CN115275101A - Graphene carbon nanotube positive plate and preparation method thereof - Google Patents

Graphene carbon nanotube positive plate and preparation method thereof Download PDF

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CN115275101A
CN115275101A CN202211031919.8A CN202211031919A CN115275101A CN 115275101 A CN115275101 A CN 115275101A CN 202211031919 A CN202211031919 A CN 202211031919A CN 115275101 A CN115275101 A CN 115275101A
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conductive
graphene
carbon nanotube
mass ratio
coating
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王瑛
王欣
肖双
张立君
冯彩霞
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Shandong Yuhuang New Energy Technology Co Ltd
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    • H—ELECTRICITY
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    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0404—Methods of deposition of the material by coating on electrode collectors
    • H—ELECTRICITY
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    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
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    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
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    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
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    • 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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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The invention provides a graphene carbon nanotube positive plate. The positive plate includes: a current collector and a conductive coating coated on the current collector. The conductive coating is obtained by coating and curing conductive slurry. The conductive paste consists of the following components: activity ofSubstance (b): organic bentonite: polyacrylic acid: carboxymethyl cellulose: the mass ratio of the conductive agent is 70-97.5%: 0.1-5%: 0.5-15%: 0.5-10%: 1 to 5 percent; wherein the conductive agent is formed from carbon nanotubes: graphene: the super conductive carbon black is prepared from the following components in a mass ratio of 0.5-1.5: 0.5-1.5: 1 to 2. The particle size of the graphene is 50-400 nm, and the pipe diameter of the carbon nano tube is 5-10 nm. The active material is LiNi 0.8 Co 0.15 Al 0.05 O 2 And LiMn 2 O 4 According to the mass ratio of 1.7-8: 1. The thickness of the conductive coating is 0.1-4 μm. The invention provides an electrode material with good conductivity, corrosion resistance, heat dissipation and adhesion.

Description

Graphene carbon nanotube positive plate and preparation method thereof
Technical Field
The invention relates to the field of electrode materials, in particular to a graphene carbon nanotube positive plate and a preparation method thereof.
Background
The existing lithium ion battery generally uses a carbon-coated aluminum foil as a carrier of a positive electrode material, however, the carbon-coated aluminum foil has the defects of poor adhesive force and easy peeling of a carbon-coated layer, and the electrical conductivity of the carbon-coated layer can be reduced by increasing a binder of carbon conductive slurry for improving the adhesive force; in addition, the aluminum foil surface has aluminum oxide film, which affects the conductivity of the carbon-coated aluminum foil.
Therefore, the development of the positive plate with good conductivity, corrosion resistance, heat dissipation and adhesion, which can effectively improve the discharge capacity of the lithium battery and prolong the cycle life, has very important significance in promoting the further development of the lithium battery field.
Disclosure of Invention
The inventor finds out through analysis that: in the prior art, a carbon-coated aluminum foil is added with a dispersing agent to ensure that a carbon-coated layer is firmly attached to a current collector; in order to ensure the adhesive force between the carbon-coated layer and the current collector, the using amount of the dispersing agent is large; however, since the dispersant used is a poor conductor of electrons, the electron conductivity of the conductive coating is limited, and the electron conductivity of the entire electrode is limited, which is disadvantageous for the performance of multiplying power of an electrochemical system. According to the graphene carbon nanotube positive plate prepared by compounding the active substance, the three composite conductive agents and the dispersing agent, the polarization of the battery can be inhibited, the thermal effect is reduced, and in addition, the conductive capability of the positive plate is improved while the binding force between the conductive coating and the current collector is not influenced.
The inventionIn one aspect, a graphene carbon nanotube positive electrode sheet is provided, which includes: a current collector and a conductive coating coated on the current collector; the conductive coating is obtained by coating and curing conductive slurry. The conductive paste consists of the following components: active substance: organic bentonite: polyacrylic acid: carboxymethyl cellulose: the mass ratio of the conductive agent is 70-97.5%: 0.1-5%: 0.5-15%: 0.5-10%: 1 to 5 percent; wherein the conductive agent is formed from carbon nanotubes: graphene: the super conductive carbon black is prepared from the following components in a mass ratio of 0.5-1.5: 0.5-1.5: 1 to 2. The particle size of the graphene is 50-400 nm, and the pipe diameter of the carbon nano tube is 5-10 nm. The active material is LiNi 0.8 Co 0.15 Al 0.05 O 2 And LiMn 2 O 4 According to the mass ratio of 1.7-8: 1. The thickness of the conductive coating is 0.1-4 μm.
The invention also provides a preparation method of the graphene carbon nanotube positive plate, which comprises the following steps:
and coating the conductive slurry on the current collector, drying and tabletting to obtain the graphene carbon nanotube positive plate.
The beneficial effects obtained by the invention comprise at least one of the following contents:
1. the graphene carbon nanotube positive plate disclosed by the invention is beneficial to improving the conductive capability of the positive plate while not influencing the binding force between the conductive coating and the current collector. For example, the conductivity does not exceed 3X 10 at normal temperature -8 Omega.m, the peel strength of the pole piece is not lower than 90N/m.
2. The graphene carbon nanotube positive plate prepared by the invention provides an electrode material with good conductivity, corrosion resistance, heat dissipation and cohesiveness by coating the conductive slurry and the current collector. In addition, the graphene carbon nanotube positive plate prepared by compounding the active substance, the three composite conductive agents and the dispersing agent can inhibit battery polarization and reduce heat effect.
Detailed Description
In one exemplary embodiment of the present invention, a graphene carbon nanotube positive electrode sheet includes: a current collector and a conductive coating coated on the current collector; the conductive coating is obtained by coating and curing conductive slurry; the current collector may be an aluminum foil, however, the present invention is not limited thereto.
The conductive paste consists of the following components: active substance: organic bentonite: polyacrylic acid: carboxymethyl cellulose: the mass ratio of the conductive agent is 70-97.5%: 0.1-5%: 0.5-15%: 0.5-10%: 1 to 5 percent; wherein the conductive agent is formed from carbon nanotubes: graphene: the super conductive carbon black is prepared from the following components in a mass ratio of 0.5-1.5: 0.5-1.5: 1 to 2. The particle size of the graphene is 50-400 nm, and the pipe diameter of the carbon nano tube is 5-10 nm. The active material is LiNi 0.8 Co 0.15 Al 0.05 O 2 And LiMn 2 O 4 According to the mass ratio of 1.7-8: 1. The thickness of the conductive coating is 0.1-4 μm.
In one exemplary embodiment of the present invention, the thickness of the conductive coating may be 2.5 to 3.5 μm. Insufficient thickness of the conductive coating may result in the current collector being susceptible to corrosion by the electrode active material, and too thick a thickness of the conductive coating of the current collector may affect the electrochemical performance of the electrochemical system.
In one exemplary embodiment of the invention, the active substance: organic bentonite: polyacrylic acid: carboxymethyl cellulose: the mass ratio of the conductive agent is 75-90%: 1.5-4%: 3-10%: 2-8%: 2 to 4 percent. Further, the active substance: organic bentonite: polyacrylic acid: carboxymethyl cellulose: the mass ratio of the conductive agent is 80-85%: 2-3%: 5-8%: 4-6%: 2.5 to 3 percent.
In one exemplary embodiment of the present invention, the carbon nanotube: graphene: the mass ratio of the super conductive carbon black is 0.8-1.2: 0.8 to 1.2:1.2 to 1.6. The particle size of the graphene is 100-300 nm, and the pipe diameter of the carbon nano tube is 7-9 nm.
In an exemplary embodiment of the present invention, the solvent of the conductive paste is at least one of deionized water, absolute ethyl alcohol, and an alkaline solution. The PH value of the alkaline solution is 9-10.
In an exemplary embodiment of the invention, organobentonite, polyacrylic acid and carboxymethyl cellulose are mixed and are sufficiently dissolved by dropping deionized water, so as to obtain a first mixture, a conductive agent is added into the first mixture and is uniformly stirred to obtain a second mixture, and an active substance is added into the second mixture and is further uniformly stirred to obtain the graphene carbon nanotube composite conductive paste. And uniformly coating the conductive slurry on a current collector, drying and tabletting to obtain the graphene carbon nanotube positive plate. For example, at 90-130 ℃, the coating is dried in a vacuum drying oven for 7-12 h and then is pressed into sheets. However, the present invention is not limited thereto.
In the invention, organic bentonite, polyacrylic acid and carboxymethyl cellulose are used as dispersing agents; carbon nanotubes, graphene and super conductive carbon black are used as conductive agents. The purpose of dissolving the dispersing agent is to ensure that the viscosity of the later prepared slurry is higher in a static state, and the precipitation and agglomeration of the slurry can be effectively prevented. For example, in forming the paste, the conductive agent: dispersing agent: the mass ratio of the solvent may be 2 to 5.
The preparation method of the graphene carbon nanotube positive plate comprises the following steps:
and coating the conductive slurry on the current collector, drying and tabletting to obtain the graphene carbon nanotube positive plate. The tabletting process may be carried out using a roller press. The following example is a specific procedure:
example 1
Grinding active substances, carbon nano tubes, graphene and super conductive carbon black required by experiments, wherein the raw materials are as follows: polyacrylic acid: the mass ratio of the carboxymethyl cellulose is 2%:3%:3%, dropwise add deionized water, carry out magnetic force constant temperature stirring, after fully dissolving, add the conductive agent stirring, wherein carbon nanotube: graphene: the mass ratio of the super conductive carbon black is 0.8:0.8:1, the particle size of graphene is 100nm, the pipe diameter of the carbon nano tube is 6nm, and finally, active substances are added for further stirring, wherein the active substances LiNi 0.8 Co 0.15 Al 0.05 O 2 And LiMn 2 O 4 The mass ratio is 2:1 to obtainThe graphene carbon nanotube composite conductive slurry is prepared by the following steps. Coating the conductive slurry on an aluminum foil, uniformly coating the conductive slurry on the aluminum foil by using a trowel of a coating machine, placing the coated conductive slurry in a vacuum drying oven, drying for 8 hours at the temperature of 100 ℃, tabletting to obtain the graphene carbon nanotube anode material, and cutting to obtain the graphene carbon nanotube anode plate.
Example 2
Grinding active substances, carbon nanotubes, graphene and super conductive carbon black required by experiments in a mortar, wherein the raw materials are as follows: polyacrylic acid: the mass ratio of the carboxymethyl cellulose is 3%:5%:5%, dropwise adding deionized water, carrying out magnetic constant-temperature stirring, fully dissolving, adding a ternary conductive agent, and uniformly stirring, wherein the carbon nano tube: graphene: the mass ratio of the super conductive carbon black is 1:0.8:1.5, the particle diameter of the graphene is 80nm, the pipe diameter of the carbon nano tube is 9nm, and finally, an active substance LiNi is added for further stirring, wherein the active substance LiNi 0.8 Co 0.15 Al 0.05 O 2 And LiMn 2 O 4 The mass ratio is 5:1, and the graphene carbon nanotube composite conductive slurry is obtained. And coating the conductive slurry on an aluminum foil, uniformly coating the conductive slurry on the aluminum foil by using a trowel of a coating machine, placing the coated conductive slurry in a vacuum drying oven, drying the conductive slurry for 12 hours at the temperature of 80 ℃, and then tabletting and cutting the conductive slurry to obtain the graphene carbon nanotube positive plate.
Example 3
Grinding active substances, carbon nanotubes, graphene and super conductive carbon black required by an experiment in a mortar, wherein the raw materials are as follows: polyacrylic acid: the mass ratio of the carboxymethyl cellulose is 2%:10%:6 percent, dropwise adding deionized water, carrying out magnetic constant-temperature stirring, and after fully dissolving, adding a ternary conductive agent and uniformly stirring, wherein the carbon nano tube: graphene: the mass ratio of the super conductive carbon black is 0.8:1:1.5, the particle diameter of the graphene is 200nm, the pipe diameter of the carbon nano tube is 6nm, and finally, an active substance LiNi is added for further stirring, wherein the active substance LiNi 0.8 Co 0.15 Al 0.05 O 2 And LiMn 2 O 4 The mass ratio is 3: 1, and the graphene carbon nanotube composite conductive slurry is obtained.And coating the conductive slurry on an aluminum foil, uniformly coating the conductive slurry on the aluminum foil by using a trowel of a coating machine, drying for 10 hours at 120 ℃ in a vacuum drying oven after coating, and then tabletting and cutting to obtain the graphene carbon nanotube positive plate.
Comparative example 1
On the basis of example 1, the difference is that no organic bentonite is added to the conductive paste.
Comparative example 2
The difference is that no polyacrylic acid is added to the conductive paste in example 1.
Comparative example 3
Based on example 1, the difference is that no carboxymethyl cellulose is added to the conductive paste.
Comparative example 4
The difference is that the thickness of the conductive coating is 15 μm on the basis of example 1.
Comparative example 5
The difference is that the thickness of the conductive coating is 30 μm on the basis of example 1.
Under the same environment, the graphene carbon nanotube positive plates provided in examples 1 to 3 and comparative examples 1 to 5 were subjected to resistance tests of the plates at different temperatures, and the results of the volume resistivity tests are shown in table 1. And (3) testing the mechanical property of the pole piece at normal temperature, testing the peel strength of the pole piece by using a tensile testing machine, and listing the test results in table 2.
TABLE 1 volume resistivity test results
Figure BDA0003817788070000051
Figure BDA0003817788070000061
TABLE 2 Pole piece Peel Strength test results
Peel strength (N/m)
Example 1 95
Example 2 94
Example 3 97
Comparative example 1 50
Comparative example 2 45
Comparative example 3 54
Comparative example 4 55
Comparative example 5 50
Referring to table 1, the volume resistivity test results of example 1, example 2 and example 3 show that the resistivity of the graphene carbon nanotube positive electrode sheet prepared by the invention is not more than 3 × 10 at 25 ℃ -8 Omega.m. At higher temperatures, e.g. 75 ℃, the resistivity does not exceed 10X 10 -8 Ω·m。
Referring to table 1, in comparative examples 1, 2 and 3, the resistivity of the graphene carbon nanotube positive electrode sheet of the present invention was improved by reducing the use of the dispersant, i.e., bentonite, polyacrylic acid and carboxymethylcellulose, as compared to example 1, but as shown in table 2, the peel strength of the sheet was reduced by about 50%.
Referring to table 1, in comparative examples 4 and 5, compared with example 1, respectively, the conductive coating is too thick to be beneficial to the electrochemical performance of the pole piece; meanwhile, referring to table 2, the peel strength of the pole piece too thick is also decreased.
In conclusion, the graphene carbon nanotube positive plate disclosed by the invention is beneficial to improving the conductive capability of the positive plate while not influencing the bonding force between the conductive coating and the current collector. For example, the conductivity does not exceed 3X 10 at normal temperature -8 Omega.m, the peel strength of the pole piece is not lower than 90N/m. In addition, the graphene carbon nanotube positive plate disclosed by the invention is good in corrosion resistance and heat dissipation, and contributes to improvement of the electrochemical performance of the battery.
The above description is only an example of the present invention, and is not intended to limit the present invention. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.

Claims (9)

1. The graphene carbon nanotube positive electrode sheet is characterized by comprising: a current collector and a conductive coating coated on the current collector; the conductive coating is obtained by coating and curing conductive slurry;
the conductive paste consists of the following components: active substance: organic bentonite: polyacrylic acid: carboxymethyl cellulose: the mass ratio of the conductive agent is 70-97.5%: 0.1-5%: 0.5-15%: 0.5-10%: 1 to 5 percent; wherein the conductive agent is formed from carbon nanotubes: graphene: the super conductive carbon black is prepared from the following components in a mass ratio of 0.5-1.5: 0.5 to 1.5: 1-2; the particle size of the graphene is 50-400 nm, and the pipe diameter of the carbon nano tube is 5-10 nm; the active material is LiNi 0.8 Co 0.15 Al 0.05 O 2 And LiMn 2 O 4 According to the mass ratio of 1.7-8: 1, preparing a composition;
the thickness of the conductive coating is 0.1-4 μm.
2. The graphene carbon nanotube positive electrode sheet according to claim 1, wherein the conductive coating has a thickness of 2.5 to 3.5 μm.
3. The graphene carbon nanotube positive electrode sheet according to claim 1, wherein the current collector is an aluminum foil.
4. The graphene carbon nanotube positive electrode sheet according to claim 1, wherein the active material: organic bentonite: polyacrylic acid: carboxymethyl cellulose: the mass ratio of the conductive agent is 75-90%: 1.5-4%: 3-10%: 2-8%: 2 to 4 percent.
5. The graphene carbon nanotube positive electrode sheet according to claim 1, wherein the active material: organic bentonite: polyacrylic acid: carboxymethyl cellulose: the mass ratio of the conductive agent is 80-85%: 2-3%: 5-8%: 4-6%: 2.5 to 3 percent.
6. The graphene carbon nanotube positive electrode sheet according to claim 1, wherein the carbon nanotube: graphene: the mass ratio of the super conductive carbon black is 0.8-1.2: 0.8 to 1.2:1.2 to 1.6.
7. The graphene carbon nanotube positive electrode sheet according to claim 1, wherein the graphene has a particle size of 100 to 300nm and a carbon nanotube diameter of 7 to 9nm.
8. The graphene carbon nanotube positive electrode sheet according to claim 1, wherein the solvent of the conductive paste is at least one of deionized water, absolute ethyl alcohol, and an alkaline solution.
9. The method for preparing the graphene carbon nanotube positive electrode sheet according to any one of claims 1 to 8, comprising the steps of:
and coating the conductive slurry on the current collector, drying and tabletting to obtain the graphene carbon nanotube positive plate.
CN202211031919.8A 2022-08-26 2022-08-26 Graphene carbon nanotube positive plate and preparation method thereof Pending CN115275101A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115939389A (en) * 2022-11-24 2023-04-07 福建蓝海黑石新材料科技有限公司 Conductive material composition, conductive paste, and preparation method and application thereof
WO2024092683A1 (en) * 2022-11-04 2024-05-10 宁德时代新能源科技股份有限公司 Positive electrode sheet, secondary battery, and electric device

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024092683A1 (en) * 2022-11-04 2024-05-10 宁德时代新能源科技股份有限公司 Positive electrode sheet, secondary battery, and electric device
CN115939389A (en) * 2022-11-24 2023-04-07 福建蓝海黑石新材料科技有限公司 Conductive material composition, conductive paste, and preparation method and application thereof
CN115939389B (en) * 2022-11-24 2024-03-15 福建蓝海黑石新材料科技有限公司 Conductive material composition, conductive paste, and preparation method and application thereof

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