CN114166596B - Transmission electron microscope sample preparation method for high-plasticity precious metal material - Google Patents
Transmission electron microscope sample preparation method for high-plasticity precious metal material Download PDFInfo
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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
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
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- B24B49/00—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation
- B24B49/16—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation taking regard of the load
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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- 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 relates to a transmission electron microscope sample preparation method for a high-plasticity noble metal material, and belongs to the technical field of noble metal material analysis and test. The method comprises the steps of carrying out linear cutting on a high-plasticity noble metal material to obtain a square metal sheet, carrying out coarse grinding on two sides of the metal sheet to remove cutting scratches until the thickness is not more than 100 mu m, cleaning and airing, and punching by using a transmission sample punching machine to obtain a wafer sample; uniformly adhering wafer samples to the surface of a sample table at equal intervals, and fixing the sample table at the grinding and polishing position of the lapping integrated machine; using water as cooling liquid and Al with different meshes 2 O 3 Grinding and polishing the grinding disc to gradually reduce the thickness to 15-20 mu m; polishing the wafer by using polishing flannelette to eliminate scratches and stress concentration to obtain a transmission wafer sample; and in the argon atmosphere, adopting an ion thinning instrument to carry out clockwise and anticlockwise rotation bombardment thinning perforation of double ion beams to obtain a thinned transmission electron microscope sample. The method can obtain a large-area thin area without stress stripes or patterns so as to effectively observe and characterize the microstructure of the material by a transmission electron microscope.
Description
Technical Field
The invention relates to a transmission electron microscope sample preparation method of a high-plasticity noble metal material, and belongs to the technical field of noble metal material preparation.
Background
The noble metal is widely used as a precise electronic functional device, a temperature measuring tool, a medical instrument, a jewelry and the like due to excellent plasticity, chemistry and high-temperature stability, and the noble metal material is easily processed into specific shapes such as tiny, narrow and thin due to the good plasticity, but the problem is also brought by the high plasticity.
The noble metal material has stronger corrosion resistance in acid and alkali, so that the material can not adopt the conventional metal electrolysis double-spraying method when a transmission electron microscope sample is prepared, and only can adopt an ion thinning method to prepare a thin area required by observation. When a sample is prepared by a conventional ion reduction method, the sample needs to be pretreated, after the sample is polished to the thickness of less than 50 mu m, the sample is placed on a pit instrument, a pit is further polished at the center of the sample by adopting a grinding wheel, the thickness of a central micro-area is reduced to be less than 20 mu m, and finally, an ion beam is used for bombarding a central area for perforating so as to obtain a thin observation area of a transmission electron microscope. When the method is adopted to prepare the transmission sample of the high-plasticity noble metal material, the method has the biggest defects that large-area stress stripes and patterns often appear in the thin area of the obtained transmission electron microscope sample and shield the microstructure in the material, and the material is difficult to effectively represent the organizational structure characteristics in the material through the transmission electron microscope, except that the grinding and polishing time is long, the area of the central thin area is small, the randomness is high and the controllability is poor.
Due to the limitation of microscopic characterization, the research depth and the heat of the noble metal material are influenced, and the further development and utilization of the high-plasticity noble metal material are restricted.
Disclosure of Invention
The invention provides a transmission electron microscope sample preparation method of a high-plasticity noble metal material, aiming at the problem of sample preparation of a transmission electron microscope sample of the high-plasticity noble metal material in the prior art, the sample is ground and polished to an ultrathin wafer with the thickness of less than 20 mu m by adopting a fine grinding all-in-one machine, the flat ultrathin sample is subjected to ion beam bombardment thinning by adopting a progressively larger incident angle, a large-area central thin area without stress concentration is obtained, and the tissue structure of the material can be effectively observed.
A transmission electron microscope sample preparation method for a high-plasticity precious metal material comprises the following specific steps:
(1) performing linear cutting on a high-plasticity noble metal material to obtain a square metal sheet, performing coarse grinding on two sides of the metal sheet to remove cutting scratches until the thickness is not more than 100 mu m, cleaning and drying, and punching by using a transmission sample punching machine to obtain a wafer sample; preferably, the size of the square metal sheet is 1cm multiplied by 1cm, and the thickness is 150-200 μm; the diameter of the wafer sample is 3mm, and the thickness of the wafer sample is 90-100 mu m;
(2) uniformly adhering wafer samples to the surface of a sample table at equal intervals, and fixing the sample table at the grinding and polishing position of the lapping integrated machine;
(3) using water as cooling liquid and Al with different meshes 2 O 3 Grinding and polishing the grinding disc to gradually reduce the thickness to 15-20 mu m; low-polishing with polishing flannelette to eliminate scratch and stress concentrationTransmitting the wafer sample;
(4) in argon atmosphere, adopting an ion thinning instrument to carry out clockwise and anticlockwise rotation bombardment thinning perforation of double ion beams to obtain a thinned transmission electron microscope sample; preferably, when the ion beam is bombarded by rotating clockwise and anticlockwise, the sample is thinned sequentially according to an acceleration voltage of 5KeV → 3KeV → 2KeV → 1KeV and a double ion beam incidence angle of +/-3 ° → +/-5 ° → +/-8 ° → +/-10 °, the ion beam bombardment time of different materials is different, and the perforation condition of the center of the sample is observed through an eyepiece after each pass is finished in the thinning process;
the distance between the wafer samples in the step (2) is 4.5-6 mm;
the contact stress of the grinding and polishing in the step (3) is 10-20N, so that the sample is not subjected to large plastic deformation while the sample is ground and polished, and stress stripes and patterns are prevented from being generated;
the specific method for grinding and polishing step-by-step thinning comprises
1) Grinding and polishing a grinding disc with the diameter of 9 mu m in a reciprocating and circulating way until the accumulated sample introduction step length is more than 40 mu m; wherein the step length of single sample introduction is 1 mu m;
2) grinding and polishing a grinding disc with the diameter of 2 micrometers in a reciprocating and circulating manner until the accumulated sample introduction step length is more than 30 micrometers; wherein the step length of single sample introduction is 1 mu m;
3) automatically feeding and polishing a grinding disc with the diameter of 0.5 mu m until the thickness of a sample is 15-20 mu m, wherein the step length of single feeding is 0.5 mu m;
further, the automatic sample feeding mode is
Using formulas
D ═ a-b-c-20, where a is the original thickness of the sample; b is the accumulated step length of grinding and polishing of a grinding disc with the diameter of 9 mu m; c is the accumulated step length of grinding and polishing of a grinding disc with the diameter of 2 mu m;
calculating the difference between the initial sample thickness and the polished accumulated step length, and switching an automatic sample feeding mode to set an automatic sample feeding and grinding thickness value;
and (4) polishing the flannelette in the step (3) at a rotating speed of 400-500 r/min.
The specific method for the double-ion-beam bombardment thinning perforation in the step (4) is
1) Performing ion beam clockwise rotation bombardment on the center of the sample for 1-2 min by adopting a voltage of 4.5-5 KeV and a double ion beam incident angle of +/-3 degrees, and then performing ion beam anticlockwise rotation bombardment for 1-2 min;
2) carrying out ion beam clockwise rotation bombardment on the center of the sample for 3-5 min by adopting a voltage of 3-3.5 KeV and a double ion beam incidence angle of +/-5 degrees, and then adopting ion anticlockwise rotation bombardment for 3-5 min;
3) performing ion beam clockwise rotation bombardment on the center of the sample for 3-10 min by adopting a voltage of 1.5-2 KeV and a double ion beam incident angle of +/-8 degrees, and performing ion counterclockwise rotation bombardment for 3-10 min;
4) and (3) carrying out ion beam clockwise rotation bombardment on the center of the sample for 5-10 min by adopting a voltage of 0.8-1 KeV and a double ion beam incident angle of +/-10 degrees, and then adopting ion anticlockwise rotation bombardment for 5-10 min.
The invention has the beneficial effects that:
(1) in the pretreatment process of the sample, pits are not ground and polished, and local plastic deformation caused by external stress is avoided, so that the influence and interference of stress generated in sample preparation on microstructure characterization are fundamentally eliminated, and more effective observation areas can be obtained in characterization;
(2) according to the invention, when the sample is ground and polished to an ultrathin wafer with the thickness of less than 20 μm by using the fine grinding all-in-one machine, a flat slice sample can be obtained, and the grinding and polishing thickness of the sample is controllable. The method is different from the traditional technology that the sample needs to be repeatedly bonded, the sample is polished and the thickness is measured, the method only needs to bond the sample once, the steps are reduced, and the time is shortened;
(3) according to the invention, 4-6 transmission electron microscope wafer samples with the diameter of 3mm can be synchronously polished on the sample table, and the sample preparation efficiency is greatly improved;
(4) the invention adopts the increasing larger incident angle to carry out ion beam bombardment thinning on the flat ultrathin sample, so that a large-area central thin area without stress concentration is easily obtained, and the tissue structure of the material is effectively observed.
Drawings
FIG. 1 is a schematic diagram comparing the technical principles of a conventional thinning sample preparation method and the method of the present invention;
FIG. 2 is an observation image of a transmission sample prepared by a conventional method of the highly plastic Au-based alloy in example 1;
FIG. 3 is an observation image of a high-plasticity Au-based alloy transmission sample prepared by the method of example 1;
FIG. 4 is an observation image of a transmission sample prepared by a conventional method using the highly plastic Pd-based and Pt-based alloys in example 2;
fig. 5 is an observation image of the high plasticity Pd-based and Pt-based alloy transmission samples prepared by the method of example 2.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a transmission electron microscope sample preparation method of a high-plasticity noble metal material comprises the following specific steps:
(1) performing linear cutting on a high-plasticity Au-based alloy bar with the diameter of 1.5cm, taking down a 1cm × 1cm square metal sheet with the thickness of 150 μm, roughly grinding two surfaces of the metal sheet to remove cutting scratches, measuring the actual thickness of the metal sheet to be 97.3 μm, cleaning the surface of the metal sheet with alcohol, then drying the metal sheet, and punching the metal sheet by using a transmission sample punching machine to obtain 4 small round sheets with the sample size of 3 mm;
(2) measuring the small wafer samples, recording the initial thicknesses and numbering, and adhering 4 samples to the center position close to the sample table at equal intervals by using hot melt adhesive, wherein the distance between the samples is about 6mm (namely the distance between the two samples); after the hot melt adhesive is firmly bonded, clamping and fixing a sample processing table at the grinding and polishing position of the lapping all-in-one machine, and after the sample is ground and polished;
(3) the sample has good plasticity and is easy to polish, and Al with different meshes is adopted 2 O 3 Grinding and polishing the grinding disc step by step to thin, adjusting the sample table to be parallel to the grinding disc before grinding and polishing, and taking water as cooling liquid during grinding and polishing;
slowly feeding a sample, slightly contacting a grinding disc with the surface of the sample to generate a contact stress value of 12N, clicking a sample position zeroing key of the equipment, and setting the position as a grinding and polishing initial position; after the first grinding and polishing, a grinding disc with the diameter of 9 mu m is adopted to advance by the step length distance of 1 mu m, the next grinding and polishing is continued, and the reciprocating circulation is carried out until the sampling step length is accumulated to be 42 mu m; grinding and polishing by replacing a grinding disc with 2 mu m, and carrying out grinding and polishing by carrying out reciprocating sample injection with a step length distance of 1 mu m until the sample injection step length is cumulated to be 31 mu m; finally, a grinding disc with the diameter of 0.5 mu m is replaced, and the mode is switched to an automatic grinding and polishing mode; according to the formula
D ═ a-b-c-20, where a is the original thickness of the sample; b is the accumulated step length of grinding and polishing of a grinding disc with the diameter of 9 mu m; c is the accumulated step length of grinding and polishing of a grinding disc with the diameter of 2 mu m,
calculating the difference between the initial sample thickness and the polished accumulated step length to be 24.3 mu m, and setting the automatic sample introduction and grinding thickness value to be 4.5 mu m because the sample introduction step length is 0.5 mu m, so that the sample thickness is polished to be 19.8 mu m, which is close to and slightly lower than 20 mu m; polishing for 5min at low rotation speed by using polishing flannelette without changing the relative position of the sample and the grinding disc, reducing scratches and surface stress;
(4) after polishing, soaking the obtained 4 ultrathin transmission wafer samples in acetone for 30min, and drying after the hot melt adhesive is completely dissolved; the samples are placed in an ion thinning instrument one by one to carry out double ion beam bombardment thinning perforation, and the Au-based alloy is sensitive to the action of the ion beam and needs to be selected for shorter bombardment time; firstly, carrying out ion beam clockwise rotation bombardment for 1min on the center of a sample by adopting a voltage of 4.5KeV and an incidence angle of +/-3 degrees, and then adopting ion beam anticlockwise rotation bombardment for 1 min; adjusting the voltage to 2.5KeV, and allowing the incident angle of the double ion beams to be +/-5 degrees, performing ion beam clockwise rotation bombardment for 3min, and performing ion beam anticlockwise rotation bombardment for 3 min; adjusting the voltage to 1.5KeV, and carrying out ion beam clockwise rotation bombardment for 5min when the incident angle of the double ion beams is +/-8 degrees, and then carrying out ion beam anticlockwise rotation bombardment for 5 min; adjusting the voltage to 0.8KeV, and carrying out ion beam clockwise rotation bombardment for 8min when the incident angle of the double ion beams is +/-10 degrees, and then carrying out ion beam anticlockwise rotation bombardment for 10 min; in the thinning process, the perforation condition of the center of the sample is observed through the ocular lens after each pass is finished;
(5) taking out the thinned sample, and placing the thinned sample in a transmission electron microscope for observation;
FIG. 2 is an electron microscope image of a high-plasticity Au-based alloy transmission sample prepared by a traditional method, and FIG. 3 is an electron microscope image of a high-plasticity Au-based alloy transmission sample prepared by a patent method; in FIG. 2, a large number of stress stripes and patterns seriously shield the texture structure of the Au-based alloy, and the characterization and identification of crystal grains, substructures and phases cannot be carried out; in fig. 3, the interference of stress fringes is eliminated, so that the characteristics of the microstructure can be clearly displayed, and the structure information of the tissue and the phase can be effectively observed; the grains with different shapes and sizes and twin structures with larger contrast difference can be clearly seen in FIG. 3 (b); compared with the image observed after the microstructure image is prepared by the traditional method in the embodiment shown in FIG. 2, the microstructure image obtained by the method has a larger thin area and an observable area is larger; and stress stripes or patterns do not appear in a visual field, the characteristic structure of the alloy is effectively observed and characterized.
Example 2: a transmission electron microscope sample preparation method of a high-plasticity noble metal material comprises the following specific steps:
(1) respectively adopting linear cutting on a high-plasticity Pd-based alloy bar with the diameter of 1.5cm and a high-plasticity Pt-based alloy bar with the diameter of 1.8cm to take down square metal sheets with the thickness of 200 mu m, and measuring the actual thicknesses of the two metal sheets to be 95.6 mu m and 91.9 mu m after removing cutting scratches by coarse grinding on the two sides; cleaning the surface with alcohol, drying, punching with a transmission sample punching machine to obtain 3 small wafers with the sample size of 3 mm;
(2) because the size of the sample table is 2.5cm, the number of samples longitudinally bonded in each row on the sample table is at most 3, and the samples made of the same material are bonded in the same row, the grinding disc is ensured to be transversely ground and polished on the same material along the horizontal direction; after the small wafer samples are measured in sequence, recording the initial thicknesses and numbering, and adhering 6 samples to the center position close to the sample table at equal intervals by using hot melt adhesive, wherein the sample interval distance is about 4.5mm (namely one half sample interval); after the hot melt adhesive is firmly bonded, clamping and fixing a processing sample table at the grinding and polishing position of the lapping all-in-one machine, and after the samples are ground and polished, keeping the sample table against rotation in the grinding and polishing process, and longitudinally arranging two substrates in left and right rows;
(3) using Al of different mesh numbers 2 O 3 Grinding and polishing the grinding disc step by step to thin, adjusting the sample table to be parallel to the grinding disc before grinding and polishing, and taking water as cooling liquid during grinding and polishing; because the original thicknesses of the two alloy materials are different, a thicker alloy sample is placed at the leftmost side, the sample is slowly fed, and a mill is usedSlightly contacting the disc with the surface of the leftmost sample to generate a contact stress value of 14N, clicking a device sample position zeroing key, and setting the position as a grinding and polishing initial position; because the right sample is thin, the sample is not polished when the sample is just fed, and the sample is polished when the thickness of the sample and the thickness of the sample are consistent, the accumulated step length is recorded, and the calculation is carried out according to the thicker end when the automatic polishing step length is calculated; after the first grinding and polishing, a grinding disc with the diameter of 9 mu m is adopted to advance by the step length distance of 1 mu m, the next grinding and polishing is continued, and the reciprocating circulation is carried out until the accumulated sample feeding step length is 41 mu m; grinding and polishing by changing a grinding disc with the diameter of 2 micrometers, and carrying out grinding and polishing by carrying out reciprocating sample injection at the step length distance of 1 micrometer until the sample injection step length is cumulatively 32 micrometers; finally, the grinding disc with the diameter of 0.5 mu m is replaced, and the mode is switched to the automatic grinding and polishing mode according to the formula
D ═ a-b-c-20, where a is the original thickness of the sample; b is the accumulated step length of grinding and polishing of a grinding disc with the diameter of 9 mu m; c is the accumulated step length of grinding and polishing of a grinding disc with the diameter of 2 mu m,
calculating to find that the difference values of the thickness of the initial Pd-based alloy sample and the grinding and polishing accumulated step length are 22.6 mu m respectively, and setting an automatic sample feeding and grinding thickness value of 3 mu m to enable the thickness of the Pd-based alloy sample to be ground and polished to be 19.6 mu m and close to or lower than 20 mu m because the sample feeding step length is 0.5 mu m; at the moment, the thickness of the Pt-based alloy sample is similar to that of the Pd-based alloy sample and is slightly lower than 20 mu m; finally, polishing for 10min at low rotation speed by using polishing flannelette without changing the relative position of the sample and the grinding disc, so as to reduce scratches and surface stress;
(4) after polishing, soaking the 6 ultrathin transmission wafer samples in acetone for 30min, and drying after the hot melt adhesive is completely dissolved; the samples are put into an ion thinning instrument one by one to carry out double ion beam bombardment thinning perforation, and because the Pd-based alloy and the Pt-based alloy are less sensitive to the ion beam than the Au-based alloy, a slightly long bombardment time can be selected;
firstly, carrying out ion beam clockwise rotation bombardment for 2min on the center of a sample by adopting a voltage of 5KeV and an incidence angle of +/-3 degrees, and then adopting ion beam anticlockwise rotation bombardment for 2 min; adjusting the voltage to 3KeV, and carrying out ion beam clockwise rotation bombardment for 5min when the incident angle of the double ion beams is +/-5 degrees, and then adopting ion beam anticlockwise rotation bombardment for 5 min; adjusting the voltage to 2KeV, and carrying out ion beam clockwise rotation bombardment for 10min when the incident angle of the double ion beams is +/-8 degrees, and then adopting ion beam anticlockwise rotation bombardment for 10 min; finally, adjusting the voltage to 1KeV and enabling the incident angle of the double ion beams to be +/-10 degrees, carrying out ion beam clockwise rotation bombardment for 10min, and then adopting ion beam anticlockwise rotation bombardment for 10 min; observing the perforation condition of the center of the sample through an ocular lens after each pass is finished in the thinning process;
(5) taking out the thinned sample, and placing the thinned sample in a transmission electron microscope for observation;
fig. 4(a) is an electron microscope collection image of a high-plasticity Pd-based alloy transmission sample prepared by a conventional method, and fig. 4(b) is an electron microscope collection image of a high-plasticity Pt-based alloy transmission sample prepared by a conventional method; in FIG. 4, a large number of stress stripes and patterns seriously shield the organization structure in the alloy, and the grains, the grain boundaries and the substructures cannot be observed and analyzed; FIG. 5 can clearly show the specific microstructure characteristics of the film due to the elimination of the interference of the stress fringes; fig. 5(a) is an electron microscope image of a Pd-based alloy sample, which can clearly observe the grain, grain boundary, orientation information, etc. of the material; FIG. 5(b) is an electron microscope image of a Pt-based alloy sample, which clearly shows the sub-grain condition, grain boundary type, twin crystal distribution and the like formed in the large grains in the material treatment process;
compared with the image observed after the microstructure image is prepared by the traditional method in the embodiment in the figure 4, the microstructure image obtained by the method has a larger thin area and a larger observable area; and stress stripes or patterns do not appear in a visual field, the characteristic structure of the alloy is effectively observed and characterized.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (5)
1. A transmission electron microscope sample preparation method of a high-plasticity noble metal material is characterized by comprising the following specific steps:
(1) performing linear cutting on a high-plasticity noble metal material to obtain a square metal sheet, performing coarse grinding on two sides of the metal sheet to remove cutting scratches until the thickness is not more than 100 mu m, cleaning and drying, and punching by using a transmission sample punching machine to obtain a wafer sample;
(2) uniformly adhering wafer samples to the surface of a sample table at equal intervals, and fixing the sample table at the grinding and polishing position of the lapping integrated machine;
(3) using water as cooling liquid and Al with different meshes 2 O 3 Grinding and polishing the grinding disc to gradually reduce the thickness to 15-20 mu m; polishing at low speed by using polishing flannelette to eliminate scratches and stress concentration to obtain a transmission wafer sample;
the specific method for grinding and polishing step-by-step thinning comprises the following steps:
1) grinding disc with abrasive grains of 9 μm is circularly polished to a sample introduction step length accumulated to be larger than 40 μm;
2) grinding and polishing a grinding disc with the diameter of 2 micrometers in a reciprocating and circulating manner until the accumulated sample introduction step length is more than 30 micrometers;
3) automatically feeding a grinding disc with the diameter of 0.5 mu m, and grinding and polishing the sample until the thickness of the sample is 15-20 mu m;
wherein the automatic sample feeding setting mode is as follows:
using formulas
D = a-b-c-20, where a is the original thickness of the sample; b is the accumulated step length of grinding and polishing of a grinding disc with the diameter of 9 mu m; c is the accumulated step length of grinding and polishing of a grinding disc with the diameter of 2 mu m,
calculating the difference between the initial sample thickness and the polished accumulated step length, and switching an automatic sample feeding mode to set an automatic sample feeding and grinding thickness value;
(4) in argon atmosphere, adopting an ion thinning instrument to carry out clockwise and anticlockwise rotation bombardment thinning perforation of double ion beams to obtain a thinned transmission electron microscope sample;
the specific method for the double-ion beam bombardment thinning perforation comprises the following steps:
1) performing ion beam clockwise rotation bombardment on the center of the sample for 1-2 min by adopting a voltage of 4.5-5 KeV and a double ion beam incident angle of +/-3 degrees, and then performing ion beam anticlockwise rotation bombardment for 1-2 min;
2) performing ion beam clockwise rotation bombardment on the center of the sample for 3-5 min by adopting a voltage of 3-3.5 KeV and a double ion beam incident angle of +/-5 degrees, and performing ion counterclockwise rotation bombardment for 3-5 min;
3) performing ion beam clockwise rotation bombardment on the center of the sample for 3-10 min by adopting a voltage of 1.5-2 KeV and a double ion beam incident angle of +/-8 degrees, and performing ion counterclockwise rotation bombardment for 3-10 min;
4) and (3) carrying out ion beam clockwise rotation bombardment on the center of the sample for 5-10 min by adopting a voltage of 0.8-1 KeV and a double ion beam incident angle of +/-10 degrees, and then adopting ion anticlockwise rotation bombardment for 5-10 min.
2. The transmission electron microscope sample preparation method of the high-plasticity precious metal material according to claim 1, wherein the method comprises the following steps: the thickness of the square metal sheet in the step (1) is 150-200 mu m.
3. The transmission electron microscope sample preparation method of the high-plasticity precious metal material according to claim 1, wherein the method comprises the following steps: and (3) the distance between the wafer samples in the step (2) is 4.5-6 mm.
4. The transmission electron microscope sample preparation method of the high-plasticity precious metal material according to claim 1, wherein the method comprises the following steps: and (4) grinding and polishing the steel plate in the step (3) to obtain the steel plate with the contact stress of 10-20N.
5. The transmission electron microscope sample preparation method of the high-plasticity precious metal material according to claim 1, wherein the method comprises the following steps: and (3) polishing the polishing flannelette at the rotating speed of 400-500 r/min.
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