CN116718621A - Preparation method of free-machining-state EBSD sample of aluminum alloy - Google Patents
Preparation method of free-machining-state EBSD sample of aluminum alloy Download PDFInfo
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- 238000001887 electron backscatter diffraction Methods 0.000 title claims abstract description 46
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000005498 polishing Methods 0.000 claims abstract description 271
- 238000000227 grinding Methods 0.000 claims abstract description 82
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000012545 processing Methods 0.000 claims abstract description 10
- 238000003754 machining Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 55
- 229910003460 diamond Inorganic materials 0.000 claims description 32
- 239000010432 diamond Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 244000137852 Petrea volubilis Species 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 238000011068 loading method Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 229920001342 Bakelite® Polymers 0.000 claims description 5
- 239000004637 bakelite Substances 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- 239000004033 plastic Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 65
- 235000019441 ethanol Nutrition 0.000 description 16
- 239000003792 electrolyte Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 9
- 238000005868 electrolysis reaction Methods 0.000 description 7
- 238000007517 polishing process Methods 0.000 description 7
- 229910001369 Brass Inorganic materials 0.000 description 6
- 239000010951 brass Substances 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000010884 ion-beam technique Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005201 scrubbing Methods 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- KFSUNTUMPUWCMW-UHFFFAOYSA-N ethanol;perchloric acid Chemical compound CCO.OCl(=O)(=O)=O KFSUNTUMPUWCMW-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 235000007516 Chrysanthemum Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005315 distribution function Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000013100 final test Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000002699 waste material Substances 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
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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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
- G01N1/34—Purifying; Cleaning
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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
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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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Abstract
The invention discloses a preparation method of an aluminum alloy free machining state EBSD sample, which comprises the following steps: (1) sawing the sample using a abrasive cutoff saw; (2) Mechanically grinding and polishing the cut sample by using an automatic grinding and polishing machine; (3) Electropolishing the sample with perchloric acid alcohol having a volume concentration of 6% -12%; (4) Finally, ultrasonic alcohol is used for cleaning, so that the EBSD sample suitable for the free processing state aluminum alloy is prepared. The EBSD sample prepared by the technical scheme of the invention can remove the plastic deformation layer formed on the surface of the aluminum alloy sample by mechanical polishing, so that a flat glossy surface is obtained, and lattice distortion of the sample surface can not be caused.
Description
Technical Field
The invention relates to the technical field of aluminum alloy surface treatment, in particular to a preparation method of an aluminum alloy free processing EBSD sample.
Background
English in electron back scattering diffraction, abbreviated as EBSD, is a powerful analytical tool for rapid and accurate crystal orientation measurement and correlation identification. Since it is based on scanning electron microscopy, so that microstructures (such as grains, phases, interfaces, deformations, etc.) can be related to crystallographic relationships, it has been widely used to analyze microstructures and textures, to obtain crystallographic orientation maps, polar maps and inverse polar maps, and to calculate Orientation Distribution Functions (ODFs). And the angular resolution and the spatial resolution of the EBSD technology can reach 0.5 DEG and 0.1 mu m respectively, the precision is quite high compared with other technologies at present, the full automation of the acquisition of the orientation information of the micro-area can be realized, the acquisition speed is relatively high, and the EBSD technology has been developed into a standard technology on the basis of the analysis means of the current crystal orientation and the microstructure of an analysis material.
The EBSD analysis not only needs to have very deep crystallographic preparation, but also needs to be tilted by 70 degrees during the sample analysis, the preparation requirement on the sample is high, the uneven or inclined surface of the sample can cause the area with a slightly higher surface to obviously block the lower area, the sample preparation is not good, the clear chrysanthemum pond pattern cannot be acquired, and the measurement and analysis of the crystal structure and the orientation are not from the beginning. Particularly, very soft or easily oxidized samples of aluminum, magnesium, lead, gold, etc., are difficult to prepare. The current common EBSD sample preparation method comprises ion beam polishing, vibration polishing and electrolytic polishing. The ion beam polishing requires a special ion beam polishing instrument, has low price and low popularization, has small polishing area, is only in a micron-sized range, has high consumable materials in the use process, and is not suitable for mass production; vibration polishing belongs to the mechanical polishing range, can reduce residual stress on the surface of a sample, but aluminum alloy is softer, tiny scratches on the surface of the sample are difficult to polish and remove, and the analysis effect of EBSD is affected.
Disclosure of Invention
The invention can solve the problems of EBSD automatic polishing parameters, electrolytic polishing solution proportion and electrolytic polishing parameters for free processing aluminum alloy, thereby preparing the EBSD sample meeting the requirements.
The specific technical scheme adopted by the invention is as follows:
the preparation method of the free-machining EBSD sample of the aluminum alloy is characterized by comprising the following steps of:
(1) Cutting by using a grinding wheel: cutting a sample by using a grinding wheel, and sawing the sample into square blocks;
(2) Mechanical grinding and polishing: the polishing machine using the center force loading mode is used for mechanically grinding and polishing the square block, and the working procedures of mechanical grinding and polishing comprise: grinding with sand paper, coarse polishing with a diamond grinding and polishing disc, coarse polishing with a coarse flannelette disc, coarse polishing with a fine flannelette disc, fine polishing with a fine flannelette disc, and fine polishing with a water-based grinding and polishing disc to obtain a mechanically polished sample;
(3) Electrolytic polishing: carrying out electrolytic polishing on the mechanically polished sample in a perchloric acid alcohol solution with the volume concentration of 6-12% to obtain an electropolished sample; the perchloric acid with lower concentration not only can ensure the electrolytic polishing effect, but also can reduce the waste of medicines and ensure the safety of the solution;
(4) Ultrasonic cleaning: and (3) ultrasonically cleaning the sample subjected to electrolytic polishing in an ultrasonic cleaning instrument for 10min to obtain a finished product.
Preferably, in the step (1), siC sand sheets bonded by bakelite with the hardness of 30-400HV are selected for sawing, and the hardness is suitable for aluminum alloy, so that the flatness of the pattern can be ensured to the greatest extent.
Preferably, in step (1), the pattern is sawed into rectangular dice of 20mm by 25 mm.
Preferably, in the step (2), the polishing machine is an automatic polishing machine, and specific process parameters of mechanical polishing and polishing are as follows:
the first procedure: grinding the sand paper: acting force: 150N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; sand paper: 220#; polishing solution: water; time: 2min;
and a second procedure: coarse polishing of a diamond polishing disc: acting force: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: diamond grinding and polishing disc; polishing solution: 9 mu m diamond polishing solution; time: 3min;
and a third procedure: coarse polishing of the coarse cotton flannel plate: acting force: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fleece cloth; polishing solution: 3 mu m diamond polishing solution; time: 2min;
and a fourth procedure: coarse polishing of the fine flannelette plate: acting force: 100N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
and a fourth procedure: fine flannelette plate fine polishing: acting force: 120N; rotational speed: polishing disc, 140rpm; a clamp at 140rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
fifth procedure: fine polishing of a water-based polishing disc: acting force: 90N; rotational speed: polishing disk, 120rpm; a clamp, 120rpm; grinding and polishing disc: a water-based grinding and polishing disc; polishing solution: 0.04 μm silica suspension; time: 1.5min. In the automatic polishing process, proper pressure, polishing time, rotating speed and rotating direction of the turntable relative to the grinding head are selected in each polishing procedure, and a center force loading mode is adopted for polishing, so that the optimal polishing effect is obtained, and the stable polishing effect is ensured.
Preferably, in the step (3), the mechanically polished sample is used as an anode, and the stainless steel plate is used as a cathode; during electrolytic polishing, the anode sample keeps shaking continuously, so that the flow of electrolyte is promoted, the enough ion diffusion in a polishing area is ensured, and the polishing uniformity is ensured.
Preferably, in the step (3), the voltage is 20-25V, the current is 0.1A-0.2A, and the electrolytic polishing temperature is room temperature; the electrolytic polishing time is 10-30s.
Preferably, in the step (4), the cleaning solution used for cleaning the instrument is absolute ethyl alcohol, and perchloric acid and other impurities on the surface of the sample after electrolytic polishing are cleaned.
The invention relates to a preparation method of an aluminum alloy free processing state EBSD sample, which is characterized by comprising the following design principle:
according to the preparation method, the EBSD sample of the free processing state aluminum alloy is prepared, and the sample is not subjected to subsequent solid solution and heat treatment, so that larger residual stress and a large amount of undissolved second phases exist in the sample, the dislocation density is higher, the subgrain size is small, the preparation of the EBSD sample is not easy, and the EBSD sample meeting the requirements can be obtained through successful implementation of the preparation method, so that the subsequent analysis work is facilitated;
the invention relates to a method for standardizing and optimizing the flow of EBSD sample preparation, in particular to improvement of mechanical grinding and polishing process and electrolytic polishing process;
in the mechanical grinding and polishing process, the prior art adopts a single-point loading mode, and the single-point loading has the advantages that the number of samples is free and flexible, the samples can be taken and placed conveniently only within the maximum hole number, and the method is particularly suitable for the periodic observation effect in the later stage of grinding and polishing. The disadvantage is that the sample has autorotation and small-range movement in the clamp holder, the autorotation strictly controls the grinding track of the sample, and the small-range movement easily causes fillets; the center loading has the advantages that the sample is locked on the clamp holder, so that the grinding track of the sample can be accurately controlled, the reproducibility of sample preparation is improved, particularly for the rough grinding and fine grinding stages, the grinding rate is high, the grinding effect of the sample is controlled, and in addition, due to the center loading, the grinding effect of the samples with different materials is the same;
in the electrolytic polishing process, the electrolyte is a low-concentration perchloric acid ethanol solution, perchloric acid belongs to a high-resistance polishing solution, and the concentration of perchloric acid can be reduced by adding organic ethanol, so that the use safety is ensured, and a complex with high viscosity and high resistance can be generated with aluminum alloy to generate polarization effect, so that the polishing effect is good; the volume concentration of the perchloric acid in the electrolyte is 6-12%, and the balance is ethanol; pouring the prepared electrolyte into a beaker, and putting an L-shaped stainless steel plate with the specification of 20mm multiplied by 30mm into the electrolyte as a cathode, specifically, keeping the area ratio of the cathode to the anode at (1-1.5): 1, and ensuring that the anode sample is parallel to the cathode during electrolysis; the electrolytic polishing is carried out at room temperature, the voltage is 20V-25V, the current is 0.1A-0.2A, the time is 10S-20S, the anode sample is continuously rocked during the electrolytic polishing, the flow of electrolyte is promoted, the sufficient ion diffusion in a polishing area is ensured, and the polishing uniformity is ensured;
the sample prepared by the invention strictly prescribes the specific operation of each working procedure from sawing to electropolishing, has small adjustable range of parameters, and can ensure that the CI (confidence factor) value of the final test result of the sample is more than 0.1.
Compared with the prior art, the invention has the advantages and positive effects that:
1. the invention further optimizes the specific process of mechanical polishing, selects proper pressure, polishing time, rotating speed and rotating direction of the turntable relative to the grinding head in each working procedure of mechanical polishing, and adopts a center force loading mode to grind and polish, so that a sample can be locked on the clamp holder, the grinding and polishing track of the sample can be accurately controlled, and the reproducibility of sample preparation is improved.
2. The electrolyte solution selected by the invention is a low-concentration perchloric acid ethanol solution with the volume concentration of 6-12%, perchloric acid belongs to a high-resistance polishing solution, and the addition of ethanol can reduce the perchloric acid concentration, ensure the use safety, and can generate a high-viscosity and high-resistance complex with aluminum alloy to generate polarization effect, so that the method is suitable for the electrolytic polishing process of the aluminum alloy; the electrolytic polishing process disclosed by the invention also has the advantages of short polishing time, high polishing efficiency and capability of being carried out at room temperature.
3. The surface of the aluminum alloy EBSD sample subjected to electrolytic polishing is bright and smooth, and no grinding mark is generated in the machining process; the EBSD sample prepared by the method can remove the plastic deformation layer formed on the surface of the aluminum alloy sample by mechanical polishing, so that a flat and glossy surface is obtained, lattice distortion on the surface of the sample is not caused, and a good sample is provided for EBSD analysis.
4. Aiming at the problems that the free processing state aluminum alloy is not subjected to subsequent solid solution and heat treatment, the aluminum alloy is high in dislocation density and fine in subgrain size due to larger residual stress and a large amount of undissolved second phases, and the preparation of an EBSD sample is not easy, the invention provides an EBSD sample preparation process, which can effectively solve the influence of the problems on an EBSD test result, simultaneously meets the requirements of the EBSD sample, and is convenient for subsequent analysis work.
5. The invention improves the sample preparation efficiency and quality of various thermally processed aluminum alloy electron back scattering samples, optimizes the EBSD sample preparation flow, greatly improves the EBSD sample preparation effect, and prepares samples with the final EBSD test result CI (confidence factor) value more than 0.1.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort to a person skilled in the art.
FIG. 1 is a hot rolled counter electrode view of 7055 aluminum alloy in the free as-machined state;
FIG. 2 is a diagram of a free working 7050 aluminum alloy forging counter electrode;
fig. 3 is a free working 6082 aluminum alloy extrusion counter electrode diagram.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1, as shown in fig. 1:
EBSD sample preparation of 7055 aluminum alloy without heat treatment after hot rolling:
the preparation method of the free processing state EBSD sample of the aluminum alloy comprises the following steps:
step (1): sawing a sample: cutting the sample into rectangular blocks of 20mm x 25mm by using a abrasive wheel dicing saw equipped with a bakelite bonded SiC abrasive wheel, wherein the hardness of the abrasive wheel is 400HV;
step (2): mechanical polishing and grinding: the method comprises the following specific procedures of mechanically grinding and polishing the square block by using an automatic grinding and polishing machine loaded by central force:
the first procedure: grinding the sand paper: acting force: 150N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; sand paper: 220#; polishing solution: water; time: 2min;
and a second procedure: coarse polishing of a diamond polishing disc: acting force: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: diamond grinding and polishing disc; polishing solution: 9 mu m diamond polishing solution; time: 3min;
and a third procedure: coarse polishing force of coarse flannelette plate: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fleece cloth; polishing solution: 3 mu m diamond polishing solution; time: 2min;
and a fourth procedure: coarse polishing force of fine flannelette disc: 100N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
and a fourth procedure: fine flannelette plate fine polishing: acting force: 120N; rotational speed: polishing disc, 140rpm; a clamp at 140rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
fifth procedure: fine polishing of a water-based polishing disc: acting force: 90N; rotational speed: polishing disk, 120rpm; a clamp, 120rpm; grinding and polishing disc: a water-based grinding and polishing disc; polishing solution: 0.04 μm silica suspension; time: 1.5min;
step (3): electrolytic polishing:
the electrolytic polishing solution is 8% perchloric acid alcohol solution, the voltage is 20V, the current is 0.1A, the polishing time is 10S, and the temperature is room temperature; a brass clip is selected to clamp a sample, the sample is used as an anode, a stainless steel plate is used as a cathode, and a 20mm multiplied by 30mm L-shaped cathode plate is used to ensure that the anode sample is parallel to the cathode during electrolysis;
the clamp is at a certain distance from the electrolyte during electrolysis, so that the brass clamp is prevented from contacting the electrolyte; continuously shaking the anode sample during electrolytic polishing to promote the flow of electrolyte, ensuring enough ion diffusion in a polishing area, ensuring uniform polishing, flushing the surface of the sample with a large amount of clean water immediately after the electrolytic polishing is finished, cleaning with alcohol, and finally scrubbing the surface of the sample with 5% nitric alcohol;
step (4): ultrasonic cleaning: after the polishing is finished, ultrasonically cleaning the sample with alcohol for 10min, removing the residual electrolytic polishing solution on the surface of the sample, and avoiding secondary corrosion of the residual electrolytic polishing solution on the sample.
Through EBSD test, the CI (confidence factor) value of the test result is 0.18, and the CI value is larger than 0.1, and the data of the test result can be considered to be credible.
Example 2, as shown in fig. 2:
EBSD sample preparation of forged 7050 aluminum alloy subjected to first and second heat deformation:
the preparation method of the free processing state EBSD sample of the aluminum alloy comprises the following steps:
step (1): sawing a sample: cutting the sample into rectangular blocks of 20mm x 25mm by using a abrasive wheel dicing saw equipped with a bakelite bonded SiC abrasive wheel, wherein the hardness of the abrasive wheel is 30HV;
step (2): mechanical polishing and grinding: the method comprises the following specific procedures of mechanically grinding and polishing the square block by using an automatic grinding and polishing machine loaded by central force:
the first procedure: grinding the sand paper: acting force: 150N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; sand paper: 220#; polishing solution: water; time: 2min;
and a second procedure: coarse polishing of a diamond polishing disc: acting force: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: diamond grinding and polishing disc; polishing solution: 9 mu m diamond polishing solution; time: 3min;
and a third procedure: coarse polishing of the coarse cotton flannel plate: acting force: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fleece cloth; polishing solution: 3 mu m diamond polishing solution; time: 2min;
and a fourth procedure: coarse polishing of the fine flannelette plate: acting force: 100N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
and a fourth procedure: fine flannelette plate fine polishing: acting force: 120N; rotational speed: polishing disc, 140rpm; a clamp at 140rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
fifth procedure: fine polishing of a water-based polishing disc: acting force: 90N; rotational speed: polishing disk, 120rpm; a clamp, 120rpm; grinding and polishing disc: a water-based grinding and polishing disc; polishing solution: 0.04 μm silica suspension; time: 1.5min;
step (3): electrolytic polishing:
the electrolytic polishing solution is 10% perchloric acid alcohol solution, the voltage is 20V, the current is 0.2A, the polishing time is 15S, and the temperature is room temperature; a brass clip is selected to clamp a sample, the sample is used as an anode, a stainless steel plate is used as a cathode, and a 20mm multiplied by 30mm L-shaped cathode plate is used to ensure that the anode sample is parallel to the cathode during electrolysis;
the clamp is at a certain distance from the electrolyte during electrolysis, so that the brass clamp is prevented from contacting the electrolyte; continuously shaking the anode sample during electrolytic polishing to promote the flow of electrolyte, ensuring enough ion diffusion in a polishing area, ensuring uniform polishing, flushing the surface of the sample with a large amount of clean water immediately after the electrolytic polishing is finished, cleaning with alcohol, and finally scrubbing the surface of the sample with 5% nitric alcohol;
step (4): ultrasonic cleaning: after the polishing is finished, ultrasonically cleaning the sample with alcohol for 10min, removing the residual electrolytic polishing solution on the surface of the sample, and avoiding secondary corrosion of the residual electrolytic polishing solution on the sample.
Through EBSD test, the CI (confidence factor) value of the test result is 0.16, and the CI value is larger than 0.1, and the data of the test result can be considered to be credible.
Example 3, as shown in fig. 3:
preparation of EBSD samples of extruded 6082 aluminum alloy without solid solution after extrusion:
the preparation method of the free processing state EBSD sample of the aluminum alloy comprises the following steps:
step (1): sawing a sample: cutting the sample into rectangular blocks of 20mm x 25mm by using a abrasive wheel dicing saw equipped with a bakelite bonded SiC abrasive wheel, wherein the hardness of the abrasive wheel is 400HV;
step (2): mechanical polishing and grinding: the method comprises the following specific procedures of mechanically grinding and polishing the square block by using an automatic grinding and polishing machine loaded by central force:
the first procedure: grinding the sand paper: acting force: 150N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; sand paper: 220#; polishing solution: water; time: 2min;
and a second procedure: coarse polishing of a diamond polishing disc: acting force: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: diamond grinding and polishing disc; polishing solution: 9 mu m diamond polishing solution; time: 3min;
and a third procedure: coarse polishing force of coarse flannelette plate: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fleece cloth; polishing solution: 3 mu m diamond polishing solution; time: 2min;
and a fourth procedure: coarse polishing force of fine flannelette disc: 100N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
and a fourth procedure: fine flannelette plate fine polishing: acting force: 120N; rotational speed: polishing disc, 140rpm; a clamp at 140rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
fifth procedure: fine polishing of a water-based polishing disc: acting force: 90N; rotational speed: polishing disk, 120rpm; a clamp, 120rpm; grinding and polishing disc: a water-based grinding and polishing disc; polishing solution: 0.04 μm silica suspension; time: 1.5min;
step (3): electrolytic polishing:
the electrolytic polishing solution is 6% perchloric acid alcohol solution, the voltage is 25V, the current is 0.1A, the polishing time is 10S, and the temperature is room temperature; a brass clip is selected to clamp a sample, the sample is used as an anode, a stainless steel plate is used as a cathode, and a 20mm multiplied by 30mm L-shaped cathode plate is used to ensure that the anode sample is parallel to the cathode during electrolysis;
the clamp is at a certain distance from the electrolyte during electrolysis, so that the brass clamp is prevented from contacting the electrolyte; continuously shaking the anode sample during electrolytic polishing to promote the flow of electrolyte, ensuring enough ion diffusion in a polishing area, ensuring uniform polishing, flushing the surface of the sample with a large amount of clean water immediately after the electrolytic polishing is finished, cleaning with alcohol, and finally scrubbing the surface of the sample with 5% nitric alcohol;
step (4): ultrasonic cleaning: after the polishing is finished, ultrasonically cleaning the sample with alcohol for 10min, removing the residual electrolytic polishing solution on the surface of the sample, and avoiding secondary corrosion of the residual electrolytic polishing solution on the sample.
Through EBSD test, the CI (confidence factor) value of the test result is 0.19, and the CI value is larger than 0.1, and the data of the test result can be considered to be credible.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. The preparation method of the free-machining EBSD sample of the aluminum alloy is characterized by comprising the following steps of:
(1) Cutting by using a grinding wheel: cutting a sample by using a grinding wheel, and sawing the sample into square blocks;
(2) Mechanical grinding and polishing: the polishing machine using the center force loading mode is used for mechanically grinding and polishing the square block, and the working procedures of mechanical grinding and polishing comprise: grinding with sand paper, coarse polishing with a diamond grinding and polishing disc, coarse polishing with a coarse flannelette disc, coarse polishing with a fine flannelette disc, fine polishing with a fine flannelette disc, and fine polishing with a water-based grinding and polishing disc to obtain a mechanically polished sample;
(3) Electrolytic polishing: carrying out electrolytic polishing on the mechanically polished sample in a perchloric acid alcohol solution with the volume concentration of 6-12% to obtain an electropolished sample;
(4) Ultrasonic cleaning: and (3) ultrasonically cleaning the sample subjected to electrolytic polishing in an ultrasonic cleaning instrument for 10min to obtain a finished product.
2. The method for preparing an aluminum alloy free machining state EBSD sample according to claim 1, wherein in the step (1), a SiC grinding wheel with 30-400HV bakelite bonding is selected for sawing.
3. The method for preparing an EBSD sample of aluminum alloy in free machining state according to claim 1, wherein in step (1), the sample is sawed into rectangular dice of 20mm x 25 mm.
4. The method for preparing an EBSD sample in free processing of aluminum alloy according to claim 1, wherein in step (2), the polishing machine is an automatic polishing machine, and the specific process parameters of mechanical polishing and polishing are:
the first procedure: grinding the sand paper: acting force: 150N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; sand paper: 220#; polishing solution: water; time: 2min;
and a second procedure: coarse polishing of a diamond polishing disc: acting force: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: diamond grinding and polishing disc; polishing solution: 9 mu m diamond polishing solution; time: 3min;
and a third procedure: coarse polishing of the coarse cotton flannel plate: 120N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fleece cloth; polishing solution: 3 mu m diamond polishing solution; time: 2min;
and a fourth procedure: coarse polishing of the fine flannelette plate: acting force: 100N; rotational speed: polishing disk, 130rpm; a clamp, 130rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
and a fourth procedure: fine flannelette plate fine polishing: acting force: 120N; rotational speed: polishing disc, 140rpm; a clamp at 140rpm; grinding and polishing disc: a fine flannelette plate; polishing solution: 1 mu m diamond polishing solution; time: 2min;
fifth procedure: fine polishing of a water-based polishing disc: acting force: 90N; rotational speed: polishing disk, 120rpm; a clamp, 120rpm; grinding and polishing disc: a water-based grinding and polishing disc; polishing solution: 0.04 μm silica suspension; time: 1.5min.
5. The method for preparing an aluminum alloy free machining state EBSD sample according to claim 1, wherein in the step (3), the sample after mechanical polishing is used as an anode, and a stainless steel plate is used as a cathode; during electrolytic polishing, the anode sample is kept continuously swaying.
6. The method for preparing an EBSD sample in free machining state of aluminum alloy according to claim 1, wherein in the step (3), the voltage is 20-25V, the current is 0.1-0.2A, and the electrolytic polishing temperature is room temperature; the electrolytic polishing time is 10-30s.
7. The method for preparing an EBSD sample of aluminum alloy in free machining state according to claim 1, wherein in step (4), the cleaning solution used for cleaning the instrument is absolute ethanol.
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