CN113588363B - Metallographic sample preparation and display method for iron-aluminum-silicon layer of aluminum-silicon coated steel plate - Google Patents
Metallographic sample preparation and display method for iron-aluminum-silicon layer of aluminum-silicon coated steel plate Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 46
- 239000010959 steel Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- -1 iron-aluminum-silicon Chemical compound 0.000 title claims abstract description 29
- 238000005498 polishing Methods 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 33
- 238000000576 coating method Methods 0.000 claims abstract description 33
- 239000012085 test solution Substances 0.000 claims abstract description 30
- 238000000227 grinding Methods 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000007797 corrosion Effects 0.000 claims abstract description 18
- 238000005260 corrosion Methods 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 17
- 238000005520 cutting process Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000003486 chemical etching Methods 0.000 claims abstract description 8
- KJYQVRBDBPBZTD-UHFFFAOYSA-N methanol;nitric acid Chemical compound OC.O[N+]([O-])=O KJYQVRBDBPBZTD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003973 paint Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- 238000007790 scraping Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims abstract description 5
- 239000000523 sample Substances 0.000 claims description 91
- 244000137852 Petrea volubilis Species 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000004744 fabric Substances 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- 239000012488 sample solution Substances 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 33
- 238000010586 diagram Methods 0.000 description 6
- 238000005530 etching Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000003628 erosive effect Effects 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 229910018125 Al-Si Inorganic materials 0.000 description 3
- 229910018520 Al—Si Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 238000005464 sample preparation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 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
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- 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
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Abstract
The invention discloses a metallographic sample preparation and display method of an iron-aluminum-silicon layer after hot stamping forming of an aluminum-silicon coated steel plate, which comprises the following steps: a steel plate with aluminum-silicon coating is taken, a layer of finish paint is scraped on the surface of the steel plate by a scraping rod with the RDS number of 20-50, the thickness of a paint film is 20-50 mu m, and the steel plate is put into a box type drying furnace for drying and heat preservation, and is dried by cold air after water cooling; cutting a sample by linear cutting, and putting the sample into a mosaic machine for mosaic; then grinding and polishing; (2) chemical etching: carrying out chemical corrosion on the sample prepared in the step (1) in a test solution a and a test solution b in sequence, wherein the test solution a is 0.1% of nitric acid methanol solution, and the test solution b is 0.1% of nitric acid+0.1% of HF aqueous solution; (3) microscopic observation: after the chemical corrosion is finished, the sample is washed clean by absolute ethyl alcohol, dried by a blower and observed under a ZISS metallographic microscope. The method provided by the invention can obtain a complete coating structure, can clearly display the morphology and the distribution state of each phase in the coating in the process of tissue observation, and has the characteristics of low detection and analysis cost, rapidness and simplicity.
Description
Technical Field
The invention belongs to the technical field of metal coating detection, and particularly relates to a metallographic sample preparation and display method for an iron-aluminum-silicon layer after hot stamping forming of an aluminum-silicon coated steel plate.
Background
Because the aluminized silicon coated steel plate has good oxidation resistance and corrosion resistance, the product is increasingly widely developed and applied, and the physical property detection technical requirement is also increasingly improved. At present, the change research of each phase of the coating after the hot stamping forming of the aluminized silicon coated steel plate is less, and particularly, the change research of an alloy layer is less. The structure and performance of the coating are changed after the hot stamping forming of the coated steel plate, and along with the completion of the hot stamping forming, the quality problems of the coating, such as cracking and adhesion failure of the coating, and the later phosphoelectrophoresis defects, are numerous, and the analysis of each phase in the coating structure is not needed to solve the problems. Therefore, analysis of the service performance of the coating is necessary to analyze the phase composition of the iron aluminum silicon layer in the coating, and thus, a simple and practical method for completing the phase composition and distribution of the iron aluminum silicon layer after hot stamping of the aluminum silicon coating product is urgently needed.
Because the aluminum-silicon plated product is very brittle after hot stamping forming, the integrity of the coating cannot be ensured by adopting a traditional metallographic sample preparation method, and meanwhile, each phase in an iron-aluminum-silicon layer cannot be distinguished by adopting a traditional nitrate alcohol etching agent, the purpose can be realized by adopting an XRD method at present, but the cost is high, and the sample preparation is difficult.
Disclosure of Invention
The invention aims to solve the technical problem of providing a metallographic sample preparation and display method for an iron-aluminum-silicon layer after hot stamping forming of an aluminum-silicon coated steel plate, wherein the provided method can obtain a complete coating structure, and can clearly display the morphology and distribution state of each phase in the coating in the process of observing the structure.
In order to solve the technical problems, the invention adopts the following technical scheme:
a metallographic sample preparation and display method for an aluminum-silicon coating steel plate iron-aluminum-silicon layer comprises sample preparation, chemical corrosion and microscopic observation, and specifically comprises the following steps:
(1) Sample preparation:
a steel plate with aluminum-silicon coating is adopted, a layer of finish paint with the thickness of about 20-50 mu m is scraped on the surface of the steel plate by a scraping rod with the RDS number of 20-50, and the steel plate is put into a box type drying furnace for drying, heat preservation and cold air drying after water cooling; cutting a sample with the length of (15+/-5) mm x (15+/-5) mm by using wire cutting, and putting the sample into a mosaic machine for mosaic;
coarsely grinding the inlaid sample on a grinder until the surface is flat and the scratch depths are consistent, and then grinding the inlaid sample with metallographic abrasive paper;
polishing the sample by using fine velvet polishing cloth uniformly sprayed with a 2.5 mu m metallographic polishing agent, and spraying absolute ethyl alcohol while polishing until the surface of the sample is bright and has no scratch;
(2) Chemical etching
Carrying out chemical corrosion on the sample prepared in the step (1) in a test solution a and a test solution b in sequence, wherein the test solution a is 0.1% of nitric acid methanol solution, and the test solution b is 0.1% of nitric acid+0.1% of HF aqueous solution;
(3) Microscopic observation
After the chemical corrosion is finished, the sample is washed clean by absolute ethyl alcohol, dried by a blower and observed under a ZISS metallographic microscope.
Further, the invention relates to a metallographic sample preparation and display method of an iron-aluminum-silicon layer of an aluminum-silicon coated steel plate, wherein: and (3) when the box-type drying furnace in the step (1) is used for drying, the furnace temperature is 347-352 ℃, and the heat preservation is carried out for 47-52 seconds.
Further, the invention relates to a metallographic sample preparation and display method of an iron-aluminum-silicon layer of an aluminum-silicon coated steel plate, wherein: and (3) grinding samples inlaid in the step (1) roughly, and then sequentially grinding on 280# metallographic sand paper, 400# metallographic sand paper, 600# metallographic sand paper and 800# metallographic sand paper.
Further, the invention relates to a metallographic sample preparation and display method of an iron-aluminum-silicon layer of an aluminum-silicon coated steel plate, wherein: and (3) when the sand paper in the step (1) is ground, the grinding direction is perpendicular to the previous scratch direction.
Further, the invention relates to a metallographic sample preparation and display method of an iron-aluminum-silicon layer of an aluminum-silicon coated steel plate, wherein: the polishing time of the sample in the step (1) is not more than 2 minutes.
Further, the invention relates to a metallographic sample preparation and display method of an iron-aluminum-silicon layer of an aluminum-silicon coated steel plate, wherein: in the step (2), the sample is eroded in the sample solution a for 1 second and eroded in the sample solution b for 1-2 seconds.
According to the invention, a painting mode is adopted to carry out surface protection on the sample in the sample preparation process, so that the surface layer can be effectively prevented from falling off in the sample preparation process.
The method provided by the invention can clearly show the morphology and distribution of each phase in the coating after the aluminum-silicon coating is formed by hot stamping, and solves the problems that the traditional nitrate alcohol etching agent can only show an alloy layer and an aluminum-silicon layer, cannot clearly show the morphology and distribution of an iron-aluminum-silicon layer and cannot distinguish each phase in the alloy layer.
The method can clearly display the form and the distribution of the iron-aluminum-silicon layer in the coating after the aluminum-silicon coating is formed by hot stamping, thereby adjusting the production process according to the composition and the distribution of the coating phase, improving the service performance of the coating, and having the characteristics of low detection and analysis cost, rapidness, simpleness and ensuring the integrity of the coating.
The beneficial effects of adopting above-mentioned technical scheme to produce lie in:
1. the invention changes the traditional sample preparation method of directly inlaid samples, and the obtained coating is complete and does not fall off.
2. The invention adopts the nitric acid methanol solution with the concentration of a.0.1 percent of the test solution, and the HF aqueous solution with the concentration of a nitric acid of a 0.1 percent of the test solution b.0.1 percent is used as the etching agent, so that the morphology, the proportion and the size of each phase in the coating can be clearly displayed, and the problem that the morphology of each phase after the hot stamping forming cannot be clearly displayed by the traditional nitric acid alcohol etching agent is solved.
3. The method has the characteristics of low detection and analysis cost, rapidness and simplicity.
Drawings
FIG. 1 is a metallographic structure diagram obtained in example 1;
FIG. 2 is a layer of Fe-Al-Si observed in example 1;
FIG. 3 is a metallographic structure diagram of comparative examples 1 to 3;
FIG. 4 is a metallographic structure obtained in example 2;
FIG. 5 is a layer of Fe-Al-Si observed in example 2;
FIG. 6 is a metallographic structure obtained in example 3;
FIG. 7 is a layer of Fe-Al-Si observed in example 3;
FIG. 8 is a metallographic structure diagram obtained in comparative example 2.
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 the metallographic structure of the iron-aluminum-silicon layer after hot stamping forming of the aluminum-silicon coated steel plate (1500+AS brand) comprises the following specific process steps of sample preparation, chemical corrosion and microscopic observation:
(1) Sample preparation:
a steel plate with aluminum-silicon coating is taken, a layer of Vigorboom finish paint with the thickness of about 20 mu m is coated on the surface of the steel plate by a RDS20 scraping rod, the steel plate is put into a box-type drying furnace, the furnace temperature is 350 ℃, the heat is preserved for 50 seconds, and cold air is dried after water cooling; cutting a sample with the length of 15mm multiplied by 15mm by linear cutting, and putting the sample into a mosaic machine for mosaic;
coarsely grinding the inlaid sample on a grinder until the surface is flat and the scratch depths are consistent, and then sequentially grinding on 280# metallographic sand paper, 400# metallographic sand paper, 600# metallographic sand paper and 800# metallographic sand paper, wherein the grinding direction is perpendicular to the previous scratch direction;
polishing the sample by using fine velvet polishing cloth uniformly sprayed with a 2.5 mu m metallographic polishing agent, spraying absolute ethyl alcohol while polishing, and polishing for 60 seconds, wherein the surface of the sample is bright and has no scratch;
(2) Chemical etching
Sequentially eroding the sample prepared in the step (1) in a test solution a for 1 second and in a test solution b for 1-2 seconds, wherein the test solution a is 0.1% of nitric acid methanol solution, and the test solution b is a mixed solution prepared from 0.1% of nitric acid and 0.1% of HF aqueous solution;
(3) Microscopic observation
After the chemical corrosion is finished, the sample is washed by absolute ethyl alcohol, dried by a blower, and observed under a ZISS metallographic microscope, a metallographic structure diagram is shown in figure 1, and a complete and continuous iron-aluminum-silicon layer is shown in figure 2.
Example 2
A steel plate with aluminum-silicon coating is taken, a layer of Vigorboom finish paint with the thickness of about 35 mu m is coated on the surface of the steel plate by a RDS 35 scraping rod, the steel plate is put into a box-type drying furnace, the furnace temperature is 347 ℃ for drying, the heat is preserved for 52 seconds, and the steel plate is dried by cold air after water cooling; cutting a 10mm multiplied by 10mm sample by linear cutting, and putting the sample into a mosaic machine for mosaic;
coarsely grinding the inlaid sample on a grinder until the surface is flat and the scratch depths are consistent, and then sequentially grinding on 280# metallographic sand paper, 400# metallographic sand paper, 600# metallographic sand paper and 800# metallographic sand paper, wherein the grinding direction is perpendicular to the previous scratch direction;
polishing the sample by using fine velvet polishing cloth uniformly sprayed with a 2.5 mu m metallographic polishing agent, spraying absolute ethyl alcohol while polishing, and polishing for 86 seconds, wherein the surface of the sample is bright and has no scratch;
(2) Chemical etching
Sequentially eroding the sample prepared in the step (1) in a test solution a for 1 second and in a test solution b for 1-2 seconds, wherein the test solution a is 0.1% of nitric acid methanol solution, and the test solution b is a mixed solution prepared from 0.1% of nitric acid and 0.1% of HF aqueous solution;
(3) Microscopic observation
After the chemical corrosion is finished, the sample is washed by absolute ethyl alcohol, dried by a blower, and observed under a ZISS metallographic microscope, a metallographic structure diagram is shown in fig. 4, and a complete and continuous iron-aluminum-silicon layer is shown in fig. 5.
Example 3
The aluminum-silicon coated steel plate is taken, a layer of Libang finish paint with the thickness of about 50 mu m is coated on the surface of the steel plate by a RDS50 scraping rod, the steel plate is put into a box-type drying furnace, the furnace temperature is 352 ℃ for drying, the heat is preserved for 47 seconds, and the steel plate is dried by cold air after water cooling; cutting a sample with the length of 20mm multiplied by 20mm by linear cutting, and putting the sample into a mosaic machine for mosaic;
coarsely grinding the inlaid sample on a grinder until the surface is flat and the scratch depths are consistent, and then sequentially grinding on 280# metallographic sand paper, 400# metallographic sand paper, 600# metallographic sand paper and 800# metallographic sand paper, wherein the grinding direction is perpendicular to the previous scratch direction;
polishing the sample by using fine velvet polishing cloth uniformly sprayed with a 2.5 mu m metallographic polishing agent, spraying absolute ethyl alcohol while polishing, and polishing for 110 seconds, wherein the surface of the sample is bright and has no scratch;
(2) Chemical etching
Sequentially eroding the sample prepared in the step (1) in a test solution a for 1 second and in a test solution b for 1-2 seconds, wherein the test solution a is 0.1% of nitric acid methanol solution, and the test solution b is a mixed solution prepared from 0.1% of nitric acid and 0.1% of HF aqueous solution;
(3) Microscopic observation
After the chemical corrosion is finished, the sample is washed by absolute ethyl alcohol, dried by a blower, and observed under a ZISS metallographic microscope, a metallographic structure diagram is shown in fig. 6, and a complete and continuous iron-aluminum-silicon layer is shown in fig. 7.
Comparative example 1
The aluminum-silicon coated steel plate (1500+AS brand) of the embodiment comprises a metallographic sample preparation and display method of a metallographic structure of an iron-aluminum-silicon layer after hot stamping forming, wherein the metallographic sample preparation and display method comprises sample preparation, chemical corrosion and microscopic observation, and the difference from embodiment 1 is that the chemical corrosion adopts different aggressive agents, and the specific process steps are as follows:
(1) Sample preparation:
a steel plate with aluminum-silicon coating is taken, a layer of Vigorboom finish paint with the thickness of about 20 mu m is coated on the surface of the steel plate by a RDS20 scraping rod, and the steel plate is put into a box-type drying furnace, dried at the furnace temperature of 350 ℃, kept for 50 seconds, cooled by water and dried by cold air; cutting a sample with the length of 15mm multiplied by 15mm by linear cutting, and putting the sample into a mosaic machine for mosaic;
coarsely grinding the inlaid sample on a grinder until the surface is flat and the scratch depths are consistent, and then sequentially grinding on 280# metallographic sand paper, 400# metallographic sand paper, 600# metallographic sand paper and 800# metallographic sand paper, wherein the grinding direction is perpendicular to the previous scratch direction;
polishing the sample by using fine velvet polishing cloth uniformly sprayed with a 2.5 mu m metallographic polishing agent, spraying absolute ethyl alcohol while polishing, and polishing for 60 seconds, wherein the surface of the sample is bright and has no scratch;
(2) Chemical etching
And (3) eroding the sample prepared in the step (1) by using 4% nitrate alcohol for 3 seconds.
(3) Microscopic observation
After the chemical corrosion is finished, the sample is washed clean by absolute ethyl alcohol, dried by a blower, and observed under a ZISS metallographic microscope, as shown in figure 3. The coating of this example was complete but did not clearly show the iron aluminum silicon phase.
The etching agent adopted in the comparative example 1 is 4% nitrate alcohol, the etching effect is poor, and the iron-aluminum-silicon phase cannot be clearly displayed; in contrast, the etchant used in example 1 contains HF, and since the FeAlSi phase can react with HF, it is significantly corroded, and the display is clear.
Comparative example 2
The aluminum-silicon coated steel plate (1500+AS brand) of the embodiment comprises metallographic sample preparation and display methods of a metallographic structure of an iron-aluminum-silicon layer after hot stamping forming, wherein the metallographic sample preparation and display methods comprise sample preparation, chemical corrosion and microscopic observation, and the difference from the embodiment 1 is that a sample is not subjected to surface protection by adopting a painting mode during sample preparation, and the specific process steps are as follows: :
(1) Sample preparation: taking an aluminum-silicon coated steel plate, cutting a sample with the length of 15mm multiplied by 15mm by linear cutting, and putting the sample into a mosaic machine for mosaic;
coarsely grinding the inlaid sample on a grinder until the surface is flat and the scratch depths are consistent, and then sequentially grinding on 280# metallographic sand paper, 400# metallographic sand paper, 600# metallographic sand paper and 800# metallographic sand paper, wherein the grinding direction is perpendicular to the previous scratch direction;
polishing the sample by using fine velvet polishing cloth uniformly sprayed with a 2.5 mu m metallographic polishing agent, spraying absolute ethyl alcohol while polishing, and polishing for 60 seconds, wherein the surface of the sample is bright and has no scratch;
(2) Chemical etching
Sequentially eroding the sample prepared in the step (1) in a test solution a for 1 second and in a test solution b for 1-2 seconds, wherein the test solution a is 0.1% of nitric acid methanol solution, and the test solution b is a mixed solution prepared from 0.1% of nitric acid and 0.1% of HF aqueous solution;
(3) Microscopic observation
After the chemical corrosion is finished, the sample is washed by absolute ethyl alcohol, dried by a blower, and observed under a ZISS metallographic microscope, the metallographic structure is shown in figure 8, the integrity of the coating is damaged, and the defect of an aluminum silicon layer is serious.
Claims (5)
1. A metallographic sample preparation and display method of an aluminum-silicon coating steel plate iron-aluminum-silicon layer is characterized by comprising the following steps: the method comprises the steps of sample preparation, chemical corrosion and microscopic observation, and comprises the following specific steps:
(1) Sample preparation
A steel plate with aluminum-silicon coating is adopted, a layer of finish paint with the thickness of about 20-50 mu m is scraped on the surface of the steel plate by a scraping rod with the RDS number of 20-50, and the steel plate is put into a box type drying furnace for drying, heat preservation and cold air drying after water cooling; cutting a sample with the length of (15+/-5) mm x (15+/-5) mm by using wire cutting, and putting the sample into a mosaic machine for mosaic;
coarsely grinding the inlaid sample on a grinder until the surface is flat, enabling the scratch depths to be consistent, and then grinding the inlaid sample with metallographic abrasive paper;
polishing the sample by using fine velvet polishing cloth uniformly sprayed with a 2.5 mu m metallographic polishing agent, and spraying absolute ethyl alcohol while polishing until the surface of the sample is bright and has no scratch;
(2) Chemical etching
Carrying out chemical corrosion on the sample prepared in the step (1) in a test solution a and a test solution b in sequence, wherein the test solution a is 0.1% of nitric acid methanol solution, and the test solution b is 0.1% of nitric acid+0.1% of HF aqueous solution;
(3) Microscopic observation
After the chemical corrosion is finished, the sample is washed clean by absolute ethyl alcohol, dried by a blower and observed under a ZISS metallographic microscope;
in the step (2), the sample is eroded in the sample solution a for 1 second and eroded in the sample solution b for 1-2 seconds.
2. The method for metallographic sample preparation and display of the iron-aluminum-silicon layer of the aluminum-silicon coated steel plate, which is characterized by comprising the following steps of: and (3) when the box-type drying furnace in the step (1) is used for drying, the furnace temperature is 347-352 ℃, and the heat preservation is carried out for 47-52 seconds.
3. The method for preparing and displaying the metallographic phase of the iron-aluminum-silicon layer of the aluminum-silicon coated steel plate, which is disclosed in claim 1, is characterized in that after the inlaid sample in the step (1) is coarsely ground, the inlaid sample is sequentially ground on 280# metallographic sand paper, 400# metallographic sand paper, 600# metallographic sand paper and 800# metallographic sand paper.
4. The method for metallographic sample preparation and display of the iron-aluminum-silicon layer of the aluminum-silicon coated steel plate according to claim 1, wherein the grinding direction is perpendicular to the previous scratch direction when the sand paper is ground in the step (1).
5. The method for metallographic sample preparation and display of iron-aluminum-silicon layer of aluminum-silicon coated steel plate according to claim 1, wherein the sample polishing time in the step (1) is not more than 2 minutes.
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