CN113358437A - Preparation method of copper-iron dual-phase alloy sample for EBSD analysis - Google Patents
Preparation method of copper-iron dual-phase alloy sample for EBSD analysis Download PDFInfo
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- RZJQYRCNDBMIAG-UHFFFAOYSA-N [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] Chemical class [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] RZJQYRCNDBMIAG-UHFFFAOYSA-N 0.000 claims description 4
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 27
- 239000010949 copper Substances 0.000 abstract description 12
- 239000011159 matrix material Substances 0.000 abstract description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 11
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- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
- B24B1/002—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes using electric current
-
- 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
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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
- G01N2001/2873—Cutting or cleaving
Abstract
The invention provides a preparation method of a sample for EBSD analysis of a copper-iron dual-phase alloy, which comprises the steps of carrying out wire cutting on the copper-iron dual-phase alloy to obtain a sample to be processed; grinding the sample to be treated, cleaning with ethanol, drying and demagnetizing to obtain a polished sample; performing argon ion polishing on the polished sample to obtain a copper-iron dual-phase alloy sample for EBSD analysis; wherein the vacuum degree in the argon ion polishing is controlled at 5 × 10‑3～9×10‑3pa, the argon ion polishing sequentially comprises a rough reduction stage and a fine modification stage, the voltage of the rough reduction stage is 5-7 kv, the time of the rough reduction stage is not less than 7h, the voltage of the fine modification stage is 2-4 kv, and the time of the fine modification stage is not less than 3 h. The method can simultaneously mark iron phase and copper matrix phase, and the prepared sample has a marking rate as high as 90%The above.
Description
Technical Field
The invention relates to the technical field of EBSD sample preparation, in particular to a preparation method of a sample for EBSD analysis of a copper-iron dual-phase alloy.
Background
In recent years, the research on the copper-iron alloy is more and more focused and the application range of the copper-iron alloy is wider due to the advantages of excellent electromagnetic shielding performance, higher strength and conductivity, low raw material cost and the like of the copper-iron alloy. High-strength and high-conductivity copper-iron materials are applied to electromagnetic shielding covers, electromagnetic shielding wires and wave-absorbing shielding coatings in the aerospace and military fields, railway contact networks, brakes, high-speed motors and the like in the traffic field, high-power heat dissipation plates, connectors, communication control wires and other high-end copper alloy products in the electrical and electronic field, and excellent material characteristics (the electrical conductivity is more than 50% IACS, the tensile strength is 400-650 MPa, and the electromagnetic shielding is more than 80dB in the frequency range of 1G-1.5 GHz) are shown in Japan and Korea. However, due to the technical secrecy, the industrial production of high-strength high-conductivity copper-iron materials with high iron content (more than or equal to 5 wt.%, and in this case, the duplex alloy) in China is still blank at present, and the bottleneck of the application of the high-strength high-conductivity copper-iron materials will restrict the development of China in the field of high-end equipment manufacturing and application. The industrial production of the copper-iron dual-phase alloy cannot be separated from corresponding basic research, and at present, the basic research on the copper-iron dual-phase alloy focuses on the aspects of second-phase strengthening and the like, which relate to SEM and TEM characterization and describe the influence of the type, volume fraction and the like of the second phase (particularly alpha-Fe phase) on strengthening and hardening. In addition, the crystal orientation also has a significant influence on the properties of the copper-iron dual-phase alloy, such as strength, hardness, electric conductivity, electromagnetic shielding and the like, and few researches on the crystal orientation of the copper-iron dual-phase alloy are related to the EBSD sample preparation difficulty of the copper-iron dual-phase alloy.
In the prior art, the crystal orientation is usually studied by the EBSD technique. EBSD technology, which is totally called Electron backscattering Diffraction (Electron Backscattered Diffraction, is an analysis technology of the orientation and crystal structure of Electron backscattering pattern crystal micro-areas assembled on SEM, and has been widely applied in the characterization of material micro-tissue structure and micro-texture, EBSD has the main characteristics of retaining the conventional characteristics of a scanning Electron microscope and simultaneously carrying out Diffraction with spatial resolution and submicron level, EBSD changes the conventional texture analysis method and forms a brand-new scientific field called microtexture, namely the microstructure and the crystallographic analysis are combined, EBSD technology can realize the full-automatic collection of micro-area orientation information, sample preparation is simpler, data collection speed is high (can reach about 36 ten thousand points/h or even faster), resolution is high (the spatial resolution and the angular resolution can reach 0.1m and 0.5m respectively), lays a foundation for the rapid quantitative statistical research of the microstructure and texture of materials, has become an effective analysis means in material research. Compared to SEM, EBSD has the function of analyzing crystal orientation information; compared with TEM, EBSD has the advantages of wide analysis area, high analysis speed and low cost. Currently, for traditional single-phase copper alloy, mechanical polishing, vibration polishing, chemical corrosion, electrolytic polishing and other methods can successfully prepare an EBSD sample.
However, the EBSD sample preparation method in the prior art for preparing the copper-iron dual-phase alloy sample has the following defects: for copper-iron dual-phase alloy (the iron content is higher than 5%), the traditional EBSD sample preparation methods cannot successfully prepare qualified EBSD samples, only can calibrate a copper matrix phase, but cannot calibrate an iron phase at the same time, and the prepared sample calibration rate is extremely low. Therefore, it is urgently needed to develop a preparation method of a sample for EBSD analysis of the copper-iron dual-phase alloy so as to solve the technical problems.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides the preparation method of the sample for the EBSD analysis of the copper-iron dual-phase alloy, the iron phase and the copper matrix phase can be calibrated simultaneously, and the calibration rate of the prepared sample is as high as 90-99%.
The invention adopts the following technical scheme:
a method of preparing a sample for EBSD analysis of a copper-iron dual phase alloy, the method comprising:
performing linear cutting on the copper-iron dual-phase alloy to obtain a sample to be processed;
grinding the sample to be treated, cleaning with ethanol, drying and demagnetizing to obtain a polished sample;
performing argon ion polishing on the polished sample, and obtaining a copper-iron dual-phase alloy sample for EBSD analysis; whereinThe vacuum degree in the argon ion polishing is controlled to be 5 multiplied by 10-3～9×10-3pa, the argon ion polishing sequentially comprises a rough reduction stage and a fine modification stage, the voltage of the rough reduction stage is 5-7 kv, the time of the rough reduction stage is not less than 7h, the voltage of the fine modification stage is 2-4 kv, and the time of the fine modification stage is not less than 3 h.
The invention carries out argon ion polishing on a polished sample, and the vacuum degree in the argon ion polishing is controlled to be 5 x 10-3～9×10-3pa, the argon ion polishing sequentially comprises a rough reduction stage and a fine modification stage, the voltage of the rough reduction stage is 5-7 kv, the time of the rough reduction stage is not less than 7h, the voltage of the fine modification stage is 2-4 kv, and the time of the fine modification stage is not less than 3 h. The argon ion polishing principle in the application is that argon is changed into argon ions under the action of an electric field, the argon ions bombard the surface of a sample, atoms on the surface of the sample are sputtered one by one, and the sample for the EBSD analysis of the copper-iron dual-phase alloy with no stress layer on the surface is obtained; the applicant finds through experiments that the sample preparation can be successfully carried out in the rough reduction stage and the fine modification stage, and the calibration rate is high, because after the argon ion polishing treatment is carried out on the surface of the metal material, the stress layer and the oxidation layer on the metal surface can be effectively removed by the high-speed argon ions.
In the above technical scheme, the vacuum degree is controlled at 5 × 10 during the argon ion polishing-3～9×10-3pa is because it is economically efficient and the degree of vacuum is less than 9X 10-3pa, the adverse effect of air interfering with the argon ions and possibly oxidizing the sample surface; if the vacuum degree is more than 5X 10-3pa, adverse effect of low experimental efficiency;
in the above technical solution, the reason why the argon ion polishing process is divided into the rough reduction stage and the fine modification stage for control is as follows: the rough shearing stage is mainly to cut off a layer of surface to improve the penetration depth of argon ions, the efficiency is high, but the surface is rough, and the voltage in the fine trimming stage is small, so that the rough part can be flattened. If the voltage of 5-7 kv is adopted all the time, the rough shearing voltage is high, the speed is high, but the adverse effect of rough surface of the sample is caused;
in the technical scheme, if the voltage in the rough reduction stage is less than 5kv, the penetration depth of argon ions is low, the efficiency is low, and if the voltage in the rough reduction stage is more than 7kv, the sample surface roughness is adversely affected, and if the time in the rough reduction stage is less than 7h, the calibration rate is extremely low;
in the technical scheme, if the voltage in the finishing stage is less than 2kv, the adverse effect that the surface of the sample cannot be effectively flattened exists, and if the voltage is more than 4kv, the adverse effect that the surface of the sample is rough exists; and the time of the fine modification stage cannot be less than 3h, otherwise, normal calibration cannot be carried out.
Preferably, in the above technical solution, the vacuum degree in the argon ion polishing is controlled at 6 × 10-3～8×10- 3pa, the voltage of the rough reduction stage is 5.5-6.5 kv, and the voltage of the fine modification stage is 2.5-3.5 kv. The argon ion polishing condition is a better parameter discovered by the applicant through experimental research, and the calibration rate of the sample prepared under the parameter is as high as more than 90%.
More preferably, in the above technical solution, the vacuum degree in the argon ion polishing is controlled at 7 × 10-3pa, the voltage of the rough reduction stage is 6kv, and the voltage of the fine modification stage is 3 kv. The argon ion polishing conditions are the best parameters found by the applicant through experimental research, and the calibration rate of the sample prepared under the parameters is as high as 100%.
Preferably, the angle formed by the argon ion beam and the polished sample surface is controlled to be 85-95 degrees. Experiments prove that the effect of vertically bombarding the surface of a sample by argon ions is good, and the experiment is specifically shown as follows: the bombardment angle of the argon ions is vertical to the surface of the sample, the penetration depth of the argon ions is high, and the permeation bombardment efficiency is high, so that the angle formed by the argon ion beam and the polished sample surface is controlled to be 85-95 degrees. In a specific embodiment of the present invention, the angle of the argon ion beam with the polished sample surface is 90 °.
Specifically, in the technical scheme, the argon ion polishing adopts an argon ion beam with the purity of more than 99.9%, and the flow rate of the argon ion beam is 0.1-0.15 sccm.
The reason why argon gas having a purity of > 99.9% is used is that when the purity is lower than this value, oxygen gas is permeated, which affects argon ions and causes a risk of surface oxidation of the sample.
The argon flow in the range is 0.1-0.15 sccm; when the flow is too small, the adverse effect that the surface of the sample cannot be effectively bombarded exists; the flow is too large, so that the adverse effect of argon waste is caused;
in a preferred embodiment of the present invention, in the grinding, SiC sandpaper of 400 mesh, 600 mesh, 1000 mesh and 1500 mesh is used in this order for multiple times of grinding; and between two adjacent times of grinding, washing the SiC sand paper and the sample to be treated by water, and rotating the sample to be treated by 90 degrees along the same direction.
The SiC sand paper with 400 meshes, 600 meshes, 1000 meshes and 1500 meshes is sequentially used for grinding for multiple times, so that the method has the advantages of effectively covering the previous grinding scratches and being high in efficiency;
in a specific embodiment of the present invention, in the grinding, SiC sandpaper of 400 mesh, 600 mesh, 1000 mesh and 1500 mesh is used in this order for multiple times of grinding; and between two adjacent times of grinding, washing the SiC sand paper and the sample to be treated by water, and rotating the sample to be treated by 90 degrees along the same direction. In this embodiment, the abrasive paper and the sample are washed with tap water in the grinding process, and the sample is cleaned when the next piece of abrasive paper is changed, so that the sand grains with thicker upper lines can be brought to the fine abrasive paper, the original grinding direction is changed by 90 degrees, and the scratch left by the previous piece of abrasive paper is ground.
In the embodiment of the invention, because the copper matrix phase in the copper-iron dual-phase alloy is soft, uniform force is required during grinding, the force cannot be too heavy, the grain sizes of two kinds of sand paper used in a cutting and marking sequence cannot be greatly different, and if the grain sizes are too large, subsequent grinding cannot effectively remove the scratches of the previous grinding.
In a specific embodiment of the invention, the grinding time is 2-5 min for 400-mesh, 600-mesh, 1000-mesh and 1500-mesh SiC sandpaper. Other milling times may also be used in other embodiments.
In a preferred embodiment of the invention, the length of the sample to be treated is less than or equal to 4mm, the width is less than or equal to 4mm, and the thickness is less than or equal to 2 mm. This is done to form a sample that is easy to hold and to facilitate subsequent placement on a sample stage within the ion bombardment apparatus, and therefore it is desirable to ensure that the length and width of the sample is no greater than 4mm and the thickness is no greater than 2 mm.
In a preferred embodiment of the present invention, the argon ion polishing temperature is room temperature (20-30 ℃), and can also be performed under liquid nitrogen cooling condition. The argon ion polishing can meet the requirements of subsequent EBSD experiments when being carried out at the normal temperature of 20-30 ℃, and can reduce the experiment efficiency and improve the experiment cost when being carried out under the condition of liquid nitrogen cooling, the rough reduction and the fine trimming temperature are carried out at the normal temperature, the liquid nitrogen cooling is not needed, the steps are simple, and the cost is low.
In a preferred embodiment of the invention, the ethanol has a mass fraction of 97% and is industrial ethanol; in other embodiments the mass fraction of ethanol may be 97% ± 2%.
In a preferred embodiment of the present invention, the drying is performed by cold air blowing with a blower. The reason for adopting cold wind to weather is to weather the ethanol on the surface of the sample as fast as possible without leaving ethanol water stain, and simultaneously avoid using hot wind and avoiding the oxidation of the surface of the sample.
In an alternative embodiment of the invention, the copper-iron dual phase alloy comprises one of a Cu-5Fe alloy, a Cu-10Fe alloy, and a Cu-14Fe alloy with varying Fe contents.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the preparation method of the sample for the EBSD analysis of the copper-iron dual-phase alloy, provided by the invention, through argon ion polishing, the applicant finds that the vacuum degree in the argon ion polishing is controlled to be 5 multiplied by 10 through tests-3～9×10-3pa, dividing the sample into a rough reduction stage and a fine modification stage, wherein the voltage of the rough reduction stage is 5-7 kv, the time of the rough reduction stage is more than or equal to 7h, the voltage of the fine modification stage is 2-4 kv, and the time of the fine modification stage is more than or equal to 3h, so that the Cu matrix phase and the Fe phase can be simultaneously calibrated on the prepared sample by an EBSD technology, and the calibration rate is as high as 90-99%; the sample preparation method can also calibrate the high-iron-content copper-iron dual phase combination with large rolling deformationGold, and the calibration rate of the sample prepared by the traditional methods such as electrolytic polishing, mechanical polishing and the like is extremely low;
2. according to the preparation method of the sample for the copper-iron dual-phase alloy EBSD analysis, after primary grinding, mechanical polishing and chemical corrosion are not needed, after the ground sample is put into argon ion polishing equipment for polishing, an experimenter is not needed to stare at the equipment all the time, the experiment can be automatically stopped after the experiment time is up, and the sample preparation process is short in flow;
3. according to the preparation method of the sample for the copper-iron dual-phase alloy EBSD analysis, provided by the invention, by the argon ion polishing, chemical reagents such as strong acid and strong base are not needed in the sample preparation process, so that the problem of pollution caused by the chemical reagents such as the strong acid is solved.
Drawings
Fig. 1 is a flowchart of a method for preparing a sample for EBSD analysis of a copper-iron dual-phase alloy according to an embodiment of the present invention;
FIG. 2 is an EBSD phase diagram of as-cast Cu-10Fe obtained in comparative example 1 of the present invention;
FIG. 3 is an EBSD phase diagram of as-cast Cu-10Fe obtained in example 1 of the present invention;
FIG. 4 is an EBSD phase diagram of the cold-rolled Cu-14Fe with an excessive deformation of 95.7% obtained in example 2 of the present invention.
Detailed Description
The present invention is further described in detail below with reference to specific examples so that those skilled in the art can more clearly understand the present invention.
The following examples are provided only for illustrating the present invention and are not intended to limit the scope of the present invention. All other embodiments obtained by a person skilled in the art based on the specific embodiments of the present invention without any inventive step are within the scope of the present invention.
In the examples of the present invention, all the raw material components are commercially available products well known to those skilled in the art, unless otherwise specified; in the examples of the present invention, unless otherwise specified, all technical means used are conventional means well known to those skilled in the art.
In the examples of the present invention, the raw materials used were all conventional commercially available products.
Example 1
The embodiment of the invention provides a preparation method of a sample for EBSD analysis of a copper-iron dual-phase alloy, which comprises the following steps of:
s1, performing linear cutting on the copper-iron dual-phase alloy to obtain a sample to be processed; specifically, the alloy of example 1 was selected as an as-cast Cu-10Fe dual-phase alloy, ensuring that the length and width of the sample were no greater than 4mm and the thickness was no greater than 2mm, taking care of the EBSD calibration direction of the sample.
S2, grinding the sample to be processed, cleaning with ethanol water solution, drying and demagnetizing to obtain a polished sample; specifically, SiC abrasive paper of 400 mesh, 600 mesh, 1000 mesh and 1500 mesh was used in this order for manual grinding, and tap water was used to rinse the abrasive paper and the sample during grinding. The sample is cleaned when the next sand paper is changed, so that the probability of bringing the thicker sand grains on the upper sand paper to the fine sand paper can be reduced, and the original grinding direction is changed by 90 degrees. Because the copper matrix phase in the copper-iron dual-phase alloy is soft, uniform force is required during grinding, the force cannot be too heavy, and the grain size difference of two kinds of sand paper used in sequence is too large. The ground sample is washed with alcohol, then dried with cold air blown by an electric blower, and demagnetized using a demagnetizer.
S3, performing argon ion polishing on the polished sample to obtain a copper-iron dual-phase alloy sample for EBSD analysis; specifically, a JEOL IB-19530CP argon ion polishing device is used for bombarding the surface of a sample, mounting the sample, and vacuumizing to 7 x 10-3pa, roughly reducing the voltage by 6kv, wherein the roughly reducing time is more than or equal to 7 h; then, fine trimming is carried out, wherein the fine trimming voltage is 3kv, the coarse trimming and the fine trimming are carried out at normal temperature within 3h without using liquid nitrogen for cooling, and the used ion beams are argon ions; the angle formed by the argon ion beam and the polished sample surface is controlled at 90 degrees. And after the argon ion polishing is finished, taking out the sample, and placing the sample into electron microscope equipment for EBSD calibration.
Example 2
The embodiment of the invention provides a preparation method of a sample for EBSD analysis of a copper-iron dual-phase alloy, which comprises the following steps of:
s1, performing linear cutting on the copper-iron dual-phase alloy to obtain a sample to be processed; specifically, the Cu-14Fe dual-phase alloy in a cold rolling state with the excessive deformation amount of 95.7% is selected, the length and the width of the sample are not more than 4mm, the thickness of the sample is not more than 2mm, and the EBSD calibration direction of the sample is noticed.
S2, grinding the sample to be processed, cleaning with ethanol water solution, drying and demagnetizing to obtain a polished sample; specifically, SiC abrasive paper of 400 mesh, 600 mesh, 1000 mesh and 1500 mesh was used in this order for manual grinding, and tap water was used to rinse the abrasive paper and the sample during grinding. When the next sand paper is changed, the sample is cleaned, the sand grains with thicker upper sand can be brought to the fine sand paper, and the original grinding direction is changed by 90 degrees. Because the copper matrix phase in the copper-iron dual-phase alloy is soft, uniform force is required during grinding, the force cannot be too heavy, and the grain size difference of two kinds of sand paper used in sequence is too large. The ground sample is washed with alcohol, then dried with cold air blown by an electric blower, and demagnetized using a demagnetizer.
S3, performing argon ion polishing on the polished sample to obtain a copper-iron dual-phase alloy sample for EBSD analysis; specifically, a JEOL IB-19530CP argon ion polishing device is used for bombarding the surface of a sample, mounting the sample, and vacuumizing to 7 x 10-3pa, roughly reducing the voltage by 6kv, wherein the roughly reducing time is more than or equal to 7 h; then, fine trimming is carried out, wherein the fine trimming voltage is 3kv, the coarse trimming and the fine trimming are carried out at normal temperature within 3h without using liquid nitrogen for cooling, and the used ion beams are argon ions; the angle formed by the argon ion beam and the polished sample surface is controlled at 85 degrees. And after the argon ion polishing is finished, taking out the sample, and placing the sample into electron microscope equipment for EBSD calibration.
Example 3
The embodiment of the invention provides a preparation method of a sample for analyzing copper-iron dual-phase alloy EBSD, as shown in figure 1, the method comprises the following steps:
s1, performing linear cutting on the copper-iron dual-phase alloy to obtain a sample to be processed; specifically, a Cu-5Fe dual-phase alloy is selected, the length and the width of the sample are ensured to be not more than 4mm, the thickness of the sample is ensured to be not more than 2mm, and the EBSD calibration direction of the sample is taken into consideration.
S2, grinding the sample to be processed, cleaning with ethanol water solution, drying and demagnetizing to obtain a polished sample; specifically, SiC abrasive paper of 400 mesh, 600 mesh, 1000 mesh and 1500 mesh was used in this order for manual grinding, and tap water was used to rinse the abrasive paper and the sample during grinding. When the next sand paper is changed, the sample is cleaned, the sand grains with thicker upper sand can be brought to the fine sand paper, and the original grinding direction is changed by 90 degrees. Because the copper matrix phase in the copper-iron dual-phase alloy is soft, uniform force is required during grinding, the force cannot be too heavy, and the grain size difference of two kinds of sand paper used in sequence is too large. The ground sample is washed with alcohol, then dried with cold air blown by an electric blower, and demagnetized using a demagnetizer.
S3, performing argon ion polishing on the polished sample to obtain a copper-iron dual-phase alloy sample for EBSD analysis; specifically, a JEOL IB-19530CP argon ion polishing device is used for bombarding the surface of a sample, mounting the sample, and vacuumizing to 7 x 10-3pa, roughly reducing the voltage by 6kv, wherein the roughly reducing time is more than or equal to 7 h; then, fine trimming is carried out, wherein the fine trimming voltage is 3kv, the coarse trimming and the fine trimming are carried out at normal temperature within 3h without using liquid nitrogen for cooling, and the used ion beams are argon ions; the angle formed by the argon ion beam and the polished sample surface is controlled at 95 deg. And after the argon ion polishing is finished, taking out the sample, and placing the sample into electron microscope equipment for EBSD calibration.
Example 4
In this example, the degree of vacuum in the argon ion polishing was controlled to 6X 10-3The voltage of the rough reduction stage is 5.5kv, and the voltage of the fine modification stage is 2.5 kv; the other steps were the same as in example 1.
Example 5
In this example, the degree of vacuum in the argon ion polishing was controlled to 8X 10-3The voltage of the rough reduction stage is 6.5kv, and the voltage of the fine modification stage is 3.5 kv; other steps are the same as the embodiment1。
Example 6
In this example, the degree of vacuum in the argon ion polishing was controlled to 5X 10-3The voltage of the rough reduction stage is 5kv, and the voltage of the fine modification stage is 2 kv; the other steps were the same as in example 1.
Example 7
In this example, the degree of vacuum in the argon ion polishing was controlled to 9X 10-3The voltage of the rough reduction stage is 7kv, and the voltage of the fine modification stage is 4 kv; the other steps were the same as in example 1.
Comparative example 1
The comparative example adopts an electrolytic polishing mode, and comprises the following specific steps:
and performing wire cutting on the as-cast Cu-10Fe dual-phase alloy to ensure that the length and the width of the sample are not more than 4mm and the thickness is not more than 2mm, and paying attention to the EBSD calibration direction of the sample, wherein the length direction is parallel to the X-axis direction.
The SiC sandpaper with 400 meshes, 600 meshes, 1000 meshes and 1500 meshes is used for manual grinding in sequence, and tap water is used for washing the sandpaper and the sample in the grinding process. When the next sand paper is changed, the sample is cleaned, the sand grains with thicker upper sand can be brought to the fine sand paper, and the original grinding direction is changed by 90 degrees. Because the copper matrix phase in the copper-iron dual-phase alloy is soft, uniform force is required during grinding, the force cannot be too heavy, and the grain size difference of two kinds of sand paper used in sequence is too large. The ground sample is washed with alcohol, then dried with cold air blown by an electric blower, and demagnetized using a demagnetizer.
During electrolytic polishing, the demagnetized as-cast Cu-10Fe alloy is used as an anode, the stainless steel sheet is used as a cathode, the electrolytic polishing solution is a mixed solution of 85% phosphoric acid and 15% deionized water, the electrolytic polishing parameter is 2.1V, the normal temperature is realized, and the polishing time is 8 min.
After the electrolytic polishing is finished, the sample can be taken out, quickly washed by alcohol, immediately dried by cold air and placed into electron microscope equipment for EBSD calibration.
Comparative example 2
In the comparative example, the argon ion polishing is not divided into a rough reduction stage and a fine modification stage, and the voltage in the whole process of the argon ion polishing is 6 kv; the other steps were the same as in example 1.
Comparative example 3
In the comparative example, the voltage of the rough reduction stage in the argon ion polishing is 3kv, and the time of the rough reduction stage is 5 h; the other steps were the same as in example 1.
Comparative example 4
In this comparative example, the voltage at the rough reduction stage in the argon ion polishing was 9 kv; the other steps were the same as in example 1.
Comparative example 5
In this comparative example, the voltage at the finishing stage in the argon ion polishing was 1 kv; the other steps were the same as in example 1.
Comparative example 6
In this comparative example, the voltage at the finishing stage in the argon ion polishing was 6 kv; the other steps were the same as in example 1.
Comparative example 7
In this comparative example, the angle of the argon ion beam with the polished sample surface in the argon ion polishing was controlled to be 9 °; the other steps were the same as in example 1.
Experimental example 1
The samples of examples 1 to 7 and comparative examples 1 to 6 were placed in an electron microscope device for EBSD calibration, and the statistics of the calibration rate are shown in table 1.
TABLE 1
Note: the experimental effects corresponding to the calibration rates in table 1 were evaluated, in order from good to bad: good, better, slightly worse, very bad.
From the data in table 1, it can be seen that:
in comparative example 1, the electrolytic polishing method was used, and as a result, the Fe phase could not be identified; the EBSD phase diagram of the as-cast Cu-10Fe obtained in the comparative example 1 is shown in FIG. 2, and a large number of black areas in FIG. 2 are Fe phases which cannot be calibrated, thus influencing the experimental result;
in comparative example 2, the argon ion polishing is not divided into a rough reduction stage and a fine modification stage, and the voltage in the whole process of the argon ion polishing is 6 kv; the defects of uneven sample surface and poor calibration effect exist;
in comparative example 3, the voltage of the rough reduction stage in the argon ion polishing is 3kv (which is less than the range of 5-7 kv of the embodiment of the invention), and the time of the rough reduction stage is 5h (which is less than the range of more than or equal to 7h of the embodiment of the invention); the defects of low penetration depth of argon ions and poor calibration effect exist;
in the comparative example 4, the voltage of the rough reduction stage in the argon ion polishing is 9kv, which is larger than the range of 5-7 kv of the embodiment of the invention, and the defects of deep penetration depth, unevenness and poor calibration effect of the argon ions exist;
in comparative example 5, the voltage at the finishing stage in the argon ion polishing was 1kv, which is less than the range of example 2 to 4kv of the present invention; the defect that the surface unevenness of the sample after rough shearing cannot be repaired exists;
in comparative example 6, the voltage at the finishing stage in the argon ion polishing was 6 kv; the calibration method is larger than the range of 2-4 kv of the embodiment of the invention, and has the defects of uneven sample surface and poor calibration effect;
in comparative example 7, the angle formed by the argon ion beam and the polished sample surface in the argon ion polishing is controlled to be 9 degrees and is smaller than the range of 85-95 degrees in the embodiment of the invention, and the defects of low penetration depth and low calibration rate of argon ions exist;
in examples 1 to 7, the iron phase and the copper matrix phase can be calibrated simultaneously, and the calibration rate of the prepared sample is as high as 90-99%. The samples obtained in the embodiments 1-3 have higher calibration rate, and are preferred embodiments; example 1-example 3 the sample calibration rate was the highest and was the best example;
an EBSD phase diagram of the as-cast Cu-10Fe obtained in the embodiment 1 of the invention is shown in FIG. 3, and a large number of red-black areas in FIG. 3 are marked Fe phases, so that information such as the distribution and size of the Fe phases can be obviously observed;
the EBSD phase diagram of the cold-rolled Cu-14Fe with the deformation of 95.7% obtained in the embodiment 2 of the invention is shown in FIG. 4, and a large number of red-black areas in FIG. 4 are marked Fe phases.
As compared with comparative example 1, the polishing method of the examples of the present application can easily produce as-cast Cu-10Fe for which conventional electrolytic polishing could not successfully produce EBSD samples. Compared with Cu-10Fe alloy, the EBSD sample preparation method can clearly and simultaneously calibrate a copper matrix phase and an iron phase no matter Cu-14Fe with higher iron content or in a cold rolling state with the excessive deformation of 95.7 percent, and can obviously see important information such as distribution, volume fraction, orientation and the like of the iron phase.
As compared with comparative examples 2 to 6, in the method for preparing samples for EBSD analysis of copper-iron dual-phase alloy of the present invention, the degree of vacuum in argon ion polishing was controlled at 5X 10-3～9×10-3pa, and dividing the calibration sample into a rough reduction stage and a fine modification stage, wherein the voltage of the rough reduction stage is 5-7 kv, the time of the rough reduction stage is more than or equal to 7h, the voltage of the fine modification stage is 2-4 kv, the time of the fine modification stage is more than or equal to 3h, and the parameters are all absent, so that the calibration iron phase and the copper matrix phase are jointly calibrated, and the calibration rate of the prepared sample is as high as 94-99%.
In conclusion, the polishing method provided by the application can calibrate the EBSD sample of the Cu-Fe dual-phase alloy which cannot be successfully prepared by the conventional method, can solve the problem that the EBSD sample of the Cu-Fe dual-phase alloy cannot be successfully prepared under the condition of ultra-large deformation, and can provide important guarantee for the basic and industrial research of the copper-iron alloy.
It should be noted that the above examples are only for further illustration and description of the technical solution of the present invention, and are not intended to further limit the technical solution of the present invention, and the method of the present invention is only a preferred embodiment, and is not intended to limit the protection scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a sample for EBSD analysis of a copper-iron dual-phase alloy is characterized by comprising the following steps:
performing linear cutting on the copper-iron dual-phase alloy to obtain a sample to be processed;
grinding the sample to be treated, cleaning with ethanol, drying and demagnetizing to obtain a polished sample;
performing argon ion polishing on the polished sample to obtain a copper-iron dual-phase alloy sample for EBSD analysis; wherein the vacuum degree in the argon ion polishing is controlled at 5 × 10-3～9×10-3pa, the argon ion polishing sequentially comprises a rough reduction stage and a fine modification stage, the voltage of the rough reduction stage is 5-7 kv, the time of the rough reduction stage is not less than 7h, the voltage of the fine modification stage is 2-4 kv, and the time of the fine modification stage is not less than 3 h.
2. The method for preparing a sample for EBSD analysis of a copper-iron dual-phase alloy according to claim 1, wherein an angle formed by the argon ion beam and the polished sample surface is controlled to 85 to 95 °.
3. The method for preparing a sample for EBSD analysis of the copper-iron dual-phase alloy according to claim 1, wherein the argon ion polishing employs an argon ion beam with a purity of not less than 99.9%, and an ion beam flow rate of the argon ion beam is 0.1-0.15 sccm.
4. The method for preparing a sample for EBSD analysis of a copper-iron dual-phase alloy according to claim 1, wherein the degree of vacuum in argon ion polishing is controlled to 6 x 10-3～8×10-3pa, the voltage of the rough reduction stage is 5.5-6.5 kv, and the voltage of the fine modification stage is 2.5-3.5 kv.
5. The method for preparing a sample for EBSD analysis of a copper-iron dual phase alloy according to claim 1, wherein the argon ion polishing medium vacuum degree controlAt 7X 10-3pa, the voltage of the rough reduction stage is 6kv, and the voltage of the fine modification stage is 3 kv.
6. The method for preparing a sample for EBSD analysis of a copper-iron dual phase alloy according to claim 1, wherein in the grinding, SiC sandpaper of 400 mesh, 600 mesh, 1000 mesh, and 1500 mesh is used in this order for multiple times of grinding; and between two adjacent times of grinding, washing the SiC sand paper and the sample to be treated by water, and rotating the sample to be treated by 90 degrees along the same direction.
7. The method for preparing a sample for EBSD analysis of the copper-iron dual-phase alloy according to claim 6, wherein the grinding time with 400 mesh, 600 mesh, 1000 mesh and 1500 mesh SiC sandpaper is 2-5 min.
8. The method for preparing a sample for EBSD analysis of a copper-iron dual-phase alloy according to claim 1, wherein the length of the sample to be treated is not more than 4mm, the width is not more than 4mm, and the thickness is not more than 2 mm.
9. The method for preparing a sample for EBSD analysis of a copper-iron dual-phase alloy according to claim 1, wherein the argon ion polishing temperature is 20-30 ℃.
10. The method for preparing a sample for EBSD analysis of a copper-iron dual-phase alloy according to claim 1, wherein the mass fraction of ethanol is 95% -99%; and the drying is realized by using cold air of a blower.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113945593A (en) * | 2021-10-18 | 2022-01-18 | 广东省科学院新材料研究所 | Magnesium-based composite material EBSD test sample and preparation method and application thereof |
| CN115728194A (en) * | 2022-11-21 | 2023-03-03 | 山东大学 | Method for detecting crystal grain morphology of copper foil section |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104089801A (en) * | 2014-06-26 | 2014-10-08 | 上海市计量测试技术研究院 | Preparation method for electron back scattered diffraction test sample of zirconium oxide thermal barrier coating |
| CN104698146A (en) * | 2013-12-06 | 2015-06-10 | 北京有色金属研究总院 | A research method of a copper alloy multielement diffusion couple |
-
2021
- 2021-06-15 CN CN202110663447.7A patent/CN113358437A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104698146A (en) * | 2013-12-06 | 2015-06-10 | 北京有色金属研究总院 | A research method of a copper alloy multielement diffusion couple |
| CN104089801A (en) * | 2014-06-26 | 2014-10-08 | 上海市计量测试技术研究院 | Preparation method for electron back scattered diffraction test sample of zirconium oxide thermal barrier coating |
Non-Patent Citations (3)
| Title |
|---|
| 任颂赞 等: "《金相分析原理及技术》", 31 August 2013, 上海科学技术文献出版社 * |
| 刘仕超: "亚稳难混溶Cu-Fe合金凝固组织及磁性能研究", 《中国优秀博硕学位论文全文数据库 工程科技Ⅰ辑》 * |
| 高尚 等: "磁场导致的EBSD花样畸变与解决方法", 《分析仪器》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113945593A (en) * | 2021-10-18 | 2022-01-18 | 广东省科学院新材料研究所 | Magnesium-based composite material EBSD test sample and preparation method and application thereof |
| CN115728194A (en) * | 2022-11-21 | 2023-03-03 | 山东大学 | Method for detecting crystal grain morphology of copper foil section |
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