CN106920952B - A kind of preparation method of modified nickel lithium manganate cathode material - Google Patents

A kind of preparation method of modified nickel lithium manganate cathode material Download PDF

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CN106920952B
CN106920952B CN201710298934.1A CN201710298934A CN106920952B CN 106920952 B CN106920952 B CN 106920952B CN 201710298934 A CN201710298934 A CN 201710298934A CN 106920952 B CN106920952 B CN 106920952B
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nickel
lithium
manganate cathode
lithium manganate
salt
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CN201710298934.1A
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CN106920952A (en
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沈中宇
刘兴亮
汪涛
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合肥国轩高科动力能源有限公司
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/366Composites as layered products
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection 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
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection 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
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M2004/026Electrodes composed of or comprising active material characterised by the polarity
    • H01M2004/028Positive electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The present invention discloses a kind of preparation method of modified nickel lithium manganate cathode material, after it is the following steps are included: first mix cerium iron complex oxides and lithium salts, nickel salt, manganese salt, ball milling dispersion is carried out again, after being then dried in vacuo, obtains the presoma of cerium iron complex oxides cladding nickel ion doped material;By presoma in air atmosphere with 700 ~ 1000 DEG C of 5 ~ 20h of calcining at constant temperature, natural cooling obtains modified nickel lithium manganate cathode material.Nickel ion doped surface is coated on by cerium iron complex oxides; stable protective layer is formed, electrolyte can be effectively reduced and be contacted with nickel ion doped, reduces electrolyte in the oxygenolysis of positive electrode surface; to improve chemical stability of the positive electrode in battery system, and improve cycle performance.

Description

A kind of preparation method of modified nickel lithium manganate cathode material

Technical field

The invention belongs to lithium battery material fields, and in particular to a kind of preparation method of modified nickel lithium manganate cathode material.

Background technique

Lithium ion battery has many advantages, such as that specific energy is high, has extended cycle life and stablize with discharge performance, closely as secondary energy sources With factors, lithium ion battery and its correlation such as universal and ballooning oil prices of electric car under national new energy strategy over year Field is rapidly developed, however is urgently broken through in current lithium-ion battery system there are still many technical problems, as can Metric density is relatively low, at high cost, security performance is not good enough etc..

Spinel-type nickel ion doped (LiNi0.5Mn1.5O4) it is to grow up on the basis of LiMn2O4, there is good follow Ring performance, reversible capacity 146.7mAh/g, and have a up to discharge platform of 4.7V, it is considered to be it is most promising High potential anode material for lithium-ion batteries.However anodic potentials height means the reproducibility enhancing of negative regions, this also causes After nickel ion doped matching graphite cathode, the dynamics that surface SEI film is formed changes, and cannot be formed with the SEI of effect Electrolyte and carbon material is isolated in film, and the cycle performance of negative electrode material is caused to substantially reduce.In addition, since nickel ion doped battery is being made During standby, ambient moisture is difficult to control again, causes inside battery moisture content excessively high, and then cause chain electrochemical reaction, Promote electrolyte decomposition, and releases a large amount of gas.Especially nickel ion doped battery is after high-temperature storage, inside battery meeting Assemble a large amount of gas, the swelling of battery clearly, seriously constrains the performance of battery performance.

Summary of the invention

It is an object of the present invention to provide a kind of preparation method of modified nickel lithium manganate cathode material, this method process letters Single, non-environmental-pollution is low in cost, and obtained product purity is high, and performance is stablized, and is suitable for large-scale industrialized production.

Technical scheme is as follows:

A kind of preparation method of modified nickel lithium manganate cathode material comprising following steps:

(1) after mixing cerium iron complex oxides and lithium salts, nickel salt, manganese salt, then ball milling dispersion is carried out, be then dried in vacuo Afterwards, the presoma of cerium iron complex oxides cladding nickel ion doped material is obtained;

(2) by the presoma of step (1) in air atmosphere with 700~1000 DEG C of 5~20h of calcining at constant temperature, natural cooling Obtain modified nickel lithium manganate cathode material.

Further scheme, the lithium salts, nickel salt, Li, Ni, Mn elemental mole ratios are 1.05:0.5:1.5 in manganese salt.

Further scheme, the molecular formula of the cerium iron complex oxides are Ce1-x FexO2, 0.05≤x≤0.2 in formula.

The mass ratio of further scheme, the cerium iron complex oxides and theoretical synthesis nickel ion doped is (0.01-0.1): 1。

Further scheme, the lithium salts are one or both of lithium hydroxide, lithium acetate, lithium carbonate.

Further scheme, the nickel salt are one or both of nickel nitrate, nickel acetate, nickel sulfate, nickel chloride.

Further scheme, the manganese salt are one or both of manganese nitrate, manganese acetate, manganese sulfate, manganous chloride.

Further scheme, the medium of ball milling dispersion is deionized water, dehydrated alcohol, ethylene glycol, third in the step (1) One or both of ketone, dimethylformamide.

This patent passes through cerium iron complex oxides Ce1-xFexO2(0.05≤x≤0.2) is coated on nickel ion doped surface, is formed Stable protective layer can effectively reduce electrolyte and contact with nickel ion doped, reduce electrolyte in the oxidation point of positive electrode surface Solution, to improve chemical stability of the positive electrode in battery system, and improves cycle performance.

In addition, presoma is to be dispersed by ball-milling medium ball milling, then obtained by high-temperature calcination in preparation process of the present invention Ce1-xFexO2(0.05≤x≤0.2) coats nickel ion doped material, and process is simple and easy to control;And the Ce of cladding1-xFexO2With vertical Square fluorite structure, chemical property is excellent, and can effectively reduce electrolyte and contact with positive electrode, to reduce electrolyte In the oxygenolysis of positive electrode surface, high rate performance and stable circulation performance of the positive electrode in battery system are improved.

Detailed description of the invention

Fig. 1 is the SEM spectrum for the Modified Nickel lithium manganate material that embodiment 1 synthesizes;

Fig. 2 is the charging and discharging curve figure for the Modified Nickel lithium manganate material 0.5C multiplying power that embodiment 1 synthesizes;

Fig. 3 is 50 weeks cyclic curves of the Modified Nickel lithium manganate material 0.5C multiplying power that embodiment 1 synthesizes.

Specific embodiment

Embodiment 1

(1) lithium carbonate, nickel acetate and manganese acetate are weighed by Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5, further according to Ce0.95Fe0.05O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is that 0.01:1 weighs Ce0.95Fe0.05O2, by Ce0.95Fe0.05O2 After lithium carbonate, nickel acetate, manganese acetate mixing, deionized water is added and carries out ball milling dispersion, obtains Ce0.95Fe0.05O2Cladding LiNi0.5Mn1.5O4The presoma of material.

(2) 700 DEG C of calcining at constant temperature 20h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1) Obtain Ce0.95Fe0.05O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.

In conjunction with attached drawing, illustrate that Modified Nickel lithium manganate material object that the present invention is prepared mutually characterizes and electricity with embodiment 1 Chemical property:

Fig. 1 is the SEM spectrum for the Modified Nickel lithium manganate material that embodiment 1 synthesizes, as can be seen from Figure 1 Ce1-xFexO2? The uniform cladding nickel ion doped surface of grain is conducive to improve nickel ion doped in charge and discharge process holding structural stability, and raising follows Ring performance.

Lithium battery pond made by the modification nickel lithium manganate cathode material that embodiment 1 synthesizes, 0.5C charging and discharging curve figure Such as Fig. 2, as can be seen from Figure 2 under 0.5C multiplying power, capacity is in 130.3mAh/g.50 weeks cyclic curves of 0.5C multiplying power are as schemed 3, as can be seen from Figure 3 under 0.5C multiplying power, capacity retention ratio is still maintained at 98.08% after it experienced 50 weeks circulations, says It is bright to pass through Ce0.95Fe0.05O2Coating nickel ion doped material has good cyclical stability.

Embodiment 2

(1) lithium hydroxide, nickel sulfate and sulphur are weighed by the Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5 of nickel ion doped Sour manganese, further according to Ce0.9Fe0.1O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is that 0.05:1 weighs Ce0.9Fe0.1O2, will Ce0.9Fe0.1O2After the mixing of lithium hydroxide, nickel sulfate and manganese sulfate, dehydrated alcohol is added and carries out ball milling dispersion, obtains Ce0.9Fe0.1O2Coat LiNi0.5Mn1.5O4The presoma of material.

(2) 800 DEG C of calcining at constant temperature 15h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1) Obtain Ce0.9Fe0.1O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.

Embodiment 2 synthesize modification nickel lithium manganate cathode material experienced 50 weeks recycle after capacity retention ratio be 98.21%.

Embodiment 3

(1) lithium acetate, nickel nitrate and nitric acid are weighed by the Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5 of nickel ion doped Manganese, further according to Ce0.9Fe0.1O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is that 0.07:1 weighs Ce0.9Fe0.1O2, will Ce0.9Fe0.1O2After the mixing of lithium acetate, nickel nitrate and manganese nitrate, ethylene glycol is added and carries out ball milling dispersion, obtains Ce0.9Fe0.1O2 Coat LiNi0.5Mn1.5O4The presoma of material.

(2) 900 DEG C of calcining at constant temperature 10h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1) Obtain Ce0.9Fe0.1O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.

Embodiment 3 synthesize modification nickel lithium manganate cathode material experienced 50 weeks recycle after capacity retention ratio be 98.34%.

Embodiment 4

(1) lithium hydroxide, nickel chloride and two are weighed by the Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5 of nickel ion doped Manganese chloride, further according to Ce0.85Fe0.15O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is 0.09:1, weighs Ce0.85Fe0.15O2, By Ce0.85Fe0.15O2Ball milling dispersion is carried out with acetone is added after the mixing of lithium hydroxide, nickel chloride and manganous chloride, is obtained Ce0.85Fe0.15O2Coat LiNi0.5Mn1.5O4The presoma of material.

(2) 900 DEG C of calcining at constant temperature 15h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1) Obtain Ce0.85Fe0.15O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.

Embodiment 4 synthesize modification nickel lithium manganate cathode material experienced 50 weeks recycle after capacity retention ratio be 98.15%.

Embodiment 5

(1) lithium carbonate, nickel sulfate and sulfuric acid are weighed by the Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5 of nickel ion doped Manganese, further according to Ce0.8Fe0.2O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is 0.1:1, weighs Ce0.8Fe0.2O2, will Ce0.8Fe0.2O2Ball milling dispersion is carried out with dimethylformamide is added after lithium carbonate, nickel acetate, manganese acetate mixing, is obtained Ce0.8Fe0.2O2Coat LiNi0.5Mn1.5O4The presoma of material.

(2) 1000 DEG C of calcining at constant temperature 5h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1) Obtain Ce0.8Fe0.2O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.

Embodiment 5 synthesize modification nickel lithium manganate cathode material experienced 50 weeks recycle after capacity retention ratio be 97.56%.

Above content is only to structure of the invention example and explanation, affiliated those skilled in the art couple Described specific embodiment does various modifications or additions or is substituted in a similar manner, without departing from invention Structure or beyond the scope defined by this claim, is within the scope of protection of the invention.

Claims (7)

1. a kind of preparation method of modified nickel lithium manganate cathode material, it is characterised in that: the following steps are included:
(1) after mixing cerium iron complex oxides and lithium salts, nickel salt, manganese salt, then ball milling dispersion is carried out, after being then dried in vacuo, Obtain the presoma of cerium iron complex oxides cladding nickel ion doped material;The molecular formula of the cerium iron complex oxides is Ce1-x FexO2, 0.05≤x≤0.2 in formula;
(2) by the presoma of step (1) in air atmosphere with 700 ~ 1000 DEG C of 5 ~ 20h of calcining at constant temperature, natural cooling is changed Property nickel lithium manganate cathode material.
2. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the lithium Salt, nickel salt, Li, Ni, Mn elemental mole ratios are 1.05:0.5:1.5 in manganese salt.
3. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the cerium The mass ratio of iron compound oxide and theoretical synthesis nickel ion doped is (0.01-0.1): 1.
4. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the lithium Salt is one or both of lithium hydroxide, lithium acetate, lithium carbonate.
5. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the nickel Salt is one or both of nickel nitrate, nickel acetate, nickel sulfate, nickel chloride.
6. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the manganese Salt is one or both of manganese nitrate, manganese acetate, manganese sulfate, manganous chloride.
7. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the step Suddenly the medium that ball milling disperses in (1) is one of deionized water, dehydrated alcohol, ethylene glycol, acetone, dimethylformamide or two Kind.
CN201710298934.1A 2017-04-29 2017-04-29 A kind of preparation method of modified nickel lithium manganate cathode material CN106920952B (en)

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CN108305999A (en) * 2017-12-30 2018-07-20 宁夏科捷锂电池股份有限公司 It is a kind of to use β-Ga2O3To LiMn2O4The method that positive electrode carries out coating modification

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CN102257659A (en) * 2009-12-01 2011-11-23 松下电器产业株式会社 Positive electrode active material for nonaqueous electrolyte secondary battery and method for producing same
CN102931388A (en) * 2012-11-23 2013-02-13 惠州亿纬锂能股份有限公司 Rare earth oxide clad lithium titanate anode material, preparation method thereof and lithium ion battery
CN106058241A (en) * 2016-07-21 2016-10-26 天津巴莫科技股份有限公司 Ce1-xZrxO2 nano solid solution homogenate modified lithium ion battery anode material and preparation method thereof
CN106492812A (en) * 2016-09-14 2017-03-15 昆明理工大学 A kind of meso-pore CexFe1‑xO2The preparation method of solid solution catalyst

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
CN102257659A (en) * 2009-12-01 2011-11-23 松下电器产业株式会社 Positive electrode active material for nonaqueous electrolyte secondary battery and method for producing same
CN102244231A (en) * 2010-05-14 2011-11-16 中国科学院物理研究所 Method for cladding surfaces of active material of anode and/or anode and methods manufacturing anode and battery
CN102931388A (en) * 2012-11-23 2013-02-13 惠州亿纬锂能股份有限公司 Rare earth oxide clad lithium titanate anode material, preparation method thereof and lithium ion battery
CN106058241A (en) * 2016-07-21 2016-10-26 天津巴莫科技股份有限公司 Ce1-xZrxO2 nano solid solution homogenate modified lithium ion battery anode material and preparation method thereof
CN106492812A (en) * 2016-09-14 2017-03-15 昆明理工大学 A kind of meso-pore CexFe1‑xO2The preparation method of solid solution catalyst

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