CN104538599A - Preparation method of lithium cobalt oxide positive electrode material coated with silicon-modified conducting polymer - Google Patents

Preparation method of lithium cobalt oxide positive electrode material coated with silicon-modified conducting polymer Download PDF

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Publication number
CN104538599A
CN104538599A CN201510009564.6A CN201510009564A CN104538599A CN 104538599 A CN104538599 A CN 104538599A CN 201510009564 A CN201510009564 A CN 201510009564A CN 104538599 A CN104538599 A CN 104538599A
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conducting polymer
positive electrode
deionized water
mixed
purity
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高淑萍
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Yao Alian
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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
    • 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
    • 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 lithium cobalt oxide positive electrode material coated with a silicon-modified conducting polymer. The chemical formula of the lithium cobalt oxide positive electrode material is LiCo1-x-yMgxAlyO2, wherein x=0.15-0.2, and y=0.12-0.15. The preparation method comprises the steps of (1) preparing the lithium cobalt oxide positive electrode material, (2) preparing the silicon-modified conducting polymer, and (3) carrying out coating. The positive electrode material is prepared from the raw material of high-purity and high-density cobaltosic oxide, so that the energy density of the composite material is improved; the raw material is doped with Al and Mg to be modified, so that the substance activity is improved; finally, the positive electrode material is coated with the silicon-modified conducting polymer, so that the conductivity and stability of the positive electrode material are further improved.

Description

A kind of Si modification is to the preparation method of the coated lithium cobaltate cathode material of conducting polymer
Technical field
The present invention relates to the preparation method of a kind of Si modification to the coated lithium cobaltate cathode material of conducting polymer.
Background technology
Lithium battery is primarily of formations such as positive electrode, negative material, barrier film and electrolyte, positive electrode occupies the ratio of more than 40% in the total cost of lithium battery, and the performance of positive electrode directly affects the property indices of lithium battery, so lithium electricity positive electrode occupies core status in lithium battery.The lithium electricity positive electrode of the at present marketization comprises the products such as cobalt acid lithium, multicomponent material, LiMn2O4 and LiFePO 4, and cobalt acid lithium is that current production technology is the most ripe, battery performance is the most reliable and obtain the anode material for lithium-ion batteries of most broad commercial applications.。
But current business-like lithium ion battery is main still based on LiCoO 2deng the rocking chair mechanism of lithium ion inlay compound, positive electrode becomes the restriction of lithium ion battery energy density, and end-point energy density can only reach 400Wh/Kg.Under the prerequisite playing identical capacity, the volume energy density of battery be improved, just need improve the loading of cell active materials unit volume.Conventional cobalt acid lithium, multicomponent material, LiMn2O4 and LiFePO4 all can not obtain sufficiently high volume capacity density.Along with market is to the continuous pursuit of high volume energy density lithium battery, the charging voltage improving positive electrode becomes the focus of research.
Summary of the invention
The invention provides the preparation method of a kind of Si modification to the coated lithium cobaltate cathode material of conducting polymer, use positive electrode prepared by the method, while there is higher energy density, the cycle performance that also tool is good.
To achieve these goals, the invention provides the preparation method of a kind of Si modification to the coated lithium cobaltate cathode material of conducting polymer, wherein the chemical formula of this lithium cobaltate cathode material is LiCo 1-x-ymg xal yo 2, wherein: x=0.15-0.2, y=0.12-0.15, the method comprises the steps:
(1) lithium cobaltate cathode material is prepared
The cobalt nitrate of technical grade and ammonium acetate being mixed with these two kinds of material concentrations respectively with deionized water is 2-3M, the mixed solution of 0.5-1M, with deionized water, the potassium hydroxide of technical grade and ammoniacal liquor being made into these two kinds of material concentrations is 3-5M, the mixed solution of 1-2M, in the water-bath of 55-65 DEG C, above-mentioned two kinds of mixed solutions are joined in reaction vessel according to volume ratio 1:2-4 simultaneously, control pH value is 10-12, the precipitation ageing that reaction generates is precipitated, spend deionized water, then filter, dry, powder will be dried at 750-880 DEG C of temperature lower calcination 4-6h, obtain the high-density spherical cobaltic-cobaltous oxide of purity >=99.9%,
Take cobaltosic oxide prepared by lithia, said method that purity is greater than 99.5% according to the mole of Li, Co, Mg, Al in above-mentioned chemical formula, magnesium oxide that aluminium oxide, purity that purity is greater than 99.5% are greater than 99.5%, melt after the above-mentioned lithia, cobaltosic oxide, aluminium oxide and the magnesium oxide mechanical mixture that take at the temperature of 1300-1500 DEG C, ball grinds after cooling, at 850-900 DEG C, sinter 2-3h, obtain cobalt acid lithium;
(2) Si modification conducting polymer is prepared
Be 2-5 μm of Si powder by particle diameter, propylene carbonate is mixed to get mixture according to the ratio of mass ratio 1:5-10, described mixture and dispersant potassium phosphate are put into deionized water, wherein put into this mixture of 150-200g and 10-15g potassium phosphate in often liter of deionized water, obtain mixed liquor, described mixed liquor is stirred 15-20h with the speed of 100-150r/min in the water-bath of 65-70 DEG C, carries out polymerization reaction, filter, washing, dry, obtain Si modification conducting polymer;
(3) coated
By above-mentioned cobalt acid lithium with above-mentioned Si modification conducting polymer according to mass ratio 100:(12-16) together with join with rotating speed 300-400r/min ball milling 10-12h in planetary ball mill, drying;
Dried material is placed in argon gas atmosphere heat treatment, and heat treatment temperature is 150-250 DEG C, and insulation 3-4h, naturally cools to room temperature, pulverizes, sieves, obtain product.
Positive electrode prepared by the present invention, high-purity high-density cobaltosic oxide is adopted to be the energy density that raw material improves composite material, doped with Al, Mg modification are to improve species activity, and last coated Si modified conductive polymer improves conductivity and the stability of material further.Therefore this composite material is when for lithium ion battery, has higher specific capacity and longer useful life.
Embodiment
embodiment one
The chemical formula of lithium cobaltate cathode material prepared by the present embodiment is LiCo 0.73mg 0.15al 0.12o 2.
The cobalt nitrate of technical grade and ammonium acetate being mixed with these two kinds of material concentrations respectively with deionized water is 2M, the mixed solution of 0.5M, with deionized water, the potassium hydroxide of technical grade and ammoniacal liquor being made into these two kinds of material concentrations is 3M, the mixed solution of 1M, in the water-bath of 55 DEG C, above-mentioned two kinds of mixed solutions are joined in reaction vessel according to volume ratio 1:2 simultaneously, control pH value is 10-12, the precipitation ageing that reaction generates is precipitated, spend deionized water, then filter, dry, powder will be dried at 750 DEG C of temperature lower calcination 6h, obtain the high-density spherical cobaltic-cobaltous oxide of purity >=99.9%.
Take cobaltosic oxide prepared by lithia, said method that purity is greater than 99.5% according to the mole of Li, Co, Mg, Al in above-mentioned chemical formula, magnesium oxide that aluminium oxide, purity that purity is greater than 99.5% are greater than 99.5%, melt after the above-mentioned lithia, cobaltosic oxide, aluminium oxide and the magnesium oxide mechanical mixture that take at the temperature of 1300 DEG C, ball grinds after cooling, at 850 DEG C, sinter 3h, obtain cobalt acid lithium.
Be 2-5 μm of Si powder by particle diameter, propylene carbonate is mixed to get mixture according to the ratio of mass ratio 1:5, described mixture and dispersant potassium phosphate are put into deionized water, wherein put into this mixture of 150g and 10g potassium phosphate in often liter of deionized water, obtain mixed liquor, described mixed liquor is stirred 20h with the speed of 100r/min in the water-bath of 65 DEG C, carries out polymerization reaction, filter, washing, dry, obtain Si modification conducting polymer.
Above-mentioned cobalt acid lithium is joined with rotating speed 300r/min ball milling 12h in planetary ball mill with above-mentioned Si modification conducting polymer together with mass ratio 100:12, dry; Dried material is placed in argon gas atmosphere heat treatment, and heat treatment temperature is 150 DEG C, and insulation 4h, naturally cools to room temperature, pulverizes, sieves, obtain product.
embodiment two
The chemical formula of lithium cobaltate cathode material prepared by the present embodiment is LiCo 0.65mg 0.2al 0.15o 2.
The cobalt nitrate of technical grade and ammonium acetate being mixed with these two kinds of material concentrations respectively with deionized water is 3M, the mixed solution of 1M, with deionized water, the potassium hydroxide of technical grade and ammoniacal liquor being made into these two kinds of material concentrations is 5M, the mixed solution of 2M, in the water-bath of 65 DEG C, above-mentioned two kinds of mixed solutions are joined in reaction vessel according to volume ratio 1:4 simultaneously, controlling pH value is 12, the precipitation ageing that reaction generates is precipitated, spend deionized water, then filter, dry, powder will be dried at 880 DEG C of temperature lower calcination 4h, obtain the high-density spherical cobaltic-cobaltous oxide of purity >=99.9%.
Take cobaltosic oxide prepared by lithia, said method that purity is greater than 99.5% according to the mole of Li, Co, Mg, Al in above-mentioned chemical formula, magnesium oxide that aluminium oxide, purity that purity is greater than 99.5% are greater than 99.5%, melt after the above-mentioned lithia, cobaltosic oxide, aluminium oxide and the magnesium oxide mechanical mixture that take at the temperature of 1500 DEG C, ball grinds after cooling, at 900 DEG C, sinter 2h, obtain cobalt acid lithium.
Be 2-5 μm of Si powder by particle diameter, propylene carbonate is mixed to get mixture according to the ratio of mass ratio 1:10, described mixture and dispersant potassium phosphate are put into deionized water, wherein put into this mixture of 200g and 15g potassium phosphate in often liter of deionized water, obtain mixed liquor, described mixed liquor is stirred 15h with the speed of 150r/min in the water-bath of 70 DEG C, carries out polymerization reaction, filter, washing, dry, obtain Si modification conducting polymer.
Above-mentioned cobalt acid lithium is joined with rotating speed 400r/min ball milling 10h in planetary ball mill with above-mentioned Si modification conducting polymer together with mass ratio 100:16, dry; Dried material is placed in argon gas atmosphere heat treatment, and heat treatment temperature is 250 DEG C, and insulation 3h, naturally cools to room temperature, pulverizes, sieves, obtain product.
comparative example
First by nickelous sulfate, cobaltous sulfate and aluminum sulfate Ni in molar ratio 2+: Co 2+: Al 3+=0.75: 0.2: 0.05 aqueous solution being hybridly prepared into 2mol/L, is mixed with the aqueous solution of 3mol/L by ammonium persulfate, lithium hydroxide be mixed with the solution 2L of 5mol/L and add the ammoniacal liquor of 0.5L 1.5mol/L.Then by the mixing salt solution prepared and ammonium persulfate solution all with the flow velocity of 10ml/min and stream adds in the 12L reactor with agitating device, stir with the speed of 550rpm and be heated to 50 DEG C, regulate the charging rate of aqueous slkali to control the pH value of reaction system between 10.5-11, terminate after reaction 8h, then filter out spherical hydroxy nickel oxide cobalt aluminium presoma.Again spherical hydroxy nickel oxide cobalt aluminium is spent after deionized water filters 6 times, in 120 DEG C of vacuum drying chambers, dry 12h obtain presoma.Again by lithium hydroxide and presoma with 1.06: 1 ratio mix after, be placed in flowing pure oxygen atmosphere stove in 700 DEG C of roasting 10h, broken classification after cooling, obtains aluminum-doped nickel lithium carbonate for lithium material.
Adopt NMP as solvent above-described embodiment one, two and comparative example products therefrom, by active material: SP: PVDF=90: 5: 5 be mixed with solid content be 70% slurry be evenly coated on Al paper tinsel, make positive pole.Negative pole adopts deionized water as solvent, by graphite: SP: SBR: CMC=90: 4: 3: 3 to be mixed with solid content be that the slurry of 45% is evenly on Cu paper tinsel.Electrolyte is the LiPF of 1mol/L 6solution, solvent is the mixed solvent of EC, DEC and EMC, and volume ratio is 1: 1: 1.The negative pole of button cell uses Li sheet.In the glove box of argon shield, positive pole, negative pole, electrolyte, barrier film and battery case are assembled into button cell.At probe temperature is 25 DEG C, carry out electric performance test, after tested this embodiment one with two material compared with the product of comparative example, specific capacity improves more than 35%, and useful life brings up to more than 40%.

Claims (1)

1. Si modification is to a preparation method for the coated lithium cobaltate cathode material of conducting polymer, and wherein the chemical formula of this lithium cobaltate cathode material is LiCo 1-x-ymg xal yo 2, wherein: x=0.15-0.2, y=0.12-0.15, the method comprises the steps:
(1) lithium cobaltate cathode material is prepared
The cobalt nitrate of technical grade and ammonium acetate being mixed with these two kinds of material concentrations respectively with deionized water is 2-3M, the mixed solution of 0.5-1M, with deionized water, the potassium hydroxide of technical grade and ammoniacal liquor being made into these two kinds of material concentrations is 3-5M, the mixed solution of 1-2M, in the water-bath of 55-65 DEG C, above-mentioned two kinds of mixed solutions are joined in reaction vessel according to volume ratio 1:2-4 simultaneously, control pH value is 10-12, the precipitation ageing that reaction generates is precipitated, spend deionized water, then filter, dry, powder will be dried at 750-880 DEG C of temperature lower calcination 4-6h, obtain the high-density spherical cobaltic-cobaltous oxide of purity >=99.9%,
Take cobaltosic oxide prepared by lithia, said method that purity is greater than 99.5% according to the mole of Li, Co, Mg, Al in above-mentioned chemical formula, magnesium oxide that aluminium oxide, purity that purity is greater than 99.5% are greater than 99.5%, melt after the above-mentioned lithia, cobaltosic oxide, aluminium oxide and the magnesium oxide mechanical mixture that take at the temperature of 1300-1500 DEG C, ball grinds after cooling, at 850-900 DEG C, sinter 2-3h, obtain cobalt acid lithium;
(2) Si modification conducting polymer is prepared
Be 2-5 μm of Si powder by particle diameter, propylene carbonate is mixed to get mixture according to the ratio of mass ratio 1:5-10, described mixture and dispersant potassium phosphate are put into deionized water, wherein put into this mixture of 150-200g and 10-15g potassium phosphate in often liter of deionized water, obtain mixed liquor, described mixed liquor is stirred 15-20h with the speed of 100-150r/min in the water-bath of 65-70 DEG C, carries out polymerization reaction, filter, washing, dry, obtain Si modification conducting polymer;
(3) coated
By above-mentioned cobalt acid lithium with above-mentioned Si modification conducting polymer according to mass ratio 100:(12-16) together with join with rotating speed 300-400r/min ball milling 10-12h in planetary ball mill, drying;
Dried material is placed in argon gas atmosphere heat treatment, and heat treatment temperature is 150-250 DEG C, and insulation 3-4h, naturally cools to room temperature, pulverizes, sieves, obtain product.
CN201510009564.6A 2015-01-09 2015-01-09 Preparation method of lithium cobalt oxide positive electrode material coated with silicon-modified conducting polymer Pending CN104538599A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105470500A (en) * 2016-01-13 2016-04-06 四川富骅新能源科技有限公司 High voltage lithium cobalt oxide positive electrode material and preparation method therefor
CN107742712A (en) * 2017-10-24 2018-02-27 长沙理工大学 A kind of conducting polymer coating-doping type anode material for lithium-ion batteries and its synthetic method
CN108550796A (en) * 2018-04-12 2018-09-18 上海空间电源研究所 Closed lithium-oxygen battery lithia-fluorocarbons anode pole piece and preparation method thereof
CN111293366A (en) * 2020-02-21 2020-06-16 陆晨杰 Preparation method of lithium ion battery with lithium iron phosphate anode
CN111564612A (en) * 2020-04-07 2020-08-21 江门市科恒实业股份有限公司 High-thermal-conductivity and high-electrical-conductivity lithium battery positive electrode material and preparation method thereof
CN113571692A (en) * 2021-07-21 2021-10-29 合肥国轩高科动力能源有限公司 High-safety conductive material modified high-nickel positive electrode material and preparation method thereof

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CN103682326A (en) * 2013-12-13 2014-03-26 南通瑞翔新材料有限公司 High-capacity lithium cobalt oxide-base lithium ion battery anode material and preparation method thereof
CN103872315A (en) * 2014-04-09 2014-06-18 周末 Preparation method of germanium-doped high-energy-density lithium cobaltate composite positive material
CN104157875A (en) * 2014-06-10 2014-11-19 西北师范大学 Method for preparing nanometer silicon conductive polymer composite material for lithium ion batteries

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1731605A (en) * 2005-07-27 2006-02-08 浙江大学 Surface modified positive pole material of lithium ion cell and preparation method thereof
CN103682326A (en) * 2013-12-13 2014-03-26 南通瑞翔新材料有限公司 High-capacity lithium cobalt oxide-base lithium ion battery anode material and preparation method thereof
CN103872315A (en) * 2014-04-09 2014-06-18 周末 Preparation method of germanium-doped high-energy-density lithium cobaltate composite positive material
CN104157875A (en) * 2014-06-10 2014-11-19 西北师范大学 Method for preparing nanometer silicon conductive polymer composite material for lithium ion batteries

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105470500A (en) * 2016-01-13 2016-04-06 四川富骅新能源科技有限公司 High voltage lithium cobalt oxide positive electrode material and preparation method therefor
CN107742712A (en) * 2017-10-24 2018-02-27 长沙理工大学 A kind of conducting polymer coating-doping type anode material for lithium-ion batteries and its synthetic method
CN107742712B (en) * 2017-10-24 2019-11-12 长沙理工大学 A kind of conducting polymer coating-doping type anode material for lithium-ion batteries and its synthetic method
CN108550796A (en) * 2018-04-12 2018-09-18 上海空间电源研究所 Closed lithium-oxygen battery lithia-fluorocarbons anode pole piece and preparation method thereof
CN111293366A (en) * 2020-02-21 2020-06-16 陆晨杰 Preparation method of lithium ion battery with lithium iron phosphate anode
CN111564612A (en) * 2020-04-07 2020-08-21 江门市科恒实业股份有限公司 High-thermal-conductivity and high-electrical-conductivity lithium battery positive electrode material and preparation method thereof
CN111564612B (en) * 2020-04-07 2022-09-06 江门市科恒实业股份有限公司 High-thermal-conductivity and high-electrical-conductivity lithium battery positive electrode material and preparation method thereof
CN113571692A (en) * 2021-07-21 2021-10-29 合肥国轩高科动力能源有限公司 High-safety conductive material modified high-nickel positive electrode material and preparation method thereof
CN113571692B (en) * 2021-07-21 2022-07-12 合肥国轩高科动力能源有限公司 High-safety conductive material modified high-nickel positive electrode material and preparation method thereof

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