CN112284860A - Etching agent for displaying austenitic structure of heat-resistant steel for air valve and using method - Google Patents
Etching agent for displaying austenitic structure of heat-resistant steel for air valve and using method Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 60
- 239000010959 steel Substances 0.000 title claims abstract description 60
- 238000005530 etching Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 86
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 65
- 238000005406 washing Methods 0.000 claims abstract description 54
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000008399 tap water Substances 0.000 claims abstract description 35
- 235000020679 tap water Nutrition 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 29
- 230000003628 erosive effect Effects 0.000 claims abstract description 24
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 18
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 18
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000007664 blowing Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 22
- 230000001066 destructive effect Effects 0.000 claims description 18
- 238000005520 cutting process Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- 238000005498 polishing Methods 0.000 claims description 11
- 229910000617 Mangalloy Inorganic materials 0.000 claims description 2
- 238000004445 quantitative analysis Methods 0.000 abstract 1
- 229910001566 austenite Inorganic materials 0.000 description 21
- 239000007789 gas Substances 0.000 description 12
- 239000013078 crystal Substances 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- 238000000265 homogenisation Methods 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 238000004881 precipitation hardening Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
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- 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
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- G01N1/31—Apparatus therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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Abstract
The invention discloses an erosion agent for displaying the austenitic structure of heat-resistant steel for an air valve and a using method thereof. The erosion agent is divided into an erosion agent 1 and an erosion agent 2, wherein the erosion agent 1 is prepared from ferric trichloride, hydrochloric acid and water, and the erosion agent 2 is prepared from anhydrous copper sulfate, sulfuric acid, hydrochloric acid and glycerol. The using method comprises the following steps: (1) preparing an etching agent; (2) sample preparation: (3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, standing for 10-30 s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen by blowing; then, immersing the sample into a culture dish filled with an etchant 2, standing for 10-20 s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; a clear and intact room temperature austenitic structure was observed under a microscope. By adopting the erosion agent and the using method provided by the invention, the quality of the metallographic structure of the heat-resistant steel for the air valve can be obviously improved, and the accuracy of metallographic quantitative analysis is improved; and the erosion agent is simple to prepare and easy to popularize.
Description
Technical Field
The invention belongs to the technical field of metallographic detection, and particularly relates to an etchant for displaying an austenitic structure of heat-resistant steel for an air valve and a using method of the etchant.
Background
The air valve is an important working part and a vulnerable part on an engine, the working condition of the air valve is extremely poor, the air valve is subject to frequent reciprocating high-speed motion and friction in high-temperature, high-pressure and corrosive gas, and the impact load is large, so that the air valve is required to have higher high-temperature performance, corrosion resistance and the like, the working performance of the air valve is directly influenced by the working quality of the air valve, and the material requirement for preparing the air valve is also extremely strict. Currently, the most widely used air valve steel material is austenitic heat-resistant steel.
The steel uses austenite as a matrix, and carbon and nitrogen compounds as precipitation hardening phases are dispersed and distributed to obtain enough high-temperature strength, toughness, higher hardness and wear resistance, and the stability of the structure and better oxidation resistance and corrosion resistance under the condition of cold and hot addition, and is widely used for manufacturing exhaust valves of engines of automobiles and motorcycles.
The heat-resistant steel for the air valve shows that the structure is austenite at room temperature, and a clear and complete microstructure cannot be obtained by adopting the traditional nital solution for corrosion.
Disclosure of Invention
The invention aims to provide an erosion agent for displaying the austenitic structure of heat-resistant steel for an air valve and a using method thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the etchant for displaying the austenitic structure of the heat-resistant steel for the air valve is divided into an etchant 1 and an etchant 2, wherein the etchant 1 is prepared from ferric trichloride, hydrochloric acid and water, and the etchant 2 is prepared from anhydrous copper sulfate, sulfuric acid, hydrochloric acid and glycerol.
Further, the invention relates to an etchant for displaying the austenitic structure of high manganese steel for ultralow temperature environment, wherein: the proportion of the destructive agent 1 is as follows: 5g of ferric trichloride, 35-50 ml of hydrochloric acid and 100ml of water; the proportion of the destructive agent 2 is as follows: 10g of anhydrous copper sulfate, 10-15 ml of sulfuric acid, 100ml of hydrochloric acid and 5-10 ml of glycerol.
The use method of the erosion agent for displaying the austenitic structure of the heat-resistant steel for the air valve comprises the following steps:
(1) preparing an etchant: adding ferric trichloride and hydrochloric acid into water respectively, and stirring uniformly to prepare an etching agent 1; respectively slowly adding anhydrous copper sulfate, sulfuric acid and glycerol into hydrochloric acid, and uniformly stirring to prepare an etching agent 2;
(2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding a surface to be detected of the sample on coarse-to-fine abrasive paper, polishing, washing the polished surface with tap water, washing with absolute ethyl alcohol with the mass fraction of 99.5%, and drying;
(3) sample erosion: immersing the metallographic sample prepared in the step (2) into a culture dish filled with an etchant 1 in a mode that the surface to be detected is downward, standing for 10-30 s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; then, immersing the sample into a culture dish filled with an etchant 2, standing for 10-20 s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the austenitic structure was observed under a microscope.
Further, the use method of the destructive agent of the invention comprises the following steps: the proportion of the aggressive agent 1 in the step (1) is as follows: 5g of ferric trichloride, 35-50 ml of hydrochloric acid and 100ml of water; the proportion of the destructive agent 2 is as follows: 10g of anhydrous copper sulfate, 10-15 ml of sulfuric acid, 100ml of hydrochloric acid and 5-10 ml of glycerol.
Further, the use method of the destructive agent of the invention comprises the following steps: in the step (1), the mass fraction concentration of the sulfuric acid is 69%, and the mass fraction concentration of the hydrochloric acid is 37%.
Further, the use method of the destructive agent of the invention comprises the following steps: in the step (1), the sulfuric acid, the hydrochloric acid and the glycerol are all analytically pure.
Further, the use method of the destructive agent of the invention comprises the following steps: in the step (2) and the step (3), the absolute ethyl alcohol is analytically pure.
Further, the use method of the destructive agent of the invention comprises the following steps: in the step (2), the size of the metallographic specimen is smaller than 400mm by the area of the check surface2The height of the sample is preferably 15mm to 20 mm.
Further, the use method of the destructive agent of the invention comprises the following steps: the specific operation of drying in the step (2) and the step (3) is as follows: and selecting a cold air gear by a blower, wherein the air direction is horizontal to the surface of the sample, and blowing until the surface is dry and no absolute ethyl alcohol remains.
The principle of the invention is as follows:
the sulfuric acid solution with higher concentration is selected because the heat-resistant steel for the air valve has an austenite structure at room temperature, and the low-concentration sulfuric acid solution is difficult to completely display the grain boundary and the twin boundary. Hydrochloric acid and glycerol are used as corrosive agents, oxidation products generated in the corrosion process are dissolved by the acidity of the hydrochloric acid, a surface oxidation layer is eliminated, and the glycerol is added, so that the glycerol does not react with metal, the corrosion of the hydrochloric acid to the interior of the crystal is slowed down, the contrast difference between a crystal boundary and the interior of the crystal is enhanced, and the metallographic observation is facilitated.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: 1. the invention starts from selecting the erosion agent for preparing the metallographic sample of the heat-resistant steel for the air valve, so that the grain boundary and the twin grain boundary of the heat-resistant steel for the air valve are clearer and the structure is easier to identify. 2. The etchant adopted by the invention is simple and applicable to preparation, low in cost and easy to popularize and use in a laboratory. 3. The method provided by the invention can be used for remarkably improving the quality of the metallographic structure of the heat-resistant steel for the gas valve, improving the definition degree of crystal boundaries and twin crystal boundaries, and further improving the calculation precision of the average grain size grade number of the heat-resistant steel for the gas valve. 4. The invention can be applied to the display of the austenitic structure of the heat-resistant steel for the air valve with similar components.
Drawings
FIG. 1 is a metallographic structure of a heat-resistant steel for a valve used in example 1;
FIG. 2 is a metallographic structure of a heat-resistant steel for a valve used in example 2;
FIG. 3 is a metallographic structure of a heat-resistant steel for a valve used in example 3;
FIG. 4 shows a metallographic structure of a heat-resistant steel for a valve used in example 4;
FIG. 5 shows a metallographic structure of a heat-resistant steel for a valve used in example 5;
FIG. 6 is a metallographic structure of heat-resistant steel for a valve used in example 6;
FIG. 7 is a metallographic structure of a heat-resistant steel for a valve used in example 7;
FIG. 8 is a metallographic structure of heat-resistant steel for a valve used in example 8;
FIG. 9 shows a metallographic structure of a heat-resistant steel for a valve used in example 9.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example 1
In this embodiment, taking a heat-resistant steel for a gas valve as an example, a sample is hot-rolled at 1150 ℃ for 15min and air-cooled, and the method for displaying the room-temperature austenite structure comprises the following steps:
1) preparing an etching agent: respectively adding 5g of ferric trichloride and 35ml of hydrochloric acid with the mass fraction of 37% into 100ml of water in sequence, and stirring uniformly to prepare an etching agent 1; respectively slowly adding 10g of anhydrous copper sulfate, 10ml of sulfuric acid and 5ml of glycerol into 100ml of hydrochloric acid with the mass fraction of 37%, and uniformly stirring to prepare an etching agent 2;
2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding and polishing the surface to be detected of the sample, wherein the polished surface is a mirror surface without scratches, washing the mirror surface with tap water, washing the mirror surface with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the mirror surface;
3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, standing for 10s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen; then, immersing the sample into a culture dish filled with an etchant 2, staying for 10s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the room temperature austenite structure was observed under a microscope.
The metallographic structure of the heat-resistant steel for the air valve is shown in fig. 1, and it can be seen from fig. 1 that the corrosion of the sample is uniform, the grain boundary is clear and complete, and the twin crystal grain boundary is obvious.
Example 2
In this embodiment, taking a heat-resistant steel for a gas valve as an example, a sample is hot-rolled at 1150 ℃ for 30min and air-cooled, and the method for displaying the room-temperature austenite structure comprises the following steps:
1) preparing an etching agent: respectively adding 5g of ferric trichloride and 35ml of hydrochloric acid with the mass fraction of 37% into 100ml of water in sequence, and stirring uniformly to prepare an etching agent 1; respectively slowly adding 10g of anhydrous copper sulfate, 10ml of sulfuric acid and 5ml of glycerol into 100ml of hydrochloric acid with the mass fraction of 37%, and uniformly stirring to prepare an etching agent 2;
2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding and polishing the surface to be detected of the sample, wherein the polished surface is a mirror surface and has no scratch, and the sample is washed clean by tap water and then washed by absolute ethyl alcohol with the mass fraction of 99.5 percent and dried by blowing;
3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, standing for 15s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen; then, immersing the sample into a culture dish filled with an etchant 2, staying for 15s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the room temperature austenite structure was observed under a microscope.
The metallographic structure of the heat-resistant steel for the air valve is shown in fig. 2, and it can be seen from fig. 2 that the corrosion of the sample is uniform, the grain boundary is clear and complete, and the twin crystal grain boundary is obvious.
Example 3
In this embodiment, taking a heat-resistant steel for a gas valve as an example, a sample is hot-rolled at 1150 ℃ for 45min and air-cooled, and the method for displaying the room-temperature austenite structure comprises the following steps:
1) preparing an etching agent: respectively adding 5g of ferric trichloride and 40ml of hydrochloric acid with the mass fraction of 37% into 100ml of water in sequence, and stirring uniformly to prepare an etching agent 1; respectively slowly adding 10g of anhydrous copper sulfate, 15ml of sulfuric acid and 5ml of glycerol into 100ml of hydrochloric acid with the mass fraction of 37%, and uniformly stirring to prepare an etching agent 2;
2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding and polishing the surface to be detected of the sample, wherein the polished surface is a mirror surface and has no scratch, and the sample is washed clean by tap water and then washed by absolute ethyl alcohol with the mass fraction of 99.5 percent and dried by blowing;
3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, standing for 15s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen; then, immersing the sample into a culture dish filled with an etchant 2, staying for 15s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the room temperature austenite structure was observed under a microscope.
The metallographic structure of the heat-resistant steel for the air valve is shown in fig. 3, and it can be seen from fig. 3 that the corrosion of the sample is uniform, the grain boundary is clear and complete, and the twin crystal grain boundary is obvious.
Example 4
In this embodiment, taking a heat-resistant steel for a gas valve as an example, a sample is hot-rolled at 1150 ℃ for 60min and air-cooled, and the method for displaying the room-temperature austenite structure comprises the following steps:
1) preparing an etching agent: respectively adding 5g of ferric trichloride and 40ml of hydrochloric acid with the mass fraction of 37% into 100ml of water in sequence, and stirring uniformly to prepare an etching agent 1; respectively slowly adding 10g of anhydrous copper sulfate, 15ml of sulfuric acid and 5ml of glycerol into 100ml of hydrochloric acid with the mass fraction of 37%, and uniformly stirring to prepare an etching agent 2;
2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding and polishing the surface to be detected of the sample, wherein the polished surface is a mirror surface and has no scratch, and the sample is washed clean by tap water and then washed by absolute ethyl alcohol with the mass fraction of 99.5 percent and dried by blowing;
3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, standing for 20s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen; then, immersing the sample into a culture dish filled with an etchant 2, staying for 20s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the room temperature austenite structure was observed under a microscope.
The metallographic structure of the heat-resistant steel for the air valve is shown in fig. 4, and the sample is uniformly corroded, the grain boundary is clear and complete, and the twin crystal grain boundary is obvious in fig. 4.
Example 5
In this embodiment, taking a heat-resistant steel for a gas valve as an example, a sample is subjected to solution treatment at 1050 ℃ for 15min, and air-cooled, and the method for displaying the room-temperature austenite structure comprises the following steps:
1) preparing an etching agent: respectively adding 5g of ferric trichloride and 45ml of hydrochloric acid with the mass fraction of 37% into 100ml of water in sequence, and stirring uniformly to prepare an etching agent 1; respectively slowly adding 10g of anhydrous copper sulfate, 10ml of sulfuric acid and 10ml of glycerol into 100ml of hydrochloric acid with the mass fraction of 37%, and uniformly stirring to prepare an etching agent 2;
2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding and polishing the surface to be detected of the sample, wherein the polished surface is a mirror surface and has no scratch, and the sample is washed clean by tap water and then washed by absolute ethyl alcohol with the mass fraction of 99.5 percent and dried by blowing;
3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, standing for 10s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen; then, immersing the sample into a culture dish filled with an etchant 2, staying for 15s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the room temperature austenite structure was observed under a microscope.
The metallographic structure of the heat-resistant steel for the air valve in the embodiment is shown in fig. 5, and it can be seen from fig. 5 that the sample is uniformly corroded, and the grain boundary is clear and complete.
Example 6
In this embodiment, taking a heat-resistant steel for a gas valve as an example, a sample is subjected to solution treatment at 1050 ℃ for 30min, and air-cooled, and the method for displaying the room-temperature austenite structure comprises the following steps:
1) preparing an etching agent: respectively adding 5g of ferric trichloride and 45ml of hydrochloric acid with the mass fraction of 37% into 100ml of water in sequence, and stirring uniformly to prepare an etching agent 1; respectively slowly adding 10g of anhydrous copper sulfate, 10ml of sulfuric acid and 10ml of glycerol into 100ml of hydrochloric acid with the mass fraction of 37%, and uniformly stirring to prepare an etching agent 2;
2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding and polishing the surface to be detected of the sample, wherein the polished surface is a mirror surface and has no scratch, and the sample is washed clean by tap water and then washed by absolute ethyl alcohol with the mass fraction of 99.5 percent and dried by blowing;
3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, standing for 15s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen; then, immersing the sample into a culture dish filled with an etchant 2, staying for 15s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the room temperature austenite structure was observed under a microscope.
The metallographic structure of the heat-resistant steel for the air valve in the embodiment is shown in fig. 6, and it can be seen from fig. 6 that the sample is uniformly corroded, and the grain boundary is clear and complete.
Example 7
In this embodiment, taking a heat-resistant steel for a gas valve as an example, a sample is subjected to solution treatment at 1050 ℃ for 45min, and air-cooled, and the method for displaying the room-temperature austenite structure comprises the following steps:
1) preparing an etching agent: respectively adding 5g of ferric trichloride and 45ml of hydrochloric acid with the mass fraction of 37% into 100ml of water in sequence, and stirring uniformly to prepare an etching agent 1; respectively slowly adding 10g of anhydrous copper sulfate, 10ml of sulfuric acid and 10ml of glycerol into 100ml of hydrochloric acid with the mass fraction of 37%, and uniformly stirring to prepare an etching agent 2;
2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding and polishing the surface to be detected of the sample, wherein the polished surface is a mirror surface and has no scratch, and the sample is washed clean by tap water and then washed by absolute ethyl alcohol with the mass fraction of 99.5 percent and dried by blowing;
3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, standing for 15s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen; then, immersing the sample into a culture dish filled with an etchant 2, staying for 20s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the room temperature austenite structure was observed under a microscope.
The metallographic structure of the heat-resistant steel for the air valve in the embodiment is shown in fig. 7, and it can be seen from fig. 7 that the sample is uniformly corroded, and the grain boundary is clear and complete.
Example 8
In the embodiment, taking the heat-resistant steel for the gas valve as an example, a sample is subjected to homogenization and solid solution treatment, wherein the homogenization temperature is 1150 ℃ and the time is 45 min; the method for displaying the room-temperature austenite structure of the steel plate through air cooling at the solid solution temperature of 750 ℃ for 15min comprises the following steps of:
1) preparing an etching agent: respectively adding 5g of ferric trichloride and 50ml of hydrochloric acid with the mass fraction of 37% into 100ml of water in sequence, and stirring uniformly to prepare an etching agent 1; respectively slowly adding 10g of anhydrous copper sulfate, 15ml of sulfuric acid and 10ml of glycerol into 100ml of hydrochloric acid with the mass fraction of 37%, and uniformly stirring to prepare an etching agent 2;
2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding and polishing the surface to be detected of the sample, wherein the polished surface is a mirror surface and has no scratch, and the sample is washed clean by tap water and then washed by absolute ethyl alcohol with the mass fraction of 99.5 percent and dried by blowing;
3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, staying for 25s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen; then, immersing the sample into a culture dish filled with an etchant 2, staying for 20s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the room temperature austenite structure was observed under a microscope.
The metallographic structure of the heat-resistant steel for the air valve in the embodiment is shown in fig. 8, and it can be seen from fig. 8 that the sample is uniformly corroded, and the grain boundary is clear and complete.
Example 9
In the embodiment, taking the heat-resistant steel for the gas valve as an example, a sample is subjected to homogenization and solid solution treatment, wherein the homogenization temperature is 1150 ℃ and the time is 60 min; the method for displaying the room-temperature austenite structure of the steel plate through air cooling at the solid solution temperature of 750 ℃ for 30min comprises the following steps:
1) preparing an etching agent: respectively adding 5g of ferric trichloride and 50ml of hydrochloric acid with the mass fraction of 37% into 100ml of water in sequence, and stirring uniformly to prepare an etching agent 1; respectively slowly adding 10g of anhydrous copper sulfate, 15ml of sulfuric acid and 10ml of glycerol into 100ml of hydrochloric acid with the mass fraction of 37%, and uniformly stirring to prepare an etching agent 2;
2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding and polishing the surface to be detected of the sample, wherein the polished surface is a mirror surface and has no scratch, and the sample is washed clean by tap water and then washed by absolute ethyl alcohol with the mass fraction of 99.5 percent and dried by blowing;
3) sample erosion: immersing the metallographic specimen prepared in the step (2) into a culture dish filled with an etchant 1 with the observation surface facing downwards, standing for 30s, taking out the specimen, washing the specimen with tap water, washing the specimen with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the specimen; then, immersing the sample into a culture dish filled with an etchant 2, staying for 20s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the room temperature austenite structure was observed under a microscope.
The metallographic structure of the heat-resistant steel for the air valve in the embodiment is shown in fig. 9, and it can be seen from fig. 9 that the sample is uniformly corroded, and the grain boundary is clear and complete.
Claims (9)
1. An etchant for displaying the austenitic structure of heat-resistant steel for air valves, which is characterized in that: the etchant comprises an etchant 1 and an etchant 2, wherein the etchant 1 is prepared from ferric trichloride, hydrochloric acid and water, and the etchant 2 is prepared from anhydrous copper sulfate, sulfuric acid, hydrochloric acid and glycerol.
2. The etchant for displaying the austenitic structure of high manganese steel for ultra-low temperature environment according to claim 1, wherein: the proportion of the destructive agent 1 is as follows: 5g of ferric trichloride, 35-50 ml of hydrochloric acid and 100ml of water; the proportion of the destructive agent 2 is as follows: 10g of anhydrous copper sulfate, 10-15 ml of sulfuric acid, 100ml of hydrochloric acid and 5-10 ml of glycerol.
3. The use method of the erosion agent for displaying the austenitic structure of heat-resistant steel for air valves as claimed in claim 1 or 2, wherein: the method comprises the following steps:
(1) preparing an etchant: adding ferric trichloride and hydrochloric acid into water respectively, and stirring uniformly to prepare an etching agent 1; respectively slowly adding anhydrous copper sulfate, sulfuric acid and glycerol into hydrochloric acid, and uniformly stirring to prepare an etching agent 2;
(2) sample preparation: cutting a heat-resistant steel sample for the air valve, grinding a surface to be detected of the sample on coarse-to-fine abrasive paper, polishing, washing the polished surface with tap water, washing with absolute ethyl alcohol with the mass fraction of 99.5%, and drying;
(3) sample erosion: immersing the metallographic sample prepared in the step (2) into a culture dish filled with an etchant 1 in a mode that the surface to be detected is downward, standing for 10-30 s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; then, immersing the sample into a culture dish filled with an etchant 2, standing for 10-20 s, taking out the sample, washing the sample with tap water, washing the sample with absolute ethyl alcohol with the mass fraction of 99.5%, and drying the sample; the austenitic structure was observed under a microscope.
4. The method of using an destructive agent according to claim 3, wherein: the proportion of the aggressive agent 1 in the step (1) is as follows: 5g of ferric trichloride, 35-50 ml of hydrochloric acid and 100ml of water; the proportion of the destructive agent 2 is as follows: 10g of anhydrous copper sulfate, 10-15 ml of sulfuric acid, 100ml of hydrochloric acid and 5-10 ml of glycerol.
5. Use of an destructive agent according to claim 3 or 4, characterized in that: in the step (1), the mass fraction concentration of the sulfuric acid is 69%, and the mass fraction concentration of the hydrochloric acid is 37%.
6. Use of an destructive agent according to claim 3 or 4, characterized in that: in the step (1), the sulfuric acid, the hydrochloric acid and the glycerol are all analytically pure.
7. Use of an destructive agent according to claim 3 or 4, characterized in that: in the step (2) and the step (3), the absolute ethyl alcohol is analytically pure.
8. Use of an destructive agent according to claim 3 or 4, characterized in that: in the step (2), the size of the metallographic specimen is smaller than 400mm by the area of the check surface2The height of the sample is preferably 15mm to 20 mm.
9. Use of an destructive agent according to claim 3 or 4, characterized in that: the specific operation of drying in the step (2) and the step (3) is as follows: and selecting a cold air gear by a blower, wherein the air direction is horizontal to the surface of the sample, and blowing until the surface is dry and no absolute ethyl alcohol remains.
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| CN116083909A (en) * | 2022-12-27 | 2023-05-09 | 成都先进金属材料产业技术研究院股份有限公司 | 9-12Cr series heat-resistant steel precipitated phase corrosive and display method |
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