CN113865953B - Method for displaying and evaluating grain boundary carbide in low-carbon stamping steel by metallographic method - Google Patents

Method for displaying and evaluating grain boundary carbide in low-carbon stamping steel by metallographic method Download PDF

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CN113865953B
CN113865953B CN202110989943.1A CN202110989943A CN113865953B CN 113865953 B CN113865953 B CN 113865953B CN 202110989943 A CN202110989943 A CN 202110989943A CN 113865953 B CN113865953 B CN 113865953B
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metallographic
carbide
grain boundary
low
sample
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CN113865953A (en
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魏焕君
邝霜
崔丽丽
田秀刚
李博昊
董茜
张靖雨
唐学斌
齐俊茹
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Tangshan Iron and Steel Group Co Ltd
HBIS Co Ltd Tangshan Branch
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Tangshan Iron and Steel Group Co Ltd
HBIS Co Ltd Tangshan Branch
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    • 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
    • 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
    • G01N1/34Purifying; Cleaning
    • 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

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  • Molecular Biology (AREA)
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Abstract

The invention belongs to the technical field of metal detection, and provides a method for displaying and evaluating grain boundary carbide in low-carbon stamping steel by a metallographic method. The method provided by the invention can clearly and completely display the appearance, the size and the distribution state of carbides at the intragranular position and the grain boundary position in the low-carbon stamping steel, and has the characteristics of low detection and analysis cost, safety, rapidness, simplicity and easiness in operation.

Description

Method for displaying and evaluating grain boundary carbide in low-carbon stamping steel by metallographic method
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a method for displaying and evaluating grain boundary carbide in low-carbon stamping steel by a metallographic method.
Background
The number, shape and distribution of carbide in the aluminum killed steel for low-carbon stamping directly affect the service performance of the aluminum killed steel, and are key factors for solving the problem of stamping cracking of the steel for low-carbon stamping; the morphology of the carbides at the grain boundaries directly affects their stamping properties. At present, 4% nitrate alcohol corrosion or picric acid corrosion is adopted for carbide display and evaluation, and a metallographic microscope or a scanning electron microscope is used for analysis by means of EBSD; however, the use of 4% nitroalcohol attack only can show granular carbide in the crystal, but can not show the granular carbide at the grain boundary, namely the strip-shaped or short rod-shaped carbide; picric acid is toxic and belongs to dangerous goods; the method has the defects of difficult sample preparation, complex operation, high cost and inaccurate evaluation proportion.
Disclosure of Invention
The invention aims to provide a method for displaying and evaluating grain boundary carbide in low-carbon stamping steel by a metallographic method, which can display all grain boundaries and carbide in the grain boundaries in a structure, can rapidly, accurately and safely observe the form, the quantity and the distribution of the carbide in the grain boundaries and at the grain boundaries, accurately evaluate the proportion of the carbide and accurately reflect the service performance of the carbide.
In order to solve the technical problems, the invention adopts the following technical scheme:
a metallographic method for displaying and evaluating grain boundary carbide in low-carbon stamping steel comprises the steps of sample preparation, chemical corrosion and microscopic observation and evaluation, wherein an aggressive agent used for the chemical corrosion is prepared from sulfuric acid alcohol solution and sodium chloride aqueous solution.
The volume concentration of the sulfuric acid alcohol solution is 0.03-0.08%.
The mass concentration of the sodium chloride aqueous solution is 0.1-0.25%.
The aggressive agent is prepared from sulfuric acid alcohol solution and sodium chloride aqueous solution according to the proportion of 2-5:1.
The etching time of the chemical etching is 1-8 s.
The specific operation of the sample preparation of the invention is as follows: and (3) taking a low-carbon steel plate for stamping, cutting a part of the sample to obtain a sample, and then sequentially inlaying and polishing the sample.
The specific operation of the inlaying and polishing treatment is as follows: putting the sample into a Simlimet 3000 automatic metallographic mosaic machine for mosaic; grinding the inlaid sample on 280# metallographic sand paper, 400# metallographic sand paper, 600# metallographic sand paper and 800# metallographic sand paper in turn, wherein the grinding direction is vertical to the previous scratch direction; and polishing at a speed of 300-1400 rpm for 1-5 minutes.
After chemical corrosion is finished, washing the sample with absolute ethyl alcohol, drying, and then observing under a ZEISS metallographic microscope to obtain a carbide metallographic picture; and opening the collected metallographic pictures in metallographic analysis software, selecting a filling color function, filling the color of carbide, extracting carbide, processing the pictures by utilizing binarization, and evaluating the percentage content of carbide.
The beneficial effects of adopting above-mentioned technical scheme to produce lie in:
1. the invention adopts 0.03-0.08% sulfuric acid alcohol solution and 0.1-0.25% NaCl aqueous solution as the aggressive agent, can clearly show the crystal boundary of the low-carbon stamping steel and the form, proportion and size of carbide in the crystal, and solves the problem that the traditional nitrate alcohol aggressive agent cannot clearly show short rod-shaped and dot-shaped carbide at the crystal boundary.
2. The carbide proportion assessed by the method is accurate, has representativeness and can directly reflect the service performance of the steel.
3. The method of the invention adopts the aggressive agent which is safe, harmless to human body, nontoxic, and has the characteristics of low detection and analysis cost, rapidness, simplicity and safety.
Drawings
FIG. 1 is a diagram showing the structure of carbide obtained in example 1;
FIG. 2 is a carbide texture map obtained in example 2;
FIG. 3 is a chart showing the structure of carbide obtained in example 3;
FIG. 4 is a metallographic structure diagram obtained in comparative example 1;
FIG. 5 is a carbide texture map obtained in comparative example 1;
FIG. 6 is a metallographic structure diagram obtained in comparative example 2;
FIG. 7 is a metallographic structure diagram obtained in comparative example 3.
Detailed Description
The invention is described in further detail below with reference to the drawings and the specific examples.
Example 1
The metallographic sample preparation and display method of carbide in the low-carbon stamping steel with the brand of DC01 comprises the following specific steps of sample preparation, chemical corrosion and microscopic observation:
(1) Sample preparation: cutting a 15mm steel plate, putting the steel plate into a Simlimet 3000 automatic metallographic mosaic machine for mosaic, and coarsely grinding the mosaic sample by an MPJ-35 metallographic specimen grinding machine until the surface is flat and the scratch depths are consistent; then carrying out fine grinding by using 280-400-600-800 metallographic sand paper in sequence, wherein the grinding direction of each pass is perpendicular to the scratch direction of the last pass; finally, the mixture is put on a space boat polisher for polishing, a pressure sensitive adhesive woolen cloth polishing cloth with the thickness of 200mm is adopted, water is uniformly sprayed on the polishing cloth, a high-efficiency metallographic polishing agent with the thickness of 2.5 micrometers is uniformly sprayed on the polishing cloth, and the polishing is carried out for 1.5 minutes at the speed of 1400 revolutions per minute.
(2) Chemical corrosion: the used aggressive agent is prepared from sulfuric acid alcohol solution with volume concentration of 0.05% and NaCl aqueous solution with mass concentration of 0.1% according to the proportion of 3:1, and the aggressive time is 8s;
(3) And (3) observing by a microscope: after chemical corrosion, the carbide is washed clean by absolute ethyl alcohol, dried by a blower, and then is placed under a ZEISS metallographic microscope for observation, so that the appearance of the carbide can be clearly obtained, and the carbide is shown in figure 1.
(4) And (5) proportion evaluation: and (3) opening the metallographic picture 1 acquired in the step (3) in metallographic analysis software, selecting a filling color function, filling the color of carbide, extracting carbide, processing the picture by utilizing binarization, and evaluating the content to be 1.5%.
Example 2
The metallographic sample preparation and display method of carbide in the galvanized sheet for the low-carbon stamping with the brand of DC51D+Z comprises the steps of sample preparation, chemical corrosion and microscopic observation, and the specific process steps are as follows:
(1) Sample preparation: cutting a 15mm steel plate, putting the steel plate into a Simlimet 3000 automatic metallographic mosaic machine for mosaic, and coarsely grinding the mosaic sample by an MPJ-35 metallographic specimen grinding machine until the surface is flat and the scratch depths are consistent; then carrying out fine grinding by using 280-400-600-800 metallographic sand paper in sequence, wherein the grinding direction of each pass is perpendicular to the scratch direction of the last pass; finally, the mixture is put on a space boat polisher for polishing, a pressure sensitive adhesive woolen cloth polishing cloth with the thickness of 200mm is adopted, water is uniformly sprayed on the polishing cloth, a high-efficiency metallographic polishing agent with the thickness of 0.5 micrometer is uniformly sprayed on the polishing cloth, and the polishing is carried out for not more than 3 minutes at the speed of 1400 revolutions per minute.
(2) Chemical corrosion: the used aggressive agent is prepared from sulfuric acid alcohol with the volume concentration of 0.08 percent and NaCl aqueous solution with the mass concentration of 0.15 percent in a ratio of 2:1, and the aggressive time is 4s;
(3) And (3) observing by a microscope: after chemical corrosion, the sample is washed clean by absolute ethyl alcohol, dried by a blower, and then is placed under a ZISS metallographic microscope for observation, so that the clear free cementite morphology can be obtained, and the appearance is shown in figure 2.
(4) And (5) proportion evaluation: and (3) opening the metallographic picture 2 acquired in the step (3) in metallographic analysis software, selecting a filling color function, filling the color of carbide, extracting carbide, processing the picture by utilizing binarization, and evaluating the percentage content to be 2.5%.
Example 3
The metallographic sample preparation and display method of carbide in the low-carbon stamping steel with the brand number of DC03 comprises the following specific steps of sample preparation, chemical corrosion and microscopic observation:
(1) Sample preparation: cutting a 15mm steel plate, putting the steel plate into a Simlimet 3000 automatic metallographic mosaic machine for mosaic, and coarsely grinding the mosaic sample by an MPJ-35 metallographic specimen grinding machine until the surface is flat and the scratch depths are consistent; then carrying out fine grinding by using 280-400-600-800 metallographic sand paper in sequence, wherein the grinding direction of each pass is perpendicular to the scratch direction of the last pass; finally, the mixture is put on a space boat polisher for polishing, a pressure sensitive adhesive woolen cloth polishing cloth with the thickness of 200mm is adopted, water is uniformly sprayed on the polishing cloth, a high-efficiency metallographic polishing agent with the thickness of 2.5 microns is uniformly sprayed on the polishing cloth, and the polishing is carried out for 2 minutes at the speed of 1400 revolutions per minute.
(2) Chemical corrosion: the used aggressive agent is prepared from sulfuric acid alcohol solution with volume concentration of 0.03% and NaCl aqueous solution with mass concentration of 0.25% according to the proportion of 5:1, and the aggressive time is 1s;
(3) And (3) observing by a microscope: after chemical corrosion, the sample is washed clean with absolute ethyl alcohol, dried by a blower, and then placed under a ZISS metallographic microscope for observation, so that the appearance of the clear carbide can be obtained, and the appearance is shown in figure 3.
(4) And (5) proportion evaluation: and (3) opening the metallographic picture 3 acquired in the step (3) in metallographic analysis software, selecting a filling color function, filling the color of carbide, extracting carbide, processing the picture by utilizing binarization, and evaluating the percentage content to be 3.5%.
Comparative example 1
The comparative example differs from example 1 in that the aggressive agent used for chemical etching is 4% HNO 3 Alcohol, etching time is 4s; after the chemical corrosion is finished, the sample is washed clean by absolute ethyl alcohol, dried by a blower, and then is placed under a ZISS metallographic microscope for observation, so that the appearance of carbide at the grain boundary can not be obtained, and the appearance is shown in figure 4; the carbide diagram is observed by using a scanning electron microscope, see fig. 5, and since the scanning electron microscope is a microscopic morphological observation, the percentage of carbide in a micro area can be only assessed, and meanwhile, the cost is higher than that of a metallographic observation mode.
Comparative example 2
The comparative example differs from example 2 in that the aggressive agent used for chemical etching is 4% HNO 3 Alcohol, etching time is 5s; after the chemical corrosion is finished, the sample is washed clean by absolute ethyl alcohol, dried by a blower, and then is placed under a ZISS metallographic microscope for observation, and the appearance of carbide at the grain boundary can not be obtained, as shown in figure 6.
Comparative example 3
This comparative example differs from example 3 in thatThe comparative example used 4% HNO with different etchants used for chemical etching 3 Alcohol, etching time is 6s; after the chemical corrosion is completed, the sample is washed clean by absolute ethyl alcohol, dried by a blower, and then is placed under a ZISS metallographic microscope for observation, and the appearance of carbide at the grain boundary can not be obtained, as shown in figure 7.

Claims (3)

1. A method for displaying and evaluating grain boundary carbide in low-carbon stamping steel by a metallographic method is characterized by comprising the following steps of: the method comprises sample preparation, chemical corrosion and metallographic microscope observation and evaluation, wherein the aggressive agent used by the chemical corrosion is prepared from sulfuric acid alcohol solution and sodium chloride aqueous solution; the volume concentration of the sulfuric acid alcohol solution is 0.03-0.08%; the mass concentration of the sodium chloride aqueous solution is 0.1-0.25%; the aggressive agent is prepared from sulfuric acid alcohol solution and sodium chloride aqueous solution according to the proportion of 2-5:1; the etching time of the chemical etching is 1-8 s.
2. A method for metallographic display and assessment of grain boundary carbides in low carbon stamping steels according to claim 1, characterized by: the concrete operation of the sample preparation is as follows: and (3) taking a low-carbon steel plate for stamping, cutting a part of the sample to obtain a sample, and then sequentially inlaying and polishing the sample.
3. A method for metallographic display and assessment of grain boundary carbides in low carbon stamping steels according to claim 1, characterized by: the assessment method of the grain boundary carbide specifically comprises the following steps: after chemical corrosion is finished, washing the sample with absolute ethyl alcohol, drying, and then observing under a metallographic microscope to obtain a carbide metallographic picture; and opening the collected metallographic pictures in metallographic analysis software, selecting a filling color function, filling the color of carbide, extracting carbide, processing the pictures by utilizing binarization, and evaluating the percentage content of carbide.
CN202110989943.1A 2021-08-26 2021-08-26 Method for displaying and evaluating grain boundary carbide in low-carbon stamping steel by metallographic method Active CN113865953B (en)

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