WO2012062110A1 - Procédé de préparation d'un composite phosphate de fer lithié/carbone pour pile lithium-ion - Google Patents

Procédé de préparation d'un composite phosphate de fer lithié/carbone pour pile lithium-ion Download PDF

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Publication number
WO2012062110A1
WO2012062110A1 PCT/CN2011/075932 CN2011075932W WO2012062110A1 WO 2012062110 A1 WO2012062110 A1 WO 2012062110A1 CN 2011075932 W CN2011075932 W CN 2011075932W WO 2012062110 A1 WO2012062110 A1 WO 2012062110A1
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WIPO (PCT)
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iron phosphate
lithium iron
graphene
carbon
ion battery
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PCT/CN2011/075932
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English (en)
Chinese (zh)
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朱杰
杜振山
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河北力滔电池材料有限公司
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Publication of WO2012062110A1 publication Critical patent/WO2012062110A1/fr

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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
    • 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
    • H01M4/58—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
    • 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
    • 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

Definitions

  • the invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a lithium ion battery composite material lithium iron phosphate/carbon. Background technique
  • the synthesis method of lithium iron phosphate material is mainly divided into a solid phase method and a liquid phase method.
  • the solid phase method mainly utilizes iron salt, lithium salt and phosphate to synthesize lithium iron phosphate at high temperature sintering.
  • a soluble iron salt, a lithium salt, and a phosphoric acid salt are dissolved in a solvent, and lithium iron phosphate or a precursor thereof is prepared by ion reaction, and then a high-temperature sintering is performed to obtain a finished product.
  • the solid phase reaction is simple, the raw materials are easy to handle, and the yield is high, but the morphology of the raw materials is not easy to control, and the tap density and compaction density of the product are low.
  • the invention patents CN101200289, CN1762798, CN101140985, etc. all adopt a solid phase synthesis process route.
  • Some new synthetic methods such as microwave synthesis (CN101172597, CN101807692A) and ultrasonic coprecipitation (CN101800311A), can be attributed to solid phase synthesis.
  • the liquid phase method requires the use of a reactor for pre-treatment, and also requires drying, filtration, etc., and the process is complicated.
  • the sphericity of the product is generally good, the tap density is high, and the capacity and high rate performance are excellent.
  • the invention patents CN101172599, CN101047242, and CN101121509 all adopt the above process route.
  • iron phosphate materials are coated with a conductive carbon layer. It is actually a lithium iron phosphate/carbon composite. Only the lithium iron phosphate material coated with carbon can exert its electrochemical performance normally. However, the carbon added by the general process is loosely distributed and loosely distributed among the lithium iron phosphate particles, which seriously reduces the bulk density of the lithium iron phosphate material, making its tap density much lower than its theoretical density, and affecting the subsequent The compact density of the pole piece. How to minimize the carbon content in the cathode material without reducing the carbon coating effect of the material, without reducing the conductivity, electrochemical capacity and cycle performance, is a concern of materials research. Summary of the invention
  • the present invention provides a method for preparing a lithium ion battery composite lithium iron phosphate/carbon in order to solve the problems existing in the prior art.
  • the object of the present invention is to provide a lithium ion battery composite lithium iron phosphate/carbon preparation method which has the advantages of simple process, convenient operation, excellent material performance, high electrical conductivity, high bulk density and high compaction density, and stable product quality.
  • Graphene is extremely thin, very soft and has excellent flexibility. It is an ideal material for coating lithium iron phosphate. It is conceivable that the lithium iron phosphate material coated with an appropriate amount of graphene has a small carbon content, but the electrical conductivity of the material is lowered. At the same time, since the graphene is tightly coated on the surface of the lithium iron phosphate particles, there is no loose carbon between the grains, and the density of the material is greatly increased.
  • the invention provides a preparation and synthesis method of a lithium iron phosphate/carbon composite material, wherein carbon is tightly coated on the surface of lithium iron phosphate in the form of graphene, thereby reducing the carbon content in the positive electrode material to less than 1% (in general materials) Containing more than 3% carbon), the material is densely distributed, increasing the density of lithium iron phosphate material.
  • the process route adopted by the invention is as follows: Firstly, a graphene stable dispersion aqueous solution system is prepared by using a thermal differential layer stripping technique, and then the pure lithium iron phosphate material is treated with the solution to adsorb the graphene on the surface of the lithium iron phosphate particles, and then subjected to heat treatment. The combination of graphene and lithium iron phosphate provides the desired lithium iron phosphate/carbon composite.
  • the preparation method of the lithium ion battery composite material lithium iron phosphate/carbon of the invention adopts the following technical solutions:
  • a lithium ion battery composite material lithium iron phosphate / carbon preparation method, coated with lithium iron phosphate, characterized by: composite lithium iron phosphate / carbon preparation process includes:
  • Preparing a suspended graphene dispersed aqueous solution system preparing a suspended graphene dispersed aqueous solution system by using a hot differential layer stripping method; pulverizing the natural graphite to a particle size of 1-5 micrometers, and adding it to steamed water or purified water. Adding 0.1-5% of the surfactant, under shear and stirring, the temperature of the seal is raised to 180-250 ° C, stirred for 2-6 hours, and the temperature is lowered;
  • the preparation method of the lithium ion battery composite material lithium iron phosphate/carbon of the invention can also adopt the following technical measures:
  • the preparation method of the lithium ion battery composite material lithium iron phosphate/carbon characterized in that: the surfactant is phenylenediamine , polyvinylpyrrolidone, alkylphenol ethoxylates, and the like. It can be peeled off between the graphite layers in the hydrothermal state and stabilizes the graphene/water system.
  • the preparation method of the lithium ion battery composite material lithium iron phosphate/carbon is characterized in that: the coupling agent is Y-mercaptopropyltrimethoxysilane, methyl isobutyl ketone decyl silane, vinyl triethoxy Silane and the like. It can adhere to the surface of lithium iron phosphate and is easily crosslinked with graphene.
  • the method for preparing a lithium ion battery composite lithium iron phosphate/carbon is characterized in that: the weight percentage concentration of graphene in the graphene-dispersed aqueous solution is ⁇ - ⁇ %.
  • the method for preparing a lithium ion battery composite material lithium iron phosphate/carbon characterized in that: adding graphene dispersion After the aqueous solution, the mixture was stirred at 20 to 40 ° C for 4 to 10 hours, and then allowed to stand for 12 to 36 hours, followed by stirring.
  • the lithium ion battery composite material lithium iron phosphate / carbon preparation method is characterized in that: when the solid powder is dried by vacuum, the vacuum drying temperature is 120-150 ° C.
  • Lithium ion battery composite material lithium iron phosphate / carbon preparation method due to the adoption of the novel technical solution of the present invention, compared with the prior art, the iron phosphate/carbon material prepared by the invention, the graphene is completely nanometerly distributed in the phosphoric acid
  • the surface of the iron-lithium material forms a surface carbon layer with extremely high electrical conductivity and does not produce a loose bulk carbon layer.
  • the bulk density and compaction density of the lithium iron phosphate cathode material are effectively increased. ⁇
  • the measured, the carbon content of the material was reduced to 0. 8-1%, the body conductivity was maintained at 0. 01S / cm.
  • the tap density is increased to 1. 8g/cm3, the 0.
  • 1C capacity is 155mAh/g
  • the compact density of the capacity pole piece is increased from 2. 2 g/cm3 to 2. 6-2. 7 g/cm3.
  • the overall performance of the lithium iron phosphate material has been greatly improved.
  • the invention has the advantages of simple process, convenient operation, excellent material performance, high electrical conductivity, high bulk density and compact density, and stable product quality. detailed description
  • a method for preparing a lithium ion battery composite lithium iron phosphate/carbon firstly preparing a stable suspended graphene-water system.
  • the concentration of graphene in the system is 1%.
  • the natural graphite is first pulverized to an average particle size of about 1 micrometer, and then added to the distilled water, and 0.1% of the surfactant phenylenediamine is added, and the temperature is raised to 180 ° C under high shear agitation. Stirring was continued for 6 hours under high temperature and high pressure, and the temperature was lowered to obtain a stable suspended graphene-water system.
  • a method for preparing a lithium ion battery composite lithium iron phosphate/carbon firstly preparing a stable suspended graphene-water system.
  • the concentration of graphene in the system is generally 10%.
  • the natural graphite was first pulverized to an average particle size of 5 ⁇ m, and then added to purified water, and 5% of a surfactant polyvinylpyrrolidone was added, and the temperature was raised to 250 ° C under high-speed shear stirring. Stirring was continued for 2 hours under high temperature and high pressure, and the temperature was lowered to obtain a stable suspended graphene-water system.
  • a method for preparing a lithium ion battery composite lithium iron phosphate/carbon firstly preparing a stable suspended graphene-water system.
  • the concentration of graphene in the system was 2%.
  • the natural graphite was first pulverized to an average particle diameter of 2 ⁇ m, and then added to pure water, and 1% of a surfactant alkylphenol ethoxylate was added, and the temperature was raised to 200 ° C under high-speed shear stirring. Stirring was continued for 4 hours under high temperature and high pressure, and the temperature was lowered to obtain a stable suspended graphene-water system.
  • the lithium iron phosphate/carbon composite material of the lithium ion battery prepared by the invention has the graphene completely distributed on the surface of the lithium iron phosphate material, forming a surface carbon layer having extremely high conductivity, and effectively increasing the lithium iron phosphate positive electrode.
  • the bulk density and compaction density of the material, the lithium iron phosphate/carbon composite material has the positive positive effects described.

Abstract

L'invention concerne un procédé de préparation d'un composite phosphate de fer lithié/carbone pour une pile lithium-ion. Le procédé selon l'invention comprend les étapes suivantes : 1) préparation d'une solution aqueuse à graphène dispersé en suspension : broyage d'un graphite jusqu'à 1-5μm, ajout d'eau distillée ou d'eau purifiée, ajout de 0,1-5% d'un tensio-actif sous agitation, augmentation de la température à 180-250℃ dans des conditions d'étanchéité, agitation pendant 2-6 heures et refroidissement; 2) broyage d'un phosphate de fer lithié jusqu'à 1-5μm, ajout d'eau distillée ou d'eau purifiée, ajout de 0,01-1% d'un agent de couplage sous agitation, agitation uniforme, ajout de la solution à graphène dispersé, agitation et filtrage; 3) séchage sous vide de la poudre solide obtenue lors du filtrage, frittage pendant 2 à 12 heures et obtention du matériau positif phosphate de fer lithié à revêtement graphène. Ce procédé utilise une technique simple et le matériau préparé par ce procédé présente avantageusement d'excellentes performances, une conductivité élevée, un empilement important, une forte intensité de compactage, etc.
PCT/CN2011/075932 2010-11-10 2011-06-20 Procédé de préparation d'un composite phosphate de fer lithié/carbone pour pile lithium-ion WO2012062110A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201010537386.1 2010-11-10
CN2010105373861A CN102013477B (zh) 2010-11-10 2010-11-10 一种锂离子电池复合材料磷酸铁锂/碳的制备方法

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CA2754372A1 (fr) 2011-10-04 2013-04-04 Hydro-Quebec Materiau d'electrode positive pour batterie secondaire au lihium-ion et methode de production connexe
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CN103427072A (zh) * 2012-05-16 2013-12-04 上海宝钢磁业有限公司 一种磷酸铁锂原位碳包覆方法
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CN105762345B (zh) * 2016-04-29 2019-03-29 湖北金泉新材料有限责任公司 一种复合正极材料、其制备方法和锂离子电池
CN106711447A (zh) * 2016-12-19 2017-05-24 重庆汉岳科技发展有限公司 一种复合型石墨烯锂电池正极材料的制备方法
CN106711425A (zh) * 2017-01-12 2017-05-24 江苏海四达电源股份有限公司 改性磷酸铁锂及其制备方法和应用以及正极材料和锂离子电池
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