CN103943850A - Method for preparing lithium-nickel-cobalt-aluminium oxide material by adopting low-heat solid-phase reaction - Google Patents

Method for preparing lithium-nickel-cobalt-aluminium oxide material by adopting low-heat solid-phase reaction Download PDF

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Publication number
CN103943850A
CN103943850A CN201410144890.3A CN201410144890A CN103943850A CN 103943850 A CN103943850 A CN 103943850A CN 201410144890 A CN201410144890 A CN 201410144890A CN 103943850 A CN103943850 A CN 103943850A
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lithium
equal
oxide material
presoma
cobalt
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CN103943850B (en
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仇卫华
段小刚
王伟东
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Shandong Tianjiao new energy Co.,Ltd.
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TIANJIAO TECH DEVELOPMENT Co Ltd SHENZHEN CITY
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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
    • 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
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a method for preparing a lithium-nickel-cobalt-aluminium oxide material by adopting low-heat solid-phase reaction. The method comprises the following steps: a. preparing a precursor, namely weighing lithium hydroxide monohydrate, nickel nitrate hexahydrate, cobalt nitrate hexahydrate, lithium nitrate nonahydrate and a doping element M according to stoichiometry of LiNi(0.8)Co(0.15)Al(0.05+/-x)M(y)O(2), wherein x is greater than or equal to 0 and is less than or equal to 0.05, y is greater than or equal to 0 and is less than or equal to 0.05, x+y is equal to 0.05, M is B, Zr, Ti or AlPO4, mixing in a high-speed mixer at the rotating speed of 2000r/m for 15 minutes according to a stoichiometric ratio so as to obtain a synthesized material, and drying the synthesized material at the temperature of 120-150 DEG C in vacuum so as to prepare the precursor; and b. roasting the precursor prepared in the step a at the temperature of 600-800 DEG C in an oxygen atmosphere or an air atmosphere so as to obtain the final product-lithium-nickel-cobalt-aluminium oxide material. The method has the following advantages that the stoichiometric ratio of the components is relatively easy to control, the components are uniformly mixed, the synthesis temperature can also be reduced, and the energy consumption and the production cost are reduced.

Description

A kind of method that adopts low fever solid phase reaction to prepare lithium nickel cobalt aluminum oxide material
Technical field
The present invention relates to preparation method's technical field of anode material of lithium battery, especially about the method for preparing lithium nickel cobalt aluminum oxide positive electrode with low fever solid phase reaction.
Background technology
Compared with business-like lithium ion cell anode material lithium cobaltate, nickel cobalt lithium aluminate has higher actual discharge specific capacity and better stores and cycle performance.In long-term high temperature storage process, NCA cathode material compares LiCoO in variation and the cation mixing situation of surface crystal/electronic structure 2cathode material is much smaller, shows that NCA has good shelf characteric [list of references Shoichiro Watanabe, Journal of Power Sources247 (2014) 412-422].
Nickel cobalt lithium aluminate (NCA) is produced and is adopted coprecipitation methods to prepare presoma more at present.
Low fever solid phase reaction refers to the chemical reaction carrying out between solid-phase compound under the condition of room temperature or nearly room temperature (≤100 DEG C).It is a kind of simple, the route that convenient, pollution-free, cost is low.Compared with liquid phase reactor, its maximum advantage is sufficient reacting and without side reaction, conversion ratio can reach 100%, pollution-free, no solvent residue.
Low fever solid phase reaction process containing crystallization water reaction system can be undertaken by mechanical lapping reactant particle, when mixing, make reaction-ure surface form one deck cold cut crucible zone, reactant molecule spreads concurrent biochemical reaction in cold cut crucible zone, generate target product, each cold cut crucible zone is equivalent to a micro-reaction zone, by mechanical lapping, particle surface is constantly updated, constantly formed new cold cut crucible zone; The product nucleation, the grain growth that generate form new product phase simultaneously.
This method adopts a kind of directly synthetic NCA presoma of method of high-speed stirred.Because the energy that high-speed stirred provides can be to the additional a kind of active force of solid matter, reduce the constraint energy barrier of particle to it around, make particle energy of thermal motion at normal temperatures also can overcome this constraint energy barrier.For the compound containing the crystallization water, in the time being heated, be generally first to slough the crystallization water, and then fusing.That is to say, crystallization water molecule in compound conventionally more easily overcomes constraint to it of particle around and is released.The hydrone that discharges forms trace solvent, can be further and compound molecule effect, form a kind of critical condition between solution state and melting state.Make the contained crystallization water of compound lower than discharging formation trace solvent under dehydration temperaturre by applied external force, although trace solvent can not be by complete reactant solvation, but can form the molten melt film of one deck at reaction-ure surface, thereby promote the carrying out of chemical reaction.
At present in the patent of delivering and article, what employing solid phase method was synthetic has " a kind of method that pure solid phase method is prepared anode material for lithium-ion batteries NCA " (CN201310084661.2), there is not yet the report that adopts the raw material identical with the present invention and synthetic this material of method.
Summary of the invention
The object of the invention is to overcome the defect that prior art exists, a kind of method that adopts low fever solid phase reaction to prepare lithium nickel cobalt aluminum oxide material is provided, high to solve high, the required energy consumption of reaction temperature existing in the synthetic lithium nickel cobalt aluminum oxide materials process of high temperature solid-state method; Chemical reaction component is wayward, mixing is difficult for uniform realistic problem.
For reaching above goal of the invention, the present invention takes following technical scheme:
Propose a kind of method that adopts low fever solid phase reaction to prepare lithium nickel cobalt aluminum oxide material, comprise the following steps:
A, presoma preparation:
According to LiNi 0.8co 0.15al 0.05 ± xm yo 2, wherein 0≤x≤0.05,0≤y≤0.05, x+y=0.05, M=B, Zr, Ti, AlPO 4, stoichiometry take a hydronium(ion) oxidation lithium LiOHH 2o, Nickelous nitrate hexahydrate Ni (NO 3) 26H 2o, cabaltous nitrate hexahydrate Co (NO 3) 26H 2o, nine nitric hydrate lithium Al (NO 3) 39H 2o and doped chemical M, wherein M=B, Mg, Zr, Ti, AlPO 4, mixing in high speed mixer by stoichiometric proportion, 2000 revs/min of mixer rotating speeds, mixed after 15 minutes, and synthetic material is carried out to 120～150 DEG C of vacuumizes, prepared presoma;
The preparation of b, product: the presoma that step a is prepared roasting 8 hours under 600～800 DEG C of oxygen atmospheres or air atmosphere, obtains end product lithium nickel cobalt aluminum oxide material LiNi 0.8co 0.15al 0.05 ± xm yo 2.
Compared with prior art, the present invention has following aspect advantage:
(1) utilize rare earth can control relatively easily the stoichiometric proportion of each component, and evenly mix between the each component making.
(2) presoma evenly mixes with Li salt, can reduce by 50 DEG C of synthesis temperatures, has reduced energy consumption.
(3) after the elements such as doping B, can, at sintetics under air conditions, reduce production cost.
brief Description Of Drawings:
Fig. 1 is the synthetic presoma XRD figure of rare earth method of the present invention, and this presoma is embodiment 1 gained;
Fig. 2 is the NCA finished product XRD figure of sintering under oxygen atmosphere, and in figure, a, b, c are respectively in embodiment 1,2,3 sintering gained finished product under presoma oxygen atmosphere;
Fig. 3 is the NCA finished product XRD figure of sintering under air atmosphere, and in figure, a, b, c are respectively in embodiment 1,2,3 sintering gained finished product under presoma air atmosphere;
Fig. 4 is the NCA finished product charging and discharging curve figure of sintering under oxygen atmosphere, and in figure, a, b, c are respectively in embodiment 1,2,3 sintering gained finished product under presoma oxygen atmosphere, and charging and discharging currents is 35mA/g, and charging/discharging voltage scope is 2.7-4.2V;
Fig. 5 is the NCA finished product charging and discharging curve figure of sintering under air atmosphere, and in figure, a, b, c are respectively in embodiment 1,2,3 sintering gained finished product under presoma air atmosphere, and charging and discharging currents is 35mA/g, and charging/discharging voltage scope is 2.7-4.2V.
Embodiment:
Below in conjunction with embodiment, the present invention is further elaborated.
Embodiment 1:
(1) by LiOHH 2o(12.445g), Ni (NO 3) 26H 2o(69.790g), Co (NO 3) 26H 2o(13.096g), Al (NO 3) 39H 2o(5.627g) in molar ratio (1.06:0.8:0.15:0.05) weighs, and in high speed mixer, mixes, and 2000 revs/min of mixer rotating speeds, mixed after 15 minutes, obtained green pasty state presoma.Carried out 120 DEG C of vacuumize 12h.
(2) by the presoma preparing roasting 8 hours under 700 DEG C of oxygen atmospheres or air atmosphere, obtain end product.
Embodiment 2
(1) by LiOHH 2o(12.445g), Ni (NO 3) 26H 2o(69.790g), Co (NO 3) 26H 2o(13.096g), Al (NO 3) 39H 2o(3.939g), MgCl 26H 2o(0.919g) in molar ratio (1.06:0.8:0.15:0.035:0.015) weighs, and in high speed mixer, mixes, and 2000 revs/min of mixer rotating speeds, mixed after 15 minutes, obtained green pasty state presoma.Carried out 120 DEG C of vacuumize 12h.
(2) by the presoma preparing roasting 8 hours under 700 DEG C of oxygen atmospheres or air atmosphere, obtain end product.
Embodiment 3
(1) by LiOHH 2o(12.445g), Ni (NO 3) 26H 2o(69.790g), Co (NO 3) 26H 2o(13.096g), Al (NO 3) 39H 2o(3.939g), H 3bO 3(0.278g) in molar ratio (1.06:0.8:0.15:0.035:0.015) weighs, and in high speed mixer, mixes, and 2000 revs/min of mixer rotating speeds, mixed after 15 minutes, obtained green pasty state presoma.Carried out 120 DEG C of vacuumize 12h.
(2) by the presoma preparing roasting 8 hours under 700 DEG C of oxygen atmospheres or air atmosphere, obtain end product.
From Fig. 1, presoma XRD collection of illustrative plates is known, and when the mode of employing high-speed mixing is prepared presoma, most of crystallization water is sloughed, and the hydroxyl in LiOH ruptures away, with the combination such as Ni, Co, forms metal hydroxides, and Li +with NO 3 -in conjunction with forming LiNO 3.
From Fig. 2, Fig. 3, fine by the crystallization of low-temperature solid-phase method gained nickel cobalt lithium aluminate sample, peak division, free from admixture peak, without mixing (I 003/ I 104be greater than 1).
From Fig. 4, Fig. 5, in oxygen atmosphere, the synthetic nickel cobalt lithium aluminate properties of sample of rare earth method is more excellent, embodiment 1, embodiment 2 and embodiment 3 synthetic sample specific discharge capacity under oxygen atmosphere is respectively 170mAh/g, 166mAh/g, 172mAh/g, and the B that adulterates under air atmosphere has higher specific capacity, synthetic NCA sample specific discharge capacity is respectively 131mAh/g, 139mAh/g, 149mAh/g.

Claims (1)

1. adopt low fever solid phase reaction to prepare a method for lithium nickel cobalt aluminum oxide material, it is characterized in that: comprise the following steps:
A, presoma preparation:
According to LiNi 0.8co 0.15al 0.05 ± xm yo 2, wherein 0≤x≤0.05,0≤y≤0.05, x+y=0.05, M=B, Zr, Ti, AlPO 4, stoichiometry take a hydronium(ion) oxidation lithium LiOHH 2o, Nickelous nitrate hexahydrate Ni (NO 3) 26H 2o, cabaltous nitrate hexahydrate Co (NO 3) 26H 2o, nine nitric hydrate lithium Al (NO 3) 39H 2o and doped chemical M, wherein M=B, Mg, Zr, Ti, AlPO 4, mixing in high speed mixer by stoichiometric proportion, 2000 revs/min of mixer rotating speeds, mixed after 15 minutes, and synthetic material is carried out to 120～150 DEG C of vacuumizes, prepared presoma;
The preparation of b, product: the presoma that step a is prepared roasting 8 hours under 600～800 DEG C of oxygen atmospheres or air atmosphere, obtains end product lithium nickel cobalt aluminum oxide material LiNi 0.8co 0.15al 0.05 ± xm yo 2.
CN201410144890.3A 2014-04-11 2014-04-11 Method for preparing lithium-nickel-cobalt-aluminium oxide material by adopting low-heat solid-phase reaction Active CN103943850B (en)

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CN106410187A (en) * 2016-10-18 2017-02-15 荆门市格林美新材料有限公司 Method for preparing doped and modified nickel-cobalt lithium aluminate anode materials
CN106784802A (en) * 2016-12-30 2017-05-31 绍兴文理学院 A kind of synthesis of anode material of lithium-ion battery and preparation method thereof
CN108428862A (en) * 2018-02-06 2018-08-21 中南大学 Aluminium cladding ternary mixes zirconium composite material, composite positive pole and its preparation and the application in lithium ion battery
CN109698340A (en) * 2018-12-28 2019-04-30 天能电池(芜湖)有限公司 The lithium ion battery preparation process of nickel cobalt aluminium tertiary cathode material

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106410187A (en) * 2016-10-18 2017-02-15 荆门市格林美新材料有限公司 Method for preparing doped and modified nickel-cobalt lithium aluminate anode materials
CN106410187B (en) * 2016-10-18 2019-02-12 荆门市格林美新材料有限公司 A kind of preparation method of the nickel cobalt lithium aluminate cathode material of doping vario-property
CN106784802A (en) * 2016-12-30 2017-05-31 绍兴文理学院 A kind of synthesis of anode material of lithium-ion battery and preparation method thereof
CN108428862A (en) * 2018-02-06 2018-08-21 中南大学 Aluminium cladding ternary mixes zirconium composite material, composite positive pole and its preparation and the application in lithium ion battery
CN108428862B (en) * 2018-02-06 2020-12-15 中南大学 Aluminum-coated ternary zirconium-doped composite material, composite anode material, preparation of composite anode material and application of composite anode material in lithium ion battery
CN109698340A (en) * 2018-12-28 2019-04-30 天能电池(芜湖)有限公司 The lithium ion battery preparation process of nickel cobalt aluminium tertiary cathode material

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