CN104300131A - Preparation method of precursor of lithium nickel cobalt manganese oxide material - Google Patents

Preparation method of precursor of lithium nickel cobalt manganese oxide material Download PDF

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Publication number
CN104300131A
CN104300131A CN201410479929.7A CN201410479929A CN104300131A CN 104300131 A CN104300131 A CN 104300131A CN 201410479929 A CN201410479929 A CN 201410479929A CN 104300131 A CN104300131 A CN 104300131A
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Prior art keywords
manganese oxide
lithium nickel
cobalt
nickel cobalt
oxide precursor
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CN201410479929.7A
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孙琦
李岩
孙慧英
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QINGDAO QIANYUN HIGH-TECH NEW MATERIAL Co Ltd
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QINGDAO QIANYUN HIGH-TECH NEW MATERIAL Co Ltd
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Priority to CN201410479929.7A priority Critical patent/CN104300131A/en
Publication of CN104300131A publication Critical patent/CN104300131A/en
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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
    • H01M4/48—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
    • 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 the field of lithium nickel cobalt manganese oxide materials and particularly relates to a preparation method of a precursor of a lithium nickel cobalt manganese oxide material. The preparation method comprises the following steps: (1) adding a mixed water solution of sulfates in the molar ratio of nickel ions to magnesium ions to cobalt ions being 5 to 3 to 2 into a synthesis reaction kettle with an ultrasonic device, introducing protective gas, simultaneously adding an alkaline precipitant and a metal complexing agent which are capable of precipitating the metal ions and regulate the pH value of the solution to be 11 which is constant, and performing filtration and ultrasonic washing to obtain slurry; (2) adding the slurry into a stirring reaction kettle, adding the mixed water solution of the sulfates in the molar ratio of nickel ions to magnesium ions to cobalt ions being 1 to 1 to 1, introducing the protective gas, simultaneously adding the alkaline precipitant and the metal complexing agent which are capable of precipitating the metals ions and regulate the pH value of the solution to be 11 which is constant, washing a precipitate and performing vacuum drying; and (3) sintering. The lithium nickel cobalt manganese oxide material prepared by utilizing the precursor of the lithium nickel cobalt manganese oxide material provided by the invention has the advantages of high tapping density, good processing performance and excellent electrochemical properties.

Description

The preparation method of lithium nickel cobalt manganese oxide precursor
Technical field
The present invention relates to nickel-cobalt lithium manganate material field, especially relate to a kind of preparation method of lithium nickel cobalt manganese oxide precursor.
Background technology
Anode material for lithium-ion batteries is the part of most critical in battery, and Postive electrode material of li-ion accumulator in the market mainly contains cobalt acid lithium, LiMn2O4, LiFePO 4 and nickel-cobalt-manganese ternary system.Wherein, cobalt acid lithium, LiFePO 4 and nickel-cobalt-manganese ternary system are mainstay material.Because cobalt resource is seriously rare, expensive, and there is potential safety hazard when overcharge, thus the application of cobalt acid lithium in high capacity cell is subject to severely restricts.Although the LiMn2O4 of stratiform has the specific capacity of 200mAhg-1, structural stability is very poor, and the LiMn2O4 specific capacity of spinel-type is very low, and the structural stability under high temperature has to be strengthened.Ferrousphosphate lithium material tap density is low, poor processability, limits the further application of this material.And nickle cobalt lithium manganate adopts relatively inexpensive nickel and manganese to instead of cobalts a large amount of in cobalt acid lithium, thus the advantage of its cost aspect clearly.Simultaneously, its reversible capacity is large, Stability Analysis of Structures, security performance is good, have higher conductivity and thermal stability, compare with other anode material for lithium-ion batteries, nickel-cobalt lithium manganate material and cobalt acid lithium material are in chemical property and processing characteristics closely, be a kind of material most possibly replacing cobalt acid lithium, there are very large market prospects.
At present, the synthesis of the technical process mainly precursor that coprecipitation prepares nickle cobalt lithium manganate, mixed lithium and sintering.General elder generation is settled out the hydroxide of nickel and cobalt containing manganese or the precursor of carbonate from soluble metallic salt, precursor is washed, dry after adopt solid phase mixing mode to mix with lithium salts after, at high temperature sinter and prepare nickle cobalt lithium manganate.The precursor spherical degree of common Co deposited synthesis controls not good, and tap density is not high, makes the nickle cobalt lithium manganate processing characteristics for preparing poor.Meanwhile, single LiNi 1/3co 1/3mn 1/3o 2material capacity is lower; Single LiNi 0.5co 0.2mn 0.3o 2material circulation poor-performing.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of tap density high, good sphericity, can overcome existing single LiNi 1/3co 1/3mn 1/3o 2material capacity is lower, single LiNi 0.5co 0.2mn 0.3o 2the preparation method of the lithium nickel cobalt manganese oxide precursor of the problem of material circulation poor performance.The method can realize the efficiency utilization of resource, gained Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2the cycle performance of solid-solution material and high rate performance and tap density obviously excellent, processing characteristics is obviously improved.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of lithium nickel cobalt manganese oxide precursor, comprise the following steps: (1) is by nickel, the mixed aqueous solution of the sulfate of cobalt and manganese joins in the synthesis reaction vessel with Vltrasonic device by measuring pump with 14mL/min, mixing speed keeps 1270r/min always, logical protection gas, synthetic environment is carried out under anaerobic, simultaneously continue to add enough precipitate metal ion with the speed of 8mL/min and make the pH value modification stability of solution 11 alkaline precipitating agent and metal chelating agent, after filtration with supersound washing after, obtain Ni 0.5co 0.2mn 0.3(OH) 2slurry,
The mixed aqueous solution metal ion total concentration of the sulfate of described nickel, cobalt and manganese is 2.5mol/L, and wherein, the mol ratio of nickel ion, manganese ion and cobalt ions is 5:3:2;
(2) step (1) gained slurry is added in stirred autoclave, control mixing speed is 265r/min, again by nickel, the mixed aqueous solution of the sulfate of cobalt and manganese adds in stirred autoclave by measuring pump with 12mL/min, control mixing speed is 1270r/min, logical protection gas, synthetic environment is carried out under anaerobic, simultaneously continue to add enough precipitate metal ion with the speed of 8mL/min and make the pH value modification stability of solution 11 alkaline precipitating agent and metal chelating agent, after the sediment obtained washs with deionized water and organic solvent successively, again through vacuumize, obtain lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2powder,
The mixed aqueous solution metal ion total concentration of the sulfate of described nickel, cobalt and manganese is 2.4mol/L, and wherein, nickel ion, manganese ion and cobalt ions mol ratio are 1:1:1;
(3) by step (2) gained lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2powder, under the gas condition passing into compaction, in 970 DEG C of sintering 9h, obtains lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2solid solution.
Preferred version is as follows:
In step (1) and step (2), described protection gas is argon gas, nitrogen, carbon monoxide or hydrogen.
In step (1) and step (2), described alkaline precipitating agent is one or more of sodium hydroxide solution, aqua calcis, potassium hydroxide solution, sal volatile, ammonium bicarbonate soln or sodium carbonate liquor.
In step (1) and step (2), described metal chelating agent is ammonia spirit, sal volatile or ammonium bicarbonate soln.
In step (2), described organic solvent is methyl alcohol, ethanol or acetone.
In step (3), described in have the gas of compaction to be oxygen, air or nitrogen.
The Ni that the present invention obtains 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2solid solution pellet even particle size distribution, good sphericity, tap density is high; With Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2solid solution is the LiNi of precursor synthesis 1/3co 1/3mn 1/3o 2-LiNi 0.5co 0.2mn 0.3o 2material tap density is high, good processability, electrochemical performance.The capability retention after 100 times that circulates be 99.3%, 1C electric discharge for 0.1C discharge 93.2%, tap density reaches 2.66g/cm 3, substantially increase processing characteristics and the chemical property of product.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but the present invention is not limited to specific embodiment.
Embodiment 1:
A kind of preparation method of lithium nickel cobalt manganese oxide precursor; comprise the following steps: the mixed aqueous solution of the sulfate of nickel, cobalt and manganese joins in the synthesis reaction vessel with Vltrasonic device by measuring pump with 14mL/min by (1); mixing speed keeps 1270r/min always; logical protection gas; synthetic environment is carried out under anaerobic; simultaneously continue to add enough precipitate metal ion with the speed of 8mL/min and make the pH value modification stability of solution 11 alkaline precipitating agent and metal chelating agent; after filtration with supersound washing after, obtain Ni 0.5co 0.2mn 0.3(OH) 2slurry;
The mixed aqueous solution metal ion total concentration of the sulfate of described nickel, cobalt and manganese is 2.5mol/L, and wherein, the mol ratio of nickel ion, manganese ion and cobalt ions is 5:3:2;
(2) step (1) gained slurry is added in stirred autoclave, control mixing speed is 265r/min, again by nickel, the mixed aqueous solution of the sulfate of cobalt and manganese adds in stirred autoclave by measuring pump with 12mL/min, control mixing speed is 1270r/min, logical protection gas, synthetic environment is carried out under anaerobic, simultaneously continue to add enough precipitate metal ion with the speed of 8mL/min and make the pH value modification stability of solution 11 alkaline precipitating agent and metal chelating agent, after the sediment obtained washs with deionized water and organic solvent successively, again through vacuumize, obtain lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2powder,
The mixed aqueous solution metal ion total concentration of the sulfate of described nickel, cobalt and manganese is 2.4mol/L, and wherein, nickel ion, manganese ion and cobalt ions mol ratio are 1:1:1;
(4) by step (2) gained lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2powder, under the gas condition passing into compaction, in 970 DEG C of sintering 9h, obtains lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2solid solution.
In step (1) and step (2), described protection gas is carbon monoxide.
In step (1) and step (2), described alkaline precipitating agent is sodium hydroxide solution, aqua calcis, potassium hydroxide solution and ammonium bicarbonate soln.
In step (1) and step (2), described metal chelating agent is sal volatile.
In step (2), described organic solvent is acetone.
In step (3), described in have the gas of compaction to be nitrogen.
Embodiment 2:
A kind of preparation method of lithium nickel cobalt manganese oxide precursor; comprise the following steps: the mixed aqueous solution of the sulfate of nickel, cobalt and manganese joins in the synthesis reaction vessel with Vltrasonic device by measuring pump with 14mL/min by (1); mixing speed keeps 1270r/min always; logical protection gas; synthetic environment is carried out under anaerobic; simultaneously continue to add enough precipitate metal ion with the speed of 8mL/min and make the pH value modification stability of solution 11 alkaline precipitating agent and metal chelating agent; after filtration with supersound washing after, obtain Ni 0.5co 0.2mn 0.3(OH) 2slurry;
The mixed aqueous solution metal ion total concentration of the sulfate of described nickel, cobalt and manganese is 2.5mol/L, and wherein, the mol ratio of nickel ion, manganese ion and cobalt ions is 5:3:2;
(2) step (1) gained slurry is added in stirred autoclave, control mixing speed is 265r/min, again by nickel, the mixed aqueous solution of the sulfate of cobalt and manganese adds in stirred autoclave by measuring pump with 12mL/min, control mixing speed is 1270r/min, logical protection gas, synthetic environment is carried out under anaerobic, simultaneously continue to add enough precipitate metal ion with the speed of 8mL/min and make the pH value modification stability of solution 11 alkaline precipitating agent and metal chelating agent, after the sediment obtained washs with deionized water and organic solvent successively, again through vacuumize, obtain lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2powder,
The mixed aqueous solution metal ion total concentration of the sulfate of described nickel, cobalt and manganese is 2.4mol/L, and wherein, nickel ion, manganese ion and cobalt ions mol ratio are 1:1:1;
(5) by step (2) gained lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2powder, under the gas condition passing into compaction, in 970 DEG C of sintering 9h, obtains lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2solid solution.
In step (1) and step (2), described protection gas is nitrogen.
In step (1) and step (2), described alkaline precipitating agent is sal volatile, ammonium bicarbonate soln and sodium carbonate liquor.
In step (1) and step (2), described metal chelating agent is ammonium bicarbonate soln.
In step (2), described organic solvent is methyl alcohol.
In step (3), described in have the gas of compaction to be oxygen.

Claims (6)

1. the preparation method of a lithium nickel cobalt manganese oxide precursor; it is characterized in that; comprise the following steps: the mixed aqueous solution of the sulfate of nickel, cobalt and manganese joins in the synthesis reaction vessel with Vltrasonic device by measuring pump with 14mL/min by (1); mixing speed keeps 1270r/min always; logical protection gas; synthetic environment is carried out under anaerobic; simultaneously continue to add enough precipitate metal ion with the speed of 8mL/min and make the pH value modification stability of solution 11 alkaline precipitating agent and metal chelating agent; after filtration with supersound washing after, obtain Ni 0.5co 0.2mn 0.3(OH) 2slurry;
The mixed aqueous solution metal ion total concentration of the sulfate of described nickel, cobalt and manganese is 2.5mol/L, and wherein, the mol ratio of nickel ion, manganese ion and cobalt ions is 5:3:2;
(2) step (1) gained slurry is added in stirred autoclave, control mixing speed is 265r/min, again by nickel, the mixed aqueous solution of the sulfate of cobalt and manganese adds in stirred autoclave by measuring pump with 12mL/min, control mixing speed is 1270r/min, logical protection gas, synthetic environment is carried out under anaerobic, simultaneously continue to add enough precipitate metal ion with the speed of 8mL/min and make the pH value modification stability of solution 11 alkaline precipitating agent and metal chelating agent, after the sediment obtained washs with deionized water and organic solvent successively, again through vacuumize, obtain lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2powder,
The mixed aqueous solution metal ion total concentration of the sulfate of described nickel, cobalt and manganese is 2.4mol/L, and wherein, nickel ion, manganese ion and cobalt ions mol ratio are 1:1:1;
(3) by step (2) gained lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2powder, under the gas condition passing into compaction, in 970 DEG C of sintering 9h, obtains lithium nickel cobalt manganese oxide precursor Ni 1/3co 1/3mn 1/3(OH) 2-Ni 0.5co 0.2mn 0.3(OH) 2solid solution.
2. the preparation method of lithium nickel cobalt manganese oxide precursor according to claim 1, is characterized in that: in step (1) and step (2), described protection gas is argon gas, nitrogen, carbon monoxide or hydrogen.
3. the preparation method of lithium nickel cobalt manganese oxide precursor according to claim 1 and 2, it is characterized in that: in step (1) and step (2), described alkaline precipitating agent is one or more of sodium hydroxide solution, aqua calcis, potassium hydroxide solution, sal volatile, ammonium bicarbonate soln or sodium carbonate liquor.
4. the preparation method of lithium nickel cobalt manganese oxide precursor according to claim 1 and 2, is characterized in that: in step (1) and step (2), described metal chelating agent is ammonia spirit, sal volatile or ammonium bicarbonate soln.
5. the preparation method of lithium nickel cobalt manganese oxide precursor according to claim 1 and 2, is characterized in that: in step (2), and described organic solvent is methyl alcohol, ethanol or acetone.
6. the preparation method of lithium nickel cobalt manganese oxide precursor according to claim 1 and 2, is characterized in that: in step (3), described in have the gas of compaction to be oxygen, air or nitrogen.
CN201410479929.7A 2014-09-18 2014-09-18 Preparation method of precursor of lithium nickel cobalt manganese oxide material Pending CN104300131A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106395920A (en) * 2016-08-29 2017-02-15 青海泰丰先行锂能科技有限公司 Element co-doping modified ternary lithium ion battery cathode material, and preparation method thereof
CN107959023A (en) * 2017-11-28 2018-04-24 清远佳致新材料研究院有限公司 A kind of preparation method of low sodium content sulphur nickel-cobalt-manganese ternary element mixed hydroxides
CN109160545A (en) * 2018-07-24 2019-01-08 格林美股份有限公司 A kind of precursor of nickel-cobalt-lithium-manganese-oxide synthesizer
CN110474047A (en) * 2019-08-28 2019-11-19 湖南金富力新能源股份有限公司 A kind of nickel-cobalt-manganese ternary presoma and the preparation method and application thereof
CN112694137A (en) * 2020-12-24 2021-04-23 荆门市格林美新材料有限公司 Small-particle-size cobalt-free lithium-rich manganese-based solid solution and lithium vanadate composite material and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106395920A (en) * 2016-08-29 2017-02-15 青海泰丰先行锂能科技有限公司 Element co-doping modified ternary lithium ion battery cathode material, and preparation method thereof
CN106395920B (en) * 2016-08-29 2018-02-06 青海泰丰先行锂能科技有限公司 A kind of codoping modified ternary anode material for lithium-ion batteries of element and preparation method
CN107959023A (en) * 2017-11-28 2018-04-24 清远佳致新材料研究院有限公司 A kind of preparation method of low sodium content sulphur nickel-cobalt-manganese ternary element mixed hydroxides
CN107959023B (en) * 2017-11-28 2021-02-19 清远佳致新材料研究院有限公司 Preparation method of sulfur, nickel, cobalt and manganese three-element mixed hydroxide with low sodium content
CN109160545A (en) * 2018-07-24 2019-01-08 格林美股份有限公司 A kind of precursor of nickel-cobalt-lithium-manganese-oxide synthesizer
CN109160545B (en) * 2018-07-24 2021-01-05 格林美股份有限公司 Nickel cobalt lithium manganate precursor synthesizer
CN110474047A (en) * 2019-08-28 2019-11-19 湖南金富力新能源股份有限公司 A kind of nickel-cobalt-manganese ternary presoma and the preparation method and application thereof
CN112694137A (en) * 2020-12-24 2021-04-23 荆门市格林美新材料有限公司 Small-particle-size cobalt-free lithium-rich manganese-based solid solution and lithium vanadate composite material and preparation method thereof

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Application publication date: 20150121