CN104817073A - 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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- CN104817073A CN104817073A CN201510145260.2A CN201510145260A CN104817073A CN 104817073 A CN104817073 A CN 104817073A CN 201510145260 A CN201510145260 A CN 201510145260A CN 104817073 A CN104817073 A CN 104817073A
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- copper mesh
- graphene film
- graphene
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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 by graphene film material transfer on TEM copper mesh, so that carry out the method for transmissioning electric mirror test.
Technical background
Graphene is the two dimensional surface material with an atomic thickness formed by the hexagonal array of carbon atom.2004, the method that Novoselov and Geim of Univ Manchester UK is peeled off by micromechanics, successfully separated Graphene from highly oriented pyrolytic graphite, from then on opens the possibility of this two-dimensional material experimental investigation of Graphene.
Because Graphene has the excellent character such as electricity, optics, calorifics, mechanics, it is made to have a very wide range of applications prospect at nanoelectronics, sensor, optics, energy transformation and storage, environmental improvement, matrix material and biological technical field.
The preparation method of Graphene is mainly divided into two kinds: from bottom to top and from top to bottom.Wherein, Self-absorption Correction Factor mainly comprises epitaxial growth method, chemical Vapor deposition process (CVD), chemical small molecule synthesis method; Top-down methods mainly comprises liquid phase stripping method, mechanically peel method etc.At present, CVD growing graphene is the mode the most generally adopted, and this method not only can the graphene film of growing large-area, and controls the number of plies of Graphene within the specific limits.Graphene film prepared by this method has been applied in the scientific research fields such as transparency electrode, solar cell, field-effect transistor and ultracapacitor.
But Graphene prepared by any method all will carry out the sign of some necessity, observes its shape characteristic, crystal property, optical property, electric property and defect etc., carry out next step research auxiliary.The characterization technique of this kind of two-dimensional material of current Graphene has been tending towards perfect, and mainly contain scanning electron microscope (SEM) and characterize, transmission electron microscope (TEM) characterizes, Raman (Raman) characterizes, XPS characterizes, and XRD characterizes, Fourier transform infrared spectroscopy sign etc.Generally all need first material to be attached in substrate in the process of characterization test, during as characterized property of thin film with Raman, film needs to be attached in silicon base or silicon-dioxide substrate, it does not almost limit for the size of material and the size of substrate, and area of base size in range of needs all can.
But what utilize in the test of transmission electron microscope exosyndrome material character is copper mesh substrate, people need the material transfer will carrying out testing just can test to TEM copper mesh.By Graphene, the step transferred on TEM copper mesh is at present: first spin coating had the graphene film of protection glue-line to suspend in deionized water; with tweezers gripping TEM copper mesh; extend in deionized water and Graphene is pulled out; then soak and remove protection glue-line in acetone, after having gone, have the copper mesh of Graphene to take out from acetone transfer with tweezers again.There is following problem in this method:
1, the area of TEM copper mesh only has several millimeter, is directly very easy to destroy its structure with tweezers grippings, makes graphene film cannot self-supporting at the copper mesh position of breakage, and comparatively easily broken, the pattern of Graphene is observed in impact simultaneously; And gripping is difficult;
2, stretch in deionized water with the TEM copper mesh that tweezers clip very small area and fish for Graphene, operation easier is high, wastes time and energy, and completing a transfer needs several hours consuming time even tens hours, requires high to the state of the art of operator;
3, after having removed protective membrane, also need have the copper mesh of Graphene to take out from acetone transfer with tweezers, the graphene-structured clipped to by tweezers is substantially destroyed, and on copper mesh, the area of Graphene is inherently limited, the effect of impact test;
4, repeatedly directly contact TEM copper mesh and Graphene with tweezers, very easily introduce pollutent.
Therefore, a kind of can efficiently by graphene film, the method transferred on TEM copper mesh urgently finds easily.
Summary of the invention
The present invention is the weak point for avoiding existing for above-mentioned prior art, provides a kind of method can efficiently transferred to by graphene film easily on TEM copper mesh.
The present invention is that technical solution problem adopts following technical scheme:
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, the graphene film of protection glue-line spin coating is had to suspend in deionized water to protect glue-line upward;
Step b, be adsorbed on electrostatic adhesion film by TEM copper mesh, the area of described electrostatic adhesion film is at least 4 times of described TEM copper mesh area, and the area of described electrostatic adhesion film is not less than the area of graphene film described in step a;
Step c, with TEM copper mesh upward, with tweezers, the electrostatic adhesion film in step b is extend in the deionized water in step a, graphene film is pulled out, and make graphene film cover described TEM copper mesh, form protection glue-line/graphene film/TEM copper mesh/electrostatic adhesion film composite structure from top to bottom;
After steps d, the protection glue-line/graphene film/TEM copper mesh/electrostatic adhesion film composite structure obtained by step c dry naturally, soak in acetone to remove protection glue-line, obtain graphene film/TEM copper mesh/electrostatic adhesion film composite structure;
On step e, graphene film/TEM copper mesh/electrostatic adhesion film composite structure of obtaining in steps d, taken off from electrostatic adhesion film together with the graphene film be located thereon by TEM copper mesh with tweezers, namely graphene film is transferred on TEM copper mesh.
Graphene film is transferred to the method on TEM copper mesh by the present invention, and its feature is also: described electrostatic adhesion film is PET film, PE film or PVC film, is preferably PET film.
Method of the present invention is except transferring to graphene film except on TEM copper mesh, can also be transferred in the less substrate of other areas, as silicon chip, silicon oxide, sheet glass, plastic tab, sapphire sheet, quartz plate, sheet metal etc., solve the problem of small area Graphene transfer difficulty.
In addition, method of the present invention also may be used for other thin-film materials to transfer in TEM copper mesh or other small area substrates, as boron nitride pellicle, molybdenum disulfide film etc.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the present invention is by being adsorbed on electrostatic adhesion film by TEM copper mesh, macroscopically indirectly expands the surface-area of copper mesh, makes it easy to gripping, and does not directly contact TEM copper mesh when gripping, avoids its structural damage; Graphene film is shifted by this composite substrate, easily realize the transfer of Graphene to TEM copper mesh, solve graphene film and not easily transfer to difficulty on small area TEM copper mesh, and it is simple to operate, the time of traditional transfer method is tapered to several minutes from tens of hours, substantially increases the efficiency that Graphene carries out TEM test;
2, method of the present invention is in operation without the introducing of any pollutent, also can not destroy shape characteristic and the textural property of Graphene, and environmental protection, efficient;
Accompanying drawing explanation
Fig. 1 is the photo that the graphene film scribbling PMMA suspends in deionized water;
Fig. 2 is by copper mesh absorption photo on a pet film;
Fig. 3 and Fig. 4 is the photo fishing for the graphene film in deionized water by 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 structure with acetone;
Fig. 6 takes off with tweezers the photo that transfer has the copper mesh of graphene film;
Fig. 7 is by SiO
2absorption photo on a pet film;
Fig. 8 and Fig. 9 is with being adsorbed with SiO
2pET film fish for the photo of the graphene film in deionized water;
Figure 10 etches away the graphene film/SiO after PMMA with acetone
2the photo of/PET film composite structure;
Figure 11 takes off with tweezers the SiO that transfer has graphene film
2photo.
Embodiment
Embodiment 1
Graphene film is transferred on TEM copper mesh by the present embodiment in accordance with the following steps:
Step a, as shown in Figure 1, has PMMA to protect the graphene film of glue-line to suspend in deionized water to protect glue-line upward by spin coating;
Step b, as shown in Figure 2, by the absorption of TEM copper mesh on a pet film;
Step c, as shown in Figure 3 and Figure 4, with TEM copper mesh upward, with tweezers, the electrostatic adhesion film in step b is extend in the deionized water in step a, graphene film is pulled out, and make graphene film cover TEM copper mesh, form protection glue-line/graphene film/TEM copper mesh/PET film composite structure from top to bottom;
Steps d, as shown in Figure 5, after the protection glue-line/graphene film/TEM copper mesh/PET film composite structure obtained by step c dries naturally, soaks in acetone to remove protection glue-line, acquisition graphene film/TEM copper mesh/PET film composite structure;
Step e, as shown in Figure 6, on graphene film/TEM copper mesh/electrostatic adhesion film composite structure that steps d obtains, taken off from electrostatic adhesion film together with the graphene film be located thereon by TEM copper mesh with tweezers, namely graphene film is transferred on TEM copper mesh.
Embodiment 2
The inventive method is also applicable to be transferred to by graphene film in the substrate of small area silicon-dioxide, so that carry out Raman test to it, concrete steps are as follows:
A, PMMA spin coating is had to protect the graphene film of glue-line to suspend in deionized water to protect glue-line upward;
B, as shown in Figure 7, by SiO
2sheet adsorbs on a pet film, and SiO
2sheet shiny surface upward.
C, as shown in Figure 8 and Figure 9, with SiO
2electrostatic adhesion film in step b, is extend into step a with tweezers upward by sheet
In deionized water in, graphene film is pulled out, and make graphene film cover SiO
2sheet, forms protection from top to bottom
Glue-line/graphene film/SiO
2sheet/PET film composite structure;
D, as shown in Figure 10, protection glue-line/graphene film/SiO that step c is obtained
2after sheet/PET film composite structure dries naturally, soak in acetone to remove protection glue-line, obtain graphene film/SiO
2sheet/PET film composite structure;
E, as shown in figure 11, at graphene film/SiO that steps d obtains
2on sheet/PET film composite structure, with tweezers by SiO
2sheet takes off from electrostatic adhesion film together with the graphene film be located thereon, and namely graphene film is transferred to SiO
2on sheet.
Claims (3)
1. graphene film is transferred to the method on TEM copper mesh, it is characterized in that carrying out as follows:
Step a, the graphene film of protection glue-line spin coating is had to suspend in deionized water to protect glue-line upward;
Step b, be adsorbed on electrostatic adhesion film by TEM copper mesh, the area of described electrostatic adhesion film is at least 4 times of described TEM copper mesh area, and the area of described electrostatic adhesion film is not less than the area of graphene film described in step a;
Step c, with TEM copper mesh upward, with tweezers, the electrostatic adhesion film in step b is extend in the deionized water in step a, graphene film is pulled out, and make graphene film cover described TEM copper mesh, form protection glue-line/graphene film/TEM copper mesh/electrostatic adhesion film composite structure from top to bottom;
After steps d, the protection glue-line/graphene film/TEM copper mesh/electrostatic adhesion film composite structure obtained by step c dry naturally, soak in acetone to remove protection glue-line, obtain graphene film/TEM copper mesh/electrostatic adhesion film composite structure;
On step e, graphene film/TEM copper mesh/electrostatic adhesion film composite structure of obtaining in steps d, taken off from electrostatic adhesion film together with the graphene film be located thereon by TEM copper mesh with tweezers, namely graphene film is transferred on TEM copper mesh.
2. the method transferred to by graphene film on TEM copper mesh according to claim 1, is characterized in that: described electrostatic adhesion film is PET film, PE film or PVC film.
3. the method transferred to by graphene film on TEM copper mesh according to claim 2, is characterized in that: described electrostatic adhesion film is PET film.
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| CN201510145260.2A CN104817073B (en) | 2015-03-27 | 2015-03-27 | Method for transferring graphene film to TEM copper net |
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| CN104817073B CN104817073B (en) | 2017-01-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106872501A (en) * | 2017-03-08 | 2017-06-20 | 北京大学 | A kind of method that direct etching metallic substrates prepare graphene-based transmission electron microscope carrier net support membrane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101458180A (en) * | 2007-12-13 | 2009-06-17 | 中芯国际集成电路制造(上海)有限公司 | Method for preprocessing TEM example and carrying out TEM test for example |
| CN102759467A (en) * | 2012-07-02 | 2012-10-31 | 浙江大学 | Method for manufacturing multi-layer graphene TEM (Transverse Electric and Magnetic Field) sample |
| CN102774118A (en) * | 2012-07-31 | 2012-11-14 | 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101458180A (en) * | 2007-12-13 | 2009-06-17 | 中芯国际集成电路制造(上海)有限公司 | Method for preprocessing TEM example and carrying out TEM test for example |
| CN102759467A (en) * | 2012-07-02 | 2012-10-31 | 浙江大学 | Method for manufacturing multi-layer graphene TEM (Transverse Electric and Magnetic Field) sample |
| CN102774118A (en) * | 2012-07-31 | 2012-11-14 | 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106872501A (en) * | 2017-03-08 | 2017-06-20 | 北京大学 | A kind of method that direct etching metallic substrates prepare graphene-based transmission electron microscope carrier net support membrane |
| 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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