CN109637697A - A kind of graphene conductive slurry and preparation method thereof - Google Patents
A kind of graphene conductive slurry and preparation method thereof Download PDFInfo
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- CN109637697A CN109637697A CN201811584545.6A CN201811584545A CN109637697A CN 109637697 A CN109637697 A CN 109637697A CN 201811584545 A CN201811584545 A CN 201811584545A CN 109637697 A CN109637697 A CN 109637697A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The invention discloses a kind of graphene conductive slurries and preparation method thereof, are related to technical field of lithium ion.This method includes that dispersing agent and solvent are carried out mixed processing to obtain mixed liquor, so that the dispersing agent and the solvent are uniformly mixed；Graphene, carbon nanotube and binder are added into the mixed liquor and obtains the first premix；First premix is stirred and obtains the second premix with ultrasonic disperse；Second premix is ground, electrocondution slurry is obtained；Electrocondution slurry progress ultrasonic disperse is obtained into the graphene conductive slurry.This method simple possible will not destroy the structure of graphene and carbon nanotube, and graphene slurry obtained has less agglomeration and excellent electric conductivity, and property stable uniform is suitble to large-scale industrial production.It is properly added the slurry into lithium ion battery, the electric conductivity of battery can be improved, makes battery that there is the excellent chemical properties such as high-energy density and long circulation life.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of graphene conductive slurry and its preparation side
Method.
Background technique
Lithium ion battery is because it has higher energy density, power density, memory-less effect and has extended cycle life, puts certainly
Many advantages, such as electrical effect is small is widely used in the fields such as portable electronic device, aerospace and electric car.In recent years
Carry out the demand sustainable growth with electric car and hybrid vehicle, the also further expansion of the demand to lithium ion battery, together
When, to its energy density, high rate performance and service life, higher requirements are also raised.
The negative electrode material of commercial Li-ion battery is mainly based on graphite at present, but the theoretical maximum storage lithium of graphite holds
Amount only has 372mAh/g, is unable to satisfy the requirement of high energy lithium ion cell.The theoretical capacity of silica-base material is significantly larger than graphite,
It is considered as one of most promising lithium ion battery negative material.However, the low conductivity and other factors of silica-base material
Limitation, it is widely applied can not also at present.Conductive agent appropriate is added in lithium battery positive and negative anodes, can be enhanced in positive and negative anodes
Active material contacts extensively with electrolyte, facilitates the insertion and abjection of lithium ion, accelerates the transmission rate of electronics, reduces resistance
It is anti-, improve coulombic efficiency for the first time, high rate performance and the cycle life of battery.Electrically conductive graphite is in industrialized production using most at present
Extensive conductive agent, have many advantages, such as it is low in cost, but due to " point-point " contact mode of graphite and active material, need compared with
Big graphite usage amount can just effectively improve electrode conductivuty.
Graphene is monoatomic crystalline solid, has ultra-thin, superpower flexibility, very big specific surface area and superpower electric conductivity
Etc. characteristics.Appropriate graphene is added in lithium ion battery silica-base material, high flexibility can alleviate silicon-based active substance and fill
Volume expansion bring electrode material falls off in discharge process, while the conduction of material can be improved in the high conductivity of graphene
Property, to improve the energy density and cycle life of lithium battery.But since single-layer graphene is easy to reunite, under causing performance violent
Drop, to limit its practical application.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of graphene conductive slurry, which can
Row, not only without the structure of destruction graphene and carbon nanotube, and graphene slurry obtained has less agglomeration
With excellent electric conductivity, property stable uniform is suitble to large-scale industrial production.
Another object of the present invention is to provide a kind of graphene conductive slurries, are prepared by the above method.It should
Graphene conductive slurry dispersibility is more preferable, more efficient.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of preparation method of graphene conductive slurry comprising:
Dispersing agent and solvent are subjected to mixed processing and obtain mixed liquor, so that dispersing agent and solvent are uniformly mixed；
Graphene, carbon nanotube and binder are added into mixed liquor and obtains the first premix；
First premix is stirred and obtains the second premix with ultrasonic disperse；
Second premix is ground, electrocondution slurry is obtained；
Electrocondution slurry progress ultrasonic disperse is obtained into graphene conductive slurry.
The present invention proposes that a kind of graphene conductive slurry is prepared by the preparation method of above-mentioned graphene conductive slurry
It arrives.
The beneficial effect of the graphene conductive slurry of the embodiment of the present invention and preparation method thereof is:
The preparation method for the graphene conductive slurry that the embodiment of the present invention provides, using carbon nanotube by intersecting
Superposition is built into staggeredly connected network to transmit electronics, and then improves the electric conductivity of slurry, is compounded with graphene,
And then contact with each other, so that the conductive capability of whole slurry is further promoted.Dispersing agent is used for filled graphite alkene and carbon nanotube
Between gap, and keep entire dispersed structure more stable and dispersion degree be substantially improved.Graphene slurry provided by the invention
Preparation method, simple process is feasible, not only without destroy graphene and carbon nanotube structure, and graphene obtained starch
Material has less agglomeration and excellent electric conductivity, and property stable uniform is suitble to large-scale industrial production.
The graphene conductive slurry that the embodiment of the present invention provides, is prepared by the above method.The graphene is led
Plasma-based material dispersibility is more preferable, more efficient.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Graphene conductive slurry of the embodiment of the present invention and preparation method thereof is specifically described below.
A kind of preparation method of graphene conductive slurry comprising:
Dispersing agent and solvent are subjected to mixed processing and obtain mixed liquor, so that dispersing agent and solvent are uniformly mixed；
Graphene, carbon nanotube and binder are added into mixed liquor and obtains the first premix；
First premix is stirred and obtains the second premix with ultrasonic disperse；
Second premix is ground, electrocondution slurry is obtained；
Electrocondution slurry progress ultrasonic disperse is obtained into graphene conductive slurry.
In detail, firstly, dispersing agent and solvent are carried out mixing treatment, the preparation time of slurry on the one hand can be saved, separately
On the one hand, graphene and carbon nanotube in following preparation process can be made to can be uniformly dispersed in by dispersing agent and solvent shape
At mixed solution in.Secondly, this method using carbon nanotube by intersecting superposition, be built into the network that is staggeredly connected with
Electronics is transmitted, and then improves the electric conductivity of slurry, is compounded with graphene, and then contact with each other, so that whole slurry
Conductive capability is further promoted.Dispersing agent makes entire dispersed structure for the gap between filled graphite alkene and carbon nanotube
It is more stable and dispersion degree is substantially improved.The preparation method of graphene slurry provided by the invention, simple process is feasible, not only
The structure of graphene and carbon nanotube is not destroyed, and graphene slurry obtained has less agglomeration and excellent
Electric conductivity, property stable uniform are suitble to large-scale industrial production.
Further, in the preferred embodiment, it is mixed by dispersing agent and solvent progress mixed processing
In the step of liquid:
Further include mixed liquor is stirred, and mixing speed be 500r/min~800r/min, mixing time be 10s~
60s.Certainly, in other embodiments of the invention, mixing speed and mixing time can be adjusted according to demand, this hair
Bright embodiment is without limitation.
Further, in the preferred embodiment, dispersing agent is polyvinylpyrrolidone, and solvent is N- methyl pyrrole
Pyrrolidone.
Further, in the preferred embodiment, the adding proportion range of solvent and dispersing agent is (4~1): (1
~6).Certainly, in the other embodiments of invention, the dosage of graphene and dispersing agent can also be selected according to demand, this
The embodiment of invention is without limitation.
Further, in the preferred embodiment, the quality of graphene, carbon nanotube and binder compares range
For (1~10): (10~1): (1~3), and binder is butadiene-styrene rubber.
Further, in the preferred embodiment, it is obtained with ultrasonic disperse being stirred the first premix
In the step of second premix:
Stirring is to be carried out by magnetic stirring apparatus, and the mixing speed of magnetic stirring apparatus is 1000r/min~2000r/
Min, mixing time are 10h~20h, and the ultrasonic disperse time is 10min~40min.Certainly, in the other embodiment of the present invention
In, the mixing speed and mixing time of magnetic stirring apparatus, the time of ultrasonic disperse can also be adjusted according to demand, not
It is only limitted to this, the embodiment of the present invention is without limitation.
Further, in the preferred embodiment, the mode of milled processed is to be sanded, and the sand milling time is 10min
~50min.
Further, in the preferred embodiment, sand milling is carried out by sand mill, and sand mill is turbine type
Sand mill, and in sand grinding process, the revolving speed for controlling sand mill is 500~2500r/min.
Further, in the preferred embodiment, the sanding media in sand mill is zirconia beads, zirconium silicate
Pearl, titanium dioxide aluminium pill are any one or more of, and the partial size of sanding media is 0.5mm~3.0mm.
Further, in the preferred embodiment, it obtains graphene by electrocondution slurry progress ultrasonic disperse and leads
In the step of plasma-based material:
The time of ultrasonic disperse is 10min~50min.
A kind of graphene conductive slurry is prepared by the preparation method of above-mentioned graphene conductive slurry.The graphene
Electrocondution slurry dispersibility is more preferable, more efficient.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of graphene conductive slurry is present embodiments provided, is prepared by the following method to obtain:
S1: dispersing agent (polyvinylpyrrolidone) and solvent (N-Methyl pyrrolidone) are subjected to mixed processing and mixed
Liquid is uniformly mixed dispersing agent and solvent, wherein the mass ratio of dispersing agent and solvent is 1:2；
S2: graphene, carbon nanotube and binder (butadiene-styrene rubber) being added into mixed liquor, obtains the first premix,
In, graphene, carbon nanotube, binder mass ratio be 4:2:1；
S3: the first premix is stirred and ultrasonic disperse, the second premix is obtained, wherein mixing speed is
1000r/min, mixing time 10h, jitter time 20min；
S4: the second premix is ground, electrocondution slurry is obtained, wherein sand mill is turbine type sand mill, sand
The revolving speed of grinding machine is 500r/min, and the sanding media in sand mill is zirconia beads, and the partial size of abrasive media is 1mm；
S5: by electrocondution slurry ultrasonic disperse, graphene conductive slurry is obtained, wherein the ultrasonic disperse time is 20min.
Embodiment 2
A kind of graphene conductive slurry is present embodiments provided, is prepared by the following method to obtain:
S1: dispersing agent (polyvinylpyrrolidone) and solvent (N-Methyl pyrrolidone) are subjected to mixed processing and mixed
Liquid is uniformly mixed dispersing agent and solvent, wherein the mass ratio of dispersing agent and solvent is 1:4；
S2: graphene, carbon nanotube and binder (butadiene-styrene rubber) being added into mixed liquor, obtains the first premix,
In, graphene, carbon nanotube, binder mass ratio be 4:3:1；
S3: the first premix is stirred and ultrasonic disperse, the second premix is obtained, wherein mixing speed is
1500r/min, mixing time 25h, jitter time 30min；
S4: the second premix is ground, electrocondution slurry is obtained, wherein sand mill is turbine type sand mill, sand
The revolving speed of grinding machine is 1000r/min, and the sanding media in sand mill is zirconia beads, and the partial size of abrasive media is 1mm；
S5: by electrocondution slurry ultrasonic disperse, graphene conductive slurry is obtained, wherein the ultrasonic disperse time is 30min.
In conclusion the preparation method of the graphene conductive slurry of the embodiment of the present invention, which can
Row, not only without the structure of destruction graphene and carbon nanotube, but also graphene slurry obtained has less agglomeration
With excellent electric conductivity, property stable uniform is suitble to large-scale industrial production.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene conductive slurry, characterized in that it comprises:
Dispersing agent and solvent are subjected to mixed processing and obtain mixed liquor, so that the dispersing agent and the solvent are uniformly mixed；
Graphene, carbon nanotube and binder are added into the mixed liquor and obtains the first premix；
First premix is stirred and obtains the second premix with ultrasonic disperse；
Second premix is ground, electrocondution slurry is obtained；
Electrocondution slurry progress ultrasonic disperse is obtained into the graphene conductive slurry.
2. the preparation method of graphene conductive slurry according to claim 1, which is characterized in that by the dispersing agent and
The solvent carried out in the step of mixed processing obtains the mixed liquor:
Further include the mixed liquor is stirred, and mixing speed be 500r/min~800r/min, mixing time be 10s~
60s。
3. the preparation method of graphene conductive slurry according to claim 1, it is characterised in that:
The dispersing agent is polyvinylpyrrolidone, and the solvent is N-Methyl pyrrolidone.
4. the preparation method of graphene conductive slurry according to claim 1, it is characterised in that:
The adding proportion range of the solvent and the dispersing agent is (4~1): (1~6).
5. the preparation method of graphene conductive slurry according to any one of claim 1 to 4, it is characterised in that:
The quality of the graphene, the carbon nanotube and the binder is (1~10): (10~1) than range: (1~
3), and the binder is butadiene-styrene rubber.
6. the preparation method of graphene conductive slurry according to claim 5, which is characterized in that premixed by described first
Material was stirred in the step of obtaining second premix with ultrasonic disperse:
Stirring is to be carried out by magnetic stirring apparatus, and the mixing speed of magnetic stirring apparatus is 1000r/min~2000r/min,
Mixing time is 10h~20h, and the ultrasonic disperse time is 10min~40min.
7. the preparation method of graphene conductive slurry according to claim 1, it is characterised in that:
The mode of milled processed is to be sanded, and the sand milling time is 10min~50min；
And being sanded is carried out by sand mill, sand mill is turbine type sand mill, and in sand grinding process, controls sand mill
Revolving speed is 500~2500r/min.
8. the preparation method of graphene conductive slurry according to claim 7, it is characterised in that:
Sanding media in the sand mill is that zirconia beads, zirconium silicate pearl, aluminium dioxide are any one or more of, and institute
The partial size for stating sanding media is 0.5mm~3.0mm.
9. the preparation method of graphene conductive slurry according to claim 1, which is characterized in that by the electrocondution slurry
It carries out in the step of ultrasonic disperse obtains the graphene conductive slurry:
The time of ultrasonic disperse is 10min~50min.
10. a kind of graphene conductive slurry, it is characterised in that:
The preparation method that the graphene conductive slurry passes through graphene conductive slurry described in any one of claims 1 to 9
It is prepared.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110327908A (en) * | 2019-07-10 | 2019-10-15 | 大英聚能科技发展有限公司 | A kind of modified graphene catalysis slurry and preparation method thereof |
| CN112164489A (en) * | 2020-09-04 | 2021-01-01 | 苏州烯时代材料科技有限公司 | Conductive carbon paddle for blood glucose test paper, preparation method of conductive carbon paddle and blood glucose test paper |
| CN113745518A (en) * | 2021-08-25 | 2021-12-03 | 金川集团股份有限公司 | Preparation method of graphene composite conductive slurry |
| CN114792585A (en) * | 2022-01-20 | 2022-07-26 | 马国庆 | Preparation treatment process of graphene slurry with strong magnetic and electric properties |
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| CN112164489A (en) * | 2020-09-04 | 2021-01-01 | 苏州烯时代材料科技有限公司 | Conductive carbon paddle for blood glucose test paper, preparation method of conductive carbon paddle and blood glucose test paper |
| CN113745518A (en) * | 2021-08-25 | 2021-12-03 | 金川集团股份有限公司 | Preparation method of graphene composite conductive slurry |
| CN114792585A (en) * | 2022-01-20 | 2022-07-26 | 马国庆 | Preparation treatment process of graphene slurry with strong magnetic and electric properties |
| CN114792585B (en) * | 2022-01-20 | 2024-05-24 | 中山市华洋塑胶颜料有限公司 | Graphene slurry preparation treatment process |
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Application publication date: 20190416 |