CN110231355A - A method of preparing micro-sized metal powder transmission electron microscope film sample - Google Patents
A method of preparing micro-sized metal powder transmission electron microscope film sample Download PDFInfo
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- CN110231355A CN110231355A CN201910520529.9A CN201910520529A CN110231355A CN 110231355 A CN110231355 A CN 110231355A CN 201910520529 A CN201910520529 A CN 201910520529A CN 110231355 A CN110231355 A CN 110231355A
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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
- G01N23/04—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 and forming images of 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 of preparing micro-sized metal powder transmission electron microscope film sample, comprising the following steps: (1), by powder to be detected with simple substance glass putty mix；(2), mixed-powder made from step (1) is placed in drying box and deoxidation is dried, later cooled to room temperature, vacuum preservation；(3), by mixed-powder hot pressed sintering made from step (2), release and cooled to room temperature, mixed-powder bulk is cut, obtains primary transmission sample, and be thinned；(4), sample made from step (3) is put into Ion Beam Thinner by transmission electron microscope film sample requirement and is finally thinned, until occur in sample aperture to get to observation micron powder institutional framework transmission electron microscope film sample；The transmissive test of this method preparation can efficiently solve the bottleneck of powder reunion, and sample is prepared into that power is high, so that preparing transmission electron microscope sample for different micron granularities, different types of metal powder material provides the new preparation method of one kind.
Description
Technical field
The present invention relates to the preparation methods of transmission electron microscope observing analysis sample, and in particular to a kind of to prepare micro-sized metal powder
The method of last transmission electron microscope film sample.
Background technique
In the manufacture of alloy material, there are the detection devices of various characterization material microstructures, and for example scanning electron is aobvious
Micro mirror, transmission electron microscope, X-ray diffraction, electron probe etc..These detection devices can disclose the microcosmic of material well
Pattern, structure and object phase composition.And a kind of analysis means of the transmission electron microscope as important detection material structure, most
Big advantage is that have high resolution ratio, the tissue and structure of observable material domain.Wherein the preparation of transmission sample is transmission
An important link of electrical microscope analysis.
For at present, the preparation of bulk transmission electron microscope sample and the preparation of nanometer grade powder transmission electron microscope film sample are more simple
It is single, mature, but the transmission electron microscope sample preparation of micron powder particle is more difficult, especially to observe micron powder particle
Internal institutional framework, the preparation difficult point of this micron powder particle transmission electron microscope sample first is that micron powder particle compared with
Nano-grade size is big, is easy in dispersion, is hardly formed suspension according to common powder sample dispersion, is difficult by copper branch
Support film is fished for；Difficult point second is that powder particle be easy reunite, it is difficult to it is evenly dispersed so that the powder particle thickness fished for is big, thoroughly
The electron beam of radio mirror cannot penetrate powder (electron beam penetration capacity 100nm to the 200nm of general transmission electron microscope).Therefore, have
Necessity explores a kind of new method for preparing micro-sized metal powder transmission electron microscope film sample, to further characterize powder
The institutional framework in intragranular portion.
Summary of the invention
In view of problem of the prior art, micro-sized metal powder transmission electron microscope is prepared the purpose of the present invention is to provide a kind of
The transmissive test of the method for film sample, this method preparation can efficiently solve the bottleneck of powder reunion, and sample is successfully prepared
Rate is high, so that preparing transmission electron microscope sample for different micron granularities, different types of metal powder material provides one kind newly
Preparation method.
In order to achieve the above objectives, The technical solution adopted by the invention is as follows:
A method of preparing micro-sized metal powder transmission electron microscope film sample, comprising the following steps:
(1), >=99.% by simple substance glass putty purity, granularity is 15~75 μm, micron order powder to be detected and simple substance tin
Powder is prepared according to volume ratio 1:1~1:5, and is placed it in 6~10h of progress in three-dimensional mixed powder machine and uniformly mixed；
(2), mixed-powder made from step (1) is placed in drying box and deoxidation is dried, wherein vacuum degree is 1 × 10-1
~1 × 10-2Pa, temperature are 60~80 DEG C, and the time is 4~6h, later cooled to room temperature, and Vacuum Package saves；
(3), by mixed-powder made from step (2) in the condition that pressure is 150~400MPa, temperature is 170~210 DEG C
0.5~1.5h of lower hot pressed sintering, release and cooled to room temperature, obtain mixed-powder bulk, to mixed powder after the completion of sintering
Last bulk is cut, and obtains primary transmission sample, and by the thickness of sample mechanical reduction to 100~200 μm；
(4), the disk that diameter is 3mm is made according to transmission electron microscope film sample requirement in sample made from step (3) to put
Entering in Ion Beam Thinner and is finally thinned, acceleration voltage is 4~6kV, and the inclination angle of ion beam and vertical plane is 5~12 °,
Until occurring aperture in sample, the transmission electron microscope film sample of observation micron powder institutional framework can be obtained.
Sample is pasted the circle of diameter 3mm if the sample after mechanical reduction is more crisp or smaller by the step (4)
On shape copper ring or molybdenum ring, place into Ion Beam Thinner.
There is the present invention beneficial effect and innovation to be:
It is completely newly evenly dispersed to powder progress by the mixed powder machine of three-dimensional, pass through low temperature and pressure technology and realizes object to be measured powder
The mechanical snap at end and tin.The transmissive test of this method preparation can efficiently solve the bottleneck of powder reunion, and sample is prepared into
Power is high.One kind is provided to prepare transmission electron microscope sample for different micron granularities, different types of metal powder material
New preparation method.
It also have the advantage that
(1) compared to curing powders materials such as rubber powder, resins, the consolidated powder materials that this method is selected are Sillim of low melting point
Belong to simple substance, it is possible to prevente effectively from curing materials melt the influence to image quality；
(2) mechanical snap that powder and tin to be detected under cryogenic conditions are realized by hot pressing and sintering technique, avoids mesh
The change for marking pulverulence is particularly suitable for the preparation of low phase transition temperature powder transmissive test (as with low phase transition temperature
Amorphous powder), it can satisfy the demand of certain special powder transmissive test preparations.
Detailed description of the invention
Fig. 1 is one tin of embodiment solidification target powder bulk image.
Fig. 2 is one transmission electron microscope of embodiment (TEM) bright field image.
Fig. 3 is two tin of embodiment solidification target powder bulk image.
Fig. 4 is two transmission electron microscope of embodiment (TEM) bright field image.
Fig. 5 is three tin of embodiment solidification target powder bulk image.
Fig. 6 is three transmission electron microscope of embodiment (TEM) bright field image.
Specific embodiment
Powder transmission electron microscope sample prepared by the present invention, key are to select suitable metallic element type solidification powder
End, the core of preparation method is to prepare powder transmission electron microscope sample to be combined with low-temperature concretion technology, passes through low-temperature sintering
Technology realizes tin element mechanical snap, then obtains the uniform transmission electron microscope sample of powder by mechanical lapping, ion milling.
It elaborates below with embodiment and attached drawing to the present invention, described is explanation of the invention, rather than is limited.
Embodiment one
The present embodiment the following steps are included:
1, >=99.% by simple substance glass putty purity, granularity is 15~75um, micron order powder to be detected and simple substance glass putty
It is prepared according to volume ratio 1:1 at end.And it places it in three-dimensional mixed powder machine and carries out 6h mixing；
2, mixed-powder made from step (1) is placed in drying box and deoxidation is dried, wherein vacuum degree is 1 × 10-1~1
×10-2Pa, temperature are 60 DEG C, time 4h.Cooled to room temperature later, Vacuum Package save；
3, by mixed-powder made from step (2) under conditions of pressure is 150MPa, temperature is 210 DEG C hot pressed sintering
0.5h, release and cooled to room temperature, obtain mixed-powder bulk, as shown in Figure 1 after the completion of sintering；To mixed-powder bulk
It is cut, obtains primary transmission sample, and by the thickness of sample mechanical reduction to 100~130 μm；
4, mechanical reduction sample made from step (3) is required that diameter is made to be 3mm's according to transmission electron microscope film sample
Disk pastes in the circular copper rings of diameter 3mm, is put into Ion Beam Thinner, acceleration voltage 4kV, ion beam and vertical plane
Inclination angle is 5~8 °, and until occurring aperture in sample, the transmission electron microscope examination of observation micron powder institutional framework can be obtained
Sample；
5, transmission electron microscope sample made from step (4) is put under transmission electron microscope and is observed, powder particle can be obtained
Internal tissue topography's TEM photo, as shown in Fig. 2, as seen from the figure, powder particle is uniformly distributed in tin matrix, the invention
Method has achieved the purpose that prepare micro-sized metal powder transmission electron microscope film sample.
Embodiment two
The present embodiment the following steps are included:
1, >=99.% by simple substance glass putty purity, granularity is 15~75um.Micron order powder to be detected and simple substance glass putty
End is prepared according to volume ratio 1:3, and is placed it in three-dimensional mixed powder machine and carried out 8h mixing；
2, mixed-powder made from step (1) is placed in drying box and deoxidation is dried, wherein vacuum degree is 1 × 10-1~1
×10-2Pa, temperature are 70 DEG C, time 5h, later cooled to room temperature, and Vacuum Package saves；
3, by mixed-powder made from step (2) under conditions of pressure is 300MPa, temperature is 190 DEG C hot pressed sintering
1h, release and cooled to room temperature after the completion of sintering, obtains mixed-powder bulk, as shown in figure 3, to mixed-powder bulk into
Row cutting obtains primary transmission sample, and by the thickness of sample mechanical lapping to 130~160 μm；
4, mechanical reduction sample made from step (3) is required that diameter is made to be 3mm's according to transmission electron microscope film sample
Disk pastes in the circular copper rings of diameter 3mm, is put into Ion Beam Thinner, acceleration voltage 5kV, ion beam and vertical plane
Inclination angle is 5~10 °, and until occurring aperture in sample, the transmission electron microscope examination of observation micron powder institutional framework can be obtained
Sample.
5, transmission electron microscope sample made from step (4) is put under transmission electron microscope and is observed, powder particle can be obtained
Internal tissue topography's TEM photo, as shown in figure 4, as seen from the figure, powder particle is uniformly distributed in tin matrix, the invention
Method has achieved the purpose that prepare micro-sized metal powder transmission electron microscope film sample.
Embodiment three
The present embodiment the following steps are included:
1, >=99.% by simple substance glass putty purity, granularity is 15~75um.Micron order powder to be detected and simple substance glass putty
End is prepared according to volume ratio 1:5, and is placed it in three-dimensional mixed powder machine and carried out 10h mixing；
2, mixed-powder made from step (1) is placed in drying box and deoxidation is dried, wherein vacuum degree is 1 × 10-1~1
×10-2Pa, temperature are 80 DEG C, time 6h, later cooled to room temperature, and Vacuum Package saves；
3, by mixed-powder made from step (2) under conditions of pressure is 400MPa, temperature is 180 DEG C hot pressed sintering
1.5h, release and cooled to room temperature, obtain mixed-powder bulk, as shown in figure 5, to mixed-powder bulk after the completion of sintering
It carries out cutting and obtains primary transmission sample, and by the thickness of sample mechanical lapping to 160~200 μm；
4, mechanical reduction sample made from step (3) is required that diameter is made to be 3mm's according to transmission electron microscope film sample
Disk pastes in the circular copper rings of diameter 3mm, is put into Ion Beam Thinner, acceleration voltage 6kV, ion beam and vertical plane
Inclination angle is 7~12 °, and until occurring aperture in sample, the transmission electron microscope examination of observation micron powder institutional framework can be obtained
Sample；
5, transmission electron microscope sample made from step (4) is put under transmission electron microscope and is observed, powder particle can be obtained
Internal tissue topography's TEM photo, as shown in fig. 6, as seen from the figure, powder particle is uniformly distributed in tin matrix, the invention
Method has achieved the purpose that prepare micro-sized metal powder transmission electron microscope film sample.
What said above is only the result that the present invention is preferably implemented, it is noted that for those skilled in the art,
Without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.
Claims (3)
1. a kind of method for preparing micro-sized metal powder transmission electron microscope film sample, which comprises the following steps:
(1), >=99.% by simple substance glass putty purity, granularity is 15~75 μm, micron order powder to be detected and simple substance tin powder
It is prepared according to volume ratio 1:1~1:5, and places it in 6~10h of progress in three-dimensional mixed powder machine and uniformly mix；
(2), mixed-powder made from step (1) is placed in drying box and deoxidation is dried, wherein vacuum degree is 1 × 10-1~1 ×
10-2Pa, temperature are 60~80 DEG C, and the time is 4~6h, later cooled to room temperature, and Vacuum Package saves；
(3), mixed-powder made from step (2) is warm under conditions of pressure is 150~400MPa, temperature is 170~210 DEG C
Pressure 0.5~1.5h of sintering, release and cooled to room temperature, obtain mixed-powder bulk, to mixed-powder block after the completion of sintering
Material is cut, and obtains primary transmission sample, and by the thickness of sample mechanical reduction to 100~200 μm；
(4), by sample made from step (3) according to transmission electron microscope film sample require be made diameter be 3mm disk be put into from
It being finally thinned in the thinned instrument of son, acceleration voltage is 4~6kV, and the inclination angle of ion beam and vertical plane is 5~12 °, until
Occur aperture in sample, the transmission electron microscope film sample of observation micron powder institutional framework can be obtained.
2. a kind of method for preparing micro-sized metal powder transmission electron microscope film sample according to claim 1, feature
It is, sample is pasted the round copper of diameter 3mm if the sample after mechanical reduction is more crisp or smaller by the step (4)
It is placed into Ion Beam Thinner on ring or molybdenum ring.
3. a kind of method for preparing micro-sized metal powder transmission electron microscope film sample according to claim 1, feature
It is, comprising the following steps:
(1), >=99.% by simple substance glass putty purity, granularity is 15~75um；Micron order powder to be detected and simple substance tin powder
It is prepared according to volume ratio 1:3, and places it in three-dimensional mixed powder machine and carry out 8h mixing；
(2), mixed-powder made from step (1) is placed in drying box and deoxidation is dried；Wherein vacuum degree is 1 × 10-1~1 ×
10-2Pa, temperature are 70 DEG C, time 5h；Cooled to room temperature later, Vacuum Package save；
(3), by mixed-powder made from step (2) under conditions of pressure is 300MPa, temperature is 190 DEG C hot pressed sintering 1h,
Release and cooled to room temperature, obtain mixed-powder bulk, cut to mixed-powder bulk after the completion of sintering, obtain just
Grade transmission sample, and by the thickness of sample mechanical lapping to 130~160 μm；
(4), mechanical reduction sample made from step (3) is required that the circle that diameter is 3mm is made according to transmission electron microscope film sample
Piece pastes in the circular copper rings of diameter 3mm, is put into Ion Beam Thinner, acceleration voltage 5kV, and ion beam and vertical plane incline
Oblique angle is 5~10 °；Until occurring aperture in sample, the transmission electron microscope sample of observation micron powder institutional framework can be obtained.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111521623A (en) * | 2020-04-28 | 2020-08-11 | 广西大学 | Method for improving sample preparation success rate of powder sample transmission electron microscope in-situ heating chip |
| 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 |
| CN112098446A (en) * | 2020-11-09 | 2020-12-18 | 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 |
| CN113804707A (en) * | 2021-08-27 | 2021-12-17 | 西安理工大学 | Method for preparing high-density powder particle transmission electron microscope sample by film support |
| CN113984468A (en) * | 2021-10-23 | 2022-01-28 | 深圳市美信咨询有限公司 | Loose metal sintered layer section observation method and ion grinding equipment |
| CN117213951A (en) * | 2023-11-07 | 2023-12-12 | 矿冶科技集团有限公司 | Preparation method of coal combustion fly ash transmission electron microscope sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111521623A (en) * | 2020-04-28 | 2020-08-11 | 广西大学 | Method for improving sample preparation success rate of powder sample transmission electron microscope in-situ heating chip |
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| CN112098446A (en) * | 2020-11-09 | 2020-12-18 | 矿冶科技集团有限公司 | Characterization method for radius-thickness ratio of flaky powder material |
| 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 |
| CN113804707A (en) * | 2021-08-27 | 2021-12-17 | 西安理工大学 | Method for preparing high-density powder particle transmission electron microscope sample by film support |
| 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 |
| CN113984468A (en) * | 2021-10-23 | 2022-01-28 | 深圳市美信咨询有限公司 | Loose metal sintered layer section observation method and ion grinding equipment |
| CN113984468B (en) * | 2021-10-23 | 2024-03-15 | 深圳市美信检测技术股份有限公司 | Loose metal sintered layer section observation method and ion grinding equipment |
| CN117213951A (en) * | 2023-11-07 | 2023-12-12 | 矿冶科技集团有限公司 | Preparation method of coal combustion fly ash transmission electron microscope sample |
| CN117213951B (en) * | 2023-11-07 | 2024-02-02 | 矿冶科技集团有限公司 | Preparation method of coal combustion fly ash transmission electron microscope sample |
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