CN104817073B - Method for transferring graphene film to TEM copper net - Google Patents
Method for transferring graphene film to TEM copper net Download PDFInfo
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- CN104817073B CN104817073B CN201510145260.2A CN201510145260A CN104817073B CN 104817073 B CN104817073 B CN 104817073B CN 201510145260 A CN201510145260 A CN 201510145260A CN 104817073 B CN104817073 B CN 104817073B
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- copper mesh
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- tem copper
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Abstract
The invention discloses a method for transferring a graphene film to a TEM copper net. The method comprises the following steps: adsorbing the TEM copper net to an electrostatic adsorption film, and transferring the graphene film to the TEM copper net. The TEM copper net is adsorbed on the electrostatic adsorption film, so the surface area of the copper net is macroscopically indirectly enlarged, thereby picking is convenient; indirect contact with the TEM copper net is realized in the picking process, so the destroy to the structure of the copper net is avoided; and the graphene film is transferred through the above composite substrate, so the transfer of graphene to the TEM copper net is easily realized, the problem of difficult transfer of the graphene film to a small area of the TEM copper net is solved, and the operation is simple.
Description
Technical field
The present invention relates to one and graphene film material is transferred on TEM copper mesh, in order to carry out the side of transmissioning electric mirror test
Method.
Technical background
Graphene is the two dimensional surface material with an atomic thickness formed by the hexagonal array of carbon atom.2004, English
The method that Novoselov and Geim of University of Manchester of state is peeled off by micromechanics, successfully shells from highly oriented pyrolytic graphite
Separate out Graphene, open the probability of Graphene this two-dimensional material experimental investigation from this.
Owing to Graphene has the electricity of excellence, optics, calorifics, the character such as mechanics so that it is nanoelectronics, sensor,
Before the conversion of optics, energy and storage, environmental improvement, composite and biological technical field have a very wide range of applications
Scape.
The preparation method of Graphene is broadly divided into two kinds: from bottom to top and from top to bottom.Wherein, Self-absorption Correction Factor mainly includes
Epitaxial growth method, chemical vapour deposition technique (CVD), chemical small molecule synthetic method；Top-down methods mainly includes that liquid phase is peeled off
Method, mechanical stripping method etc..At present, CVD growth Graphene is the most commonly used mode, and this method is possible not only to raw
Long large-area graphene film, and control the number of plies of Graphene within the specific limits.Graphene film prepared by this method is
Through being applied in the scientific research fields such as transparency electrode, solaode, field-effect transistor and ultracapacitor.
But, Graphene prepared by the most any method will carry out the sign of some necessity, observes its shape characteristic, knot
Brilliant performance, optical property, electric property and defect etc., assist next step research.This kind of two-dimensional material of Graphene at present
Characterization technique tended to perfect, mainly have scanning electron microscope (SEM) to characterize, transmission electron microscope (TEM) characterize, Raman (Raman)
Characterizing, XPS characterizes, and XRD characterizes, Fourier transform infrared spectroscopy sign etc..Elder generation it is typically necessary during characterization test
Being attached in substrate by material, during as characterized property of thin film with Raman, thin film needs to be attached to silicon base or silicon dioxide substrate
On, it is for the size of material and the size of substrate almost without restriction, and area of base size in range of needs all may be used.
But, transmission electron microscope characterizes utilize in the test of material character is copper mesh substrate, and people need to carry out testing
Material is transferred to just can test on TEM copper mesh.The step transferred graphene at present on TEM copper mesh is: first will rotation
The graphene film being coated with protected glue-line suspends in deionized water, grips TEM copper mesh with tweezers, and extending in deionized water will
Graphene is pulled out, then soaks and removes protection glue-line in acetone, with tweezers, transfer is had the copper mesh of Graphene from third again after having gone
Ketone takes out.There is following problem in this method:
1, the area of TEM copper mesh only has several millimeter, directly is very easy to destroy its structure with tweezers gripping so that Graphene
Thin film at damaged copper mesh position cannot self-supporting, more broken, the pattern of Graphene is observed in impact simultaneously；And gripping difficulty；
2, clipping the TEM copper mesh of the least area with tweezers to stretch into and fish for Graphene in deionized water, operation easier is high, takes
Time laborious, completing a transfer needs the most several hours even tens hours, and the technical merit of operator is required height；
3, after having removed protecting film, also need have the copper mesh of Graphene to take out from acetone transfer with tweezers, clipped to by tweezers
Graphene-structured is the most destroyed, and on copper mesh, the area of Graphene is the most limited, the effect of impact test；
4, repeatedly directly contact TEM copper mesh and Graphene with tweezers, easily introduce pollutant.
Therefore, a kind of method that can be transferred on TEM copper mesh by graphene film the most easily urgently finds.
Summary of the invention
The present invention is for avoiding the weak point existing for above-mentioned prior art, it is provided that one can be thin by Graphene the most easily
Film transfers to the method on TEM copper mesh.
The present invention solves that technical problem adopts the following technical scheme that
Graphene film is transferred to the method on TEM copper mesh by the present invention, and its feature is to carry out as follows:
Step a, by the graphene film of protected for spin coating glue-line with protection glue-line suspend upward in deionized water；
Step b, by TEM copper mesh adsorb on Electrostatic Absorption film, the area of described Electrostatic Absorption film is at least described TEM copper
4 times of web area, and the area of described Electrostatic Absorption film is not less than the area of graphene film described in step a；
Step c, with TEM copper mesh upward, the deionized water Electrostatic Absorption film in step b being extend in step a with tweezers
In, graphene film is pulled out, and makes graphene film cover described TEM copper mesh, form protection glue-line/graphite from top to bottom
Alkene thin film/TEM copper mesh/Electrostatic Absorption film composite construction；
Step d, protection step c obtained glue-line/graphene film/TEM copper mesh/Electrostatic Absorption film composite construction dry in the air naturally
After Gan, soak in acetone to remove protection glue-line, it is thus achieved that graphene film/TEM copper mesh/Electrostatic Absorption film composite construction；
Step e, on graphene film/TEM copper mesh/Electrostatic Absorption film composite construction that step d is obtained, with tweezers by TEM
Copper mesh takes off from Electrostatic Absorption film together with being positioned at graphene film thereon, and graphene film is i.e. transferred to TEM copper mesh
On.
Graphene film is transferred to the method on TEM copper mesh by the present invention, and its feature lies also in: described Electrostatic Absorption film is PET
Film, PE film or PVC film, preferably PET film.
The method of the present invention is in addition to can transferring to graphene film on TEM copper mesh, it is also possible to be transferred into other faces
In long-pending less substrate, such as silicon chip, silicon oxide, sheet glass, plastic tab, sapphire sheet, piezoid, foil etc.,
The problem solving little area graphite alkene transfer difficulty.
Additionally, the method for the present invention can be used for being transferred to by other thin-film materials on TEM copper mesh or other little area substrates,
Such as boron nitride pellicle, molybdenum disulfide film etc..
Compared with the prior art, the present invention has the beneficial effect that:
1, the present invention is by adsorbing TEM copper mesh on Electrostatic Absorption film, the most indirectly expands the surface area of copper mesh, makes
It is easy to gripping, and is not directly contacted with TEM copper mesh when gripping, it is to avoid to its structural damage；Turn by this composite substrate
Move graphene film, easily realize the Graphene transfer to TEM copper mesh, solve graphene film and be difficult to transfer to little area
Difficulty on TEM copper mesh, and simple to operate, the time of traditional transfer method was tapered to a few minutes from tens of hours, significantly
Improve Graphene and carry out the efficiency of TEM test；
2, the method for the present invention is in operation without the introducing of any pollutant, also will not destroy shape characteristic and the knot of Graphene
Structure character, and environmental protection, efficiently；
Accompanying drawing explanation
Fig. 1 is to scribble the graphene film of PMMA to suspend photo in deionized water；
Fig. 2 is that copper mesh is adsorbed photo on a pet film；
Fig. 3 and Fig. 4 is the photo fishing for graphene film in deionized water with the PET film being adsorbed with copper mesh；
Fig. 5 is the photo etching away the graphene film after PMMA/TEM copper mesh/PET film composite construction with acetone；
Fig. 6 is to take off, with tweezers, the photo that transfer has the copper mesh of graphene film；
Fig. 7 is by SiO2Absorption photo on a pet film；
Fig. 8 and Fig. 9 is for being adsorbed with SiO2PET film fish for the photo of the graphene film in deionized water；
Figure 10 is to etch away the graphene film/SiO after PMMA with acetone2The photo of/PET film composite construction；
Figure 11 is to take off transfer with tweezers to have the SiO of graphene film2Photo.
Detailed description of the invention
Embodiment 1
Graphene film is transferred on TEM copper mesh by the present embodiment in accordance with the following steps:
Step a as it is shown in figure 1, there is the graphene film of PMMA protection glue-line to be suspended in upward with protection glue-line by spin coating
In ionized water；
Step b is as in figure 2 it is shown, adsorb TEM copper mesh on a pet film；
Step c, as shown in Figure 3 and Figure 4, with TEM copper mesh upward, extend into the Electrostatic Absorption film in step b with tweezers
In deionized water in step a, graphene film is pulled out, and make graphene film cover TEM copper mesh, formed from top to bottom
Protection glue-line/graphene film/TEM copper mesh/PET film composite construction；
Step d is as it is shown in figure 5, protection glue-line/graphene film/TEM copper mesh/PET film composite junction of step c being obtained
After structure dries naturally, soak in acetone to remove protection glue-line, it is thus achieved that graphene film/TEM copper mesh/PET film composite construction；
Step e, as shown in Figure 6, on graphene film/TEM copper mesh/Electrostatic Absorption film composite construction that step d is obtained,
Being taken off from Electrostatic Absorption film together with being positioned at graphene film thereon by TEM copper mesh with tweezers, graphene film is i.e. turned
Move on on TEM copper mesh.
Embodiment 2
The inventive method applies also for being transferred to by graphene film in little area silica substrate, in order to it is carried out Raman
Test, specifically comprises the following steps that
A, spin coating is had PMMA protection glue-line graphene film with protection glue-line suspend upward in deionized water；
B is as it is shown in fig. 7, by SiO2Sheet adsorbs on a pet film, and SiO2Sheet shiny surface is upward.
C, as shown in Figure 8 and Figure 9, with SiO2Electrostatic Absorption film in step b upward, is extend into step a with tweezers by sheet
In deionized water in, graphene film is pulled out, and make graphene film cover SiO2Sheet, forms protection from top to bottom
Glue-line/graphene film/SiO2Sheet/PET film composite construction；
D, as shown in Figure 10, protection glue-line/graphene film/SiO that step c is obtained2Sheet/PET film composite construction is natural
After drying, soak in acetone to remove protection glue-line, it is thus achieved that graphene film/SiO2Sheet/PET film composite construction；
E, as shown in figure 11, in graphene film/SiO that step d is obtained2On sheet/PET film composite construction, will with tweezers
SiO2Sheet takes off from Electrostatic Absorption film together with being positioned at graphene film thereon, and graphene film is i.e. transferred to SiO2Sheet
On.
Claims (2)
1. method graphene film transferred on TEM copper mesh, it is characterised in that carry out as follows:
Step a, by the graphene film of protected for spin coating glue-line with protection glue-line suspend upward in deionized water；
Step b, by TEM copper mesh adsorb on Electrostatic Absorption film, the area of described Electrostatic Absorption film is at least described TEM copper
4 times of web area, and the area of described Electrostatic Absorption film is not less than the area of graphene film described in step a；Described electrostatic
Adsorbed film is PET film, PE film or PVC film；
Step c, with TEM copper mesh upward, the deionized water Electrostatic Absorption film in step b being extend in step a with tweezers
In, graphene film is pulled out, and makes graphene film cover described TEM copper mesh, form protection glue-line/graphite from top to bottom
Alkene thin film/TEM copper mesh/Electrostatic Absorption film composite construction；
Step d, protection step c obtained glue-line/graphene film/TEM copper mesh/Electrostatic Absorption film composite construction dry in the air naturally
After Gan, soak in acetone to remove protection glue-line, it is thus achieved that graphene film/TEM copper mesh/Electrostatic Absorption film composite construction；
Step e, on graphene film/TEM copper mesh/Electrostatic Absorption film composite construction that step d is obtained, with tweezers by TEM
Copper mesh takes off from Electrostatic Absorption film together with being positioned at graphene film thereon, and graphene film is i.e. transferred to TEM copper mesh
On.
Method graphene film transferred on TEM copper mesh the most according to claim 1, it is characterised in that: described
Electrostatic Absorption film is PET film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510145260.2A CN104817073B (en) | 2015-03-27 | 2015-03-27 | Method for transferring graphene film to TEM copper net |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510145260.2A CN104817073B (en) | 2015-03-27 | 2015-03-27 | Method for transferring graphene film to TEM copper net |
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| CN104817073A CN104817073A (en) | 2015-08-05 |
| CN104817073B true CN104817073B (en) | 2017-01-11 |
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| CN106872501B (en) * | 2017-03-08 | 2019-04-16 | 北京大学 | A kind of method that direct etching metallic substrates prepare graphene-based transmission electron microscope carrier net support membrane |
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| CN102759467B (en) * | 2012-07-02 | 2014-10-29 | 浙江大学 | Method for manufacturing multi-layer graphene TEM (Transverse Electric and Magnetic Field) sample |
| CN102774118B (en) * | 2012-07-31 | 2015-05-13 | 无锡格菲电子薄膜科技有限公司 | Method for transferring graphene film with static protective film as medium |
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