of energization in step S4 were different. Specifically, the high nitrogen austenitic stainless steel etchant configured was the high nitrogen austenitic stainless steel etchant described in example 2: sequentially adding 95ml of alcohol and 5ml of perchloric acid, uniformly stirring, and standing for more than 2 hours; in the step S4, the voltage is 5v, and the power-on time is 15S.
The sample corroded by the method is observed under a microscope, and the metallographic structure obtained by observation is shown in figure 3, so that the crystal boundary is clear, complete and uniform, the corrosion effect is good, the observation is easy, and the metallographic structure is clearer than that of figure 2.
Example 7
The method of etching high nitrogen austenitic stainless steel was the same as in example 4 except that the etchant prepared in step S1 and the voltage and time of energization in step S4 were different. Specifically, the high nitrogen austenitic stainless steel etchant configured was the high nitrogen austenitic stainless steel etchant described in example 3: sequentially adding 92ml of alcohol and 8ml of perchloric acid, uniformly stirring, and standing for more than 2 hours; the voltage in the step S4 is 8v, and the power-on time is 2S.
The sample corroded by the method is observed under a microscope, and the metallographic structure obtained by observation is shown in fig. 4, and the corrosion of part of grain boundaries is corroded, but the corrosion is uneven, and the corrosion effect is better at the part close to the boundary of the sample, at the moment, the grain boundaries in the sample are shallower, and the effect is inferior to that of examples 5 and 6.
Comparative example 1
A metallographic etching method of high-nitrogen austenitic stainless steel is the same as the rest except that the etchant prepared in the step S1 and the S4 etching are different from those of the embodiment 5. Specifically, step S1 is as follows: preparing CuCl 2 corrosive liquid: 4g of copper sulfate, 20mL of deionized water and 22mL of concentrated hydrochloric acid with the concentration of 38% are sequentially added into a beaker, the mixture is continuously stirred by a glass rod, and the mixture is kept stand for more than 10 minutes for standby after the copper sulfate is completely dissolved. Step S4, corrosion: dipping the CuCl 2 corrosive liquid prepared in the step S1 by absorbent cotton, repeatedly wiping the surface of the sample for 8S until the polished surface of the sample is silver gray, sequentially flushing with clear water and alcohol, and drying.
The sample corroded by the method is observed under a microscope, and the metallographic structure obtained by observation is shown in figure 5, so that the corrosion is shallow, only partial grain boundaries appear, and a few fine polishing marks appear along with the corrosion, and the corrosion effect is poor.
Comparative example 2
A metallographic etching method of high-nitrogen austenitic stainless steel is the same as the rest except that the etchant prepared in the step S1 and the S4 etching are different from those of the embodiment 5. Specifically, step S1 is as follows: preparing aqua regia corrosive liquid: 60mL of concentrated hydrochloric acid with the concentration of 38% and 20mL of concentrated nitric acid with the concentration of 68% are sequentially added into a beaker, the mixture is continuously stirred by a glass rod, and the mixture is kept stand for more than 10 minutes for later use after the solution is uniformly mixed. Step S4, corrosion: immersing the polished sample into the aqua regia corrosive liquid prepared in the step S1, corroding for 80S until the polished surface of the sample presents silver gray, sequentially flushing with clear water and alcohol, and drying.
The sample corroded by the method is observed under a microscope, the metallographic structure obtained by observation is shown as figure 6, the surface of the sample is corroded unevenly, one part of dendrites are corroded excessively, and the other part of dendrites are not corroded; the dendrite profile is blurred and the corrosion effect is poor.
The embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.

Claims (10)

1. A high nitrogen austenitic stainless steel corrosive agent, characterized by: the water-based paint is prepared from 3-8% of perchloric acid and 92-97% of alcohol.
2. The high nitrogen austenitic stainless steel corrosive of claim 1, wherein: it is prepared from perchloric acid with the volume fraction of 5% and alcohol with the volume fraction of 95%.
3. The high nitrogen austenitic stainless steel corrosive of claim 1, wherein: the content of N in the high-nitrogen austenitic stainless steel is more than or equal to 0.45 percent.
4. The high nitrogen austenitic stainless steel corrosive according to claim 2, wherein: the concentration of the perchloric acid is 70-72%.
5. The high nitrogen austenitic stainless steel corrosive according to claim 2, wherein: the alcohol is absolute ethanol.
6. A method for corrosion of high nitrogen austenitic stainless steel, characterized by: the method comprises the following steps:
s1, configuring the high-nitrogen austenitic stainless steel corrosive agent as claimed in claims 1-5: sequentially adding alcohol and perchloric acid according to the formula proportion, uniformly stirring, and standing for more than 2 hours;
s2, embedding a sample;
S3, grinding and polishing;
S4, metallographic corrosion: and (3) taking the sample as an anode and connecting the sample with the anode of a power supply, taking platinum as a cathode and connecting the sample with the cathode of the power supply, immersing the sample in the high-nitrogen austenitic stainless steel corrosive liquid prepared in the step (S1), then switching on a direct-current stabilized power supply to corrode the sample until the polished surface of the sample is silver gray, taking out the sample, sequentially flushing the sample with clear water and alcohol, and drying the sample.
7. The method of corrosion of high nitrogen austenitic stainless steel of claim 6, wherein: the specific method of the step S3 is as follows: and (3) sequentially polishing and polishing the detection surface of the sample to be detected by using sand paper until scratches, pits and stains on the surface of the detection surface are removed, so that the surface is smooth and bright, flushing the polished detection surface by using running water, scrubbing by using alcohol and drying.
8. The method of corrosion of high nitrogen austenitic stainless steel of claim 7, wherein: the polishing method comprises the following steps: sequentially polishing with 320 mesh, 600 mesh, 1000 mesh, 1500 mesh, 2000 mesh, 3000 mesh, 5000 mesh and 7000 mesh sand paper under flowing water.
9. The method of corrosion of high nitrogen austenitic stainless steel of claim 7, wherein: the polishing method in the step S3 is as follows: firstly, carrying out rough polishing by using flocking polishing cloth and diamond polishing paste with the granularity of 5 mu m, and after polishing marks are removed and the polishing mark directions are consistent, carrying out fine polishing by using cashmere polishing cloth and diamond polishing paste with the granularity of 1 mu m until the surface is specular gloss and no polishing mark is observed under an optical microscope.
10. The method of corrosion of high nitrogen austenitic stainless steel of claim 6, wherein: the power supply in the step S4 is a direct current stabilized voltage power supply, the voltage is 3-8 v, and the electrifying time is 2-40S.
CN202410399788.1A 2024-04-03 2024-04-03 High-nitrogen austenitic stainless steel corrosive and corrosion method Pending CN118360654A (en)

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