CN105203360A - Preparing method for micron-order particle sample for transmission electron microscope (TEM) - Google Patents
Preparing method for micron-order particle sample for transmission electron microscope (TEM) Download PDFInfo
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- CN105203360A CN105203360A CN201510598641.6A CN201510598641A CN105203360A CN 105203360 A CN105203360 A CN 105203360A CN 201510598641 A CN201510598641 A CN 201510598641A CN 105203360 A CN105203360 A CN 105203360A
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Abstract
The invention discloses a preparing method for a micron-order particle sample for a TEM. The preparing method includes the steps that a groove is formed in a flat plate and then filled with curing adhesive mixed with micron-order particle sample bodies, the mixture is heated, cured, cooled and then taken out, and a sheet-shaped block sample is obtained; the two surfaces of the sheet-shaped block sample are manually grinded and polished on a sample support, and a sample sheet is obtained; then supporting rings are bound through curing and binding agents, heating is carried out, the sample support is removed, and meanwhile the supporting rings are cured and bound to the sample sheet; the sample is finished, ion thinning is finally carried out, and the micron-order particle sample for the TEM is obtained. According to the preparing method, an operation technology is simple, adopted sampling devices and adopted sampling technologies are mature, the sampling success rate is high, practicability is high, and the preparing method is suitable for preparing various micron-order particle samples.
Description
Technical field
The present invention relates to electron microscopic sample technology of preparing, be specifically related to a kind of preparation method of micron particles example of transmission electron microscope.
Background technology
Transmission electron microscope TEM utilizes the electron beam patterning penetrating sample, can with the resolution characteristic of atomic scale, there is provided many-sided information such as microstructure structure, composition of material, it obtains increasingly extensive application in many fields such as modern science, engineering and bio-medicals.Because the penetration capacity of electron beam is lower, TEM requires that sample is " transparent " for electron beam, and the thickness in usual sample observation region is to control to be advisable at below 100nm, and this brings certain difficulty to TEM sample preparation.
Method prepared by TEM sample is a lot, the information depending primarily on material type He will obtain.For nano-scale particle material, electron beam can penetrate sample, and therefore method for making sample is fairly simple.Conventional method for making sample gets a little sample, is placed in alcohol or other solvents, with dripping on supporting film or micro-grid after ultrasound wave dispersion, just can carry out tem observation after drying.And for micron particles sample, electron beam can not penetrate, the simple method for making sample of nano-scale particle cannot be adopted.Conventional method is investment, and key step is: mixed by particulate samples with epoxide-resin glue, is embedded in the copper pipe of external diameter 3mm, dicing sheet after solidification, then carry out grinding, pit, ion milling.This method for making sample more complicated, and often can form hole owing to there being bubble in the process being embedded into copper pipe at sample, this can affect follow-up ion milling and cause sample preparation failure.Ultrathin sectioning can also be selected in addition, but for harder micron particles sample, ultra-thin section often can be introduced stress and affect tem observation.Therefore, the existing complex technical process preparing micron particles TEM sample, sample preparation success ratio is low.
Summary of the invention
In order to solve the shortcoming that micron particles TEM sample exists in traditional sample making technology, in conjunction with the sampling in general TEM laboratory, the invention provides the preparation method of a kind of simple and fast, practical micron particles TEM sample, improve sample preparation success ratio simultaneously.
The object of the present invention is to provide a kind of preparation method of micron particles example of transmission electron microscope.
The preparation method of micron particles example of transmission electron microscope of the present invention, comprises the following steps:
1) for the preparation of the groove of solidified sample:
Flat board processes the groove for solidified sample, for subsequent use;
2) solidification process micron particles sample:
Micron particles sample to be tested is blended in equably solidification glue in, be then filled into step 1) in groove in, be then put on warm table and be heating and curing, after solidification, be cooled to room temperature, take out from groove, obtain the sheet block sample be cured;
3) grinding and polishing block sample:
By step 2) in the surface melt viscosity of sheet block sample that obtains on the special sample carrier of grinding TEM sample, carry out hand lapping and polishing, then similarly hand lapping and polishing are carried out to another surface, until thickness is below 30 microns, obtain sample sheet;
4) sticky supporting ring and finishing sample:
By step 3) in another surface curing adhesive of grinding and polished sample sheet be stained with one or more supporting ring, if be stained with multiple supporting ring, then be not in contact with each other between multiple supporting ring, then a surface hot melt adhesive is stained with sample carrier and the sample sheet that another surface cured binders is stained with supporting ring is put on warm table and heats, curing adhesive solidification thus by sample sheet and supporting ring strong bond, simultaneously, hotmelt melts thus sample sheet is separated with sample carrier, the sample sheet being bonded with supporting ring is taken off from sample carrier, with blade, sample sheet is cut according to supporting ring, obtain the sample sheet of one or more independently fritter of bonding supporting ring, then put into organic solution to soak, the hot melt adhesive on removing sample sheet surface, sample sheet is taken out again from organic solution, repair, redundance outside each supporting ring is cut away, obtain the sample sheet of one or more bonding supporting ring trimmed,
5) ion milling sample:
By step 4) in the sample sheet being bonded with supporting ring trimmed that obtains carry out ion milling, until pass an aperture at center, micron particles TEM sample can be obtained, thus carry out tem observation.
Wherein, in step 1) in, dull and stereotyped adopt not with the material of solidification glue bond, as teflon; The degree of depth of groove is between 1 ~ 3mm, and the radial dimension of groove is between 5 ~ 15mm.Solidification glue can adopt the one in G-1 epoxide-resin glue, G-2 epoxide-resin glue and M-bond610 glue.
In step 2) in, warm table is heating and curing more than 2 hours.
In step 4) in, be put into time that warm table heats between 3 ~ 8 minutes; The time of soaking in organic solution is between 20 ~ 40 minutes.
In step 5) in, the aperture of the aperture that ion milling goes out is relevant with the material type of ion milling instrument and micron order chip sample.
Advantage of the present invention:
The present invention first processes groove on flat board, then the solidification glue being mixed with micron particles sample is filled in groove and is heating and curing, take out after cooling, obtain sheet block sample, sample carrier carries out hand lapping to two surfaces of sheet block sample and polishing obtains sample sheet, then supporting ring is glued with cured binders, sample carrier is removed in heating, make supporting ring solidify is bonded on sample sheet simultaneously, trim sample again, finally carry out ion milling and obtain micron particles TEM sample; Preparation method of the present invention, operating procedure is simple, and the sample making apparatus of use and technology maturation, sample preparation success ratio is high, practical, is suitable for the preparation of multiple micron particles sample.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the preparation method of micron particles example of transmission electron microscope of the present invention;
Fig. 2 is the schematic diagram of the sample sheet of the bonding supporting ring trimmed obtained according to the preparation method of micron particles example of transmission electron microscope of the present invention, wherein, a () is the superincumbent schematic diagram of supporting ring, (b) is supporting ring schematic diagram below; Fig. 3 is the TEM image of the micron particles TEM sample obtained according to the preparation method of micron particles example of transmission electron microscope of the present invention, wherein, a () is the low power TEM bright field image of micron order carbon granule TEM sample, b () is the high power TEM bright field image of micron order carbon granule TEM sample, c () is corresponding SEAD style figure, (d) is corresponding energy spectrogram.
Embodiment
Below in conjunction with accompanying drawing, by embodiment, the present invention will be further described.
The preparation method of the micron particles example of transmission electron microscope of the present embodiment, as shown in Figure 1, comprises the following steps:
1) for the preparation of the groove of solidified sample:
Flat board processes the groove for solidified sample, dull and stereotyped employing polyfluortetraethylene plate, the diameter of groove is 10mm, and the degree of depth is 2mm, for subsequent use;
2) solidification process micron particles sample:
Micron order carbon granule sample to be tested is blended in G-1 epoxy resin cure glue equably, then be filled into step 1) in groove in, then be put on warm table, temperature is 130 DEG C and is heating and curing 2 hours, room temperature is cooled to after solidification, take out from groove, the diameter 10mm obtaining being cured, the disc-shaped block sample of thickness 2mm;
3) grinding and polishing block sample:
By step 2) in the surface paraffin of block sample that obtains adhere on the special sample carrier of grinding TEM sample, carry out hand lapping and polishing, then similarly hand lapping and polishing are carried out to another surface, until thickness is below 30 microns, obtain sample sheet;
4) sticky supporting ring and finishing sample:
By step 3) in gluing upper 3 the molybdenum supporting rings of a surface AB of grinding and polished sample sheet, be not in contact with each other between 3 supporting rings, supporting ring adopts the molybdenum supporting ring of external diameter 3.0mm internal diameter 1.0mm, then be put on warm table and heat 5 minutes, curing adhesive AB adhesive curing thus by sample sheet and molybdenum supporting ring strong bond, simultaneously, hot melt adhesive melted paraffin wax thus sample sheet is separated with sample carrier, the sample sheet of bonding molybdenum supporting ring is taken off from sample carrier, with blade, sample sheet is split according to supporting ring, form the sample sheet that 3 are independently bonded with the fritter of a molybdenum supporting ring, then put into organic solution acetone to soak 30 minutes, the paraffin on removing surface, sample sheet is taken out again from organic solution acetone, repair by the pointed portion of knife blade, redundance outside each supporting ring is cut away, obtain the sample sheet of the bonding molybdenum supporting ring that 3 trim,
5) ion milling sample:
By step 4) in the sample sheet of the bonding molybdenum supporting ring trimmed that obtains carry out ion milling, until pass an aperture at center, micron order carbon granule TEM sample can be obtained, thus carry out tem observation, as shown in Figure 2, micron particles TEM sample comprises supporting ring 1, sample sheet 2 and aperture 3.
Tem observation is carried out to the micron order carbon granule TEM sample that above-mentioned preparation method obtains, observations as shown in Figure 3, can find out, adopt above-mentioned preparation method, successfully can observe the shape appearance figure of micron particles and the electron diffraction pattern of correspondence, EDAX results confirms that this micron particles is carbon granule sample simultaneously.
It is finally noted that, the object publicizing and implementing mode is to help to understand the present invention further, but it will be appreciated by those skilled in the art that: without departing from the spirit and scope of the invention and the appended claims, various substitutions and modifications are all possible.Therefore, the present invention should not be limited to the content disclosed in embodiment, and the scope that the scope of protection of present invention defines with claims is as the criterion.
Claims (8)
1. a preparation method for micron particles example of transmission electron microscope, is characterized in that, described preparation method comprises the following steps:
1) for the preparation of the groove of solidified sample:
Flat board processes the groove for solidified sample, for subsequent use;
2) solidification process micron particles sample:
Micron particles sample to be tested is blended in equably solidification glue in, be then filled into step 1) in groove in, be then put on warm table and be heating and curing, after solidification, be cooled to room temperature, take out from groove, obtain the sheet block sample be cured;
3) grinding and polishing block sample:
By step 2) in the surface melt viscosity of sheet block sample that obtains on the special sample carrier of grinding TEM sample, carry out hand lapping and polishing, then similarly hand lapping and polishing are carried out to another surface, until thickness is below 30 microns, obtain sample sheet;
4) sticky supporting ring and finishing sample:
By step 3) in another surface curing adhesive of grinding and polished sample sheet be stained with one or more supporting ring, if be stained with multiple supporting ring, then be not in contact with each other between multiple supporting ring, then a surface hot melt adhesive is stained with sample carrier and the sample sheet that another surface cured binders is stained with supporting ring is put on warm table and heats, curing adhesive solidification thus by sample sheet and supporting ring strong bond, simultaneously, hotmelt melts thus sample sheet is separated with sample carrier, the sample sheet being bonded with supporting ring is taken off from sample carrier, with blade, sample sheet is cut according to supporting ring, obtain the fritter sample sheet of one or more independently bonding supporting ring, then put into organic solution to soak, the hot melt adhesive on removing sample sheet surface, sample sheet is taken out again from organic solution, repair, redundance outside each supporting ring is cut away, obtain the sample sheet of one or more bonding supporting ring trimmed,
5) ion milling sample:
By step 4) in the sample sheet being bonded with supporting ring trimmed that obtains carry out ion milling, until pass an aperture at center, micron particles TEM sample can be obtained, thus carry out tem observation.
2. preparation method as claimed in claim 1, is characterized in that, in step 1) in, described flat board adopt not with the material of solidification glue bond.
3. preparation method as claimed in claim 1, is characterized in that, in step 1) in, the degree of depth of described groove is between 1 ~ 3mm, and the radial dimension of groove is between 5 ~ 15mm.
4. preparation method as claimed in claim 1, is characterized in that, in step 2) in, warm table is heating and curing more than 2 hours.
5. preparation method as claimed in claim 1, is characterized in that, in step 4) in, be put into time that warm table heats between 3 ~ 8 minutes.
6. preparation method as claimed in claim 1, is characterized in that, in step 4) in, the time of soaking in organic solution is between 20 ~ 40 minutes.
7. preparation method as claimed in claim 2, is characterized in that, described flat board adopts polyfluortetraethylene plate.
8. preparation method as claimed in claim 1, is characterized in that, in step 1) in, described solidification glue can adopt the one in G-1 epoxide-resin glue, G-2 epoxide-resin glue and M-bond610 glue.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107271726A (en) * | 2017-07-19 | 2017-10-20 | 中南大学 | A kind of preparation method of mineral samplers piece |
| CN107607071A (en) * | 2017-09-26 | 2018-01-19 | 深圳市领先医疗服务有限公司 | The measuring method of coating of degradable medicaments coating bracket coating layer thickness |
| CN108169266A (en) * | 2017-11-09 | 2018-06-15 | 广东科技学院 | A kind of preparation method of the scanning electron microscope example of micron order ionic crystals powder |
| CN110487823A (en) * | 2019-08-13 | 2019-11-22 | 西安工业大学 | A kind of preparation method of powder particle tem specimen |
| CN110595848A (en) * | 2018-06-12 | 2019-12-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of micron-sized particle transmission electron microscope sample |
| CN111141811A (en) * | 2019-12-26 | 2020-05-12 | 中国科学院地质与地球物理研究所 | Target holder assembly of ion probe and method for preparing sample target of ion probe |
| 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 |
| CN112917280A (en) * | 2021-03-23 | 2021-06-08 | 包钢集团矿山研究院（有限责任公司） | Simple and rapid sanding sheet grinding method |
| 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 |
| CN116223168A (en) * | 2023-05-08 | 2023-06-06 | 中山大学 | Preparation method for preparing TEM and AFM region observation sample by using FIB |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107271726A (en) * | 2017-07-19 | 2017-10-20 | 中南大学 | A kind of preparation method of mineral samplers piece |
| CN107271726B (en) * | 2017-07-19 | 2019-06-28 | 中南大学 | A kind of preparation method of mineral samplers piece |
| CN107607071A (en) * | 2017-09-26 | 2018-01-19 | 深圳市领先医疗服务有限公司 | The measuring method of coating of degradable medicaments coating bracket coating layer thickness |
| CN108169266A (en) * | 2017-11-09 | 2018-06-15 | 广东科技学院 | A kind of preparation method of the scanning electron microscope example of micron order ionic crystals powder |
| CN110595848A (en) * | 2018-06-12 | 2019-12-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of micron-sized particle transmission electron microscope sample |
| CN110487823A (en) * | 2019-08-13 | 2019-11-22 | 西安工业大学 | A kind of preparation method of powder particle tem specimen |
| CN111141811A (en) * | 2019-12-26 | 2020-05-12 | 中国科学院地质与地球物理研究所 | Target holder assembly of ion probe and method for preparing sample target of ion probe |
| 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 |
| CN112917280A (en) * | 2021-03-23 | 2021-06-08 | 包钢集团矿山研究院（有限责任公司） | Simple and rapid sanding sheet grinding method |
| 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 |
| CN116223168A (en) * | 2023-05-08 | 2023-06-06 | 中山大学 | Preparation method for preparing TEM and AFM region observation sample by using FIB |
| CN116223168B (en) * | 2023-05-08 | 2023-09-15 | 中山大学 | Preparation method for preparing TEM and AFM region observation sample by using FIB |
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