CN112751000A - Process method for coating nickel cobalt lithium manganate with zirconium carbide - Google Patents

Process method for coating nickel cobalt lithium manganate with zirconium carbide Download PDF

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CN112751000A
CN112751000A CN202011598063.3A CN202011598063A CN112751000A CN 112751000 A CN112751000 A CN 112751000A CN 202011598063 A CN202011598063 A CN 202011598063A CN 112751000 A CN112751000 A CN 112751000A
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zirconium carbide
nickel cobalt
lithium manganate
cobalt lithium
carbide powder
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CN112751000B (en
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赵春阳
钱飞鹏
李佳军
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Wuxi Jewel Power & Materials Co ltd
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Wuxi Jewel Power & Materials Co ltd
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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
    • H01M4/36—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
    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/52—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
    • H01M4/36—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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a process method for coating nickel cobalt lithium manganate with zirconium carbide, which comprises the steps of selecting zirconium carbide powder with the particle size of D502-5 mu m, putting the zirconium carbide powder into a planetary ball mill for ball milling, wherein the ball milling material ball ratio is 1:1, mixing and coating the zirconium carbide powder, so that the zirconium carbide powder can have a smaller particle size and can be conveniently adsorbed to the surface of the nickel cobalt lithium manganate; a wet coating and spray drying process is adopted to ensure that the coating agent and the nickel cobalt lithium manganate can be uniformly distributed; the process temperature and time adopted by sintering can ensure that zirconium carbide and nickel cobalt lithium manganate can be effectively combined; the good coating effect can effectively improve the circulation, the multiplying power and the safety performance of the nickel cobalt lithium manganate product.

Description

Process method for coating nickel cobalt lithium manganate with zirconium carbide
Technical Field
The invention relates to a process method of zirconium carbide coated nickel cobalt lithium manganate.
Background
The nickel cobalt lithium manganate material has high research value and improvement space as a novel power type lithium ion battery anode material, and currently, the field of lithium cobalt oxide, nickel cobalt lithium manganate, lithium iron phosphate, lithium manganate, lithium aluminate and other materials are generally adopted in the lithium ion battery anode material field, and the materials are emphasized in performance, so that the nickel cobalt lithium manganate material (LiNixCoyMn1-x-yO2) has higher capacity, multiplying power, circulation, high temperature and other properties, but the safety performance of the nickel cobalt lithium manganate material always limits the further development of the nickel cobalt lithium manganate material.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide a method.
In order to solve the technical problems, the invention provides the following technical scheme:
a process method for coating nickel cobalt lithium manganate with zirconium carbide comprises the following steps:
s1, selecting zirconium carbide powder with the granularity D50 of about 2-5 mu m, putting the zirconium carbide powder into a planetary ball mill for ball milling, and mixing the zirconium carbide powder and the ball milling material in a ball milling ratio of 1: 1; mixing at 1500 +/-200R/min for 3-5 h. Preferably, 1500R/min, and mixing for 4 h; the granularity of the coating agent zirconium carbide is different from that of the coating agents such as magnesium oxide, aluminum oxide, zirconium oxide and the like which are used for coating in the prior art;
s2, sieving, separating out zirconium carbide powder, weighing the weight which is about 800-1200ppm of the amount of the nickel-cobalt lithium manganate to be coated;
s3, putting the weighed zirconium carbide powder into an organic solvent, wherein the organic solvent is ethylene glycol, or nitrobenzene, bromobenzene, carbon tetrachloride, chloroform, bromohydrocarbon, glycerol and the like), the coating agent accounts for 0.8-1.2% and preferentially accounts for 1%, a small amount of dispersant is added, and the zirconium carbide powder is effectively dispersed by magnetic stirring for later use;
s4, adding a certain amount of nickel cobalt lithium manganate material into the purified water, and dispersing at a high speed, wherein the dispersion speed is 1000 +/-100R/min, and the dispersion speed is 20-40 min. Preferably, the high-speed dispersion is 1000R/min and 30 min.
S5, adding the prepared solid-liquid mixture, and continuing to perform high-speed mixing and dispersing, wherein the high-speed dispersing is preferably performed for 50-70 min and is performed for 60 min;
s6, placing the mixture into a spray tower, heating the mixture to 230 ℃ at 200 ℃ and then carrying out spray drying;
s7, sintering the sprayed powder at the high temperature of 920 and 950 ℃ for 4 h;
and S8, naturally cooling, taking out the sinter, crushing, screening and packaging to obtain the material.
The coating agent zirconium carbide is effectively attached to the surface of the nickel cobalt lithium manganate, the problem of uniform distribution of two substances is solved, and the sintering temperature and time can directly influence the coating effect.
Has the advantages that:
according to the invention, the coating agent zirconium carbide is effectively subjected to ball milling and dispersion, so that the coating agent zirconium carbide can have a smaller particle size, and is convenient to adsorb on the surface of nickel cobalt lithium manganate; a wet coating and spray drying process is adopted to ensure that the coating agent and the nickel cobalt lithium manganate can be uniformly distributed; the process temperature and time adopted by sintering can ensure that zirconium carbide and nickel cobalt lithium manganate can be effectively combined; the good coating effect can effectively improve the circulation, the multiplying power and the safety performance of the nickel cobalt lithium manganate product.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is an SEM of the coated nickel cobalt lithium manganate 15.kV 11.4mm 2.00K produced in the examples;
FIG. 2 is an SEM of the coated nickel cobalt lithium manganate produced in the examples 15.kV 11.4mm 5.00K;
FIG. 3 is an SEM of the coated nickel cobalt lithium manganate produced in the examples 15.kV 11.4mm 10.00K;
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Examples
A process method for coating nickel cobalt lithium manganate with zirconium carbide comprises the following steps:
s1, selecting zirconium carbide powder with the particle size D50 of about 2-5 microns, putting the zirconium carbide powder into a planetary ball mill for ball milling, wherein the ball milling material-ball ratio is 1:1, and mixing for 4 hours at 1500R/min;
s2, sieving, separating out zirconium carbide powder, weighing the weight which is about 800-1200ppm of the amount of the nickel-cobalt lithium manganate to be coated;
s3, putting the weighed zirconium carbide powder into an organic solvent ethylene glycol, wherein the coating agent accounts for about 1%, adding a small amount of dispersant, and effectively dispersing by magnetic stirring for later use;
s4, adding a quantitative nickel cobalt lithium manganate material into the purified water, and dispersing at a high speed for 1000R/min for 30 min;
s5, adding the prepared solid-liquid mixture, and continuing to perform high-speed mixing and dispersing for 60 min;
s6, placing the mixture into a spray tower, heating the mixture to 230 ℃ at 200 ℃ and then carrying out spray drying;
s7, sintering the sprayed powder at the high temperature of 920 and 950 ℃ for 4 h;
and S8, naturally cooling, taking out the sinter, crushing, screening and packaging to obtain the required product.
Fig. 1 is an SEM of coated nickel cobalt lithium manganate 15.kV 11.4mm 2.00K produced in example, fig. 2 is an SEM of coated nickel cobalt lithium manganate 15.kV 11.4mm 5.00K produced in example, and fig. 3 is an SEM of coated nickel cobalt lithium manganate 15.kV 11.4mm 10.00K produced in example.
The good coating effect can effectively improve the circulation, the multiplying power and the safety performance of the nickel cobalt lithium manganate product. According to the current implementation results, the cycle can be improved to 80% of the normal temperature 1C cycle after 1500 weeks, and the rate performance can be improved to 30C.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. 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 (5)

1. A process method for coating nickel cobalt lithium manganate with zirconium carbide is characterized by comprising the following steps:
s1, selecting zirconium carbide powder with the particle size D502-5 mu m, putting the zirconium carbide powder into a planetary ball mill for ball milling, and mixing the zirconium carbide powder and the ball milling material in a ball milling ratio of 1: 1;
s2, sieving, separating out zirconium carbide powder, weighing the weight of the zirconium carbide powder, wherein the usage amount of the zirconium carbide powder is 800-1200ppm of the amount of the nickel-cobalt lithium manganate required to be coated;
s3, putting the weighed zirconium carbide powder into an organic solvent, wherein the coating agent accounts for 0.8-1.2%, adding a small amount of dispersing agent, and performing effective dispersion through magnetic stirring for later use;
s4, adding a certain amount of nickel cobalt lithium manganate material into the purified water, and dispersing at a high speed;
s5, adding the prepared solid-liquid mixture, and continuing to perform high-speed mixing and dispersing;
s6, placing the mixture into a spray tower, heating the mixture to 230 ℃ at 200 ℃ and then carrying out spray drying;
s7, sintering the sprayed powder at the high temperature of 920 and 950 ℃ for 4 h;
and S8, naturally cooling, taking out the sinter, crushing, screening and packaging to obtain the material.
2. The process method of claim 1, wherein the zirconium carbide coated lithium nickel cobalt manganese oxide is mixed in S1 at 1500 + -200R/min for 3-5 h.
3. The process of claim 1, wherein the organic solvent in S3 is any one of ethylene glycol, nitrobenzene, bromobenzene, carbon tetrachloride, chloroform, bromohydrocarbon or glycerol.
4. The process method of claim 1, wherein the high-speed dispersion in S4 is 1000 +/-100R/min for 20-40 min.
5. The process method of claim 1, wherein the zirconium carbide coated lithium nickel cobalt manganese oxide is dispersed at a high speed in S5 for 50-70 min.
CN202011598063.3A 2020-12-29 2020-12-29 Process method for coating nickel cobalt lithium manganate with zirconium carbide Active CN112751000B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115498166A (en) * 2022-10-19 2022-12-20 楚能新能源股份有限公司 Ternary cathode material, preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101070148A (en) * 2007-05-22 2007-11-14 无锡市凯天星电光材料有限公司 Method for preparing lithium iron phosphate as lithium ion cell positive-pole material
CN101217195A (en) * 2007-12-28 2008-07-09 龚思源 A lithium ion battery anode material of lithium iron phosphate and the corresponding vapor deposition and cladding method of conductive network
CN108258209A (en) * 2017-12-27 2018-07-06 温州大学 A kind of carbide/carbon nano tube/graphene carries sulphur composite material and preparation method and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101070148A (en) * 2007-05-22 2007-11-14 无锡市凯天星电光材料有限公司 Method for preparing lithium iron phosphate as lithium ion cell positive-pole material
CN101217195A (en) * 2007-12-28 2008-07-09 龚思源 A lithium ion battery anode material of lithium iron phosphate and the corresponding vapor deposition and cladding method of conductive network
CN108258209A (en) * 2017-12-27 2018-07-06 温州大学 A kind of carbide/carbon nano tube/graphene carries sulphur composite material and preparation method and application

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115498166A (en) * 2022-10-19 2022-12-20 楚能新能源股份有限公司 Ternary cathode material, preparation method and application thereof
CN115498166B (en) * 2022-10-19 2024-01-30 楚能新能源股份有限公司 Ternary positive electrode material, preparation method and application thereof

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