CN106498468A - A kind of method for preparing nano-graphene piece - Google Patents
A kind of method for preparing nano-graphene piece Download PDFInfo
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- CN106498468A CN106498468A CN201610984426.4A CN201610984426A CN106498468A CN 106498468 A CN106498468 A CN 106498468A CN 201610984426 A CN201610984426 A CN 201610984426A CN 106498468 A CN106498468 A CN 106498468A
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- graphite
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- graphene piece
- graphene
- natural flake
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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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
Abstract
A kind of method for preparing nano-graphene piece, belongs to graphite deep process technology field.The problems such as preparing the high cost of Graphene in order to solve above-mentioned technology, pollute environment, the method comprising the steps of：First, with natural flake graphite as raw material, binding agent is added in natural flake graphite, is sufficiently mixed, stirs.2nd, the graphite of mix homogeneously is put in mould, while heating, while applies pressure, cooled down after holding certain time.3rd, by molding after graphite block be put in vacuum induction heating furnace and carry out high-temperature heat treatment.4th, the graphite block through high-temperature process is carried out differential arc oxidation process, while applying supersound process, obtains nano-graphene piece.Present invention process is simple, and environmental protection, steady quality are easy to produce in enormous quantities.
Description
Technical field
The invention belongs to graphite deep process technology field, is related to a kind of preparation method of nano-graphene piece.
Background technology
Nano-graphene piece is ultra-thin graphite laminate accumulation body of the thickness in 20 nanometer ranges.Relative to common stone
Ink, the thickness of nano-graphene piece are in the range of nanoscale.Nano-graphene piece has high intensity, high connductivity, high heat conduction
Performance and good lubricity, heat-resisting quantity, corrosion resistance and high-specific surface area, can be used for ultracapacitor, conduction, anti-quiet
The field such as electricity and electromagnetic shielding.Nano-graphene piece itself has high heat conductivity, is fully compatible for as hot interface material
The filler of material, is greatly improved the heat conductivity of matrix material；Through the modified composite of nano-graphene piece, both changed
It has been apt to the decay resistance of polymer, but also with good heat conductivity, while can also reduce the thermal coefficient of expansion of composite,
Can be widely applied to LED radiator, hot-water pipeline system or the heat-exchange apparatus with corrosivity industrial media；Through nanometer stone
The modified elastomer of black alkene piece, such as packing ring and heat conductive rubber piece etc., it both provided safe and reliable sinking path for device, rose again
To sealing, the effect of damping；For the thermal conductive adhesive requirement more and more higher for being used as sealing and thermal interfacial material.It is added with and receives
The adhesive of rice graphene film is widely used in the bonding of chemical industry heat exchanger, heat conduction embedding, semiconductive ceramic substrate and heat conduction bottom
The nonisulated fields of heat conduction such as the bonding of seat；The conductivity percolation threshold values of the conductive plasticss prepared by nano-graphene piece is far below general
Logical conductive filler, overcomes the deficiency of common graphite filler, before having wide application in terms of Plastic conductive, anti-static material
Scape, improves the wear-resisting of plastic cement, greasy property and corrosion resistance；Nano-graphene piece has corrosion-resistant, resistant to elevated temperatures characteristic, and moistens
Sliding effect substantially, can be used as high-temperature lubricating material；Nano-graphene piece is in electromagnetic shielding material, senior electrically conductive ink, high intensity
The fields such as engineering plastics, all have in fields such as national defense industry, aerospace industry, auto industry, communication industry and energy industries
There is potential application prospect.
The method for preparing Graphene at present mainly has chemical oxidization method, chemical vapour deposition technique and liquid phase stripping method, wherein：Chemistry
Oxidizing process pollutes environment due in a large number using strong acid and strong oxidizer；Chemical vapour deposition technique high cost, efficiency are low；Liquid phase is shelled
From method as dispersant is out difficult, few layer graphene is prepared difficult.In addition, said method production small size Graphene is non-
Often difficult.
Content of the invention
The problems such as preparing the high cost of Graphene in order to solve above-mentioned technology, pollute environment, the invention provides a kind of system
The method of standby nano-graphene piece.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method for preparing nano-graphene piece, comprises the following steps：
First, with natural flake graphite as raw material, binding agent is added in natural flake graphite, is sufficiently mixed, stirs, control is viscous
20～30wt% of the addition of knot agent for natural flake graphite.
2nd, the graphite of mix homogeneously is put in mould, while heating, while applies pressure, carry out after holding certain time cold
But, heating-up temperature is controlled for 100～220 DEG C, and applying pressure is 80～100MPa, and temperature retention time is 1～3 hour.
3rd, by molding after graphite block be put in vacuum induction heating furnace and carry out high-temperature heat treatment, controlling heating-up temperature is
2500～2800 DEG C, programming rate is 30～50 DEG C/min, is slowly cooled to room temperature after being incubated 3～5 hours.
4th, the graphite block through high-temperature process is carried out differential arc oxidation process, while applying supersound process, obtains a nanometer stone
Black alkene piece, the voltage for controlling differential arc oxidation are 250～400V, and frequency is 500～1000Hz, and electrolyte is sulphuric acid and potassium hydroxide
Mixed solution；Supersonic vibration frequency is 20～25KHz, and power is 2～3KW.
In the present invention, the size of the natural flake graphite is 80～200 mesh.
In the present invention, the binding agent is epoxy resin, phenolic resin or Colophonium.
Present invention process is simple, and environmental protection, steady quality are easy to produce in enormous quantities.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of nano-graphene piece prepared by embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of nano-graphene piece prepared by embodiment 1.
Specific embodiment
Below in conjunction with the accompanying drawings technical scheme is further described, but is not limited thereto, every to this
Inventive technique scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should cover
In protection scope of the present invention.
Embodiment 1
With natural flake graphite as raw material, adopt epoxy resin for binding agent, natural flake graphite is added in the ratio of 20wt%
In, it is sufficiently mixed, stirs.The graphite of mix homogeneously is put in mould, is heated and is applied pressure, control heating temperature
Spend for 220 DEG C, applying pressure is 100MPa, is cooled down after being kept for 1 hour.Graphite block after by cooling shaping is put into vacuum sense
Answering in stove carries out high-temperature heat treatment, controls heating-up temperature for 2600 DEG C, and programming rate is 50 DEG C/min, slow after being incubated 5 hours
Room temperature is cooled to, the graphite block through high-temperature heat treatment is carried out differential arc oxidation process, while applying ultrasonic vibration treatment, you can
Nano-graphene piece is obtained, the voltage for controlling differential arc oxidation is 300V, and frequency is 1000Hz, and electrolyte is 80% sulphuric acid and 20% hydrogen
The mixed solution of potassium oxide；Supersonic vibration frequency is 20KHz, and power is 3KW.
From figure 1 it appears that Graphene thickness manufactured in the present embodiment is less than 10nm, the number of plies is at 20 layers or so.
From figure 2 it can be seen that graphene powder manufactured in the present embodiment is cotton-shaped in group.
Embodiment 2
With natural flake graphite as raw material, adopt phenolic resin for binding agent, natural flake graphite is added in the ratio of 25wt%
In, it is sufficiently mixed, stirs.The graphite of mix homogeneously is put in mould, is heated and is applied pressure, control heating temperature
Spend for 200 DEG C, applying pressure is 90MPa, is cooled down after being kept for 2 hours.Graphite block after by cooling shaping is put into vacuum sense
Answering in stove carries out high-temperature heat treatment, controls heating-up temperature for 2500 DEG C, and programming rate is 40 DEG C/min, slow after being incubated 4 hours
Room temperature is cooled to, the graphite block through high-temperature heat treatment is carried out differential arc oxidation process, while applying ultrasonic vibration treatment, you can
Nano-graphene piece is obtained, the voltage for controlling differential arc oxidation is 250V, and frequency is 500Hz, and electrolyte is 80% sulphuric acid and 20% hydrogen
The mixed solution of potassium oxide；Supersonic vibration frequency is 25KHz, and power is 2KW.
Embodiment 3
With natural flake graphite as raw material, adopt Colophonium for binding agent, be added in natural flake graphite in the ratio of 30wt%,
It is sufficiently mixed, stirs.The graphite of mix homogeneously is put in mould, is heated and is applied pressure, controlling heating-up temperature is
100 DEG C, applying pressure is 80MPa, is cooled down after being kept for 3 hours.Graphite block after by cooling shaping is put into vaccum sensitive stove
In carry out high-temperature heat treatment, control heating-up temperature for 2800 DEG C, programming rate is 40 DEG C/min, Slow cooling after insulation 4 hours
To room temperature, the graphite block through high-temperature heat treatment is carried out differential arc oxidation process, while applying ultrasonic vibration treatment, you can obtain
Nano-graphene piece, the voltage for controlling differential arc oxidation are 400V, and frequency is 800Hz, and electrolyte is 80% sulphuric acid and 20% hydroxide
The mixed solution of potassium；Supersonic vibration frequency is 20KHz, and power is 2KW.
Claims (4)
1. a kind of method for preparing nano-graphene piece, it is characterised in that methods described step is as follows：
First, with natural flake graphite as raw material, binding agent is added in natural flake graphite, is sufficiently mixed, stirs；
2nd, the graphite of mix homogeneously is put in mould, while heating, while applies pressure, cooled down after being kept for certain time, control
Heating-up temperature processed is 100～220 DEG C, and applying pressure is 80～100MPa, and temperature retention time is 1～3 hour；
3rd, by molding after graphite block be put in vacuum induction heating furnace and carry out high-temperature heat treatment, control heating-up temperature for 2500
～2800 DEG C, programming rate is 30～50 DEG C/min, is slowly cooled to room temperature after being incubated 3～5 hours；
4th, the graphite block through high-temperature process is carried out differential arc oxidation process, while applying supersound process, obtains nano-graphene
Piece, the voltage for controlling differential arc oxidation are 250～400V, and frequency is 500～1000Hz, and electrolyte is the mixed of sulphuric acid and potassium hydroxide
Close solution；Supersonic vibration frequency is 20～25KHz, and power is 2～3KW.
2. the method for preparing nano-graphene piece according to claim 1, it is characterised in that the addition of the binding agent
20～30wt% for natural flake graphite.
3. the method for preparing nano-graphene piece according to claim 1 and 2, it is characterised in that the natural flake graphite
Size be 80～200 mesh.
4. the method for preparing nano-graphene piece according to claim 1 and 2, it is characterised in that the binding agent is epoxy
Resin, phenolic resin or Colophonium.
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Citations (7)
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| CN102807213A (en) * | 2012-08-30 | 2012-12-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for electrochemically preparing graphene |
| CN103204494A (en) * | 2012-01-16 | 2013-07-17 | 中央研究院 | Device and method used for scale production of graphene and graphene oxide |
| US20140166496A1 (en) * | 2012-12-14 | 2014-06-19 | Chung-Shan Institute Of Science And Technology | Method for producing shaped graphene sheets |
| CN103991862A (en) * | 2013-12-27 | 2014-08-20 | 杭州金马能源科技有限公司 | Method for preparing high-quality graphene through electrochemical high-efficiency exfoliation |
| CN104495835A (en) * | 2015-01-16 | 2015-04-08 | 黑龙江科技大学 | Method for preparing multilayer graphene through step-by-step oxidization and step-by-step dissociation |
| CN105347330A (en) * | 2015-11-06 | 2016-02-24 | 新乡远东电子科技有限公司 | Preparation method of high specific surface area graphene |
| TW201620826A (en) * | 2014-12-09 | 2016-06-16 | 國立高雄應用科技大學 | Electrochemical method for producing graphene |
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2016
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| CN103204494A (en) * | 2012-01-16 | 2013-07-17 | 中央研究院 | Device and method used for scale production of graphene and graphene oxide |
| CN102807213A (en) * | 2012-08-30 | 2012-12-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for electrochemically preparing graphene |
| US20140166496A1 (en) * | 2012-12-14 | 2014-06-19 | Chung-Shan Institute Of Science And Technology | Method for producing shaped graphene sheets |
| CN103991862A (en) * | 2013-12-27 | 2014-08-20 | 杭州金马能源科技有限公司 | Method for preparing high-quality graphene through electrochemical high-efficiency exfoliation |
| TW201620826A (en) * | 2014-12-09 | 2016-06-16 | 國立高雄應用科技大學 | Electrochemical method for producing graphene |
| CN104495835A (en) * | 2015-01-16 | 2015-04-08 | 黑龙江科技大学 | Method for preparing multilayer graphene through step-by-step oxidization and step-by-step dissociation |
| CN105347330A (en) * | 2015-11-06 | 2016-02-24 | 新乡远东电子科技有限公司 | Preparation method of high specific surface area graphene |
Non-Patent Citations (2)
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| JILEI LIU ET AL: "High-Quality Thin Graphene Films from Fast Electrochemical Exfoliation", 《NANO ENERGY》 * |
| KHALED PARVEZ ET AL: "Electrochemically Exfoliated Graphene as Solution-Processable, Highly Conductive Electrodes for Organic Electronics", 《JOURANL OF THE AMERICAN CHEMICAL SOCIETY》 * |
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Effective date of registration: 20191025 Address after: No. 563, Fengyuan street, tangningjun community, Wanda City, Songbei District, Harbin City, Heilongjiang Province Patentee after: Heilongjiang Yimo Xuan New Material Technology Co., Ltd Address before: 150027, 2468, Pu Yuan Road, Harbin, Heilongjiang, Songbei Patentee before: Heilongjiang University of Science and Technology |
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