CN104316730B - Low-temperature brittle failure device for manufacturing scanning electron microscope sample section - Google Patents
Low-temperature brittle failure device for manufacturing scanning electron microscope sample section Download PDFInfo
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- CN104316730B CN104316730B CN201410637248.9A CN201410637248A CN104316730B CN 104316730 B CN104316730 B CN 104316730B CN 201410637248 A CN201410637248 A CN 201410637248A CN 104316730 B CN104316730 B CN 104316730B
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Abstract
The invention discloses a low-temperature brittle failure device for manufacturing a scanning electron microscope sample section. The device comprises a sample fixing device, two pressing plates and a closed shell. A circle of wall plates are arranged on the periphery of a base of the sample fixing device. A containing portion is formed between the base and the wall plates. The upper end faces of two opposite wall plates are provided with screw holes, wherein one wall plate with the screw holes is provided with a plurality of grooves where cylindrical samples are placed. The two pressing plates are in a flat plate shape and are provided with through holes corresponding to the screw holes in the end faces of the wall plates. A plurality of grooves corresponding to the grooves in the end face of one wall plate in shape and position are formed in the face of one pressing plate. The closed shell is used for containing a liquid nitrogen container. A sample fixing device is soaked in the liquid nitrogen container. The shell is the container made of thermal insulation and cold insulation materials. Two impact holes are formed in the position, corresponding to the inner sides of the wall plates with the screw holes, of an upper cover of the shell and used for enabling impact rods to stretch into the shell. The low-temperature brittle failure device is applicable to manufacturing sample fracture surfaces of biological tissue in a thin film and sheet shape, and convenience is brought to observation of a scanning electron microscope.
Description
Technical field
The present invention relates to a kind of film (sheet) sample section preparing sem observation under ultralow temperature
Device.
Background technology
The electron beam of SEM (abbreviation ESEM, sem) is interacted with sample and produces multi-signal, than
As secondary electron.The pattern of accurate response sample surfaces is capable of in the secondary electron imaging that electron beam scanning obtains, and resolution ratio is usual
Nanometer (10 can be reached-9M) rank, thus it is widely used in each research field, the particularly surface of microscopic species, nano material etc.
Morphology characterization.With the development of scientific research, SEM has obtained greatly as a kind of observational technique of intuitive and convenient
Using.Go deep into biological field research now with to environmental area, the film sample to biological sample and water process aspect
Research relatively many, in the rhizome of the plant sample such as such as paddy rice, leaf and water process, frequent research is hydrophilic and hydrophobic thin
Membrane material etc..It is known that simple cuts, cuts and sample section will certainly be caused by deforming that external force produces, have a strong impact on electricity
The observing effect of mirror, and the inside cell observation of biological sample and the structural research of multilayered film material, most important method
It is exactly the observational study of section.
Currently used for the fracture surface of sample device also simply having for studying alloy layer metallographic structure of low-temperature brittle fracture, it makes
Also simply sample is placed in ultralow temperature medium (such as liquid nitrogen) with method, then takes out sample again from liquid nitrogen and cut at room temperature
The section materialsed, this method is difficult to be suitable for and mostly is shirtsleeve operation pattern for biological and toughness membrane sample brittle failure.
Low-temperature brittle fracture device is part and parcel in the preparation of sample early stage, and domestic it is studied is gone back seldom, currently used for low
The fracture surface of sample device also simply having for studying alloy layer metallographic structure of warm brittle failure, is difficult to be suitable for for biological and toughness
The brittle failure of membrane sample mostly is shirtsleeve operation pattern, but is as the research depth of biological toxicological study and water quality multilayered film material
Enter, the early stage based on Electronic Speculum processes important supplementary means and the developing direction that low-temperature brittle fracture apparatus system would is that this quasi-instrument.
Realize various types of materials sample, widely studied needs that biological sample is imaged in electron microscopic.
Research with biological toxicological study and water quality multilayered film material is goed deep into, and it is crisp that the early stage based on Electronic Speculum processes low temperature
Disconnected device would is that important supplementary means and the developing direction of this quasi-instrument, realizes various types of materials sample, biological sample in electronics
The widely studied needs of micro-imaging.
Content of the invention
It is an object of the invention to provide a kind of low-temperature brittle fracture device preparing SEM sample section, with convenient
Preparation various types of materials, biological section sample.
For achieving the above object, the low-temperature brittle fracture device of the preparation SEM sample section that the present invention provides,
Comprising:
One sample fixing device, the base of this sample fixing device is formed around a circle wallboard, makes between base and wallboard
Form a receiving portion；
It is provided with screw, it is recessed that the wallboard that one of them is provided with screw is provided with several above two relative wallboard end faces
Groove, for placing cylindrical sample；
Two pressing plates, are tabular, be provided with the through hole corresponding with the screw on wallboard, one of hold-down plate surface sets
There is the corresponding groove of several groove shapes with wallboard end face, position；
One airtight housing, for placing liquid nitrogen container, soaks sample fixing device in this liquid nitrogen container；
The container that this housing is made for the cold material of heat insulation, the upper lid of housing is correspondingly provided with inside the wallboard of screw and is provided with two
Individual impact opening, for stretching into impact bar in housing.
Described low-temperature brittle fracture device, wherein, is divided into two accommodating chambers by a dividing plate in the middle of receiving portion.
Described low-temperature brittle fracture device, wherein, the base of sample fixing device is polytetrafluoroethylene (PTFE), is provided with some apertures
Entrance for liquid nitrogen.
Described low-temperature brittle fracture device, wherein, sample fixing device is provided with hand basket.
Described low-temperature brittle fracture device, wherein, the impact head of impact bar is wedge shape tip.
The present invention, compared with technical background, has the beneficial effect that
1) large-sized iron and steel of traditional brittle failure device and the restriction of alloy sample are breached；
2) compared to traditional large scale sample brittle failure device, this brittle failure device volume is less, and operation is more convenient；
3) compensate for traditional sample section preparation method cannot obtain section indeformable original form shortcoming；
4) this brittle failure device is the design that the pre-treatment for SEM is carried out, thus with strong points, practical
Property is strong.
Brief description
Fig. 1 is the schematic diagram of the low-temperature brittle fracture device of the present invention.
Fig. 2 is the pressing plate schematic diagram of fixing sample.
Fig. 3 is the body diagram of the present invention.
Fig. 4 is the cross-sectional scanning electron microscope figure of toughness film's sample of the low-temperature brittle fracture device preparation using the present invention
Piece.
Fig. 5 is the cross-sectional scanning electron microscope figure of the plant leaf blade sample of the low-temperature brittle fracture device preparation using the present invention
Piece.
Symbol description in accompanying drawing:
1 wallboard, 2 receiving portions, 3,31 grooves, 4 screws, 41 through holes, 5 wallboard end faces, 6 dividing plates, 7 pressing plates, 8 housings, 81 shells
The upper lid of body, 9 impact openings.
Specific embodiment
The low-temperature brittle fracture device liquid of the present invention, is located in realizing the brittle failure of sample in airtight liquid nitrogen solution, is not breaking
Rupture on the premise of bad sample original appearance easily, fracture is neat, and effect is obvious.The low-temperature brittle fracture apparatus structure of the present invention is simple, light
Ingeniously, energy is rapid, easily prepare fracture, is particularly suited for being prepared as studying biological tissue and multi-layer tough film sample fracture.
The present invention is especially suitable for the section research of toughness film's sample and biological sample, you can realize scanning electron microscopy
Observation under mirror.
The low-temperature brittle fracture device of the present invention, including a sample fixing device, the leaching of this sample fixing device is put in a liquid nitrogen
In container, and this sample fixing device is placed in the cold housing 8 of an airtight heat insulation (as Fig. 3 together with liquid nitrogen container
Shown).The upper lid 81 of this housing 8 offers two rectangular impact openings 9, for impact bar is stretched into intercepting sample in housing
Product.The cold shell material of heat insulation is polytetrafluoroethylene (PTFE), and in one embodiment of the invention, the thickness of housing is 10mm.Adopt
With the housing that heat insulation is cold, it is the safety for experimenter, not frost bitten, can slow down the evaporation rate of liquid nitrogen simultaneously again.
Liquid nitrogen container can be made up of stainless steel, is used for holding liquid nitrogen, sample is carried out soak cooling shaping.
Impact bar is stainless steel material, and one end makes wedgewise, is for the convenient impact brittle failure to sample.
Because above-mentioned liquid nitrogen container and impact bar are according to its effect and function, it is easy to be thought by those skilled in the art
As therefore not elaborating, also not recommending accompanying drawing.
In conjunction with accompanying drawing, the sample fixing device of the present invention is elaborated below.
Refer to Fig. 1 and Fig. 3.The sample fixing device of the present invention can be made using polytetrafluoroethylene (PTFE), is solid in sample
That determines device pedestal is formed around wallboard 1, makes to form a receiving portion 2 between base and wallboard 1.Two relative wallboard end faces 5
Top be provided with screw 4, the wallboard 5 that one of them is provided with screw is provided with several semicircular grooves 3, for place column or
The sample of hollow form, the wallboard end face being not provided with groove is used for for placing flat film and biological sample.Due to this
Invention sample fixing device can two kinds of samples of different shapes of brittle failure simultaneously, for avoiding two kinds of samples to obscure in brittle failure,
In the middle of receiving portion 2, two accommodating chambers are divided into by a dividing plate 6.
Sample fixing device is also configured with the flat pressing plate 7 of stainless steel, and this pressing plate is provided with and wallboard end face
On the corresponding through hole 41 of screw, the face of one of pressing plate is provided with several groove 3 shapes with wallboard end face, position
Put corresponding groove 31.In concrete operations, sample is placed on wallboard end face, is passed through sample with screw with pressing plate 7
It is fixed on sample fixing device, if cylindrical sample, then sample is placed in the groove 3 of wallboard end face, uses pressing plate simultaneously
On groove 31 fixing.
The impact opening 9 of aforementioned case top lid is in order to the entrance of impact bar is reserved, and its position corresponds to the fixing dress of sample
The medial surface put, neat with the sample section that ensures brittle failure.
The sample fixing device of the present invention is also provided with a hand basket, for by the sample fixing device after brittle failure from liquid nitrogen
Take out in tank.
The following is the concrete preparation process of sample brittle failure of the present invention:
1) fixation of sample: flat sheet membranes or sheet plant sample are cut into elongated；Put it to sample fixing device
Base on (note: need to stretch out a part), then put pressing plate, and with screw, pressing plate fixed, so that sample is fixed.
2) add liquid nitrogen in liquid nitrogen container: liquid nitrogen is added liquid nitrogen container, generally requires 8 liters about.
3) cooling of sample becomes fragile: the sample fixing device fixing sample is put into liquid nitrogen container so that sample cooling becomes
Crisp, and case top lid is covered.
4) brittle failure of sample: pick up impact bar be aligned sample fixing side carry out moment impact.
5) take out the sample after brittle failure: open the upper lid of housing, sample fixing device is taken out, the appearance of sample fixing device
The sample received after falling to having brittle failure in portion.
6) sample is dried process, is put under SEM and observes test.
Sample section prepared by the present invention obtains section observation result under a scanning electron microscope with additive method
As follows:
As shown in figure 4, being to be tied using microscopical observation of toughness film's cross-sectional scanning electron of assembly of the invention preparation
Really.
As shown in figure 5, being to be tied using microscopical observation of plant leaf blade cross-sectional scanning electron of assembly of the invention preparation
Really.
Claims (5)
1. a kind of low-temperature brittle fracture device preparing SEM sample section, comprising:
One sample fixing device, the base of this sample fixing device is formed around a circle wallboard, makes to be formed between base and wallboard
One receiving portion；
It is provided with screw above two relative wallboard end faces, the wallboard that one of them is provided with screw is provided with several grooves, use
In placement cylindrical sample；
Two pressing plates, are tabular, are provided with the through hole corresponding with the screw on wallboard end face, on the face of one of pressing plate
It is provided with the corresponding groove in several groove shapes with wallboard end face, position；
One airtight housing, for placing liquid nitrogen container, soaks sample fixing device in this liquid nitrogen container；
The container that this housing is made for the cold material of heat insulation, housing is covered with two impact openings, and its position corresponds to and is provided with
The wallboard medial surface of screw, for stretching into impact bar in housing.
2. low-temperature brittle fracture device according to claim 1, wherein, is divided into two accommodating chambers by a dividing plate in the middle of receiving portion.
3. low-temperature brittle fracture device according to claim 1, wherein, the base of sample fixing device is polytetrafluoroethylene (PTFE), its
Base is provided with some apertures for the entrance of liquid nitrogen.
4. low-temperature brittle fracture device according to claim 1, wherein, sample fixing device is provided with hand basket.
5. low-temperature brittle fracture device according to claim 1, wherein, the impact head of impact bar is wedge shape tip.
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| CN201410637248.9A CN104316730B (en) | 2014-11-05 | 2014-11-05 | Low-temperature brittle failure device for manufacturing scanning electron microscope sample section |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410637248.9A CN104316730B (en) | 2014-11-05 | 2014-11-05 | Low-temperature brittle failure device for manufacturing scanning electron microscope sample section |
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| CN104316730A CN104316730A (en) | 2015-01-28 |
| CN104316730B true CN104316730B (en) | 2017-01-18 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699167B (en) * | 2016-01-26 | 2019-01-01 | 哈尔滨工业大学深圳研究生院 | A kind of fexible film brittle failure method |
| WO2018000350A1 (en) * | 2016-06-30 | 2018-01-04 | 周肇梅 | Method for fracturing fixable film |
| CN107765038B (en) * | 2017-09-13 | 2020-04-17 | 上海海洋大学 | Fixing device for functional modification of atomic force microscope substrate |
| CN107976460B (en) * | 2017-11-06 | 2020-09-25 | 上海恩捷新材料科技有限公司 | Freezing sample preparation device and sample preparation method for scanning electron microscope |
| CN111089872A (en) * | 2019-12-30 | 2020-05-01 | 江苏厚生新能源科技有限公司 | Method for preparing sample of section of microporous lithium battery diaphragm |
| CN113533402A (en) * | 2021-07-14 | 2021-10-22 | 北京市理化分析测试中心 | Film coating brittle fracture method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5654546A (en) * | 1995-11-07 | 1997-08-05 | Molecular Imaging Corporation | Variable temperature scanning probe microscope based on a peltier device |
| CN102235947A (en) * | 2010-04-29 | 2011-11-09 | 中芯国际集成电路制造(上海)有限公司 | Method for preparing observation sample of transmission electron microscope |
| CN201707254U (en) * | 2010-07-05 | 2011-01-12 | 中国人民解放军第四军医大学 | Ice box suitable for low temperature operation |
| JP2012189322A (en) * | 2011-03-08 | 2012-10-04 | Olympus Corp | Liquid-state biological phantom and manufacturing method of liquid-state biological phantom |
| CN103185676A (en) * | 2011-12-27 | 2013-07-03 | 国家纳米技术与工程研究院 | Sample preparation method for fracture of tungsten carbide coating on magnesium-alloy surface via scanning electron microscope |
| CN203432830U (en) * | 2013-09-19 | 2014-02-12 | 中国烟草总公司郑州烟草研究院 | Pretreatment device for quickly preparing fresh tobacco leaf sample of metabonomics |
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