CN113092199A - Cadmium stannate metallographic specimen and preparation method thereof - Google Patents
Cadmium stannate metallographic specimen and preparation method thereof Download PDFInfo
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- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 103
- 229940071182 stannate Drugs 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000005498 polishing Methods 0.000 claims abstract description 81
- 238000000034 method Methods 0.000 claims abstract description 37
- 230000007797 corrosion Effects 0.000 claims abstract description 23
- 238000005260 corrosion Methods 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 239000002253 acid Substances 0.000 claims description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000007654 immersion Methods 0.000 claims description 14
- 244000137852 Petrea volubilis Species 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 10
- 239000010931 gold Substances 0.000 claims description 10
- 229910052737 gold Inorganic materials 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003486 chemical etching Methods 0.000 claims description 4
- 230000007547 defect Effects 0.000 abstract description 18
- 239000013078 crystal Substances 0.000 abstract description 9
- 238000011156 evaluation Methods 0.000 abstract description 4
- 239000012770 industrial material Substances 0.000 abstract description 2
- 239000003518 caustics Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000010408 film Substances 0.000 description 6
- 239000000080 wetting agent Substances 0.000 description 6
- 239000013077 target material Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- 238000004544 sputter deposition 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
- G01N1/286—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
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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
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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
- G01N1/286—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
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Abstract
The invention discloses a cadmium stannate metallographic specimen and a preparation method thereof, belonging to the field of industrial material preparation. According to the preparation method of the cadmium stannate metallographic specimen, the cadmium stannate specimen is subjected to specific grinding and mechanical polishing treatment, so that the defect that the metallographic phase is blurred during observation due to the inclined plane in the traditional grinding process can be effectively avoided; after the metallographic specimen is subjected to subsequent surface chemical corrosion treatment, microscopic structures can be clearly and completely observed under microscopic observation, and the sample has no obvious scratches, defects or pit defects; the method has the advantages of simple operation steps, low cost and short consumed time, and has practical significance in evaluating the condition of cadmium stannate target crystal grains and researching the performance. The invention also discloses the cadmium stannate metallographic specimen obtained by the preparation method of the cadmium stannate metallographic specimen, the surface of the product is flat, smooth and flawless, the microstructure is clear under microscopic observation, and effective evaluation on the size and uniformity of the crystal grain can be realized.
Description
Technical Field
The invention relates to the field of industrial material preparation, in particular to a cadmium stannate metallographic specimen and a preparation method thereof.
Background
The transparent conductive film is mainly classified into three types, i.e., a metal film, an oxide film, and other compound films. Cadmium stannate thin films have become one of the most widely studied compound thin films in recent years due to their excellent electrical and optical properties. At present, the cadmium stannate film is mainly prepared by sputtering a cadmium stannate target material, so the performance of the cadmium stannate target material has direct influence on the performance of the film. Since the size and uniformity of the crystal grain are one of the important influencing factors of the performance of the cadmium stannate target material, the observation of the size and uniformity of the crystal grain of the cadmium stannate target material has high practical value.
In the prior art, most of the detection methods for the grain size and the uniformity of the cadmium stannate target material adopt a section scanning electron microscope for direct observation, but the preparation of an observation sample of the method is complex, and the sample is generally required to be processed into a thin slice; meanwhile, the method has high testing cost, and part of grains are cracked in the sample preparation and breaking process. On the other hand, the metallographic observation method plays a significant role in the research of materials because it can judge the grain size and uniformity of a sample and has a low test cost. However, no report is available about the preparation of metallographic samples of cadmium stannate targets and metallographic observation.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide the preparation method of the cadmium stannate metallographic specimen, the method is simple and convenient to operate and low in cost, the vacancy of preparation of the cadmium stannate metallographic specimen in the prior art is made up, the surface of the prepared specimen is flat and free of defects, and the complete metallographic structure can be clearly observed under a metallographic microscope.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a cadmium stannate metallographic specimen comprises the following steps:
(1) cutting the cadmium stannate target into a cadmium stannate sample A according to a metallographic sample preparation standard;
(2) polishing a cadmium stannate sample A: firstly, polishing a sample by using 400-mesh water-based sand paper for a first preset time, and applying a vertical downward force to the sample during polishing; then, rotating the sample by 180 degrees and polishing the sample by the same method, wherein the polishing time is the same as the first preset time; after polishing is finished, sequentially using 800-mesh, 1500-mesh and 3000-mesh water-based sand paper to repeat the steps to obtain a cadmium stannate sample B; the water-based sand paper rotates the test sample for 90 degrees when being replaced;
(3) and (3) carrying out mechanical polishing treatment on the cadmium stannate sample B: firstly, mechanically polishing a sample by using gold velvet for a second preset time, and applying a vertical downward force to the sample during mechanical polishing; then, rotating the sample by 180 degrees and mechanically polishing the sample by the same method, wherein the mechanical polishing time is the same as the second preset time, so as to obtain a cadmium stannate sample C;
(4) and (4) carrying out metallographic chemical corrosion immersion treatment on the cadmium stannate sample C obtained in the step (3), washing the sample C clean, and naturally drying the sample C in the air to obtain the cadmium stannate metallographic sample.
According to the preparation method of the cadmium stannate metallographic specimen, the cadmium stannate specimen is subjected to specific grinding and mechanical polishing treatment, so that the defect that the metallographic phase is blurred during observation due to the inclined plane in the traditional grinding process can be effectively avoided; after the metallographic specimen is subjected to subsequent surface chemical corrosion treatment, a microstructure can be clearly and completely observed under a metallographic microscope, and the sample has no obvious scratch, defect or pit defect; the method has the advantages of simple operation steps, low cost and short consumed time, and has practical significance in evaluating the condition of cadmium stannate target crystal grains and researching the performance.
Preferably, the first preset time is 1-2 min, and the second preset time is 4-6 min.
The surface of the metallographic specimen can be effectively smoother and smoother under the grinding and mechanical polishing time, defects such as flaws or pits cannot occur, and the metallographic structure can be clearly shown under microscopic observation.
Preferably, the vertical downward force applied to the sample in the steps (2) and (3) is 20-25N.
The applied vertical force has moderate strength, and can effectively ensure that the phenomenon of oblique phase or metallographic fracture can not occur in the process of grinding and polishing the metallographic specimen.
Preferably, the polishing treatment and the mechanical polishing treatment in the steps (2) and (3) are performed by using a polishing machine, the water-based sand paper or the spun gold velvet is fixed on an electric turntable of the polishing machine during the treatment, the electric turntable rotates clockwise, and meanwhile, the cadmium stannate sample is placed in a direction perpendicular to the rotation tangent of the electric turntable according to the linear cutting lines.
More preferably, the rotating speed of the electric rotating disc during the grinding treatment is 100-200 r/min, and the rotating speed of the electric rotating disc during the mechanical polishing treatment is 200-300 r/min.
The metallographic specimen is polished and mechanically polished on the polishing machine, so that the direction consistency and the processing degree during polishing can be effectively guaranteed to be the same, and the metallographic specimen is not damaged while the surface is smooth.
Preferably, the metallographic corrosive agent used for the metallographic chemical corrosion immersion treatment is an acid solution obtained by mixing a solvent and an acid solution;
more preferably, the solvent is pure water, the volume ratio of the pure water to the acid liquor in the metallographic corrosive agent is 17:8, the acid liquor is a nitric acid solution, and the mass fraction of the nitric acid in the solution is 68%.
More preferably, the solvent is absolute ethyl alcohol, the volume ratio of the absolute ethyl alcohol to the acid liquor in the metallographic corrosive agent is 32.5:1, the acid liquor is a hydrochloric acid solution, and the mass fraction of the hydrochloric acid in the solution is 38%.
More preferably, the solvent is pure water, the volume ratio of the pure water to the acid liquor in the metallographic corrosive is 75:15, the acid liquor is a hydrochloric acid solution, and the mass fraction of the hydrochloric acid in the solution is 37%.
More preferably, the time of the metallographic chemical etching immersion treatment is 0.5-5 min.
After the chemical treatment of the specific acidic metallographic corrosive agent, the grain boundary of the metallographic structure of the cadmium stannate sample can be clearer during observation, and the surface structure of the sample cannot be damaged.
Preferably, the washing process in the step (4) is performed by sequentially using pure water and absolute ethyl alcohol, the washing time of the pure water is 10-120 s, and the washing time of the absolute ethyl alcohol is 5-30 s.
The residual liquid after the corrosion treatment can be sufficiently removed by washing with pure water and absolute ethyl alcohol, and the washing time is determined by the experimental screening of the inventor: the corrosion liquid residue can be caused by too short pure water washing time, and the crystal boundary is unclear when metallographic observation is carried out; however, the corroded surface of the sample is fragile, the washing time is too long, and the surface structure of the sample can be damaged due to the impulsive force of pure water, so that the metallographic observation is not facilitated. Similarly, too short washing time of absolute ethyl alcohol can cause pure water residue, so that the drying time is too long; too long a time will cause some damage to the surface structure of the sample after corrosion.
The invention also aims to provide the cadmium stannate metallographic specimen obtained by the preparation method of the cadmium stannate metallographic specimen.
The surface of the cadmium stannate metallographic specimen obtained by the method is flat, smooth and flawless, the metallographic microstructure can be clearly observed under microscopic observation, and effective evaluation on the size and uniformity of the crystal grains is realized.
The preparation method has the beneficial effects that the cadmium stannate metallographic specimen is subjected to specific grinding and mechanical polishing treatment, so that the defect that the metallographic phase is blurred during observation due to the inclined plane in the traditional grinding process can be effectively avoided; after the metallographic specimen is subjected to subsequent surface chemical corrosion treatment, a microstructure can be clearly and completely observed under a metallographic microscope, and the sample has no obvious scratch, defect or pit defect; the method has the advantages of simple operation steps, low cost and short consumed time, and has practical significance in evaluating the condition of cadmium stannate target crystal grains and researching the performance. The invention also provides the cadmium stannate metallographic specimen obtained by the preparation method of the cadmium stannate metallographic specimen, the surface of the product is flat, smooth and flawless, the microstructure is clear under microscopic observation, and effective evaluation on the size and uniformity of the crystal grains can be realized.
Drawings
FIG. 1 is a metallographic structure display diagram of a sample under 20-fold microscopic magnification before metallographic corrosion in a preparation method of a cadmium stannate metallographic sample according to embodiment 1 of the present invention;
FIG. 2 is a metallographic structure display diagram of a sample under a microscopic magnification of 100 times after metallographic corrosion in the preparation method of a cadmium stannate metallographic sample according to embodiment 1 of the present invention;
FIG. 3 is a metallographic structure display diagram of a sample under a microscopic magnification of 100 times after metallographic corrosion in the preparation method of a cadmium stannate metallographic sample according to embodiment 2 of the present invention;
FIG. 4 is a metallographic structure display diagram of a sample under a microscopic magnification of 100 times after metallographic corrosion in the preparation method of a cadmium stannate metallographic sample according to embodiment 3 of the present invention;
fig. 5 is a scanning electron microscope display image of the sample after metallographic corrosion in the preparation method of the cadmium stannate metallographic sample according to embodiment 1 of the present invention.
Detailed Description
In order to better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples and comparative examples, which are intended to be understood in detail, but not intended to limit the invention. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention. The experimental reagents and instruments designed for implementing the invention are common reagents and instruments unless otherwise specified.
Example 1
One embodiment of the preparation method of the cadmium stannate metallographic specimen comprises the following steps:
(1) according to the metallographic sample preparation standard, cutting a cadmium stannate target into a cadmium stannate sample A by using a wire;
(2) polishing a cadmium stannate sample A: the method comprises the following steps of firstly, polishing a sample by using 400-mesh water-based abrasive paper, fixing the abrasive paper with a set specification on an electric turntable of a polishing machine during polishing, taking pure water as a wetting agent, enabling the electric turntable to rotate clockwise, setting the rotating speed to be 200r/min, polishing for 1min, placing a cadmium stannate sample A in a direction perpendicular to a linear cutting line and a rotating tangent of the electric turntable during polishing, and applying 20N vertical downward force to the sample; then, rotating the sample by 180 degrees and grinding for 1min by the same method; after polishing is finished, sequentially using 800-mesh, 1500-mesh and 3000-mesh water-based sand paper to repeat the steps to obtain a cadmium stannate sample B; the water-based sand paper rotates the test sample for 90 degrees when being replaced;
(3) and (3) carrying out mechanical polishing treatment on the cadmium stannate sample B: firstly, mechanically polishing a sample by using gold velvet, fixing the gold velvet on an electric turntable of a polishing machine during treatment, adding diamond polishing solution by using pure water as a wetting agent, enabling the electric turntable to rotate clockwise, mechanically polishing for 5min at a set rotating speed of 300r/min, placing a cadmium stannate sample A in a direction vertical to a linear cutting line and a rotating tangent of the electric turntable during polishing, and applying 20N vertical downward force to the sample; (ii) a Then, rotating the sample by 180 degrees and mechanically polishing the sample for 5min by the same method to obtain a cadmium stannate sample C;
(4) carrying out metallographic chemical corrosion immersion treatment on the cadmium stannate sample C obtained in the step (3) for 5min, sequentially and respectively washing the sample C with pure water for 30s and absolute ethyl alcohol for 5s, and naturally drying the sample C to obtain the cadmium stannate metallographic sample; the metallographic corrosive agent used for the metallographic chemical corrosion immersion treatment is an acid solution obtained by mixing pure water and an acid solution, wherein the volume ratio of the pure water to the acid solution is 17:8, the acid solution is a nitric acid solution, and the mass fraction of nitric acid in the nitric acid solution is 68%.
The microscopic structure observation of the cadmium stannate sample C and the finally prepared cadmium stannate metallographic sample in the embodiment is carried out, as shown in fig. 1 and 2, it can be obviously seen that compared with the metallographic corrosion, the microscopic structure of the finally prepared sample after corrosion is clear and complete, and no scratch, defect or pit defect exists, which indicates that the cadmium stannate metallographic sample prepared by the method in the embodiment is successfully prepared and has excellent quality, and as can be seen through the observation of a scanning electron microscope (as shown in fig. 5), the particle outline is clear and visible, and the grain evaluation can be effectively carried out.
Example 2
One embodiment of the preparation method of the cadmium stannate metallographic specimen comprises the following steps:
(1) according to the metallographic sample preparation standard, cutting a cadmium stannate target into a cadmium stannate sample A by using a wire;
(2) polishing a cadmium stannate sample A: the method comprises the following steps of firstly, polishing a sample by using 400-mesh water-based abrasive paper, fixing the abrasive paper with a set specification on an electric turntable of a polishing machine during polishing, taking pure water as a wetting agent, enabling the electric turntable to rotate clockwise, setting the rotating speed to be 200r/min, polishing for 1min, placing a cadmium stannate sample A in a direction perpendicular to a linear cutting line and a rotating tangent of the electric turntable during polishing, and applying 20N vertical downward force to the sample; then, rotating the sample by 180 degrees and grinding for 1min by the same method; after polishing is finished, sequentially using 800-mesh, 1500-mesh and 3000-mesh water-based sand paper to repeat the steps to obtain a cadmium stannate sample B; the water-based sand paper rotates the test sample for 90 degrees when being replaced;
(3) and (3) carrying out mechanical polishing treatment on the cadmium stannate sample B: firstly, mechanically polishing a sample by using gold velvet, fixing the gold velvet on an electric turntable of a polishing machine during treatment, adding diamond polishing solution by using pure water as a wetting agent, enabling the electric turntable to rotate clockwise, mechanically polishing for 5min at a set rotating speed of 300r/min, placing a cadmium stannate sample A in a direction vertical to a linear cutting line and a rotating tangent of the electric turntable during polishing, and applying 20N vertical downward force to the sample; (ii) a Then, rotating the sample by 180 degrees and mechanically polishing the sample for 5min by the same method to obtain a cadmium stannate sample C;
(4) carrying out metallographic chemical corrosion immersion treatment on the cadmium stannate sample C obtained in the step (3) for 60s, sequentially washing with pure water for 2min and absolute ethyl alcohol for 30s respectively, and naturally drying to obtain the cadmium stannate metallographic sample; the metallographic corrosive agent used for the metallographic chemical corrosion immersion treatment is an acid solution obtained by mixing absolute ethyl alcohol and an acid solution, wherein the volume ratio of the absolute ethyl alcohol to the acid solution is 32.5:1, the acid solution is a hydrochloric acid solution, and the mass fraction of hydrochloric acid in the hydrochloric acid solution is 38%.
When microscopic structure observation is performed on the cadmium stannate metallographic specimen finally prepared in the embodiment, as shown in fig. 3, it is obvious that the microscopic structure of the final sample is clear and complete and has no scratch, defect or pit defect, similar to that of the embodiment 1.
Example 3
One embodiment of the preparation method of the cadmium stannate metallographic specimen comprises the following steps:
(1) according to the metallographic sample preparation standard, cutting a cadmium stannate target into a cadmium stannate sample A by using a wire;
(2) polishing a cadmium stannate sample A: the method comprises the following steps of firstly, polishing a sample by using 400-mesh water-based abrasive paper, fixing the abrasive paper with a set specification on an electric turntable of a polishing machine during polishing, taking pure water as a wetting agent, enabling the electric turntable to rotate clockwise, setting the rotating speed to be 100r/min, polishing for 2min, placing a cadmium stannate sample A in a direction perpendicular to a linear cutting line and a rotating tangent of the electric turntable during polishing, and applying 20N vertical downward force to the sample; then, rotating the sample by 180 degrees and grinding for 2min by the same method; after polishing is finished, sequentially using 800-mesh, 1500-mesh and 3000-mesh water-based sand paper to repeat the steps to obtain a cadmium stannate sample B; the water-based sand paper rotates the test sample for 90 degrees when being replaced;
(3) and (3) carrying out mechanical polishing treatment on the cadmium stannate sample B: firstly, mechanically polishing a sample by using gold velvet, fixing the gold velvet on an electric turntable of a polishing machine during treatment, adding diamond polishing solution by using pure water as a wetting agent, enabling the electric turntable to rotate clockwise, mechanically polishing for 4min at a set rotating speed of 300r/min, placing a cadmium stannate sample A in a direction vertical to a linear cutting line and a rotating tangent of the electric turntable during polishing, and applying 20N vertical downward force to the sample; then, rotating the sample by 180 degrees and mechanically polishing the sample for 4min by the same method to obtain a cadmium stannate sample C;
(4) carrying out metallographic chemical corrosion immersion treatment on the cadmium stannate sample C obtained in the step (3) for 50s, sequentially washing the sample C with pure water for 30s and absolute ethyl alcohol for 10s respectively, and naturally drying the sample C to obtain the cadmium stannate metallographic sample; the metallographic corrosive agent used for the metallographic chemical corrosion immersion treatment is an acid solution obtained by mixing pure water and an acid solution, wherein the volume ratio of the pure water to the acid solution is 75:15, the acid solution is a hydrochloric acid solution, and the mass fraction of hydrochloric acid in the hydrochloric acid solution is 37%.
When microscopic structure observation is performed on the cadmium stannate metallographic specimen finally prepared in the embodiment, as shown in fig. 4, it is obvious that the microscopic structure of the final sample is clear and complete and has no scratch, defect or pit defect, similar to that of the embodiment 1.
Comparative example 1
The comparative example differs from example 1 only in that the volume ratio of pure water to acid solution in the metallographic etchant used in the metallographic chemical etching immersion treatment was 25: 3.
Through test and detection, the product obtained by the comparative example cannot observe a clear microstructure and measure the grain size.
Comparative example 2
The comparative example only differs from example 1 in that the solvent in the metallographic etchant used in the metallographic chemical etching immersion treatment is absolute ethyl alcohol.
Through test and detection, the product obtained by the comparative example cannot observe a clear microstructure and measure the grain size.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation method of the cadmium stannate metallographic specimen is characterized by comprising the following steps of:
(1) cutting the cadmium stannate target into a cadmium stannate sample A according to a metallographic sample preparation standard;
(2) polishing a cadmium stannate sample A: firstly, polishing a sample by using 400-mesh water-based sand paper for a first preset time, and applying a vertical downward force to the sample during polishing; then, rotating the sample by 180 degrees and polishing the sample by the same method, wherein the polishing time is the same as the first preset time; after polishing is finished, sequentially using 800-mesh, 1500-mesh and 3000-mesh water-based sand paper to repeat the steps to obtain a cadmium stannate sample B; the water-based sand paper rotates the test sample for 90 degrees when being replaced;
(3) and (3) carrying out mechanical polishing treatment on the cadmium stannate sample B: firstly, mechanically polishing a sample by using gold velvet for a second preset time, and applying a vertical downward force to the sample during mechanical polishing; then, rotating the sample by 180 degrees and mechanically polishing the sample by the same method, wherein the mechanical polishing time is the same as the second preset time, so as to obtain a cadmium stannate sample C;
(4) and (4) carrying out metallographic chemical corrosion immersion treatment on the cadmium stannate sample C obtained in the step (3), washing the sample C clean, and naturally drying the sample C in the air to obtain the cadmium stannate metallographic sample.
2. The method for preparing the cadmium stannate metallographic specimen according to claim 1, wherein the first predetermined time is 1 to 2min, and the second predetermined time is 4 to 6 min.
3. The method for preparing the cadmium stannate metallographic specimen according to claim 1, wherein the vertical downward force applied to the specimen in the steps (2) and (3) is 20 to 25N.
4. The method for preparing the cadmium stannate metallographic specimen according to claim 1, wherein the polishing treatment and the mechanical polishing treatment in the steps (2) and (3) are performed by using a polishing machine, and in the treatment, water-based abrasive paper or spun gold velvet is fixed on an electric turntable of the polishing machine, the electric turntable rotates clockwise, and the cadmium stannate metallographic specimen is placed in a direction perpendicular to a rotation tangent of the electric turntable according to linear cutting lines; the rotating speed of the electric rotating disc during the grinding treatment is 100-200 r/min, and the rotating speed of the electric rotating disc during the mechanical polishing treatment is 200-300 r/min.
5. The method for preparing the cadmium stannate metallographic specimen according to claim 1, wherein the metallographic etchant used for the metallographic chemical etching immersion treatment is an acid solution obtained by mixing a solvent and an acid solution; the time of the metallographic chemical corrosion immersion treatment is 0.5-5 min.
6. The method for preparing the cadmium stannate metallographic specimen according to claim 5, wherein the solvent is pure water, the volume ratio of the pure water to the acid solution in the metallographic etchant is 17:8, the acid solution is a nitric acid solution, and the mass fraction of the nitric acid in the solution is 68%.
7. The method for preparing the cadmium stannate metallographic specimen according to claim 5, wherein the solvent is absolute ethyl alcohol, the volume ratio of the absolute ethyl alcohol to the acid solution in the metallographic etchant is 32.5:1, the acid solution is a hydrochloric acid solution, and the mass fraction of the hydrochloric acid in the solution is 38%.
8. The method for preparing the cadmium stannate metallographic specimen according to claim 5, wherein the solvent is pure water, the volume ratio of the pure water to the acid solution in the metallographic etchant is 75:15, the acid solution is a hydrochloric acid solution, and the mass fraction of the hydrochloric acid in the solution is 37%.
9. The method for preparing the cadmium stannate metallographic specimen according to claim 1, wherein the rinsing process in the step (4) is performed by using pure water and absolute ethyl alcohol in sequence, the rinsing time of the pure water is 10-120 s, and the rinsing time of the absolute ethyl alcohol is 5-30 s.
10. The cadmium stannate metallographic specimen obtained by the method for preparing the cadmium stannate metallographic specimen according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202110273640.XA CN113092199A (en) | 2021-03-12 | 2021-03-12 | Cadmium stannate metallographic specimen and preparation method thereof |
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| CN113670236A (en) * | 2021-10-21 | 2021-11-19 | 广东奥迪威传感科技股份有限公司 | Thickness detection method of silver-tin interface metal eutectic layer |
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Inventor after: Zhou Rongyan Inventor after: Wu Caihong Inventor after: Yu Fei Inventor after: Wen Chongbin Inventor before: Zhou Rongyan Inventor before: Wu Caihong Inventor before: Yu Fei Inventor before: Wen Chongbin |
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