CN109950117A - A kind of graphite oxide olefinic carbon support film transmission electron microscope carrier net - Google Patents
A kind of graphite oxide olefinic carbon support film transmission electron microscope carrier net Download PDFInfo
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- CN109950117A CN109950117A CN201910200704.6A CN201910200704A CN109950117A CN 109950117 A CN109950117 A CN 109950117A CN 201910200704 A CN201910200704 A CN 201910200704A CN 109950117 A CN109950117 A CN 109950117A
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Abstract
A kind of graphite oxide olefinic carbon support film transmission electron microscope carrier net, the present invention carries out spin coating by mature spin coating method in smooth substrate, obtain the graphene film that structure is uniform, thickness is controllable, and support grid further is prepared using ionic salt secondary transfer, low hydrophilic collective effect after the hydration of ion of ion salt, the slightly water-wet of silicon and graphene reduction, allows graphene and substrate is cracking is detached from；Meanwhile ionic salt also helps cross-linked graphene, plays certain humidification；By the invention it is possible to very simple and efficiently uniform graphene oxide membrane is laid on bearing assembly.
Description
Technical field
The present invention relates to a kind of transmission electron microscope carrier nets and preparation method thereof, are used for transmission electron microscopy more particularly to one kind
The redox graphene carbon of mirror supports film transmission electron microscope carrier net and preparation method thereof.
Background technique
Transmission electron microscope makees light source because of the electronics for using wavelength shorter, it can be seen that optical microscopy can not be seen
200nm structure below, while guaranteeing high-resolution, because of the above characteristic, it in material science, the fields such as life science
Through becoming indispensable detection means.Since the diameter of protein and various nano materials is smaller and dispersed fine, in order to
It can ensure that sample can carry in support grid, one layer of organic film can be covered in support grid, referred to as " support film ".But due to supporting film to lead
It is electrically poor, it is easy to generate charge accumulated under the irradiation of electron beam, makes elegant, bounce even support film rupture of sample etc..For
Solution this problem can improve electric conductivity by spraying one layer of graphene on organic support film, however directly support
Graphene film is prepared on film, thickness is uncontrollable, and film is uneven, this significantly limits this graphene with lamellar structure
Application in Electronic Speculum support grid.
Summary of the invention
The purpose of the present invention is to provide one kind to have structure uniform, the uniform transmission electron microscope carrier net of thickness.
The purpose of the present invention is what is be achieved through the following technical solutions: a kind of graphite oxide olefinic carbon support film transmission electron microscope carrier
Net, including bearing assembly, the bearing assembly have hollow hole；It further include the few layer graphene oxide being covered on hollow hole,
The number of plies of widow's layer graphene oxide is less than 30 layers.Widow's layer graphene oxide is covered in the carrying by the following method
On component:
Ionic salt is added into graphene oxide solution, is spun on silicon wafer after mixing；Surface is loaded with graphite
The silicon wafer of alkene film is placed in reproducibility steam, carries out electronation to the graphene oxide on its surface；By the silicon after reduction treatment
Piece is put into deionized water with certain orientation, so that the graphene oxide after reduction peels off automatically, is floated on the water surface；With holding
It carries component to pick up from the bottom up, redox graphene film is laid on bearing assembly, naturally dry.
Further, the material of the bearing assembly is selected from copper, nickel, molybdenum, titanium, gold, carbon etc..
Further, whether the bearing assembly surface, which has, is supported film.
Further, the solvent of graphene oxide solution is by water, methanol, ethyl alcohol, N-Methyl pyrrolidone, acetone, diformazan
Sulfoxide, pyridine, dioxane, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, tetrahydrofuran, butanone, ethylene glycol, two
One of glycol is a variety of by any proportion mixing composition.
Further, the incidence of the silicon wafer is horizontal by 10-45 degree.
Further, the quality of the ionic salt of addition is the 1%~0.1% of the quality of graphene oxide.
The beneficial effects of the present invention are: the present invention carries out spin coating by mature spin coating method in smooth substrate, obtain
Graphene film uniform to structure, thickness is controllable, and support grid is further prepared using ionic salt secondary transfer, ion salt
Low hydrophilic collective effect after hydration of ion, the slightly water-wet of silicon and graphene reduction, so that graphene and base
Bottom cracking can be detached from；Meanwhile ionic salt also helps cross-linked graphene, plays certain humidification；By this hair
It is bright, it can be laid on bearing assembly with very simple and efficiently by uniform graphene oxide membrane.
Detailed description of the invention
Fig. 1 a and b are respectively the transmission electron microscope picture of Electronic Speculum support grid a1 and a2, and c is the support grid (200KeV) of not cover film；
Fig. 2 a and b are respectively the transmission electron microscope picture of Electronic Speculum support grid a1 and a2 observation after ten minutes.
Specific embodiment
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it should not be understood as limiting the scope of the invention, those skilled in the art's content according to the present invention is made
Nonessential change and adjustment, all belong to the scope of protection of the present invention.
Embodiment 1:
The graphene oxide solution that 100ml concentration is 10ug/ml is prepared, thereto plus the sodium chloride of 1ug, is uniformly mixed
Afterwards, it is spun on silicon wafer with certain speed, obtains the graphene oxide membrane with a thickness of 30nm；Surface is loaded with to the silicon of graphene film
Piece is placed in iodine steam, is carried out electronation 10 minutes to the graphene oxide on its surface；By the silicon wafer after reduction treatment to incline
Oblique 45 degree of angles are put into deionized water, and the graphene oxide after reduction peels off automatically, floats on the water surface；With carbon net from lower past
On pick up, redox graphene film is laid on bearing assembly, naturally dry, obtains Electronic Speculum support grid a1.
Comparative example 1
The graphene oxide solution that 100ml concentration is 10ug/ml is prepared, is directly revolved according to the identical spin coating parameters of embodiment
It is online to be coated in carbon, naturally dry obtains Electronic Speculum support grid a2.
The transmission electron microscope picture (200KeV) of Electronic Speculum support grid a1 and a2 as shown in figures i a andb, it can be seen from the figure that Electronic Speculum carry
It is uniform on the whole to net a1, and support grid a2 is only that part is uniform, this has made in the peep hole of part thickness (graphene number of plies)
It is different.
It is observed under above-mentioned bombarding energy after ten minutes, support grid a2 has apparent chromatic aberration, this may be because of the stone
Black alkene film-strength is weaker, causes in high-power electron beam bombardment lower film structural failure, and support grid a1 is substantially without chromatic aberration.Respectively
As shown in Fig. 2 a and b.
Claims (6)
1. a kind of graphite oxide olefinic carbon supports film transmission electron microscope carrier net, including bearing assembly, the bearing assembly to have hollow hole；
It is characterized in that, further including the few layer graphene oxide being covered on hollow hole, the number of plies of widow's layer graphene oxide is less than
30 layers.Widow's layer graphene oxide is covered in by the following method on the bearing assembly:
Ionic salt is added into graphene oxide solution, is spun on silicon wafer after mixing；Surface is loaded with graphene film
Silicon wafer be placed in reproducibility steam, electronation is carried out to the graphene oxide on its surface；By the silicon wafer after reduction treatment with
Certain orientation is put into deionized water, so that the graphene oxide after reduction peels off automatically, is floated on the water surface；With carrying group
Part picks up from the bottom up, and redox graphene film is laid on bearing assembly, naturally dry.
2. graphite oxide olefinic carbon as described in claim 1 supports film transmission electron microscope carrier net, it is characterised in that: the bearing assembly
Material be selected from copper, nickel, molybdenum, titanium, gold, carbon etc..
3. graphite oxide olefinic carbon according to claim 1 supports film transmission electron microscope carrier net, which is characterized in that the carrying group
Whether part surface, which has, is supported film.
4. graphite oxide olefinic carbon as described in claim 1 supports film transmission electron microscope carrier net, it is characterised in that: graphene oxide is molten
The solvent of liquid is by water, methanol, ethyl alcohol, N-Methyl pyrrolidone, acetone, dimethyl sulfoxide, pyridine, dioxane, N, N- dimethyl
One of formamide, DMAC N,N' dimethyl acetamide, tetrahydrofuran, butanone, ethylene glycol, diethylene glycol (DEG) are a variety of mixed by any proportion
It is combined into.
5. graphite oxide olefinic carbon according to claim 1 supports film transmission electron microscope carrier net, which is characterized in that the silicon wafer
Incidence is horizontal by 10-45 degree.
6. graphite oxide olefinic carbon according to claim 1 supports film transmission electron microscope carrier net, which is characterized in that the ion of addition
The quality of type salt is the 1%~0.1% of the quality of graphene oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910200704.6A CN109950117B (en) | 2019-03-17 | 2019-03-17 | Transmission electron microscope carrier net of graphene oxide carbon supporting film |
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| CN201910200704.6A CN109950117B (en) | 2019-03-17 | 2019-03-17 | Transmission electron microscope carrier net of graphene oxide carbon supporting film |
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| CN109950117B CN109950117B (en) | 2020-12-08 |
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Cited By (3)
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| CN110540195A (en) * | 2019-08-08 | 2019-12-06 | 广东工业大学 | Graphene nanopore array and preparation method and application thereof |
| CN113960089A (en) * | 2020-07-20 | 2022-01-21 | 清华大学 | Multifunctional graphene carrying net and preparation method 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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| 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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| CN109950117B (en) | 2020-12-08 |
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