CN108493429A - The preparation method of anode composite material of lithium ion battery - Google Patents
The preparation method of anode composite material of lithium ion battery Download PDFInfo
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- CN108493429A CN108493429A CN201810414098.3A CN201810414098A CN108493429A CN 108493429 A CN108493429 A CN 108493429A CN 201810414098 A CN201810414098 A CN 201810414098A CN 108493429 A CN108493429 A CN 108493429A
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- lithium
- ion battery
- composite material
- lithium ion
- positive electrode
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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
- H01M4/364—Composites as mixtures
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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
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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
- H01M4/52—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 present invention provides a kind of preparation method of anode composite material of lithium ion battery, includes the following steps：1）After tungsten source is dissolved in solvent, PVP is added and disperses to form mixed solution；2）Nickelic positive electrode is added into mixed solution, and solvent evaporated is heated after constant temperature stirring；3）Step 2）Resulting materials carry out dry-mixed with lithium salts after being dried；4）Dry-mixed resulting materials are calcined under aerobic conditions obtains the nickelic positive electrode of tungstate lithium cladding.Resulting materials clad homogeneity is good, and the tungstate lithium of cladding helps to improve the chemical property of nickelic positive electrode, the especially cyclical stability in hot environment.
Description
Technical field
The present invention relates to lithium ion battery material preparing technical fields, it particularly relates to a kind of lithium ion cell positive
The preparation method of composite material, especially a kind of lithium ion battery coat the anode composite material of nickelic positive electrode with tungstate lithium
Preparation method.
Background technology
Positive electrode is most important component part in lithium ion battery, is limit since its specific capacity is less than negative material
The key factor of preparing lithium ion battery energy density.In the development of lithium ion battery, positive electrode becomes the weight of researcher
Point.Currently, with the development of science and technology, requirement of the movable equipment to battery various aspects of performance increasingly improves, lithium-ion electric
Pond positive electrode just develops towards the direction of high voltage, high power capacity.In the past twenty years, anode material for lithium-ion batteries
Research focuses primarily upon stratiform cobalt acid lithium, lithium nickelate, nickle cobalt lithium manganate, nickel cobalt lithium aluminate, lithium manganate having spinel structure and olive
Stone-type LiFePO 4 material etc..LiFePO4 is one of most common positive electrode active materials in battery, not only due to ferro element is honest and clean
Valence and environmental protection, and it capacity attenuation will not occur with excellent cyclical stability after hundreds of cycles.Although phosphoric acid
Iron lithium has excellent cyclical stability, but its conductivity is low, hinders its actual use.Cobalt acid lithium possesses higher theoretical appearance
Amount, but since the lithium ion content of the reversible embedded abjection of material itself is limited, when deviating from lithium ion excess, it be easy to cause material
Stable structure sex chromosome mosaicism.In addition, due in nature cobalt element reserves it is low so that use lithium cobaltate cathode material battery price
It is higher.Another positive electrode LiMn2O4For spinel oxide, due to Mn characteristics of low cost and environmental-friendly, point is brilliant
Graphite/oxide material is by very big concern.In addition to this, due to its unique structure, LiMn2O4Three can be provided for lithium ion
Tie up transmission channel.However, the high temperature cyclic performance of spinel anode material is poor, even if being recycled at a high temperature of about 50 DEG C, hold
Amount will sharp-decay.LiNiO2LiCoO can be classified as2Same type material, with same space group hexagonal symmetry.
In addition, LiNiO2Material ratio LiCoO2Toxicity is lower and cheaper.However, due to Ni2+With Li+Radius is close, LiNiO2
In Li layers always by Ni2+Ion occupies.To hinder the diffusion of lithium ion in the material.This effect is referred to as that " lithium nickel is mixed
Row ".In order to reduce this effect, material structure stability can be improved on a large scale by the way of cobalt and manganese part substitution nickel.
Just because of this, LiNi1-x-yCoxMnyO2Ternary material is systematically studied, so as to obtain chemical property preferably, cost
Cheap, the higher anode material for lithium-ion batteries of capacity.But there are still significantly ask for nickelic tertiary cathode material used at present
Topic, such as security performance, high voltage cycle stability, storage performance etc..
In addition, during lithium ion battery charge and discharge cycles, the tetravalence nickel ion in nickelic positive electrode has very
Strong catalytic oxidation activity be easy to cause the decomposition of electrolyte, causes the destruction of material surface structure, transition metal dissolution, polarization
A series of problems, such as increase；Especially during high temperature circulation, the nickelic positive electrode of lithium ion and electrolyte side reaction aggravation,
Transition metal dissolution is apparent, electro-chemical activity positive electrode content declines.Therefore, inertia lithium is introduced on nickelic positive electrode surface
Electrode layer can effectively avoid the generation of positive electrode interface side reaction between electrolyte under high voltage, high temperature, be to solve
One of most effective approach of these problems.
Invention content
For above-mentioned technical problem in the related technology, the present invention proposes a kind of system of anode composite material of lithium ion battery
The nickelic positive electrode of tungstate lithium cladding is prepared by low temperature liquid polymerization process for Preparation Method, and resulting materials are under room temperature and high temperature
Surface stability greatly improves, and chemical property is substantially improved.
To realize the above-mentioned technical purpose, the technical proposal of the invention is realized in this way：
On the one hand, the present invention provides a kind of preparation method of anode composite material of lithium ion battery, includes the following steps：
1) after tungsten source being dissolved in solvent, PVP is added and disperses to form mixed solution；
2) nickelic positive electrode is added into mixed solution, and solvent evaporated is heated after constant temperature stirring；
3) it is dry-mixed with lithium salts progress after step 2) resulting materials are dried；
4) dry-mixed resulting materials are calcined under aerobic conditions obtains the nickelic positive electrode of tungstate lithium cladding.
Further, the tungsten source includes ammonium metatungstate, tungsten trichloride, tungsten pentachloride or combinations thereof.
Further, the solvent includes water, ethyl alcohol or combinations thereof.Preferably, the solvent is the mixing of water and ethyl alcohol
Solvent, the two are mixed at 1: 1 by volume.
Further, the chemical formula of the nickelic positive electrode is LiNixM1-xO2, wherein：M be Co, Mn, Al at least
One kind, 0.8≤x≤1.
Further, the chemical formula of the nickelic positive electrode includes Ni0.8Co0.1Mn0.1(OH)2、Ni0.6Co0.2Mn0.2
(OH)2、Ni0.5Co0.2Mn0.3(OH)2Deng.
Further, the mass percent that the tungsten source prepares gained tungstate lithium and nickelic positive electrode is 0.05%~
10%.Preferably 0.1%, 5%, 1%, 6%, 10%.
Further, the constant temperature stirring refers to carrying out constant temperature at 30 DEG C to stir 1~5h.It is preferred that constant temperature stirs 2h, 4h.
Further, the temperature of the heating solvent evaporated is 80~90 DEG C.
Further, the method for the drying includes vacuum drying, forced air drying, spray drying or its combination.It is preferred that dry
The dry time is 6~12h.Preferably 6h, 8h, 10h, 12h.
Further, the dosage of the lithium salts is 1.0~1.1 of the mole of metal ion in step 2) resulting materials
Times.
Further, the temperature of the calcining is 750~900 DEG C.Preferable temperature is 800 DEG C or 900 DEG C.Further,
The time of the calcining is 15h~18h.It is preferred that the time is 15h, 16h or 18h.
Further, the lithium salts includes lithium hydroxide or lithium carbonate.
On the other hand, the present invention provides a kind of anode composite material of lithium ion battery, through the invention the method system
It is standby to obtain.
Further, the thickness of the clad on the anode composite material of lithium ion battery surface is about 5nm.
On the other hand, the present invention provides a kind of anode, including compound with lithium ion cell positive of the present invention
Material is prepared for raw material.
On the other hand, the present invention provides a kind of battery, including anode of the present invention.
The present invention is dissolved in by tungsten source in medium, after being dispersed through agent PVP dispersions, is uniformly mixed with nickelic positive electrode,
While constantly evaporating solvent in heating process, tungsten source crystallizes or is adsorbed on the surface of nickelic positive electrode, and tungsten source cladding is uniform,
By high-temperature calcination so that tungsten source is converted into tungstate lithium and is coated on nickelic positive electrode surface, though the specific capacity of resulting materials does not increase
Add, but coat uniform, surface stability and greatly improve, and then chemical property is improved.
Beneficial effects of the present invention：
The present invention provides a kind of preparation method of anode composite material of lithium ion battery, the side coated by low temperature liquid phase
Method coats the surface of nickelic positive electrode using tungstate lithium.This method is compared to the mechanical mixtures mode such as ball milling, gained
Anode composite material of lithium ion battery clad homogeneity is good, and the tungstate lithium of cladding helps to improve the electrification of nickelic positive electrode
Performance is learned, especially in the cyclical stability of hot environment, building-up process of the invention is simple, of low cost, and electrification can be made
Learn the nickelic positive electrode of modification haveing excellent performance.
Description of the drawings
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the present invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the TEM collection of illustrative plates of sample in the embodiment of the present invention 1.
Fig. 2 is sample room temperature first charge-discharge curve graph in the embodiment of the present invention 1.
Fig. 3 is cycle performance figure of the sample under room temperature 2C multiplying powers in the embodiment of the present invention 1.
Fig. 4 is cycle performance figure of the sample at 55 DEG C under 2C multiplying powers in the embodiment of the present invention 1.
Fig. 5 is the XRD spectrum of sample in the embodiment of the present invention 2.
Fig. 6 is the XRD spectrum of sample in the embodiment of the present invention 3.
In figure：Voltage voltages, intensity intensity, specific capacity specific capacities, cycle number are followed
Number of rings, capacity capacity.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained belong to what the present invention protected
Range.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
Except there is a special instruction, the various reagents used in the present invention, raw material be can be commercially commodity or
Person can pass through product made from well known method.
Embodiment 1
Ammonium metatungstate 0.0088g (0.1wt%) is dissolved in 30 DEG C of 200ml ethanol waters, and (absolute ethyl alcohol is with water by volume
Than 1: 1 mixing) in, 0.1g PVP (polyvinylpyrrolidone) are then added, in the case where 30 degree of constant temperature is stirred continuously, are added thereto
10g Ni0.8Co0.1Mn0.1(OH)2Material simultaneously keeps temperature constant agitation 2h.It is evaporated in 80 DEG C of oil bath pans after being sufficiently stirred molten
Agent, being transferred at 80 DEG C of thermostatic drying chamber dry a whole night makes tungsten source crystallizes or is adsorbed on positive electrode surface to obtain forerunner
Body.Mixed lithium (mixed lithium be carry out lithium salts and presoma in the agate mortar dry-mixed) is carried out again, and lithium salts uses lithium hydroxide, hydrogen-oxygen
Change lithium dosage is 2.584g.Resulting materials are calcined after the completion of mixed lithium, 800 DEG C of sintering temperature, and sintering time 15 hours is natural
Cooling obtains covering material.
Its structure and Electrochemical Characterization are shown in Fig. 1, Fig. 2, Fig. 3 and Fig. 4.It can be seen that material surface has one layer from TEM figures
The tungstate lithium clad that uniform and thickness is about 5nm or so.Products therefrom is assembled into button cell, in voltage range 2.8-
Charge/discharge capacity is tested within the scope of 4.3V, within the scope of voltage range 2.8-4.3V.Charging and discharging curve does not have tungsten under 0.1C multiplying powers
Sour lithium charge and discharge platform illustrates that clad is not involved in removal lithium embedded, and the specific capacity for coating front and back material does not reduce.From material
2C circulations performance map and room temperature 2C cycles are as can be seen that the material circulation stability after cladding obtains very greatly at 55 DEG C
Enhancing, the especially thermal stability under high temperature.
Embodiment 2：
Tungsten trichloride 0.103g is dissolved in 200ml ethanol waters (absolute ethyl alcohol mixes at 1: 1 by volume with water), then
It adds in 0.1gPVP, 2h is stirred continuously for 30 degree in constant temperature, calculated for 1wt% with tungstate lithium covering amount, be charged with 10g
Ni0.5Co0.2Mn0.3(OH)2Material simultaneously keeps temperature constant.After being sufficiently stirred in 85 DEG C of oil bath pans solvent evaporated, be transferred to perseverance
Dry a whole night at 85 DEG C of warm drying box.Carrying out mixed lithium later, (mixed lithium is carry out lithium salts and presoma in the agate mortar dry
It is mixed) lithium salts is using lithium hydroxide, and dosage 2.494g, it is Ni to mix lithium amount0.5Co0.2Mn0.3(OH)2Contained in metal ion
1.01 times of mole, then calcined, 900 DEG C of sintering temperature, sintering time 16 hours, natural cooling obtains covering material.
XRD shows no tungstate lithium dephasign peak.
Embodiment 3：
Tungsten pentachloride 0.641g is dissolved in 200ml ethanol waters (absolute ethyl alcohol mixes at 1: 1 by volume with water), so
After add 0.1gPVP, be stirred continuously 2h in 30 degree of constant temperature, with tungstate lithium covering amount be 5wt% calculating be charged with 10g
Ni0.6Co0.2Mn0.2(OH)2Material simultaneously keeps temperature constant.The solvent evaporated in 90 DEG C of oil bath pans is transferred to thermostatic drying chamber 90
Dry a whole night at DEG C carries out mixed lithium (mixed lithium be carry out lithium salts and presoma in the agate mortar dry-mixed) lithium salts and uses later
Lithium carbonate, dosage 4.191g, it is Ni to mix lithium amount0.6Co0.2Mn0.2(OH)2Contained in 1.1 times of mole of metal ion,
It is calcined again, 850 DEG C of sintering temperature, 18 hours processing times, natural cooling obtains covering material.XRD shows no tungstate lithium
Dephasign peak.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of preparation method of anode composite material of lithium ion battery, which is characterized in that include the following steps：
1）After tungsten source is dissolved in solvent, PVP is added and disperses to form mixed solution；
2）Nickelic positive electrode is added into mixed solution, and solvent evaporated is heated after constant temperature stirring；
3）Step 2）Resulting materials carry out dry-mixed with lithium salts after being dried；
4）Dry-mixed resulting materials are calcined under aerobic conditions obtains the nickelic positive electrode of tungstate lithium cladding.
2. the preparation method of anode composite material of lithium ion battery according to claim 1, which is characterized in that the tungsten source
Including ammonium metatungstate, tungsten trichloride, tungsten pentachloride or combinations thereof.
3. the preparation method of anode composite material of lithium ion battery according to claim 1, which is characterized in that described nickelic
The chemical formula of positive electrode is LiNixM1-xO2, wherein：M is at least one of Co, Mn, Al, 0.8≤x≤1.
4. the preparation method of anode composite material of lithium ion battery according to claim 3, which is characterized in that described nickelic
The chemical formula of positive electrode includes Ni0.8Co0.1Mn0.1(OH)2、Ni0.6Co0.2Mn0.2(OH)2Or Ni0.5Co0.2Mn0.3(OH)2。
5. the preparation method of anode composite material of lithium ion battery according to claim 1, which is characterized in that the tungsten source
The mass percent for preparing gained tungstate lithium and nickelic positive electrode is 0.05% ~ 10%.
6. the preparation method of anode composite material of lithium ion battery according to claim 1, which is characterized in that the solvent
Including water, ethyl alcohol or combinations thereof；
The constant temperature stirring refers to carrying out constant temperature at 30 DEG C to stir 1 ~ 5h；
The temperature of the heating solvent evaporated is 80 ~ 90 DEG C；
The method of the drying includes vacuum drying, forced air drying, spray drying or its combination.
7. the preparation method of anode composite material of lithium ion battery according to claim 1, which is characterized in that the lithium salts
Dosage be step 2）1.0 ~ 1.1 times of the mole of metal ion in resulting materials；
The temperature of the calcining is 750 ~ 900 DEG C；
The time of the calcining is 15h ~ 18h；
The lithium salts includes lithium hydroxide or lithium carbonate.
8. a kind of anode composite material of lithium ion battery, which is characterized in that prepared by any method of claim 1 ~ 7
It obtains.
9. a kind of anode, which is characterized in that including anode composite material of lithium ion battery according to any one of claims 8 be raw material
It prepares.
10. a kind of battery, which is characterized in that including the anode described in claim 9.
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| CN109742336A (en) * | 2018-12-07 | 2019-05-10 | 北京理工大学 | A kind of surface layer coats the tertiary cathode material and preparation method of tungstate lithium and doping W |
| CN109768271A (en) * | 2018-12-29 | 2019-05-17 | 桂林电器科学研究院有限公司 | Modified LiNi0.7Co0.1Mn0.2O2The preparation method and product and battery of tertiary cathode material |
| CN111082026A (en) * | 2019-12-31 | 2020-04-28 | 中南大学 | Ternary cathode material coated with lithium tungstate and preparation method thereof |
| CN111129482A (en) * | 2019-08-14 | 2020-05-08 | 江苏正崴新能源科技有限公司 | Method for improving characteristics of lithium battery positive electrode material |
| CN114551794A (en) * | 2021-12-17 | 2022-05-27 | 远景动力技术(江苏)有限公司 | Positive electrode active material, positive electrode, preparation method and lithium ion battery |
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| CN109742336A (en) * | 2018-12-07 | 2019-05-10 | 北京理工大学 | A kind of surface layer coats the tertiary cathode material and preparation method of tungstate lithium and doping W |
| CN109768271A (en) * | 2018-12-29 | 2019-05-17 | 桂林电器科学研究院有限公司 | Modified LiNi0.7Co0.1Mn0.2O2The preparation method and product and battery of tertiary cathode material |
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| CN111082026A (en) * | 2019-12-31 | 2020-04-28 | 中南大学 | Ternary cathode material coated with lithium tungstate and preparation method thereof |
| CN114551794A (en) * | 2021-12-17 | 2022-05-27 | 远景动力技术(江苏)有限公司 | Positive electrode active material, positive electrode, preparation method and lithium ion battery |
| CN114551794B (en) * | 2021-12-17 | 2023-08-25 | 远景动力技术(江苏)有限公司 | Positive electrode active material, positive electrode, preparation method and lithium ion battery |
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Application publication date: 20180904 |
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