CN111830229A - Metallographic corrosive agent for primary banded structure of steel and metallographic display method - Google Patents
Metallographic corrosive agent for primary banded structure of steel and metallographic display method Download PDFInfo
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Abstract
The invention belongs to the technical field of metallographic detection, and particularly relates to a metallographic corrosive agent for a steel primary banded structure and a metallographic display method. The metallographic corrosive agent comprises: water, methanol, copper chloride and hydrochloric acid; wherein the volume of the water, the volume of the methanol, and the ratio of the mass of the copper chloride to the volume of the hydrochloric acid are as follows: (25-35) ml, (20-30) g, (1-3) ml. The metallographic corrosive and the metallographic display method are mainly suitable for hot rolled steel products after rolling deformation and rolled heat-treated steel products, are convenient to operate, have stable corrosion effect, can clearly display the primary banded structure of a steel sample, and can be used for evaluating the quality and performance of the steel products.
Description
Technical Field
The invention belongs to the technical field of metallographic examination, and particularly relates to a metallographic corrosive agent for a steel primary banded structure and a metallographic display method.
Background
Generally, the band-shaped structure is caused by dendrite segregation of the steel ingot. Because molten steel is selectively crystallized during solidification, the components of the molten steel on the branches are pure, and impurities such as carbon, alloy elements, phosphorus, sulfur and the like are enriched among the branches and the crystals. In the forging and rolling deformation, the steel ingot is elongated into a fiber structure by rolling between the stem and dendrite thereof, thereby forming a so-called primary band-like structure which is an original band-like structure formed by extending dendrite segregation in the hot working direction. The root cause of the secondary banded structure is that carbon and other alloy elements are segregated and enriched among branches in the solidification process of the continuous casting slab, and the Ar3 point temperature of each area in the steel is inconsistent due to the element segregation during hot rolling and heating. When the hypoeutectoid steel is cooled from the austenitic state at the time of finish rolling, proeutectoid ferrite starts to precipitate at the Ar3 point temperature first, and pearlite starts to form only when it is cooled to Ar1, whereby a ferrite + pearlite band structure is formed. The microstructure band generated by the solid phase transition is a secondary band, and the band structure observed after the etching with nitric acid and alcohol is a secondary band. The primary banded structure refers to dendritic crystal segregation formed in the solidification process of molten steel, has relative stability, and is formed into a fiber band shape by the fact that primary crystal grains disappear after heating, but dendritic crystal segregation still remains and then is rolled, deformed and extended. The primary band-shaped tissue was not revealed with ordinary nital. The secondary banded structure can be formed on the basis of the primary banded structure, but the steel with the primary banded structure does not necessarily have the secondary banded structure, and the secondary banded structure is closely related to processes such as controlled rolling and controlled cooling during rolling. The ribbon structure causes directionality in the mechanical properties of the steel, reduces the transverse toughness index of the steel, and deteriorates the machinability of the steel.
In general, we will consider the secondary band-shaped structure as the microstructure defect of steel, but the secondary band-shaped structure is the product of solid phase transformation, and the primary band-shaped structure essentially has negative influence on the material use performance, so it is crucial to improve the shape and distribution of the primary band-shaped structure from the aspect of metallurgical technology. However, corrosion and display of primary band structures have been a problem, and it has not been possible to corrode and display clear primary band structures.
Disclosure of Invention
In view of the above problems, the present invention provides a metallographic etchant for a steel primary band structure and a method for displaying the metallographic structure. The metallographic corrosive and the metallographic display method are mainly suitable for hot rolled steel products after rolling deformation and rolled heat-treated steel products, are convenient to operate, have stable corrosion effect, can clearly display the primary banded structure of a steel sample, and can be used for evaluating the quality and performance of the steel products.
The technical scheme of the invention for realizing the purpose is as follows:
the invention provides a metallographic corrosive agent for a primary steel strip structure, which comprises the following components in part by weight: water, methanol, copper chloride and hydrochloric acid;
wherein the volume of the water, the volume of the methanol, and the ratio of the mass of the copper chloride to the volume of the hydrochloric acid are as follows: (25-35) ml, (20-30) g, (1-3) ml.
In some preferred embodiments, in the steel primary band structure metallographic etchant according to the present invention, the ratio of the volume of water, the volume of methanol, the mass of copper chloride and the volume of hydrochloric acid is: 30ml, 25g, 2 ml.
In some embodiments, in the corrosive agent for a steel primary band structure metallographic phase, the hydrochloric acid is 36-38 w% in mass percentage.
In some embodiments, the preparation method of the steel primary band structure metallographic corrosive agent comprises the following steps: and uniformly mixing the water, the methanol, the copper chloride and the hydrochloric acid according to the proportion to obtain the steel primary banded structure metallographic corrosive agent.
The invention also provides a steel primary banded structure metallographic phase display method, which comprises the following steps:
polishing the steel sample (or grinding the steel sample before polishing) to obtain a polished surface of the steel sample;
adopting the steel primary banded structure metallographic corrosive of the invention to corrode the polished surface of the steel sample to obtain a metallographic corrosive sample;
washing and drying the metallographic corrosion sample to obtain a metallographic observation sample;
and (4) observing the metallographic observation sample under a metallographic microscope, and collecting pictures.
In some embodiments, the method for metallographic display of a steel primary band structure according to the present invention comprises the steps of:
polishing the steel sample to obtain a polished surface of the steel sample;
immersing the polished surface of the steel sample into the steel primary banded structure metallographic corrosive agent of the invention for corrosion treatment to obtain a metallographic corrosive sample;
washing and drying the metallographic corrosion sample to obtain a metallographic observation sample;
and (4) observing the metallographic observation sample under a metallographic microscope, and collecting pictures.
In some embodiments, in the method for displaying metallographic phase of a primary steel strip according to the present invention, the immersing the polished surface of the steel sample in the corrosive agent for metallographic phase of a primary steel strip according to the present invention includes: and the polished surface of the steel sample is vertical to the liquid level of the steel primary banded structure metallographic corrosive.
In some embodiments, the etching treatment of the present invention may also be any of various metallographic etching treatments known to those skilled in the art, such as etching, rubbing etching, and dropping etching.
In some embodiments, in the method for metallographic representation of a steel primary band structure according to the present invention, the steel sample is a longitudinal section sample parallel to the rolling direction.
In some embodiments, in the steel primary band metallographic display method according to the present invention, the polishing step of the steel sample includes: and inlaying, grinding and polishing the steel sample until the polished surface of the steel sample is smooth and has no obvious scratch or stain.
In some embodiments, the polishing process may be electrochemical polishing, mechanical polishing, and chemical polishing; and after the polishing treatment, obtaining a flat polished surface on the steel sample.
In some embodiments, in the method for displaying metallographic structure of a primary steel strip according to the present invention, the time for the etching treatment is 1 to 10 seconds.
In some embodiments, in the method for displaying metallographic structure of a primary steel strip according to the present invention, the method for performing corrosion treatment includes: etching, rubbing or dropping.
In some embodiments, in the method for metallographic representation of a steel primary band structure according to the present invention, the polished surface of the steel sample is brownish red after the corrosion treatment.
In some embodiments, in the steel primary band metallographic display method according to the present invention, the washing includes: washing with water for 3-8 seconds, and then washing with absolute ethyl alcohol for 3-8 seconds.
In some embodiments, in the method for displaying metallographic of a primary steel strip structure, the metallographic microscope adopts a field of view magnified by 50 to 200 times.
In some embodiments, in the method for displaying metallographic structure of a primary steel strip, the metallographic observation sample is observed under a metallographic microscope (with a field of view magnified by 50-200 times), and an obvious white strip appears in an acquired picture, that is, the primary steel strip is formed.
In some embodiments, in the steel primary band metallographic display method according to the present invention, the steel is a rolled steel;
in some preferred embodiments, in the method for displaying metallographic structure of a primary band-shaped structure of a steel material according to the present invention, the steel material is a rolled steel material that has been heat-treated.
In some embodiments, in the method for displaying metallographic structure of a primary band structure of a steel material according to the present invention, the steel material is a 20CrMnTi steel material or a Q420 steel material.
One or more technical embodiments of the present invention have at least the following technical effects or advantages:
(1) the preparation method of the metallographic corrosive agent is simple and convenient, can be used at room temperature, and does not need heating treatment; the metallographic corrosive agent has a good corrosion effect, can clearly display the primary banded structure of a steel sample, and solves the problems that the primary banded structure of rolled steel is difficult to display and is difficult to display clearly;
(2) compared with the prior art, the metallographic corrosive agent and the metallographic display method can enable the primary banded structure in the rolled steel to be easily distinguished, and are beneficial to evaluating the quality of rolled steel products.
(3) In order to prove that the white strip eroded by the method is a primary banded structure, the method carries out microhardness and electron probe element surface scanning tests. The metallographic observation sample is subjected to microhardness test, the hardness of a strip corroded by the method is obviously higher, the hardness of a general element segregation area is higher than that of a matrix, and the strip is an element segregation position when an element casting blank is solidified; meanwhile, when the electronic probe equipment scans the element surface, the element content high-low regions can be displayed in different colors according to the content of alloy elements, so that an element segregation band is represented. And after the sample at the position of the strip corroded by the metallographic phase is subjected to alloy element surface scanning by the electronic probe, finding that the element segregation distribution obtained by scanning with the electronic probe is consistent. The hardness test and the electronic probe test show that the strip corroded by the method is an element segregation part when an element casting blank is solidified, namely the strip corroded and displayed by the test method is an alloy element segregation strip which is a primary strip-shaped structure.
(4) In the invention, the metallographic observation sample is placed under a metallographic microscope (a field of view is magnified by 50-200 times) for observation, a gray mode of the microscope can be adopted, and the collected picture is black and white and an obvious white strip appears; a color mode may also be used, where the picture is collected reddish brown, with light colored bands appearing in the reddish brown field of view.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 (a) and (b) show primary band-shaped tissue images obtained in example 1 of the present invention;
FIGS. 2(a) and (b) show a primary picture of a banded tissue obtained in example 3 of the present invention;
FIG. 3 is a photograph showing the metallographic structure obtained in comparative example 1 of the present invention;
fig. 4 (a) and (b) show metallographic structure pictures obtained in comparative example 2 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In order to solve the technical problems, the embodiment of the invention provides the following general ideas:
the invention provides a metallographic corrosive agent for a primary steel strip structure, which comprises the following components in part by weight: water, methanol, copper chloride and hydrochloric acid;
wherein the volume of the water, the volume of the methanol, and the ratio of the mass of the copper chloride to the volume of the hydrochloric acid are as follows: (25-35) ml, (20-30) g, (1-3) ml.
The inventor of this application has finally confirmed the ratio relation of water, methyl alcohol, copper chloride and hydrochloric acid through a large amount of screening tests, thereby makes metallographic corrosive agent's corrosion effect is good, can clearly show the primary banding tissue of steel sample, has solved the primary banding tissue of rolled steel and has shown the difficulty and show clear problem, has realized good technological effect.
In some preferred embodiments, in the steel primary band structure metallographic etchant according to the present invention, the ratio of the volume of water, the volume of methanol, the mass of copper chloride and the volume of hydrochloric acid is: 30ml, 25g, 2 ml.
Aiming at the metallographic display method of the primary steel strip structure, which proportion relation of water, methanol, copper chloride and hydrochloric acid is most suitable is selected, the inventor further conducts screening and optimization, and finds that when the volume of the water, the volume of the methanol, the mass of the copper chloride and the volume of the hydrochloric acid are in the following proportion: 30ml:30ml:25g:2ml is most advantageous for displaying the primary band-shaped structure of the steel sample.
The invention also provides a steel primary banded structure metallographic phase display method, which comprises the following steps:
polishing the steel sample to obtain a polished surface of the steel sample;
adopting the steel primary banded structure metallographic corrosive of the invention to corrode the polished surface of the steel sample to obtain a metallographic corrosive sample;
washing and drying the metallographic corrosion sample to obtain a metallographic observation sample;
and (4) observing the metallographic observation sample under a metallographic microscope, and collecting pictures.
The steel primary banded structure metallographic phase display method is obtained through a large number of experiments, so that the primary banded structure in the rolled steel is easy to distinguish, and the quality of the rolled steel product is favorably evaluated.
In some embodiments, the method for metallographic display of a steel primary band structure according to the present invention comprises the steps of:
polishing the steel sample to obtain a polished surface of the steel sample;
immersing the polished surface of the steel sample into the steel primary banded structure metallographic corrosive agent of the invention for corrosion treatment to obtain a metallographic corrosive sample;
washing and drying the metallographic corrosion sample to obtain a metallographic observation sample;
and (4) observing the metallographic observation sample under a metallographic microscope, and collecting pictures.
The inventor finds out through experiments that the polished surface of the steel sample is immersed in the metallographic corrosive agent for corrosion treatment (etching method), the obtained corrosion effect is good, and the obtained metallographic observation sample can clearly display a primary banded structure.
In some embodiments, in the steel primary band metallographic display method according to the present invention, the steel sample is a longitudinal section sample parallel to a rolling direction; the strip-shaped structure can be deformed along the rolling direction, and the strip-shaped structure is not obvious in the cross section direction.
In some embodiments, in the method for displaying metallographic phase of a primary band-shaped structure of a steel material according to the present invention, the time of the etching treatment is 1 to 10 seconds; the corrosion time is too long, so that the corrosion surface is blackened, and the definition of the sample structure is influenced.
In some embodiments, in the steel primary band metallographic display method according to the present invention, after the corrosion treatment is performed on the polished surface of the steel sample, the polished surface of the steel sample is reddish brown. In the present invention, since the etchant contains copper chloride, the chemical reaction occurring during etching causes copper to appear on the polished surface, and therefore the color appearing on the etched surface is the same as that of copper and is reddish brown.
In some embodiments, in the steel primary band metallographic display method according to the present invention, the washing includes: the film is washed by water for 3-8 seconds. The washing time is too long, which is not beneficial to the drying of the sample; washing with absolute ethyl alcohol for 3-8 seconds; the time is too long, the ethanol is not easy to volatilize, and the polished surface is not clean.
In some embodiments, in the method for displaying metallographic of a primary steel strip structure, the metallographic microscope adopts a field of view magnified by 50 to 200 times. If the multiple is too large, the observation area is too small, which is not beneficial to observing the macroscopic morphology of the banded tissue.
The metallographic etchant and the metallographic display method for a steel primary band structure according to the present application will be described in detail below with reference to examples, comparative examples, and experimental data.
Example 1:
preparing the metallographic corrosive agent of the primary banded structure of the steel material, which is disclosed by the invention: 25ml of water, 25ml of methanol, 20g of copper chloride and 1ml of hydrochloric acid with the mass percentage concentration of 36w percent are uniformly mixed to obtain the steel primary banded structure metallographic corrosive agent, and the corrosive agent is put into a container for later use.
(1) Taking 20CrMnTi steel (subjected to heat treatment, namely heating to a 930-degree austenite region, preserving heat for 30min, then performing water cooling treatment), obtaining a longitudinal section along a direction parallel to the rolling direction of the steel to obtain a 20CrMnTi steel sample, and inlaying, grinding and polishing the sample until a polished surface is smooth and has no obvious scratch or stain;
(2) adopting the prepared steel primary strip structure metallographic corrosive to abrade the polished surface of the steel sample obtained in the step (1) for 10 seconds, wherein the polished surface is brownish red, so as to obtain a metallographic corrosive sample;
(3) immediately washing the metallographic corrosion sample obtained in the step (2) with water for 3 seconds, quickly putting the metallographic corrosion sample into ethanol for washing for 3 seconds, and drying (blow-drying) to obtain a metallographic observation sample for later use;
(4) observing the metallographic observation sample obtained in the step (3) under a metallographic microscope, magnifying the field of view by 50 times, and collecting pictures; the image shows distinct bands, primary bands of tissue, some of which are thicker throughout the field of view, as shown in fig. 1.
Example 2:
preparing the metallographic corrosive agent of the primary banded structure of the steel material, which is disclosed by the invention: and uniformly mixing 35ml of water, 35ml of methanol, 30g of copper chloride and 3ml of hydrochloric acid with the mass percentage concentration of 38 w% to obtain the primary steel strip structure metallographic corrosive agent, and putting the primary steel strip structure metallographic corrosive agent into a container for later use.
(1) Taking Q420 steel, obtaining a longitudinal section along the direction parallel to the rolling direction of the steel to obtain a Q420 steel sample, and inlaying, grinding and polishing the sample until a polished surface is smooth and has no obvious scratch or stain;
(2) carrying out drop etching treatment on the polished surface of the steel sample obtained in the step (1) for 8 seconds by using the prepared steel primary banded structure metallographic corrosive agent, wherein the polished surface is red to obtain a metallographic corrosive sample;
(3) immediately washing the metallographic corrosion sample obtained in the step (2) with water for 8 seconds, quickly putting the metallographic corrosion sample into ethanol for washing for 8 seconds, and drying (blow-drying) to obtain a metallographic observation sample for later use;
(4) observing the metallographic observation sample obtained in the step (3) under a metallographic microscope, amplifying the metallographic observation sample by 100 times of a field of view, and collecting pictures; the image shows distinct bands, which are primary band-shaped tissues that are relatively small in spacing, thin and dense (some of which are thicker), and the majority of the bands extend across the field of view.
Example 3:
preparing the metallographic corrosive agent of the primary banded structure of the steel material, which is disclosed by the invention: 30ml of water, 30ml of methanol, 25g of copper chloride and 2ml of hydrochloric acid with the mass percentage concentration of 36w percent are uniformly mixed to obtain the steel primary banded structure metallographic corrosive agent, and the corrosive agent is put into a container for later use.
(1) Taking Q420 steel, obtaining a longitudinal section along the direction parallel to the rolling direction of the steel to obtain a Q420 steel sample, and inlaying, grinding and polishing the sample until a polished surface is smooth and has no obvious scratch or stain;
(2) immersing the polished surface of the steel sample obtained in the step (1) into the steel primary banded structure metallographic corrosive agent, wherein the polished surface of the steel sample is vertical to the liquid level of the steel primary banded structure metallographic corrosive agent, and performing corrosion treatment for 1 second, wherein the polished surface is red to obtain a metallographic corrosion sample;
(3) immediately washing the metallographic corrosion sample obtained in the step (2) with water for 5 seconds, quickly putting the metallographic corrosion sample into ethanol for washing for 5 seconds, and drying (blow-drying) to obtain a metallographic observation sample for later use;
(4) observing the metallographic observation sample obtained in the step (3) under a metallographic microscope, amplifying the metallographic observation sample by 200 times of a field of view, and collecting pictures; the image shows distinct bands, which are primary band-shaped tissues that are relatively closely spaced, thin and dense bands (some of which are thicker), with the majority of the bands extending through the field of view, as shown in fig. 2.
Comparative example 1:
(1) taking a 20CrMnTi rolled material sample (subjected to heat treatment, namely heating to a 930-degree austenite region, preserving heat for 30min, and then carrying out water cooling treatment), inlaying, grinding and polishing the sample until a polished surface is smooth and has no obvious scratch or stain;
(2) corroding the polished surface of the steel sample obtained in the step (1) for 2 seconds by adopting 4% nitric acid alcohol to obtain a metallographic corrosion sample;
(3) immediately washing the metallographic corrosion sample obtained in the step (2) with water and ethanol, and drying to obtain a metallographic observation sample for later use;
(4) observing the metallographic observation sample obtained in the step (3) under a metallographic microscope, amplifying the metallographic observation sample by 200 times of a field of view, and collecting pictures; the pictures show that the metallographic structure is a martensite structure and has no obvious strip shape, as shown in the attached figure 3.
Comparative example 2:
(1) taking a Q420 rolled material sample, inlaying, grinding and polishing the sample until a polished surface is smooth and has no obvious scratch or stain;
(2) corroding the polished surface of the steel sample obtained in the step (1) for 2 seconds by adopting 4% nitric acid alcohol to obtain a metallographic corrosion sample;
(3) immediately washing the metallographic corrosion sample obtained in the step (2) with water and ethanol, and drying to obtain a metallographic observation sample for later use;
(4) observing the metallographic observation sample obtained in the step (3) under a metallographic microscope, amplifying the metallographic observation sample by 200 times of a field of view, and collecting pictures; the pictures show that the metallographic structure is a bainite structure without obvious bands, as shown in the attached figure 4.
Example 4: experiment for optimizing process
The influence of the mixture ratio relationship of each component in the steel primary banded structure metallographic corrosive agent on the primary banded structure display definition is inspected:
the method comprises the following steps: the procedure was followed as in example 1, except that the metallographic etchant contained: 22ml of water, 23ml of methanol, 18g of copper chloride and 4ml of hydrochloric acid.
The method 2 comprises the following steps: the procedure was followed as in example 1, except that the metallographic etchant contained: 37ml of water, 37ml of methanol, 32g of copper chloride and 0.5ml of hydrochloric acid.
The method 3 comprises the following steps: the procedure was followed as in example 1, except that the metallographic etchant contained: 22ml of water, 40ml of methanol, 35g of copper chloride and 3.5ml of hydrochloric acid.
The method 4 comprises the following steps: the procedure was followed as in example 1, except that the metallographic etchant contained: 40ml of water, 20ml of methanol, 35g of copper chloride and 0.8ml of hydrochloric acid.
The method 5 comprises the following steps: inventive example 1;
the method 6 comprises the following steps: example 2 of the invention;
the method 7 comprises the following steps: example 3 of the invention;
the results are shown in Table 1.
Table 1: influence of the proportion relation of the components in the corrosive on the display definition of the primary banded structure
As can be seen by comparing methods 1-7: through screening of the 7 metallographic corrosive agents, the primary banded structures obtained by the methods 1 to 4 are not clear and have no obvious bands. The primary banded tissues obtained by the methods 5 to 7 have high definition and obvious bands; in particular, the primary banding pattern obtained by method 7 is the most sharp, with very distinct banding.
Through the screening test, the invention finally determines that the volume of the water, the volume of the methanol and the ratio of the mass of the copper chloride to the volume of the hydrochloric acid are as follows: (25-35) ml, (20-30) g, (1-3) ml, and further preferably, the ratio of the volume of the water, the volume of the methanol, and the mass of the copper chloride to the volume of the hydrochloric acid is as follows: 30ml, 25g, 2 ml; therefore, the metallographic corrosive agent has a good corrosion effect, can clearly display the primary banded structure of the steel sample, solves the problems of difficult display and clear display of the primary banded structure of rolled steel, and realizes a good technical effect.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A steel primary tape microstructure metallographic etchant comprising: water, methanol, copper chloride and hydrochloric acid;
wherein the volume of the water, the volume of the methanol, and the ratio of the mass of the copper chloride to the volume of the hydrochloric acid are as follows: (25-35) ml, (20-30) g, (1-3) ml.
2. The steel primary tape structure metallographic etchant of claim 1, wherein the ratio of the volume of water, the volume of methanol, the mass of copper chloride and the volume of hydrochloric acid is: 30ml, 25g, 2 ml.
3. A steel primary banded structure metallographic phase display method comprises the following steps:
polishing the steel sample to obtain a polished surface of the steel sample;
adopting the steel primary belt structure metallographic corrosive agent according to claim 1 or 2 to carry out corrosion treatment on the polished surface of the steel sample to obtain a metallographic corrosion sample;
washing and drying the metallographic corrosion sample to obtain a metallographic observation sample;
and (4) observing the metallographic observation sample under a metallographic microscope, and collecting pictures.
4. The steel primary band metallographic display method according to claim 3, wherein said steel sample is a longitudinal section sample parallel to a rolling direction.
5. The steel primary band metallographic display method according to claim 3 or 4, wherein said polishing of a steel sample comprises: inlaying, grinding and polishing the steel sample until no obvious scratch or stain exists on the polished surface of the steel sample.
6. The steel primary band structure metallographic phase display method according to claim 3 or 4, wherein a time of said etching treatment is 1 to 10 seconds;
preferably, the method of corrosion treatment comprises: etching, rubbing or dropping.
7. A steel primary band metallographic display method according to claim 3 or 4, characterized in that said washing comprises: washing with water for 3-8 seconds, and then washing with absolute ethyl alcohol for 3-8 seconds.
8. The steel primary belt structure metallographic display method according to claim 3 or 4, wherein said metallographic microscope employs a field of view magnified 50 to 200 times.
9. The steel primary band metallographic display method according to claim 3 or 4, wherein said steel is a rolled steel;
preferably, the steel material is a rolled steel material which is heat-treated.
10. The steel primary band structure metallographic display method according to claim 9, wherein said steel is a 20CrMnTi steel or a Q420 steel.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113702124A (en) * | 2021-08-11 | 2021-11-26 | 马鞍山钢铁股份有限公司 | Test method for obtaining dendrite morphology of medium-low carbon steel casting blank |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101533A (en) * | 1986-07-29 | 1987-02-11 | 上海第五钢铁厂 | The method of testing of chromium bearing steel hot rolling microstructure band shape |
| CN1308226A (en) * | 2000-11-23 | 2001-08-15 | 东北大学 | Display technology for solidifying structure of continuously cast steel billet |
| CN101144762A (en) * | 2006-09-13 | 2008-03-19 | 鞍钢股份有限公司 | Corrosive agent for displaying silicon steel coagulation tissue and its preparation method |
| CN102023112A (en) * | 2009-09-18 | 2011-04-20 | 鞍钢股份有限公司 | Corrosive capable of displaying ultra low carbon steel solidification arborescent structure and preparation method thereof |
| CN103471900A (en) * | 2013-09-07 | 2013-12-25 | 鞍钢股份有限公司 | Corrosive for displaying billet rimholes and preparation method thereof |
| CN104977203A (en) * | 2014-04-11 | 2015-10-14 | 鞍钢股份有限公司 | Cold-etching agent displaying dendritic structure form of high-carbon steel continuous casting billet and preparation method |
| CN105200429A (en) * | 2015-10-14 | 2015-12-30 | 安徽工业大学 | Etching agent for displaying solidification dendritic structures of middle-high grade non-oriented silicon steel as well as etching method |
| CN105386057A (en) * | 2015-11-24 | 2016-03-09 | 太原理工大学 | Erosion agent capable of displaying solidified dendritic structure of Fe-36 Ni invar alloy and erosion method of erosion agent |
| CN105887090A (en) * | 2016-05-12 | 2016-08-24 | 河北钢铁股份有限公司 | Nickel-base superalloy metallographical corrosive liquid, preparation method and corrosion method |
| CN106596235A (en) * | 2016-12-07 | 2017-04-26 | 东北大学 | Dendritic crystal corroding agent for high nitrogen austenitic stainless steel and preparation method thereof |
| CN107843592A (en) * | 2017-10-11 | 2018-03-27 | 河钢股份有限公司 | A kind of austenitic stainless steel weld joint tissue corrosive agent and its application method |
| CN107991161A (en) * | 2017-11-30 | 2018-05-04 | 东北大学 | The metallographic etching agent and caustic solution of a kind of super austenitic stainless steel |
| CN109358066A (en) * | 2018-10-23 | 2019-02-19 | 沈阳市启光科技有限公司 | One kind is for continuous casting steel billet dendrite corrosion reagent and its preparation and application method |
-
2020
- 2020-07-12 CN CN202010666073.XA patent/CN111830229B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101533A (en) * | 1986-07-29 | 1987-02-11 | 上海第五钢铁厂 | The method of testing of chromium bearing steel hot rolling microstructure band shape |
| CN1308226A (en) * | 2000-11-23 | 2001-08-15 | 东北大学 | Display technology for solidifying structure of continuously cast steel billet |
| CN101144762A (en) * | 2006-09-13 | 2008-03-19 | 鞍钢股份有限公司 | Corrosive agent for displaying silicon steel coagulation tissue and its preparation method |
| CN102023112A (en) * | 2009-09-18 | 2011-04-20 | 鞍钢股份有限公司 | Corrosive capable of displaying ultra low carbon steel solidification arborescent structure and preparation method thereof |
| CN103471900A (en) * | 2013-09-07 | 2013-12-25 | 鞍钢股份有限公司 | Corrosive for displaying billet rimholes and preparation method thereof |
| CN104977203A (en) * | 2014-04-11 | 2015-10-14 | 鞍钢股份有限公司 | Cold-etching agent displaying dendritic structure form of high-carbon steel continuous casting billet and preparation method |
| CN105200429A (en) * | 2015-10-14 | 2015-12-30 | 安徽工业大学 | Etching agent for displaying solidification dendritic structures of middle-high grade non-oriented silicon steel as well as etching method |
| CN105386057A (en) * | 2015-11-24 | 2016-03-09 | 太原理工大学 | Erosion agent capable of displaying solidified dendritic structure of Fe-36 Ni invar alloy and erosion method of erosion agent |
| CN105887090A (en) * | 2016-05-12 | 2016-08-24 | 河北钢铁股份有限公司 | Nickel-base superalloy metallographical corrosive liquid, preparation method and corrosion method |
| CN106596235A (en) * | 2016-12-07 | 2017-04-26 | 东北大学 | Dendritic crystal corroding agent for high nitrogen austenitic stainless steel and preparation method thereof |
| CN107843592A (en) * | 2017-10-11 | 2018-03-27 | 河钢股份有限公司 | A kind of austenitic stainless steel weld joint tissue corrosive agent and its application method |
| CN107991161A (en) * | 2017-11-30 | 2018-05-04 | 东北大学 | The metallographic etching agent and caustic solution of a kind of super austenitic stainless steel |
| CN109358066A (en) * | 2018-10-23 | 2019-02-19 | 沈阳市启光科技有限公司 | One kind is for continuous casting steel billet dendrite corrosion reagent and its preparation and application method |
Non-Patent Citations (6)
| Title |
|---|
| 刘宗昌等: "42CrMo钢锻轧材的带状组织", 《包头钢铁学院学报》 * |
| 刘胜新等: "33Mn2V油井管用钢奥氏体晶界的显示", 《金属热处理》 * |
| 国家技术监督局: "《GB/T_13298-91 中华人民共和国国家标准》", 1 October 1992 * |
| 宋维锡: "《金属学》", 31 May 1980, 冶金工业出版社 * |
| 梁克中: "《金相原理与应用》", 31 January 1983, 中国铁道出版社 * |
| 陈家祥: "《炼钢常用图表数据手册》", 31 January 2010, 冶金工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113702124A (en) * | 2021-08-11 | 2021-11-26 | 马鞍山钢铁股份有限公司 | Test method for obtaining dendrite morphology of medium-low carbon steel casting blank |
| CN113702124B (en) * | 2021-08-11 | 2023-08-25 | 马鞍山钢铁股份有限公司 | Test method for obtaining dendrite morphology of medium-low carbon steel casting blank |
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