CN113436779A - Composite conductive powder and preparation method thereof - Google Patents
Composite conductive powder and preparation method thereof Download PDFInfo
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- CN113436779A CN113436779A CN202110662018.8A CN202110662018A CN113436779A CN 113436779 A CN113436779 A CN 113436779A CN 202110662018 A CN202110662018 A CN 202110662018A CN 113436779 A CN113436779 A CN 113436779A
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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
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of 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
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention belongs to the technical field of material chemistry, and particularly relates to composite conductive powder and a preparation method thereof. The composite powder material has the advantages of good dispersibility and difficult agglomeration, and can be suitable for lithium ion battery oil and water system materials, and the initial capacity and the rate capability of the battery are improved.
Description
Technical Field
The invention belongs to the technical field of material chemistry, and particularly relates to composite conductive powder and a preparation method thereof.
Background
The lithium ion battery has the advantages of high working voltage, large specific capacity, stable discharge, small volume, light weight, no memory effect, safety, long service life, environmental friendliness and the like, and has wide application prospect in the fields of portable electronic equipment, electric automobiles, space technology, national defense industry and the like. The positive and negative electrode active materials of the lithium ion battery are generally transition metal oxides, such as: LiCoO2、LiNixCo(1-x)O2And spinel LiMn2O4Etc., and a transition metal phosphate LiMPO4. These transition metal oxides are generally semiconductors or insulators, and generally have low conductivity, so that the capacity is often difficult to fully exert when the lithium ion is discharged under a high current condition, and the power performance of the lithium ion is severely limited. The main solution at present is to add a large amount of carbon materials with higher electronic conductivity as a conductive agent in the battery preparation process, so as to improve the performance of the lithium ion battery under the high-power working condition by constructing a fast electronic conduction network in the electrode.
The lithium ion battery conductive agent used in the prior art mainly comprises: (1) conductive carbon black; (2) a carbon nanotube; (3) graphene, and the like.
Wherein, the conductive carbon black is added into the positive and negative active materials in the form of powder. The conductive carbon black added in the prior art has the advantages of directly adding powder, not needing to be made into slurry, simple process and convenient operation, and has the disadvantages that the conductive performance of the conductive carbon black is poorer than that of carbon nano tubes and graphene, and the addition amount is high and generally reaches 3-6 percent, and if the addition amount is low, the battery capacity is low.
The carbon nano tube and the graphene are prepared into uniformly dispersed conductive slurry and added into the positive and negative active materials. The carbon nanotube and graphene added in the prior art have the advantages of good conductivity, low addition amount in a battery active substance, capacity and rate capability improvement of the battery, and the disadvantage that the carbon nanotube and graphene need to be made into uniformly dispersed slurry to be added into the active substance.
Disclosure of Invention
The composite conductive powder is prepared into water-based slurry by a high-pressure homogenizing or sanding method in a water system under the action of a dispersing agent, then is prepared into powder by spray drying, and then is dispersed into uniform granularity by an airflow crushing method. The composite powder material has the advantages of good dispersibility and difficult agglomeration, can be suitable for lithium ion battery oil and water system materials, and improves the initial capacity and rate capability of the battery, and the content of the invention is as follows:
the first purpose of the invention is to provide a composite conductive powder, which is characterized in that: according to the weight parts, the composite conductive powder comprises 30-60 parts of graphene powder, 10-30 parts of carbon nano tubes, 10-30 parts of conductive carbon black and 10-20 parts of dispersing agent.
In some embodiments of the present invention, the graphene powder is prepared from crystalline flake graphite or expanded graphite.
In some embodiments of the present invention, the carbon nanotubes are multi-walled carbon nanotubes or single-walled carbon nanotubes.
In some embodiments of the present invention, the dispersant in the composite conductive powder formula system is any one of lecithin, polyvinyl alcohol, and polyvinylpyrrolidone.
The second purpose of the invention is to provide a preparation method of composite conductive powder, which has the technical points that: comprises the following steps
Step one, preparing water system composite slurry: placing raw material graphite powder and a dispersant into deionized water, uniformly mixing, and then placing the mixture into a high-pressure homogenizer for primary homogenization treatment to obtain water-based composite slurry with the granularity D90 being less than 10 mu m;
step two, preparing the composite conductive slurry: uniformly mixing the carbon nano tube and the conductive carbon black, and then placing the mixture into the water-based composite slurry with the granularity D90 being less than 10 mu m obtained in the step one for second homogenization treatment to obtain composite conductive slurry with the granularity D90 being less than 7 mu m;
step three, preparing the composite conductive powder: and (3) carrying out spray drying on the composite conductive slurry with the granularity D90 being less than 7 mu m obtained in the step (II), and then carrying out jet milling on the composite conductive slurry to obtain composite conductive powder with the granularity D90 being less than 5 mu m.
In some embodiments of the present invention, the pressure of the first homogenization treatment in the first step of the preparation method of the composite conductive powder is 700-900 bar.
In some embodiments of the invention, the pressure of the second homogenization treatment in the second step of the preparation method of the composite conductive powder is 300-500 bar.
In some embodiments of the invention, the viscosity of the composite conductive paste in the second step of the preparation method of the composite conductive powder is 300-2000 cp.
In some embodiments of the invention, in the third step of the preparation method of the composite conductive powder, the feeding temperature of spray drying is 200-.
Compared with the prior art, the composite conductive powder and the preparation method thereof have the beneficial effects that:
1. the composite conductive powder does not contain solvent NMP, so that the solvent NMP is volatilized by baking when the composite conductive powder is not used, the cost is reduced, the subsequent preparation procedures are reduced, the operation is simpler and more convenient, and the industrial large-scale production is facilitated.
2. The conductivity of the composite conductive powder is better than that of a single carbon nano tube, so the addition amount of the composite conductive powder is lower than that of the carbon nano tube.
3. The composite conductive powder can be added into a lithium ion battery anode material and a lithium ion battery cathode material.
Drawings
FIG. 1 is a curve of different additive amounts and pole piece resistivity in positive lithium iron phosphate in examples 1-5 and comparative examples 1-2;
FIG. 2 is a graph showing the resistivity curves of different additive amounts in the positive ternary material and the pole piece of examples 1 to 5 and comparative examples 1 to 2.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.
Example 1
The method comprises the following steps: weighing 12g of graphene powder, 4.8g of lecithin and 470g of deionized water, uniformly mixing the graphene powder and the lecithin in deionized water, pouring the mixture into a material cup of a high-pressure homogenizer, and carrying out primary homogenizing and dispersing treatment under the pressure of 800bar until the granularity D90 of the slurry is tested to be less than 10 mu m, wherein the graphene powder is prepared from crystalline flake graphite;
step two: weighing 8.4g of carbon nano tube and 4.8g of conductive carbon black, placing the carbon nano tube and the conductive carbon black into a homogeneous cup, uniformly mixing, and performing second homogeneous dispersion treatment under the pressure of 400bar until the granularity D90 of the slurry is less than 7 mu m to obtain the composite conductive slurry, wherein the viscosity of the slurry is about 300cp, and the carbon nano tube is a multi-wall carbon nano tube.
Step three: the slurry was spray-dried at a feed temperature of 210 ℃ and a discharge temperature of 130 ℃ to obtain about 30g of composite powder (40% by weight of graphene powder, 28% by weight of carbon nanotubes, 16% by weight of conductive carbon black, and 16% by weight of dispersant). And (3) carrying out jet milling on the composite powder until the particle size D90 is less than 5 mu m. To obtain the composite powder finally used for the battery.
Example 2
The method comprises the following steps: weighing 9g of graphene powder, 6g of polyvinyl alcohol and 470g of deionized water, placing the graphene powder and lecithin in deionized water, uniformly mixing, pouring into a high-pressure homogenizer cup, and carrying out primary homogenizing and dispersing treatment under the pressure of 800bar until the granularity D90 of the slurry is tested to be less than 7 mu m, wherein the graphene powder is prepared from crystalline flake graphite.
Step two: weighing 6g of carbon nano tube and 9g of conductive carbon black, placing the carbon nano tube and the conductive carbon black in a homogeneous cup, uniformly mixing, and performing second homogeneous dispersion treatment under the pressure of 400bar until the granularity D90 of the slurry is less than 5 mu m to obtain the composite conductive slurry, wherein the viscosity of the slurry is about 1000cp, and the carbon nano tube is a single-walled carbon nano tube.
Step three: the slurry was spray-dried at a feed temperature of 210 ℃ and a discharge temperature of 130 ℃ to obtain about 30g of composite powder (30% of graphene powder, 20% of carbon nanotubes, 30% of conductive carbon black, and 20% of dispersant). And (3) carrying out jet milling on the composite powder until the particle size D90 is less than 5 mu m. To obtain the composite powder finally used for the battery.
Example 3
The method comprises the following steps: weighing 15g of graphene powder, 4.8g of polyvinylpyrrolidone and 470g of deionized water, uniformly mixing the graphene powder and lecithin in deionized water, pouring the mixture into a cup of a high-pressure homogenizer, and carrying out primary homogenizing and dispersing treatment under the pressure of 800bar until the granularity D90 of the slurry is tested to be less than 10 mu m, wherein the graphene powder is prepared from expanded graphite.
Step two: weighing 4.8g of carbon nano tube and 5.4g of conductive carbon black, placing the carbon nano tube and the conductive carbon black into a homogeneous cup, uniformly mixing, and performing second homogeneous dispersion treatment under the pressure of 400bar until the granularity D90 of the slurry is less than 7 mu m to obtain the composite conductive slurry, wherein the viscosity of the slurry is about 2000cp, and the carbon nano tube is a single-walled carbon nano tube.
Step three: the slurry was spray-dried at a feed temperature of 210 ℃ and a discharge temperature of 130 ℃ to obtain about 30g of composite powder (50% of graphene powder, 16% of carbon nanotubes, 18% of conductive carbon black, and 16% of dispersant). And (3) carrying out jet milling on the composite powder until the particle size D90 is less than 5 mu m. To obtain the composite powder finally used for the battery.
Example 4
The method comprises the following steps: weighing 18g of graphene powder, 5g of polyvinylpyrrolidone, 1g of lecithin and 470g of deionized water, uniformly mixing the graphene powder, the polyvinylpyrrolidone and the lecithin in deionized water, pouring the mixture into a cup of a high-pressure homogenizer, and carrying out primary homogenizing dispersion treatment under the pressure of 800bar until the granularity D90 of the slurry is tested to be less than 10 microns, wherein the graphene powder is prepared from expanded graphite.
Step two: weighing 3g of carbon nano tube and 3g of conductive carbon black, placing the carbon nano tube and the conductive carbon black in a homogenizing cup, uniformly mixing, and then carrying out second homogenizing and dispersing treatment under the pressure of 400bar until the granularity D90 of the slurry is less than 7 mu m, thereby obtaining the composite conductive slurry, wherein the viscosity of the slurry is about 2000cp, and the carbon nano tube is a multi-wall carbon nano tube.
Step three: the slurry was spray-dried at a feed temperature of 210 ℃ and a discharge temperature of 130 ℃ to obtain about 30g of composite powder (graphene: 60%, carbon nanotube: 10%, conductive carbon black: 10%, and dispersant: 20%). And (3) carrying out jet milling on the composite powder until the particle size D90 is less than 5 mu m. To obtain the composite powder finally used for the battery.
Example 5
The method comprises the following steps: weighing 12g of graphene powder, 2g of polyvinyl alcohol, 1g of polyvinylpyrrolidone and 470g of deionized water, uniformly mixing the graphene powder, the polyvinylpyrrolidone and the polyvinyl alcohol in deionized water, pouring the mixture into a cup of a high-pressure homogenizer, and carrying out primary homogenizing dispersion treatment under the pressure of 800bar until the granularity D90 of the slurry is tested to be less than 10 microns, wherein the graphene powder is prepared from flake graphite.
Step two: weighing 9g of carbon nano tube and 6g of conductive carbon black, placing the carbon nano tube and the conductive carbon black in a homogenizing cup, uniformly mixing, and performing second homogenizing and dispersing treatment under the pressure of 400bar until the granularity D90 of the slurry is less than 7 mu m to obtain the composite conductive slurry, wherein the viscosity of the slurry is about 2000cp, and the carbon nano tube is a multi-wall carbon nano tube.
Step three: the slurry was spray-dried at a feed temperature of 210 ℃ and a discharge temperature of 130 ℃ to obtain about 30g of composite powder (40% of graphene powder, 30% of carbon nanotubes, 20% of conductive carbon black, and 10% of dispersant). And (3) carrying out jet milling on the composite powder until the particle size D90 is less than 5 mu m. To obtain the composite powder finally used for the battery.
Test examples
Pure carbon nanotube slurry (CNT slurry) with 5% carbon content is used as comparative example 1, ultra-dense high-super P conductive carbon black (SP) is used as comparative example 1, then examples 1-5 and comparative examples 1-2 are respectively added into a lithium iron phosphate and ternary cathode material system according to different addition ratios, the change of film resistivity is verified when different addition amounts are added, and the addition amount range of a conductive agent in the system and the conductivity of the comparative examples and comparative examples can be judged according to the trend of the change of resistivity of different addition amounts.
Fig. 1 shows the application effects of examples 1 to 5 and comparative examples 1 to 2 in lithium iron phosphate as a lithium ion cathode material, and it can be seen from the figure that the optimal process is example 1, the addition amount is 0.6% to 0.8%, and the addition amounts of examples 2 to 5 are as follows: 0.8% -1.2%, while the slurry of comparative example 1 was added at: 1.0% -1.4%, while comparative example 2 was added in the following amounts: 3 to 5 percent. The resistivity is lowest and the conductivity is best in the embodiment 1 under the condition of the same adding amount, and compared with the CNT paste and SP powder, the embodiment of the invention has the advantages of conductivity.
FIG. 2 shows the application effects of examples 1-5 and comparative examples 1-2 in the ternary lithium ion positive electrode material, and it can be seen from the figure that the optimal process is example 1, the addition amount is 0.4% -0.6%, and the addition amounts of examples 2-5 are as follows: 0.5% -0.8%, while the slurry of comparative example 1 was added in the following amounts: 0.6% -1.0%, while comparative example 2 was added in the following amounts: 1.0 to 1.4 percent. The resistivity is lowest and the conductivity is best in the embodiment 1 under the condition of the same adding amount, and compared with the CNT paste and SP powder, the embodiment of the invention has the advantages of conductivity.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (9)
1. A composite conductive powder characterized in that: according to the weight parts, the composite conductive powder comprises 30-60 parts of graphene powder, 10-30 parts of carbon nano tubes, 10-30 parts of conductive carbon black and 10-20 parts of dispersing agent.
2. The composite conductive powder according to claim 1, characterized in that: the graphene powder is prepared from crystalline flake graphite or expanded graphite.
3. The composite conductive powder according to claim 1, characterized in that: the carbon nano tube is a multi-wall carbon nano tube or a single-wall carbon nano tube.
4. The composite conductive powder according to claim 1, characterized in that: the dispersing agent is any one of lecithin, polyvinyl alcohol and polyvinylpyrrolidone.
5. A preparation method of composite conductive powder is characterized by comprising the following steps: comprises the following steps
Step one, preparing water system composite slurry: placing raw material graphite powder and a dispersant into deionized water, uniformly mixing, and then placing the mixture into a high-pressure homogenizer for primary homogenization treatment to obtain water-based composite slurry with the granularity D90 being less than 10 mu m;
step two, preparing the composite conductive slurry: uniformly mixing the carbon nano tube and the conductive carbon black, and then placing the mixture into the water-based composite slurry with the granularity D90 being less than 10 mu m obtained in the step one for second homogenization treatment to obtain composite conductive slurry with the granularity D90 being less than 7 mu m;
step three, preparing the composite conductive powder: and (3) carrying out spray drying on the composite conductive slurry with the granularity D90 being less than 7 mu m obtained in the step (II), and then carrying out jet milling on the composite conductive slurry to obtain composite conductive powder with the granularity D90 being less than 5 mu m.
6. The method for preparing a composite conductive powder according to claim 5, wherein: the pressure of the first homogenization treatment in the first step is 700-900 bar.
7. The method for preparing a composite conductive powder according to claim 5, wherein: the pressure of the second homogenization treatment in the second step is 300-500 bar.
8. The method for preparing a composite conductive powder according to claim 5, wherein: the viscosity of the composite conductive paste in the second step is 300-2000 cp.
9. The method for preparing a composite conductive powder according to claim 5, wherein: in the third step, the feeding temperature of spray drying is 200-220 ℃, and the discharging temperature is 120-140 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114789998A (en) * | 2021-11-01 | 2022-07-26 | 广东一纳科技有限公司 | Negative electrode material, preparation method thereof and battery |
| CN114864938A (en) * | 2021-11-22 | 2022-08-05 | 广东一纳科技有限公司 | Conductive paste containing carbon material and secondary battery |
| CN114976001A (en) * | 2022-04-27 | 2022-08-30 | 广东一纳科技有限公司 | Composite conductive powder, preparation method thereof and lithium battery |
| CN114988395A (en) * | 2022-06-22 | 2022-09-02 | 湖北冠毓新材料科技有限公司 | Method for manufacturing solid dispersion type carbon tube |
-
2021
- 2021-06-15 CN CN202110662018.8A patent/CN113436779A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114789998A (en) * | 2021-11-01 | 2022-07-26 | 广东一纳科技有限公司 | Negative electrode material, preparation method thereof and battery |
| CN114789998B (en) * | 2021-11-01 | 2024-03-19 | 广东一纳科技有限公司 | Negative electrode material, preparation method thereof and battery |
| CN114864938A (en) * | 2021-11-22 | 2022-08-05 | 广东一纳科技有限公司 | Conductive paste containing carbon material and secondary battery |
| CN114864938B (en) * | 2021-11-22 | 2023-11-21 | 广东一纳科技有限公司 | Conductive paste containing carbon material and secondary battery |
| CN114976001A (en) * | 2022-04-27 | 2022-08-30 | 广东一纳科技有限公司 | Composite conductive powder, preparation method thereof and lithium battery |
| CN114976001B (en) * | 2022-04-27 | 2024-03-19 | 广东一纳科技有限公司 | Composite conductive powder, preparation method thereof and lithium battery |
| CN114988395A (en) * | 2022-06-22 | 2022-09-02 | 湖北冠毓新材料科技有限公司 | Method for manufacturing solid dispersion type carbon tube |
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Application publication date: 20210924 |