CN104466136A - Preparation method of composite positive material of high-power lithium ion battery - Google Patents

Preparation method of composite positive material of high-power lithium ion battery Download PDF

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Publication number
CN104466136A
CN104466136A CN201410792965.9A CN201410792965A CN104466136A CN 104466136 A CN104466136 A CN 104466136A CN 201410792965 A CN201410792965 A CN 201410792965A CN 104466136 A CN104466136 A CN 104466136A
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composite positive
lithium ion
ion battery
aniline
active material
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CN104466136B (en
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高淑萍
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Lih Yuan Electronic Co., Ltd.
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高淑萍
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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
    • H01M4/362—Composites
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
    • 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
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
    • H01M4/623—Binders being polymers fluorinated polymers
    • 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
    • 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

Abstract

The invention relates to a preparation method of a composite positive material of a high-power lithium ion battery. The preparation method comprises the following steps: (1) preparing a cobalt-nickel active material; (2) preparing a conductive polymer; and (3) preparing the composite positive material. According to the prepared composite positive material, the nickel-cobalt material with high nickel content is used as a main active substance of the positive material, so that the energy density of the material is relatively high, then the conductive polymer of sulfide poly(aniline-co-pyrrole) with high energy density and good conductive performance is compounded, and finally the positive material with high capacity and good cycle stability can be obtained. When the composite material is used for the lithium ion battery, the lithium ion battery has the characteristics of high capacity and long service life.

Description

A kind of preparation method of high capacity lithium ion battery composite positive pole
Technical field
The present invention relates to a kind of preparation method of high capacity lithium ion battery composite positive pole.
Background technology
In recent decades, along with developing rapidly of battery industry, the specific energy of secondary cell is also improving constantly, from 30 ~ 40Wh/kg of lead-acid battery, 40 ~ 50Wh/kg of nickel-cadmium cell, 60 ~ 80Wh/kg of Ni-MH battery, develops into nineteen nineties commercial lithium ion battery and reaches 100 ~ 130Wh/kg, now reach 200Wh/kg.
Along with people's craving for high-energy-density power supply, in the urgent need to the development & application of cheapness, safety, environmental protection and high performance secondary cell.At present, lithium-ions battery has the good feature of high-energy-density, high-specific-power and high-temperature behavior because of it, is generally subject to people and welcomes.
And the key that limiting lithium ion cell specific capacity improves to be the specific capacity of positive electrode too low, and the specific capacity difficulty increasing substantially positive electrode is comparatively large, be thus improve the very important aspect of of lithium secondary battery chemical property for the research of cell positive material.And be subject to the restriction of theoretical specific capacity, it is unpractical for improving its specific capacity further, and exploitation has high power capacity and good reversible positive pole raw material just seem particularly crucial and urgent.
Summary of the invention
The invention provides a kind of preparation method of high capacity lithium ion battery composite positive pole, the positive electrode using the method to prepare, has large energy density and cyclical stability.
To achieve these goals, the invention provides a kind of preparation method of high capacity lithium ion battery composite positive pole, the method comprises the steps:
(1) cobalt nickel active material is prepared
The chemical formula of this cobalt nickel active material is Li 1.02ni 1-x-yco xnb yo 2, wherein: x=0.22-0.24, y=0.05-0.10;
Solid sintering technology is adopted to prepare above-mentioned active material Li 1.02ni 1-x-yco xnb yo 2:
By lithium carbonate, nickel hydroxide, cobalt hydroxide and niobium hydroxide according to being placed in tube furnace after the mol ratio=1.02:1-x-y:x:y ball milling mixing fully of Li:Ni:Co:Nb, under oxygen atmosphere, roasting 8-10h at 700-750 DEG C, Temperature fall is to room temperature, ball milling sieves, obtained active material Li 1.02ni 1-x-yco xnb yo 2;
(2) conducting polymer is prepared
By gather (aniline-pyrroles) powder, purity higher than 99% sulphur powder and anhydrous propanone add ball mill ball with 300-400r/min turn attainment mill 20-30min after, obtain mixed material, wherein the mass ratio of poly-(aniline-pyrroles) powder, sulphur powder and acetone is: 10:1-3:10-15;
The mixed material obtained is loaded in tube furnace, argon gas deaeration is passed into glass boat, and 160-180 DEG C is heated to the heating rate of 5-10 DEG C/min under argon atmosphere, and be incubated 3-4h at such a temperature, then 250-280 DEG C is heated to the heating rate of 15-20 DEG C/min, and after being incubated 2-3h at such a temperature, the conducting polymer of obtained sulfuration poly-(aniline-pyrroles);
(3) composite positive pole is prepared
After above-mentioned positive electrode active materials, above-mentioned conducting polymer, acetylene black and PVDF being mixed according to mass ratio 100:15-20:3-5:20-25, after putting into ball mill ball milling 1-2h, obtain composite positive pole of the present invention.
Composite positive pole prepared by the present invention, adopt the nickel cobalt lithium material with high nickel content as the main active substances of positive electrode, the energy density of material is made to be in higher degree, and then compound enters to have the conducting polymer of the sulfuration poly-(aniline-pyrroles) of high-energy-density and excellent conductive performance, finally obtain Large Copacity and the good positive electrode of cyclical stability.This composite material, when for lithium ion battery, has the feature of Large Copacity and long life.
Embodiment
embodiment one
Solid sintering technology is adopted to prepare above-mentioned active material Li 1.02ni 0.73co 0.22nb 0.05o 2.By lithium carbonate, nickel hydroxide, cobalt hydroxide and niobium hydroxide according to being placed in tube furnace after the mol ratio=1.02:0.73:0.22:0.05 ball milling mixing fully of Li:Ni:Co:Nb, under oxygen atmosphere, roasting 10h at 700 DEG C, Temperature fall is to room temperature, ball milling sieves, obtained active material Li 1.02ni 0.73co 0.22nb 0.05o 2;
By gather (aniline-pyrroles) powder, purity higher than 99% sulphur powder and anhydrous propanone add ball mill ball with 300r/min turn attainment mill 30min after, obtain mixed material, wherein the mass ratio of poly-(aniline-pyrroles) powder, sulphur powder and acetone is: 10:1:10.
The mixed material obtained is loaded in tube furnace; argon gas deaeration is passed into glass boat; and 160 DEG C are heated to the heating rate of 5 DEG C/min under argon atmosphere; and be incubated 4h at such a temperature; then 250 DEG C are heated to the heating rate of 15 DEG C/min; and after being incubated 3h at such a temperature, the conducting polymer of obtained sulfuration poly-(aniline-pyrroles).
After above-mentioned positive electrode active materials, above-mentioned conducting polymer, acetylene black and PVDF being mixed according to mass ratio 100:15:3:20, after putting into ball mill ball milling 1h, obtain composite positive pole of the present invention.
embodiment two
Solid sintering technology is adopted to prepare above-mentioned active material Li 1.02ni 0.66co 0.24nb 0.1o 2.By lithium carbonate, nickel hydroxide, cobalt hydroxide and niobium hydroxide according to being placed in tube furnace after the mol ratio=1.02:0.66:0.24:0.1 ball milling mixing fully of Li:Ni:Co:Nb, under oxygen atmosphere, roasting 8-10h at 700-750 DEG C, Temperature fall is to room temperature, ball milling sieves, obtained active material Li 1.02ni 0.66co 0.24nb 0.1o 2;
By gather (aniline-pyrroles) powder, purity higher than 99% sulphur powder and anhydrous propanone add ball mill ball with 400r/min turn attainment mill 20min after, obtain mixed material, wherein the mass ratio of poly-(aniline-pyrroles) powder, sulphur powder and acetone is: 10:3:15.
The mixed material obtained is loaded in tube furnace; argon gas deaeration is passed into glass boat; and 180 DEG C are heated to the heating rate of 10 DEG C/min under argon atmosphere; and be incubated 3h at such a temperature; then 280 DEG C are heated to the heating rate of 20 DEG C/min; and after being incubated 2h at such a temperature, the conducting polymer of obtained sulfuration poly-(aniline-pyrroles).
After above-mentioned positive electrode active materials, above-mentioned conducting polymer, acetylene black and PVDF being mixed according to mass ratio 100:20:5:25, after putting into ball mill ball milling 2h, obtain composite positive pole of the present invention.
comparative example
By 4.064 g Fe 2(SO 4) 39H 2o, 5.516 g LiNO 3be dissolved in 10 mL deionized waters, stir about 4 h, then in above-mentioned solution, dropwise drip the NH that concentration is 0.08 mol 4h 2pO 4the aqueous solution 10 mL, obtains colloidal sol.Meanwhile, in this colloidal sol, 15.8536 g acetylene blacks are added., under the condition of constant temperature 50 DEG C, in this colloidal sol, dropwise drip 2 mL expoxy propane, control colloidal sol pH value over time rate ( pH/min) be 2 ~ 2.4, obtain the gel of the homodisperse g., jelly-like of each predecessor component.By aging for this gel 1 h, then at 200 DEG C of drying 1 h, obtain LiFePO 4head product.Finally, at Ar/H 2(H in gaseous mixture 2volume fraction be 10 %), 800 DEG C calcining LiFePO 4head product 0.5 h obtains end-product LiFePO 4/ C.By the LiFePO of preparation 4/ C is used as anode material for lithium-ion batteries, is mixed to get composite positive pole with acetylene black, PVDF according to the ratio of mass ratio 75:15:10.
Above-described embodiment one, two and comparative example products therefrom being coated in respectively on Copper Foil, is to pole with metal lithium sheet, is to electrode with lithium sheet, and Celgard 2340 polypropylene screen is barrier film, 1 M LiPF 6/ EC+DMC (EC:DMC=1:1) is electrolyte, in the glove box being full of argon gas, be assembled into button cell.Be carry out electric performance test under the environment of 20 DEG C at probe temperature, after tested this embodiment one with two material compared with the product of comparative example, specific capacity improves 35-40% first, and useful life brings up to more than 60%.

Claims (1)

1. a preparation method for high capacity lithium ion battery composite positive pole, the method comprises the steps:
(1) cobalt nickel active material is prepared
The chemical formula of this cobalt nickel active material is Li 1.02ni 1-x-yco xnb yo 2, wherein: x=0.22-0.24, y=0.05-0.10;
Solid sintering technology is adopted to prepare above-mentioned active material Li 1.02ni 1-x-yco xnb yo 2:
By lithium carbonate, nickel hydroxide, cobalt hydroxide and niobium hydroxide according to being placed in tube furnace after the mol ratio=1.02:1-x-y:x:y ball milling mixing fully of Li:Ni:Co:Nb, under oxygen atmosphere, roasting 8-10h at 700-750 DEG C, Temperature fall is to room temperature, ball milling sieves, obtained active material Li 1.02ni 1-x-yco xnb yo 2;
(2) conducting polymer is prepared
By gather (aniline-pyrroles) powder, purity higher than 99% sulphur powder and anhydrous propanone add ball mill ball with 300-400r/min turn attainment mill 20-30min after, obtain mixed material, wherein the mass ratio of poly-(aniline-pyrroles) powder, sulphur powder and acetone is: 10:1-3:10-15;
The mixed material obtained is loaded in tube furnace, argon gas deaeration is passed into glass boat, and 160-180 DEG C is heated to the heating rate of 5-10 DEG C/min under argon atmosphere, and be incubated 3-4h at such a temperature, then 250-280 DEG C is heated to the heating rate of 15-20 DEG C/min, and after being incubated 2-3h at such a temperature, the conducting polymer of obtained sulfuration poly-(aniline-pyrroles);
(3) composite positive pole is prepared
After above-mentioned positive electrode active materials, above-mentioned conducting polymer, acetylene black and PVDF being mixed according to mass ratio 100:15-20:3-5:20-25, after putting into ball mill ball milling 1-2h, obtain composite positive pole of the present invention.
CN201410792965.9A 2014-12-20 2014-12-20 Preparation method of composite positive material of high-power lithium ion battery Active CN104466136B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006147500A (en) * 2004-11-24 2006-06-08 Sumitomo Metal Mining Co Ltd Positive electrode active material for non-aqueous electrolyte secondary battery, its manufacturing method, and non-aqueous electrolyte secondary battery using this
CN101278424A (en) * 2005-08-01 2008-10-01 株式会社三德 Positive electrode active material, positive electrode for nonaqueous electrolyte battery, and nonaqueous electrolyte battery
CN101740758A (en) * 2010-01-04 2010-06-16 北京航空航天大学 Preparation method of vulcanized conducting polymer composite anode for lithium ion battery
KR101001567B1 (en) * 2005-04-11 2010-12-17 히다치 막셀 가부시키가이샤 Lithium ion secondary battery
CN102005604A (en) * 2009-08-20 2011-04-06 株式会社东芝 Non-aqueous electrolyte battery, battery pack and vehicle

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006147500A (en) * 2004-11-24 2006-06-08 Sumitomo Metal Mining Co Ltd Positive electrode active material for non-aqueous electrolyte secondary battery, its manufacturing method, and non-aqueous electrolyte secondary battery using this
KR101001567B1 (en) * 2005-04-11 2010-12-17 히다치 막셀 가부시키가이샤 Lithium ion secondary battery
CN101278424A (en) * 2005-08-01 2008-10-01 株式会社三德 Positive electrode active material, positive electrode for nonaqueous electrolyte battery, and nonaqueous electrolyte battery
CN102005604A (en) * 2009-08-20 2011-04-06 株式会社东芝 Non-aqueous electrolyte battery, battery pack and vehicle
CN101740758A (en) * 2010-01-04 2010-06-16 北京航空航天大学 Preparation method of vulcanized conducting polymer composite anode for lithium ion battery

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