CN105800602B - Copper particle is remotely catalyzed the method for directly growing graphene on an insulating substrate - Google Patents
Copper particle is remotely catalyzed the method for directly growing graphene on an insulating substrate Download PDFInfo
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- CN105800602B CN105800602B CN201610125301.6A CN201610125301A CN105800602B CN 105800602 B CN105800602 B CN 105800602B CN 201610125301 A CN201610125301 A CN 201610125301A CN 105800602 B CN105800602 B CN 105800602B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
Abstract
The method for directly growing graphene on an insulating substrate is remotely catalyzed the invention discloses a kind of copper particle, specifically copper acetate is coated uniformly on silica, alundum (Al2O3), aluminium nitride, magnesia, zirconium oxide, boron carbide or carborundum high-temperature insulation substrate by dipping, utilize the method for chemical vapor deposition, graphene is grown with the nano particle remote assistant situ catalytic of the copper of copper acetate high temperature generation, prepares the composite conducting material of graphene.Continuous, graphene can be grown by the present invention, avoid the transfering process of complexity, and graphene can carry out full clad type growth along the structure of substrate, realize duplication of the graphene to underlying structure, the material of preparation can be applied to the numerous areas such as photovoltaic, conduction.
Description
Technical field
The invention belongs to field of preparation of graphene, and in particular to a kind of copper particle remotely directly give birth on an insulating substrate by catalysis
The method of long graphene.
Background technology
Graphene, with performances such as its special optics, electricity, mechanics, calorifics, has turned into scientists and ground since being found
The focus studied carefully.These excellent performances make it, and in fields such as micro-nano device, ultracapacitor, sensor, energy storage, there is latent
Application prospect.In the numerous areas of graphene research, the preparation of graphene, particularly large-size high-quality, the number of plies can
The graphene of control preparation turn into graphene can large-scale application key.Industrially generally use chemical vapor deposition at present
Method prepares large-area graphene, but the graphene prepared is not directly applicable electronic device, be required for the transfer of complexity,
Realize on an insulating substrate direct growth graphene be field of preparation of graphene important topic.
The content of the invention
The side for directly growing graphene on an insulating substrate is remotely catalyzed it is an object of the invention to provide a kind of copper particle
Method, the technical barrier to be solved are directly to prepare graphene on an insulating substrate at relatively low temperature.
Realizing the concrete technical scheme of the object of the invention is：
A kind of copper particle remotely catalysis directly on an insulating substrate grow graphene method, feature be this method include with
Lower specific steps：
(1) substrate is cleaned up, and made annealing treatment；
(2) place the substrate into copper acetate solution, 1-60 minutes take out drying, copper acetate solution is uniformly overlayed on substrate
On；
(3) substrate for being covered with copper acetate is put into tube furnace center, by chemical vapour deposition technique, utilizes copper acetate high temperature
The copper particulate catalytic auxiliary carbon source for decomposing generation decomposes, and in Grown graphene, graphene composite material is made；Wherein：
The substrate is silica, alundum (Al2O3), aluminium nitride, magnesia, zirconium oxide, boron carbide or silicon carbide-based
Bottom；
The substrate cleaning, is respectively cleaned 30 minutes with ethanol and acetone solvent by ultrasonic wave respectively；Substrate annealing temperature
For 800-1200 DEG C, annealing time is 10-60 minutes；
The copper acetate solution concentration is in 0.001-1 mol/L；
The mode for making copper acetate solution uniformly overlay on substrate is immersion, Best-Effort request, spin coating or dropwise addition；
The chemical vapour deposition technique includes：
(a) it is passed through protective gas and reducing gas excludes inner air tube, evacuation time is 0-120 minutes；And in protection gas
Heating is heated to 600-1300 DEG C of reaction temperature under body and reducing gas atmosphere, and heating rate is at 0.5-20 DEG C/min；It is incubated 0-
120 minutes；
(b) carbon source, gas flow 1-800sccm are then passed to, the reaction time is 1-240 minutes；
(c) after reaction terminates, stopping is passed through carbon source, and it is 10-50 DEG C/min to control rate of temperature fall, is cooled to room temperature；Its
In：
The carbon source is methane, ethane, propane, ethene, acetylene, ethanol or its gaseous mixture；The protective gas be argon gas,
Nitrogen, helium or its gaseous mixture；The reducing gas is hydrogen.
Inventive silica substrate uses monodisperse silica nanosphere, and the nanosphere can be according to document（L. B.
Tau, Y. W. De. Colloids and Surfaces A: Physicochem. Eng. Aspects 356 (2010)
145–149）To prepare.
Beneficial effects of the present invention：
The present invention can grow continuous, graphene, avoid the transfering process of complexity, and stone
Black alkene can carry out full clad type growth along the structure of substrate, realize duplication of the graphene to underlying structure, the material energy of preparation
It is applied to the numerous areas such as photovoltaic, conduction.
Brief description of the drawings
Fig. 1 is the graphene transmission electron microscope that the copper particulate catalytic in the embodiment of the present invention 1 directly grows in quartzy plane
Photo figure；
Fig. 2 is the Raman spectrogram of the graphene in the embodiment of the present invention 4；
Fig. 3 is the transmission electron microscope of graphene/alumina composite material with one-dimensional channels in the embodiment of the present invention 8
Photo figure.
Embodiment
The present invention is described in detail below, and illustrated embodiment is served only for explaining the present invention, without forming to the present invention
The limitation of scope.
Embodiment 1
Commercially available quartz plate is cut into 1cm*1cm quartz plate substrate, first cleaned with liquid detergent and deionized water, then by quartz
Substrate is respectively cleaned 30 minutes with ethanol and acetone solvent by ultrasonic wave respectively, after with deionized water rinse well after 60 DEG C baking
It is dry, made annealing treatment 20 minutes at 1000 DEG C afterwards.Quartz substrate after processing is immersed in 0.1M copper acetate solution 10 points
Clock, take out drying after be put into chemical vapor deposition (CVD) reacting furnace, high temperature furnace keep sealing, be passed through 230sccm argon gas and
15sccm hydrogen 30 minutes excludes inner air tube, keeps argon gas and hydrogen flowing quantity constant and with 20 DEG C/min of heating afterwards
Speed rises 1000 DEG C, after being incubated 30min, is passed through 15sccm methane, regulation hydrogen flowing quantity to 5sccm, the reaction time is 20 points
Clock.Reaction stops being passed through methane after terminating, and keeps argon gas and hydrogen flowing quantity constant, naturally cools to room temperature, obtain graphene/stone
English base material.The transmission electron microscope photo of sample is as shown in Figure 1.
Embodiment 2
Commercially available quartz plate is cut into 1cm*1cm quartz plate substrate, first cleaned with liquid detergent and deionized water, then by quartz
Substrate is respectively cleaned 30 minutes with ethanol and acetone solvent by ultrasonic wave respectively, after with deionized water rinse well after 60 DEG C baking
It is dry, made annealing treatment 20 minutes at 1000 DEG C afterwards.Quartz substrate after processing is immersed in 0.1M copper acetate solution 10 points
Clock, take out drying after be put into chemical vapor deposition (CVD) reacting furnace, high temperature furnace keep sealing, be passed through 230sccm argon gas and
15sccm hydrogen 30 minutes excludes inner air tube, keeps argon gas and hydrogen flowing quantity constant and with 20 DEG C/min of heating afterwards
Speed rises 1000 DEG C, after being incubated 30min, is passed through 15sccm methane, regulation hydrogen flowing quantity to 5sccm, the reaction time is 10 points
Clock.Reaction stops being passed through methane after terminating, and keeps argon gas and hydrogen flowing quantity constant, naturally cools to room temperature, obtain graphene/stone
English base material.
Embodiment 3
The monodispersed silica nanosphere coated substrate of individual layer is prepared, by silica nanosphere substrate at 1000 DEG C
Annealing 20 minutes.Silica nanosphere substrate after processing is immersed in 0.1M copper acetate solution 10 minutes, taken out
It is put into after drying in chemical vapor deposition (CVD) reacting furnace, high temperature furnace keeps sealing, is passed through 230sccm argon gas and 15sccm
Hydrogen 30 minutes exclude inner air tube, keep argon gas afterwards and hydrogen flowing quantity be constant and heating rate liter with 20 DEG C/min
1000 DEG C, after being incubated 30min, 15sccm methane, regulation hydrogen flowing quantity to 5sccm are passed through, the reaction time is 20 minutes.Reaction
Stop being passed through methane after end, keep argon gas and hydrogen flowing quantity constant, naturally cool to room temperature, obtain graphene/silicon dioxide
Nanosphere composite.
Embodiment 4
The method for preparing monodisperse silica nanosphere prepares the monodispersed silica nanosphere coated substrate of individual layer,
Silica nanosphere substrate is made annealing treatment 20 minutes at 1000 DEG C.Silica nanosphere substrate after processing is immersed in
10 minutes in 0.1M copper acetate solution, it is put into after taking out drying in chemical vapor deposition (CVD) reacting furnace, high temperature furnace keeps close
Envelope, the hydrogen of the argon gas and 15sccm that are passed through 230sccm exclude inner air tube in 30 minutes, keep argon gas and hydrogen flowing quantity not afterwards
Become and rise 1000 DEG C with 20 DEG C/min of heating rate, after being incubated 30min, be passed through 15sccm methane, regulation hydrogen flowing quantity arrives
5sccm, reaction time are 10 minutes.Reaction stops being passed through methane after terminating, and keeps argon gas and hydrogen flowing quantity constant, natural cooling
To room temperature, graphene/silicon dioxide nanosphere composite is obtained.The Raman spectrum of sample is as shown in Figure 2.
Embodiment 5
The method for preparing monodisperse silica nanosphere prepares the monodispersed silica nanosphere coated substrate of individual layer,
Silica nanosphere substrate is made annealing treatment 20 minutes at 1000 DEG C.Silica nanosphere substrate after processing is immersed in
10 minutes in 0.1M copper acetate solution, it is put into after taking out drying in chemical vapor deposition (CVD) reacting furnace, high temperature furnace keeps close
Envelope, the hydrogen of the argon gas and 15sccm that are passed through 230sccm exclude inner air tube in 30 minutes, keep argon gas and hydrogen flowing quantity not afterwards
Become and rise 1050 DEG C with 20 DEG C/min of heating rate, after being incubated 30min, be passed through 15sccm methane, regulation hydrogen flowing quantity arrives
5sccm, reaction time are 20 minutes.Reaction stops being passed through methane after terminating, and keeps argon gas and hydrogen flowing quantity constant, natural cooling
To room temperature, graphene/silicon dioxide nanosphere composite is obtained.
Embodiment 6
The method for preparing monodisperse silica nanosphere prepares the monodispersed silica nanosphere coating lining of individual layer
Bottom, silica nanosphere substrate is made annealing treatment 20 minutes at 1000 DEG C.By the silica nanosphere substrate after processing
It is immersed in 0.1M copper acetate solution 10 minutes, is put into after taking out drying in chemical vapor deposition (CVD) reacting furnace, high temperature furnace is protected
Sealing is held, the hydrogen of the argon gas and 15sccm that are passed through 230sccm excludes inner air tube in 30 minutes, keeps argon gas and hydrogen stream afterwards
Measure constant and with 20 DEG C/min heating rates and rise 950 DEG C, after being incubated 30min, be passed through 15sccm methane, adjust hydrogen stream
5sccm is measured, the reaction time is 15 minutes.Reaction stops being passed through methane after terminating, and keeps argon gas and hydrogen flowing quantity constant, natural
Room temperature is cooled to, obtains graphene/silicon dioxide nanosphere composite.
Embodiment 7
The method for preparing monodisperse silica nanosphere prepares the monodispersed silica nanosphere coated substrate of individual layer,
Silica nanosphere substrate is made annealing treatment 20 minutes at 1000 DEG C.Silica nanosphere substrate after processing is immersed in
10 minutes in 0.1M copper acetate solution, it is put into after taking out drying in chemical vapor deposition (CVD) reacting furnace, high temperature furnace keeps close
Envelope, the hydrogen of the argon gas and 15sccm that are passed through 230sccm exclude inner air tube in 30 minutes, keep argon gas and hydrogen flowing quantity not afterwards
Become and rise 900 DEG C with 20 DEG C/min of heating rate, after being incubated 30min, be passed through 15sccm methane, regulation hydrogen flowing quantity arrives
5sccm, reaction time are 10 minutes.Reaction stops being passed through methane after terminating, and keeps argon gas and hydrogen flowing quantity constant, natural cooling
To room temperature, graphene/silicon dioxide nanosphere composite is obtained.
Embodiment 8
By commercially available one-dimensional channels alundum (Al2O3) substrate（About 100 nanometers of channel diameter）Led to respectively with ethanol and acetone solvent
Cross ultrasonic wave respectively cleaning 30 minutes, after with deionized water rinse well after 60 DEG C drying, make annealing treatment 20 at 1000 DEG C afterwards
Minute.Alumina substrate after processing is immersed in 0.1M copper acetate solution 10 minutes, chemical gaseous phase is put into after taking out drying
Deposit in (CVD) reacting furnace, high temperature furnace keeps sealing, is passed through 230sccm argon gas and 15sccm 30 minutes drains of hydrogen
Interior air, argon gas is kept afterwards and hydrogen flowing quantity is constant and heating rate with 20 DEG C/min rises 1000 DEG C, after being incubated 30min,
15sccm methane, regulation hydrogen flowing quantity to 5sccm are passed through, the reaction time is 20 minutes.Reaction stops being passed through methane after terminating,
Keep argon gas and hydrogen flowing quantity constant, naturally cool to room temperature, obtain graphene/Al 2 O 3 composition.Sample it is saturating
It is as shown in Figure 3 to penetrate electromicroscopic photograph.
Embodiment 9
Magnesia substrate is respectively cleaned 30 minutes with ethanol and acetone solvent by ultrasonic wave respectively, after use deionized water
60 DEG C of drying, make annealing treatment 20 minutes at 1000 DEG C afterwards after rinsing well.Alumina substrate after processing is immersed in 0.1M
Copper acetate solution in 10 minutes, take out drying after be put into chemical vapor deposition (CVD) reacting furnace, high temperature furnace keep sealing,
The hydrogen of the argon gas and 15sccm that are passed through 230sccm excludes inner air tube in 30 minutes, keeps argon gas and hydrogen flowing quantity constant afterwards
And 1000 DEG C are risen with 20 DEG C/min of heating rate, after being incubated 30min, 15sccm methane is passed through, regulation hydrogen flowing quantity arrives
5sccm, reaction time are 20 minutes.Reaction stops being passed through methane after terminating, and keeps argon gas and hydrogen flowing quantity constant, natural cooling
To room temperature, graphene/magnesium oxide composite material is obtained.
Embodiment 10
Boron carbide substrate is respectively cleaned 30 minutes with ethanol and acetone solvent by ultrasonic wave respectively, after rushed with deionized water
60 DEG C of drying, make annealing treatment 20 minutes at 1000 DEG C afterwards after wash clean.Alumina substrate after processing is immersed in 0.1M's
10 minutes in copper acetate solution, it is put into after taking out drying in chemical vapor deposition (CVD) reacting furnace, high temperature furnace keeps sealing, leads to
The hydrogen of the argon gas and 15sccm that enter 230sccm excludes inner air tube in 30 minutes, keeps argon gas and hydrogen flowing quantity constant simultaneously afterwards
1000 DEG C are risen with 20 DEG C/min of heating rate, after being incubated 30min, is passed through 15sccm methane, regulation hydrogen flowing quantity arrives
5sccm, reaction time are 20 minutes.Reaction stops being passed through methane after terminating, and keeps argon gas and hydrogen flowing quantity constant, natural cooling
To room temperature, graphene/carbon boron composite is obtained.
Claims (2)
1. a kind of copper particle is remotely catalyzed the method for directly growing graphene on an insulating substrate, it is characterised in that this method includes
Step in detail below：
（1）Substrate is cleaned up, and made annealing treatment；
（2）Place the substrate into copper acetate solution, 1-60 minutes take out drying, copper acetate solution is uniformly overlayed on substrate；
（3）The substrate for being covered with copper acetate is put into tube furnace center, by chemical vapour deposition technique, utilizes copper acetate pyrolytic
The copper particulate catalytic auxiliary carbon source of generation decomposes, and in Grown graphene, graphene composite material is made；Wherein：
The substrate is silica, alundum (Al2O3), aluminium nitride, magnesia, zirconium oxide, boron carbide or silicon carbide substrate；
The substrate cleaning, is respectively cleaned 30 minutes with ethanol and acetone solvent by ultrasonic wave respectively；Substrate annealing temperature is
800-1200 DEG C, annealing time is 10-60 minutes；
The copper acetate solution concentration is in 0.001-1 mol/L；
The mode for making copper acetate solution uniformly overlay on substrate is immersion, Best-Effort request, spin coating or dropwise addition.
2. according to the method for claim 1, it is characterised in that the chemical vapour deposition technique includes：
(a) it is passed through protective gas and reducing gas excludes inner air tube, evacuation time is 30 minutes；And in protective gas and also
Heating is heated to 600-1300 DEG C of reaction temperature under raw-gas atmosphere, and heating rate is at 0.5-20 DEG C/min；Insulation 10 minutes or
20 minutes；
(b) carbon source, gas flow 1-800sccm are then passed to, the reaction time is 1-240 minutes；
(c) after reaction terminates, stopping is passed through carbon source, and it is 10-50 DEG C/min to control rate of temperature fall, is cooled to room temperature；Wherein：
The carbon source is methane, ethane, propane, ethene, acetylene, ethanol or its gaseous mixture；The protective gas is argon gas, nitrogen
Gas, helium or its gaseous mixture；The reducing gas is hydrogen.
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| CN107604338B (en) * | 2017-09-11 | 2019-06-25 | 信阳师范学院 | The method of large area bilayer graphene film is prepared on an insulating substrate |
| CN110155991A (en) * | 2019-04-24 | 2019-08-23 | 华东师范大学 | A kind of preparation method of redox graphene and nitrogen-doped graphene |
| CN110474037B (en) * | 2019-08-30 | 2021-08-31 | 石家庄尚太科技股份有限公司 | Preparation method of porous silicon-carbon composite negative electrode material |
| CN110590173A (en) * | 2019-10-18 | 2019-12-20 | 北京大学 | Method for preparing graphene glass with assistance of metal nanoparticles, graphene glass and defogging glass |
| CN112240896A (en) * | 2020-03-30 | 2021-01-19 | 天津理工大学 | Composite carbon electrode and preparation method and application thereof |
| CN113604100B (en) * | 2021-07-30 | 2022-12-20 | 雷索新材料(苏州)有限公司 | Graphene/copper/micron particle composite material, preparation method thereof, graphene high-temperature heating ink and application |
| CN113788474B (en) * | 2021-11-04 | 2023-03-17 | 航天特种材料及工艺技术研究所 | Graphene nanoribbon horizontal array and preparation method and application thereof |
| CN114735684A (en) * | 2022-06-14 | 2022-07-12 | 之江实验室 | Preparation method of graphene powder |
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| CN103172061A (en) * | 2013-04-16 | 2013-06-26 | 北京大学 | Method for growing large-area graphene on insulating substrate |
| CN104532206A (en) * | 2014-12-12 | 2015-04-22 | 中国科学院重庆绿色智能技术研究院 | Preparation method of graphene doped film growing on insulating substrate in in-situ growth mode |
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