CN112390248A - Preparation and testing method of modified graphene conductive material - Google Patents
Preparation and testing method of modified graphene conductive material Download PDFInfo
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- CN112390248A CN112390248A CN202011310965.2A CN202011310965A CN112390248A CN 112390248 A CN112390248 A CN 112390248A CN 202011310965 A CN202011310965 A CN 202011310965A CN 112390248 A CN112390248 A CN 112390248A
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Abstract
The invention discloses a preparation and test method of a modified graphene conductive material, which comprises the following steps: taking a graphite block as an original material; melting graphite blocks into an organic solution to obtain a first mixed solution; placing the first mixed solution in a heating table for heating treatment; vibrating the first solution heated to a certain temperature by using an ultrasonic oscillator to peel off graphite blocks from inside to outside to obtain a multilayer graphene solution; separating and purifying the multilayer graphene solution to obtain a single-layer graphene solution; and finally, adding the single-layer graphene solution into a modifier, and mixing and stirring uniformly to obtain the modified graphene. The modified graphene prepared by adopting the liquid-phase stripping mode replaces the graphene prepared by the traditional oxidation-reduction mode, so that the consumption of carbon atoms in the graphene is avoided, and the structural integrity of the graphene is ensured, thereby improving the quality of the graphene and further improving the conductivity of the graphene.
Description
Technical Field
The invention relates to the technical field of graphene production and preparation, in particular to a preparation and test method of a modified graphene conductive material.
Background
Graphene is a material having a single-layer two-dimensional honeycomb lattice structure composed of carbon atoms, and has many excellent properties, such as high young's modulus and carrier mobility, a large specific surface area, excellent thermal conductivity and light transmittance, and the like. The graphene material has shown wide application prospects in the fields of catalyst carriers, flexible photoelectric devices, biological materials, sensing materials and the like. At present, the preparation method of graphene mainly comprises a micro-mechanical separation method, an epitaxial growth method, chemical vapor deposition, a graphite oxide reduction method and the like. Among them, the graphite oxide reduction method is one of the most widely used methods for preparing graphene so far.
Graphene has good conductivity, and the existing graphene preparation method is a graphite oxide reduction method, and is highly regarded by relevant technologists as a chemical method which is low in cost and capable of realizing mass production of graphene. However, when graphene is produced by an oxidation-reduction method, part of carbon atoms are also consumed, so that the defect of reduced graphene is high, the quality of the graphene is reduced, and the conductivity of the graphene is affected.
Disclosure of Invention
The invention aims to provide a preparation and test method of a modified graphene conductive material, and aims to solve the problem that when graphene is produced by an oxidation-reduction method provided in the background art, part of carbon atoms are consumed, so that the defect of reduced graphene is high, the quality of the graphene is reduced, and the conductivity of the graphene is affected.
In order to achieve the purpose, the invention provides the following technical scheme:
the preparation method of the modified graphene conductive material comprises the following steps:
s1: taking a graphite block as an original material;
s2: melting graphite blocks into an organic solution to obtain a first mixed solution;
s3: placing the first mixed solution in a heating table for heating treatment;
s4: vibrating the first solution heated to a certain temperature by using an ultrasonic oscillator to peel off graphite blocks from inside to outside to obtain a multilayer graphene solution;
s5: separating and purifying the multilayer graphene solution to obtain a single-layer graphene solution;
s6: and finally, adding the single-layer graphene solution into a modifier, and mixing and stirring uniformly to obtain the modified graphene.
Preferably, the organic solution is one of an NMP solution, a DMSO solution, and a DMF solution.
Preferably, the concentration of the NMP solution, the DMSO solution and the DMF solution is 1-5 mg/ml.
Preferably, the heating stage is electromagnetically controlled to heat and maintain the first mixed solution to 40-80 ℃.
Preferably, the ultrasonic oscillator is used for oscillating and stripping the heated first solution for 4-8 hours, so that van der waals force is eliminated between the surface layer graphite and the bottom layer graphite under the action of ultrasonic waves, and graphene is stripped.
Preferably, the multilayer graphene separation method includes centrifuging, and separating the multilayer graphene in a separator to obtain single-layer graphene.
Preferably, the modifier is an external additive and is added according to the required properties of the product, so as to obtain the modified graphene.
Preferably, the modifier is a silane coupling agent, and the silane coupling agent and the single-layer graphene are uniformly mixed and stirred.
A testing method of a modified graphene conductive material comprises the following steps:
filtering and purifying the multilayer graphene solution prepared by the preparation method of the graphene modified coating material according to any one of claims 1 to 8 to obtain multilayer graphene solid; filling and compacting the multilayer graphene fixed body into a special conductive testing container;
the resulting monolayer of graphene immobilizate was packed and compacted into a dedicated further conductive test vessel.
Preferably, the finished multilayer graphene conductive testing container and the finished single-layer graphene conductive testing container are respectively placed into a conductive performance tester for conducting testing, and data are recorded for comparison.
Compared with the prior art, the invention provides a preparation method of a modified graphene conductive material, which has the following beneficial effects:
the modified graphene prepared by adopting the liquid-phase stripping mode replaces the graphene prepared by the traditional oxidation-reduction mode, avoids the consumption of carbon atoms contained in the graphene, and ensures the structural integrity of the graphene, so that the quality of the graphene is improved, the conductivity of the graphene is further improved, the graphene is suitable for the higher scientific and technical fields, and the use limitation of the graphene is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention without limiting the invention in which:
fig. 1 is a schematic outflow diagram of a method for preparing a modified graphene conductive material according to the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, the present invention provides a technical solution:
the preparation method of the modified graphene conductive material comprises the following steps:
taking a graphite block as an original material, cleaning the surface of the graphite block, and removing impurities on the surface;
melting graphite blocks into an organic solution to obtain a first mixed solution;
placing the first mixed solution in a heating table for heating treatment;
vibrating the first solution heated to a certain temperature by using an ultrasonic oscillator to peel off graphite blocks from inside to outside to obtain a multilayer graphene solution;
separating and purifying the multilayer graphene solution to obtain a single-layer graphene solution;
and finally, adding the single-layer graphene solution into a modifier, and mixing and stirring uniformly to obtain the modified graphene.
The organic solution is NMP solution, and the NMP solution is N-methyl pyrrolidone solution.
NMP solution was 3mg/ml, 15mg of NMP (N-methylpyrrolidone) was dissolved in 500ml of purified water to obtain 3mg/ml NPM (N-methylpyrrolidone) solution, and then the graphite cake was poured into 3mg/ml NPM (N-methylpyrrolidone) solution to obtain a first mixed solution.
The heating table is electromagnetically controlled to heat, the first mixed solution is heated and kept to 40-80 ℃, the first mixed solution is placed on the heating table, the temperature of the heating table is set and kept at 60 ℃ to heat the first solution, the activity degree of the solution is improved, and the reaction between the NPM (N-methyl pyrrolidone) solution and the graphite block is accelerated.
And the ultrasonic oscillator is used for carrying out oscillation stripping on the heated first solution, the oscillation time is 4-8 hours, van der waals force is eliminated between the surface layer graphite and the bottom layer graphite under the action of ultrasonic waves, van der waals force between graphite molecules is destroyed through the driving force of the ultrasonic waves, and the van der waals force is acting force between the molecules, so that the graphene is stripped.
The multilayer graphene separation method comprises the steps of performing centrifugal separation, wherein the multilayer graphene is prevented from being separated in a separator, the rotating speed of the separator is 10000-.
A testing method of a modified graphene conductive material comprises the following steps:
filtering and purifying the multilayer graphene solution prepared by the preparation method of the graphene modified coating material according to any one of claims 1 to 8 to obtain multilayer graphene solid; filling and compacting the multilayer graphene fixed body into a special conductive testing container;
the resulting monolayer of graphene immobilizate was packed and compacted into a dedicated further conductive test vessel.
Preferably, the finished multilayer graphene conductive testing container and the finished single-layer graphene conductive testing container are respectively placed into a conductive performance tester for conducting testing, and data are recorded for comparison.
The modifier is an external additive, is added according to the required properties of the product, and then is uniformly distributed with the single-layer graphene in the sealed stirring device, so that the modified graphene is obtained.
The modifier is a silane coupling agent, the silane coupling agent and the single-layer graphene are uniformly mixed and stirred, the silane coupling modification is that chemical coupling reaction occurs on the particle surface, the particle surface can generate good compatibility with organic matters after being treated by the coupling agent, and the dispersibility of the graphene can be improved.
Example 2
Referring to fig. 1, the present invention provides a technical solution:
the preparation method of the modified graphene conductive material comprises the following steps:
taking a graphite block as an original material, cleaning the surface of the graphite block, and removing impurities on the surface;
melting graphite blocks into an organic solution to obtain a first mixed solution;
placing the first mixed solution in a heating table for heating treatment;
vibrating the first solution heated to a certain temperature by using an ultrasonic oscillator to peel off graphite blocks from inside to outside to obtain a multilayer graphene solution;
separating and purifying the multilayer graphene solution to obtain a single-layer graphene solution;
and finally, adding the single-layer graphene solution into a modifier, and mixing and stirring uniformly to obtain the modified graphene.
The organic solution is DMSO solution, and the DMSO solution is DMSO solution.
The concentration of the DMSO solution was 4mg/ml, 20mg of DMSO (dimethyl sulfoxide solution) was dissolved in 500ml of purified water to obtain a DMSO (dimethyl sulfoxide solution) solution with a concentration of 4mg/ml, and then the graphite cake was poured into the DMSO (dimethyl sulfoxide solution) solution with a concentration of 4mg/ml to obtain a first mixed solution.
The heating table is electromagnetically controlled to heat, the first mixed solution is heated and kept to 40-80 ℃, the first mixed solution is placed on the heating table, the temperature of the heating table is set and kept at 60 ℃ to heat the first solution, the activity degree of the solution is improved, and the DMSO (dimethyl sulfoxide solution) solution is enabled to accelerate the reaction with the graphite block.
And the ultrasonic oscillator is used for carrying out oscillation stripping on the heated first solution, the oscillation time is 4-8 hours, van der waals force is eliminated between the surface layer graphite and the bottom layer graphite under the action of ultrasonic waves, van der waals force between graphite molecules is destroyed through the driving force of the ultrasonic waves, and the van der waals force is acting force between the molecules, so that the graphene is stripped.
The multilayer graphene separation method comprises the steps of performing centrifugal separation, wherein the multilayer graphene is prevented from being separated in a separator, the rotating speed of the separator is 10000-.
The modifier is an external additive, is added according to the required properties of the product, and then is uniformly distributed with the single-layer graphene in the sealed stirring device, so that the modified graphene is obtained.
The modifier is a silane coupling agent, the silane coupling agent and the single-layer graphene are uniformly mixed and stirred, the silane coupling modification is that chemical coupling reaction occurs on the particle surface, the particle surface can generate good compatibility with organic matters after being treated by the coupling agent, and the dispersibility of the graphene can be improved.
A testing method of a modified graphene conductive material comprises the following steps:
filtering and purifying the multilayer graphene solution prepared by the preparation method of the graphene modified coating material according to any one of claims 1 to 8 to obtain multilayer graphene solid; filling and compacting the multilayer graphene fixed body into a special conductive testing container;
the resulting monolayer of graphene immobilizate was packed and compacted into a dedicated further conductive test vessel.
Preferably, the finished multilayer graphene conductive testing container and the finished single-layer graphene conductive testing container are respectively placed into a conductive performance tester for conducting testing, and data are recorded for comparison.
Example 3
Referring to fig. 1, the present invention provides a technical solution:
the preparation method of the modified graphene conductive material comprises the following steps:
taking a graphite block as an original material, cleaning the surface of the graphite block, and removing impurities on the surface;
melting graphite blocks into an organic solution to obtain a first mixed solution;
placing the first mixed solution in a heating table for heating treatment;
vibrating the first solution heated to a certain temperature by using an ultrasonic oscillator to peel off graphite blocks from inside to outside to obtain a multilayer graphene solution;
separating and purifying the multilayer graphene solution to obtain a single-layer graphene solution;
and finally, adding the single-layer graphene solution into a modifier, and mixing and stirring uniformly to obtain the modified graphene.
The organic solution is DMF solution, and the DMF solution is N, N-dimethylformamide.
The concentration of the DMF solution was 5mg/ml each, 25mg of DMF (N, N-dimethylformamide) was dissolved in 500ml of purified water to give a 5mg/ml DMF (N, N-dimethylformamide) solution, and then the graphite cake was poured into the 5mg/ml DMF (N, N-dimethylformamide) solution to give a first mixed solution.
The heating table is electromagnetically controlled to heat, the first mixed solution is heated and kept to 40-80 ℃, the first mixed solution is placed on the heating table, the temperature of the heating table is set and kept at 60 ℃ to heat the first solution, the activity degree of the solution is improved, and the reaction of the DMF (N, N-dimethylformamide) solution and the graphite block is accelerated.
And the ultrasonic oscillator is used for carrying out oscillation stripping on the heated first solution, the oscillation time is 4-8 hours, van der waals force is eliminated between the surface layer graphite and the bottom layer graphite under the action of ultrasonic waves, van der waals force between graphite molecules is destroyed through the driving force of the ultrasonic waves, and the van der waals force is acting force between the molecules, so that the graphene is stripped.
The multilayer graphene separation method comprises the steps of performing centrifugal separation, wherein the multilayer graphene is prevented from being separated in a separator, the rotating speed of the separator is 10000-.
The modifier is an external additive, is added according to the required properties of the product, and then is uniformly distributed with the single-layer graphene in the sealed stirring device, so that the modified graphene is obtained.
The modifier is a silane coupling agent, the silane coupling agent and the single-layer graphene are uniformly mixed and stirred, the silane coupling modification is that chemical coupling reaction occurs on the particle surface, the particle surface can generate good compatibility with organic matters after being treated by the coupling agent, and the dispersibility of the graphene can be improved.
A testing method of a modified graphene conductive material comprises the following steps:
filtering and purifying the multilayer graphene solution prepared by the preparation method of the graphene modified coating material according to any one of claims 1 to 8 to obtain multilayer graphene solid; filling and compacting the multilayer graphene fixed body into a special conductive testing container;
the resulting monolayer of graphene immobilizate was packed and compacted into a dedicated further conductive test vessel.
Preferably, the finished multilayer graphene conductive testing container and the finished single-layer graphene conductive testing container are respectively placed into a conductive performance tester for conducting testing, and data are recorded for comparison.
In summary, the invention has the advantages that:
the modified graphene prepared by adopting the liquid-phase stripping mode replaces the graphene prepared by the traditional oxidation-reduction mode, avoids the consumption of carbon atoms contained in the graphene, and ensures the structural integrity of the graphene, so that the quality of the graphene is improved, the conductivity of the graphene is further improved, the graphene is suitable for the higher scientific and technical fields, and the use limitation of the graphene is improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The preparation method of the modified graphene conductive material is characterized by comprising the following steps: the method comprises the following steps:
s1: taking a graphite block as an original material;
s2: melting graphite blocks into an organic solution to obtain a first mixed solution;
s3: placing the first mixed solution in a heating table for heating treatment;
s4: vibrating the first solution heated to a certain temperature by using an ultrasonic oscillator to peel off graphite blocks from inside to outside to obtain a multilayer graphene solution;
s5: separating and purifying the multilayer graphene solution to obtain a single-layer graphene solution;
s6: and finally, adding the single-layer graphene solution into a modifier, and mixing and stirring uniformly to obtain the modified graphene.
2. The preparation method of the modified graphene conductive material according to claim 1, wherein the preparation method comprises the following steps: the organic solution is one of NMP solution, DMSO solution and DMF solution.
3. The preparation method of the modified graphene conductive material according to claim 2, wherein the preparation method comprises the following steps: the concentration of the NMP solution, the DMSO solution and the DMF solution is 1-5 mg/ml.
4. The preparation method of the modified graphene conductive material according to claim 1, wherein the preparation method comprises the following steps: the heating stage is electromagnetically controlled to heat, and the first mixed solution is heated and maintained at 40-80 ℃.
5. The preparation method of the modified graphene conductive material according to claim 1, wherein the modified graphene conductive material comprises the following steps: the ultrasonic oscillator is used for oscillating and stripping the heated first solution for 4-8 hours, so that van der Waals force is eliminated between the surface layer graphite and the bottom layer graphite under the action of ultrasonic waves, and graphene is stripped.
6. The preparation method of the modified graphene conductive material according to claim 1, wherein the modified graphene conductive material comprises the following steps: the multilayer graphene separation method comprises the steps of performing centrifugal separation, and preventing multilayer graphene from being separated in a separator to obtain single-layer graphene.
7. The preparation method of the modified graphene conductive material according to claim 1, wherein the preparation method comprises the following steps: the modifier is an external additive and is added according to the required properties of the product, so that the modified graphene is obtained.
8. The preparation method of the modified graphene conductive material according to claim 1, wherein the modified graphene conductive material comprises the following steps: the modifier is a silane coupling agent, and the silane coupling agent and the single-layer graphene are uniformly mixed and stirred.
9. A testing method of a modified graphene conductive material is characterized by comprising the following steps: the method comprises the following steps:
filtering and purifying the multilayer graphene solution prepared by the preparation method of the graphene modified coating material according to any one of claims 1 to 8 to obtain multilayer graphene solid; filling and compacting the multilayer graphene fixed body into a special conductive testing container;
the resulting monolayer of graphene immobilizate was packed and compacted into a dedicated further conductive test vessel.
10. The method for testing the modified graphene conductive material according to claim 9, wherein the method comprises the following steps: and respectively putting the multilayer graphene conductive testing container and the single-layer graphene conductive testing container which are filled into the conductive testing instrument for conducting a conductive test, and recording data for comparison.
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Cited By (1)
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| CN117550593A (en) * | 2024-01-11 | 2024-02-13 | 上海巴库斯超导新材料有限公司 | Novel preparation process of natural graphite anode material |
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Application publication date: 20210223 |