CN108519396A - A kind of preparation method of ultra-thin section - Google Patents
A kind of preparation method of ultra-thin section Download PDFInfo
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- CN108519396A CN108519396A CN201810385243.XA CN201810385243A CN108519396A CN 108519396 A CN108519396 A CN 108519396A CN 201810385243 A CN201810385243 A CN 201810385243A CN 108519396 A CN108519396 A CN 108519396A
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- thin section
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—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 measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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Abstract
The present invention provides a kind of preparation method of ultra-thin section, includes the following steps：The target particles of extraction are fixed on the bucking ladder surface of resin；In the above-mentioned resin bucking ladder surface embeding resin for being fixed with target particles；Resin surface is accomplished into trapezoidal mesa-shaped after the resin solidification of the embedding, it is sliced using ultramicrotome, preparation method of the present invention prepares multi-disc ultra-thin section by individual particle, it can make full use of sample, only need a small amount of sample that a variety of characterizations to sample can be realized, the maximization of scientific achievement, ultra-thin section surface prepared by this method is contributed to not to have ion dam age, the TEM high resolution picture photos of high quality can be obtained.
Description
Technical field
The invention belongs to microscopic analysis field, the preparation method of specifically a kind of ultra-thin section.
Background technology
Transmission electron microscope (TEM) be it is accelerated and aggregation e-beam projection to very thin sample on, due to
The de Broglie wavelength of electronics is very short, and the resolution ratio of transmission electron microscope can reach 0.1~0.2nm.Therefore, using saturating
The fine structure of sample can be observed by penetrating electron microscope, it might even be possible to the structure for observing an only row atom.TEM requirements
Analyzed thickness of sample is less than 100nm, therefore the problem of TEM is applied to most critical in the research of the samples such as rock, mineral
It is exactly the preparation of ultra-thin sample.In addition, how to utilize sample few as possible for precious or rare sample (such as lunar soil, lunar dust)
Obtain the problem that most, more perfect scientific achievement is also very crucial.
At present there are mainly three types of the preparation methods of ultra-thin section：1, ion milling method-can prepare the non-original of bulk sample
The ultra-thin slice in position, part is not suitable for being thinned for single microparticle；2, focused ion beam-can be used for subtracting for individual particle
Thin, principle is to be degraded finally to obtain ultra-thin sample to sample surfaces by high energy ion beam, but it is for the damage of sample
Consumption is irreversible, and a particle is only capable of obtaining a piece of ultra-thin section, and the sheet surface being sliced has nano level amorphous
Layer, causes TEM high resolution pictures ineffective；3, ultramicrotome method-is used to prepare powder (combinations of a large amount of single microparticles)
The ultra-thin section of sample cannot prepare the ultra-thin section of individual particle, it is therefore necessary to which development is a kind of more by individual particle preparation
The new method of piece ultra-thin section.
Invention content
It is an object of the invention to solve above-mentioned problems of the prior art, a kind of preparation side of ultra-thin section is provided
Method, the preparation method can prepare multi-disc ultra-thin section by individual particle.
For achieving the above object, the technical solution adopted in the present invention is：
A kind of preparation method of ultra-thin section, includes the following steps：
(1) target particles of extraction are fixed on the bucking ladder surface of resin；
(2) in the above-mentioned resin bucking ladder surface embeding resin for being fixed with target particles；
(3) resin surface is accomplished into trapezoidal mesa-shaped after the resin solidification of the embedding, is sliced using ultramicrotome.
Preferably, grain size≤15 μm of the target particles.
Preferably, in step (1) when the particle in in-situ extraction bulk sample, the extracting method of the target particles
It is：The surface for the target particles selected on sample with Pt protections under focused ion beam, then uses focused ion beam in sample
Both ends are degraded, then are extracted target particles with nano-machine hand.
Preferably, in step (1) when extracting particle from powder sample, the extracting method of the target particles is：
Selected target particle in powder sample is extracted the target particles with nano-machine hand.
Preferably, in step (1) when sample is individual particle, the extracting method of the target particles is to use nano-machine
Hand extracts the sample particle.
Preferably, the fixing means of target particles described in step (1) is：The target particles are put with nano-machine hand
It sets on resin bucking ladder surface, then the target particles is welded on bucking ladder surface with Pt.
Preferably, the resin is low viscosity resin.
Preferably, the low viscosity resin is the mixture of tetra- kinds of resins of ERL4221, DER736, NAS and DMAE.
Preferably, the bucking ladder surface of the resin is that resin surface is accomplished trapezoidal mesa-shaped system with blade under the microscope
Standby.
The beneficial effects of the invention are as follows：Preparation method provided by the invention is to prepare multi-disc ultra-thin section by individual particle,
Sample is can make full use of, only needs a small amount of sample that a variety of characterizations to sample can be realized, contributes to the maximum of scientific achievement
Change；In addition, ultra-thin section surface prepared by this method does not have ion dam age, the TEM high resolution picture photos of high quality can be obtained.
Description of the drawings
The flow chart of Fig. 1 ultra-thin section preparation methods of the present invention；
The SEM photograph on the bucking ladder top of Fig. 2 resins；
The STEM photos of ultra-thin section prepared by Fig. 3；
The TEM photos (left side) and HRTEM photos (right side) of ultra-thin section prepared by Fig. 4.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear
Chu is fully described by, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without creative efforts
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
As shown in Figure 1, the preparation method of ultra-thin section of the present invention, includes the following steps：
1. under focused ion beam with Pt protection on bulk sample select target particles surface, then with focus from
Beamlet degrades at sample both ends, then is extracted target particles with nano-machine hand, after being placed on the bucking ladder surface of resin
Target particles are welded on bucking ladder surface with Pt；Grain size≤15 μm of the target particles；
2. in the above-mentioned resin bucking ladder surface embeding resin for being fixed with target particles；
3. resin surface is accomplished trapezoidal mesa-shaped after the resin solidification of the embedding, it is sliced using ultramicrotome.
The resin is low viscosity hybrid resin, is the mixture of tetra- kinds of resins of ERL4221, DER736, NAS and DMAE.
As shown in Fig. 2, the bucking ladder surface of the resin is that resin surface is accomplished bucking ladder with blade under the microscope
Prepared by shape.
Embodiment 2
As shown in Figure 1, the preparation method of ultra-thin section of the present invention, includes the following steps：
1. target particles are extracted with nano-machine hand, are placed on resin by the selected target particle in powder sample
Bucking ladder surface after target particles are welded on bucking ladder surface with Pt；Grain size≤15 μm of the target particles；
2. in the above-mentioned resin bucking ladder surface embeding resin for being fixed with target particles；
3. resin surface is accomplished trapezoidal mesa-shaped after the resin solidification of the embedding, it is sliced using ultramicrotome.
The resin is low viscosity hybrid resin, is the mixture of tetra- kinds of resins of ERL4221, DER736, NAS and DMAE.
As shown in Fig. 2, the bucking ladder surface of the resin is that resin surface is accomplished bucking ladder with blade under the microscope
Prepared by shape.
Prepared ultra-thin section can be used for STEM analyses (Fig. 3) and tem analysis, and the high-resolution that can obtain high quality shines
Piece (Fig. 4) can measure its spacing of lattice and obtain structural information；Prepared ultra-thin section can be additionally used in other analyses, such as Auger
Electron spectrum etc..
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features；
And these modifications or replacements, various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (9)
1. a kind of preparation method of ultra-thin section, which is characterized in that include the following steps：
(1) target particles of extraction are fixed on the bucking ladder surface of resin；
(2) in the above-mentioned resin bucking ladder surface embeding resin for being fixed with target particles；
(3) resin surface is accomplished into trapezoidal mesa-shaped after the resin solidification of the embedding, is sliced using ultramicrotome.
2. a kind of preparation method of ultra-thin section according to claim 1, which is characterized in that the grain size of the target particles
≤15μm。
3. a kind of preparation method of ultra-thin section according to claim 1, which is characterized in that carried when in situ in step (1)
When taking the particle in bulk sample, the extracting method of the target particles is：Under focused ion beam with Pt protections on sample
Then the surface of selected target particles is degraded with focused ion beam at sample both ends, then with nano-machine hand by target particles
It extracts.
4. a kind of preparation method of ultra-thin section according to claim 1, which is characterized in that when from powder in step (1)
When extracting particle in sample, the extracting method of the target particles is：The selected target particle in powder sample, uses nano-machine
Hand extracts the target particles.
5. a kind of preparation method of ultra-thin section according to claim 1, which is characterized in that when sample is in step (1)
When individual particle, the extracting method of the target particles is to be extracted the sample microparticle with nano-machine hand.
6. a kind of preparation method of ultra-thin section according to claim 1, which is characterized in that target described in step (1)
The fixing means of particle is：The target particles are placed on resin bucking ladder surface with nano-machine hand, then with Pt by institute
Target particles are stated to be welded on bucking ladder surface.
7. a kind of preparation method of ultra-thin section according to claim 1, which is characterized in that the resin is low viscosity tree
Fat.
8. a kind of preparation method of ultra-thin section according to claim 7, which is characterized in that the low viscosity resin is
The mixture of tetra- kinds of resins of ERL4221, DER736, NAS and DMAE.
9. a kind of preparation method of ultra-thin section according to claim 1, which is characterized in that the bucking ladder table of the resin
Face is that resin surface is accomplished trapezoidal mesa-shaped with blade under the microscope to prepare.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810385243.XA CN108519396A (en) | 2018-04-26 | 2018-04-26 | A kind of preparation method of ultra-thin section |
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| CN201810385243.XA CN108519396A (en) | 2018-04-26 | 2018-04-26 | A kind of preparation method of ultra-thin section |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109141959A (en) * | 2018-11-15 | 2019-01-04 | 甘肃农业大学 | A kind of potato tubers ultra-thin section production method for transmission electron microscope observing |
| CN112964775A (en) * | 2021-02-01 | 2021-06-15 | 中国地质大学（武汉） | Manufacturing method of target for LA-ICP-MS analysis |
| CN113109114A (en) * | 2021-04-14 | 2021-07-13 | 中山大学 | Pretreatment method for analyzing rare earth elements in apatite and detection method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101458180A (en) * | 2007-12-13 | 2009-06-17 | 中芯国际集成电路制造(上海)有限公司 | Method for preprocessing TEM example and carrying out TEM test for example |
| CN103558055A (en) * | 2013-09-29 | 2014-02-05 | 中国疾病预防控制中心病毒病预防控制所 | Positioning ultrathin slice method for pathologic cell infected with virus |
| CN105571912A (en) * | 2015-10-16 | 2016-05-11 | 中南大学 | Method for cutting flexible materials into ultrathin slices at normal temperatures |
| CN107941832A (en) * | 2017-10-26 | 2018-04-20 | 中国科学院地质与地球物理研究所 | A kind of preparation method of micron order pre solar grain transmission electron microscope sample |
| CN105865862B (en) * | 2016-03-25 | 2018-12-14 | 江苏省沙钢钢铁研究院有限公司 | A kind of preparation method of three-dimensional atom probe sample |
-
2018
- 2018-04-26 CN CN201810385243.XA patent/CN108519396A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101458180A (en) * | 2007-12-13 | 2009-06-17 | 中芯国际集成电路制造(上海)有限公司 | Method for preprocessing TEM example and carrying out TEM test for example |
| CN103558055A (en) * | 2013-09-29 | 2014-02-05 | 中国疾病预防控制中心病毒病预防控制所 | Positioning ultrathin slice method for pathologic cell infected with virus |
| CN105571912A (en) * | 2015-10-16 | 2016-05-11 | 中南大学 | Method for cutting flexible materials into ultrathin slices at normal temperatures |
| CN105865862B (en) * | 2016-03-25 | 2018-12-14 | 江苏省沙钢钢铁研究院有限公司 | A kind of preparation method of three-dimensional atom probe sample |
| CN107941832A (en) * | 2017-10-26 | 2018-04-20 | 中国科学院地质与地球物理研究所 | A kind of preparation method of micron order pre solar grain transmission electron microscope sample |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109141959A (en) * | 2018-11-15 | 2019-01-04 | 甘肃农业大学 | A kind of potato tubers ultra-thin section production method for transmission electron microscope observing |
| CN112964775A (en) * | 2021-02-01 | 2021-06-15 | 中国地质大学（武汉） | Manufacturing method of target for LA-ICP-MS analysis |
| CN112964775B (en) * | 2021-02-01 | 2022-05-31 | 中国地质大学（武汉） | Manufacturing method of target for LA-ICP-MS analysis |
| CN113109114A (en) * | 2021-04-14 | 2021-07-13 | 中山大学 | Pretreatment method for analyzing rare earth elements in apatite and detection method thereof |
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