CN107298437A - A kind of method of PVD method low temperature preparation graphene - Google Patents
A kind of method of PVD method low temperature preparation graphene Download PDFInfo
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- CN107298437A CN107298437A CN201710667742.3A CN201710667742A CN107298437A CN 107298437 A CN107298437 A CN 107298437A CN 201710667742 A CN201710667742 A CN 201710667742A CN 107298437 A CN107298437 A CN 107298437A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of method of PVD method low temperature preparation graphene, utilize vacuum magnetron sputtering coating film technology, in deposition on substrate atom grain metal film, recycle solid high purity graphite to do target and be embedded in carbon atom in metallic film surface magnetron sputtering, metallic film surface crystallization separates out carbon formation graphene after vacuum heat.When it is applied to field of batteries, lithium battery high rate performance can be significantly improved, cycle life is improved.The more current other graphene preparation methods of the present invention, also with cost is low, graphene layer continuity is good, simple to operate, commercially viable production the features such as.
Description
Technical field
The present invention relates to grapheme material manufacturing, and in particular to a kind of method of PVD method low temperature preparation graphene.
Background technology
Graphene is a kind of two dimensional crystal, is arranged by carbon atom according to hexagon, is connected with each other, and forms a carbon point
Son, its Stability Analysis of Structures is a kind of extensive carbon material of with high content of technology, application potential, in semiconductor industry, photovoltaic industry, lithium
The traditional fields such as ion battery, display of new generation and emerging field all have extensive use.
The current main manufacture method of graphene has four kinds：1. micromechanics stripping method；2. epitaxial growth method；3. aoxidize stone
Black reducing process；4. vapor phase deposition method.
1. micromechanics stripping method
Micromechanics stripping method is：Surface ion is carried out to highly oriented pyrolytic graphite (HOPG) thick 1mm using oxonium ion etc.
Etching；Graphite block surface etch goes out 20 μm~2mm of width, depth and it is adhered into glass substrate with photoresist after 5 μm of microflute
On；Tear-off repeatedly is carried out with cellotape；Unnecessary HOPG is removed；The glass substrate for being stained with microplate is put into acetone soln
It is middle to carry out ultrasound；Monocrystalline silicon piece is put into acetone soln, " pulled single-layer graphene " out using Van der Waals force or capillary force,
So as to obtain graphene film.
Micromechanics stripping method method is simple, but the size of the graphene obtained is difficult to control, it is difficult to obtain sufficient length
Graphene, it is impossible to meet industrialization demand.
2. epitaxial growth method
Epitaxial growth method is the silicon atom evaporation in monocrystalline silicon carbide (SiC), carbon atom warp in high temperature and ultrahigh vacuum
Cross structural rearrangement formation graphene film.The graphene area that epitaxial growth method is obtained is larger, and quality is higher, has the disadvantage monocrystalline
SiC is expensive, and the cost of manufacture of graphene is high, and growth conditions is harsh, and the graphene of generation is difficult transfer.
3. graphite oxide reducing process
Graphite oxide reducing process is that current cost is minimum, be easiest to the graphene preparation method accomplished scale production.Oxygen
Graphite reducing process is native graphite and strong acid and Strong oxdiative thing reaction generation graphite oxide (GO), is prepared by ultrasonic disperse
Into graphene oxide, the oxy radical for adding reducing agent removal graphite oxide surface obtains graphene.Graphite oxide reduces legal system
Make graphene relative efficiency, environmental protection and cost is relatively low, enough large-scale industrial productions；During having the disadvantage redox, stone
The electronic structure and perfection of crystal of black alkene are vulnerable to the destruction of strong oxidizer, influence the molecular characterization of graphene.
4. vapour deposition process
Chemical vapor deposition principle is that one or more gaseous materials are imported into a reaction chamber to chemically react,
Generate a kind of new material and be deposited on substrate surface.It is by carbonaceous gas organic matter methane (CH4), acetylene when preparing graphene
Etc. (C2H2) pyrolytic on the metallic matrix such as nickel or copper, deviates from hydrogen atom, and carbon atom deposition absorption is continuous in metal surface
Grow into graphene.Vapour deposition process making graphene is relatively easy easy, and graphene is more complete, and quality preferably, is easily shifted
Used on to other matrixes, maximum shortcoming is exactly that cost is very high, and difficulty reaches industrialized requirement.
The contrast of four kinds of graphene preparation methods is as shown in the table.
| Produce | Size | Quality | System | Industrialization |
| Machinery | It is medium and small | Molecular structure is complete | It is low | It should not measure |
| Extension | Big chi | Thin slice is difficult and SiC | It is high | It is adapted to small |
| Oxidation | Big chi | Molecular structure easily quilt | It is low | It can advise greatly |
| Gas phase | Big chi | Structural integrity, quality | It is high | It can advise greatly |
The preparation of graphene and apply in world wide also in the Industrialization stage, CVDization can be drawn from upper table
Learn vapour deposition process and prepare graphene, can both obtain high-quality graphene and can be mass-produced.Its principle is：With methane
(CH4) carbon atom or acetylene (C2H2) is as carbon-source gas, is decomposited at a temperature of 600-1100 DEG C；Play carbon and decompose catalytic action
Metallic substrates (Ni, Tu etc.) be heated to zero boundary's molten condition；The carbon atom decomposited is fused into metal lattice；With 10 DEG C/S
Gradient cooling to normal temperature, now base metal is recrystallized, metal tetrahedra and octahedral lattice voids, it is difficult to incorporate atom half
The larger carbon atom in footpath, it is impossible to which the carbon atom of involvement is expressed into metal substrate surface in metal recrystallization process；Metal watch
The carbon atom that face is separated out turns into the growth core of graphene crystal grain, and carbon atom is constantly formed, spread, and graphene crystal grain is constantly
Grow up, finally connect film forming formation graphene.
Chemical vapour deposition technique is good in copper foil surface growth graphene controllability, can obtain large area, high-quality stone
Black alkene, and chemical vapour deposition technique can also grow graphene at ambient pressure.Although it is considered as graphite that CVD, which prepares graphene,
Alkene obtains wide variety of most promising method, but the reaction of gas high-temperature catalytic obtains carbon source control hardly possible, graphene generation temperature
Degree is high (700 DEG C -1200 DEG C) so that CVD produces that quality of graphene is unstable and manufacturing cost is high.
PVD (PhysicalVaporDeposition), refers to and realizes that material is shifted using physical process, by atom or molecule
The process on substrate surface is transferred to by source.Its effect is can to make some have specific characteristics can (intensity height, wearability, radiating
Property, rotproofness etc.) particulate be sprayed on the relatively low parent of performance so that parent has better performance.PVD basic skills：
Be evaporated in vacuo, sputtering, ion plating (hallow cathode deposition, HCD, hot cathode ion plating, arc ion plating, activated reactive evaporation,
RF ion plating, direct-current discharge ion plating).
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of PVD method low temperature produces graphene
Device and technique, i.e., sharp vacuum magnetron sputtering coating film technology, in deposition on substrate atom grain metal film, utilize the high-purity stone of solid
Ink does target magnetron sputtering insertion carbon atom again, separates out carbon formation graphene after metal membrane crystallization after vacuum heat.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of method of PVD method low temperature preparation graphene, it is former in deposition on substrate using vacuum magnetron sputtering coating film technology
Seed metal film, recycles solid high purity graphite to do target and is embedded in carbon atom in metallic film surface magnetron sputtering, by Vacuum Heat
Metallic film surface crystallization separates out carbon formation graphene after processing.
Preferably, the above method has specifically included following steps：
A. film substrate to be plated is put into substrate frame and sends into vacuum chamber, be evacuated to background vacuum 2x10-2Pa~
8x10-4Pa；
B. heating substrate makes its surface temperature reach 100~350 DEG C；
C. cooling down makes substrate temperature reach 50~100 DEG C；
D. treat that vacuum chamber background vacuum is stable in 2x10-2Pa~8x10-4Pa, heating-up temperature are stable 100~350
DEG C, cryogenic temperature it is stable after 50~100 DEG C, toward vacuum chamber in be passed through 120~500Sccm high-purity argon gas；
E. argon flow amount is adjusted, vacuum chamber is really reached technique vacuum 10Pa~6x10-1Pa；
F. DC cathode copper target is opened, in substrate surface sputter 200~500nm thickness copper films；
G. direct current or radio frequency negative electrode graphite target are opened, 5~20nm thickness carbon films are deposited in the substrate surface of copper plating film；
H. substrate plated film completed carries out vacuum heat；
I. the substrate after vacuum heat is cooled down, film surface separates out multi-layer graphene.
Preferably, the substrate uses 0.4mmITO white glasses for experiment.
Preferably, the purity of high-purity argon gas described in step d is 99.995%.
Preferably, the heat time of vacuum heat described in step h is 2~8 minutes.
Preferably, in step i, cooldown rate is 10~30 DEG C/min.
Preferably, the atom grain metal film is Cu atoms grain metal film.
After above-mentioned technology, the present invention has the beneficial effect that：Using vacuum magnetron sputtering coating film technology, in deposition on substrate
Atom grain metal film, recycles solid high purity graphite to do target and is embedded in carbon atom in metallic film surface magnetron sputtering, by vacuum
The carbon atom that metallic film surface is constantly separated out after heat treatment is constantly crystallized using the carbon atom for primarily occur inning film surface as nucleus
It is diffused in substrate surface and forms continuous multi-layer graphene, when it is applied to field of batteries, lithium battery multiplying power can be significantly improved
Performance, improves cycle life.The more current other graphene preparation methods of the present invention, also with cost is low, graphene layer is continuous
Property is good, simple to operate, commercially viable production the features such as.
Figure of description
Fig. 1 is the process flow diagram of the embodiment of the present invention 1.
Embodiment
Below in conjunction with embodiment of the present invention, the technology in embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of scheme of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment party that those of ordinary skill in the art are obtained under the premise of creative work is not made
Case, belongs to the scope of protection of the invention.
Embodiment 1, with reference to shown in Fig. 1, is provided with delivery roll 1, delivery roll 1 in vacuum tank 4 and is provided with substrate frame 3,
The top of delivery roll 1 is sequentially provided with copper film sputter area 10, graphite sputter area 11, vacuum heat area 9 and cooling by its transmission direction
Area 8, copper film sputter area 10 is provided with high-purity copper targets 12, and graphite sputter area 11 is provided with high purity graphite target 13, copper film sputter
Area 10 and graphite sputter area 11 are equipped with magnetic control sputtering cathode, and substrate 2 is positioned in substrate frame 3, by being deposited on substrate 2
Copper atom granulosa, in general, can also deposit other metal films, metal film here is preferred with copper film, recycle solid high
Pure graphite does target and is embedded in carbon atom in copper film surface magnetic control sputtering, and copper film surface crystallization separates out carbon shape after vacuum heat
Into graphene, copper film 5 and graphite ene coatings 7 are finally formed on substrate 2.
Specifically, the process of the test of the above method has specifically included following steps：
A. experiment is put into substrate frame using after the cleaning of 0.4mmITO plated film grades white glass as film substrate to be plated；
B. background vacuum 2x10 is evacuated to after substrate frame being sent into vacuum chamber-2Pa~8x10-4Pa；
C. vacuum heat heater 91 is opened, adjustment heater power makes substrate surface temperature reach 100~350 DEG C；
D. vacuum cooled coil pipe 81 is opened, adjustment refrigeration work consumption makes substrate temperature reach 50~100 DEG C；
E. treat that vacuum chamber background vacuum is stable in 2x10-2Pa~8x10-4Pa, heating-up temperature are stable 100~350
DEG C, cryogenic temperature it is stable after 50~100 DEG C, open gas mass flow gauge and be passed through 120~500Sccm, purity is
99.995% high-purity argon gas；
F. argon flow amount is adjusted, the vacuum of vacuum chamber is reached technique vacuum 10Pa~6x10-1Pa；
G. DC cathode copper target is opened, adjustment target power output is in substrate surface sputter 200~500nm thickness copper films；
H. direct current or radio frequency negative electrode graphite target are opened, adjustment target power output and sputtering voltage sink in the substrate surface of copper plating film
Product or embedded 5~20nm thickness carbon films；
I. substrate to the vacuum heat area for moving plated film completion carries out copper atom and carbon atom hybrid-sorting, control heating
2~8 minutes time；
J. the substrate after heating is moved to vacuum coil pipe cooling zone and carries out analysis carbon, and cooldown rate sets 10~30 DEG C/min,
The carbon atom constantly separated out is diffused in substrate surface as nucleus constantly crystallization to primarily occur in the carbon atom of film surface and formed
Continuous multi-layer graphene.
By the above method, sputter copper film 5 and graphene layer 7 on base material 2, when it is applied to field of batteries, energy
Lithium battery high rate performance is significantly improved, cycle life is improved.The more current other graphene preparation methods of the present invention, also with into
This low, graphene layer continuity is good, simple to operate, commercially viable production the features such as.
While embodiments of the invention have been illustrated and described, for the ordinary skill in the art, may be used
A variety of to the progress of these embodiments can be changed without departing from the principles and spirit of the present invention with understanding, changed,
Replace and modification, the scope of the present invention is defined by the appended.
In the description of this specification, reference term " embodiment ", " some embodiments ", " an implementation
The description of example ", " some embodiments ", " example ", " specific example " or " some examples " etc. means to combine the embodiment or example
Specific features, structure, material or the feature of description are contained at least one embodiment of the present invention or example.In this explanation
In book, identical embodiment or example are not necessarily referring to the schematic representation of above-mentioned term.Moreover, the specific spy of description
Levy, structure, material or feature can in an appropriate manner be combined in any one or more embodiments or example.
Above content is to combine specific embodiment further description made for the present invention, it is impossible to assert this hair
Bright specific implementation is confined to these explanations.For general technical staff of the technical field of the invention, do not taking off
On the premise of from present inventive concept, some simple deduction or replace can also be made.
Claims (7)
1. a kind of method of PVD method low temperature preparation graphene, it is characterised in that vacuum magnetron sputtering coating film technology is utilized, in substrate
Upper deposition and atomic grain metal film, recycles solid high purity graphite to do target and is embedded in carbon atom, warp in metallic film surface magnetron sputtering
Cross metallic film surface crystallization after vacuum heat and separate out carbon formation graphene.
2. the method for a kind of PVD method low temperature preparation graphene according to claim 1, it is characterised in that include following step
Suddenly：
A. film substrate to be plated is put into substrate frame and sends into vacuum chamber, be evacuated to background vacuum 2x10-2Pa~8x10- 4Pa；
B. heating substrate makes its surface temperature reach 100~350 DEG C；
C. cooling down makes substrate temperature reach 50~100 DEG C；
D. treat that vacuum chamber background vacuum is stable in 2x10-2Pa~8x10-4Pa, heating-up temperature are stable in 100~350 DEG C, system
Cold temperature stabilization after 50~100 DEG C, toward vacuum chamber in be passed through 120~500Sccm high-purity argon gas；
E. argon flow amount is adjusted, vacuum chamber is really reached technique vacuum 10Pa~6x10-1Pa；
F. DC cathode copper target is opened, in substrate surface sputter 200~500nm thickness copper films；
G. direct current or radio frequency negative electrode graphite target are opened, 5~20nm thickness carbon films are deposited in the substrate surface of copper plating film；
H. substrate plated film completed carries out vacuum heat；
I. the substrate after vacuum heat is cooled down, film surface separates out multi-layer graphene.
3. the method for a kind of PVD method low temperature preparation graphene according to claim 2, it is characterised in that the substrate is real
Test and use 0.4mmITO white glasses.
4. the method for a kind of PVD method low temperature preparation graphene according to claim 2, it is characterised in that described in step d
The purity of high-purity argon gas is 99.995%.
5. the method for a kind of PVD method low temperature preparation graphene according to claim 2, it is characterised in that described in step h
The heat time of vacuum heat is 2~8 minutes.
6. the method for a kind of PVD method low temperature preparation graphene according to claim 2, it is characterised in that in step i, cooling
Speed is 10~30 DEG C/min.
7. a kind of method of PVD method low temperature preparation graphene according to claim 1, it is characterised in that the atom grain gold
It is Cu atoms grain metal film to belong to film.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108258226A (en) * | 2018-01-25 | 2018-07-06 | 深圳市德方纳米科技股份有限公司 | A kind of carbon coating tertiary cathode material and preparation method thereof |
| CN109399622A (en) * | 2018-09-04 | 2019-03-01 | 中国电子科技集团公司第十六研究所 | A kind of preparation method of graphene |
| CN114906840A (en) * | 2022-06-13 | 2022-08-16 | 沈阳金锋特种刀具有限公司 | Graphene with laminated pore structure, cutter and preparation method of graphene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108258226A (en) * | 2018-01-25 | 2018-07-06 | 深圳市德方纳米科技股份有限公司 | A kind of carbon coating tertiary cathode material and preparation method thereof |
| CN109399622A (en) * | 2018-09-04 | 2019-03-01 | 中国电子科技集团公司第十六研究所 | A kind of preparation method of graphene |
| CN114906840A (en) * | 2022-06-13 | 2022-08-16 | 沈阳金锋特种刀具有限公司 | Graphene with laminated pore structure, cutter and preparation method of graphene |
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