CN107093543A - A kind of graphite oxide olefinic carbon supports film transmission electron microscope carrier net and preparation method thereof - Google Patents
A kind of graphite oxide olefinic carbon supports film transmission electron microscope carrier net and preparation method thereof Download PDFInfo
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- CN107093543A CN107093543A CN201710214991.7A CN201710214991A CN107093543A CN 107093543 A CN107093543 A CN 107093543A CN 201710214991 A CN201710214991 A CN 201710214991A CN 107093543 A CN107093543 A CN 107093543A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 230000005540 biological transmission Effects 0.000 title claims abstract description 17
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 13
- 239000010439 graphite Substances 0.000 title claims abstract description 13
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical class CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims 2
- 150000001412 amines Chemical class 0.000 claims 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 10
- 150000001336 alkenes Chemical class 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- -1 graphite Alkene Chemical class 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229940113088 dimethylacetamide Drugs 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Film transmission electron microscope carrier net and preparation method thereof is supported the invention discloses a kind of graphite oxide olefinic carbon.Its step of, is as follows：(1) take and a piece of be commonly placed on without carbon film Electronic Speculum contained network on filter paper；(2) graphene oxide solution is uniformly layered on to contained network upper surface；(3) solvent is made to volatilize under normal temperature or heating condition.The present invention can prepare ultra-thin carbon and support film, realize high contrast, high-resolution.And unreduced carbon supports there is elecrtonegativity functional group on film, can strengthen the adhesiveness of carbon film and sample.This kind prepares carbon and supports film method has the advantages that simple to operate, with low cost.
Description
Technical field
It is more particularly to a kind of to be used for transmission electron microscopy the present invention relates to a kind of transmission electron microscope carrier net and preparation method thereof
The graphite oxide olefinic carbon of mirror supports film transmission electron microscope carrier net and preparation method thereof.
Background technology
Transmission electron microscope using the shorter electronics of wavelength because making light source, it can be seen that what light microscope can not be seen
Below 200nm structure, while ensureing high-resolution, because above characteristic, it is in material science, in the field such as life science
Through as indispensable detection means.Because the diameter of protein and various nano materials is smaller and dispersed fine, in order to
It can ensure that sample can be carried in contained network, one layer of organic film can be covered in contained network, is referred to as " support film ".But due to supporting film to lead
It is electrically poor, it is easy to produce charge accumulated under the irradiation of electron beam, makes elegant sample, bounce or even support film rupture etc..For
This problem is solved, electric conductivity can be improved by spraying one layer of carbon film on organic support film, general carbon film thickness is in 7-
10nm.And ultrathin carbon films refer to carbon film of the thickness in 3-5nm.The thickness of carbon film is thinner, and its contrast is higher, and resolution ratio is higher；
But excessively thin carbon film can cause its mechanical strength step-down.Existing carbon supports film preparation complex process and thickness is thicker, for
Sample segment is unable to reach contrast requirement.
Graphene is the two-dimentional monoatomic layer crystal being bonded by carbon atom with hexagon, the chemical constitution based on it, graphite
Alkene has many excellent physicochemical properties for exceeding traditional material, it is easy to modification and large-scale production.Its thickness only has
0.34nm, and high mechanical strength.
The content of the invention
It is an object of the invention to provide the graphite oxide that one kind has high mechanical properties, high sample adhesiveness and high contrast
Olefinic carbon supports film transmission electron microscope carrier net and preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions：A kind of graphite oxide olefinic carbon supports film transmission electron microscope carrier
Net, including bearing assembly, the bearing assembly have hollow hole；Also include the few layer graphene oxide being covered on hollow hole,
The number of plies of the few layer graphene oxide is less than 10 layers.
A kind of graphite oxide olefinic carbon supports the preparation method of film transmission electron microscope carrier net, and this method is：By concentration be 0.001~
10mg/mL graphene oxide solution is uniformly layered on bearing assembly surface, and Electronic Speculum contained network is obtained after drying.
Further, the material of the bearing assembly is selected from copper, nickel, molybdenum, titanium, gold, carbon.
Further, whether the bearing assembly surface, which has, is supported film.
Further, the solvent of graphene oxide solution is by water, methanol, ethanol, 1-METHYLPYRROLIDONE, acetone, diformazan
Sulfoxide, pyridine, dioxane, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, tetrahydrofuran, butanone, ethylene glycol, two
One or more in glycol are by any proportioning mixing composition；
Further, graphene oxide solution is uniformly layered on bearing assembly surface, is realized by the following method：Directly pass through
Dropwise addition method makes solution cover contained network；Contained network immersion again is lifted out in the solution；Or by solution spin coating or be applied directly to
In contained network；
Further, the speed of spin coating is in 300~8000rpm；
Further, the graphene solution volume in contained network is added dropwise in 2~20 μ L；
Further, contained network is soaked into the pull rate for lifting out again in the solution in 0.1~200mm/min.
The beneficial effects of the invention are as follows：Form the few-layer graphene alkene is covered on hollow hole by the present invention by simple method, most
It is thin to can reach single-layer graphene oxide thickness 0.34nm；Ensure that sample shoot when high contrast and high-resolution while it is same
When taken into account intensity, it is ensured that in load sample product, carbon film will not rupture；Further, since surface of graphene oxide carries many elecrtonegativities
Functional group, can produce good adhesive attraction by electrostatic interaction to electropositive sample；Graphene oxide preparation technology is simple
And existing large-scale production, simply, raw material is cheap and easy to get for the preparation method step of this kind of carbon film.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph and partial enlarged drawing of ultrathin carbon films contained network prepared by the present invention；
Fig. 2 is the electron diffraction diagram of ultrathin carbon films contained network prepared by the present invention；
Fig. 3 is the electron microscope that ultrathin carbon films contained network prepared by the present invention loads silicon grain.
Embodiment
A kind of graphite oxide olefinic carbon supports film transmission electron microscope carrier net and preparation method thereof, it the step of it is as follows：(1) take a piece of
Commonly it is placed on without carbon film Electronic Speculum contained network on filter paper；(2) graphene oxide solution is uniformly layered on to contained network upper surface；(3) normal temperature or
Solvent is set to volatilize under heating condition.
The present invention is a kind of with high mechanical properties, high sample adhesiveness, the preparation side of the ultrathin carbon films of high contrast in providing
Method.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
Bright, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art makes according to present disclosure
Nonessential change and adjustment, belong to protection scope of the present invention.
Embodiment 1：
(1) the transmission electron microscope copper grid without 1000 mesh for supporting film is taken to be placed on filter paper；
(2) it is 0.1mgmL concentration to be pipetted with liquid-transfering gun-1The μ L of graphene oxide water solution 5, copper mesh table is dropped in naturally
Face；
(3) above-mentioned bulk sample is placed in clean dustless room temperature environment, done until water volatilizees naturally.
Find out that graphene sheet layer is laid on hollow hole by Fig. 1, Fig. 2 electron diffraction diagram is found out, in most thick place only
It is made up of three layer graphenes.The contained network is used for the sample preparation of silicon nanoparticle, as shown in figure 3, in fig. 3 it can be seen that this kind
Graphene supports that film-strength is higher, still keeps supporting the integrality of film after silicon nanoparticle has been loaded.
Embodiment 2：
(1) transmission electron microscope carrier net for 200 mesh that film is supported with micro-grid is taken, concentration is dipped in for 0.5mgmL-1Oxygen
Changing graphite alkene ethanol solution, with 1mm/min speed, uniformly lifting comes up again；
(2) above-mentioned sample is placed on 40 DEG C of heating in clean dustless baking oven, done until water volatilizees naturally.By test,
The graphene supports that film-strength is higher, and contrast is high.
Embodiment 3：
(1) transmission electron microscope carrier net for 300 mesh that film is supported with micro-grid is taken, by the oxidation fossil that concentration is 0.001mg/mL
Black alkene ethanol solution carries out spin coating 5-10s to transmission electron microscope carrier net, and the speed of spin coating is 300rpm；
(2) above-mentioned sample is placed on 40 DEG C of heating in clean dustless baking oven, done until water volatilizees naturally.Spread out by electronics
Test is penetrated, is only made up of in most thick place 10 layer graphenes, the graphene supports that film-strength is higher, and contrast is high.
Embodiment 4：
(1) transmission electron microscope carrier net for 300 mesh that film is supported with micro-grid is taken, the oxidation that concentration is 10mg/mL is dipped in
With 1mm/min speed, uniformly lifting comes up graphite alkene tetrahydrofuran solution again；
(2) above-mentioned sample is placed on 40 DEG C of heating in clean dustless baking oven, done until water volatilizees naturally.By test,
The graphene supports that film-strength is higher, and contrast is high.
Claims (9)
1. a kind of graphite oxide olefinic carbon supports film transmission electron microscope carrier net, including bearing assembly, the bearing assembly has hollow hole；
Characterized in that, also including the few layer graphene oxide being covered on hollow hole, the number of plies of the few layer graphene oxide is less than
10 layers.
2. the graphite oxide olefinic carbon described in a kind of claim 1 supports the preparation method of film transmission electron microscope carrier net, it is characterised in that
This method is：Concentration is uniformly layered on bearing assembly surface for 0.001~10mg/mL graphene oxide solution, after drying
To Electronic Speculum contained network.
3. preparation method as claimed in claim 2, it is characterised in that:The material of the bearing assembly be selected from copper, nickel, molybdenum, titanium,
Gold, carbon etc..
4. preparation method according to claim 2, it is characterised in that whether the bearing assembly surface, which has, is supported that film is equal
Can.
5. preparation method as claimed in claim 2, it is characterised in that:The solvent of graphene oxide solution is by water, methanol, second
Alcohol, 1-METHYLPYRROLIDONE, acetone, dimethyl sulfoxide, pyridine, dioxane, N,N-dimethylformamide, N, N- dimethylacetamides
One or more in amine, tetrahydrofuran, butanone, ethylene glycol, diethylene glycol (DEG) are by any proportioning mixing composition.
6. preparation method as claimed in claim 2, it is characterised in that:Graphene oxide solution is uniformly layered on bearing assembly table
Face, is realized by the following method：Directly solution is set to cover contained network by dropwise addition method.Contained network immersion is lifted out again in the solution
Come；Or by solution spin coating or be applied directly in contained network.
7. preparation method as claimed in claim 6, it is characterised in that:The speed of spin coating is in 300~8000rpm.
8. preparation method as claimed in claim 6, it is characterised in that:Be added dropwise graphene solution volume in contained network 2~
20μ。
9. preparation method as claimed in claim 6, it is characterised in that:Contained network is soaked to the lifting for lifting out again in the solution
Speed is in 0.1~200mm/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710214991.7A CN107093543A (en) | 2017-04-02 | 2017-04-02 | A kind of graphite oxide olefinic carbon supports film transmission electron microscope carrier net and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710214991.7A CN107093543A (en) | 2017-04-02 | 2017-04-02 | A kind of graphite oxide olefinic carbon supports film transmission electron microscope carrier net and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN107093543A true CN107093543A (en) | 2017-08-25 |
Family
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|---|---|---|---|
| CN201710214991.7A Pending CN107093543A (en) | 2017-04-02 | 2017-04-02 | A kind of graphite oxide olefinic carbon supports film transmission electron microscope carrier net and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109950117A (en) * | 2019-03-17 | 2019-06-28 | 杭州高烯科技有限公司 | A kind of graphite oxide olefinic carbon support film transmission electron microscope carrier net |
| CN112582244A (en) * | 2020-12-14 | 2021-03-30 | 中南林业科技大学 | Non-porous TEM grid-supported supporting film based on wood slices and preparation method and application thereof |
| EP4060094A1 (en) | 2021-03-18 | 2022-09-21 | Jozef Stefan Institute | An apparatus for anodic oxidation of very small metal grids |
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|---|---|---|---|---|
| CN102142348A (en) * | 2011-02-18 | 2011-08-03 | 南京大学 | Supporting membrane of transmission electron microscope sample and manufacturing method for transmission electron microscope sample |
| WO2015022510A1 (en) * | 2013-08-13 | 2015-02-19 | Medical Research Council | Electron microscopy sample support comprising porous metal foil |
| CN105140083A (en) * | 2015-06-24 | 2015-12-09 | 中国科学院生物物理研究所 | Preparation method of grid of transmission electron microscope |
| CN105658574A (en) * | 2013-08-13 | 2016-06-08 | 医药研究委员会 | Graphene modification |
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2017
- 2017-04-02 CN CN201710214991.7A patent/CN107093543A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102142348A (en) * | 2011-02-18 | 2011-08-03 | 南京大学 | Supporting membrane of transmission electron microscope sample and manufacturing method for transmission electron microscope sample |
| WO2015022510A1 (en) * | 2013-08-13 | 2015-02-19 | Medical Research Council | Electron microscopy sample support comprising porous metal foil |
| CN105658574A (en) * | 2013-08-13 | 2016-06-08 | 医药研究委员会 | Graphene modification |
| CN105140083A (en) * | 2015-06-24 | 2015-12-09 | 中国科学院生物物理研究所 | Preparation method of grid of transmission electron microscope |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109950117A (en) * | 2019-03-17 | 2019-06-28 | 杭州高烯科技有限公司 | A kind of graphite oxide olefinic carbon support film transmission electron microscope carrier net |
| CN109950117B (en) * | 2019-03-17 | 2020-12-08 | 杭州高烯科技有限公司 | Transmission electron microscope carrier net of graphene oxide carbon supporting film |
| CN112582244A (en) * | 2020-12-14 | 2021-03-30 | 中南林业科技大学 | Non-porous TEM grid-supported supporting film based on wood slices and preparation method and application thereof |
| EP4060094A1 (en) | 2021-03-18 | 2022-09-21 | Jozef Stefan Institute | An apparatus for anodic oxidation of very small metal grids |
| WO2022194832A1 (en) | 2021-03-18 | 2022-09-22 | Jozef Stefan Institute | An apparatus for anodic oxidation of very small metal grids |
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