CN105206828A - Nickel and cobalt-based lithium-ion cathode material and preparation method thereof - Google Patents

Nickel and cobalt-based lithium-ion cathode material and preparation method thereof Download PDF

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CN105206828A
CN105206828A CN201510567414.7A CN201510567414A CN105206828A CN 105206828 A CN105206828 A CN 105206828A CN 201510567414 A CN201510567414 A CN 201510567414A CN 105206828 A CN105206828 A CN 105206828A
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sintering
preparation
lithium ion
coated
solution
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虞志远
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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
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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

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

Abstract

The invention discloses a nickel and cobalt-based lithium-ion cathode material, and the general chemical formula of a base material is LipNixCo1-xMmO2, wherein p is larger than or equal to 0.98 and less than or equal to 1.21, x is larger than or equal to 0.63 and less than 1, m is larger than or equal to 0.01 and less than 0.1, M is a doping agent, and a clad material is an active substance N. The preparation method comprises the steps of preparing a lithium ion secondary battery cathode material precursor; preparing a lithium ion secondary battery cathode material. In the invention, a nickel-cobalt binary precursor is a continuous coprecipitation reaction, elements are mixed uniformly, and the reaction is full, the control on morphological structure is facilitated, and through doping proper elements in a binary high-nickel material to reduce cation mixing phenomena, the structure is stabilized, and the safety and high-temperature properties of a battery material are improved, and the initial charge-discharge efficiency and energy density of the material is improved to a certain degree through active substance cladding.

Description

Nickel cobalt-based lithium ion anode material and preparation method thereof
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries, particularly a kind of nickel cobalt-based anode material for lithium-ion batteries and preparation method thereof of high-energy-density.
Background technology
Lithium ion battery has lightweight, the advantage such as volume is little, discharge platform is high, capacity is large, have extended cycle life, memory-less effect, thus be widely applied to the mobile electronic device such as mobile phone, notebook computer, be also applied to the fields such as artificial satellite, electric automobile, space flight and aviation simultaneously.
LiNi xco 1-xo 2the advantages such as (0.63 < x < 1) positive electrode has possessed cobalt acid lithium and the advantage of lithium nickelate, and specific discharge capacity is high, good cycle, cost are low and environmental pollution is little, but there is Ni due to high-nickel material 2+be difficult to be completely oxidized to Ni 3+, and cause Ni in high temperature crystallization process 2+with Ni 3+between there is cation mixing phenomenon, thus there will be poor heat stability and the defect such as first charge-discharge efficiency is low.
At present in order to head it off, doping coating modification etc. is carried out to this, really to a certain degree improve its cation mixing phenomenon, stabilize structure, but owing to adulterate or coated material is inert matter, reduce the specific capacity of battery to a certain extent.
In order to solve the problem, herein by Li pni xco 1-xo 2carry out adulterating and it is carried out to the structure of modified stable material, again by coated active material, the further chemical property improving material, not only increase stability and the high-temperature behavior of material, the chemical property, particularly specific capacity and the first charge-discharge efficiency that also improve material largely increase simultaneously.
Summary of the invention
Goal of the invention: nickel cobalt-based anode material for lithium-ion batteries that the invention provides a kind of high-energy-density and preparation method thereof, thus overcome the deficiencies in the prior art.
Technical scheme of the present invention: nickel cobalt-based lithium ion anode material, the chemical general formula of base material is: Li pni xco 1-xm mo 2, wherein 0.98≤p≤1.21,0.63≤x < 1,0.01≤m < 0.1, M is dopant, and clad material is active material N, 0.01 ~ 25wt% of base material gross mass shared by N.
The preparation method of the nickel cobalt-based lithium ion anode material of described high-energy-density, comprises the steps:
The first step, the preparation of lithium ion secondary battery anode material presoma:
The preparation of a, solution: Ni: Co=x: 1-x be mixed with mixing salt solution A1 in molar ratio, makes concentration of metal ions in this salting liquid be 0.5 ~ 3mol/L; Compound concentration is the aqueous slkali of 1.5 ~ 12mol/L, and compound concentration is the enveloping agent solution of 0.5 ~ 5mol/L, wherein 0.63≤x < 1;
The preparation of b, first liquid: inject pure water in reaction vessel, and the pH value regulating solution with aqueous slkali, and keep the temperature in reaction vessel to be 45 ~ 75 DEG C, pass into inert gas simultaneously, and run through whole course of reaction;
The reaction of c, presoma: add A1 solution in reaction vessel, coutroi velocity is 3 ~ 20L/min, slowly adds appropriate complexing agent and aqueous slkali simultaneously, and keep the temperature in reaction vessel to be 45 ~ 75 DEG C, adjustment mixing speed is 200 ~ 950r/min;
D, Separation of Solid and Liquid: material in step c is carried out surface treatment, the binary positive material presoma of synthesis goes to maturation groove and carries out Separation of Solid and Liquid, spend the binary positive material presoma of deionized water Separation of Solid and Liquid gained, the chemical formula being drying to obtain required binary precursor A 2, A2 is Ni xco 1-x(OH) 2;
Second step, the preparation of lithium ion secondary battery anode material:
E, once sintered: by lithium source substance, A2 and dopant M material according to molecular formula Li pni xco 1-xm mo 2in ratio mix, wherein 0.98≤p≤1.21,0.63≤x < 1,0.01≤m < 0.1, M is dopant, and controlling sintering temperature is 450 ~ 1000 DEG C, sintering time is 5 ~ 35h, sintering process passes into air or oxygen, by the material after sintering through PROCESS FOR TREATMENT such as fragmentation, classification, deironing, obtains materials A;
F, surface treatment: materials A is carried out washing process to reduce alkali content, the proportion of substance A and water is 1: 1 ~ 1: 6, is sieved by dry materials after washing;
G, coated: with the material after f process or substance A for matrix, coated active matter material N on matrix, method for coating is that dry type is coated, wet type is coated or co-precipitation cladding process, wherein, 0.01 ~ 25wt% of base material gross mass shared by N;
H, secondary or repeatedly sinter: sinter through the coated good material of g, sintering main temperature controls at 450 ~ 1000 DEG C, main warm area sintering time is 5 ~ 30h, need in sintering process to pass into air or oxygen, according to properties of product requirement, can carry out sintering for more than three times, the same double sintering of sintering condition.The PROCESS FOR TREATMENT such as the material after sintering carries out fragmentation, classification as required, sieves, deironing.
In some embodiments: in described step b, pH value is adjusted to 9 ~ 13.
In some embodiments: in described step c, pH value is adjusted to 10 ~ 13.
In some embodiments: the D50 scope of precursor A 2 is 8 ~ 20 μm.
Beneficial effect: in the present invention, nickel cobalt binary presoma is continous way coprecipitation reaction, and element mixes, sufficient reacting, is conducive to the control of pattern.Binary high-nickel material reduces cation mixing phenomenon by the element that doping is suitable, and stabilize structure, improve security performance and the high-temperature behavior of battery material, coated active material improves first charge-discharge efficiency and the energy density of material to a certain extent.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1:
The preparation of presoma: Ni: Co=0.63: 0.4 mixed solution A 1 being mixed with 0.5mol/L, the sodium hydroxide solution of preparation 1.5mol/L and 0.5mol/L ammonium sulfate; In reaction vessel, inject pure water, and regulate the pH value of just liquid to be 8.5 with 1.5mol/L sodium hydroxide solution, regulate the temperature in reaction vessel to be 40 DEG C, rotating speed is 200r/min, passes into nitrogen; The flow velocity regulating A1 solution is 20L/min, slowly drips NaOH and ammonium sulfate simultaneously, when granularity reaches requirement, carries out Separation of Solid and Liquid, dry, obtains required precursor A 2.
The preparation of positive electrode: by lithium hydroxide, A2 and aluminium hydroxide according to molecular formula Li pni xco 1-xm mo 2in ratio mix, wherein p=1.21, x=0.63, m=0.1, control sintering temperature be 1050 DEG C, sintering time is 40h, and sintering process passes into air, by sintering after material through PROCESS FOR TREATMENT such as fragmentation, classification, deironing, obtain materials A;
Surface treatment: according to A: water=1: the ratio of 1 is washed, dry, sieve;
Coated: with the above-mentioned sample handled well for matrix, coated LiCrO on matrix 2, method for coating is that dry type is coated, 0.01% of base material gross mass shared by N.
Double sintering: the above-mentioned material handled well is carried out double sintering, sintering main temperature controls at 400 DEG C, and the sintering time of main warm area is 35h, passes into air in sintering process.
Embodiment 2:
The preparation of presoma: Ni: Co=0.85: 0.15 mixed solution A 1 being mixed with 3mol/L, the sodium hydroxide solution of preparation 12mol/L and 5mol/L ammonium sulfate; In reaction vessel, inject pure water, and regulate the pH value of just liquid to be 13.5 with 8mol/L sodium hydroxide solution, regulate the temperature in reaction vessel to be 80 DEG C, rotating speed is 200r/min, passes into nitrogen; The flow velocity regulating A1 solution is 3L/min, slowly drips NaOH and ammonium sulfate simultaneously, when granularity reaches requirement, carries out Separation of Solid and Liquid, dry, obtains required precursor A 2.
The preparation of positive electrode: by lithium hydroxide, A2 and aluminium hydroxide according to molecular formula Li pni xco 1-xm mo 2in ratio mix, wherein p=0.98, x=0.85, m=0.01, control sintering temperature be 400 DEG C, sintering time is 4h, and sintering process passes into oxygen, by sintering after material through PROCESS FOR TREATMENT such as fragmentation, classification, deironing, obtain materials A;
Surface treatment: according to A: water=1: the ratio of 6 is washed, dry, sieve.
Coated: with the above-mentioned sample handled well for matrix, coated aluminum oxide and Li on matrix 2cO 3mixture, method for coating is that dry type is coated, 0.01% of base material gross mass shared by N.
Double sintering: the above-mentioned material handled well is carried out double sintering, sintering main temperature controls at 1050 DEG C, and the sintering time of main warm area is 3h, passes into air in sintering process.
Embodiment 3:
The preparation of presoma: Ni: Co=0.80: 0.20 mixed solution A 1 being mixed with 2mol/L, the sodium hydroxide solution of preparation 2.5mol/L and 1.8mol/L ammonium sulfate; In reaction vessel, inject pure water, and regulate the pH value of just liquid to be 12 with 2.5mol/L sodium hydroxide solution, regulate the temperature in reaction vessel to be 60 DEG C, rotating speed is 500r/min, passes into nitrogen; The flow velocity regulating A1 solution is 10L/min, slowly drips NaOH and ammonium sulfate simultaneously, when granularity reaches requirement, carries out Separation of Solid and Liquid, dry, obtains required precursor A 2.
The preparation of positive electrode: by lithium hydroxide, A2 and zirconia according to molecular formula Li pni xco 1-xm mo 2in ratio mix, wherein p=0.11, x=0.80, m=0.04, control sintering temperature be 400 DEG C, sintering time is 4h, and sintering process passes into oxygen, by sintering after material through PROCESS FOR TREATMENT such as fragmentation, classification, deironing, obtain materials A;
Coated: to be matrix with A, coated LiAIO on matrix 2, method for coating is that dry type is coated, 0.08% of base material gross mass shared by N.
Double sintering: the above-mentioned material handled well is carried out double sintering, sintering main temperature controls at 750 DEG C, and the sintering time of main warm area is 6h, passes into air in sintering process.

Claims (3)

1. nickel cobalt-based lithium ion anode material, is characterized in that: the chemical general formula of base material is: Li pni xco 1-xm mo 2, wherein 0.98≤p≤1.21,0.63≤x < 1,0.01≤m < 0.1, M is dopant, and clad material is active material N, 0.01 ~ 25wt% of base material gross mass shared by N.
2. the preparation method of the nickel cobalt-based lithium ion anode material of high-energy-density according to claim 1, is characterized in that: comprise the steps:
The first step, the preparation of lithium ion secondary battery anode material presoma:
The preparation of a, solution: Ni: Co=x: 1-x be mixed with mixing salt solution A1 in molar ratio, makes concentration of metal ions in this salting liquid be 0.5 ~ 3mol/L; Compound concentration is the aqueous slkali of 1.5 ~ 12mol/L, and compound concentration is the enveloping agent solution of 0.5 ~ 5mol/L, wherein 0.63≤x < 1;
The preparation of b, first liquid: inject pure water in reaction vessel, and pH value to 9 ~ 13 regulating solution with aqueous slkali, and keep the temperature in reaction vessel to be 45 ~ 75 DEG C, pass into inert gas simultaneously, run through whole course of reaction;
The reaction of c, presoma: add A1 solution in reaction vessel, coutroi velocity is 3 ~ 20L/min, slowly adds appropriate complexing agent and aqueous slkali simultaneously, regulates pH value to 10 ~ 13 of solution, keep the temperature in reaction vessel to be 45 ~ 75 DEG C, adjustment mixing speed is 200 ~ 950r/min;
D, Separation of Solid and Liquid: material in step c is carried out surface treatment, the binary positive material presoma of synthesis goes to maturation groove and carries out Separation of Solid and Liquid, spend the binary positive material presoma of deionized water Separation of Solid and Liquid gained, the chemical formula being drying to obtain required binary precursor A 2, A2 is Ni xco 1-x(OH) 2;
Second step, the preparation of lithium ion secondary battery anode material:
E, once sintered: by lithium source substance, A2 and dopant M material according to molecular formula Li pni xco 1-xm mo 2in ratio mix, wherein 0.98≤p≤1.21,0.63≤x < 1,0.01≤m < 0.1, M is dopant, and controlling sintering temperature is 450 ~ 1000 DEG C, sintering time is 5 ~ 35h, sintering process passes into air or oxygen, by the material after sintering through PROCESS FOR TREATMENT such as fragmentation, classification, deironing, obtains materials A;
F, surface treatment: materials A is carried out washing process to reduce alkali content, the proportion of substance A and water is 1: 1 ~ 1: 6, is sieved by dry materials after washing;
G, coated: with the material after f process or substance A for matrix, coated active matter material N on matrix, method for coating is that dry type is coated, wet type is coated or co-precipitation cladding process, wherein, 0.01 ~ 25wt% of base material gross mass shared by N;
H, secondary or repeatedly sinter: sinter through the coated good material of g, sintering main temperature controls at 450 ~ 1000 DEG C, main warm area sintering time is 5 ~ 30h, need in sintering process to pass into air or oxygen, according to properties of product requirement, can carry out sintering for more than three times, the same double sintering of sintering condition;
The PROCESS FOR TREATMENT such as the material after sintering carries out fragmentation, classification as required, sieves, deironing.
3. the preparation method of the nickel cobalt-based lithium ion anode material of high-energy-density according to claim 2, is characterized in that: the D50 scope of precursor A 2 is 8 ~ 20 μm.
CN201510567414.7A 2015-09-08 2015-09-08 Nickel and cobalt-based lithium-ion cathode material and preparation method thereof Pending CN105206828A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107799764A (en) * 2017-10-23 2018-03-13 金川集团股份有限公司 A kind of preparation method of the type tertiary cathode material of high compacted density 523
CN107910549A (en) * 2017-10-31 2018-04-13 中国科学院青海盐湖研究所 Positive electrode for lithium ion battery and its preparation method and application
CN108206280A (en) * 2016-12-19 2018-06-26 天津国安盟固利新材料科技股份有限公司 A kind of preparation method of low however, residual base nickel cobalt lithium aluminate cathode material
CN110034297A (en) * 2019-03-28 2019-07-19 欣旺达电动汽车电池有限公司 A kind of nickelic lithium ion anode material and preparation method thereof
CN110767899A (en) * 2019-10-24 2020-02-07 厦门厦钨新能源材料有限公司 Preparation method of composite anode material of lithium ion battery
CN111517377A (en) * 2020-04-28 2020-08-11 蜂巢能源科技有限公司 High-nickel ternary positive electrode material precursor, high-nickel ternary positive electrode material and preparation method of high-nickel ternary positive electrode material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108206280A (en) * 2016-12-19 2018-06-26 天津国安盟固利新材料科技股份有限公司 A kind of preparation method of low however, residual base nickel cobalt lithium aluminate cathode material
CN107799764A (en) * 2017-10-23 2018-03-13 金川集团股份有限公司 A kind of preparation method of the type tertiary cathode material of high compacted density 523
CN107910549A (en) * 2017-10-31 2018-04-13 中国科学院青海盐湖研究所 Positive electrode for lithium ion battery and its preparation method and application
CN110034297A (en) * 2019-03-28 2019-07-19 欣旺达电动汽车电池有限公司 A kind of nickelic lithium ion anode material and preparation method thereof
CN110767899A (en) * 2019-10-24 2020-02-07 厦门厦钨新能源材料有限公司 Preparation method of composite anode material of lithium ion battery
CN111517377A (en) * 2020-04-28 2020-08-11 蜂巢能源科技有限公司 High-nickel ternary positive electrode material precursor, high-nickel ternary positive electrode material and preparation method of high-nickel ternary positive electrode material

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Application publication date: 20151230