CN106884153B - A method of copper substrate is prepared based on dry method cleaning process - Google Patents
A method of copper substrate is prepared based on dry method cleaning process Download PDFInfo
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- CN106884153B CN106884153B CN201510934979.4A CN201510934979A CN106884153B CN 106884153 B CN106884153 B CN 106884153B CN 201510934979 A CN201510934979 A CN 201510934979A CN 106884153 B CN106884153 B CN 106884153B
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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
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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
- C23C16/22—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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The present invention provides a kind of method based on dry method cleaning process preparation copper substrate, comprising steps of step 1), provides the copper substrate for preparing graphene；The copper substrate is placed in aerobic environment and handles by step 2, makes the copper substrate surface oxidation, forms oxide layer；And step 3), it goes the copper to remove the oxide layer of substrate surface, obtains clean brass bottom surface.The present invention is by graphene oxide growth copper substrate, so that substrate surface layer is aoxidized and fallen off from substrate, obtains the clean copper surface of suitable high-quality graphene preparation, the copper substrate that this method obtains can obviously reduce nucleation density, reduce the defects of graphene.Method repeatability of the invention is high, simple and easy, and controllability is strong, is suitble to the mass processing of industrial applications.
Description
Technical field
The invention belongs to field of preparation of graphene, prepare CVD graphene copper based on dry method cleaning process more particularly to one kind
The method of substrate.
Background technique
Graphene is with unusual electric conductivity, intensity beyond steel decades of times and fabulous translucency, it
Appearance is expected to cause a wheel revolution in modern electronic technology field.In graphene, electronics can be migrated extremely efficiently, and be passed
The semiconductor and conductor of system, such as silicon and the copper graphene that is far from show well.Due to the collision of electronics and atom, traditional half
The form of conductor and conductor heat releases some energy, and general computer chip wastes 72%-81%'s in this way
Electric energy, graphene is then different, its electron energy will not be depleted, this makes it be provided with extraordinary good characteristic.
In recent years, graphene caused huge concern with its unique performance and broad application prospect.In graphene
In many preparation methods, in metal substrate CVD method be suitable for preparation high quality large-area graphene, wherein copper as substrate most
Suitable for preparing high quality monolayer graphene.Research has shown that the surface quality of copper has a major impact the growth of graphene, copper surface
Defect and impurity can not only increase the nucleation density of graphene, but also more defects can be introduced, be easy to make graphene
The phenomenon that being etched in temperature-fall period.Therefore, cleaning, smooth substrate surface are the bases for preparing high-quality graphene.
Common copper substrate cleaning method is first with soda acid, organic reagent removal surface contamination, then with deionized water wash and remove residual
Reagent.In addition, polishing be found to be cleaned, the effective ways on flat substrate surface, polishing treatment substrate can effectively drop
The nucleation density of low graphene domain, and reduce the spot defect in graphene.Traditional cleaning method and polishing requires
Various reagents and a large amount of deionized water, and process is more complicated, it is time-consuming and laborious.
In view of the above, a kind of simple process is provided, is belonged in fact without the method for the dry method cleaning copper substrate of any reagent
It is necessary.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide one kind to be based on dry method cleaning process system
The method of standby copper substrate, for solving the problems, such as copper substrate complex treatment process and higher cost in the prior art.
In order to achieve the above objects and other related objects, the present invention provides a kind of based on dry method cleaning process preparation copper substrate
Method, comprising steps of step 1), provides the copper substrate for preparing graphene；The copper substrate is placed in aerobic ring by step 2)
It is handled in border, makes the copper substrate surface oxidation, form oxide layer；And step 3), go the copper to remove the oxidation of substrate surface
Layer, obtains clean brass bottom surface.
As a kind of preferred embodiment of the method for the invention based on dry method cleaning process preparation copper substrate, the copper substrate
Material include copper or copper alloy.
As a kind of preferred embodiment of the method for the invention based on dry method cleaning process preparation copper substrate, the brass
The thickness range at bottom is 1 μm~1m.
As a kind of preferred embodiment of the method for the invention based on dry method cleaning process preparation copper substrate, the aerobic ring
Border includes pure oxygen atmosphere or the mixed-gas atmosphere comprising oxygen.
As a kind of preferred embodiment of the method for the invention based on dry method cleaning process preparation copper substrate, the aerobic ring
Border is open space or closed environment.
As a kind of preferred embodiment of the method for the invention based on dry method cleaning process preparation copper substrate, the aerobic ring
The air pressure range in border is 0.1~7600torr.
As a kind of preferred embodiment of the method for the invention based on dry method cleaning process preparation copper substrate, step 2) is to copper
The temperature range of substrate processing is 20~1100 DEG C.
As a kind of preferred embodiment of the method for the invention based on dry method cleaning process preparation copper substrate, step 2) is to copper
The time of substrate processing is 0.001-99999min.
As a kind of preferred embodiment of the method for the invention based on dry method cleaning process preparation copper substrate, in step 3),
The method of removal copper substrate surface oxide layer includes: to blow away oxide layer using gas or make copper substrate vibration using external force, turn round
Song is so that oxide layer falls off from brass bottom surface.
As a kind of preferred embodiment of the method for the invention based on dry method cleaning process preparation copper substrate, the copper substrate
Copper substrate including being used to prepare CVD graphene.
As described above, the method for the invention based on dry method cleaning process preparation copper substrate, has the advantages that
1) present invention is obtained by graphene oxide growth copper substrate so that substrate surface layer is aoxidized and fallen off from substrate
It must be suitable for the clean copper surface of high-quality graphene preparation, the copper substrate that this method obtains can obviously reduce nucleation density, reduce
The defects of graphene.
2) method of the invention repeatability is high, simple and easy, and controllability is strong, is suitble at the mass of industrial applications
Reason.
Detailed description of the invention
Fig. 1 is shown as the step flow diagram of the method for the invention based on dry method cleaning process preparation copper substrate.
Fig. 2~Fig. 4 is shown as what method each step of the invention based on dry method cleaning process preparation copper substrate was presented
Structural schematic diagram.
Fig. 5 a is shown as the SEM figure of untreated copper substrate surface, and Fig. 5 b is shown pass by the processed copper substrate of the present invention
Surface SEM figure.
Fig. 6 a and Fig. 6 c are shown as the SEM picture of graphene in untreated copper substrate, and Fig. 6 b and Fig. 6 d are shown pass by
The SEM picture of graphene in the copper substrate that the present invention is handled.
Component label instructions
101 copper substrates
102 pollutants
103 oxide layers
S11~S13 step 1)~step 3)
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Please refer to FIG. 1 to FIG. 5.It should be noted that diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, only shown in diagram then with related component in the present invention rather than package count when according to actual implementation
Mesh, shape and size are drawn, when actual implementation kenel, quantity and the ratio of each component can arbitrarily change for one kind, and its
Assembly layout kenel may also be increasingly complex.
As shown in Fig. 1~Fig. 6, the present embodiment provides a kind of method based on dry method cleaning process preparation copper substrate 101, packets
Include step:
As shown in Figure 1, carrying out step 1) S11 first, the copper substrate 101 for preparing graphene is provided.
As an example, the material of the copper substrate 101 includes the alloy of copper or copper.In the present embodiment, the brass
The material at bottom 101 is fine copper.The copper substrate 101 is to be used to prepare the copper substrate 101 of CVD graphene.
As an example, the thickness range of the copper substrate 101 is 1 μm~1m.
As shown in Figure 1, as an example, the copper substrate 101 is the copper substrate 101 without surface treatment, surface one
As have a large amount of or a small amount of pollutants 102.
As shown in Fig. 2, then carrying out step 2) S12, the copper substrate 101 is placed in aerobic environment and is handled, made described
101 surface oxidation of copper substrate, forms oxide layer 103, and the growth course of the oxide layer 103 is downward from 101 surface of copper substrate
It is longitudinal to extend, due to the lattice and mismatch of copper oxide and copper, after oxide layer 103 reaches certain thickness, include pollution
The oxide layer 103 of object 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
0.1~7600torr.
As an example, being 20~1100 DEG C to the temperature range of the processing of copper substrate 101, to the time of the processing of copper substrate 101
For 0.001-99999min.
As shown in figure 3, finally carrying out step 3) S13, goes the copper to remove the oxide layer 103 of substrate surface, obtain clean
101 surface of copper substrate.
As an example, the method for removal 101 surface oxide layer 103 of copper substrate includes: to be blown using gas (such as high pressure gas)
It walks oxide layer 103 or makes the vibration of copper substrate 101 using external force, distorts so that oxide layer 103 falls off from 101 surface of copper substrate.
In a specific implementation process, include the following steps:
100 microns of thick copper foils are put into the quartz ampoule of growth graphene by step 1), and quartz ampoule is not closed, therefore, stone
Ying Guanzhong is full of air, then heats up to quartz ampoule, and aoxidize copper foil 30 minutes under 500 degrees Celsius.
Step 2) cools down rapidly copper foil, and in temperature-fall period, surface oxidation layers of copper and lower section containing impurity are unoxidized
Very big stress can be generated between copper foil, cause most oxide layer 103 to fall off automatically from unoxidized copper surface, Shao Xuwei
The oxide layer 103 of Automatic-falling can make it fall off by touching copper foil with tweezers.
Unwashed copper foil and the processed copper foil surface SEM picture of the present invention are as shown in Figure 5.We can be with from Fig. 5 a
See, there are apparent pollutant 102, some in these pollutants 102 are prepared untreated copper foil surface in graphene
Hot environment in can not completely remove, it will influence the growth of graphene.It can be seen from figure 5b that the present invention is processed
Copper surface and out-of-flatness, there is also some small particles, but in Fig. 5 a influence growth pollutant 102 have been removed.
Untreated copper foil and the copper foil cleaned through the present invention are put into the equipment of growth graphene by step 3), are pressed
The preparation method of CVD graphene domain routine carries out the growth of graphene on conventional 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, 200sccm hydrogen annealing is passed through, by 20
After the process of minute annealing, temperature is risen to 1050 degrees Celsius.
C) hydrogen intake is changed to 20sccm, and be passed through 1.5sccm mix methane (volume ratio of methane and argon gas be 5:
1000) graphene, is grown, growth time is 30 minutes.
D) methane is closed, heating is stopped, being down to room temperature, obtains graphene sample on copper.
In view of unpolished copper surface impurity and defect are relatively more, for the nucleation density for reducing graphene, the present embodiment
The methane concentration of selection is very low.The SEM picture for growing graphene is as shown in Figure 6.Comparison diagram 6a and Fig. 6 b, it can be seen that this hair
Graphene domain density is significantly lower than the result on copper foil not processed by the invention on the copper foil of daylight reason.Comparison diagram 6c and
6d can see graphene domain on untreated copper foil from Fig. 6 c and apparent etching (breakage) occurs, and copper foil surface is also
It can be seen that the bright spot (remaining impurity) of many whites, and the graphene on the copper foil of mistake processed by the invention does not occur then
Apparent etching phenomenon, as shown in fig 6d.Research is it has been proved that the defect and impurity on the copper surface nucleation that can increase graphene is close
The defects of degree, and increase graphene.These defect areas are relatively unstable, are easy to be etched.The result explanation of Fig. 6 is through this
Processed copper substrate 101 is invented, surface cleanness significantly improves, and graphene nucleation density is substantially reduced, and reduces graphene
The defects of, significantly improve the quality of graphene.
As described above, the method for the invention based on dry method cleaning process preparation copper substrate 101, has below beneficial to effect
Fruit:
1) present invention is by graphene oxide growth copper substrate 101, so that substrate surface layer is aoxidized and is fallen off from substrate,
The clean copper surface of suitable high-quality graphene preparation is obtained, the copper substrate 101 that this method obtains can obviously reduce nucleation density,
Reduce the defects of graphene.
2) method of the invention repeatability is high, simple and easy, and controllability is strong, is suitble at the mass of industrial applications
Reason.
So the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (7)
1. a kind of method based on dry method cleaning process preparation copper substrate, which is characterized in that comprising steps of
Step 1) provides the copper substrate for preparing graphene；
The copper substrate is placed in aerobic environment and handles by step 2), makes the copper substrate surface oxidation, forms oxide layer, institute
Stating oxide layer includes pollutant, after the oxide layer reaches certain thickness, the oxide layer and copper substrate due to lattice not
It matches and separates；
Step 3) removes the oxide layer of the brass bottom surface, obtains clean brass bottom surface, removes copper substrate Surface Oxygen
Change layer method include: using gas blow away oxide layer or using external force make copper substrate vibration, distortion thus oxide layer from copper
Substrate surface falls off.
2. the method according to claim 1 based on dry method cleaning process preparation copper substrate, it is characterised in that: the brass
The material at bottom includes the alloy of copper or copper.
3. the method according to claim 1 based on dry method cleaning process preparation copper substrate, it is characterised in that: the copper
The thickness range of substrate is 1 μm~1m.
4. the method according to claim 1 based on dry method cleaning process preparation copper substrate, it is characterised in that: described aerobic
Environment includes pure oxygen atmosphere or the mixed-gas atmosphere comprising oxygen.
5. the method according to claim 1 based on dry method cleaning process preparation copper substrate, it is characterised in that: described aerobic
Environment is open space or closed environment.
6. the method according to claim 1 based on dry method cleaning process preparation copper substrate, it is characterised in that: step 2) is right
The temperature range of copper substrate processing is 20~1100 DEG C.
7. the method according to claim 1 based on dry method cleaning process preparation copper substrate, it is characterised in that: the brass
Bottom includes the copper substrate for being used to prepare CVD graphene.
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| CN201510934979.4A CN106884153B (en) | 2015-12-15 | 2015-12-15 | A method of copper substrate is prepared based on dry method cleaning process |
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| CN201510934979.4A CN106884153B (en) | 2015-12-15 | 2015-12-15 | A method of copper substrate is prepared based on dry method cleaning process |
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| CN106884153A CN106884153A (en) | 2017-06-23 |
| CN106884153B true CN106884153B (en) | 2019-04-30 |
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