CN103512785A - Method for preparing section SEM sample by micropore thin film material - Google Patents
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- CN103512785A CN103512785A CN201310482162.9A CN201310482162A CN103512785A CN 103512785 A CN103512785 A CN 103512785A CN 201310482162 A CN201310482162 A CN 201310482162A CN 103512785 A CN103512785 A CN 103512785A
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Abstract
The invention discloses a method for preparing a section SEM (scanning electron microscope) sample through a micropore thin film material. The method comprises the following steps of 1, firstly, cutting the micropore thin film material into a rectangular thin film sample; 2, placing the rectangular thin film sample prepared in the step 1 into a container and then injecting a liquid into the container to enable the liquid to coat the whole thin film sample; 3, placing the container containing the thin film sample and the liquid in the step 2 into a vacuum standing machine to carry out vacuumizing standing, enabling the thin film sample to be fully impregnated with the liquid and the micropores of the thin film sample to be filled with the liquid in the vacuum environment, and at the same time, discharging air bubbles in the thin film sample and the liquid through vacuum standing; 4, taking out the container subjected to vacuumizing standing and then carrying out cooling to change the liquid into a solidified body; 5, taking out the solidified body containing the thin film sample and splitting the solidified body; 6, drying the split solidified body to obtain the split sample with a section. The method has the advantages of simplicity, high operability, high sample reproducibility and capability of keeping a complete hole shape structure.
Description
Technical field
The present invention relates to high molecular film material measuring technology, especially relate to a kind of method prepared by profile scanning electron microscopic sample of microporous membrane material.
Background technology
Along with the continuous lifting of science and technology level, to the detection means of material and analytical approach also in continuous progress.In manufacturing industry, from finding material, exploitation processing procedure, analytical property, improving performance, to failure analysis, often need to use electron-microscope scanning (SEM) analysis, from this angle, electron microscope is one of important checkout equipment of associated each work-in-process concrete analysis technology.
SEM is a kind of microscopic appearance Observations Means between transmission electron microscope and optical microscope, can directly utilize the physical property of sample surfaces material to carry out microcosmic imaging.Scanning electron microscope has higher enlargement factor, can be adjustable continuously between doubly to hundreds of thousands at hundreds of; And the visual field is large, imaging is rich in the advantages such as stereoscopic sensation, utilizes scanning electron microscope can directly observe the surface structure of various samples, and the microcosmos area of material is carried out to crystal structure analysis.
Electron-microscope scanning is as one of important analysis means, but the method for testing of section SEM report seldom, and the test that high molecule micropore membraneous material is carried out to section SEM still less, on this due to membraneous material thinner thickness, material is softer, and intensity is compared with high, and the difficulty of sample preparation is very large.At present to high-molecular porous film sample preparation and test be also difficult to use section SEM.In the actual test process of high molecule micropore film, the preparation method of the section SEM sample that neither one is unified, and method in the past is also difficult to prepare that reappearance is higher, the sample of complete pass, has so also limited the observation analysis to microporous membrane material internal micromechanism.
Summary of the invention
For overcoming above-mentioned shortcoming, the object of the present invention is to provide a kind of preparation method simple, workable, equipment and frock clamp are required low, and reappearance is higher, can retain method prepared by the profile scanning electron microscopic sample of the microporous membrane material of complete pass structure.
The present invention is achieved through the following technical measures, and a kind of method prepared by profile scanning electron microscopic sample of microporous membrane material, comprises the steps:
1), first microporous membrane material is cut into rectangular film sample;
2), rectangle film sample prepared by step 1) puts into a container, then, to filling liquid in container, liquid can all be wrapped up film sample;
3), by step 2) in the container that carries film sample and liquid be positioned in vacuum standing machine, vacuumize standing, in vacuum environment, allow liquid infiltrate to film sample fully inner, be filled in the micropore of film sample, by vacuum is standing, bubble in film sample and liquid discharged simultaneously;
4), the container vacuumizing after standing is taken out, then carry out the cooling liquid that makes and become solidifying body;
5), the interior solidifying body that has a film sample is taken out, solidifying body is split off;
6), the solidifying body of division is dried to the sample with section that obtains splitting off.
As a kind of optimal way, after step 6), also comprise step 7), the sample with section is sticked on conducting resinl, after section metal spraying, complete the preparation of scanning electron microscope example.Then carry out the shooting of scanning electron microscope.
As a kind of optimal way, described container is bag film.
As a kind of optimal way, state step 2) in liquid be the liquid good to film sample wellability.
As a kind of optimal way, described liquid is any one or more the mixing in ethanol, acetone, methylene chloride or carbonic ester.
As a kind of optimal way, described step 2) centre position of middle film sample in liquid.
As a kind of optimal way, the vacuum tightness in described step 3) is not higher than-0.09MPa, and vacuum time of repose is not less than 5min.
As a kind of optimal way, the neutralization of described step 4) is cooled to and under sealing, in liquid nitrogen, is cooled to solidifying body.
As a kind of optimal way, first whether described step 5) observe in solidifying body without bubble, if any entering step 4) after dissolving; As without bubble, solidifying body is taken out, with Jie's cutter, on solidifying body surface, mark one linear pattern impression, then along impression direction, with hard thing, solidifying body is broken into pieces rapidly, now the micropore of film sample is along with the liquid solidifying is together by the neat two halves that are divided into.
The present invention utilizes the high-molecular porous film of liquid-soaked, makes liquid filling in film micropore, the low temperature that recycling produces fast (as being-196 ℃ with liquid nitrogen boiling point-77K()), it is solidified rapidly.In the process of solidifying, because infiltrating, barrier film micropore place is filled with liquid, and can guarantee that the microcellular structure of sample interior keeps the truly complete of shape in the process of brittle failure sample preparation, thereby prepare the thin-membrane section sample with true complete pass.
The present invention has advantages of following:
(1) prepare the simple and easy operating of the method for sample, consumptive material used is less, and the sample preparation cycle is short, and less demanding to frock clamp;
(2) can protect fully the microcellular structure of macromolecule membrane not to be destroyed in sample making course, can access true complete aperture structure;
(3) utilize liquid nitrogen boiling point low, free from extraneous odour, corrosion-free, and the feature such as noresidue after volatilization, the sample of preparation is not polluted and section neat, be beneficial to the morphology analysis of scanning electron microscope.
Accompanying drawing explanation
Fig. 1 is unilateral stretching polypropylene film section Sample Scan Electronic Speculum picture in the embodiment of the present invention;
Fig. 2 is unilateral stretching polypropylene ceramic coated thin-membrane section Sample Scan Electronic Speculum picture in the embodiment of the present invention.
Embodiment
Below in conjunction with embodiment and contrast accompanying drawing the present invention is described in further detail.
1), first microporous membrane material is cut into rectangular film sample;
In this enforcement, be will on polypropylene film to be measured, polypropylene ceramic coated membrane sample, to intercept respectively rectangle sample with cutting knife, sample size is about 10mm * 30mm;
2), rectangle film sample prepared by step 1) puts into a container, then, to filling liquid in container, liquid can all be wrapped up film sample;
In this enforcement, two samples that cut are respectively charged in two sample sacks, then in each sample sack, inject 200ml left and right analysis absolute alcohol, alcohol liquid level covers sample, and sample is fully immersed in alcohol; Liquid can also be that alcohol, acetone, methylene chloride, carbonates etc. can infiltrate to the organic solvent of one or more mixing of high molecule micropore film inside in other embodiments;
3), by step 2) in the container that carries film sample and liquid be positioned in vacuum standing machine, vacuumize standing, in vacuum environment, allow liquid infiltrate to film sample fully inner, be filled in the micropore of film sample, by vacuum is standing, bubble in film sample and liquid discharged simultaneously;
In this enforcement, be that the sample sack of putting into sample and alcohol (open state) is placed in to vacuum standing machine, open the pattern, be set to-0.095MPa of vacuum tightness of vacuumizing; In order to guarantee that alcohol is fully immersed in film inside, the bubble between solvent and sample can be eliminated completely, and vacuum time of repose is set to 10min; Vacuum tightness is not generally higher than-0.09MPa in other embodiments, and vacuum time of repose is not less than 5min;
4), the container vacuumizing after standing is taken out, then carry out the cooling liquid that makes and become solidifying body;
In this enforcement, be that liquid nitrogen is poured in a steel cylinder, sealing bag is taken out and puts into liquid nitrogen from vacuum tank, the liquid level of liquid nitrogen should be higher than the liquid level of alcohol in sealing bag, after freezing 15min, the interior alcohol of bag to be sealed all solidifies and without bubble, tweezers gripping goes out the sample after " freezing ";
5), the interior solidifying body that has a film sample is taken out, solidifying body is split off;
In this enforcement, be at the sample surfaces of " freezing ", to mark together straight trace with Jie's cutter, then along the direction of streak, break into pieces solid-state alcohol is broken, film now also splits together.In operating process, the measure that properly protects, is strictly on guard against the generation of the perils such as frostbite;
6), the solidifying body of division is dried to the sample with section that obtains splitting off.
In this enforcement, be that the sample of preparing in previous step is put into 60 ℃ of constant temperature oven bakings or normal temperature environment, after alcohol volatilization, cutting fritter sample sticks in respectively on conducting resinl, completes the preparation of scanning electron microscope example after metal spraying, then carries out the shooting of scanning electron microscope.
With reference to accompanying drawing, Fig. 1 is unilateral stretching polypropylene film section Sample Scan Electronic Speculum picture in the present embodiment; Fig. 2 is for originally executing unilateral stretching polypropylene ceramic coated thin-membrane section Sample Scan Electronic Speculum picture in example.As can be seen from Figure two samples all do not have to pollute and section neat, the pattern of scanning electron microscope can retain complete pass structure, imaging is rich in stereoscopic sensation, is conducive to the microcosmos area of material to carry out crystal structure analysis.
More than that method prepared by the profile scanning electron microscopic sample of microporous membrane material of the present invention is set forth; be used for helping to understand the present invention; but embodiments of the present invention are not restricted to the described embodiments; anyly do not deviate from the change done under the principle of the invention, modification, substitute, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (9)
1. the method that prepared by the profile scanning electron microscopic sample of microporous membrane material, is characterized in that comprising the steps:
1), first microporous membrane material is cut into rectangular film sample;
2), rectangle film sample prepared by step 1) puts into a container, then, to filling liquid in container, liquid can all be wrapped up film sample;
3), by step 2) in the container that carries film sample and liquid be positioned in vacuum standing machine, vacuumize standing, in vacuum environment, allow liquid infiltrate to film sample fully inner, be filled in the micropore of film sample, by vacuum is standing, bubble in film sample and liquid discharged simultaneously;
4), the container vacuumizing after standing is taken out, then carry out the cooling liquid that makes and become solidifying body;
5), the interior solidifying body that has a film sample is taken out, solidifying body is split off;
6), the solidifying body of division is dried to the sample with section that obtains splitting off.
2. the method that prepared by the profile scanning electron microscopic sample of microporous membrane material according to claim 1, it is characterized in that: after step 6), also comprise step 7), the sample with section is sticked on conducting resinl, after section metal spraying, complete the preparation of scanning electron microscope example.
3. the method that prepared by the profile scanning electron microscopic sample of microporous membrane material according to claim 1 and 2, is characterized in that: described container is bag film.
4. the method that prepared by the profile scanning electron microscopic sample of microporous membrane material according to claim 1 and 2, is characterized in that: the liquid described step 2) is the liquid good to film sample wellability.
5. the method that prepared by the profile scanning electron microscopic sample of microporous membrane material according to claim 7, is characterized in that: described liquid is any one or more the mixing in ethanol, acetone, methylene chloride or carbonic ester.
6. the method that prepared by the profile scanning electron microscopic sample of microporous membrane material according to claim 1 and 2, is characterized in that: the centre position of the film sample described step 2) in liquid.
7. the method that prepared by the profile scanning electron microscopic sample of microporous membrane material according to claim 1 and 2, is characterized in that: the vacuum tightness in described step 3) is not higher than-0.09MPa, and vacuum time of repose is not less than 5min.
8. the method that prepared by the profile scanning electron microscopic sample of microporous membrane material according to claim 1 and 2, is characterized in that: the neutralization of described step 4) is cooled to and under sealing, in liquid nitrogen, is cooled to solidifying body.
9. the method that prepared by the profile scanning electron microscopic sample of microporous membrane material according to claim 1 and 2, is characterized in that: first whether described step 5) observe in solidifying body without bubble, if any entering step 4) after dissolving; As without bubble, solidifying body is taken out, with Jie's cutter, on solidifying body surface, mark one linear pattern impression, then along impression direction, with hard thing, solidifying body is broken into pieces rapidly, now the micropore of film sample is along with the liquid solidifying is together by the neat two halves that are divided into.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103792121A (en) * | 2014-02-10 | 2014-05-14 | 河北钢铁股份有限公司邯郸分公司 | Preparation method for metallurgical powdered test sample |
| CN104198766A (en) * | 2014-08-11 | 2014-12-10 | 中国石油天然气股份有限公司 | Method for eliminating depth-of-field false images during focused ion beam-scanning electron microscope (FIB-SEM) imaging |
| CN105486890A (en) * | 2014-09-11 | 2016-04-13 | 山东省地质科学研究院 | Novel method for testing fluid inclusion in minerals |
| CN106814095A (en) * | 2017-02-12 | 2017-06-09 | 马新军 | For the freezing sample preparation device of ESEM |
| 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 |
| CN109752400A (en) * | 2018-12-26 | 2019-05-14 | 上海神力科技有限公司 | A kind of fuel cell membrane electrode interfacial structure characterization sample treatment |
| CN109916942A (en) * | 2019-04-18 | 2019-06-21 | 攀钢集团攀枝花钢铁研究院有限公司 | The electron microscope characterizing method of collecting agent |
| CN110514490A (en) * | 2019-07-31 | 2019-11-29 | 东莞维科电池有限公司 | A kind of method and device making pole piece section |
| 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 |
| CN111122629A (en) * | 2020-01-08 | 2020-05-08 | 上海神力科技有限公司 | Method for manufacturing thin-film material section scanning electron microscope sample |
| CN112345568A (en) * | 2020-10-30 | 2021-02-09 | 同济大学 | Sample preparation method of fuel cell membrane electrode section structure |
| CN114112569A (en) * | 2021-11-08 | 2022-03-01 | 浙江唐锋能源科技有限公司 | Sample preparation method and cutting device for section of membrane electrode |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103792121A (en) * | 2014-02-10 | 2014-05-14 | 河北钢铁股份有限公司邯郸分公司 | Preparation method for metallurgical powdered test sample |
| CN104198766A (en) * | 2014-08-11 | 2014-12-10 | 中国石油天然气股份有限公司 | Method for eliminating depth-of-field false images during focused ion beam-scanning electron microscope (FIB-SEM) imaging |
| CN105486890A (en) * | 2014-09-11 | 2016-04-13 | 山东省地质科学研究院 | Novel method for testing fluid inclusion in minerals |
| CN106814095A (en) * | 2017-02-12 | 2017-06-09 | 马新军 | For the freezing sample preparation device of ESEM |
| CN106814095B (en) * | 2017-02-12 | 2019-05-24 | 马新军 | Freezing sample preparation device for scanning electron microscope |
| 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 |
| CN109752400A (en) * | 2018-12-26 | 2019-05-14 | 上海神力科技有限公司 | A kind of fuel cell membrane electrode interfacial structure characterization sample treatment |
| CN109752400B (en) * | 2018-12-26 | 2022-06-07 | 上海神力科技有限公司 | Method for processing characterization sample of membrane electrode interface structure of fuel cell |
| CN109916942B (en) * | 2019-04-18 | 2021-09-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Electron microscopy characterization method of collecting agent |
| CN109916942A (en) * | 2019-04-18 | 2019-06-21 | 攀钢集团攀枝花钢铁研究院有限公司 | The electron microscope characterizing method of collecting agent |
| CN110514490A (en) * | 2019-07-31 | 2019-11-29 | 东莞维科电池有限公司 | A kind of method and device making pole piece section |
| CN110514490B (en) * | 2019-07-31 | 2022-04-08 | 东莞维科电池有限公司 | Method and device for manufacturing section of pole piece |
| 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 |
| CN111122629A (en) * | 2020-01-08 | 2020-05-08 | 上海神力科技有限公司 | Method for manufacturing thin-film material section scanning electron microscope sample |
| CN111122629B (en) * | 2020-01-08 | 2024-04-09 | 上海神力科技有限公司 | Method for manufacturing thin film material section scanning electron microscope sample |
| CN112345568A (en) * | 2020-10-30 | 2021-02-09 | 同济大学 | Sample preparation method of fuel cell membrane electrode section structure |
| CN114112569A (en) * | 2021-11-08 | 2022-03-01 | 浙江唐锋能源科技有限公司 | Sample preparation method and cutting device for section of membrane electrode |
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Inventor after: Xu Jianguang Inventor after: Wang Jingang Inventor after: Li Shilong Inventor after: Chen Xiufeng Inventor after: Chen Liang Inventor after: Yang Jiafu Inventor before: Chen Xiufeng Inventor before: Chen Liang Inventor before: Yang Jiafu Inventor before: Xu Jianguang Inventor before: Li Shilong Inventor before: Wang Jingang |
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Address after: 518000 Guangdong province Shenzhen Guangming New District Office of Gongming rural road Applicant after: Shenzhen Senior Technology Material Co., Ltd. Address before: 518000, Guangdong, Shenzhen, Nanshan District Lang Road, Tong Fang information port, block A, building 5 Applicant before: SHENZHEN SENIOR TECHNOLOGY CO., LTD. |
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