CN114113086A - Preparation and application method of high-carbon high-alloy steel isothermal quenching tissue corrosive - Google Patents

Preparation and application method of high-carbon high-alloy steel isothermal quenching tissue corrosive Download PDF

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CN114113086A
CN114113086A CN202111341720.0A CN202111341720A CN114113086A CN 114113086 A CN114113086 A CN 114113086A CN 202111341720 A CN202111341720 A CN 202111341720A CN 114113086 A CN114113086 A CN 114113086A
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alloy steel
sample
isothermal quenching
carbon high
corrosive
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周丽娜
尹龙承
童锐
刘晓宇
索志鹏
杨晶
刘明
王文雪
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AVIC Harbin Bearing Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing 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
    • G01N2001/2866Grinding or homogeneising

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Abstract

A preparation and application method of a high-carbon high-alloy steel isothermal quenching tissue corrosive agent belongs to the field of analysis and test. The method solves the problems that the prior Lepera corrosive is forbidden to use picric acid as a raw material, and the conventional nitric acid alcohol corrosive is difficult to efficiently and accurately corrode and shows a metallographic structure of high-carbon high-alloy steel after isothermal quenching. Preparation: mixing the nitric acid alcohol solution with the volume fraction of 4-10% with the sodium metabisulfite solution with the mass fraction of 0.5-1%. Use of: firstly, wire cutting and sample preparation; secondly, grinding and polishing a sample; thirdly, corroding the sample; and fourthly, observing a metallographic structure. The invention has low cost, convenient and safe operation and no pollution; on the premise of ensuring safety, the corrosive is utilized to realize efficient and accurate observation, analysis and evaluation of the high-carbon high-alloy steel isothermal quenching structure so as to further evaluate the effectiveness of the isothermal quenching process; when in use, the ideal tissue topography can be obtained within 25 s. The method is suitable for metallographic etching of the high-carbon high-alloy steel isothermal quenching structure.

Description

Preparation and application method of high-carbon high-alloy steel isothermal quenching tissue corrosive
Technical Field
The invention belongs to the field of analysis and test, and particularly relates to a preparation method and a use method of a high-carbon high-alloy steel isothermal quenching tissue corrosive agent.
Background
The isothermal quenching heat treatment process is generally used for obtaining a composite structure of martensite and lower bainite so as to meet the requirement of the material on toughness, so that the isothermal quenching of the lower bainite is a metal toughening process which is commonly used for high-carbon high-alloy steel at present. Metallographic observation and analysis of the metallographic structure after quenching are generally required to evaluate the quality of the isothermal quenching process.
The Lepera reagent is a common corrosive used for observing metallographic structures after isothermal quenching, and the corrosive is composed of a 1:1 aqueous solution of sodium metabisulfite (10g/L) and a picric acid ethanol solution (40g/L), and even modified Lepera corrosive generally contains a picric acid solution. Picric acid, also known as trinitrophenol, is a main raw material of TNT explosives and is forbidden to be used in laboratories at present because it has certain harm to human health, environment and the like. The nitric alcohol is the most commonly used corrosive agent at present, but the corrosive effect of the nitric alcohol on the microstructure (martensite, bainite, carbide and the like) after isothermal quenching is not ideal. Therefore, the conventional common corrosive agent is difficult to realize efficient and accurate corrosion on the high-carbon high-alloy steel austempered structure, and directly influences the evaluation of heat treatment process parameters.
Disclosure of Invention
The invention aims to solve the problems that the prior Lepera corrosive is forbidden in raw material picric acid, and the conventional nitric acid alcohol corrosive is difficult to efficiently and accurately corrode and shows a metallographic structure of high-carbon high-alloy steel after isothermal quenching, and provides a preparation method and a use method of the high-carbon high-alloy steel isothermal quenching structure corrosive.
A preparation method of a corrosive agent for a high-carbon high-alloy steel isothermal quenching structure is realized according to the following steps:
firstly, preparing a nitric acid alcohol solution with the volume fraction of 4-10%, and then preparing a sodium metabisulfite solution with the mass fraction of 0.5-1%;
and secondly, mixing the alcohol nitrate solution and the sodium metabisulfite solution according to the volume ratio of 1mL (0.2-1) mL to obtain the high-carbon high-alloy steel isothermal quenching tissue corrosive agent, and finishing the preparation method.
The use method of the high-carbon high-alloy steel isothermal quenching structure corrosive is realized by the following steps:
firstly, wire cutting sample preparation: performing line cutting on a high-carbon high-alloy steel isothermal quenching part or sample needing metallographic structure observation by using line cutting equipment, and setting the size of the sample according to the requirement of subsequent grinding and polishing sample preparation to obtain a sample after line cutting;
secondly, grinding and polishing sample preparation: grinding, polishing, cleaning and blow-drying the sample subjected to the linear cutting by using a pre-grinding machine or a full-automatic grinding and polishing machine to obtain a mirror surface sample;
thirdly, sample corrosion: corroding the mirror surface sample by using a high-carbon high-alloy steel isothermal quenching structure corrosive agent, adopting drop corrosion or immersion corrosion, immediately washing the mirror surface sample by using running water after the corrosion is finished, then washing the mirror surface sample by using absolute ethyl alcohol, and drying the mirror surface sample by blowing to obtain a metallographic sample;
fourthly, metallographic structure observation: and observing and analyzing the metallographic specimen by using a metallographic microscope to obtain the microstructure morphology of the high-carbon high-alloy steel after isothermal quenching, thereby completing the using method.
The invention has the advantages that:
the high-carbon high-alloy steel isothermal quenching structure corrosive prepared by the invention does not adopt forbidden components, is simple to prepare, low in cost, convenient and safe to operate, easy to control and free of pollution.
The invention solves the defects of the existing corrosive, provides the preparation and use method of the metallographic corrosive with high efficiency, good effect and high safety, and realizes efficient and accurate observation, analysis and evaluation of the high-carbon high-alloy steel isothermal quenching structure by using the corrosive on the premise of ensuring safety so as to further evaluate the effectiveness of the isothermal quenching process.
When the corrosive disclosed by the invention is used, an ideal tissue morphology graph can be obtained only in 25s, and after the corrosive disclosed by the invention is used for corrosion, the contrast among phases is obvious, wherein carbides are bright white, short rod-shaped bainite is black, needle-shaped martensite is brown, and part of grain boundary martensite is blue.
The method is suitable for metallographic etching of the high-carbon high-alloy steel isothermal quenching structure.
Drawings
FIG. 1 is a metallographic image of a microstructure obtained by carrying out 25s of dropwise etching on 18Cr4Mo4V high-carbon high-alloy steel by using an etchant after the high-carbon high-alloy steel is subjected to treatment by an isothermal quenching process 1 in example;
FIG. 2 is a metallographic image of a microstructure obtained by performing 25s of corrosion dropping on 18Cr4Mo4V high-carbon high-alloy steel by using an etchant after the high-carbon high-alloy steel is subjected to the isothermal quenching process 2 in the example;
FIG. 3 is a metallographic image of a microstructure of a comparative group, in which 18Cr4Mo4V high-carbon high-alloy steel is subjected to immersion corrosion for 3min after being treated by an isothermal quenching process 1 in the example;
FIG. 4 is a metallographic image of a microstructure of a comparative group, in which 18Cr4Mo4V high-carbon high-alloy steel of the example is subjected to immersion corrosion for 8min after being treated by an isothermal quenching process 1;
FIG. 5 is a metallographic image of a microstructure of a comparative group, in which 18Cr4Mo4V high-carbon high-alloy steel is subjected to immersion corrosion for 3min after being treated by an isothermal quenching process 2 in example;
FIG. 6 is a metallographic phase diagram of a microstructure of a comparative group, which is obtained by soaking and corroding the 18Cr4Mo4V high-carbon high-alloy steel subjected to the isothermal quenching process 2 for 8 min.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the embodiment provides a preparation method of a high-carbon high-alloy steel isothermal quenching structure corrosive agent, which is realized by the following steps:
firstly, preparing a nitric acid alcohol solution with the volume fraction of 4-10%, and then preparing a sodium metabisulfite solution with the mass fraction of 0.5-1%;
and secondly, mixing the alcohol nitrate solution and the sodium metabisulfite solution according to the volume ratio of 1mL (0.2-1) mL to obtain the high-carbon high-alloy steel isothermal quenching tissue corrosive agent, and finishing the preparation method.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that in the first step, a nital solution with a volume fraction of 8% is prepared, and then a sodium metabisulfite solution with a mass fraction of 0.7% is prepared. The rest is the same as the first embodiment.
The third concrete implementation mode: the difference between the first embodiment and the second embodiment is that the alcohol nitrate solution and the sodium metabisulfite solution are mixed according to the volume ratio of 1mL to 0.8mL in the second embodiment. The rest is the same as the first embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is that the configuration of the nital solution in the first step: absolute ethyl alcohol is poured into a beaker, and then concentrated nitric acid with the mass fraction of 68% is added under the stirring state to prepare a nitric acid alcohol solution with the volume fraction of 4% -10%. Other steps and parameters are the same as those in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is that the sodium metabisulfite solution is prepared in the second step: the solute is sodium metabisulfite, and the solvent is distilled water. Other steps and parameters are the same as in one of the first to fourth embodiments.
The sixth specific implementation mode: the application method of the high-carbon high-alloy steel isothermal quenching structure corrosive agent in the embodiment is realized by the following steps:
firstly, wire cutting sample preparation: performing line cutting on a high-carbon high-alloy steel isothermal quenching part or sample needing metallographic structure observation by using line cutting equipment, and setting the size of the sample according to the requirement of subsequent grinding and polishing sample preparation to obtain a sample after line cutting;
secondly, grinding and polishing sample preparation: grinding, polishing, cleaning and blow-drying the sample subjected to the linear cutting by using a pre-grinding machine or a full-automatic grinding and polishing machine to obtain a mirror surface sample;
thirdly, sample corrosion: corroding the mirror surface sample by using a high-carbon high-alloy steel isothermal quenching structure corrosive agent, adopting drop corrosion or immersion corrosion, immediately washing the mirror surface sample by using running water after the corrosion is finished, then washing the mirror surface sample by using absolute ethyl alcohol, and drying the mirror surface sample by blowing to obtain a metallographic sample;
fourthly, metallographic structure observation: and observing and analyzing the metallographic specimen by using a metallographic microscope to obtain the microstructure morphology of the high-carbon high-alloy steel after isothermal quenching, thereby completing the using method.
In the third step of the embodiment, the steel is immediately flushed by running water so as to remove the remaining high-carbon high-alloy steel isothermal quenching structure corrosive agent.
The seventh embodiment: the sixth embodiment differs from the sixth embodiment in that a pre-mill is used in the first step: and sequentially polishing the cut test sample by using a 240# sand paper, a 400# sand paper, an 800# sand paper, a 1000# sand paper, a 1500# sand paper and a diamond polishing agent with the particle size of less than or equal to 3 mu m. Other steps and parameters are the same as those in the sixth embodiment.
The specific implementation mode is eight: the difference between the sixth or seventh embodiment is that, in the first step, a full-automatic polishing machine is used: and (3) carrying out sample inlaying treatment according to the aperture of the automatic grinding and polishing disk, and then selecting a proper grinding and polishing machine program to prepare a sample, wherein the size of the final suspension is required to be less than or equal to 3 mu m. Other steps and parameters are the same as those of the sixth or seventh embodiment.
The specific implementation method nine: the difference between this embodiment and one of the sixth to eighth embodiments is that, in the step one, the cleaning and drying are performed: and after being washed by clean water, the mixture is sprayed and washed by absolute ethyl alcohol and is dried. Other steps and parameters are the same as those in one of the sixth to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the sixth to ninth embodiments is that in the third step, if the drop etching is performed, the drop etching time is 5-120 s; if soaking corrosion is adopted, the soaking time is 5-30 s. Other steps and parameters are the same as those in one of the sixth to ninth embodiments.
The beneficial effects of the present invention are demonstrated by the following examples:
example (b):
a preparation method of a corrosive agent for a high-carbon high-alloy steel isothermal quenching structure is realized according to the following steps:
firstly, preparing a nitric acid alcohol solution with the volume fraction of 10%, and then preparing a sodium metabisulfite solution with the mass fraction of 1%;
and secondly, mixing the alcohol nitrate solution and the sodium metabisulfite solution according to the volume ratio of 1mL to 0.8mL to obtain the high-carbon high-alloy steel isothermal quenching tissue corrosive, and finishing the preparation method.
The preparation of the nital solution in the first step of this embodiment: pouring 180mL of absolute ethyl alcohol into a 300mL beaker, and adding 20mL of concentrated nitric acid with the mass fraction of 68% while stirring to prepare a nital solution with the volume fraction of 10%.
Preparation of the sodium metabisulfite solution in step two of this example: 2g of sodium metabisulfite is weighed by an electronic balance and filter paper and poured into a 250mL beaker, 198mL of distilled water is added, and the mixture is fully stirred and dissolved by a glass rod to prepare a sodium metabisulfite solution with the mass fraction of 1%.
The application method of the high-carbon high-alloy steel isothermal quenching structure corrosive prepared by the method comprises the following steps:
firstly, wire cutting sample preparation: performing line cutting on a high-carbon high-alloy steel isothermal quenching part or sample needing metallographic structure observation by using line cutting equipment, and setting the size of the sample according to the requirement of subsequent grinding and polishing sample preparation to obtain a sample after line cutting;
secondly, grinding and polishing sample preparation: grinding, polishing, cleaning and blow-drying the sample subjected to the linear cutting by using a pre-grinding machine or a full-automatic grinding and polishing machine to obtain a mirror surface sample;
thirdly, sample corrosion: corroding the mirror surface sample by using a high-carbon high-alloy steel isothermal quenching structure corrosive agent, adopting drop corrosion or immersion corrosion, immediately washing the mirror surface sample by using running water after the corrosion is finished, then washing the mirror surface sample by using absolute ethyl alcohol, and drying the mirror surface sample by blowing to obtain a metallographic sample;
fourthly, metallographic structure observation: and observing and analyzing the metallographic specimen by using a metallographic microscope to obtain the microstructure morphology of the high-carbon high-alloy steel after isothermal quenching, thereby completing the using method.
The operation of this example is as follows:
respectively carrying out linear cutting sampling on the 8Cr4Mo4V high-carbon high-alloy bearing steel treated by two different isothermal quenching processes, and taking a phi 12 multiplied by 15mm sample;
two different isothermal quenching processes are respectively a process 1: keeping the temperature of 1105 ℃ for 30min, and then keeping the temperature in a salt bath with the temperature of 200 ℃ for 2h for isothermal quenching treatment; and (2) a process: the temperature is kept for 30min at 1120 ℃, and then isothermal quenching treatment is carried out by keeping the temperature in a salt bath at 200 ℃ for 2 h.
Embedding the sample by using a phi 30mm cold embedding die and a metallographic special embedding material; then, grinding and polishing the sample by using an automatic grinding and polishing machine (Tegraminin-25, Struers company), setting a program to sequentially use 9-micron, 3-micron and 1-micron suspensions, and washing and drying the sample by using flowing water and absolute ethyl alcohol in sequence after the grinding and polishing are finished to obtain a mirror surface sample;
high-carbon high-alloy steel isothermal quenching structure corrosive agent: 10mL of the prepared 10% nital solution and 8mL of the prepared 1% sodium metabisulfite solution are poured into a 25mL beaker in sequence and are fully stirred to obtain a mixed corrosive agent;
taking the mixed corrosive agent by using a rubber head dropper to quickly cover the surface of the mirror surface sample, carrying out drop etching, keeping for 25s, then washing by using flowing water and absolute ethyl alcohol, and drying to obtain a metallographic sample;
under the condition that other step parameters are not changed, in order to form a contrast with the traditional nitric acid alcohol corrosion effect, the sample under the same process is subjected to soaking corrosion treatment by using the prepared 10% nitric acid alcohol solution to obtain a metallographic sample (marked as a contrast group).
Respectively carrying out metallographic structure observation and analysis on the metallographic samples by using a metallographic microscope (NIM-910, Nanjing Yongxin company), and obtaining the martensite compound structure morphology of the high-carbon high-alloy steel after isothermal quenching by adopting a magnification of 1000 times;
as a result, as shown in fig. 1, it can be seen that after the 8Cr4Mo4V high-carbon high-alloy steel in this embodiment is processed by the isothermal quenching process 1, when the corrosive in this embodiment is used, an ideal microstructure morphology diagram can be obtained in only 25 seconds, and it can be seen that after the corrosive in this embodiment is used, the contrast between phases is relatively obvious, wherein carbides are bright white, the "short rod" bainite is black, needle-like martensite is brown, and a part of grain boundary martensite is blue.
The results of the control group of 8Cr4Mo4V steel treated by the same process of 10% nitric acid alcohol corrosion are shown in figures 3 and 4, and it can be seen that when the steel is soaked and corroded for 3min (shown in figure 3), only clear grain boundaries can be seen, and the carbide contrast is similar to that of a matrix; when the corrosion time is prolonged to 8min (shown in figure 4), the 'short rod-shaped' bainite in the interior of the crystal grains can be seen, and the martensite structure is not corroded.
The 8Cr4Mo4V steel treated by the isothermal quenching process 2 is corroded by the corrosive agent and 10% nitric acid alcohol of the embodiment, and the results are shown in the attached drawings 2, 5 and 6 respectively; as can be seen from FIG. 2, the contrast between the phases is more obvious after the etching by the etchant of the present embodiment, wherein the carbide is bright white, the "short rod" bainite is black, and the acicular martensite is brown.
8Cr4Mo4V steel treated by the same process is corroded by 10% nitric acid alcohol, and the results of the control group are shown in FIGS. 5 and 6; it can be seen that when the immersion etching is carried out for 3min (shown in fig. 5), only a clearer grain boundary can be seen, and the carbide contrast is similar to that of the matrix in the same way as in the process 1; when the corrosion time is prolonged to 8min (shown in figure 6), the 'short rod-shaped' bainite in the interior of the crystal grains can be seen, and the martensite structure is not corroded.

Claims (10)

1. A preparation method of a high-carbon high-alloy steel isothermal quenching structure corrosive agent is characterized by comprising the following steps:
firstly, preparing a nitric acid alcohol solution with the volume fraction of 4-10%, and then preparing a sodium metabisulfite solution with the mass fraction of 0.5-1%;
and secondly, mixing the alcohol nitrate solution and the sodium metabisulfite solution according to the volume ratio of 1mL (0.2-1) mL to obtain the high-carbon high-alloy steel isothermal quenching tissue corrosive agent, and finishing the preparation method.
2. The method for preparing corrosive agent for austempered structure of high carbon high alloy steel as set forth in claim 1, wherein in the first step, 8% by volume of nital solution is prepared, and then 0.7% by mass of sodium metabisulfite solution is prepared.
3. The method for preparing the corrosive agent for the austempered structure of high-carbon high-alloy steel according to claim 1, wherein the alcohol nitrate solution and the sodium metabisulfite solution are mixed according to a volume ratio of 1mL to 0.8mL in the second step.
4. The method for preparing the corrosive agent for the austempered structure of high-carbon high-alloy steel according to claim 1, wherein the preparation of the nital solution in the step one is as follows: absolute ethyl alcohol is poured into a beaker, and then concentrated nitric acid with the mass fraction of 68% is added under the stirring state to prepare a nitric acid alcohol solution with the volume fraction of 4% -10%.
5. The method for preparing the corrosive agent for the austempered structure of high-carbon high-alloy steel according to claim 1, wherein the sodium metabisulfite solution is prepared in the second step: the solute is sodium metabisulfite, and the solvent is distilled water.
6. The use method of the high-carbon high-alloy steel austempered structure corrosive prepared according to the claim 1 is characterized by comprising the following steps:
firstly, wire cutting sample preparation: performing line cutting on a high-carbon high-alloy steel isothermal quenching part or sample needing metallographic structure observation by using line cutting equipment, and setting the size of the sample according to the requirement of subsequent grinding and polishing sample preparation to obtain a sample after line cutting;
secondly, grinding and polishing sample preparation: grinding, polishing, cleaning and blow-drying the sample subjected to the linear cutting by using a pre-grinding machine or a full-automatic grinding and polishing machine to obtain a mirror surface sample;
thirdly, sample corrosion: corroding the mirror surface sample by using a high-carbon high-alloy steel isothermal quenching structure corrosive agent, adopting drop corrosion or immersion corrosion, immediately washing the mirror surface sample by using running water after the corrosion is finished, then washing the mirror surface sample by using absolute ethyl alcohol, and drying the mirror surface sample by blowing to obtain a metallographic sample;
fourthly, metallographic structure observation: and observing and analyzing the metallographic specimen by using a metallographic microscope to obtain the microstructure morphology of the high-carbon high-alloy steel after isothermal quenching, thereby completing the using method.
7. The use method of the high-carbon high-alloy steel austempered structure corrosive agent according to claim 6, characterized in that in the step one, a pre-grinding machine is utilized: and sequentially polishing the cut test sample by using a 240# sand paper, a 400# sand paper, an 800# sand paper, a 1000# sand paper, a 1500# sand paper and a diamond polishing agent with the particle size of less than or equal to 3 mu m.
8. The use method of the high-carbon high-alloy steel austempered structure corrosive agent according to claim 6, characterized in that in the step one, a full-automatic grinding and polishing machine is utilized: and (3) carrying out sample inlaying treatment according to the aperture of the automatic grinding and polishing disk, and then selecting a proper grinding and polishing machine program to prepare a sample, wherein the size of the final suspension is required to be less than or equal to 3 mu m.
9. The use method of the high-carbon high-alloy steel austempered structure corrosive agent according to claim 6, characterized in that the cleaning and blow-drying in the step one: and after being washed by clean water, the mixture is sprayed and washed by absolute ethyl alcohol and is dried.
10. The use method of the high-carbon high-alloy steel isothermal quenching structure corrosive agent according to claim 6, characterized in that in the third step, if the corrosion is carried out by dripping, the dripping time is 5 s-120 s; if soaking corrosion is adopted, the soaking time is 5-30 s.
CN202111341720.0A 2021-11-12 2021-11-12 Preparation and application method of high-carbon high-alloy steel isothermal quenching tissue corrosive Pending CN114113086A (en)

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