CN106884153A - A kind of method that copper substrate is prepared based on dry method cleaning - Google Patents
A kind of method that copper substrate is prepared based on dry method cleaning Download PDFInfo
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- CN106884153A CN106884153A CN201510934979.4A CN201510934979A CN106884153A CN 106884153 A CN106884153 A CN 106884153A CN 201510934979 A CN201510934979 A CN 201510934979A CN 106884153 A CN106884153 A CN 106884153A
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- copper substrate
- copper
- substrate
- graphene
- dry method
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
Abstract
The present invention provides a kind of method that copper substrate is prepared based on dry method cleaning, including step：Step 1）, there is provided prepare the copper substrate of Graphene；Step 2）, the copper substrate is placed in aerobic environment and is processed, make the copper substrate surface oxidation, form oxide layer；And step 3）, the copper is removed except the oxide layer of substrate surface, the brass basal surface for being cleaned.The present invention is by graphene oxide growth copper substrate so that the oxidation of substrate surface layer simultaneously comes off from substrate, obtains clean copper surface prepared by suitable high-quality graphene, and the copper substrate that the method is obtained can obviously reduce nucleation density, reduce the defect in Graphene.Method of the present invention repeatability is high, simple and easy to apply, and controllability is strong, is adapted to the mass treatment of industrial applications.
Description
Technical field
The invention belongs to field of preparation of graphene, more particularly to a kind of method that CVD Graphene copper substrates are prepared based on dry method cleaning.
Background technology
Graphene has unusual electric conductivity, the intensity beyond steel decades of times and fabulous translucency, and its appearance is expected to trigger one to take turns revolution in hyundai electronicses sciemtifec and technical sphere.In Graphene, electronics can be migrated extremely efficiently, and traditional semiconductor and conductor, such as silicon and copper are far from, Graphene show must well.Due to the collision of electronics and atom, the form of traditional semiconductor and conductor heat releases some energy, and general computer chip wastes the electric energy of 72%-81% by this way, and Graphene is then different, its electron energy will not be depleted, and this makes it be provided with extraordinary good characteristic.
In recent years, Graphene was with its unique performance and is widely applied prospect and causes huge concern.In many preparation methods of Graphene, CVD is suitable to prepare high-quality large-area graphene in metal substrate, wherein, copper is most suitable for preparing high quality monolayer Graphene as substrate.Research has shown that, the growth of the surface quality of copper to Graphene has a major impact, and the defect and impurity on copper surface can not only increase the nucleation density of Graphene, but also can introduce more defects, Graphene is occurred the phenomenon of etching in temperature-fall period.Therefore, cleaning, smooth substrate surface are the bases for preparing high-quality graphene.Common copper substrate cleaning method is first to remove surface contamination with soda acid, organic reagent, then with the reagent of deionized water wash and remove residual.In addition, polishing be found to be cleaned, the effective ways on flat substrate surface, polishing substrate can effectively reduce the nucleation density of graphene domain, and reduce the spot defect in Graphene.Traditional cleaning method and polishing is required for various reagents and substantial amounts of deionized water, and process is more complicated, wastes time and energy.
In view of the above, there is provided a kind of method that process is simple, the dry method without any reagent clean copper substrate is necessary.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of method that copper substrate is prepared based on dry method cleaning, for solving the problems, such as copper substrate complex treatment process in the prior art and relatively costly.
In order to achieve the above objects and other related objects, the present invention provides a kind of method that copper substrate is prepared based on dry method cleaning, including step：Step 1), there is provided prepare the copper substrate of Graphene；Step 2), the copper substrate is placed in aerobic environment and is processed, make the copper substrate surface oxidation, form oxide layer；And step 3), the copper is removed except the oxide layer of substrate surface, the brass basal surface for being cleaned.
Used as a kind of preferred scheme of the method that copper substrate is prepared based on dry method cleaning of the invention, the material of the copper substrate includes the alloy of copper or copper.
Used as a kind of preferred scheme of the method that copper substrate is prepared based on dry method cleaning of the invention, the thickness range of described copper substrate is 1 μm~1m.
Used as a kind of preferred scheme of the method that copper substrate is prepared based on dry method cleaning of the invention, the aerobic environment includes pure oxygen atmosphere or the mixed-gas atmosphere comprising oxygen.
Used as a kind of preferred scheme of the method that copper substrate is prepared based on dry method cleaning of the invention, the aerobic environment is open space or closed environment.
Used as a kind of preferred scheme of the method that copper substrate is prepared based on dry method cleaning of the invention, the air pressure range of the aerobic environment is 0.1~7600torr.
As it is of the invention based on dry method cleaning prepare copper substrate method a kind of preferred scheme, step 2) to copper substrate treatment temperature range be 20~1100 DEG C.
As it is of the invention based on dry method cleaning prepare copper substrate method a kind of preferred scheme, step 2) to copper substrate treatment time be 0.001-99999min.
As a kind of preferred scheme of the method that copper substrate is prepared based on dry method cleaning of the invention, step 3) in, the method for removing copper substrate surface oxide layer includes：Oxide layer is blown away using gas or copper substrate shaken, distorted so that oxide layer comes off from brass basal surface using external force.
Used as a kind of preferred scheme of the method that copper substrate is prepared based on dry method cleaning of the invention, the copper substrate includes the copper substrate for preparing CVD Graphenes.
As described above, the method that copper substrate is prepared based on dry method cleaning of the invention, is had the advantages that：
1) present invention is by graphene oxide growth copper substrate, so that substrate surface layer is aoxidized and come off from substrate, clean copper surface prepared by suitable high-quality graphene is obtained, the copper substrate that the method is obtained can obviously reduce nucleation density, reduce the defect in Graphene.
2) method of the present invention repeatability is high, simple and easy to apply, and controllability is strong, is adapted to the mass treatment of industrial applications.
Brief description of the drawings
Fig. 1 be shown as it is of the invention based on dry method cleaning prepare copper substrate method the step of schematic flow sheet.
Fig. 2~Fig. 4 is shown as the structural representation that each step of method for preparing copper substrate based on dry method cleaning of the invention is presented.
Fig. 5 a are shown as the SEM figures of untreated copper substrate surface, and Fig. 5 b are shown pass by the treated brass basal surface SEM figures of the present invention.
Fig. 6 a and Fig. 6 c are shown as the SEM pictures of Graphene in untreated copper substrate, and Fig. 6 b and Fig. 6 d are shown pass by the SEM pictures of Graphene in the copper substrate of present invention treatment.
Component label instructions
101 copper substrates
102 pollutants
103 oxide layers
S11~S13 steps 1)~step 3)
Specific embodiment
Embodiments of the present invention are illustrated below by way of specific instantiation, the content that those skilled in the art can be as disclosed by this specification understands other advantages of the invention and effect easily.The present invention can also be embodied or practiced by way of a different and different embodiment, and without departing from the spirit of the present invention the various details in this specification can also carry out various modifications or alterations based on different viewpoints and application.
Refer to Fig. 1~Fig. 5.It should be noted that, diagram provided in the present embodiment only illustrates basic conception of the invention in a schematic way, then component count, shape and size when only display is with relevant component in the present invention rather than according to actual implementation in illustrating are drawn, it is actual when the implementing kenel of each component, quantity and ratio can be a kind of random change, and its assembly layout kenel be likely to it is increasingly complex.
As shown in Fig. 1~Fig. 6, the present embodiment provides a kind of method that copper substrate 101 is prepared based on dry method cleaning, including step：
As shown in figure 1, carrying out step 1 first) S11, there is provided prepare the copper substrate 101 of Graphene.
As an example, the material of the copper substrate 101 includes the alloy of copper or copper.In the present embodiment, the material of the copper substrate 101 is fine copper.The copper substrate 101 is the copper substrate 101 for preparing CVD Graphenes.
As an example, the thickness range of described copper substrate 101 is 1 μm~1m.
As shown in figure 1, as an example, the copper substrate 101 be without surface treatment copper substrate 101, its surface typically have a large amount of or a small amount of pollutants 102.
As shown in Figure 2, then step 2 is carried out) S12, the copper substrate 101 is placed in aerobic environment and is processed, make the surface oxidation of the copper substrate 101, form oxide layer 103, the growth course of the oxide layer 103 is from the downward Longitudinal extending in the surface of copper substrate 101, due to cupric oxide and copper lattice and mismatch, therefore, after oxide layer 103 reaches certain thickness, the oxide layer 103 comprising pollutant 102 can be separated with copper substrate 101.
As an example, the aerobic environment includes pure oxygen atmosphere or the mixed-gas atmosphere comprising oxygen.
As an example, the aerobic environment is open space or closed environment, the air pressure range of the aerobic environment is 0.1~7600 torr.
As an example, being 20~1100 DEG C to the temperature range of the treatment of copper substrate 101, the time to the treatment of copper substrate 101 is 0.001-99999min.
As shown in figure 3, finally carrying out step 3) S13, removes the copper except the oxide layer 103 of substrate surface, the surface of copper substrate 101 cleaned.
As an example, the method for the removal surface oxide layer 103 of copper substrate 101 includes：Oxide layer 103 is blown away using gas (such as gases at high pressure) or copper substrate 101 shaken, distorted using external force so that oxide layer 103 comes off from the surface of copper substrate 101.
In a specific implementation process, comprise the following steps：
Step 1), the Copper Foil of 100 microns of thickness is put into the quartz ampoule of growth Graphene, quartz ampoule is not closed, therefore, air is full of in quartz ampoule, then quartz ampoule is heated up, and Copper Foil is aoxidized 30 minutes under 500 degrees Celsius.
Step 2), Copper Foil is lowered the temperature rapidly, in temperature-fall period, very big stress can be produced between the unoxidized Copper Foil of surface oxidation layers of copper containing impurity and lower section, most oxide layer 103 is caused to be come off from unoxidized copper surface automatically, the oxide layer 103 of a little non-Automatic-falling, can make it come off by rapping Copper Foil with tweezers.
The unwashed Copper Foil copper foil surface SEM picture treated with the present invention is as shown in Figure 5.It will be seen that untreated copper foil surface has obvious pollutant 102 from Fig. 5 a, some can not be removed completely in hot environment prepared by Graphene in these pollutants 102, it will the growth of influence Graphene.As can be seen that the treated copper surface of the present invention and out-of-flatness, also in the presence of some small particles, but the pollutant 102 of the influence growth in Fig. 5 a has been removed from Fig. 5 b.
Step 3) Copper Foil that was cleaned by untreated Copper Foil and through the present invention is put into the equipment of growth Graphene, and routinely the conventional preparation method of CVD graphene domains carries out the growth of Graphene on copper, specifically includes：
A) 1.5Pa, applying argon gas to normal pressure are evacuated to.
B) Copper Foil is warming up to 1000 degrees Celsius under the protection of 1000sccm argon gas, is passed through 200sccm hydrogen annealings, by after 20 minutes processes of annealing, temperature being risen into 1050 degrees Celsius.
C) hydrogen intake is changed to 20sccm, and (methane is 5 with the volume ratio of argon gas to be passed through the mixed methane of 1.5sccm:1000) Graphene, is grown, growth time is 30 minutes.
D) methane is closed, stops heating, be down to room temperature, obtain Graphene sample on copper.
Relatively more in view of unpolished copper surface impurity and defect, to reduce the nucleation density of Graphene, the methane concentration that the present embodiment is chosen is very low.The SEM pictures for growing Graphene are as shown in Figure 6.Comparison diagram 6a and Fig. 6 b, it can be seen that graphene domain density is significantly lower than the result on Copper Foil not processed by the invention on the Copper Foil of present invention treatment.Comparison diagram 6c and 6d, graphene domain on undressed Copper Foil is can see from Fig. 6 c occur in that obvious etching (breakage), copper foil surface can also be seen that the bright spot (impurity of residual) of many whites, and the Graphene on the Copper Foil of mistake processed by the invention does not occur then significantly etching phenomenon, as shown in fig 6d.Research is it has been proved that the defect and impurity on copper surface can increase the nucleation density of Graphene, and increase the defect in Graphene.These defect areas are relatively unstable, are easily etched.The result of Fig. 6 illustrates the copper substrate 101 of mistake processed by the invention, and surface cleanness is significantly improved, and Graphene nucleation density is substantially reduced, and reduces the defect in Graphene, significantly improves the quality of Graphene.
As described above, the method that copper substrate 101 is prepared based on dry method cleaning of the invention, is had the advantages that：
1) present invention is grown by graphene oxide and uses copper substrate 101, so that substrate surface layer is aoxidized and come off from substrate, clean copper surface prepared by suitable high-quality graphene is obtained, the copper substrate 101 that the method is obtained can obviously reduce nucleation density, reduce the defect in Graphene.
2) method of the present invention repeatability is high, simple and easy to apply, and controllability is strong, is adapted to the mass treatment of industrial applications.
So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.Any person skilled in the art all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Therefore, those of ordinary skill in the art is completed under without departing from disclosed spirit and technological thought such as all equivalent modifications or change, should be covered by claim of the invention.
Claims (10)
1. it is a kind of based on dry method cleaning prepare copper substrate method, it is characterised in that including step：
Step 1), there is provided prepare the copper substrate of Graphene；
Step 2), the copper substrate is placed in aerobic environment and is processed, make the copper substrate surface oxidation, form oxide layer；
Step 3), the copper is removed except the oxide layer of substrate surface, the brass basal surface for being cleaned.
2. it is according to claim 1 based on dry method cleaning prepare copper substrate method, it is characterised in that：The copper substrate
Material includes the alloy of copper or copper.
3. it is according to claim 1 based on dry method cleaning prepare copper substrate method, it is characterised in that：Described copper substrate
Thickness range be 1 μm~1m.
4. it is according to claim 1 based on dry method cleaning prepare copper substrate method, it is characterised in that：The aerobic environment
Mixed-gas atmosphere including pure oxygen atmosphere or comprising oxygen.
5. it is according to claim 1 based on dry method cleaning prepare copper substrate method, it is characterised in that：The aerobic environment
It is open space or closed environment.
6. it is according to claim 1 based on dry method cleaning prepare copper substrate method, it is characterised in that：The aerobic environment
Air pressure range be 0.1~7600torr.
7. it is according to claim 1 based on dry method cleaning prepare copper substrate method, it is characterised in that：Step 2) to copper
The temperature range of substrate processing is 20~1100 DEG C.
8. it is according to claim 1 based on dry method cleaning prepare copper substrate method, it is characterised in that：Step 2) to copper
The time of substrate processing is 0.001-99999min.
9. it is according to claim 1 based on dry method cleaning prepare copper substrate method, it is characterised in that：Step 3) in,
The method for removing copper substrate surface oxide layer includes：Oxide layer is blown away using gas or copper substrate is shaken using external force,
Distortion is so that oxide layer comes off from brass basal surface.
10. it is according to claim 1 based on dry method cleaning prepare copper substrate method, it is characterised in that：The copper substrate
Including the copper substrate for preparing CVD Graphenes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109023291A (en) * | 2018-08-14 | 2018-12-18 | 北京镭硼科技有限责任公司 | A kind of graphene film and the preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445164A (en) * | 2014-11-18 | 2015-03-25 | 扬州大学 | Universal method for controllable growth of nano structure on single-layer graphene film |
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- 2015-12-15 CN CN201510934979.4A patent/CN106884153B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445164A (en) * | 2014-11-18 | 2015-03-25 | 扬州大学 | Universal method for controllable growth of nano structure on single-layer graphene film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109023291A (en) * | 2018-08-14 | 2018-12-18 | 北京镭硼科技有限责任公司 | A kind of graphene film and the preparation method and application thereof |
| CN109023291B (en) * | 2018-08-14 | 2020-12-22 | 河北镭传科技有限责任公司 | Graphene film and preparation method and application thereof |
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