CN110231355B - Method for preparing micron-sized metal powder transmission electron microscope film sample - Google Patents
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- 239000000843 powder Substances 0.000 title claims abstract description 76
- 230000005540 biological transmission Effects 0.000 title claims abstract description 57
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 15
- 239000002184 metal Substances 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000011812 mixed powder Substances 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000007731 hot pressing Methods 0.000 claims abstract description 9
- 208000032369 Primary transmission Diseases 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 238000010884 ion-beam technique Methods 0.000 claims description 6
- 238000009461 vacuum packaging Methods 0.000 claims description 6
- 230000001133 acceleration Effects 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 16
- 238000002360 preparation method Methods 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 10
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 238000007789 sealing Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 50
- 238000005516 engineering process Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 3
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- 239000007788 liquid Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G01N23/02—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 transmitting the radiation through the material
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- 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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Abstract
A method for preparing a micron-sized metal powder transmission electron microscope film sample comprises the following steps: (1) mixing the powder to be detected with elemental tin powder; (2) placing the mixed powder prepared in the step (1) in a drying oven for drying and deoxidizing, then naturally cooling to room temperature, and sealing and storing in vacuum; (3) hot-pressing and sintering the mixed powder prepared in the step (2), releasing pressure, naturally cooling to room temperature, cutting the mixed powder block to obtain a primary transmission sample, and thinning; (4) placing the sample prepared in the step (3) into an ion thinning instrument according to the requirements of the transmission electron microscope film sample for final thinning until small holes appear in the sample, and obtaining the transmission electron microscope film sample for observing the micron-sized powder tissue structure; the transmission sample prepared by the method can effectively solve the bottleneck of powder agglomeration, and the success rate of sample preparation is extremely high, so that a novel preparation method is provided for preparing transmission electron microscope samples from metal powder materials with different micron particle sizes and different types.
Description
Technical Field
The invention relates to a preparation method of a transmission electron microscope observation and analysis sample, in particular to a method for preparing a micron-sized metal powder transmission electron microscope film sample.
Background
In the manufacture of alloy materials, there are various inspection devices that characterize the microstructure of the material, such as scanning electron microscopes, transmission electron microscopes, X-ray diffraction, electron probes, and the like. The detection devices can well reveal the microscopic morphology, the structure and the phase composition of the material. The transmission electron microscope is an important analysis means for detecting the structure of the material, and has the greatest advantage of high resolution and capability of observing the organization and the structure of a micro-area of the material. The preparation of the transmission sample is an important link of the transmission electron microscope analysis technology.
At present, bulk transmission electron microscope sample preparation and nano-scale powder transmission electron microscope film sample preparation are simple and mature, but the transmission electron microscope sample preparation of micron-scale powder particles is difficult, especially the observation of the internal organization structure of the micron-scale powder particles is required, one of the preparation difficulties of the micron-scale powder particle transmission electron microscope sample is that the micron-scale powder particles are larger than the nano-scale size and are easy to sink during dispersion, suspension liquid is difficult to form according to the dispersion of common powder samples, and the suspension liquid is difficult to be fished by a copper support film; the second difficulty is that the powder particles are easy to agglomerate and difficult to disperse uniformly, so that the thickness of the fished powder particles is large, and the electron beam of the transmission electron microscope cannot penetrate through the powder (generally, the electron beam penetration capacity of the transmission electron microscope is 100nm to 200 nm). Therefore, a new method for preparing a micron-sized metal powder transmission electron microscope film sample is needed to be explored so as to further characterize the organization structure inside the powder particles.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a method for preparing a micron-sized metal powder transmission electron microscope film sample, the transmission sample prepared by the method can effectively solve the bottleneck of powder agglomeration, and the success rate of sample preparation is extremely high, so that a novel preparation method is provided for preparing transmission electron microscope samples from metal powder materials with different micron particle sizes and different types.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a micron-sized metal powder transmission electron microscope film sample comprises the following steps:
(1) the purity of the single tin powder is more than or equal to 99%, the granularity of the single tin powder is 15-75 mu m, the micron-sized powder to be detected and the single tin powder are prepared according to the volume ratio of 1: 1-1: 5, and the micron-sized powder to be detected and the single tin powder are placed in a three-dimensional powder mixer to be uniformly mixed for 6-10 hours;
(2) putting the mixed powder prepared in the step (1) into a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-1～1×10-2Pa, the temperature is 60-80 ℃, the time is 4-6 h, then the natural cooling is carried out to the room temperature, and the vacuum packaging and the storage are carried out;
(3) hot-pressing and sintering the mixed powder prepared in the step (2) for 0.5-1.5 h under the conditions that the pressure is 150-400 MPa and the temperature is 170-210 ℃, releasing the pressure and naturally cooling to room temperature after sintering is finished to obtain a mixed powder block, cutting the mixed powder block to obtain a primary transmission sample, and mechanically reducing the thickness of the sample to 100-200 mu m;
(4) and (3) preparing the sample prepared in the step (3) into a wafer with the diameter of 3mm according to the requirements of the transmission electron microscope film sample, placing the wafer into an ion thinning instrument for final thinning, wherein the acceleration voltage is 4-6 kV, the inclination angle of an ion beam and a vertical surface is 5-12 degrees, and the transmission electron microscope film sample for observing the micron-sized powder tissue structure can be obtained until small holes appear in the sample.
And (4) if the sample after mechanical thinning is fragile or small, sticking the sample to a circular copper ring or molybdenum ring with the diameter of 3mm, and then putting the sample into an ion thinning instrument.
The invention has the advantages and innovations that:
uniformly dispersing the powder by using a three-dimensional powder mixer, and mechanically occluding the target powder to be detected and the tin by using a low-temperature hot-pressing technology. The transmission sample prepared by the method can effectively solve the bottleneck of powder agglomeration, and the success rate of sample preparation is extremely high. Thereby providing a new preparation method for preparing transmission electron microscope samples from metal powder materials with different micron particle sizes and different types.
The invention also has the following advantages:
(1) compared with the solidification powder materials such as rubber powder, resin and the like, the solidification powder material selected by the method is a tin metal simple substance with a low melting point, so that the influence of the melting of the solidification material on the imaging quality can be effectively avoided;
(2) the mechanical occlusion of the powder to be detected and tin under the low-temperature condition is realized by means of a hot-pressing sintering technology, the change of the target powder state is avoided, the method is particularly suitable for preparing the low-phase-transition-temperature powder transmission sample (such as amorphous powder with low phase transition temperature), and the preparation requirements of some special powder transmission samples can be met.
Drawings
FIG. 1 is an image of a bulk of a tin solidification target powder of an example.
FIG. 2 is a Transmission Electron Microscope (TEM) bright field image of an embodiment.
Fig. 3 is an image of a bulk of example tin-curing target powder.
FIG. 4 is a bright field image of a Transmission Electron Microscope (TEM) according to the second embodiment.
Fig. 5 is an image of a bulk of the tin solidification target powder of example three.
FIG. 6 is a bright field image of a three-Transmission Electron Microscope (TEM) according to an example.
Detailed Description
The key point of the powder transmission electron microscope sample prepared by the invention is to select proper metal element types to solidify powder, the core of the preparation method is to combine the preparation of the powder transmission electron microscope sample with a low-temperature consolidation technology, realize the mechanical occlusion of tin element by a low-temperature sintering technology, and obtain the transmission electron microscope sample with uniform powder by mechanical grinding and ion thinning.
The present invention will now be described in detail by way of examples and figures, which are illustrative of the invention and not limiting.
Example one
The embodiment comprises the following steps:
1. the purity of the elemental tin powder is more than or equal to 99%, the granularity of the elemental tin powder is 15-75 micrometers, and the micron-sized powder to be detected and the elemental tin powder are prepared according to the volume ratio of 1: 1. Placing the mixture into a three-dimensional powder mixer for mixing for 6 hours;
2. putting the mixed powder prepared in the step (1) into a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-1～1×10-2Pa, 60 ℃ and 4 h. Naturally cooling to room temperature, and vacuum packaging and storing;
3. hot-pressing and sintering the mixed powder prepared in the step (2) for 0.5h under the conditions that the pressure is 150MPa and the temperature is 210 ℃, releasing the pressure after sintering is finished, and naturally cooling to room temperature to obtain a mixed powder block, wherein the mixed powder block is shown in figure 1; cutting the mixed powder block to obtain a primary transmission sample, and mechanically reducing the thickness of the sample to 100-130 mu m;
4. preparing the mechanical thinning sample prepared in the step (3) into a wafer with the diameter of 3mm according to the requirements of a transmission electron microscope film sample, pasting the wafer onto a circular copper ring with the diameter of 3mm, putting the wafer into an ion thinning instrument, wherein the accelerating voltage is 4kV, the inclination angle of an ion beam and a vertical surface is 5-8 degrees until small holes appear in the sample, and obtaining the transmission electron microscope sample for observing the micron-sized powder tissue structure;
5. and (3) observing the transmission electron microscope sample prepared in the step (4) under a transmission electron microscope to obtain a TEM (transmission electron microscope) picture of the tissue morphology inside the powder particles, wherein as shown in FIG. 2, the powder particles are uniformly distributed on the tin matrix.
Example two
The embodiment comprises the following steps:
1. the purity of the elemental tin powder is more than or equal to 99 percent, and the granularity is 15-75 um. Preparing micron-sized powder to be detected and elemental tin powder according to the volume ratio of 1:3, and placing the micron-sized powder and the elemental tin powder into a three-dimensional powder mixer for mixing for 8 hours;
2. putting the mixed powder prepared in the step (1) into a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-1～1×10-2Pa, the temperature is 70 ℃, the time is 5 hours, then the mixture is naturally cooled to the room temperature, and the vacuum packaging and the storage are carried out;
3. hot-pressing and sintering the mixed powder prepared in the step (2) for 1h under the conditions that the pressure is 300MPa and the temperature is 190 ℃, releasing the pressure after sintering is completed, naturally cooling to room temperature to obtain a mixed powder block, cutting the mixed powder block to obtain a primary transmission sample as shown in figure 3, and mechanically grinding the thickness of the sample to 130-160 mu m;
4. and (4) preparing the mechanical thinning sample prepared in the step (3) into a wafer with the diameter of 3mm according to the requirements of the transmission electron microscope film sample, pasting the wafer onto a circular copper ring with the diameter of 3mm, putting the wafer into an ion thinning instrument, wherein the acceleration voltage is 5kV, the inclination angle of an ion beam and a vertical surface is 5-10 degrees until small holes appear in the sample, and obtaining the transmission electron microscope sample for observing the micron-sized powder tissue structure.
5. And (3) observing the transmission electron microscope sample prepared in the step (4) under a transmission electron microscope to obtain a TEM (transmission electron microscope) picture of the tissue morphology inside the powder particles, wherein as shown in FIG. 4, the powder particles are uniformly distributed on the tin matrix.
EXAMPLE III
The embodiment comprises the following steps:
1. the purity of the elemental tin powder is more than or equal to 99 percent, and the granularity is 15-75 um. Preparing micron-sized powder to be detected and elemental tin powder according to the volume ratio of 1:5, and placing the micron-sized powder and the elemental tin powder into a three-dimensional powder mixer for mixing for 10 hours;
2. mixing the mixture prepared in the step (1)Placing the powder in a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-1～1×10-2Pa, the temperature is 80 ℃, the time is 6 hours, then the mixture is naturally cooled to the room temperature, and the vacuum packaging and the storage are carried out;
3. hot-pressing and sintering the mixed powder prepared in the step (2) for 1.5h under the conditions that the pressure is 400MPa and the temperature is 180 ℃, releasing the pressure after sintering is finished, naturally cooling to room temperature to obtain a mixed powder block, cutting the mixed powder block to obtain a primary transmission sample as shown in figure 5, and mechanically grinding the thickness of the sample to 160-200 mu m;
4. preparing the mechanical thinning sample prepared in the step (3) into a wafer with the diameter of 3mm according to the requirements of a transmission electron microscope film sample, pasting the wafer onto a circular copper ring with the diameter of 3mm, putting the wafer into an ion thinning instrument, wherein the acceleration voltage of the ion thinning instrument is 6kV, and the inclination angle between an ion beam and a vertical surface is 7-12 degrees until small holes appear in the sample, so that a transmission electron microscope sample for observing a micron-sized powder tissue structure can be obtained;
5. and (3) observing the transmission electron microscope sample prepared in the step (4) under a transmission electron microscope to obtain a TEM (transmission electron microscope) picture of the tissue morphology inside the powder particles, wherein as shown in FIG. 6, the powder particles are uniformly distributed on the tin matrix.
The foregoing is only a result of the preferred embodiments of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (3)
1. A method for preparing a micron-sized metal powder transmission electron microscope film sample is characterized by comprising the following steps:
(1) the purity of the single tin powder is more than or equal to 99%, the granularity of the single tin powder is 15-75 mu m, the micron-sized powder to be detected and the single tin powder are prepared according to the volume ratio of 1: 1-1: 5, and the micron-sized powder to be detected and the single tin powder are placed in a three-dimensional powder mixer to be uniformly mixed for 6-10 hours;
(2) placing the mixed powder prepared in the step (1) in a drying ovenPerforming dry deoxidation, wherein the vacuum degree is 1 × 10-1～1×10-2Pa, the temperature is 60-80 ℃, the time is 4-6 h, then the natural cooling is carried out to the room temperature, and the vacuum packaging and the storage are carried out;
(3) hot-pressing and sintering the mixed powder prepared in the step (2) for 0.5-1.5 h under the conditions that the pressure is 150-400 MPa and the temperature is 170-210 ℃, releasing the pressure and naturally cooling to room temperature after sintering is finished to obtain a mixed powder block, cutting the mixed powder block to obtain a primary transmission sample, and mechanically reducing the thickness of the sample to 100-200 mu m;
(4) and (3) preparing the sample prepared in the step (3) into a wafer with the diameter of 3mm according to the requirements of the transmission electron microscope film sample, placing the wafer into an ion thinning instrument for final thinning, wherein the acceleration voltage is 4-6 kV, the inclination angle of an ion beam and a vertical surface is 5-12 degrees, and the transmission electron microscope film sample for observing the micron-sized powder tissue structure can be obtained until small holes appear in the sample.
2. The method for preparing micron-sized metal powder transmission electron microscope film samples according to claim 1, wherein in the step (4), if the mechanically thinned samples are brittle or small, the samples are pasted on a circular copper ring or a molybdenum ring with the diameter of 3mm and then placed in an ion thinning instrument.
3. The method for preparing micron-sized metal powder transmission electron microscope film samples according to claim 1, characterized by comprising the following steps:
(1) the purity of the single tin powder is more than or equal to 99%, and the granularity of the single tin powder is 15-75 um; preparing micron-sized powder to be detected and elemental tin powder according to the volume ratio of 1:3, and placing the micron-sized powder and the elemental tin powder into a three-dimensional powder mixer for mixing for 8 hours;
(2) putting the mixed powder prepared in the step (1) into a drying oven for drying and deoxidizing, wherein the vacuum degree is 1 × 10-1～1×10-2Pa, the temperature is 70 ℃, and the time is 5 h; naturally cooling to room temperature, and vacuum packaging and storing;
(3) hot-pressing and sintering the mixed powder prepared in the step (2) for 1h under the conditions that the pressure is 300MPa and the temperature is 190 ℃, releasing the pressure after sintering is finished, naturally cooling to room temperature to obtain a mixed powder block, cutting the mixed powder block to obtain a primary transmission sample, and mechanically grinding the thickness of the sample to 130-160 mu m;
(4) preparing the mechanical thinning sample prepared in the step (3) into a wafer with the diameter of 3mm according to the requirements of a transmission electron microscope film sample, pasting the wafer onto a circular copper ring with the diameter of 3mm, putting the wafer into an ion thinning instrument, wherein the accelerating voltage is 5kV, and the inclination angle of an ion beam and a vertical surface is 5-10 degrees; and obtaining the transmission electron microscope sample for observing the microstructure of the micron-sized powder until a small hole appears in the sample.
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| CN111982948A (en) * | 2020-08-27 | 2020-11-24 | 矿冶科技集团有限公司 | Preparation method of scanning electron microscope section sample of micron-sized powder |
| CN112098446B (en) * | 2020-11-09 | 2021-03-05 | 矿冶科技集团有限公司 | Characterization method for radius-thickness ratio of flaky powder material |
| CN113009185A (en) * | 2021-04-25 | 2021-06-22 | 中国科学院物理研究所 | Preparation method of micron-sized powder sample of transmission electron microscope |
| CN113804707B (en) * | 2021-08-27 | 2023-07-14 | 西安理工大学 | Method for preparing high-density powder particle transmission electron microscope sample by film support |
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