CN110453222B - Corrosive liquid for displaying austenite grain boundary of ultrahigh-strength steel, and preparation method and application thereof - Google Patents
Corrosive liquid for displaying austenite grain boundary of ultrahigh-strength steel, and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of displaying of austenite grain boundaries and intragranular microstructures of ultra-high strength steel, and discloses a corrosive liquid for displaying the austenite grain boundaries of the ultra-high strength steel, a preparation method and application thereof, wherein the corrosive liquid comprises the following components: glacial acetic acid, absolute ethyl alcohol; wherein the volume ratio of the glacial acetic acid to the absolute ethyl alcohol is as follows: 1: 3-7. The corrosive liquid for displaying the austenite grain boundary of the ultrahigh-strength steel, the preparation method and the application are used for solving the technical problems that the temperature and the corrosion time of a corrosive liquid preparation are difficult to control and a clearer corrosion effect cannot be obtained in the prior art.
Description
Technical Field
The invention belongs to the technical field of displaying of austenite grain boundaries and intragranular microstructures of ultrahigh-strength steel, and particularly relates to a corrosive liquid for displaying the austenite grain boundaries of the ultrahigh-strength steel, and a preparation method and application thereof.
Background
The ultra-high strength steel is generally considered that the tensile strength is not less than 1000MPa, and the ultra-high strength steel is applied to manufacturing various structural members and workpieces bearing higher stress due to the ultra-high strength, hardness and good toughness. The ultra-high strength steel can be classified into low alloy, medium alloy and high alloy ultra-high strength steel according to alloying degree and microstructure. The high-alloy ultrahigh-strength steel includes maraging steel, precipitation hardening stainless steel and the like. The microstructure of the ultra-high strength steel at the room temperature of 20 ℃ is mainly one or a combination of more of martensite, bainite and austenite. The volume ratio of the above microstructures is not less than 90%. The size of the austenite grain of the ultra-high strength steel has great influence on the microstructure morphology at room temperature, and the display technology of the ultra-high strength steel is very important. Numerous researchers have conducted research on austenite grain boundary corrosive agents and corrosion methods, which are summarized as follows:
1. most of the above reagents and methods mainly use saturated picric acid solution, detergent, copper sulfate, hydrofluoric acid, hydrochloric acid, xylene, etc. as auxiliary drugs. The proportion and content of each component, the corrosion temperature and the corrosion time are different. The corrosion reagent and the method are only effective for steel types with specific components;
2. most of the above corrosive solutions contain picric acid reagent. Picric acid and its main preparations have been listed in the latest catalog of dangerous chemicals (2015 edition) with CAS numbers 88-89-1, 3324-58-1, 131-74-8, 146-84-9, and 131-74-8, which are difficult to purchase and obtain in ordinary experimental process due to the hazardous properties of picric acid, such as toxicity and explosiveness. The invention needs to invent an austenite grain boundary corrosive agent without picric acid;
3. in the partial corrosion method, heating is needed in the corrosion process, the applicability to partial temperature-sensitive microstructures is poor, and additional heating treatment is needed, so that the difficulty and the cost of austenite display operation are increased;
4. aiming at the ultrahigh-strength steel researched by the invention, because bainite and martensite in a microstructure of the ultrahigh-strength steel at room temperature are in a body-centered cubic crystal structure, and residual austenite is in a cubic crystal oriented structure, and the 'corrosion activation energy' of the crystal structures of the two types is different, the conventional corrosion liquid on the market cannot obtain an austenite crystal boundary, only can obtain an intra-crystal bainite and martensite microstructure of the steel, and is inconvenient for judging the performance of the ultrahigh-strength steel researched by the invention.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention has three purposes: the purpose is to provide a corrosive liquid for displaying austenite grain boundary of ultrahigh-strength steel; the second purpose is to provide a preparation method of the corrosive liquid for displaying the austenite grain boundary of the ultrahigh-strength steel; the third purpose is to provide the application of the corrosive liquid for displaying the austenite grain boundary of the ultrahigh-strength steel, so as to solve the technical problems in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: an etching solution for displaying austenite crystal boundary of ultrahigh-strength steel, which comprises the following components: glacial acetic acid, absolute ethyl alcohol; wherein the volume ratio of the glacial acetic acid to the absolute ethyl alcohol is as follows: 1: 3-7.
Further, the corrosive liquid comprises the following components: glacial acetic acid, absolute ethyl alcohol; wherein the volume ratio of the glacial acetic acid to the absolute ethyl alcohol is as follows: 1: 3.
further, the corrosive liquid comprises the following components: glacial acetic acid, absolute ethyl alcohol; wherein the volume ratio of the glacial acetic acid to the absolute ethyl alcohol is as follows: 1: 5.
further, the corrosive liquid comprises the following components: glacial acetic acid, absolute ethyl alcohol; wherein the volume ratio of the glacial acetic acid to the absolute ethyl alcohol is as follows: 1: 7.
further, the alloy components of the ultrahigh-strength steel are, by weight, C: 0.15-0.25%, Si: 1.5-2.0%, Mn: 1.0-1.9%, P: less than or equal to 0.1 percent, S: less than or equal to 0.1 percent, Al: 0.1-0.2%, Nb + V + Ti + Cr + Mo + B: less than or equal to 2.6 percent, and the balance being Fe.
A preparation method of corrosive liquid for displaying austenite grain boundary of ultrahigh-strength steel comprises the following steps:
s1, taking glacial acetic acid and placing the glacial acetic acid in a beaker;
s2, pouring absolute ethyl alcohol into the beaker added with the glacial acetic acid in the step S1, and mixing the absolute ethyl alcohol with the glacial acetic acid to obtain the corrosive liquid showing the austenite crystal boundary of the ultrahigh-strength steel.
The application of the corrosive liquid for displaying the austenite grain boundary of the ultrahigh-strength steel is used for displaying the austenite grain boundary of the ultrahigh-strength steel, and in-crystal bainite and martensite.
Further, the use method of the corrosive liquid comprises the following steps:
s1, sample preparation: taking a metallographic sample, and carrying out hot inlaying on the metallographic sample to obtain a metallographic sample;
s2, grinding: grinding the metallographic sample obtained in the step S1 by using metallographic abrasive paper or a grinding machine until the surface scratches are shallow and only have one direction to obtain a ground metallographic sample;
s3, polishing: coating diamond polishing paste on the surface to be corroded of the ground metallographic specimen, and performing dry polishing on the surface to be corroded in a direction perpendicular to the scratches on a polishing machine until the scratches are almost eliminated, and performing water-adding wet polishing to obtain a scratch-free mirror surface;
s4, corrosion: placing the non-scratch mirror surface of the metallographic sample obtained in the step S3 in a prepared corrosive liquid in an upward mode, and standing for 10-40min at the corrosion environment temperature of 0-40 ℃;
s5, observation: and (5) taking out the metallographic sample obtained in the step (S4), cleaning the corroded surface by using water, cleaning the corroded surface by using alcohol, drying and observing.
The invention has the advantages that: the glacial acetic acid and the absolute ethyl alcohol selected by the invention are common chemical reagents, the toxicity of the glacial acetic acid and the absolute ethyl alcohol is far less than that of picric acid, the purchase is convenient, the method is relatively convenient and fast compared with the purchase of picric acid such as dangerous chemical reagents, and the purchase difficulty is reduced; the corrosive liquid for displaying the austenite grain boundary of the ultrahigh-strength steel provided by the invention can obtain a clearer austenite grain boundary without controlling the temperature; the preparation method is simple, and can be applied to displaying the austenite grain boundary of the ultrahigh-strength steel researched by the invention; according to the corrosion liquid disclosed by the invention, the research on the difference of corrosion activation energy existing between the corrosion liquid and the corrosion liquid skillfully utilizes the corrosion activation energy, so that the corrosion liquid can reach the corrosion activation energy of residual austenite within a controllable period of time, but can not reach the corrosion activation energy of bainite and martensite, and finally the bainite and the martensite are not displayed, but are only clearly displayed in austenite crystal boundaries.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a gold phase diagram of original austenite after corrosion of a sample of the same type of ultra-high strength steel by a corrosion solution of example 1 of the present invention;
FIG. 2 is a diagram of the original austenite gold phase after the same type of ultra-high strength steel sample is corroded by the corrosive liquid of example 2 of the invention;
FIG. 3 is a gold phase diagram of the original austenite of the same type of ultra-high strength steel sample after being corroded by the corrosive liquid of example 3 of the invention;
FIG. 4 is a diagram showing the original austenite gold phase after etching a sample of ultra-high strength steel with a picric acid-hydrochloric acid distilled water solution of comparative example 1 of the present invention as an etchant;
FIG. 5 is a photograph of the gold phase of the original austenite of a sample of super-high strength steel after being corroded by comparative example 2 Lawegian gull brand shampoo of the present invention and distilled water as a corrosive agent.
Detailed Description
The invention is further described with reference to the accompanying drawings and specific embodiments:
example 1
Preparing a corrosive liquid for displaying austenite grain boundary of the ultrahigh-strength steel:
s1, taking 10ml of glacial acetic acid and placing the glacial acetic acid in a beaker;
s2, pouring 30ml of absolute ethyl alcohol into the beaker added with the glacial acetic acid in the step S1, and mixing the absolute ethyl alcohol with the glacial acetic acid to obtain the corrosive liquid showing the austenite crystal boundary of the ultrahigh-strength steel.
The using method of the corrosive liquid comprises the following steps:
s1, sample preparation: taking a metallographic sample, and carrying out hot inlaying on the metallographic sample to obtain a metallographic sample;
s2, grinding: grinding the metallographic sample obtained in the step S1 by using metallographic abrasive paper or a grinding machine until the surface scratches are shallow and only have one direction to obtain a ground metallographic sample;
s3, polishing: coating diamond polishing paste on the surface to be corroded of the ground metallographic specimen, and performing dry polishing on the surface to be corroded in a direction perpendicular to the scratches on a polishing machine until the scratches are almost eliminated, and performing water-adding wet polishing to obtain a scratch-free mirror surface;
s4, corrosion: placing the non-scratch mirror surface of the metallographic sample obtained in the step S3 in a prepared corrosive liquid in an upward mode, and standing for 10min, wherein the temperature of a corrosive environment is 0 ℃;
s5, observation: and (5) taking out the metallographic sample obtained in the step (S4), cleaning the corroded surface by using water, cleaning the corroded surface by using alcohol, drying and observing.
Example 2
Preparing a corrosive liquid for displaying austenite grain boundary of the ultrahigh-strength steel:
s1, taking 10ml of glacial acetic acid and placing the glacial acetic acid in a beaker;
s2, pouring 70ml of absolute ethyl alcohol into the beaker added with the glacial acetic acid in the step S1, and mixing the absolute ethyl alcohol with the glacial acetic acid to obtain the corrosive liquid showing the austenite crystal boundary of the ultrahigh-strength steel.
The using method of the corrosive liquid comprises the following steps:
s1, sample preparation: taking a metallographic sample, and carrying out hot inlaying on the metallographic sample to obtain a metallographic sample;
s2, grinding: grinding the metallographic sample obtained in the step S1 by using metallographic abrasive paper or a grinding machine until the surface scratches are shallow and only have one direction to obtain a ground metallographic sample;
s3, polishing: coating diamond polishing paste on the surface to be corroded of the ground metallographic specimen, and performing dry polishing on the surface to be corroded in a direction perpendicular to the scratches on a polishing machine until the scratches are almost eliminated, and performing water-adding wet polishing to obtain a scratch-free mirror surface;
s4, corrosion: placing the non-scratch mirror surface of the metallographic sample obtained in the step S3 in a prepared corrosive liquid in an upward mode, and standing for 40min, wherein the temperature of a corrosive environment is 40 ℃;
s5, observation: and (5) taking out the metallographic sample obtained in the step (S4), cleaning the corroded surface by using water, cleaning the corroded surface by using alcohol, drying and observing.
Example 3
Preparing a corrosive liquid for displaying austenite grain boundary of the ultrahigh-strength steel:
s1, taking 10ml of glacial acetic acid and placing the glacial acetic acid in a beaker;
s2, pouring 50ml of absolute ethyl alcohol into the beaker added with the glacial acetic acid in the step S1, and mixing the absolute ethyl alcohol with the glacial acetic acid to obtain the corrosive liquid showing the austenite crystal boundary of the ultrahigh-strength steel.
The using method of the corrosive liquid comprises the following steps:
s1, sample preparation: taking a metallographic sample, and carrying out hot inlaying on the metallographic sample to obtain a metallographic sample;
s2, grinding: grinding the metallographic sample obtained in the step S1 by using metallographic abrasive paper or a grinding machine until the surface scratches are shallow and only have one direction to obtain a ground metallographic sample;
s3, polishing: coating diamond polishing paste on the surface to be corroded of the ground metallographic specimen, and performing dry polishing on the surface to be corroded in a direction perpendicular to the scratches on a polishing machine until the scratches are almost eliminated, and performing water-adding wet polishing to obtain a scratch-free mirror surface;
s4, corrosion: placing the non-scratch mirror surface of the metallographic sample obtained in the step S3 in a prepared corrosive liquid in an upward mode, and standing for 25min, wherein the temperature of a corrosive environment is 20 ℃;
s5, observation: and (5) taking out the metallographic sample obtained in the step (S4), cleaning the corroded surface by using water, cleaning the corroded surface by using alcohol, drying and observing.
Comparative example 1
Preparing a picric acid hydrochloric acid distilled water solution corrosive agent:
adding 70mL of distilled water into a small beaker, adding 1.5g of seagull brand shampoo paste and 2.5g of picric acid, putting the small beaker into a large beaker filled with water, heating the large beaker by using an electric stove to enable the small beaker to be in a water bath state, and adding one drop of xylene and a very small amount of CuCl2 (stirring) when the indicated temperature is 40 ℃; when the indicated temperature is 50 ℃ a drop of HCl and a drop of HF are added (stirring). When the indicated temperature is 54 ℃ (the actual temperature of the caustic is around 50 ℃), the incubation is for about 20-30 min.
Corroding the metallographic sample:
s1, sample preparation: taking a metallographic sample, and carrying out hot inlaying on the metallographic sample to obtain a metallographic sample;
s2, grinding: grinding the metallographic sample obtained in the step S1 by using metallographic abrasive paper or a grinding machine until the surface scratches are shallow and only have one direction to obtain a ground metallographic sample;
s3, polishing: coating diamond polishing paste on the surface to be corroded of the ground metallographic specimen, and performing dry polishing on the surface to be corroded in a direction perpendicular to the scratches on a polishing machine until the scratches are almost eliminated, and performing water-adding wet polishing to obtain a scratch-free mirror surface;
s4, corrosion: clamping the metallographic sample obtained in the step S3 by using a pair of tweezers, enabling the surface to be corroded to face upwards, putting the metallographic sample into a prepared corrosive agent, and controlling the metallographic sample to be shaken without stopping, wherein the time is controlled to be 15-35S, and the corrosion environment temperature is 0-40 ℃;
s5, observation: and (5) taking out the metallographic sample obtained in the step (S4), cleaning the corroded surface by using water, cleaning the corroded surface by using alcohol, drying and observing.
Comparative example 2
Preparing picric acid gull brand shampoo paste and adding distilled water corrosive agent:
adding 100mL distilled water into a small beaker, adding 4g of Haiou brand shampoo paste and 5g of picric acid, heating the large beaker by using an electric stove to enable the small beaker to be in a water bath state, boiling the corrosive agent for 3-5min, stopping heating, gradually cooling the corrosive agent to 60 ℃, and preserving heat.
Corroding the metallographic sample:
s1, sample preparation: taking a metallographic sample, and carrying out hot inlaying on the metallographic sample to obtain a metallographic sample;
s2, grinding: grinding the metallographic sample obtained in the step S1 by using metallographic abrasive paper or a grinding machine until the surface scratches are shallow and only have one direction to obtain a ground metallographic sample;
s3, polishing: coating diamond polishing paste on the surface to be corroded of the ground metallographic specimen, and performing dry polishing on the surface to be corroded in a direction perpendicular to the scratches on a polishing machine until the scratches are almost eliminated, and performing water-adding wet polishing to obtain a scratch-free mirror surface;
s4, corrosion: clamping the metallographic sample obtained in the step S3 by using tweezers, putting the metallographic sample into a prepared corrosive agent with the surface to be corroded facing upwards, shaking for a few times to ensure that the surface is fully corroded by the corrosive agent, and taking out the metallographic sample after keeping for 1 minute and 30 seconds;
s5, observation: and (5) taking out the metallographic sample obtained in the step (S4), cleaning the corroded surface by using water, cleaning the corroded surface by using alcohol, drying and observing.
The original austenite phase diagrams of fig. 1 to 5 show that the corrosive liquid provided by the invention and showing the austenite grain boundary of the ultra-high strength steel can clearly and completely show the austenite grain boundary of the ultra-high strength steel researched by the invention, while the austenite grain boundaries cannot be shown in comparative examples 1 and 2.
It should be explained that, in the embodiments 1 to 3, the selection of 0 ℃, 20 ℃ and 40 ℃ respectively is not that the etching solution for displaying the austenite grain boundary of the ultra-high strength steel and the in-crystal bainite and martensite provided by the present invention needs to be temperature controlled, but is to verify that the etching solution for displaying the austenite grain boundary of the ultra-high strength steel and the in-crystal bainite and martensite provided by the present invention can perform the etching operation under the room temperature conditions of different seasons and regions of 0 ℃, 20 ℃ and 40 ℃, thereby proving that the etching solution for displaying the austenite grain boundary of the ultra-high strength steel and the in-crystal bainite and martensite provided by the present invention can perform the etching operation at room temperature without heating.
Meanwhile, the corrosive liquid for displaying the austenite crystal boundary of the ultrahigh-strength steel and the bainite and martensite in the crystal can be taken out at any time in the corrosion process according to the observation requirement to observe, so that the corrosion process of the austenite crystal boundary can be observed and recorded conveniently, the operation is convenient, the corrosion process of the austenite crystal boundary can be clearly reflected, the ultrahigh-strength and rigidity performance can be predicted conveniently in the later period, and the accuracy of the prediction of the ultrahigh-strength and rigidity performance can be ensured.
The above description is only exemplary of the present invention, and not intended to limit the present invention, and any modifications, equivalents, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Other technical features than those described in the specification are known to those skilled in the art, and are not described in detail herein in order to highlight the novel features of the present invention.
Claims (6)
1. The application of the corrosive liquid in displaying the austenite crystal boundary of the ultrahigh-strength steel and not displaying bainite and martensite is characterized in that: the corrosive liquid consists of the following components: glacial acetic acid, absolute ethyl alcohol; wherein the volume ratio of the glacial acetic acid to the absolute ethyl alcohol is as follows: 1: 3-7.
2. Use according to claim 1, characterized in that: the corrosive liquid consists of the following components: glacial acetic acid, absolute ethyl alcohol; wherein the volume ratio of the glacial acetic acid to the absolute ethyl alcohol is as follows: 1: 3.
3. use according to claim 1, characterized in that: the corrosive liquid consists of the following components: glacial acetic acid, absolute ethyl alcohol; wherein the volume ratio of the glacial acetic acid to the absolute ethyl alcohol is as follows: 1: 5.
4. use according to claim 1, characterized in that: the corrosive liquid consists of the following components: glacial acetic acid, absolute ethyl alcohol; wherein the volume ratio of the glacial acetic acid to the absolute ethyl alcohol is as follows: 1: 7.
5. use according to claim 1, characterized in that: the alloy components of the ultrahigh-strength steel are as follows by weight percent: 0.15-0.25%, Si: 1.5-2.0%, Mn: 1.0-1.9%, P: less than or equal to 0.1 percent, S: less than or equal to 0.1 percent, Al: 0.1-0.2%, Nb + V + Ti + Cr + Mo + B: less than or equal to 2.6 percent, and the balance being Fe.
6. Use according to claim 1, characterized in that: the using method of the corrosive liquid comprises the following steps:
s1, sample preparation: taking a metallographic sample, and carrying out hot inlaying on the metallographic sample to obtain a metallographic sample;
s2, grinding: grinding the metallographic sample obtained in the step S1 by using metallographic abrasive paper or a grinding machine until the surface scratches are shallow and only have one direction to obtain a ground metallographic sample;
s3, polishing: coating diamond polishing paste on the surface to be corroded of the ground metallographic specimen, and performing dry polishing on the surface to be corroded in a direction perpendicular to the scratches on a polishing machine until the scratches are almost eliminated, and performing water-adding wet polishing to obtain a scratch-free mirror surface;
s4, corrosion: placing the non-scratch mirror surface of the metallographic sample obtained in the step S3 in a prepared corrosive liquid in an upward mode, and standing for 10-40min at the corrosion environment temperature of 0-40 ℃;
s5, observation: and (5) taking out the metallographic sample obtained in the step (S4), cleaning the corroded surface by using water, cleaning the corroded surface by using alcohol, drying and observing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910730275.3A CN110453222B (en) | 2019-08-08 | 2019-08-08 | Corrosive liquid for displaying austenite grain boundary of ultrahigh-strength steel, and preparation method and application thereof |
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| CN201910730275.3A CN110453222B (en) | 2019-08-08 | 2019-08-08 | Corrosive liquid for displaying austenite grain boundary of ultrahigh-strength steel, and preparation method and application thereof |
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| CN110453222A CN110453222A (en) | 2019-11-15 |
| CN110453222B true CN110453222B (en) | 2021-07-13 |
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| KR20110000913A (en) * | 2009-06-29 | 2011-01-06 | 김선권 | Corrosion inhibitor for metal and method for producing the same |
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