CN108709897A - A kind of 3DTEM and across the scale characterization universal sample platforms of 3DAP - Google Patents
A kind of 3DTEM and across the scale characterization universal sample platforms of 3DAP Download PDFInfo
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- CN108709897A CN108709897A CN201810766996.5A CN201810766996A CN108709897A CN 108709897 A CN108709897 A CN 108709897A CN 201810766996 A CN201810766996 A CN 201810766996A CN 108709897 A CN108709897 A CN 108709897A
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- copper pipe
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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
- G01N23/2204—Specimen supports therefor; Sample conveying means therefore
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
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Abstract
The invention belongs to technical field of nano material, discloses a kind of across scale characterization universal sample platforms of 3DTEM and 3DAP and be provided with：Sample stage pedestal；Sample stage pedestal tail end is rectangular, front end is dovetail-shape, it is rectangular with rear end, sample stage pedestal tail end offers circular hole, sample stage pan frontward end is welded with outer copper pipe, outer copper pipe front end sleeve is equipped with interior copper pipe, is fixed by frictional force between outer copper pipe and interior copper pipe, interior copper pipe front end is connected with the needle-shaped sample of three-dimensional atom probe.The present invention is ingenious in design, it is easily disassembled, it is easy to operate, cost is relatively low, and sample stage can reuse, which is easy to combine with the preparation method of two kinds of three-dimensional atom probe needle-shaped specimens, sample preparation and electronic micro-analysis efficiently link up, the chemical composition information of three-dimensional atom probe is fully combined with the microstructure information of 3-D transmission electron microscope, there is preferable applicability, more common of application can be obtained.
Description
Technical field
The invention belongs to technical field of nano material more particularly to a kind of 3DTEM and across the scale characterization universal samples of 3DAP
Platform.
Background technology
Currently, the prior art commonly used in the trade is such：As a kind of more universal electron microscopic characterization method, thoroughly
It penetrates electron microscope to be widely used in fields such as material science, current transmission electron microscope field is mainly absorbed in
Development on " in situ, three-dimensional, high-resolution " three directions, although the Three Dimensional Reconfiguration under transmission electron microscope can get
The information such as defect and crystalline orientation in material, but it is a lack of elemental composition information, three-dimensional atom probe is that a kind of ion is three-dimensional
Reconfiguration technique, the technology are applied successfully in characterizing material in terms of the segregation situation of element, and software reconfiguration is passed through
Can reducing material Three-dimensional atom distributed intelligence, but the defects of sample and crystallography information can not be obtained.Transmitted electron is shown
Three-dimensionalreconstruction data under micro mirror carry out corresponding with the chemical composition information under three dimension scale in material, are one of material characterization
New challenge can push people to material if the microscopic structure and chemical composition of sample can simultaneously be obtained under three-dimensional condition
Further understanding.
In conclusion problem of the existing technology is：Material characterization under transmission electron microscope lacks three dimension scale
Accurate elemental composition and distributed intelligence down, since the extension of X-ray in the material influences, in conventional transmission electron microscope
Subsidiary X-ray energy Dispersive Spectroscopy can not provide the composition information of atomic scale under three-dimensional condition；On the other hand, Three-dimensional atom
Probe although having good advantage in terms of providing accurate Elemental redistribution, be difficult obtain defect under sample three dimensions with
Crystallography information.The advantages of two kinds of characterization techniques, is fully combined currently, lacking a kind of simple and practicable interface.
Solve the difficulty and meaning of above-mentioned technical problem：Three-dimensional atom probe sample prepared by conventional electrochemical optical polishing is needle
Shape, length usually between 5~10mm, generally put it into copper pipe reuse pliers make copper pipe deformation sample and its are consolidated
It is scheduled on together.The transmission electron microscope sample of common standard is the disk of a diameter of 3mm, and observation area need to be transparent to electron beam.How will
It is a problem to be put into three-dimensional atom probe secure sample in transmission electron microscope and carry out observation.In addition, will be in transmission electricity
Three-dimensionalreconstruction is carried out to sample in mirror, sample must just be rotated, in rotary course, to keep the rotation of sample as far as possible
The rotation of shaft, the rotary shaft of sample club head, specimen holderAxis is as much as possible on same axis.How a kind of satisfaction is designed The interface of above-mentioned condition is also a problem.
Invention content
In view of the problems of the existing technology, the present invention provides a kind of 3DTEM and across the scale characterization universal samples of 3DAP
Platform.
The invention is realized in this way a kind of across the scale characterization universal sample platforms of 3DTEM and 3DAP are provided with：Sample stage bottom
Seat；
Sample stage pedestal tail end is rectangular, and front end is dovetail-shape, and sample stage base center offers circular hole, sample stage pedestal
Outer copper pipe is welded at front end center axis, outer copper pipe front end sleeve is equipped with interior copper pipe, and outer copper pipe and interior copper pipe pass through between the two
Frictional force fix, interior copper pipe front end is placed with the needle-shaped sample of three-dimensional atom probe.
Further, outer copper pipe uses argon arc welding together with sample stage tube chamber welds with base.
Further, the length of outer copper pipe is 6~7mm, and outer diameter is 1.4~1.7mm, and internal diameter is 1.0~1.3mm, outer copper pipe
0.01mm is must not exceed with the concentricity of the geometric center of sample stage front end, outer copper pipe must not surpass with sample stage front end face verticality
Cross 0.1 °.
Further, the length of interior copper pipe is 7~9mm, and outer diameter is 1.0~1.3mm, and internal diameter is 0.6~0.8mm.
Further, the needle-shaped sample of three-dimensional atom probe is thrown before use, diameter is decreased to 0.6~0.7mm by electrobrightening
Specimen length after light is 5~8mm.
Advantages of the present invention and good effect are：
Gorman et al. (Microscopy Today (2008) 42-47) and Felfer et al. (Microscopy
Research and Technique (2012) 484-491) method can only prepare sample using focused ion beam, and operate not
Convenient, sample installation process needs more people to simultaneously participate in, and causes in operation since briquetting is larger to the active force of sample
It is easily broken, to keep the failure of an experiment rate very high.The method of Chinese catalpas Liu Ji et al. (CN205692794U) is although place sample
It is fairly simple when product, but electrochemical polishing method sample preparation can only be used, there is certain limitation.In addition, other methods are due to again
The certain positions for devising specimen holder, cause manufacturing cost higher, and versatility is poor.
The invention has the advantages that：
1, the present invention is ingenious in design, and easily disassembled, easy to operate, cost is relatively low, and sample stage can reuse, the sample
Platform is easy to combine, sample preparation with the preparation method (focused ion beam or chemical polishing) of two kinds of three-dimensional atom probe needle-shaped specimens
It is efficiently linked up with electronic micro-analysis.
2, three-dimensional atom probe technology and 3-D transmission Electron Microscopy can be effectively combined together by the present invention,
In composition information and corresponding microstructure information, crystallography multiple dimensioned, that realize visual single atom in multi-angle
Orientation information etc. realizes material composition information and the expression of microstructure information in three dimensions and corresponding.
3, the present invention is a kind of sample interface of three-dimensional atom probe and 3-D transmission Electronic Speculum, and there is no be individually transformed certain
Specimen holder, cost is relatively low, has preferable applicability, can obtain more common of application.
Description of the drawings
Fig. 1 is 3DTEM provided in an embodiment of the present invention and across the scale characterization universal sample platform structural schematic diagrams of 3DAP；
Fig. 2 is that 3DTEM provided in an embodiment of the present invention illustrates with copper pipe structure outside across the scale characterization universal sample platforms of 3DAP
Figure；
In figure：1, sample stage pedestal；2, outer copper pipe；3, interior copper pipe；4, the needle-shaped sample of three-dimensional atom probe.
Specific implementation mode
In order to further understand the content, features and effects of the present invention, the following examples are hereby given, and coordinate attached drawing
Detailed description are as follows.
The structure of the present invention is explained in detail below in conjunction with the accompanying drawings.
As depicted in figs. 1 and 2, across the scale characterization universal sample platforms of 3DTEM provided in an embodiment of the present invention and 3DAP include：
The needle-shaped sample of sample stage pedestal 1, outer copper pipe 2, interior copper pipe 3, three-dimensional atom probe 4.
1 material of sample stage pedestal is copper, and the one end to link together with specimen holder is tail end, and tail end is rectangular,
One end that sample stage pedestal 1 is connect with outer copper pipe 2 is front end, and front end is dovetail-shape, rectangular with rear end, and junction has certain straight
The chamfering of diameter, sample stage pedestal 1 offer circular hole close to end section.
Outer copper pipe 2 is welded together using argon arc welding with sample stage pedestal 1, and the outer diameter of interior copper pipe 3 is slightly smaller than outer copper pipe 2
Internal diameter, two sections of copper pipes easily can detach and combine.
Fixed by frictional force between outer copper pipe 2 and interior copper pipe 3, the needle-shaped sample of three-dimensional atom probe 4 can steadily with sample
Sample platform is combined together.
The length of outer copper pipe 2 is 6~7mm, and outer diameter is 1.4~1.7mm, and internal diameter is 1.0~1.3mm, outer copper pipe 2 and sample
The concentricity of the geometric center of platform front end must not exceed 0.01mm and outer copper pipe 2 must not exceed with sample stage front end face verticality
0.1°。
The length of interior copper pipe 3 is 7~9mm, and outer diameter is 1.0~1.3mm, and internal diameter is 0.6~0.8mm.
The needle-shaped sample of the three-dimensional atom probe that uses 4 should use electrobrightening that diameter is decreased to 0.6~0.7mm first,
Specimen length after polishing is 5~8mm, and sample is put into 3 suitable position of interior copper pipe, interior copper pipe is deformed with nipper plier, makes examination
Sample firm grip.
The present invention is in use, the needle-shaped sample of the three-dimensional atom probe used 4 should use electrobrightening to reduce diameter first
To 0.6~0.7mm, the specimen length after polishing is 5~8mm, and sample is put into 3 suitable position of interior copper pipe, will be interior with nipper plier
Copper pipe deforms, and keeps sample holder secured, and the interior copper pipe 3 after the needle-shaped sample of fixed three-dimensional atom probe 4 is put into outer copper pipe 2,
The use of nipper plier is slightly an ellipse by the folder of outer copper pipe 2, by rubbing after determining that the relative position of both inside and outside copper pipes is correct
It wipes power and fixes inside and outside copper pipe 3, then the present invention is fixed on the specimen holder of transmission electron microscope by circular hole, it is careful to rotate
Specimen holder, checks whether sample is stablized, and sample stage is inserted into transmission electron microscope, is observed by X rays topographs and checks that three-dimensional is former
Whether contain interested region in the needle-shaped sample of sub- probe 4, and shoot 2-dimentional photo, is shot by the specimen holder that verts a series of
Sample photo, then according to electronics Three Dimensional Reconfiguration obtain nanometer pinpoint three-dimensional appearance and structure picture.
After transmission electron microscope observation is complete, sample stage is taken out from electron microscope, repeat the action, taken out
It is fixedly arranged at the front end with the interior copper pipe 3 of nanometer pinpoint sample, is fed directly to carry out the observation of next step in three-dimensional atom probe instrument, obtain
Three-dimensional atom probe data are taken, the reconstruct data of existing transmission electron microscope data and three-dimensional atom probe are compared
Matching analyzes three-dimensional composition information corresponding with material internal defect or crystalline orientation, and sample may be implemented and transmiting
Wide-angle verts (± 80 °) and carries out Image Acquisition or Determination of Orientation in electron microscope, can be obtained eventually by reconstruction software
The 3 D tropism reconstruct image of needle point sample or the Three-dimensional Gravity composition of defect in material.
The present invention is ingenious in design, and easily disassembled, easy to operate, cost is relatively low, and sample stage can reuse, the sample stage
It is easy to combine with the preparation method of two kinds of three-dimensional atom probe needle-shaped specimens, sample preparation and electronic micro-analysis efficiently join
It has been fully to tie the chemical composition information of three-dimensional atom probe and the microstructure information of 3-D transmission electron microscope
It closes, there is preferable applicability, more common of application can be obtained.
The above is only the preferred embodiments of the present invention, and is not intended to limit the present invention in any form,
Every any simple modification made to the above embodiment according to the technical essence of the invention, equivalent variations and modification, belong to
In the range of technical solution of the present invention.
Claims (5)
1. a kind of 3DTEM and across the scale characterization universal sample platforms of 3DAP, which is characterized in that the 3DTEM and across the scale tables of 3DAP
Sign universal sample platform is provided with：Sample stage pedestal；
Sample stage pedestal tail end is rectangular, and front end is dovetail-shape, rectangular with rear end, and sample stage pedestal tail end offers circular hole,
Sample stage pan frontward end is welded with outer copper pipe, and outer copper pipe front end sleeve is equipped with interior copper pipe, passes through friction between outer copper pipe and interior copper pipe
Power is fixed, and interior copper pipe front end is connected with the needle-shaped sample of three-dimensional atom probe.
2. 3DTEM as described in claim 1 and across the scale characterization universal sample platforms of 3DAP, which is characterized in that outer copper pipe uses argon
Together with sample stage tube chamber welds with base, junction is welded with chamfering for arc-welding.
3. 3DTEM as described in claim 1 and across the scale characterization universal sample platforms of 3DAP, which is characterized in that the outer copper pipe
Length is 6~7mm, and outer diameter is 1.4~1.7mm, and internal diameter is 1.0~1.3mm, outer copper pipe and the geometric center of sample stage front end
Concentricity is less than 0.01mm, and outer copper pipe is less than 0.1 ° with sample stage front end face verticality.
4. 3DTEM as described in claim 1 and across the scale characterization universal sample platforms of 3DAP, which is characterized in that the length of interior copper pipe
For 7~9mm, outer diameter is 1.0~1.3mm, and internal diameter is 0.6~0.8mm.
5. 3DTEM as described in claim 1 and across the scale characterization universal sample platforms of 3DAP, which is characterized in that three-dimensional atom probe
Needle-shaped specimen finish is 0.6~0.7mm, and length is 5~8mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810766996.5A CN108709897A (en) | 2018-07-13 | 2018-07-13 | A kind of 3DTEM and across the scale characterization universal sample platforms of 3DAP |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810766996.5A CN108709897A (en) | 2018-07-13 | 2018-07-13 | A kind of 3DTEM and across the scale characterization universal sample platforms of 3DAP |
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| CN108709897A true CN108709897A (en) | 2018-10-26 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111307847A (en) * | 2020-03-11 | 2020-06-19 | 中国科学院地质与地球物理研究所 | Micro-nano-scale sample vacuum storage device |
| CN111337522A (en) * | 2018-11-30 | 2020-06-26 | 浙江大学 | Multi-degree-of-freedom sample rod with sample clamping nozzle |
| CN112782198A (en) * | 2020-12-07 | 2021-05-11 | 上海大学 | Multi-equipment combined three-dimensional atom probe sample universal interface device |
| CN113063967A (en) * | 2021-02-18 | 2021-07-02 | 上海大学 | Rotary sample table device capable of realizing three-dimensional atom probe microtip array sample rotation |
| CN114002240A (en) * | 2021-09-27 | 2022-02-01 | 中国科学院广州地球化学研究所 | Electron microscopic three-dimensional reconstruction characterization method for geological sample microstructure |
| CN114295865A (en) * | 2021-12-19 | 2022-04-08 | 南京理工大学 | Multi-sample table combined with atom probe equipment and transmission electron microscope |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111337522A (en) * | 2018-11-30 | 2020-06-26 | 浙江大学 | Multi-degree-of-freedom sample rod with sample clamping nozzle |
| CN111337522B (en) * | 2018-11-30 | 2021-10-19 | 浙江大学 | Multi-degree-of-freedom sample rod with sample clamping nozzle |
| CN111307847A (en) * | 2020-03-11 | 2020-06-19 | 中国科学院地质与地球物理研究所 | Micro-nano-scale sample vacuum storage device |
| CN112782198A (en) * | 2020-12-07 | 2021-05-11 | 上海大学 | Multi-equipment combined three-dimensional atom probe sample universal interface device |
| CN113063967A (en) * | 2021-02-18 | 2021-07-02 | 上海大学 | Rotary sample table device capable of realizing three-dimensional atom probe microtip array sample rotation |
| CN113063967B (en) * | 2021-02-18 | 2023-02-10 | 上海大学 | Rotary sample table device capable of realizing three-dimensional atom probe microtip array sample rotation |
| CN114002240A (en) * | 2021-09-27 | 2022-02-01 | 中国科学院广州地球化学研究所 | Electron microscopic three-dimensional reconstruction characterization method for geological sample microstructure |
| CN114295865A (en) * | 2021-12-19 | 2022-04-08 | 南京理工大学 | Multi-sample table combined with atom probe equipment and transmission electron microscope |
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