CN113865966A - Corrosive liquid for displaying aluminum-rich phase dendrite of aluminum-silicon layer and dendrite measurement method - Google Patents
Corrosive liquid for displaying aluminum-rich phase dendrite of aluminum-silicon layer and dendrite measurement method Download PDFInfo
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- CN113865966A CN113865966A CN202110955929.XA CN202110955929A CN113865966A CN 113865966 A CN113865966 A CN 113865966A CN 202110955929 A CN202110955929 A CN 202110955929A CN 113865966 A CN113865966 A CN 113865966A
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- 210000001787 dendrite Anatomy 0.000 title claims abstract description 74
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 49
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 49
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000007788 liquid Substances 0.000 title claims abstract description 13
- 238000000691 measurement method Methods 0.000 title abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000005260 corrosion Methods 0.000 claims abstract description 18
- 230000007797 corrosion Effects 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 238000005530 etching Methods 0.000 claims abstract description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- 229910018125 Al-Si Inorganic materials 0.000 claims description 6
- 229910018520 Al—Si Inorganic materials 0.000 claims description 6
- 238000003486 chemical etching Methods 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 24
- 238000000576 coating method Methods 0.000 abstract description 24
- 238000009826 distribution Methods 0.000 abstract description 10
- 238000001514 detection method Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 description 26
- 239000010410 layer Substances 0.000 description 21
- 239000004744 fabric Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 238000005406 washing Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 210000002268 wool Anatomy 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/20—Sample handling devices or methods
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Radiology & Medical Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
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- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention belongs to the technical field of metal coating detection, and particularly provides a corrosive liquid for displaying aluminum-rich phase dendrites of an aluminum-silicon layer and a dendrite measurement method. The provided corrosive liquid comprises sodium hydroxide solution with the mass concentration g/ml of l.2-10% and hydrochloric acid solution with the volume concentration v/v of 0.1-0.5%; the method for displaying the aluminum-silicon-layer aluminum-rich phase dendrite comprises the steps of preparing a sample, carrying out chemical corrosion by adopting the corrosion solution, cleaning and observing by a scanning electron microscope; and after aluminum-silicon-layer aluminum-rich phase dendrites are observed, selecting 3-8 dendrites, measuring the sizes of the dendrites, and dividing the total size by the number of the dendrites to obtain the dendrite spacing. The etching solution and the method provided by the invention can obtain a complete and clear aluminum-rich phase dendrite three-dimensional structure, can fully display the morphology, size distribution and growth condition of the aluminum-rich phase dendrite, can accurately measure the size of the dendrite spacing, and have the characteristics of low detection cost, rapidness, simplicity, accuracy and safety.
Description
Technical Field
The invention belongs to the technical field of metal coating detection, and particularly relates to a corrosive liquid for displaying aluminum-rich phase dendrites of an aluminum-silicon layer and a dendrite measurement 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. The performance of the aluminum-silicon layer in the aluminum-silicon coating directly influences the service performance of the coating, and particularly, the dendritic structure of the aluminum-rich phase is directly related to the production process, so that the research on the dendritic morphology and the spacing of the aluminum-rich phase is significant. At present, the research aiming at the phase structure of the aluminum-silicon-plated coating mainly stays on the phase structure of the plane and the cross section of the aluminum-silicon layer, the method can only display a part of the aluminum-rich phase, and can not display the whole three-dimensional appearance of the aluminum-rich phase.
The method provided by the invention can clearly and completely display the three-dimensional morphology of the aluminum-rich phase dendrite structure in the aluminum-silicon coating layer for cold stamping, accurately measure the size of the complete aluminum-rich phase dendrite, observe the distribution of the aluminum-rich phase dendrite and accurately measure the dendrite spacing of the aluminum-rich phase dendrite, change the tradition that the phase structure of the aluminum-silicon coating layer for cold stamping adopts the surface and the cross section (can not display the three-dimensional morphology), and enable the research of the coating phase structure to enter a deeper stage.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a corrosive liquid for displaying aluminum-silicon-layer aluminum-rich phase dendrite and a dendrite spacing measuring method, the provided method can obtain a complete and clear aluminum-rich phase dendrite three-dimensional structure, can fully display the morphology, size distribution and growth condition of the aluminum-rich phase dendrite, can accurately measure the size of the dendrite spacing, and has the characteristics of low detection cost, rapidness, simplicity, accuracy and safety.
In order to solve the technical problems, the invention adopts the technical scheme that:
an etching solution for displaying aluminum-rich phase dendrites of an aluminum-silicon layer comprises a sodium hydroxide solution with the mass concentration g/ml of l.2% -10% and a hydrochloric acid solution with the volume concentration v/v of 0.1-0.5%.
The invention also provides a method for displaying the aluminum-rich phase dendrite of the aluminum-silicon layer, which comprises the steps of preparing a sample, carrying out chemical corrosion by adopting the corrosive liquid, cleaning and observing by a scanning electron microscope.
The method for displaying the aluminum-silicon-layer aluminum-rich phase dendrite comprises the specific operation of chemical corrosion, namely, placing an aluminum-silicon coating steel plate subjected to inlaying and polishing treatment into a sodium hydroxide solution with the mass concentration of l.2-10% g/ml, placing a hydrochloric acid solution with the volume concentration of 0.1-0.5% v/v after chemical corrosion for 3-15 minutes, and shaking and corroding for 3-5 seconds.
The invention also provides a method for measuring the dendritic spacing of the aluminum-silicon-layer aluminum-rich phase, which is specifically characterized in that after the dendritic crystals of the aluminum-silicon-layer aluminum-rich phase are observed by adopting the method, 3-8 dendritic crystals are selected, the sizes of the dendritic crystals are measured, and the total size is divided by the number of the dendritic crystals, so that the dendritic spacing is obtained.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
1. the corrosion liquid provided by the invention can clearly and completely display the three-dimensional morphology of the aluminum-rich phase dendrite in the aluminum-silicon coating aluminum-silicon layer for cold stamping, and accurately measure the dendrite spacing of the aluminum-rich phase dendrite in the aluminum-silicon layer.
2. The method provided by the invention can clearly and completely display and observe the structure, morphology, proportion, size and distribution of the aluminum-rich phase dendrite, can accurately measure the dendrite spacing of the dendrite, and can provide a basis for process improvement and quality improvement.
3. The method provided by the invention has the characteristics of low detection cost, rapidness, simplicity, accuracy and safety.
Drawings
FIG. 1 shows the three-dimensional morphology and dendrite spacing of the aluminum-rich dendrites in the Al-Si layer obtained in example 1;
FIG. 2 shows the three-dimensional morphology and dendrite spacing of the aluminum-rich dendrites in the Al-Si layer obtained in example 2;
FIG. 3 shows the three-dimensional morphology and dendrite spacing of the aluminum-rich dendrites in the Al-Si layer obtained in example 3;
FIG. 4 is a phase structure diagram of the Al-Si coating obtained in comparative example 1;
fig. 5 is a phase structure diagram of the aluminum-silicon coating layer obtained in comparative example 2.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example 1
A method for displaying and measuring aluminum-rich phase dendrites and the spacing thereof in an aluminum-silicon layer comprises sample preparation, chemical corrosion, cleaning and microscopic observation, and specifically comprises the following operations:
(1) preparing a sample: taking an aluminum-silicon coating steel plate (DC 51D + AS mark), cutting a sample with the thickness of 15mm multiplied by 15mm, 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 2.5 microns on a pressure-sensitive adhesive wool fabric polishing cloth with the particle size of 200mm, and then performing polishing treatment for 15s at the rotating speed of a polishing machine of 300 revolutions per minute.
(2) Chemical corrosion: and (2) putting the sample prepared in the step (1) into a sodium hydroxide solution with the mass concentration of 4%, chemically corroding for 3 minutes, then putting dilute hydrochloric acid with the volume concentration of 0.3%, and shaking and corroding for 5 seconds.
(3) Cleaning: and washing the corroded sample for 1 minute by using clean water, ultrasonically cleaning for 2 minutes, washing by using alcohol, and then blowing to dry.
(4) And (3) observing by a scanning electron microscope: and (4) putting the sample cleaned in the step (3) under a KYKY-EM3200 scanning electron microscope, observing the morphology, size and distribution of the aluminum-rich phase dendrites, and calculating the dendrite spacing.
The three-dimensional morphology of the aluminum-rich phase dendrite in the aluminum-silicon coating aluminum-silicon layer for cold stamping obtained by the embodiment is shown in fig. 1, and as can be seen from fig. 1, the method can clearly display the morphology, size, distribution and growth conditions of the aluminum-rich phase dendrite; then, the dendrite spacing is calculated: 3 dendrites were selected and measured to have a size of 25.47 microns between them, and the dendrite spacing was calculated to be 8.49 microns by dividing the total size by the number of dendrites.
Example 2
A method for displaying and measuring aluminum-rich phase dendrites and the spacing thereof in an aluminum-silicon layer comprises sample preparation, chemical corrosion, cleaning and microscopic observation, and specifically comprises the following operations:
(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: and (2) putting the sample prepared in the step (1) into a sodium hydroxide solution with the mass concentration of 1.2%, chemically corroding for 15 minutes, then putting dilute hydrochloric acid with the volume concentration of 0.1%, and shaking and corroding for 3 seconds.
(3) Cleaning: and washing the corroded sample for 1 minute by using clean water, ultrasonically cleaning for 2 minutes, washing by using alcohol, and then blowing to dry.
(4) And (3) observing by a scanning electron microscope: and (4) putting the sample cleaned in the step (3) under a KYKY-EM3200 scanning electron microscope, observing the morphology, size and distribution of the aluminum-rich phase dendrites, and calculating the dendrite spacing.
The three-dimensional morphology of the aluminum-rich phase dendrite in the aluminum-silicon coating aluminum-silicon layer for cold stamping obtained by the embodiment is shown in fig. 2, and as can be seen from fig. 2, the method can clearly display the morphology, size, distribution and growth conditions of the aluminum-rich phase dendrite; then, the dendrite spacing is calculated: 5 dendrites were selected and measured to have a size of 69.52 microns between them, and the dendrite spacing was calculated to be 13.904 microns by dividing the total size by the number of dendrites.
Example 3
A method for displaying and measuring aluminum-rich phase dendrites and the spacing thereof in an aluminum-silicon layer comprises sample preparation, chemical corrosion, cleaning and scanning electron microscope observation, and specifically comprises the following operations:
(1) preparing a sample: taking an aluminum-silicon coating steel plate (DC 53D + 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: and (2) putting the sample prepared in the step (1) into a sodium hydroxide solution with the mass concentration of 10%, chemically corroding for 10 minutes, then putting dilute hydrochloric acid with the volume concentration of 0.5%, and shaking and corroding for 4 seconds.
(3) Cleaning: and washing the corroded sample for 1 minute by using clean water, ultrasonically cleaning for 2 minutes, washing by using alcohol, and then blowing to dry.
(4) And (3) observing by a scanning electron microscope: and (4) putting the sample cleaned in the step (3) under a KYKY-EM3200 scanning electron microscope, observing the morphology, size and distribution of the aluminum-rich phase dendrites, and calculating the dendrite spacing.
The three-dimensional morphology of the aluminum-rich phase dendrite in the aluminum-silicon coating aluminum-silicon layer for cold stamping obtained by the embodiment is shown in fig. 3, and as can be seen from fig. 3, the method can clearly display the morphology, size, distribution and growth conditions of the aluminum-rich phase dendrite; then, the dendrite spacing is calculated: 5 dendrites were selected and measured to have a size of 54.72 microns, and the dendrite spacing was calculated to be 10.944 microns by dividing the total size by the number of dendrites.
Comparative example 1
(1) Preparing a sample: taking an aluminum-silicon coating steel plate (DC 51D + AS mark), cutting a sample with the thickness of 15mm multiplied by 15mm, placing the sample perpendicular to the coating surface into an embedding machine for embedding, carrying out coarse grinding and fine grinding on the sample, and then carrying out 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 2.5 microns on a pressure-sensitive adhesive wool fabric polishing cloth with the particle size of 200mm, and then performing polishing treatment for 15s at the rotating speed of a polishing machine of 300 revolutions per minute.
(2) Chemical corrosion: and (2) placing the sample prepared in the step (1) into a corrosive liquid for chemical corrosion, wherein the corrosive liquid is 4% nitric acid alcohol, and corroding for 5 seconds.
(3) And (4) washing the sample with alcohol and drying.
(4) The sample is placed under a microscope for observation, the phase structure diagram of the sample is shown in figure 4, and the complete morphology of the aluminum-rich phase dendrites cannot be seen.
Comparative example 2
(1) Preparing a sample: taking an aluminum-silicon coated steel plate (DC 52D + AS mark), cutting a sample with the thickness of 15mm multiplied by 15mm, placing the surface of a sample coating into a mosaic machine for mosaic, and polishing the sample, which specifically comprises the following steps: 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 15s at the rotating speed of a polishing machine of 300 revolutions per minute.
(2) Chemical corrosion: and (2) placing the sample prepared in the step (1) into a corrosive liquid for chemical corrosion, wherein the corrosive liquid is 4% nitric acid alcohol, and corroding for 5 seconds.
(3) And (4) washing the sample with alcohol and drying.
(4) The sample is placed under a microscope for observation, the phase structure diagram of the sample is shown in figure 5, and the complete morphology of the aluminum-rich phase dendrites cannot be seen.
Claims (4)
1. The etching solution for displaying the aluminum-rich phase dendrites of the aluminum-silicon layer is characterized by comprising a sodium hydroxide solution with the mass concentration g/ml of l.2% -10% and a hydrochloric acid solution with the volume concentration v/v of 0.1-0.5%.
2. A method for displaying aluminum-rich phase dendrites on an aluminum-silicon layer, which is characterized by comprising the steps of preparing a sample, carrying out chemical corrosion by using the corrosive liquid according to claim 1, cleaning and observing by a scanning electron microscope.
3. The method for displaying the aluminum-rich phase dendrites on the Al-Si layer according to claim 2, wherein the chemical etching is performed by putting the inlaid and polished Al-Si coated steel plate into a sodium hydroxide solution with a mass concentration of l.2% -10%, chemically etching for 3-15 minutes, then putting a hydrochloric acid solution with a volume concentration of v/v of 0.1-0.5%, and shaking for 3-5 seconds.
4. A method for measuring the dendritic spacing of an aluminum-silicon-layer aluminum-rich phase is characterized in that the method specifically comprises the steps of selecting 3-8 dendritic crystals after observing aluminum-silicon-layer aluminum-rich phase dendritic crystals by the method of claim 2 or 3, measuring the sizes of the dendritic crystals, and dividing the total size by the number of the dendritic crystals to obtain the dendritic spacing.
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