CN114447286A - High-compatibility modified slurry, preparation method and application in positive electrode material - Google Patents

High-compatibility modified slurry, preparation method and application in positive electrode material Download PDF

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CN114447286A
CN114447286A CN202210094471.8A CN202210094471A CN114447286A CN 114447286 A CN114447286 A CN 114447286A CN 202210094471 A CN202210094471 A CN 202210094471A CN 114447286 A CN114447286 A CN 114447286A
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iron phosphate
lithium iron
modified slurry
compatibility
preparation process
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黄美灵
王昊
谢正伟
彭工厂
王国冬
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Chengdu Organic Chemicals Co Ltd of CAS
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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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Abstract

The invention relates to the technical field of battery materials, and aims to solve the problem that existing lithium iron phosphate anode materials are poor in dispersibility among a conductive substance, a dopant and a lithium iron phosphate main material during battery preparation and material preparation. It discloses a preparation process of high-compatibility modified slurry, which comprises the following steps: dissolving a carbon source, a dispersing agent and a complexing agent in a solvent to obtain a solution A; blending a conductive agent and a doping agent to obtain a mixture I; and adding the mixture I into the solution A, and dispersing to obtain the high-compatibility modified slurry. The high-compatibility modified slurry is applied to the lithium iron phosphate anode material, can effectively solve the dispersion and uniformity problems in the industry, improves the dispersion characteristic of a conductive network, improves the uniformity of doped elements and reduces the processing cost of a lithium ion battery based on the lithium iron phosphate anode material; the electrochemical performance of the lithium iron phosphate anode material is improved, and the plateau rate under high multiplying power is obviously improved.

Description

High-compatibility modified slurry, preparation method and application in positive electrode material
Technical Field
The invention relates to the technical field of battery materials, in particular to high-compatibility modified slurry, a preparation method and application in a positive electrode material.
Background
The lithium iron phosphate is considered to be a lithium ion battery anode material with large-scale application potential due to the characteristics of good safety performance, stable discharge platform, high cycle performance, environmental friendliness, no toxicity and the like. One FeO exists in the lithium iron phosphate crystal lattice6Octahedron, two LiO6Octahedron and a PO4Tetrahedra share, belonging to the Pmnb space group in orthorhombic system in crystallographic classification, unit cell volume
Figure BDA0003490281610000011
Lithium ions in the lithium iron phosphate have mobility in one-dimensional direction, can be inserted/extracted in the charging and discharging process, and are reduced/oxidized along with central metal iron. After the lithium ions are extracted, FePO which is the Pmnb space group is generated4Unit lattice constant to unit lattice volume
Figure BDA0003490281610000012
The one-dimensional lithium ion migration channel in the crystal lattice and the change of the crystal lattice in the charging and discharging process cause the problem that the lithium iron phosphate is low in ionic and electronic conductivity.
In the preparation process of the material, modification processes such as carbon coating and element doping are generally used to improve the low electron/ion conduction rate of the lithium iron phosphate. In the battery preparation process, the electrochemical performance of the lithium ion battery based on the lithium iron phosphate cathode material is improved by adding conductive agents such as carbon nanotubes, graphene or SuperP.
However, the conventional modification process has two obvious problems: firstly, the problems of incomplete doping, uneven distribution of doping elements and unstable valence bond combination are caused by taking crystallography into consideration in the doping process; and secondly, the battery preparation and material preparation processes are mutually stripped, so that the conductive agent and the lithium iron phosphate material are not sufficiently combined, and the problem of poor conductivity of the lithium iron phosphate is difficult to fundamentally solve. And from the perspective of the whole industry chain, the problem of dispersion of the conductive agent is also needed to be solved, and the fracture is not different from the increase of the production cost of the battery.
Therefore, a more concise process route is needed to be developed, the problems of dispersion and uniformity of the conductive substance, the dopant and the lithium iron phosphate main material are solved, and the method can be applied to the production of the large-scale lithium iron phosphate anode material.
Disclosure of Invention
< problems to be solved by the present invention >
The existing lithium iron phosphate anode material has the problem of poor dispersibility among a conductive substance, a doping element and a lithium iron phosphate main material in battery preparation and material preparation.
< technical solution adopted in the present invention >
In view of the above technical problems, the present invention is directed to a highly compatible modified slurry, a preparation method, and an application in a positive electrode material. The main raw material and the additive in the preparation process of the lithium iron phosphate are divided in a memorable manner. The high-compatibility modified slurry is innovatively provided through research on a conductive agent and a doping element. Compared with the conventional slurry applied to electrode preparation, the high-compatibility modified slurry provided by the invention is applied to the preparation process of the lithium iron phosphate anode material, and organically unifies the battery preparation process and the material preparation process. The dispersibility and compatibility of the conductive agent and the doping elements are solved, so that the electrochemical performance of the lithium ion battery based on the lithium iron phosphate anode material is improved.
The specific contents are as follows:
the invention provides a preparation process of high-compatibility modified slurry, which comprises the following steps:
s1, sequentially dissolving a carbon source, a dispersing agent and a complexing agent in a solvent to obtain a solution A;
s2, blending the conductive agent and the doping agent to obtain a mixture I;
s3, adding the mixture I into the solution A, and dispersing to obtain high-compatibility modified slurry.
Secondly, the invention provides a high-compatibility modified slurry obtained by the preparation method.
Thirdly, the invention provides the application of the high-compatibility modified slurry in a lithium iron phosphate anode material.
Fourthly, the invention provides a preparation process of a lithium iron phosphate anode material, which comprises the following steps: and after blending the lithium source, the ferric phosphate and the high-compatibility modified slurry, carrying out homogenization, grinding, spraying, sintering, gas breaking and demagnetizing treatment to obtain the lithium iron phosphate cathode material.
Fifth, the invention provides a lithium iron phosphate positive electrode material obtained by the preparation process.
< technical mechanism adopted in the present invention >
The invention is at least used for solving the following problems: the carbon nano tube is applied to the problems of dispersibility and uniformity in the lithium iron phosphate anode material, and the invention is used for solving the problems by the following mechanism:
(1) in the prior art, a local agglomeration phenomenon can be formed by directly adding the carbon nano tube into the lithium iron phosphate slurry. Therefore, the invention firstly utilizes the conductive agent (including the carbon nano tube) to prepare the slurry; meanwhile, the slurry also comprises a dispersing agent and a complexing agent which are used for ensuring the self-dispersing uniformity of the carbon nano tube;
(2) the complexing agent is added into the slurry, so that the purpose of ensuring that the doping agent can be stably combined on the conductive agent and ensuring the uniform dispersion of the doping agent is also achieved;
(3) the dopant has the same polyanion structure as the lithium iron phosphate anode, and is stably combined on the carbon nano tube, so that the stable combination of the conductive agent and the lithium iron phosphate anode material can be ensured.
< advantageous effects achieved by the present invention >
(1) The high-compatibility conductive slurry is mainly applied to the synthesis stage of the lithium iron phosphate anode material, and LiMPO formed after cations in the dopant occupy Fe positions is utilized4With main material LiFePO4Has similar crystal structure and is easier to form solid solution LiFexM1-xPO4The lithium iron phosphate crystal has the characteristics of enhancing the structural stability of the lithium iron phosphate crystal and improving the multiplying power under the synergistic action of the conductive agent;
(2) the high-compatibility modified slurry is applied to the lithium iron phosphate anode material, can effectively solve the dispersion and uniformity problems in the industry, improves the dispersion characteristic and reduces the processing cost of the lithium ion battery based on the lithium iron phosphate anode material; the electrochemical performance of the lithium iron phosphate anode material is improved, and the plateau rate under high rate is remarkably improved;
(3) the high-compatibility modified slurry provided by the invention is applied to the preparation process of the lithium iron phosphate anode material, and organically unifies the battery preparation process and the material preparation process. The dispersibility and compatibility of the conductive agent and the doping elements are solved, so that the electrochemical performance of the lithium ion battery based on the lithium iron phosphate anode material is improved.
Drawings
FIG. 1 is a scanning electron microscope image of lithium iron phosphate in example 1;
fig. 2 is a rate curve of a button cell prepared from the lithium iron phosphate of example 1;
fig. 3 is a rate curve of a button cell prepared with the lithium iron phosphate of comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The invention provides a preparation process of high-compatibility modified slurry, which comprises the following steps:
s1, sequentially dissolving a carbon source, a dispersing agent and a complexing agent in a solvent to obtain a solution A;
s2, blending the conductive agent and the doping agent to obtain a mixture I;
s3, adding the mixture I into the solution A, and dispersing to obtain high-compatibility modified slurry.
According to the invention, 10-15 parts of carbon source, 1-2 parts of dispersing agent and 1-2 parts of complexing agent are taken to prepare a mixture, and the mass ratio of the mixture to the solvent is 1: 1-1.5.
In the invention, the mass ratio of the conductive agent to the dopant to the solvent is 0.005-0.3: 0.005-0.2: 1.
In the invention, the components of the high-compatibility modified slurry can be selected from the following raw materials:
the carbon source comprises at least one of glucose, sucrose or phenolic resin;
the dispersing agent comprises at least one of polyvinylpyrrolidone, polyethylene glycol, isobutanol, cyclohexanol or paraffin oil;
the complexing agent comprises at least one of citric acid, oxalic acid, lactic acid, tartaric acid or ethylenediamine tetraacetic acid;
the solvent comprises at least one of water, ethanol, or propanol.
The conductive agent comprises at least one of spherical conductive agent, linear conductive agent or flake conductive agent; specifically, the spherical conductive agent includes mesocarbon microbeads; the linear conductive agent comprises single-walled carbon nanotubes and multi-walled carbon nanotubes; the flake conductive agent comprises graphene oxide and reduced graphene oxide.
The dopant includes at least one of aluminum phosphate, cobalt phosphate, phosphomolybdic acid, lanthanum phosphate, or manganese phosphate.
In the invention, the pH value of the high-compatibility modified slurry is 3-6, the particle size of D50 is 0.2-10 mu m, and the solid content is 5-50%.
In the invention, in S3, a vertical or horizontal sand mill is adopted for dispersion, and a turbine or a pin type stirring shaft is adopted; the rotation speed of a main shaft of the sand mill is 500-2000 rpm; the grinding medium is 0.3-3 μm zirconium balls; the loading of the grinding medium is 50-80%.
Secondly, the invention provides a high-compatibility modified slurry obtained by the preparation process.
Thirdly, the invention provides application of the high-compatibility modified slurry in a cathode material.
Fourthly, the invention provides a preparation process of a lithium iron phosphate anode material, which comprises the following steps: and after blending the lithium source, the ferric phosphate and the high-compatibility modified slurry, carrying out homogenization, grinding, spraying, sintering, gas breaking and demagnetizing treatment to obtain the lithium iron phosphate cathode material.
According to the invention, the mass ratio of the high-compatibility modified slurry to the lithium source to the iron phosphate is 0.2-0.3: 1.
In the present invention, the lithium source includes at least one of lithium carbonate, lithium hydroxide, or lithium phosphate.
Fifth, the invention provides a lithium iron phosphate positive electrode material obtained by the preparation process. The prepared material has good conductivity and lattice stability, and a conductive agent is not added in the homogenization stage of preparing the lithium ion battery, so that the preparation process and the production cost of the lithium ion battery are reduced.
< example >
Example 1
(1) 1.5kg of glucose, 0.3kg of polyvinylpyrrolidone and 0.2kg of citric acid were dissolved in 2kg of water and recorded as solution A.
(2) 0.05kg of multi-walled carbon nanotubes with a diameter of 50nm and 0.02kg of aluminum phosphate were mixed and the mixture was designated as mixture I.
(3) And adding the mixture I into the solution A, and performing homogeneous dispersion by using a horizontal turbine type sand mill to obtain the high-compatibility modified slurry. Wherein the rotation speed of the main shaft of the sand mill is 1200rpm, the grinding medium is 0.5 mu m zirconium balls, the filling amount of the grinding medium is 70%, the pH value range of the slurry is 3-6, the particle size range D50 of the slurry is less than 0.5 mu m, and the solid content of the slurry is 31%.
(4) In the blending stage of the lithium iron phosphate positive electrode material, 2.47kg of lithium carbonate and 10.0kg of iron phosphate are weighed, and then the high-compatibility modified slurry in the step (3) is added. And then homogenizing, grinding, spraying, sintering, breaking gas and demagnetizing (the working procedures are all conventional preparation procedures of the existing lithium iron phosphate material), so as to obtain the modified lithium iron phosphate cathode material.
(5) And (3) taking the lithium iron phosphate prepared in the step (4) as a positive electrode active material, taking polyvinylidene fluoride as a binder, taking N-methyl pyrrolidone as a solvent, and carrying out ball milling and size mixing on the lithium iron phosphate and the polyvinylidene fluoride at a mass ratio of 19:1, wherein the solid content of the size is 33.3%. And (3) preparing a positive pole piece of the battery, assembling the positive pole piece and the negative pole piece into a button type half battery by taking a metal lithium piece as a negative pole, and testing the multiplying power performance of the button type half battery. As can be seen from FIG. 2, the charge-discharge curve of the sample is smooth, the charge-discharge plateau is stable, and the plateau rate can be kept better under the high rate of 3C.
Example 2
This example differs from example 1 in that (2) multi-walled carbon nanotubes were replaced with reduced graphene oxide. 0.02kg of aluminum phosphate was replaced by 0.03kg of phosphomolybdic acid.
Example 3
This example differs from example 1 in that:
(1) in the solution A, 3kg of sucrose, 0.6kg of polyethylene glycol and 0.6kg of tartaric acid are dissolved in 6.3kg of water in sequence.
(2) In the method, mesocarbon microbeads are adopted, and 0.02kg of aluminum phosphate is replaced by 0.01kg of lanthanum phosphate.
Example 4
This example differs from example 1 in that:
(1) the composition of solution A was 0.6kg glucose, 0.15kg isobutanol and 0.03kg oxalic acid in 0.78kg water.
(2) In the method, a single-walled carbon nanotube with the tube diameter of 10nm is adopted, and 0.02kg of aluminum phosphate is replaced by 0.15kg of manganese phosphate
(4) The lithium source used was a mixture of 2.45kg of lithium carbonate and 0.04kg of lithium phosphate.
< comparative example >
Comparative example 1
A preparation method of a lithium iron phosphate anode material comprises the following steps:
(1) in the blending stage of the lithium iron phosphate positive electrode material, 2.47kg of lithium carbonate and 10.0kg of iron phosphate are weighed, and 1.5kg of glucose is added. The carbon-coated lithium iron phosphate anode material can be obtained after homogenization, grinding, spraying, sintering, gas breaking and demagnetization;
(2) taking the lithium iron phosphate prepared in the step (1) as a positive electrode active material, taking conductive carbon black with the diameter less than 10 microns as a conductive agent, taking polyvinylidene fluoride as a binder, taking N-methylpyrrolidone as a solvent, taking the mass ratio of the lithium iron phosphate to the carbon nano tube to the polyvinylidene fluoride as 18:1:1, and performing ball milling and size mixing to obtain a slurry with the solid content of 33.3%. And (3) preparing a positive pole piece of the battery, assembling the positive pole piece and the negative pole piece into a button type half battery by taking a metal lithium piece as a negative pole, and testing the multiplying power performance of the button type half battery.
< test example >
A scanning electron micrograph of the sample was taken from the lithium iron phosphate prepared in example 1, and the result is shown in fig. 1 (magnification is 20000 times).
As can be seen from fig. 1, the prepared material, the carbon nanotubes enter the interior of the spherical particles, and a stronger conductive network is constructed. No clumped carbon nanotube clusters were observed.
The rate curves of the button cell prepared from the lithium iron phosphate prepared in example 1 and comparative example 1 were measured by using the button cell prepared from the lithium iron phosphate prepared in example 1 and comparative example 1 as a sample, and performing two-time activation through charging and discharging at 0.1C, then performing 0.3C charging, and performing 0.3, 0.5, 1, 2, and 3C discharging at different rates, and the results are shown in fig. 2 (example 1) and fig. 3 (comparative example 1).
As can be seen from FIG. 2, the charge-discharge curve of the sample is smooth, the charge-discharge plateau is stable, and the plateau rate can be kept better under the high rate of 3C.
As can be seen from fig. 3, the lithium iron phosphate prepared by the conventional process has poor stability of the charge and discharge platform and is attenuated more rapidly under high rate.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A preparation process of high-compatibility modified slurry is characterized by comprising the following steps:
s1 dissolving a carbon source, a dispersing agent and a complexing agent in a solvent to obtain a solution A;
s2, blending the conductive agent and the doping agent to obtain a mixture I;
s3, adding the mixture I into the solution A, and dispersing to obtain high-compatibility modified slurry.
2. The preparation process of the high-compatibility modified slurry according to claim 1, wherein in S1, 10-15 parts of carbon source, 1-2 parts of dispersant and 1-2 parts of complexing agent are mixed to form a mixture, and the mass ratio of the mixture to the solvent is 1: 1-1.5.
3. The preparation process of the highly compatible modified slurry according to claim 1, wherein the mass ratio of the conductive agent, the dopant and the solvent is 0.005-0.3: 0.005-0.2: 1.
4. The process for preparing high compatible modified slurry according to any one of claims 1 to 3, wherein the carbon source comprises at least one of glucose, sucrose, or phenolic resin; the dispersing agent comprises at least one of polyvinylpyrrolidone, polyethylene glycol, isobutanol, cyclohexanol or paraffin oil; the complexing agent comprises at least one of citric acid, oxalic acid, lactic acid, tartaric acid or ethylenediamine tetraacetic acid; the solvent comprises at least one of water, ethanol, or propanol.
5. The process for preparing high compatible modified slurry according to any one of claims 1 to 3, wherein the conductive agent comprises at least one of a spherical conductive agent, a linear conductive agent or a flake conductive agent; the dopant includes at least one of aluminum phosphate, cobalt phosphate, phosphomolybdic acid, lanthanum phosphate, or manganese phosphate.
6. A high-compatibility modified slurry obtained by the preparation process according to any one of claims 1 to 5.
7. The use of the high compatible modified slurry according to claim 6 in a positive electrode material.
8. A preparation process of a lithium iron phosphate anode material is characterized by comprising the following steps: and (3) blending a lithium source and iron phosphate with the high-compatibility modified slurry as claimed in claim 6, and then carrying out homogenization, grinding, spraying, sintering, gas breaking and demagnetizing treatment to obtain the modified lithium iron phosphate cathode material.
9. The preparation process of the lithium iron phosphate cathode material according to claim 8, wherein the mass ratio of the high-compatibility modified slurry to the lithium source to the iron phosphate is 0.1-0.5: 0.2-0.3: 1.
10. The lithium iron phosphate positive electrode material obtained by the preparation process according to claim 8 or 9.
CN202210094471.8A 2022-01-26 2022-01-26 High-compatibility modified slurry, preparation method and application in positive electrode material Pending CN114447286A (en)

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