CN110194450A - A kind of preparation method of graphene composite material - Google Patents
A kind of preparation method of graphene composite material Download PDFInfo
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- CN110194450A CN110194450A CN201910394028.0A CN201910394028A CN110194450A CN 110194450 A CN110194450 A CN 110194450A CN 201910394028 A CN201910394028 A CN 201910394028A CN 110194450 A CN110194450 A CN 110194450A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
Abstract
The invention discloses a kind of preparation methods of graphene composite material, the following steps are included: weighing a certain amount of graphite, and graphite is put into grinder and is ground, smashed graphite particle is screened by 200-300 mesh, obtain graphite particle, the graphite particle that above-mentioned steps are obtained is added in a certain amount of ethanol solution, it stirs evenly, it mixes them thoroughly, and mixed solution is removed under the action of ultrasonic peel-off device, obtain the preparation method of this graphene composite material of graphene oxide dispersion, by the way that dimethylformamide and hydrazine hydrate is added in graphene oxide solution, in reduction process, ammonium hydroxide is added, the adjusting of pH value can be carried out by ammonium hydroxide, it can effectively avoid the reunion of graphene.
Description
Technical field
The present invention relates to graphene composite material preparation technical field, specially a kind of preparation side of graphene composite material
Method.
Background technique
Graphene is the most thin material being currently known；And it is not only frivolous, and it is also very securely and soft；Graphite
Alkene has very high mechanical strength, good thermal conductivity and quick carrier mobility；Graphene composite material is made in recent years
For a kind of new material, is paid attention to and applied by more and more people.
The preparation of graphene composite material is there are many kinds of method, which has become the hot spot of scholars' attention, especially
It is that graphene composite material has become in current new material " star ".
Graphene is that the hexangle type of only one carbon atom thickness is in the flat film of honeycomb lattice, has extraordinary lead
Hot, electrical conductance, translucency, and there are the characteristics such as high intensity, ultra-thin, extra specific surface area, thus it is known as " super material
Material ".The purposes of graphene is very extensive, can be applied to lithium ion battery electrode material, thin film transistor (TFT), sensor, half
Conductor device, composite material preparation, transparence display touch screen etc..
As the nova of material circle, graphene is to be currently known best at room temperature conduction and Heat Conduction Material.Graphene is excellent
Different performance makes it have change potentiality in multiple fields, and the field gained ground includes flexible touch panel, miniature
Sensor, secondary cell, chip material etc..
Currently, the technical bottleneck of graphene prepare with scale is gradually broken through substantially, limitation graphene industry development is not
It is again the scale preparation of graphene, but the graphene of preparation how is allowed to meet the needs of different application field, how makes stone
The high-performance of black alkene such as high conductivity, high-termal conductivity, high light transmittance give full play in application field.This is to be currently undertaken by graphene
One crucial technical problem of research institution and enterprise's facing of material, while being also graphene industry future to need to break through
Key bottleneck.Meanwhile China's graphene industry is also faced with the problems such as technical transform ability is weak, commercial application field is narrow.
At present since graphene is easy to happen reunion, the group of being easy to appear in graphene composite material preparation process
It is poly-, it is therefore necessary to improvement is designed to it.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of graphene composite material, to solve in above-mentioned background technique
The problem of proposition.
In order to solve the above technical problems, the present invention provides a kind of preparation method of graphene composite material, including it is following
Step:
A. a certain amount of graphite is weighed, and graphite is put into grinder and is ground, smashed graphite particle passes through 200-
300 meshes are screened, and graphite particle is obtained；
B. graphite particle above-mentioned steps obtained is added in a certain amount of ethanol solution, stirs evenly, mixes them thoroughly, and
Mixed solution is removed under the action of ultrasonic peel-off device, obtains graphene oxide dispersion；
C. graphene oxide dispersion above-mentioned steps obtained is added in dimethyl formamide solution, and above-mentioned mixed solution is existed
Be sufficiently stirred under the action of uniform device 1-2 hours, uniformly after aqueous solution hydrazine hydrate and ammonium hydroxide be added be again stirring for, and anti-
Reduction in kettle is answered to obtain graphene aqueous solution；
D. by the graphene aqueous solution of above-mentioned acquisition, distillation obtains graphene platelet in distillation ware, by the graphene platelet of acquisition
Pulverized particles are obtained under the grinding of spherical grinder；
E., the graphene of acquisition is passed through to such as a certain proportion of hydrogen and nitrogen in high temperature PVT growth furnace, 1500-1600's
At a temperature of react 2-3h, then pass to argon gas and heat 2000-2300 degrees Celsius, then cooling obtain graphene composite material.
Further, the volume ratio of the hydrogen and nitrogen is 1:20.
Further, evacuated state is always maintained inside the high temperature PVT growth furnace.
Further, the reaction kettle be heating reaction kettle, and graphene oxide dispersion reduction when, reaction kettle
Temperature is 80-100 degrees Celsius.
The beneficial effects of the present invention are: the preparation method of this graphene composite material, by adding in graphene oxide solution
Enter dimethylformamide and hydrazine hydrate, in reduction process, ammonium hydroxide is added, the adjusting of pH value can be carried out by ammonium hydroxide, can effectively be kept away
Exempt from the reunion of graphene.
Specific embodiment
Further instruction With reference to embodiment, but following detailed description should not be done and be managed
Solution is the limitation invented ontology.Those of ordinary skill in the art can apparently make various on the basis of the present invention
Change and change, it should within the scope of invention.
Embodiment 1:
A kind of preparation method of graphene composite material, comprising the following steps:
A. a certain amount of graphite is weighed, and graphite is put into grinder and is ground, smashed graphite particle passes through 200 mesh
It is screened, obtains graphite particle；
B. graphite particle above-mentioned steps obtained is added in a certain amount of ethanol solution, stirs evenly, mixes them thoroughly, and
Mixed solution is removed under the action of ultrasonic peel-off device, obtains graphene oxide dispersion；
C. graphene oxide dispersion above-mentioned steps obtained is added in dimethyl formamide solution, and above-mentioned mixed solution is existed
Be sufficiently stirred under the action of uniform device 1 hour, uniformly after aqueous solution hydrazine hydrate and ammonium hydroxide be added be again stirring for, and reacting
Reduction obtains graphene aqueous solution in kettle；
D. by the graphene aqueous solution of above-mentioned acquisition, distillation obtains graphene platelet in distillation ware, by the graphene platelet of acquisition
Pulverized particles are obtained under the grinding of spherical grinder；
E., the graphene of acquisition is passed through to such as a certain proportion of hydrogen and nitrogen in high temperature PVT growth furnace, in 1500 temperature
Lower reaction 2h then passes to argon gas and heats 2000 degrees Celsius, and then cooling obtains graphene composite material.
The volume ratio of the hydrogen and nitrogen is 1:20.
Evacuated state is always maintained inside the high temperature PVT growth furnace.
The reaction kettle is heating reaction kettle, and graphene oxide dispersion, in reduction, the temperature of reaction kettle is 80
Degree Celsius.
Embodiment 2:
The present invention provides a kind of preparation methods of graphene composite material, comprising the following steps:
A. a certain amount of graphite is weighed, and graphite is put into grinder and is ground, smashed graphite particle passes through 250 mesh
It is screened, obtains graphite particle；
B. graphite particle above-mentioned steps obtained is added in a certain amount of ethanol solution, stirs evenly, mixes them thoroughly, and
Mixed solution is removed under the action of ultrasonic peel-off device, obtains graphene oxide dispersion；
C. graphene oxide dispersion above-mentioned steps obtained is added in dimethyl formamide solution, and above-mentioned mixed solution is existed
Be sufficiently stirred under the action of uniform device 1.5 hours, uniformly after aqueous solution hydrazine hydrate and ammonium hydroxide be added be again stirring for, and anti-
Reduction in kettle is answered to obtain graphene aqueous solution；
D. by the graphene aqueous solution of above-mentioned acquisition, distillation obtains graphene platelet in distillation ware, by the graphene platelet of acquisition
Pulverized particles are obtained under the grinding of spherical grinder；
E., the graphene of acquisition is passed through to such as a certain proportion of hydrogen and nitrogen in high temperature PVT growth furnace, in 1550 temperature
Lower reaction 2.5h then passes to argon gas and heats 2200 degrees Celsius, and then cooling obtains graphene composite material.
The volume ratio of the hydrogen and nitrogen is 1:20.
Evacuated state is always maintained inside the high temperature PVT growth furnace.
The reaction kettle is heating reaction kettle, and graphene oxide dispersion, in reduction, the temperature of reaction kettle is 90
Degree Celsius.
Embodiment 3:
The present invention provides a kind of preparation methods of graphene composite material, comprising the following steps:
A. a certain amount of graphite is weighed, and graphite is put into grinder and is ground, smashed graphite particle passes through 300 mesh
It is screened, obtains graphite particle；
B. graphite particle above-mentioned steps obtained is added in a certain amount of ethanol solution, stirs evenly, mixes them thoroughly, and
Mixed solution is removed under the action of ultrasonic peel-off device, obtains graphene oxide dispersion；
C. graphene oxide dispersion above-mentioned steps obtained is added in dimethyl formamide solution, and above-mentioned mixed solution is existed
Be sufficiently stirred under the action of uniform device 2 hours, uniformly after aqueous solution hydrazine hydrate and ammonium hydroxide be added be again stirring for, and reacting
Reduction obtains graphene aqueous solution in kettle；
D. by the graphene aqueous solution of above-mentioned acquisition, distillation obtains graphene platelet in distillation ware, by the graphene platelet of acquisition
Pulverized particles are obtained under the grinding of spherical grinder；
E., the graphene of acquisition is passed through to such as a certain proportion of hydrogen and nitrogen in high temperature PVT growth furnace, in 1600 temperature
Lower reaction 3h then passes to argon gas and heats 2300 degrees Celsius, and then cooling obtains graphene composite material.
The volume ratio of the hydrogen and nitrogen is 1:20.
Evacuated state is always maintained inside the high temperature PVT growth furnace.
The reaction kettle is heating reaction kettle, and graphene oxide dispersion, in reduction, the temperature of reaction kettle is 100
Degree Celsius.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art
Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein
Can technical characteristic replaced mutually and the technical solution that is formed.
Claims (4)
1. a kind of preparation method of graphene composite material, which comprises the following steps:
A. a certain amount of graphite is weighed, and graphite is put into grinder and is ground, smashed graphite particle passes through 200-
300 meshes are screened, and graphite particle is obtained；
B. graphite particle above-mentioned steps obtained is added in a certain amount of ethanol solution, stirs evenly, mixes them thoroughly, and
Mixed solution is removed under the action of ultrasonic peel-off device, obtains graphene oxide dispersion；
C. graphene oxide dispersion above-mentioned steps obtained is added in dimethyl formamide solution, and above-mentioned mixed solution is existed
Be sufficiently stirred under the action of uniform device 1-2 hours, uniformly after aqueous solution hydrazine hydrate and ammonium hydroxide be added be again stirring for, and anti-
Reduction in kettle is answered to obtain graphene aqueous solution；
D. by the graphene aqueous solution of above-mentioned acquisition, distillation obtains graphene platelet in distillation ware, by the graphene platelet of acquisition
Pulverized particles are obtained under the grinding of spherical grinder；
E., the graphene of acquisition is passed through to such as a certain proportion of hydrogen and nitrogen in high temperature PVT growth furnace, 1500-1600's
At a temperature of react 2-3h, then pass to argon gas and heat 2000-2300 degrees Celsius, then cooling obtain graphene composite material.
2. a kind of preparation method of graphene composite material according to claim 1, which is characterized in that the hydrogen and
The volume ratio of nitrogen is 1:20.
3. a kind of preparation method of graphene composite material according to claim 1, which is characterized in that the high temperature PVT
Evacuated state is always maintained inside growth furnace.
4. a kind of preparation method of graphene composite material according to claim 1, which is characterized in that the reaction kettle
To heat reaction kettle, and graphene oxide dispersion, in reduction, the temperature of reaction kettle is 80-100 degrees Celsius.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110964354A (en) * | 2019-12-20 | 2020-04-07 | 欧伊翔 | Preparation method of composite coating based on graphene |
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| US20140183415A1 (en) * | 2012-12-31 | 2014-07-03 | Cheil Industries Inc. | Graphene-Based Composite and Method of Preparing the Same |
| CN104347877A (en) * | 2013-07-31 | 2015-02-11 | 北京海特远舟新能源科技有限公司 | A nanometer level graphene-based composite material and a preparing method thereof |
| CN107324325A (en) * | 2017-07-20 | 2017-11-07 | 山西晋尤特环境科技有限公司 | A kind of preparation method of graphene composite material |
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| CN101830458A (en) * | 2010-05-06 | 2010-09-15 | 西安交通大学 | Preparation method of high purity and high concentration graphene suspension |
| CN102659096A (en) * | 2012-04-27 | 2012-09-12 | 湖南大学 | Preparation methods of graphene dispersion solution and thin film of graphene |
| US20140183415A1 (en) * | 2012-12-31 | 2014-07-03 | Cheil Industries Inc. | Graphene-Based Composite and Method of Preparing the Same |
| CN104347877A (en) * | 2013-07-31 | 2015-02-11 | 北京海特远舟新能源科技有限公司 | A nanometer level graphene-based composite material and a preparing method thereof |
| CN103570010A (en) * | 2013-10-17 | 2014-02-12 | 河南科技大学 | Preparation method of graphene powder material |
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| CN110964354A (en) * | 2019-12-20 | 2020-04-07 | 欧伊翔 | Preparation method of composite coating based on graphene |
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Application publication date: 20190903 |