CN113658743A - Carbon dot composite conductive agent and preparation method and application thereof - Google Patents
Carbon dot composite conductive agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a carbon dot composite conductive agent, and a preparation method and application thereof, wherein the preparation method of the carbon dot composite conductive agent comprises the following operations: 1, 3-dihydroxynaphthalene and potassium periodate are mixed according to a mass ratio of 1: 2-1: 8, mixing, synthesizing a precursor through a solvothermal reaction, and dialyzing or centrifuging the precursor to obtain the conductive carbon dot material; and mixing the conductive carbon dot material and the multi-walled carbon nano tube, adding the mixture and a dispersing agent into a solvent according to a certain mass ratio, stirring at high viscosity, diluting, and performing ultrasonic dispersion to obtain the carbon dot composite conductive agent. The invention also discloses a positive plate and a negative plate comprising the carbon dot composite conductive agent and a lithium ion battery. The conductive agent obtained by the preparation method is applied to the lithium ion battery, so that the dispersing capacity of a conductive material in a solvent can be improved, the processing performance of the conductive slurry is improved, and the conductivity of the lithium ion battery is improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a carbon dot composite conductive agent, and a preparation method and application thereof.
Background
When the 3C electronic product is updated and iterated to be infinite, the performance of the lithium ion battery, which is used as a basic component of the electronic product, affects the overall performance of the electronic product to a certain extent, and especially, the performance of the battery, which directly affects the cruising ability of the electronic product, such as the quick charging performance and the battery capacity, is of great concern. On one hand, the performances are limited by the upper limit of energy density of the anode and cathode active substances and the bottleneck of structural design of the battery cell, and on the other hand, scientific research personnel are promoted to continuously explore the improvement effect of the additives except the active substances in the anode and cathode formula. In the practical application process of the lithium ion battery anode and cathode materials, the whole conductivity of the anode and cathode plates is often improved by adding conductive materials such as graphene, carbon nanotubes and conductive carbon black.
However, the existing conductive materials such as carbon materials of carbon nanotubes, graphene and the like are difficult to disperse in solvents, poor in stirring and homogenizing processability with other materials, and difficult to effectively and uniformly disperse on the surface of an active substance, so that the overall conductivity of a pole piece is influenced, and further the electrical performance of a lithium ion battery is influenced. Therefore, it is necessary to improve the dispersibility of the conductive material in the solvent.
In view of the above, it is necessary to provide a technical solution to the above technical problems.
Disclosure of Invention
One of the objects of the present invention is: the conductive agent obtained by the preparation method is applied to the lithium ion battery, so that the dispersing capacity of a conductive material in a solvent can be improved, the processing performance of conductive slurry is improved, the ionic resistance of the lithium ion battery is reduced, and the conductivity is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a carbon dot composite conductive agent comprises the following operations:
and mixing the conductive carbon dot material and the multi-walled carbon nano tube, adding the mixture and a dispersing agent into a solvent according to a certain mass ratio, stirring at high viscosity, diluting, and performing ultrasonic dispersion to obtain the carbon dot composite conductive agent.
The conductive carbon dot material is obtained by the following preparation method: mixing 1, 3-dihydroxynaphthalene and potassium periodate, synthesizing a precursor through solvothermal reaction, and dialyzing or centrifuging the precursor to obtain the conductive carbon dot material. Wherein the mass ratio of the 1, 3-dihydroxynaphthalene to the potassium periodate is 1: 2-1: 8; in some embodiments, the mass ratio of 1, 3-dihydroxynaphthalene to potassium periodate is 1:2, 1:4, 1:6, 1:8, and the like. Preferably, the precursor is reduced at high temperature after being prepared, and the precursor is placed in a pure argon environment at high temperature of 900 ℃ for 1 hour. Preferably, the solvent is ethanol or water; the thermal reaction is finished by heating in a high-temperature high-pressure reaction kettle. Preferably, dialysis or centrifugation is performed using a dialysis machine or a centrifuge.
Furthermore, the conductive carbon material is carbon nanotubes or graphene, and preferably, the carbon nanotubes are multi-walled carbon nanotubes which are economical and practical.
In some embodiments, the mass ratio of the conductive carbon dot material to the multi-walled carbon nanotubes is 10: 1-2: 1, for example: the mass ratio of the conductive carbon dot material to the multi-wall carbon nano-tubes is 10:1 or 8:1 or 6:1 or 5:1 or 4:1 or 2:1, and the like. The obtained conductive carbon dot material has a large specific surface area, a small monomer particle size and easy dispersibility, and the multi-walled carbon nanotube has a certain specific surface area; the conductive carbon dot material can be well filled in the gaps of the carbon tubes to form a better conductive network, and the conductive carbon dot material can be uniformly dispersed on the surfaces of the multi-walled carbon nanotubes, so that the agglomeration of the conductive material can be inhibited, the advantage of stirring, dispersing and processing properties of the conductive slurry can be improved, the difficulty of the dispersing process can be effectively reduced, the binding force between a pole piece and a current collector can be improved, and the ionic resistance of the lithium ion battery can be reduced to improve the conductivity. In addition, the conductive carbon dot material and the multi-wall carbon nano tube are mixed physically, so that the conductivity of the two materials is ensured, and the mixing stability is prolonged.
Further, a mixture obtained by uniformly stirring the conductive carbon dot material and the multi-walled carbon nanotube and a dispersing agent are added into a solvent for dispersing and diluting. The mass ratio of the mixture to the dispersing agent is 6: 10-10: 1, the dispersing agent is used for dispersing the conductive carbon dot material and the multi-walled carbon nanotube, and preferably, the dispersing agent is polyvinylidene fluoride. The positive electrode binder is generally an oily binder, the oily binder is insoluble in water, and preferably, N-methylpyrrolidone, into which the oily binder is soluble, is used as a solvent. Wherein the dilution ratio is 3wt% -10 wt%; in some embodiments, the dilution ratio is 3wt%, 5wt%, 7wt%, 8wt%, 10wt%, etc.
The invention also provides a carbon dot composite conductive agent, which is prepared by the preparation method of the carbon dot composite conductive agent, and the prepared carbon dot composite conductive agent has strong dispersing ability and conductivity in a solvent.
The invention also provides a positive plate, which comprises a positive current collector and a positive material coated on the surface of the positive current collector, wherein the preparation process of the positive plate comprises the following steps: preparing a positive electrode material with the coating solid content of 50% -80%, coating the positive electrode material on a positive electrode current collector in a coating mode, and then drying, rolling and pasting a positive electrode tab to obtain a positive electrode sheet of the lithium ion battery. Preferably, non-limiting examples of the positive electrode current collector include one of aluminum foil, carbon-coated aluminum foil, lithium iron phosphate-coated aluminum foil. In some embodiments, the coating solids content is 50%, 55%, 60%, 65%, 70%, 75%, 80%, etc.
The cathode material comprises the following components in percentage by mass:
the content of the positive active substance is 80-98 wt%. Preferably, non-limiting examples of the positive electrode active material include one or a mixture of several of lithium nickel cobalt manganese oxide, lithium nickel cobalt aluminate, lithium cobalt oxide, and lithium iron phosphate.
The content of the first conductive agent is 1-10 wt%, the first conductive agent is the carbon dot composite conductive agent prepared by the preparation method, and the first conductive agent is used for endowing the positive electrode with conductivity.
The content of the first binder is 1wt% -10 wt%. Preferably, the first adhesive includes one or a mixture of polyvinylidene fluoride, styrene-butadiene rubber, polyvinyl alcohol, and polytetrafluoroethylene. The first binder serves to improve the binding of the positive electrode active material particles to each other and the binding of the positive electrode active material to the positive electrode current collector.
Mixing the positive active substance, the first conductive agent and the first adhesive with the first solvent according to the formula amount, and uniformly stirring to obtain the positive material. Wherein the first solvent is N-methyl pyrrolidone.
The invention also provides a negative plate which comprises a negative current collector and a negative material coated on the surface of the negative current collector. The preparation process of the negative plate comprises the following steps: preparing a negative electrode material with the coating solid content of 30-60%, coating the negative electrode material on a negative electrode current collector in a coating mode, and then drying, rolling and attaching a negative electrode lug to obtain a negative electrode piece of the lithium ion battery. Preferably, the negative current collector is one or a mixture of copper foil and carbon-coated copper foil; in some embodiments, the coating solids content is 30%, 35%, 40%, 45%, 50%, 55%, 60%, etc.
The negative electrode material comprises the following components in percentage by mass:
the content of the negative active material is 90-98 wt%. Preferably, non-limiting examples of the negative active material include one or a mixture of several of artificial graphite, natural graphite, soft carbon, hard carbon, and silicon.
The content of the second conductive agent is 1-3 wt%, the second conductive agent is the carbon dot composite conductive agent prepared by the method, and the second conductive agent is used for endowing the negative electrode with conductivity.
The content of the second adhesive is 1-7 wt%. Preferably, the second adhesive includes one or more of styrene-butadiene rubber, acrylate, sodium carboxymethyl cellulose, and lithium carboxymethyl cellulose. The second binder serves to improve the binding of the anode active material particles to each other and the binding of the anode active material to the anode current collector.
And mixing the negative electrode active material, the second conductive agent and the second adhesive with the second solvent according to the formula amount, and uniformly stirring to obtain the negative electrode material. Wherein the second solvent is water.
The invention also provides a lithium ion battery which comprises the positive plate and the negative plate, and a diaphragm, an aluminum-plastic film and electrolyte which are arranged between the positive plate and the negative plate. Specifically, the positive plate, the negative plate and the diaphragm are made into a winding core by a winding or gasket method, the winding core is sealed in an aluminum plastic film, and electrolyte is injected to prepare the lithium ion battery. The lithium ion battery has a voltage of 4.35V and a capacity of 3 Ah. The lithium ion battery containing the conductive agent reduces the ionic resistance of the lithium ion battery and improves the conductivity.
The lithium ion battery of the present invention is provided with a separator between the positive electrode tab and the negative electrode tab to prevent short circuit, and the material and shape of the separator used in the lithium ion battery are not particularly limited and may be any of the techniques disclosed in the prior art. In the present invention, the aluminum plastic film and the electrolyte may be any of the techniques disclosed in the prior art.
Compared with the prior art, the beneficial effects of the invention include but are not limited to:
(1) the conductive carbon dot material which is easy to disperse is prepared, has a large specific surface area and a small monomer particle size and can be uniformly dispersed on the surfaces of other conductive materials, so that the advantages of inhibiting the conductive materials from agglomerating and improving the stirring and dispersing processability of the conductive slurry are achieved, and the conductive carbon dot material is easy to uniformly disperse on the surface of an active substance.
(2) The conductive carbon dot material can be well filled in the gaps of the carbon tubes to form a better conductive network, and the conductive carbon dot material can be uniformly dispersed on the surfaces of the multi-walled carbon nanotubes, so that the agglomeration of the conductive material can be inhibited, the advantage of stirring, dispersing and processing properties of the conductive slurry can be improved, the difficulty of the dispersing process can be effectively reduced, the binding force between a pole piece and a current collector can be improved, and the ionic resistance of the lithium ion battery can be reduced to improve the conductivity.
(3) The conductive carbon dot material and the multi-wall carbon nano tube are physically compounded and are not chemically compounded, so that the conductivity of the two materials is ensured, and the mixing stability is prolonged.
Drawings
FIG. 1 is a structural formula of a conductive carbon dot material.
Detailed Description
Embodiments of the present application will be described in detail below. The examples of the present application should not be construed as limiting the present application.
The present application is further illustrated with reference to specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the claims.
Example 1
(1) Preparing a conductive carbon dot material:
1, 3-dihydroxynaphthalene and potassium periodate were mixed in a ratio of 1:4, adding the solution into an ethanol solvent for dissolving, transferring the solution into a high-temperature high-pressure reaction kettle, heating to 180 ℃ for 2 hours to react and synthesize a precursor, naturally cooling the precursor to room temperature, and obtaining the purified precursor conductive carbon dot material by a dialysis method.
(2) Preparing a carbon dot composite conductive agent:
conductive carbon dot material, multi-walled carbon nanotubes: the mass ratio of the polyvinylidene fluoride is 5:1: 10;
the conductive carbon dot material and the multi-wall carbon nano tube are mixed according to the mass ratio of 5:1, mixing the mixture with polyvinylidene fluoride according to a mass ratio of 6:10 is added into N-methyl pyrrolidone solvent to be stirred for 60min with high viscosity, and mixed solution with mass concentration of 50wt% is obtained; and continuously adding N-methyl pyrrolidone to dilute the mixed solution into a mixed solution with the mass concentration of 3wt%, and performing ultrasonic dispersion for 1h to obtain a stable mixed solution, namely the carbon dot composite conductive agent.
(3) Preparing a positive plate:
preparing nickel cobalt lithium manganate: carbon dot composite conductive agent: polyvinylidene fluoride is dissolved in N-methylpyridine according to the mass ratio of 95:2.5:2.5Dispersing and stirring in a pyrrolidone solvent to obtain uniform slurry with the solid content of 75 percent, namely the anode material; coating the positive electrode material on an aluminum foil in a coating mode, drying, rolling at normal temperature, and attaching a positive electrode tab to obtain a single-sided surface with the density of 0.01g/m2The positive plate of the lithium ion battery.
(4) Preparing a negative plate:
mixing natural graphite: carbon dot composite conductive agent: dissolving acrylic ester in an aqueous solvent according to the mass ratio of 97.5:1.3:1.2, and dispersing and stirring to obtain uniform slurry with the solid content of 45%, namely the negative electrode material; coating the negative electrode material on a copper foil in a coating mode, drying, rolling at normal temperature, and attaching negative electrode tabs to obtain the negative electrode material with the single-sided surface density of 0.01g/m2The negative plate of the lithium ion battery.
(5) Preparing a lithium ion battery:
and (3) preparing the positive plate, the negative plate and the composite diaphragm into a winding core by a winding method, sealing the winding core into an aluminum-plastic film, and injecting an electrolyte to prepare the lithium ion battery with 4.35V and 3Ah of capacity.
Example 2
This example provides a lithium ion battery, which is different from example 1 in step (3):
in the preparation process of the positive plate, the lithium nickel cobalt manganese oxide: carbon dot composite conductive agent: the mass ratio of the polyvinylidene fluoride is 97.5:1: 1.5.
The rest is the same as embodiment 1, and the description is omitted here.
Example 3
This example provides a lithium ion battery, which is different from example 1 in step (3):
in the preparation process of the positive plate, the lithium nickel cobalt manganese oxide: carbon dot composite conductive agent: the mass ratio of the polyvinylidene fluoride is 97.5:1.5: 1.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 1
The present embodiment provides a lithium ion battery, which is different from embodiment 1 in that:
the multi-wall carbon nano tube is selected as a single conductive agent, and a carbon dot composite conductive agent is not adopted.
(1) Preparing a positive plate:
preparing nickel cobalt lithium manganate: multi-walled carbon nanotubes: dissolving polyvinylidene fluoride in an N-methyl pyrrolidone solvent according to the mass ratio of 95:2.5:2.5, and dispersing and stirring to obtain uniform slurry with the solid content of 75%, namely the positive electrode material; coating the positive electrode material on an aluminum foil in a coating mode, drying, rolling at normal temperature, and attaching a positive electrode tab to obtain a single-sided surface with the density of 0.01g/m2The positive plate of the lithium ion battery.
(2) Preparing a negative plate:
mixing natural graphite: multi-walled carbon nanotubes: dissolving acrylic ester in an aqueous solvent according to the mass ratio of 97.5:1.3:1.2, and dispersing and stirring to obtain uniform slurry with the solid content of 45%, namely the negative electrode material; coating the negative electrode material on a copper foil in a coating mode, drying, rolling at normal temperature, and attaching negative electrode tabs to obtain the negative electrode material with the single-sided surface density of 0.01g/m2The negative plate of the lithium ion battery.
(3) Preparing a lithium ion battery:
and (3) preparing the positive plate, the negative plate and the composite diaphragm into a winding core by a winding method, sealing the winding core into an aluminum-plastic film, and injecting an electrolyte to obtain the 4.35V lithium ion battery with the capacity of 3 Ah.
And (3) performance testing:
(I) slurry mixing stability
The positive electrode materials of example 1, example 2, example 3 and comparative example 1 were subjected to viscosity tests using a rotational viscometer, and the test results are shown in table 1:
| viscosity of positive electrode slurry | 0h | 12h | 24h | 48h |
| Example 1 | 4313 | 5264 | 5656 | 5636 |
| Example 2 | 4625 | 5940 | 6656 | 6439 |
| Example 3 | 4841 | 5682 | 6104 | 6008 |
| Comparative example 1 | 4163 | 5738 | 6928 | 7014 |
TABLE 1
The conclusion is drawn from table 1 above:
example 1, example 2, example 3 compared to comparative example 1: from the observation of the experimental data of 0 h-48 h, the viscosity values of the positive electrode materials prepared in the examples 1, 2 and 3 are smaller than that of the positive electrode material prepared in the comparative example 1; the larger the viscosity change, the worse the slurry stability, and the slurry stability of the positive electrode materials in examples 1, 2, and 3 was significantly better than that of comparative example 1. Therefore, the carbon dot composite conductive agent is adopted to replace a multi-walled carbon nanotube as a single conductive agent, and the dispersion uniformity of the slurry can be improved.
(II) Pole piece conductivity
The positive electrode sheets in example 1, example 2, example 3 and comparative example 1 were tested for sheet resistance, and the sheet conductivity was illustrated by sheet resistance values, with the test results shown in table 2:
| membrane resistance omega | |
| Example 1 | 0.34 |
| Example 2 | 0.19 |
| Example 3 | 0.62 |
| Comparative example 1 | 0.98 |
TABLE 2
The conclusion is drawn from table 2 above:
example 1, example 2, example 3 compared to comparative example 1: the sheet resistances of the positive electrode sheets obtained in example 1, example 2, and example 3 were all smaller than the sheet resistance of the positive electrode sheet obtained in comparative example 1. Therefore, the conductivity of the positive electrode sheets obtained in examples 1, 2 and 3 was higher than that of comparative example 1, and the conductivity of the positive electrode sheet obtained in example 2 was the most excellent. The carbon dot composite conductive agent is adopted to replace a multi-walled carbon nanotube as a single conductive agent, so that the conductivity of the lithium ion battery can be improved.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. A preparation method of a carbon dot composite conductive agent is characterized by comprising the following operations:
and mixing the conductive carbon dot material and the multi-walled carbon nano tube, adding the mixture and a dispersing agent into a solvent according to a certain mass ratio, stirring at high viscosity, diluting, and performing ultrasonic dispersion to obtain the carbon dot composite conductive agent.
2. The preparation method of the carbon dot composite conductive agent according to claim 1, wherein the mass ratio of the conductive carbon dot material to the multi-walled carbon nanotube is 10: 1-2: 1; the mass ratio of a mixture obtained by uniformly stirring the conductive carbon dot material and the multi-walled carbon nanotube to the dispersing agent is 6: 10-10: 1.
3. The method for preparing the carbon dot composite conductive agent according to claim 1, wherein the solvent is N-methylpyrrolidone, and the dilution ratio is 3wt% to 10 wt%.
4. The method for preparing the carbon dot composite conductive agent according to claim 1, wherein the method for preparing the conductive carbon dot material comprises the following steps: 1, 3-dihydroxynaphthalene and potassium periodate are mixed according to a mass ratio of 1: 2-1: 8, mixing and synthesizing a precursor through a solvothermal reaction, and dialyzing or centrifuging the precursor to obtain the conductive carbon dot material.
5. A carbon dot composite conductive agent, which is characterized by being prepared by the preparation method of the carbon dot composite conductive agent according to any one of claims 1 to 4.
6. A positive electrode sheet comprising a positive electrode current collector and a positive electrode material coated on the surface of the positive electrode current collector, wherein the positive electrode material contains the carbon dot composite conductive agent according to claim 5.
7. The positive electrode sheet according to claim 6, wherein the positive electrode material comprises the following composition in percentage by mass:
80-98 wt% of positive active material;
the content of the first conductive agent is 1-10 wt%;
1-10 wt% of a first binder;
the first conductive agent is the carbon dot composite conductive agent according to claim 5.
8. A negative electrode sheet comprising a negative electrode current collector and a negative electrode material coated on a surface of the negative electrode current collector, wherein the negative electrode material comprises the carbon dot composite conductive agent according to claim 5.
9. The negative electrode sheet according to claim 8, wherein the negative electrode material comprises the following composition in percentage by mass:
90-98 wt% of a negative electrode active material;
the content of the second conductive agent is 1-3 wt%;
the content of the second binder is 1-7 wt%;
the second conductive agent is the carbon dot composite conductive agent according to claim 5.
10. A lithium ion battery comprising the positive electrode sheet according to any one of claims 6 to 7, the negative electrode sheet according to any one of claims 8 to 9, a separator, an aluminum-plastic film, and an electrolyte, wherein the positive electrode sheet, the negative electrode sheet, and the separator are wound or made into a roll core by a method of a gasket, and the roll core is sealed in the aluminum-plastic film and the electrolyte is injected to obtain the lithium ion battery.
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| CN111342001A (en) * | 2020-03-06 | 2020-06-26 | 上海汽车集团股份有限公司 | Composite sulfur positive electrode for solid-state lithium-sulfur battery, and preparation method and application thereof |
| CN111769284A (en) * | 2020-06-23 | 2020-10-13 | 合肥国轩高科动力能源有限公司 | Carbon quantum dot/CNTs composite positive electrode conductive agent and preparation method thereof |
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| CN114874433A (en) * | 2022-05-11 | 2022-08-09 | 四川大学 | Preparation method of manganous oxide doped isomelanin nano material and film with electromagnetic shielding function and product |
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