CN107195520B - A kind of sample fixed station and the freezing scanning electron microscope comprising it - Google Patents
A kind of sample fixed station and the freezing scanning electron microscope comprising it Download PDFInfo
- Publication number
- CN107195520B CN107195520B CN201710418761.2A CN201710418761A CN107195520B CN 107195520 B CN107195520 B CN 107195520B CN 201710418761 A CN201710418761 A CN 201710418761A CN 107195520 B CN107195520 B CN 107195520B
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- China
- Prior art keywords
- sample
- cylinder
- tabletting
- fixed station
- fixed
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/20—Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
- H01J2237/201—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated for mounting multiple objects
Abstract
The present invention relates to sample fixing device technical fields, and in particular to a kind of sample fixed station, including：Pedestal and the cylinder being set on pedestal, cylinder upper end are arranged multiple samples and place position, and sample places fixed part of the setting to fixed sample on position；A kind of freezing scanning electron microscope comprising above-mentioned sample fixed station is further related to.A kind of sample fixed station provided by the invention and the freezing scanning electron microscope comprising it, by the way that multiple fixed parts are arranged in cylinder upper end, multiple blade class samples can be fixed simultaneously, experiment is time-consuming short, conventional efficient greatly improves, while reducing the economic cost in experimentation.
Description
Technical field
It is swept the present invention relates to sample fixing device technical field more particularly to a kind of sample fixed station and comprising its freezing
Retouch Electronic Speculum.
Background technique
Freezing scanning electron microscope is a kind of microscopic appearance Observations Means to grow up on the basis of scanning electron microscope, resolution ratio
Between transmission electron microscope and optical microscopy, can directly to metal, chemistry and High water cut biomedical material carry out it is microcosmic at
Picture is one of the important research tool in life field.Scanning electron microscope chamber interior is vacuum environment, if by the biological sample of High water cut
Product, which are directly placed into sample room, will cause sample dehydration deformation, influence ortho states topographical information, and conventional fixation, dehydration, critical point
It is the methods of dry since step is lengthy and tedious, it is more demanding to the technical level of operator, experiment it is less reproducible.And it freezes and sweeps
It retouches Electronic Speculum to be not necessarily to carry out pre-treatment to High water cut sample, target sample need to be only fixed on sample stage, be then placed in liquid nitrogen snow
Water in sample is changed into glassy state by liquid, remains the original appearance of sample to greatest extent by (- 210 DEG C) rapid cooling in mud
Information.Using processing such as distillation etching, plated films after transmitting device shifts, it is finally putting into the Electronic Speculum chamber that temperature is -130 DEG C
In interior cold bench, observe under vacuum conditions.Freezing scanning electron microscope goes out the electronic signal of sample surfaces using electron-beam excitation, then
Through specific detector, such as secondary electron detector, backscatter detector, detect electron probe after sample interaction
The signal of generation converts optical signals into electric signal, and carries out preposition amplification and video amplifier, then electric signal is made to be transformed into voltage
Display is delivered to after signal.
The fixed sample fixed station of following two mode is generallyd use in existing freezing scanning electron microscope, concrete mode is such as
Under：
One, the sample fixed station fixed using method of clamping：As shown in Figure 1, by red copper tabletting 1, aluminium ripping bar 2 and brass
Pedestal 3 forms.The aluminium crowbar 2 for being inserted into rectangular recess 4 is semicolumn, when the flat surface of semicolumn is parallel with tabletting, red copper
Tabletting 1 is in closed state, and after aluminium ripping bar 2 is rotated by 90 °, red copper tabletting 1 is in open configuration, is put into sample at this time, fixed
Aluminium ripping bar 2 is extracted out completion sample fixed operation again after clamping sample.Then being inserted into extension bar for slotting transfer device is docked
Mouth 5, compresses after and is rotated by 90 °, then release stress, and under the action of docking club head spring, transmission head can automatic clamping
Tapping in 3 front end of brass pedestal completes sample and shifts docking operation.
Two, the sample fixed station fixed using bonding method：As shown in Fig. 2, red copper cylinder objective table 6 and pedestal 9 cooperate
Use fixed sample.Red copper cylinder objective table 6 is put at circular hole 7, by 8 captive screw of threaded hole by red copper cylinder objective table
6 is fixed.1 is pressed with carbon paste and frozen rubber：1 ratio mixing, mixture glue viscosity is very weak at this time, is applied to red copper cylinder objective table
On 6, sample then is being placed above, is clamping hole 10 by the first tweezers and the second tweezers clamps hole 11, sample is put into liquid nitrogen
In slush, mixture glue instantaneous solidification, completes fixed operation at this time.The loading of red copper cylinder is ejected from the bottom end of circular hole 7 when taking-up
Platform 6.Docking operation is shifted with reference to the transfer docking operation for the sample fixed station fixed in Fig. 1 using method of clamping.
In actual operation, the fixed sample fixed station of above two mode, all different degrees of there are some problems：
One, the sample fixed station fixed using method of clamping：Since tabletting 1 is whole tabletting, single can only fix 1
A blade class sample, it is then pre-cooled, transfer, distillation, plated film and etc. could complete observation demand, overall process time-consuming 1-2
Hour., will be time-consuming more long if sample treatment is ineffective or observation sample size is more, conventional efficient is lower.And it tests
Whole process requires continual consumption high pure nitrogen (1 steel cylinder/day) and liquid nitrogen (being greater than 15L/ days) to guarantee low temperature, inefficiency
Caused by direct result be exactly to increase economic cost.
Two, the sample fixed station fixed using bonding method：There are the following defects：(1) it is opposite to paste sample size
It is few：Because stickup glue can just play fixed function only in liquid nitrogen, room temperature viscosity is very weak, sample can only be pasted onto diameter
On the former platform 1 of 10mm, leaf sample biggish for area, observation number is just limited；It (2) is not the best solid of blade class sample
Determine mode：The mode of gripping is the preferred fixed form of blade class sample observation, pastes fixation and is easy to cause blade in table top
The surface of class sample generates ice crystal during processing, increases late-run sample processing difficulty, influences final imaging quality.
Based on above-mentioned status, existing freezing scanning electron microscope example fixed station how to be allow to fix multiple blade classes simultaneously
Sample, just become urgent need to resolve the technical issues of.In view of this, the present invention is specifically proposed.
Summary of the invention
(1) technical problems to be solved
The purpose of the present invention is to provide a kind of sample fixed station and include its freezing scanning electron microscope, it is intended to solve existing
The technical issues of scanning electron microscope example fixed station cannot fix multiple blade class samples simultaneously is freezed in technology.
(2) technical solution
In order to solve the above-mentioned technical problems, the present invention provides a kind of sample fixed stations, including：It pedestal and is set to described
Cylinder on pedestal, the cylinder upper end are arranged multiple samples and place position, and the sample, which is placed, to be arranged to fixed sample on position
Fixed part.
Preferably, the fixed part is tabletting, and the tabletting and the upper surface of the cylinder are arranged in a one-to-one correspondence, and described
Tabletting divides valve to be arranged with its center, forms multiple tablettings and divides valve.
Preferably, the shape of the tabletting is the sequentially connected helical form of the center point, and all tablettings divide valve along institute
The outer rim for stating tabletting is uniformly distributed.
Preferably, the tabletting is made of highly elastic material.
Preferably, the highly elastic material is copper, nickel or memorial alloy.
Preferably, the cylinder is cylindrical body, and the upper end side of the cylindrical body is uniformly provided with multiple grooves, the circle
The lower end of cylinder is matched with the pedestal.
Preferably, the shape of the groove is domatic, cylinder or semi-cylindrical.
Preferably, the cylinder is set on the pedestal by annular spring leaf, and the annular spring leaf is sheathed on institute
State the lower part of cylinder；The upper end of the cylinder is provided with the screw for fixing tabletting, can be made by the rotation screw described
Cylinder is relative to the base rotation.
Preferably, the annular spring leaf includes ontology, and the ontology is tubular structure, and one end of the ontology is along axial direction
Extend multiple elasticity of flexure thin slices.
The present invention also provides a kind of freezing scanning electron microscope, include above-mentioned sample fixed station.
(3) beneficial effect
Above-mentioned technical proposal of the invention has the advantages that：Sample fixed station provided by the present invention, by
Multiple fixed parts are arranged in cylinder upper end, can fix multiple blade class samples simultaneously, experiment is time-consuming short, and conventional efficient mentions significantly
Height, while reducing the economic cost in experimentation.
Detailed description of the invention
Fig. 1 is in the prior art using the structural schematic diagram of the fixed sample fixed station of method of clamping；
Fig. 2 is in the prior art using the structural schematic diagram of the fixed sample fixed station of bonding method；
Fig. 3 is the structural schematic diagram of the sample fixed station of the embodiment of the present invention；
Fig. 4 is the structural schematic diagram of the cylinder in Fig. 3；
Fig. 5 is the structural schematic diagram of the tabletting in Fig. 3；
Fig. 6 is the structural schematic diagram of the annular spring leaf in Fig. 3；
Wherein, 1, red copper tabletting；2, aluminium ripping bar；3, brass pedestal；4, rectangular recess；5, to interface；6, brass cylinder
Objective table；7, circular hole；8, threaded hole；9, pedestal；10, the first tweezers clamp hole；11, the second tweezers clamp hole；12, cylinder；
12a, butt end；12b, taper end；12c, groove；13, tabletting；13a, tabletting divide valve；14, annular spring leaf；14a, ontology；It is 14b, curved
Bent elastic sheet.
Specific embodiment
Embodiments of the present invention are described in further detail with reference to the accompanying drawings and examples.Following embodiment is used for
Illustrate the present invention, but cannot be used to limit the scope of the invention.
In the description of the present invention, unless otherwise indicated, the meaning of " plurality " is two or more；Unless otherwise saying
Bright, the meaning of " nick shaped " is the shape in addition to section is concordant.It is term " on ", "lower", "left", "right", "inner", "outside", " preceding
The orientation or positional relationship of the instructions such as end ", " rear end ", " head ", " tail portion " is to be based on the orientation or positional relationship shown in the drawings,
Be merely for convenience of description of the present invention and simplification of the description, rather than the device or element of indication or suggestion meaning must have it is specific
Orientation, be constructed and operated in a specific orientation, therefore be not considered as limiting the invention.In addition, term " first ",
" second ", " third " etc. are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, it can also be indirectly connected through an intermediary.For this
For the those of ordinary skill in field, the concrete meaning of above-mentioned term in the present invention can be understood depending on concrete condition.
Also referring to Fig. 3 to Fig. 6, now a kind of sample fixed station provided by the invention is illustrated.A kind of sample is solid
Determine platform, including：Pedestal 9 and the cylinder 12 being set on pedestal 9,12 upper end of cylinder are arranged multiple samples and place position, and sample is placed
Fixed part to fixed sample is set on position.
Sample fixed station provided by the present invention can be fixed more simultaneously by the way that multiple fixed parts are arranged in cylinder upper end
A blade class sample, experiment is time-consuming short, and conventional efficient greatly improves, while reducing the economic cost in experimentation.
Further, Fig. 5 is referred to, as a kind of a kind of specific embodiment of sample fixed station provided by the invention,
Fixed part is tabletting 13, and tabletting 13 and the upper surface of cylinder 12 are arranged in a one-to-one correspondence, and tabletting 13 divides valve to be arranged with its center, shape
Divide valve 13a at multiple tablettings.
Preferably, the shape of tabletting 13 is the sequentially connected helical form of the center point, and all tablettings divide valve 13a along tabletting 13
Outer rim be uniformly distributed.Since 12 surface diameter of cylinder is only 10mm, if tabletting mode referring to Fig.1, to elastic properties of materials
It is required that very high, the selection of 13 material of tabletting is just limited；Tabletting 13 designs spiral, and spiral helicine design effectively extends power
Arm, has widened the material selection of tabletting 13, while also mitigating the mechanical pressure damage to blade class specimen material.
In the present embodiment, tabletting divides the quantity of valve 13a to be six, and six tablettings divide valve 13a uniformly to divide with the center of circle of tabletting
Cloth.Tabletting divides the quantity of valve 13a that can be arranged according to the quantity of fixed sample, the amount doesn't matter.
Preferably, tabletting 13 is made of highly elastic material.13 entirety of tabletting in the present embodiment is made of nickel material.Except this
Except, tabletting 13 can also be other highly elastic materials such as copper, memorial alloy.
Further, Fig. 4 is referred to, as a kind of a kind of specific embodiment of sample fixed station provided by the invention,
Cylinder 12 is cylindrical body, and the upper end side of cylindrical body is uniformly provided with multiple groove 12c, and the lower end of cylindrical body and pedestal match
It closes.
In the present embodiment, cylindrical body is stepped cylindrical, and the diameter of the butt end 12a of stepped cylindrical is 10mm, stepped cylindrical
The diameter of taper end 12b is 9mm；Although the diameter of cylinder 12 the big more can reduce requirement to 13 material of tabletting, also can simultaneously
Increase sample and shift the risk of bulkhead touching, equally can also reduce effective viewing area of sample.
In addition, fluted 12c is arranged in the butt end 12a of stepped cylindrical, the domatic that the concrete shape of groove 12c is 45 degree is recessed
Slot；Groove 12c may be designed as semi-cylindrical or cylinder etc. in addition to being designed to domatic, facilitates and agitates tabletting with tweezers and divide valve
13a and design.
It should be noted that convenient, neat in order to fix sample, quantity and the tabletting of groove 12c divides the quantity phase of valve 13a
Deng.
Further, Fig. 6 is referred to, as a kind of a kind of specific embodiment of sample fixed station provided by the invention,
Cylinder 12 is set on pedestal 9 by annular spring leaf 14, and annular spring leaf 14 is sheathed on the lower part of cylinder 12；Cylinder 12 it is upper
End is provided with the screw for fixing tabletting 13, cylinder 12 can be made to rotate relative to pedestal 9 by rotation screw.
Specifically, annular spring leaf 14 includes ontology 14a, ontology 14a is tubular structure, and one end of ontology 14a is along axial direction
Extend multiple elasticity of flexure thin slice 14b.Multiple elasticity of flexure thin slice 14b are set, are to make annular spring leaf 14 fasten rank
When the taper end 12b of terraced cylinder, other than fastening effect, moreover it is possible to guarantee that stepped cylindrical rotates on pedestal 9.
In use, being first fixed on tabletting 13 on cylinder 9 with standard screw, then spring leaf 13 is put into positioned at pedestal 9
In the circular hole 7 on top, finally the taper end 12b of the above-mentioned cylinder 9 for being connected with tabletting 13 is put into above-mentioned circular hole 7 again, completes sample
The installation of product fixed station.Then it is indoor mounted sample fixed station to be placed on freezing Transmission system PP3000T slush chamber
It docks on frame, pries open tabletting from domatic groove 12c with tweezers and divide valve 13a, be put into the 1st sample at this time and be fixed, then
The screw on 13 top of tabletting is rotated clockwise with wide opening tweezers or Phillips screwdriver, then is pried open next tabletting and divided valve 13a,
The 2nd sample is put into be fixed, and so on, the sample fixed station in the present embodiment can at most fix 6 samples.
A kind of freezing scanning electron microscope includes above-mentioned sample fixed station.
Freezing scanning electron microscope provided by the present invention has 6 sample tablettings to divide valve 13a at the top of sample fixed station, can be with
Single grips 6 blade class samples, and efficiency is increased to original 6 times, saves 5 times of economic cost and time cost.
The embodiment of the present invention is given for the purpose of illustration and description, and is not exhaustively or by this to send out
It is bright to be limited to disclosed form.Many modifications and variations are obvious for the ordinary skill in the art.Choosing
Selecting and describe embodiment is and to make those skilled in the art to more preferably illustrate the principle of the present invention and practical application
It will be appreciated that the present invention is to design various embodiments suitable for specific applications with various modifications.
Claims (8)
1. a kind of sample fixed station, which is characterized in that including：Pedestal (9) and the cylinder (12) being set on the pedestal (9),
Cylinder (12) upper end is arranged multiple samples and places position, and the sample places fixed part of the setting to fixed sample on position；
The fixed part is tabletting (13), and the tabletting (13) and the upper surface of the cylinder (12) are arranged in a one-to-one correspondence, and institute
It states tabletting (13) and divides valve to be arranged with its center, form multiple tablettings and divide valve (13a)；
The shape of the tabletting (13) is the sequentially connected helical form of the center point, and the tabletting divides valve (13a) along the tabletting
(13) outer rim is uniformly distributed.
2. sample fixed station according to claim 1, which is characterized in that the tabletting (13) is made of highly elastic material.
3. sample fixed station according to claim 2, which is characterized in that the highly elastic material is that copper, nickel or memory are closed
Gold.
4. sample fixed station according to claim 1, which is characterized in that the cylinder (12) is cylindrical body, the cylinder
The upper end side of body is uniformly provided with multiple grooves (12c), and the lower end of the cylindrical body is matched with the pedestal.
5. sample fixed station according to claim 4, which is characterized in that the shape of the groove (12c) is domatic, cylinder
Shape or semi-cylindrical.
6. sample fixed station according to claim 1, which is characterized in that the cylinder (12) passes through annular spring leaf (14)
It is set on the pedestal (9), the annular spring leaf (14) is sheathed on the lower part of the cylinder (12)；The cylinder (12)
Upper end is provided with the screw for fixing tabletting (13), the cylinder (12) can be made relative to the bottom by rotating the screw
Seat (9) rotation.
7. sample fixed station according to claim 6, which is characterized in that the annular spring leaf (14) includes ontology
(14a), the ontology (14a) are tubular structure, and one end of the ontology (14a) axially extends multiple elasticity of flexure thin slices
(14b)。
8. a kind of freezing scanning electron microscope, which is characterized in that fixed comprising sample described in any one of the claims 1 to 7
Platform.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710418761.2A CN107195520B (en) | 2017-06-06 | 2017-06-06 | A kind of sample fixed station and the freezing scanning electron microscope comprising it |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710418761.2A CN107195520B (en) | 2017-06-06 | 2017-06-06 | A kind of sample fixed station and the freezing scanning electron microscope comprising it |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107195520A CN107195520A (en) | 2017-09-22 |
| CN107195520B true CN107195520B (en) | 2018-11-20 |
Family
ID=59877158
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710418761.2A Expired - Fee Related CN107195520B (en) | 2017-06-06 | 2017-06-06 | A kind of sample fixed station and the freezing scanning electron microscope comprising it |
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| Country | Link |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111855720A (en) * | 2019-04-26 | 2020-10-30 | 中国科学院广州能源研究所 | Novel frozen scanning electron microscope sample stage and sampling method |
| CN112113807A (en) * | 2020-08-19 | 2020-12-22 | 中国科学院广州能源研究所 | In-situ SEM sampling device and method containing gas hydrate |
| CN113252717B (en) * | 2021-06-15 | 2021-09-10 | 中国科学院地质与地球物理研究所 | Intelligent preparation system and method for frozen electron microscope sample and electronic equipment |
| CN114923941A (en) * | 2022-07-22 | 2022-08-19 | 中国科学院遗传与发育生物学研究所 | Sample rotating platform applied to frozen scanning electron microscope |
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| CN206116342U (en) * | 2016-09-29 | 2017-04-19 | 长城汽车股份有限公司 | Sample strutting arrangement |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02271204A (en) * | 1989-04-13 | 1990-11-06 | Toshiba Corp | Sample moving table |
| GB2424198A (en) * | 2005-03-16 | 2006-09-20 | Cambridge Magnetic Refrigerati | Cryogenic support |
| CN101441970A (en) * | 2007-11-22 | 2009-05-27 | 上海华虹Nec电子有限公司 | Sample platform for observing silicon chip sample of scanning electron microscope |
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| CN206116342U (en) * | 2016-09-29 | 2017-04-19 | 长城汽车股份有限公司 | Sample strutting arrangement |
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|---|---|
| CN107195520A (en) | 2017-09-22 |
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