CN113866200A - Preparation method of segregation-method high-purity aluminum EBSD sample - Google Patents
Preparation method of segregation-method high-purity aluminum EBSD sample Download PDFInfo
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- CN113866200A CN113866200A CN202111150427.6A CN202111150427A CN113866200A CN 113866200 A CN113866200 A CN 113866200A CN 202111150427 A CN202111150427 A CN 202111150427A CN 113866200 A CN113866200 A CN 113866200A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 47
- 238000005204 segregation Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000001887 electron backscatter diffraction Methods 0.000 title claims abstract 9
- 238000005498 polishing Methods 0.000 claims abstract description 67
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000005070 sampling Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 30
- 239000010959 steel Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 18
- 238000005520 cutting process Methods 0.000 claims description 12
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 8
- 230000003064 anti-oxidating effect Effects 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 4
- 239000002390 adhesive tape Substances 0.000 claims description 4
- 239000002274 desiccant Substances 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 3
- 238000005553 drilling Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000011888 foil Substances 0.000 abstract description 25
- 238000004458 analytical method Methods 0.000 abstract description 14
- 238000012360 testing method Methods 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 229910052742 iron Inorganic materials 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000005464 sample preparation method Methods 0.000 description 3
- 241000723353 Chrysanthemum Species 0.000 description 2
- 235000007516 Chrysanthemum Nutrition 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000003860 storage 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
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/203—Measuring back scattering
-
- 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
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/053—Investigating materials by wave or particle radiation by diffraction, scatter or reflection back scatter
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/102—Different kinds of radiation or particles beta or electrons
Abstract
The invention provides a preparation method of a segregation method high-purity aluminum EBSD sample, belonging to the technical field of segregation method high-purity aluminum preparation, and comprising the following steps: manufacturing a clamping tool; mechanically sampling; mechanically grinding; mechanical polishing; electrolytic polishing; drying and storing. The method can conveniently and quickly obtain the sample test surface of the segregation method high-purity aluminum foil meeting the EBSD analysis requirements, provides convenience for obtaining the grain orientation information of the segregation method high-purity aluminum foil, such as single crystal orientation, texture occupancy, orientation difference distribution and the like, and lays a foundation for the correlation research of the texture evolution and the deformation of the segregation method high-purity aluminum foil. And the polishing clamping tool can be repeatedly used, so that the experimental time is greatly shortened, and the experimental cost is greatly reduced.
Description
Technical Field
The invention relates to the technical field of electronic aluminum foil detection and analysis, in particular to a preparation method of a segregation-method high-purity aluminum EBSD sample.
Background
The aluminum electrolytic capacitor is one of important elements in the electronic industry, and is widely applied to the traditional consumer electronics field and a plurality of emerging fields such as energy-saving lamps, new energy sources and the like. With the rapid development of the modern electronic industry, the integration level of electromechanical products is higher and higher, and capacitors are required to be advanced with time, and the progress is made towards 'ultra-large capacity and ultra-small volume'. To achieve this goal, one would typically increase the specific capacitance by chemical etching, and the annealed aluminum foil needs to have a strong cubic texture (cubic texture occupancy > 95%) because high purity aluminum is most susceptible to pitting along its crystallographic <001> direction.
The factors influencing the texture occupancy rate are various, wherein the influence of raw materials on the texture occupancy rate is not small, the two main sources of the high-purity aluminum ingot are provided at present, one is a widely applied three-layer liquid electrolytic refining method, the other is segregation method refined aluminum purification, the composition control is not more accurate than that of the three-layer liquid method, but the method has the advantages of obvious energy saving and consumption reduction, is a main means for obtaining high-purity aluminum in the future, and the problems of unstable texture control and the like still exist when the segregation method high-purity aluminum is used for preparing electronic aluminum foils in China at present.
The Electron Back Scattering Diffraction (EBSD) technology can simultaneously obtain the micro-morphology, structure and orientation distribution of the crystal material, is widely applied to the field of material analysis, and is an important means for analyzing the grain orientation and micro-texture condition of the segregation-method high-purity aluminum foil. However, because of the current few published data about the segregation method high-purity aluminum foil, the record of the sample preparation process of the EBSD sample is also few, when the EBSD sample of the aluminum foil is prepared conventionally, a small piece is cut from the complete aluminum foil directly for electrolytic polishing, but the sample prepared by the method is extremely easy to damage, and cannot be transported for a long distance. And the aluminum foil sample is softer, and the operation difficulty is very large. Chamelamely (2019) in order to mechanically polish the sample, the sample is embedded and cured by using epoxy resin, and the embedded resin is dissolved by using acetone after electrolytic polishing, so that the sample is favorably processed. However, resin curing typically takes several hours, and the use of resin and acetone solutions adds a number of variables, increases experimental error, and lengthens experimental time and cost. Therefore, it is necessary to perform a large number of tests on EBSD test of high-purity aluminum foil by segregation method and to summarize a complete and convenient sample preparation method.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a segregation-method high-purity aluminum EBSD sample, which adopts a clamping tool to assist in grinding, so that the experimental time is greatly shortened, and the experimental cost is greatly reduced.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a high-purity aluminum EBSD sample by a segregation method,
s1, manufacturing a polishing clamping tool: the base comprises a cylinder, a groove is formed in the top of the base, a screw hole is formed in the outer wall of one side of the groove, and a fixing screw penetrates through the screw hole.
S2, mechanical sampling: samples were taken by wire cutting.
S3, mechanical polishing: winding a sample on a steel ingot, placing the steel ingot in a groove of the clamping tool, selecting the smoothest surface as a polishing surface to be upward, fixing the surface by using a fixing screw, and mechanically polishing by using SiC water sand paper and absolute ethyl alcohol polishing solution.
S4, mechanical polishing: the mechanically ground sample was mechanically polished using a fine-yarn lint and absolute ethanol polishing solution.
S5, electrolytic polishing: and performing electrolytic polishing on the mechanically polished sample, wherein the polishing solution is a mixed solution of perchloric acid and absolute ethyl alcohol.
S6, drying and storing: covering the detection surface of the electropolished sample by using an anti-oxidation adhesive tape, and placing the sample in a sample box filled with a drying agent for standby.
Preferably, the sanding clamping tool in step S1 is made as follows:
(1) manufacturing a steel base with the diameter of 12-20 mm and the height of 8-12 mm;
(2) cutting a groove with the width of 8-12 mm and the depth of 3-5 mm in the middle of the base;
(3) drilling a screw hole with the diameter of 1-3 mm in the middle of the outer wall of one side of the groove, and matching with a fixing screw with a proper size;
(4) and grinding and polishing the surface.
Preferably, in step S3, the SiC sandpaper of 1000#, 2000#, and 5000# is used in sequence to perform the sanding treatment in an absolute ethanol environment.
Preferably, the steel ingot is a cuboid steel ingot, the length of the steel ingot is smaller than the diameter of the base, the width of the steel ingot is smaller than the width of the groove, and the height of the steel ingot is smaller than the depth of the groove.
Preferably, in step S5, the volume ratio of perchloric acid to ethanol is 1: 8-10.
Preferably, in step S5, the electropolishing is performed at a current of 0.2-1.5A, a voltage of 15-22V and a time of 30-70S.
The purpose of electrolytic polishing is to remove an oxide layer on the surface of a sample, and incomplete removal or excessive degradation can be caused by improper selection of parameters such as current density, voltage, time and the like, so that the definition of the final pattern of the sample is influenced.
The test surface is covered by the anti-oxidation glue after EBSD detection, so that the storage time of the test surface can be prolonged, the test surface can be tested repeatedly, the condition that the test surface of the sample is corroded when the subsequent supplementary test is needed is avoided, and the maximum utilization of the sample is ensured.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. the preparation method of the EBSD sample of the high-purity aluminum by the segregation method can conveniently and quickly obtain the sample test surface of the high-purity aluminum foil by the segregation method, which meets the EBSD analysis requirements, provides convenience for obtaining the crystal orientation information of the high-purity aluminum foil by the segregation method, such as single crystal orientation, texture occupancy rate, orientation difference distribution and the like, and lays a foundation for the correlation research of the texture evolution and the deformation of the high-purity aluminum foil by the segregation method.
2. The clamping tool manufactured by the invention can assist in polishing, does not adopt an organic solvent, has simple experimental process and reduced influence factors, and can be repeatedly used, so that the experimental effect is improved, the experimental time is greatly shortened, and the experimental cost is greatly reduced.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a front view of a clamping tool;
FIG. 2 is a side view of the clamping tool;
in the figure, 1-base; 2-a groove; 3-outer wall; 4-a set screw;
FIG. 3 is an orientation profile of EBSD analysis of the sample prepared in example 1;
FIG. 4 is an orientation profile of EBSD analysis of the sample prepared in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A sample preparation method for EBSD analysis of a high-purity aluminum foil by a segregation method comprises the following steps:
s1, manufacturing a polishing clamping tool: cutting and sampling by using a wire to obtain a base 1 with the diameter of 15mm and the height of 10 mm; cutting a groove 2 with the width of 10mm and the depth of 4mm in the middle of the base 1; a screw hole with the diameter of 2mm is drilled in the right middle of the outer wall of one side of the groove 2, and a fixing screw 4 with proper size is matched; sampling by linear cutting to obtain a grinding and clamping tool with the size of 4mm multiplied by 6mm multiplied by 9mm, and grinding and flattening the surface of the grinding and clamping tool.
S2, mechanical sampling: a high-purity aluminum foil of segregation method with a thickness of 0.133mm and a thickness of 22mm 8mm was sampled by wire cutting, and the most flat surface (size 9mm 4mm) was selected as a ground surface by winding it on a steel ingot. The steel ingot is 12mm in length, 6mm in width and 3mm in depth.
S3, mechanical polishing: and placing the steel ingot in the groove 2 of the clamping tool, selecting the smoothest surface as a grinding surface to be upward, fixing the steel ingot by using a fixing screw 4, and mechanically grinding the steel ingot by using SiC water sand paper and absolute ethyl alcohol polishing solution.
Sequentially using 1000#, 2000#, 5000# SiC waterproof abrasive paper to perform hand grinding in an absolute ethyl alcohol environment, rotating the sample by a certain angle after sand change until scratches of the previous procedure are completely ground off, and the new scratch directions are consistent; the hand abrasion force is moderate, deep scratches are easily left on the surface of the aluminum when the force is too large, and the original scratches are not easily abraded when the force is too small.
S4, mechanical polishing: the method is carried out on a polishing machine padded with fine velvet cloth, and a sample after hand grinding is placed at a position close to the center of the polishing machine so as to prevent the polishing speed from generating new scratches on the surface of the aluminum foil too fast; during polishing, absolute ethyl alcohol polishing solution is required to be continuously sprayed on the sample, so that the polishing surface is kept wet; after polishing, the surface of the sample looks bright and has no visible scratches;
s5, electrolytic polishing: turning on a power supply of the polishing machine, adjusting the voltage to 20V, clamping the mechanically polished sample by using tweezers, and connecting the positive electrode of the polishing machine with the tweezers; placing a beaker filled with polishing solution (the proportion of perchloric acid to absolute ethyl alcohol is 1: 9) on a magnetic stirring instrument, placing a rotor, preparing an iron sheet with proper size, bending the iron sheet into an L shape, immersing one end of the iron sheet into the polishing solution, connecting the other end of the iron sheet with the negative electrode of a polishing machine, adjusting the speed of the rotor, immersing the surface of a sample into the polishing solution for electrolytic polishing, and after about 50s, washing the sample with alcohol and then drying the surface by using a blower; inspecting the polishing quality of the surface of the sample by using a metallographic microscope;
s6, EBSD analysis: placing a sample to be tested in an electron microscope, and obtaining a chrysanthemum pool pattern by using an EBSD analysis system;
s7, drying and storing: after the detection is finished, taking down the steel ingot coated with the aluminum foil sample, covering the detection surface with an anti-oxidation adhesive tape, and placing the steel ingot in a sample box filled with a drying agent;
in this example, the orientation distribution diagram of the electronic aluminum foil for the electrolytic capacitor in EBSD analysis is shown in fig. 3, and the calibration rate of the sample reaches 94%, which is good and short in experimental time.
Example 2
A sample preparation method for EBSD analysis of a high-purity aluminum foil by a segregation method comprises the following steps:
s1, manufacturing a clamping tool: cutting and sampling by using a wire to obtain a base 1 with the diameter of 15mm and the height of 10 mm; cutting a groove 2 with the width of 10mm and the depth of 4mm in the middle of the base 1; a screw hole with the diameter of 2mm is drilled in the right middle of the outer wall of one side of the groove 2, and a fixing screw 4 with proper size is matched; a sample was taken by wire cutting to obtain a holding tool having a size of 4mm X6 mm X9 mm, and the surface thereof was polished flat.
S2, mechanical sampling: a high-purity aluminum foil of 21mm x 7mm thickness by segregation method was sampled by wire cutting and wound around a steel ingot, and the most flat surface (6 mm x 4mm in size) was selected as a ground surface. The steel ingot is 12mm in length, 6mm in width and 3mm in depth.
S3, mechanical polishing: and placing the steel ingot in the groove 2 of the clamping tool, selecting the smoothest surface as a grinding surface to be upward, fixing the steel ingot by using a fixing screw 4, and mechanically grinding the steel ingot by using SiC water sand paper and absolute ethyl alcohol polishing solution.
Sequentially using 1000#, 2000#, 5000# SiC waterproof abrasive paper to perform hand grinding in an absolute ethyl alcohol environment, rotating the sample by a certain angle after sand change until scratches of the previous procedure are completely ground off, and the new scratch directions are consistent; the hand abrasion force is moderate, deep scratches are easily left on the surface of the aluminum when the force is too large, and the original scratches are not easily abraded when the force is too small.
S4, mechanical polishing: the method is carried out on a polishing machine padded with fine velvet cloth, and a sample after hand grinding is placed at a position close to the center of the polishing machine so as to prevent the polishing speed from generating new scratches on the surface of the aluminum foil too fast; during polishing, absolute ethyl alcohol polishing solution is required to be continuously sprayed on the sample, so that the polishing surface is kept wet; after polishing, the surface of the sample looks bright and has no visible scratches;
s5, electrolytic polishing: turning on a power supply of the polishing machine, adjusting the voltage to 18V, clamping the mechanically polished sample by using tweezers, and connecting the positive electrode of the polishing machine with the tweezers; placing a beaker filled with polishing solution (the proportion of perchloric acid to absolute ethyl alcohol is 1: 9) on a magnetic stirring instrument, placing a rotor, preparing an iron sheet with proper size, bending the iron sheet into an L shape, immersing one end of the iron sheet into the polishing solution, connecting the other end of the iron sheet with the negative electrode of a polishing machine, adjusting the speed of the rotor, immersing the surface of a sample into the polishing solution for electrolytic polishing, and after about 60s, washing the sample with alcohol and then drying the surface by using a blower; inspecting the polishing quality of the surface of the sample by using a metallographic microscope;
s6, EBSD analysis: placing a sample to be tested in an electron microscope, and obtaining a chrysanthemum pool pattern by using an EBSD analysis system;
s7, drying and storing: after the detection is finished, taking down the steel ingot coated with the aluminum foil sample, covering the detection surface with an anti-oxidation adhesive tape, and placing the steel ingot in a sample box filled with a drying agent;
in this example, the EBSD analysis of the orientation distribution diagram of the electronic aluminum foil for electrolytic capacitors is shown in fig. 4, and the calibration rate of the sample reaches 94%, which is highly effective and requires a short experimental time.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.
Claims (6)
1. A preparation method of a segregation method high-purity aluminum EBSD sample is characterized by comprising the following steps:
s1, manufacturing a polishing clamping tool: the base comprises a cylinder, a groove is formed in the top of the base, a screw hole is formed in the outer wall of one side of the groove, and a fixing screw penetrates through the screw hole;
s2, mechanical sampling: cutting the sample by a wire;
s3, mechanical polishing: winding a sample on a steel ingot, placing the steel ingot in the groove of the clamping tool, fixing the steel ingot by using a fixing screw, and mechanically grinding by using SiC waterproof abrasive paper and absolute ethyl alcohol polishing solution;
s4, mechanical polishing: mechanically polishing the mechanically polished sample by using a fine velvet cloth and absolute ethyl alcohol polishing solution;
s5, electrolytic polishing: performing electrolytic polishing on the mechanically polished sample, wherein the polishing solution is a mixed solution of perchloric acid and absolute ethyl alcohol;
s6, drying and storing: covering the detection surface of the electropolished sample by using an anti-oxidation adhesive tape, and placing the sample in a sample box filled with a drying agent for standby.
2. The method of preparing the segregation process high purity aluminum EBSD sample of claim 1 wherein the grinding fixture of step S1 is made as follows:
(1) manufacturing a base with the diameter of 12-20 mm and the height of 8-12: mm;
(2) cutting a groove with the width of 8-12 mm and the depth of 3-5 mm in the middle of the base;
(3) drilling a screw hole with the diameter of 1-3 mm in the middle of the outer wall of one side of the groove, and matching with a fixing screw with a proper size;
(4) and grinding and polishing the surface.
3. The method for preparing the segregation-based high-purity aluminum EBSD sample according to claim 1, wherein in step S3, SiC water sand paper of 1000#, 2000#, and 5000# is used in sequence to perform grinding treatment in an absolute ethanol environment.
4. The method for preparing the segregation-process high-purity aluminum EBSD sample according to the claim 1, wherein in the step S3, the steel ingot is a cuboid steel ingot, the length of the steel ingot is smaller than the diameter of the base, the width of the steel ingot is smaller than the width of the groove, and the height of the steel ingot is smaller than the depth of the groove.
5. The method for preparing the segregation-based high-purity aluminum EBSD sample according to claim 1, wherein in the step S5, the volume ratio of perchloric acid to ethanol is 1: 8-10.
6. The method for preparing the segregation-based high-purity aluminum EBSD sample according to claim 1, wherein in step S5, the electropolishing is carried out at a current of 0.2-1.5A, a voltage of 15-22V and a time of 30-70S.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116558932A (en) * | 2023-07-07 | 2023-08-08 | 北京科技大学 | Method for preparing small-size sample by using large-size hot-inlaid machine |
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| KR20080111573A (en) * | 2007-06-19 | 2008-12-24 | 현대자동차주식회사 | Manufacturing method of specimen for transmission electron microscopy |
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