CN105800602A - Method for directly growing graphene on insulating substrate through remote catalysis of copper particle - Google Patents
Method for directly growing graphene on insulating substrate through remote catalysis of copper particle Download PDFInfo
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- CN105800602A CN105800602A CN201610125301.6A CN201610125301A CN105800602A CN 105800602 A CN105800602 A CN 105800602A CN 201610125301 A CN201610125301 A CN 201610125301A CN 105800602 A CN105800602 A CN 105800602A
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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 invention discloses a method for directly growing graphene on an insulating substrate through remote catalysis of copper particles. Specifically, the method comprises the following steps: uniformly coating a high-temperature-resistant insulating substrate of silicon dioxide, aluminum oxide, aluminum nitride, magnesium oxide, zirconium oxide, boron carbide or silicon carbide with cupric acetate in a steeping manner, and by using a chemical vapor deposition method, implementing remote assistant in-situ catalytic growth of graphene by using copper nanoparticles generated from the cupric acetate at high temperature, thereby preparing a graphene composite conductive material. By adopting the method, continuous, large-scale and low-defect graphene can be generated, complex transfer procedures are avoided, the graphene can grow along the structure of a substrate in a full-wrapping manner, duplication of the substrate structure can be achieved by using the graphene, and the prepared material can be used in multiple fields such as the photovoltaic industry and the electric conduction industry.
Description
Technical field
The invention belongs to field of preparation of graphene, be specifically related to a kind of method that long-range catalysis of copper granule directly grows Graphene on an insulating substrate.
Background technology
Graphene with performances such as its special optics, electricity, mechanics, calorifics, has become the focus of scientists study since being found.The performance of these excellences makes it there is potential application prospect in fields such as micro-nano device, ultracapacitor, sensor, energy storage.In the numerous areas of Graphene research, the preparation of Graphene, particularly large-size high-quality, can the preparation of the Graphene that the number of plies is controlled becomes Graphene the key of large-scale application.Current industrial commonly used chemical vapour deposition technique prepares large-area graphene, but the Graphene of preparation is not directly applicable electronic device, it is required for the transfer of complexity, it is achieved direct growth Graphene is the important topic of field of preparation of graphene on an insulating substrate.
Summary of the invention
It is an object of the invention to provide a kind of method that long-range catalysis of copper granule directly grows Graphene on an insulating substrate, the technical barrier that solve is directly to prepare Graphene on an insulating substrate at relatively low temperature.
The concrete technical scheme realizing the object of the invention is:
A kind of method that long-range catalysis of copper granule directly grows Graphene on an insulating substrate, is characterized as being the method and includes step in detail below:
(1) substrate is cleaned up, and make annealing treatment；
(2) place the substrate in copper acetate solution, within 1-60 minute, take out and dry, make copper acetate solution uniformly overlay on substrate；
(3) substrate being covered with copper acetate is put into tube furnace central authorities, by chemical vapour deposition technique, utilize the copper particulate catalytic auxiliary carbon source that copper acetate pyrolytic generates to decompose, at Grown Graphene, prepare graphene composite material；Wherein:
Described substrate is silicon dioxide, aluminium sesquioxide, aluminium nitride, magnesium oxide, zirconium oxide, boron carbide or silicon carbide substrate；
Described substrate cleans, and respectively cleans 30 minutes with ethanol and acetone solvent by ultrasound wave respectively；Substrate annealing temperature is 800-1200 DEG C, and annealing time is 10-60 minute；
Described copper acetate solution concentration is at 0.001-1mol/L；
The described mode making copper acetate solution uniformly overlay on substrate is immersion, Best-Effort request, spin coating or dropping；
Described chemical vapour deposition technique includes:
A () passes into protective gas and reducing gas gets rid of inner air tube, and evacuation time is 0-120 minute；And the heating that heats up under protective gas and reducing gas atmosphere is to reaction temperature 600-1300 DEG C, heating rate is at 0.5-20 DEG C/min；It is incubated 0-120 minute；
B () then passes to carbon source, gas flow is 1-800sccm, and the response time is 1-240 minute；
C () reaction stops passing into carbon source after terminating, control rate of temperature fall and be 10-50 DEG C/min, be cooled to room temperature；Wherein:
Described carbon source is methane, ethane, propane, ethylene, acetylene, ethanol or its gaseous mixture；Described protective gas is argon, nitrogen, helium or its gaseous mixture；Described reducing gas is hydrogen.
Inventive silica substrate adopts monodisperse silica nanosphere, and this nanosphere can be prepared according to document (L.B.Tau, Y.W.De.ColloidsandSurfacesA:Physicochem.Eng.Aspects356 (2010) 145 149).
Beneficial effects of the present invention:
The present invention can grow the Graphene of continuous print, defect large-area, low, avoid the transfering process of complexity, and Graphene can carry out full clad type growth along the structure of substrate, it is achieved the Graphene duplication to underlying structure, the material of preparation can be applied to the numerous areas such as photovoltaic, conduction.
Accompanying drawing explanation
Fig. 1 is the directly Graphene transmission electron microscope photo figure of growth in quartz plane of the copper particulate catalytic in the embodiment of the present invention 1；
Fig. 2 is the Raman spectrogram of the Graphene in the embodiment of the present invention 4；
Fig. 3 is the transmission electron microscope photo figure of the alumina composite material of the Graphene in the embodiment of the present invention 8/have one-dimensional channels.
Detailed description of the invention
The present invention is described in detail below, and illustrated embodiment is served only for explaining the present invention, and is not meant to limit the scope of the invention.
Embodiment 1
Commercially available piezoid is cut into the piezoid substrate of 1cm*1cm, first clean with liquid detergent and deionized water, again quartz substrate is respectively cleaned 30 minutes by ultrasound wave with ethanol and acetone solvent respectively, after rinse rear 60 DEG C of drying well with deionized water, annealing 20 minutes at 1000 DEG C afterwards.Quartz substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 1000 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 20 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain Graphene/silica base material.The transmission electron microscope photo of sample is as shown in Figure 1.
Embodiment 2
Commercially available piezoid is cut into the piezoid substrate of 1cm*1cm, first clean with liquid detergent and deionized water, again quartz substrate is respectively cleaned 30 minutes by ultrasound wave with ethanol and acetone solvent respectively, after rinse rear 60 DEG C of drying well with deionized water, annealing 20 minutes at 1000 DEG C afterwards.Quartz substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 1000 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 10 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain Graphene/silica base material.
Embodiment 3
Prepare the monodispersed silica nanosphere coated substrate of monolayer, silica nanosphere substrate is made annealing treatment 20 minutes at 1000 DEG C.Silica nanosphere substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 1000 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 20 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain graphene/silicon dioxide nanosphere composite.
Embodiment 4
The method preparing monodisperse silica nanosphere prepares the monodispersed silica nanosphere coated substrate of monolayer, is made annealing treatment 20 minutes by silica nanosphere substrate at 1000 DEG C.Silica nanosphere substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 1000 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 10 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain graphene/silicon dioxide nanosphere composite.The Raman spectrum of sample is as shown in Figure 2.
Embodiment 5
The method preparing monodisperse silica nanosphere prepares the monodispersed silica nanosphere coated substrate of monolayer, is made annealing treatment 20 minutes by silica nanosphere substrate at 1000 DEG C.Silica nanosphere substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 1050 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 20 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain graphene/silicon dioxide nanosphere composite.
Embodiment 6
The method preparing monodisperse silica nanosphere prepares the monodispersed silica nanosphere coated substrate of monolayer, is made annealing treatment 20 minutes by silica nanosphere substrate at 1000 DEG C.Silica nanosphere substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 950 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 15 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain graphene/silicon dioxide nanosphere composite.
Embodiment 7
The method preparing monodisperse silica nanosphere prepares the monodispersed silica nanosphere coated substrate of monolayer, is made annealing treatment 20 minutes by silica nanosphere substrate at 1000 DEG C.Silica nanosphere substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 900 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 10 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain graphene/silicon dioxide nanosphere composite.
Embodiment 8
Commercially available one-dimensional channels aluminium sesquioxide substrate (channel diameter about 100 nanometers) is respectively cleaned 30 minutes by ultrasound wave with ethanol and acetone solvent respectively, after rinse rear 60 DEG C of drying well with deionized water, annealing 20 minutes at 1000 DEG C afterwards.Alumina substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 1000 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 20 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain Graphene/Al 2 O 3 composition.The transmission electron microscope photo of sample is as shown in Figure 3.
Embodiment 9
Magnesium oxide substrate is respectively cleaned 30 minutes by ultrasound wave with ethanol and acetone solvent respectively, after rinse rear 60 DEG C of drying well with deionized water, annealing 20 minutes at 1000 DEG C afterwards.Alumina substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 1000 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 20 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain Graphene/magnesium oxide composite material.
Embodiment 10
Boron carbide substrate is respectively cleaned 30 minutes by ultrasound wave with ethanol and acetone solvent respectively, after rinse rear 60 DEG C of drying well with deionized water, annealing 20 minutes at 1000 DEG C afterwards.Alumina substrate after processing is immersed in the copper acetate solution of 0.1M 10 minutes, take out and put in chemical vapour deposition (CVD) (CVD) reacting furnace after drying, high temperature furnace keeps sealing, the hydrogen of the argon and 15sccm that pass into 230sccm gets rid of inner air tube in 30 minutes, keep argon afterwards and hydrogen flowing quantity is constant and rises 1000 DEG C with the heating rate of 20 DEG C/min, after insulation 30min, pass into the methane of 15sccm, regulating hydrogen flowing quantity to 5sccm, the response time is 20 minutes.Reaction stops passing into methane after terminating, and keeps argon and hydrogen flowing quantity constant, naturally cools to room temperature, obtain graphene/carbon boron composite.
Claims (2)
1. the method that the long-range catalysis of copper granule directly grows Graphene on an insulating substrate, it is characterised in that the method includes step in detail below:
(1) substrate is cleaned up, and make annealing treatment；
(2) place the substrate in copper acetate solution, within 1-60 minute, take out and dry, make copper acetate solution uniformly overlay on substrate；
(3) substrate being covered with copper acetate is put into tube furnace central authorities, by chemical vapour deposition technique, utilize the copper particulate catalytic auxiliary carbon source that copper acetate pyrolytic generates to decompose, at Grown Graphene, prepare graphene composite material；Wherein:
Described substrate is silicon dioxide, aluminium sesquioxide, aluminium nitride, magnesium oxide, zirconium oxide, boron carbide or silicon carbide substrate；
Described substrate cleans, and respectively cleans 30 minutes with ethanol and acetone solvent by ultrasound wave respectively；Substrate annealing temperature is 800-1200 DEG C, and annealing time is 10-60 minute；
Described copper acetate solution concentration is at 0.001-1mol/L；
The described mode making copper acetate solution uniformly overlay on substrate is immersion, Best-Effort request, spin coating or dropping.
2. method according to claim 1, it is characterised in that described chemical vapour deposition technique includes:
A () passes into protective gas and reducing gas gets rid of inner air tube, and evacuation time is 0-120 minute；And the heating that heats up under protective gas and reducing gas atmosphere is to reaction temperature 600-1300 DEG C, heating rate is at 0.5-20 DEG C/min；It is incubated 0-120 minute；
B () then passes to carbon source, gas flow is 1-800sccm, and the response time is 1-240 minute；
C () reaction stops passing into carbon source after terminating, control rate of temperature fall and be 10-50 DEG C/min, be cooled to room temperature；Wherein:
Described carbon source is methane, ethane, propane, ethylene, acetylene, ethanol or its gaseous mixture；Described protective gas is argon, nitrogen, helium or its gaseous mixture；Described reducing gas is hydrogen.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107604338A (en) * | 2017-09-11 | 2018-01-19 | 信阳师范学院 | The method for preparing large area bilayer graphene film 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 |
| CN110474037A (en) * | 2019-08-30 | 2019-11-19 | 石家庄尚太科技有限公司 | A kind of preparation method of porous silicon-carbon composite cathode 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 |
| CN113604100A (en) * | 2021-07-30 | 2021-11-05 | 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 |
| CN113788474A (en) * | 2021-11-04 | 2021-12-14 | 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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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107604338A (en) * | 2017-09-11 | 2018-01-19 | 信阳师范学院 | The method for preparing large area bilayer graphene film on an insulating substrate |
| 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 |
| CN110474037A (en) * | 2019-08-30 | 2019-11-19 | 石家庄尚太科技有限公司 | A kind of preparation method of porous silicon-carbon composite cathode 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 |
| CN113604100A (en) * | 2021-07-30 | 2021-11-05 | 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 |
| CN113788474A (en) * | 2021-11-04 | 2021-12-14 | 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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