CN104316730A - 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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- CN104316730A CN104316730A CN201410637248.9A CN201410637248A CN104316730A CN 104316730 A CN104316730 A CN 104316730A CN 201410637248 A CN201410637248 A CN 201410637248A CN 104316730 A CN104316730 A CN 104316730A
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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 device preparing film (sheet) sample section of sem observation under ultralow temperature.
Background technology
The electron beam of scanning electron microscope (being called for short scanning electron microscope, SEM) and sample interact and produce multi-signal, such as secondary electron.The secondary electron imaging that electron beam scanning obtains can the pattern of accurate response sample surfaces, and resolution can reach nanometer (10 usually
-9m) rank, the surface topography being thus widely used in each research field, particularly microscopic species, nano material etc. characterizes.Along with the development of scientific research, scanning electron microscope obtains great utilization as a kind of observational technique of intuitive and convenient.At present along with going deep into of studying environmental area and biological field, relatively many to the research of the film sample of biological sample and water treatment aspect, hydrophilic and hydrophobic-film materials of often research in the rhizome of the plant samples such as such as paddy rice, leaf and water treatment etc.As everyone knows, simple to cut, cut the distortion that sample section will certainly be caused produced by external force, have a strong impact on the observing effect of Electronic Speculum, and the structural research of the inside cell observation of biological sample and multilayered film material, most important method is exactly the observational study of section.
At present for the fracture surface of sample device also just had for studying alloy layer metallographic structure of low-temperature brittle fracture, sample is also just placed in ultralow temperature medium (such as liquid nitrogen) by its using method, and then from liquid nitrogen, take out the section that sample at room temperature intercepts sample, this method is difficult to be suitable for and mostly is shirtsleeve operation pattern for brittle failure that is biological and tough film sample.
Low-temperature brittle fracture device is part and parcel in sample preparation in early stage, domestic also little to its research, at present for the fracture surface of sample device also just had for studying alloy layer metallographic structure of low-temperature brittle fracture, be difficult to be suitable for and mostly be shirtsleeve operation pattern for brittle failure that is biological and tough film sample, but along with the research of biological toxicological study and water quality multilayered film material is goed deep into, process important supplementary means and developing direction that low-temperature brittle fracture apparatus system will be this quasi-instrument the early stage based on Electronic Speculum.Realize various types of materials sample, biological sample at the extensive research needs of electron microscopic imaging.
Along with the research of biological toxicological study and water quality multilayered film material is goed deep into, process important supplementary means and developing direction that low-temperature brittle fracture device will be this quasi-instrument the early stage based on Electronic Speculum, realize various types of materials sample, biological sample at the extensive research needs of electron microscopic imaging.
Summary of the invention
The object of this invention is to provide a kind of low-temperature brittle fracture device preparing scanning electron microscope sample section, to facilitate preparation various types of materials, biological section sample.
For achieving the above object, the low-temperature brittle fracture device of preparation scanning electron microscope sample section provided by the invention, it comprises:
One sample fixing device, the base surrounding of this sample fixing device is provided with a circle wallboard, makes to form an accommodation section between base and wallboard;
Be provided with screw above two relative wallboard end faces, one of them wallboard being provided with screw is provided with several grooves, for placing cylindrical sample;
Two pressing plates are tabular, are provided with the through hole corresponding with the screw on wallboard, and one of them hold-down plate surface 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;
This housing is the container that the cold material of heat insulation is made, and is provided with two impact openings, for being stretched in housing by impact bar inside the corresponding wallboard being provided with screw of upper cover of housing.
Described low-temperature brittle fracture device, wherein, is divided into two accommodating chambers by a dividing plate in the middle of accommodation section.
Described low-temperature brittle fracture device, wherein, the base of sample fixing device is teflon, is provided with some apertures entering for liquid nitrogen.
Described low-temperature brittle fracture device, wherein, sample fixing device is provided with puies forward indigo plant.
Described low-temperature brittle fracture device, wherein, the impact head of impact bar is wedge shape tip.
The present invention is compared with technical background, and the beneficial effect had is:
1) large-sized iron and steel of traditional brittle failure device and the restriction of alloy sample is breached;
2) compared to traditional large scale sample brittle failure device, this brittle failure device volume is less, and it is more convenient to operate;
3) the section preparation method that compensate for traditional sample cannot obtain the shortcoming of the indeformable original form of section;
4) this brittle failure device is the design carried out for the pre-treatment of scanning electron microscope, thus with strong points, practical.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of low-temperature brittle fracture device of the present invention.
Fig. 2 is the pressing plate schematic diagram of fixed sample.
Fig. 3 is body diagram of the present invention.
Fig. 4 is the cross-sectional scanning electron microscope photograph of the toughness film's sample utilizing low-temperature brittle fracture device of the present invention to prepare.
Fig. 5 is the cross-sectional scanning electron microscope photograph of the plant leaf blade sample utilizing low-temperature brittle fracture device of the present invention to prepare.
Symbol description in accompanying drawing:
1 wallboard, 2 accommodation sections, 3,31 grooves, 4 screws, 41 through holes, 5 wallboard end faces, 6 dividing plates, 7 pressing plates, 8 housings, the upper cover of 81 housings, 9 impact openings.
Embodiment
Low-temperature brittle fracture device liquid of the present invention is placed on the brittle failure realizing sample in airtight liquid nitrogen solution, and under the prerequisite not destroying sample original appearance, fracture easily, and fracture is neat, successful.Low-temperature brittle fracture apparatus structure of the present invention is simple, light and handy, can prepare fracture rapidly, easily, is particularly useful for being prepared as postgraduate's fabric texture and multi-layer tough film sample fracture.
The present invention is specially adapted to the section research of toughness film's sample and biological sample, can realize the observation under scanning electron microscope.
Low-temperature brittle fracture device of the present invention, comprise a sample fixing device, the leaching of this sample fixing device is put in a liquid nitrogen container, and is placed on together with liquid nitrogen container by this sample fixing device in the cold housing 8 of an airtight heat insulation (as shown in Figure 2).The upper cover 81 of this housing 8 offers two rectangular impact openings 9, intercepts sample for being stretched in housing by impact bar.The cold shell material of heat insulation is teflon, and in one embodiment of the invention, the thickness of housing is 10mm.Adopting the housing that heat insulation is cold, is the safety in order to experimenter, not frost bitten, can slow down again the evaporation rate of liquid nitrogen simultaneously.
Liquid nitrogen container can be made for stainless steel, for holding liquid nitrogen, carries out immersion cooling shaping to sample.
Impact bar is stainless steel material, and one end is made into wedge shape, is to the impact brittle failure of sample in order to convenient.
Because above-mentioned liquid nitrogen container and impact bar are according to its effect and function, as easy as rolling off a logly to be imagined by those skilled in the art, therefore do not elaborate, also do not recommend accompanying drawing.
Below by reference to the accompanying drawings sample fixing device of the present invention is elaborated again.
Refer to Fig. 1 and Fig. 3.Sample fixing device of the present invention can adopt teflon to make, and is to be provided with wallboard 1 in the surrounding of sample fixing device base, makes to form an accommodation section 2 between base and wallboard 1.Screw 4 is provided with above two relative wallboard end faces 5, one of them wallboard 5 being provided with screw is provided with several semicircular grooves 3, for placing the sample of column or hollow form, the wallboard end face not arranging groove is for for placing flat film and biological sample.Because sample fixing device of the present invention can simultaneously brittle failure two kinds of difform samples, for avoiding two kinds of samples to obscure when brittle failure, in the middle of accommodation section 2, be divided into two accommodating chambers by a dividing plate 6.
Sample fixing device is also configured with the flat pressing plate 7 of stainless steel, this pressing plate is provided with the through hole 41 corresponding with the screw on wallboard end face, and the face of one of them pressing plate is provided with the corresponding groove 31 in several groove 3 shapes with wallboard end face, position.When concrete operations, sample being placed on wallboard end face, with pressing plate 7 by sample being fixed on sample fixing device with screw, if cylindrical sample, then sample being placed in the groove 3 of wallboard end face, fix with the groove 31 on pressing plate simultaneously.
The impact opening 9 of aforementioned case top lid be entering in order to impact bar reserve, its position corresponds to the medial surface of sample fixing device, neat to ensure the sample section of brittle failure.
Sample fixing device of the present invention can also be provided with a hand basket, for being taken out from liquid nitrogen container by the sample fixing device after brittle failure.
Below the concrete preparation process of sample brittle failure of the present invention:
1) sample is fixing: be cut into microscler by flat sheet membranes or sheet plant sample; Put it on the base of sample fixing device and (note: need to stretch out a part), then put compressing tablet, and with screw, compressing tablet is fixed, sample is fixed.
2) liquid nitrogen is added in liquid nitrogen container: liquid nitrogen is added liquid nitrogen container, general needs about 8 liters.
3) cooling of sample becomes fragile: the sample fixing device fixing sample is put into liquid nitrogen container, sample is cooled and becomes fragile, and case top lid built.
4) brittle failure of sample: pick up impact bar aim at sample fix side carry out moment impact.
5) take out the sample after brittle failure: the upper cover opening housing, sample fixing device is taken out, in the accommodation section of sample fixing device, can fall to having the sample after brittle failure.
6) sample is carried out drying process, be put into observation test under scanning electron microscope.
It is as follows that sample section prepared by the present invention and additive method obtain section observations under a scanning electron microscope:
As shown in Figure 4, be the microscopical observations of toughness film's cross-sectional scanning electron utilizing device of the present invention to prepare.
As shown in Figure 5, be the microscopical observations of plant leaf blade cross-sectional scanning electron utilizing device of the present invention to prepare.
Claims (5)
1. prepare a low-temperature brittle fracture device for scanning electron microscope sample section, it comprises:
One sample fixing device, the base surrounding of this sample fixing device is provided with a circle wallboard, makes to form an accommodation section between base and wallboard;
Be provided with screw above two relative wallboard end faces, one of them wallboard being provided with screw is provided with several grooves, for placing cylindrical sample;
Two pressing plates are tabular, are provided with the through hole corresponding with the screw on wallboard end face, and the face of one of them pressing plate 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;
This housing is the container that the cold material of heat insulation is made, and is provided with two impact openings, for being stretched in housing by impact bar inside the corresponding wallboard being provided with screw of upper cover of 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 accommodation section.
3. low-temperature brittle fracture device according to claim 1, wherein, the base of sample fixing device is teflon, is provided with some apertures entering for liquid nitrogen.
4. low-temperature brittle fracture device according to claim 1, wherein, sample fixing device is provided with puies forward indigo plant.
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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| 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 true CN104316730A (en) | 2015-01-28 |
| CN104316730B CN104316730B (en) | 2017-01-18 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699167A (en) * | 2016-01-26 | 2016-06-22 | 哈尔滨工业大学深圳研究生院 | Flexible film brittle failure method |
| WO2018000350A1 (en) * | 2016-06-30 | 2018-01-04 | 周肇梅 | Method for fracturing fixable film |
| CN107765038A (en) * | 2017-09-13 | 2018-03-06 | 上海海洋大学 | The fixing device of AFM substrate functional modification |
| CN107976460A (en) * | 2017-11-06 | 2018-05-01 | 上海恩捷新材料科技股份有限公司 | Freezing sample preparation device and method for making sample 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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| 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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| US5654546A (en) * | 1995-11-07 | 1997-08-05 | Molecular Imaging Corporation | Variable temperature scanning probe microscope based on a peltier device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699167A (en) * | 2016-01-26 | 2016-06-22 | 哈尔滨工业大学深圳研究生院 | Flexible film brittle failure method |
| WO2018000350A1 (en) * | 2016-06-30 | 2018-01-04 | 周肇梅 | Method for fracturing fixable film |
| CN107765038A (en) * | 2017-09-13 | 2018-03-06 | 上海海洋大学 | The fixing device of AFM substrate functional modification |
| CN107765038B (en) * | 2017-09-13 | 2020-04-17 | 上海海洋大学 | Fixing device for functional modification of atomic force microscope substrate |
| CN107976460A (en) * | 2017-11-06 | 2018-05-01 | 上海恩捷新材料科技股份有限公司 | Freezing sample preparation device and method for making sample 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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| CN104316730B (en) | 2017-01-18 |
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