CN112945688A - Method for displaying silicon-rich phase three-dimensional structure in aluminum-silicon coating by metallographic method - Google Patents

Method for displaying silicon-rich phase three-dimensional structure in aluminum-silicon coating by metallographic method Download PDF

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CN112945688A
CN112945688A CN202110192735.9A CN202110192735A CN112945688A CN 112945688 A CN112945688 A CN 112945688A CN 202110192735 A CN202110192735 A CN 202110192735A CN 112945688 A CN112945688 A CN 112945688A
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silicon
sample
rich phase
aluminum
metallographic
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CN112945688B (en
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魏焕君
邝霜
何先勇
赵江林
贾慧淑
孙晓梅
崔丽丽
唐学斌
尹芳
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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
    • G01N1/32Polishing; Etching
    • 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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Abstract

The invention belongs to the technical field of metal coating detection, and provides a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, which comprises the following steps of sample preparation, chemical corrosion and microscopic observation: (1) preparing a sample: taking an aluminum-silicon coated steel plate, cutting a part of the aluminum-silicon coated steel plate to be used as a sample, and then sequentially carrying out inlaying and polishing treatment on the sample; (2) chemical corrosion: putting the sample prepared in the step (1) into corrosive liquid for chemical corrosion, wherein the corrosive liquid is prepared from hydrochloric acid aqueous solution and sodium chloride aqueous solution; (3) and (4) microscopic observation: and after the chemical corrosion is finished, washing the sample, drying the sample, and observing the sample by using a ZISS metallographic microscope. The method provided by the invention can obtain a complete and clear silicon-rich phase three-dimensional structure, can fully display the growth condition of the silicon-rich phase, and has the characteristics of low detection cost, rapidness and simplicity.

Description

Method for displaying silicon-rich phase three-dimensional structure in aluminum-silicon coating by metallographic method
Technical Field
The invention belongs to the technical field of metal coating detection, and particularly relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method.
Background
Because the aluminum silicon coated steel plate has good oxidation resistance and corrosion resistance, the research and development and the application of the product are increasingly wide, and the requirements on the physical properties of the product are also increasingly improved. At present, the research aiming at the phase structure of the aluminum-plated silicon coating mainly stays in the display of the phase structure of a plane and a section, and a method for displaying a three-dimensional phase structure is not found. The study of the three-dimensional morphology of the phase structure can better study the growth condition of the phase and can also visually reflect the production process.
The method provided by the invention initiates the three-dimensional morphology analysis of the coating phase structure, changes the tradition that the research on the coating structure is only limited to a planar structure, and enables the research on the coating structure to enter a three-dimensional morphology stage.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for displaying the silicon-rich phase three-dimensional structure in the aluminum-silicon coating by a metallographic method, the provided method can obtain a complete and clear silicon-rich phase three-dimensional structure, can fully display the growth condition of the silicon-rich phase, and has the characteristics of low detection cost, rapidness and simplicity.
In order to solve the technical problems, the invention adopts the technical scheme that:
a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method comprises sample preparation, chemical corrosion and microscopic observation, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coated steel plate, cutting a part of the aluminum-silicon coated steel plate to be used as a sample, and sequentially carrying out inlaying and polishing treatment on the sample;
(2) chemical corrosion: putting the sample prepared in the step (1) into corrosive liquid for chemical corrosion, wherein the corrosive liquid is prepared from hydrochloric acid aqueous solution and sodium chloride aqueous solution;
(3) and (4) microscopic observation: and after the chemical corrosion is finished, washing the sample, drying the sample, and observing the sample by using a ZISS metallographic microscope.
Further, the invention relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, wherein the method comprises the following steps: the sample size was (15. + -.5) mm X (15. + -.5) mm.
Further, the specific operations of the inlaying in the step (1) are as follows: and horizontally placing the surface of the sample coating into an inlaying machine for inlaying, wherein the inlaid sample is ensured to be completely exposed on the surface of the coating.
Further, the invention relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, wherein the method comprises the following steps: the polishing treatment in the step (1) comprises the following specific operations: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent on the polishing cloth, and then performing polishing treatment at the rotating speed of the polishing machine of 300-600 revolutions per minute.
Further, the invention relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, wherein the method comprises the following steps: the polishing cloth in the step (1) is pressure-sensitive adhesive wool fabric polishing cloth with the thickness of 200mm and 250 mm.
Further, the invention relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, wherein the method comprises the following steps: the particle size of the high-efficiency metallographic polishing agent in the step (1) is 0.5-2.5 mu m.
Further, the invention relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, wherein the method comprises the following steps: the polishing time of the polishing treatment in the step (1) is less than or equal to 30 s.
Further, the invention relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, wherein the method comprises the following steps: the volume concentration of the hydrochloric acid in the hydrochloric acid aqueous solution in the step (2) is 10-12%
Further, the invention relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, wherein the method comprises the following steps: and (3) the mass concentration of sodium chloride in the sodium chloride aqueous solution in the step (2) is 5-8%.
Further, the invention relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, wherein the method comprises the following steps: the corrosive liquid in the step (2) is prepared from a hydrochloric acid aqueous solution and a sodium chloride aqueous solution according to the volume ratio of 1: 1.
Further, the invention relates to a method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method, wherein the method comprises the following steps: the corrosion time of the chemical corrosion in the step (2) is 10-20s
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
1. the method provided by the invention changes the fact that the research on the coating structure is limited to the tradition of a planar structure, and the research on the coating structure enters a three-dimensional morphology stage.
2. The method provided by the invention adopts HCl aqueous solution and NaCl aqueous solution as aggressive agents, and can clearly and completely display the three-dimensional structure of the silicon-rich phase in the coating.
3. The method provided by the invention has the characteristics of low detection cost, rapidness and simplicity.
Drawings
FIG. 1 is a three-dimensional map of the silicon-rich phase obtained in example 1;
FIG. 2 is a three-dimensional morphology of the silicon-rich phase obtained in example 2;
FIG. 3 is a three-dimensional map of the silicon-rich phase obtained in example 3;
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example 1
A method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method comprises sample preparation, chemical corrosion and microscopic observation, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coating steel plate (1500 + AS mark), cutting a sample with the thickness of 15mm multiplied by 15mm, horizontally placing the surface of the sample coating into an inlaying machine for inlaying, completely exposing the surface of the inlaid sample coating, and then performing polishing treatment, specifically: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent with the particle size of 2.5 microns on a pressure-sensitive adhesive wool fabric polishing cloth with the particle size of 200mm, and then performing polishing treatment for 30s at the rotating speed of a polishing machine of 300 revolutions per minute.
(2) Chemical corrosion: putting the sample prepared in the step (1) into an etching solution for chemical etching, wherein the etching solution is prepared from a hydrochloric acid aqueous solution with the volume concentration of 10% and a sodium chloride aqueous solution with the mass concentration of 5% according to the volume ratio of 1:1, and the etching time is 20 s;
(3) and (4) microscopic observation: and after the chemical corrosion is finished, washing the sample with absolute ethyl alcohol, drying the sample with a blower, and observing the sample under a ZISS metallographic microscope.
The silicon-rich phase stereo-morphology graph obtained in the embodiment is shown in fig. 1, and it can be seen from fig. 1 that the method provided by the invention can obtain a complete silicon-rich phase stereo structure, and can fully display the morphology and growth condition of the silicon-rich phase.
Example 2
A method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method comprises sample preparation, chemical corrosion and microscopic observation, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coating steel plate (DC 52D + AS mark), cutting a sample with the size of 20mm multiplied by 20mm, horizontally placing the surface of a sample coating into an inlaying machine for inlaying, completely exposing the surface of the inlaid sample coating, and then performing polishing treatment, wherein the method specifically comprises the following steps: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent with the particle size of 0.5 mu m on pressure-sensitive adhesive wool fabric polishing cloth with the particle size of 250mm, and then performing polishing treatment for 20s at the rotating speed of a polishing machine of 600 revolutions per minute.
(2) Chemical corrosion: putting the sample prepared in the step (1) into an etching solution for chemical etching, wherein the etching solution is prepared from a hydrochloric acid aqueous solution with the volume concentration of 12% and a sodium chloride aqueous solution with the mass concentration of 8% according to the volume ratio of 1:1, and the etching time is 10 s;
(3) and (4) microscopic observation: and after the chemical corrosion is finished, washing the sample with absolute ethyl alcohol, drying the sample with a blower, and observing the sample under a ZISS metallographic microscope.
The silicon-rich phase stereo-morphology graph obtained in the embodiment is shown in fig. 2, and it can be seen from fig. 2 that the method provided by the invention can obtain a complete silicon-rich phase stereo structure, and can fully display the morphology and growth condition of the silicon-rich phase.
Example 3
A method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method comprises sample preparation, chemical corrosion and microscopic observation, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coated steel plate (DC 51D + AS mark), cutting a sample with the thickness of 10mm multiplied by 10mm, horizontally placing the surface of a sample coating into an inlaying machine for inlaying, completely exposing the surface of the inlaid sample coating, and then performing polishing treatment, wherein the method specifically comprises the following steps: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent with the particle size of 1.5 mu m on pressure-sensitive adhesive wool fabric polishing cloth with the particle size of 200mmmm, and then performing polishing treatment for 25s at the rotating speed of a polishing machine of 450 revolutions per minute.
(2) Chemical corrosion: putting the sample prepared in the step (1) into an etching solution for chemical etching, wherein the etching solution is prepared from a hydrochloric acid aqueous solution with the volume concentration of 11% and a sodium chloride aqueous solution with the mass concentration of 6.5% according to the volume ratio of 1:1, and the etching time is 15 s;
(3) and (4) microscopic observation: and after the chemical corrosion is finished, washing the sample with absolute ethyl alcohol, drying the sample with a blower, and observing the sample under a ZISS metallographic microscope.
The silicon-rich phase stereo-morphology graph obtained in the embodiment is shown in fig. 3, and it can be seen from fig. 3 that the method provided by the invention can obtain a complete silicon-rich phase stereo structure, and can fully display the morphology and growth condition of the silicon-rich phase.
Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and it is intended to cover in the claims the invention as defined in the appended claims.

Claims (10)

1. A method for displaying a silicon-rich phase three-dimensional structure in an aluminum-silicon coating by a metallographic method is characterized by comprising the following steps: the method comprises sample preparation, chemical corrosion and microscopic observation, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coated steel plate, cutting a part of the aluminum-silicon coated steel plate to be used as a sample, and sequentially carrying out inlaying and polishing treatment on the sample;
(2) chemical corrosion: putting the sample prepared in the step (1) into corrosive liquid for chemical corrosion, wherein the corrosive liquid is prepared from hydrochloric acid aqueous solution and sodium chloride aqueous solution;
(3) and (4) microscopic observation: and after the chemical corrosion is finished, washing the sample, drying the sample, and observing the sample by using a ZISS metallographic microscope.
2. The method for displaying the silicon-rich phase spatial structure in the aluminum-silicon coating by a metallographic method according to claim 1, wherein the method comprises the following steps: the concrete operations of the inlaying in the step (1) are as follows: and horizontally placing the surface of the sample coating into an inlaying machine for inlaying, wherein the inlaid sample is ensured to be completely exposed on the surface of the coating.
3. The method for displaying the silicon-rich phase spatial structure in the aluminum-silicon coating by a metallographic method according to claim 1, wherein the method comprises the following steps: the polishing treatment in the step (1) comprises the following specific operations: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent on the polishing cloth, and then performing polishing treatment at the rotating speed of the polishing machine of 300-600 revolutions per minute.
4. A method of metallographically displaying the silicon-rich phase spatial structure in an al-si coating according to claim 3, characterised in that: the polishing cloth in the step (1) is pressure-sensitive adhesive wool fabric polishing cloth with the thickness of 200mm and 250 mm.
5. A method of metallographically displaying the silicon-rich phase spatial structure in an al-si coating according to claim 3, characterised in that: the particle size of the high-efficiency metallographic polishing agent in the step (1) is 0.5-2.5 mu m.
6. A method for metallographic representation of the silicon-rich phase spatial structure in an Al-Si coating according to any of claims 3-5, characterised in that: the polishing time of the polishing treatment in the step (1) is less than or equal to 30 s.
7. The method for displaying the silicon-rich phase spatial structure in the aluminum-silicon coating by a metallographic method according to claim 1, wherein the method comprises the following steps: the volume concentration of the hydrochloric acid in the hydrochloric acid aqueous solution in the step (2) is 10-12%.
8. The method for displaying the silicon-rich phase spatial structure in the aluminum-silicon coating by a metallographic method according to claim 1, wherein the method comprises the following steps: and (3) the mass concentration of sodium chloride in the sodium chloride aqueous solution in the step (2) is 5-8%.
9. The method for displaying the silicon-rich phase spatial structure in the aluminum-silicon coating by a metallographic method according to claim 1, wherein the method comprises the following steps: the corrosive liquid in the step (2) is prepared from a hydrochloric acid aqueous solution and a sodium chloride aqueous solution according to the volume ratio of 1: 1.
10. The method for displaying the silicon-rich phase spatial structure in the aluminum-silicon coating by a metallographic method according to claim 1, wherein the method comprises the following steps: and (3) the corrosion time of the chemical corrosion in the step (2) is 10-20 s.
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