CN106450286B - A kind of nickel-cobalt lithium manganate material and preparation method thereof - Google Patents
A kind of nickel-cobalt lithium manganate material and preparation method thereof Download PDFInfo
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- CN106450286B CN106450286B CN201611200917.1A CN201611200917A CN106450286B CN 106450286 B CN106450286 B CN 106450286B CN 201611200917 A CN201611200917 A CN 201611200917A CN 106450286 B CN106450286 B CN 106450286B
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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
- 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
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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
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- 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
A kind of preparation method of nickel-cobalt lithium manganate material, using soluble nickel, cobalt, manganese salt as raw material, using coprecipitation reaction technique, it is characterized in that the molecular formula of the nickle cobalt lithium manganate is LiNixCoyMnzO2The specific process step that it is prepared is as follows; 1) coprecipitation reaction nickel cobalt manganese presoma adds water that mixed aqueous solution is made in nickel sulfate, cobaltous sulfate, manganese sulfate respectively in reaction kettle device; sodium hydrate aqueous solution is added and makees precipitating reagent; ammonium hydroxide is added, carries out coprecipitation reaction under heating and protective gas existence condition, filters to get filtrate and filter residue; filter residue cleaning, is made hydroxide nickel cobalt manganese presoma;2) nickle cobalt lithium manganate product processed is reacted, by the hydroxide nickel cobalt manganese presoma of preparation, drying is dry, it is sufficiently mixed after sieving with lithium salts stirring as hydroxide nickel cobalt manganese presoma and lithium salt mixture, hydroxide nickel cobalt manganese presoma and lithium salt mixture are filled into alms bowl, high temperature is fired, is broken, sieving, mixing, sieving, removing iron, packing and nickel-cobalt lithium manganate material is made, lithium ion battery is made in nickle cobalt lithium manganate product prepared by the present invention, has excellent security performance, high-temperature behavior and long circulation life.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, especially a kind of nickel-cobalt lithium manganate material and
Preparation method.
Background technique
Wireless communication, communications and transportation, aerospace is widely applied in a kind of battery of the lithium ion battery as novel green
Etc. various aspects, lithium ion battery is mainly by the transition metal oxide of for example embedding lithium of positive electrode, negative electrode material such as height graphite
The composition such as the carbon of change, diaphragm such as MIcroporous polyolefin film and electrolyte.And lithium ion anode material is to restrict lithium ion battery
The vital factor of various aspects of performance.
For anode material for lithium-ion batteries as one of the critical material in lithium ion battery, its performance quality directly can shadow
Ring the performance of entire performance of lithium ion battery.Therefore, it to solve the problem in lithium ion battery use or to improve lithium
When ion battery performance, researcher is mainly the performance and feature that can pay close attention to lithium ion battery plus-negative plate material.Existing market
Upper lithium ion anode material is more, mainly there is cobalt acid lithium, LiMn2O4 and LiFePO4.And the nickel cobalt manganese as tertiary cathode material
Sour lithium is shown one's talent in the positive electrode of various lithium batteries with its excellent performance, and super quality and competitive price etc., is used widely.
Chinese patent notification number be a kind of anode material lithium nickle cobalt manganic acid of lithium ion battery disclosed in CN103296270A and
Then and sodium hydroxide nickel, cobalt, manganese in sulfate is matched by mole and is configured to mixed aqueous solution for 1:1:1 by preparation method,
And ammonium hydroxide is reacted in reaction unit, while injecting nitrogen and water hydrazine, and it is aged, it filters, washing dries and hydroxide is made
Spherical nickel-cobalt mangaic acid lithium is made in nickel cobalt manganese product and lithium carbonate mixed sintering.
But compound is more, and reaction process step is too long, and simultaneous reactions process cannot automate in the presence of being added for the above method
Control.Manual operation large labor intensity, and reaction process is not easy to control.How reliable in quality is prepared, tertiary cathode material
The nickel-cobalt lithium manganate material for haveing excellent performance i.e. differentiation of nickle cobalt lithium manganate, preparation process whole-process automatic control, and prepare
Nickle cobalt lithium manganate properties of product are stablized.
On the other hand, the sintering procedure of nickle cobalt lithium manganate is the chemical reaction process under an oxidizing atmosphere, sintering procedure
In how to control oxygen concentration i.e. oxygen atmosphere, make reaction can be sufficiently carried out, be to prepare high-quality nickle cobalt lithium manganate material
The high nickel-cobalt lithium manganate material of one of key factor of material, especially nickel content, the requirement to oxygen atmosphere are higher.
Summary of the invention
The present invention seeks to provide a kind of nickel-cobalt lithium manganate material and preparation method thereof, with soluble nickel, cobalt, mn sulphate
For raw material, hydroxide nickel cobalt manganese presoma is made using coprecipitation reaction, after mixing with lithium carbonate, by optimizing sintering procedure
Oxidizing atmosphere, be fired in roller kilns, the nickel-cobalt lithium manganate material product of high quality be prepared.
A kind of preparation method of nickel-cobalt lithium manganate material of the present invention, using soluble nickel, cobalt, manganese salt as raw material, use is coprecipitated
Shallow lake reaction process, the molecular formula of the nickle cobalt lithium manganate are LiNixCoyMnzO2, wherein x+y+z=1;
The specific process step that it is prepared is as follows,
1) coprecipitation reaction nickel cobalt manganese presoma adds water respectively by nickel sulfate, cobaltous sulfate, sulphur in reaction kettle device
Sour manganese is made mixed aqueous solution, and sodium hydrate aqueous solution is added and makees precipitating reagent, ammonium hydroxide is added, and in heating and protective gas, there are items
Coprecipitation reaction is carried out under part, filters to get filtrate and hydroxide nickel cobalt manganese presoma is made in filter residue, filter residue cleaning;As needed
Nickel cobalt manganese ratio control mixed aqueous solution in nickel sulfate, cobaltous sulfate, manganese sulfate stoichiometric ratio;Control the reaction time be
12-20 hours, reaction temperature was 40-85 DEG C, while controlling ammonia concn in reaction process is 0.75-0.95mol/l, is reacted molten
Liquid pH is 10.5-12.5;
2) nickle cobalt lithium manganate product processed is reacted, by the hydroxide nickel cobalt manganese presoma of preparation, drying is dry, after sieving
It is sufficiently mixed with lithium salts stirring as hydroxide nickel cobalt manganese presoma and lithium salt mixture, by hydroxide nickel cobalt manganese presoma and lithium salts
Mixture fills alms bowl, and high temperature is fired, is broken, sieving, mixing, sieving, removing iron, being packaged as that nickel-cobalt lithium manganate material is made;Control is burnt
Time 20-36 hours processed, firing temperature was 600-1000 DEG C.
The present invention is preferably 2) the step hydroxide nickel cobalt manganese presoma and lithium salt mixture dress alms bowl, and it is control that high temperature, which is fired,
The mixture is made under the conditions of strong oxygen atmosphere in progress high temperature firing in baking apparatus;The strong oxygen atmosphere condition refers to
Active oxygen-increasing device will be set in mixture under the conditions of logical oxygen atmosphere in baking apparatus loaded on the mixture in alms bowl, by institute
It states active oxygen-increasing device and is placed in baking apparatus together loaded on the mixture in alms bowl and carry out releasing oxygen under high temperature firing condition
Gas is that mixture high temperature fires secondary oxygenation, forms strong oxygen atmosphere.
It further, be the active oxygen-increasing device include active automatic aerator and the chemical enhancement in active automatic aerator
Agent, the chemical enhancement agent are peroxide salt and/or permanganate.
It further, be the active oxygen-increasing device is high-temp-resistant micro crucible, the peroxide salt is sodium peroxide
And/or potassium peroxide and/or potassium permanganate.
It further, is that 1) cleaning of filter residue described in step is first rinsed using dilute alkaline aqueous solution, it is then clear with deionized water
The pH of filter residue is washed till lower than 8.5;The dilute alkaline aqueous solution is the sodium hydrate aqueous solution that concentration is 0.15-0.35mol/l.
Preferably, be the nickle cobalt lithium manganate preparation method overall process, temperature and pH value control, high temperature fire, dry
Drying is all made of artificial intelligence control;The high temperature is fired to be sintered using roller kilns, controls a length of 25-40 of roller-way of roller kilns
Rice.
Preferably, be 2) be crushed described in step, sieving, dry packing be using corundum roller pair breaking device it is broken after be sent into vibration
It is dynamic to be sieved through sieve, the nickle cobalt lithium manganate for reaching granularity sieve under, then through far-infrared ray drying, after further water is adsorbed in removing, into complete
Automatic vacuum packaging device bagging and packaging is to nickle cobalt lithium manganate LiNixCoyMnzO2, the wherein product of x+y+z=1;Object on sieve
Material returns to crushing device using the square law device of air-flow conveying and is crushed again;Controlling the granularity is 6-13 microns.
It preferably, is the 1) step in reaction kettle device, before the addition of each material, in bottom material is added in reaction kettle device
Liquid, the addition bottom material liquid accounts for the 20-25% of reaction kettle device effective volume, while the effective ingredient for controlling the bottom material liquid is
Ammonium hydroxide and/or sodium hydroxide solution, the ammonium hydroxide and concentration of sodium hydroxide solution controlled in bottom material liquid is 0.2-0.4 mol/l.
It further, is to control the concentration of sodium hydroxide solution 1) as 6.5-7.5mol/l;The addition ammonia concn is
10-30Wt%。
Nickel-cobalt lithium manganate material of the present invention is prepared according to methods described above.
The method of the present invention processing step is as follows: nickel cobalt manganese sulfate liquor preparation+aqueous slkali preparation → coprecipitation reaction →
Filters pressing cleaning → detection, drying → hydroxide nickel cobalt manganese presoma → mixing lithium salts → pressure alms bowl (provide oxygen in dress alms bowl material
Source) → fire → broken → crushing → sieving → mixing → sieving → remove iron → packaging nickle cobalt lithium manganate product.
(stoichiometric ratio of nickel cobalt manganese is 5:2:3 to the nickle cobalt lithium manganate of the method for the present invention preparation, and chemical formula is
LiNi0.5Co0.2Mn0.3O2) product detects through relevant departments, all technical is shown in Table 1 as follows, storage, traffic condition, shady and cool,
It is dry, moisture-proof, damp proof.
Table 1
Illustrate, lithium ion battery is made in nickle cobalt lithium manganate product prepared by the present invention, has excellent security performance, high temperature
Performance and long circulation life.
Detailed description of the invention:
Fig. 1, for using a kind of nickel-cobalt lithium manganate material LiNi of the method for the present invention preparation0.5Co0.2Mn0.3O2Product granularity
Distribution map;
Fig. 2, for using a kind of nickel-cobalt lithium manganate material LiNi of the method for the present invention preparation0.5Co0.2Mn0.3O2Product SEM
Figure;
Fig. 3, for using a kind of nickle cobalt lithium manganate LiNi of the method for the present invention preparation0.5Co0.2Mn0.3O2Product XRD diagram.
Specific embodiment: the present invention is described in further detail With reference to embodiment, it should be understood that this
Invention foregoing general description and subsequent specific embodiment be it is exemplary and illustrative, for claimed invention
Further explanation is provided.Stoichiometric ratio described in the present embodiment is quality molar ratio.
Mixture described in 1 the present embodiment of embodiment is also the mixture of hydroxide nickel cobalt manganese and lithium carbonate, will be mixed
Object fills in alms bowl in saggar, in the interior i.e. alms bowl of saggar, similarly hereinafter.
The present embodiment 1 is to prepare a kind of nickel-cobalt lithium manganate material, the nickel cobalt manganese chemistry meter of the material using the method for the present invention
Amount is than being 8:1:1, chemical formula LiNi0.8Co0.1Mn0.1O2, using soluble nickel, cobalt, manganese salt as raw material, specific process step
As follows, 1) coprecipitated reaction precursor of nickel-cobalt-lithium-manganese-oxide processed adds water to distinguish using soluble nickel, cobalt sulfate and manganese chloride as raw material
Be made nickel, cobalt, manganese salt mixed aqueous solution, be added sodium hydrate aqueous solution make precipitating reagent, complexing agent is made with ammonium hydroxide, heating and
Coprecipitated reaction is carried out under alkali existence condition, is filtered to get filtrate and filter residue, before hydroxide nickel cobalt manganese is made in the once purged drying of filter residue
Drive body;The molar ratio of nickel, cobalt, manganese in control mixed aqueous solution is 8:1:1, total concentration 2.0mol/L, controls the reaction time
It is 20 hours, reaction temperature is 50 DEG C, reaction solution pH is 11.0.
2) by the hydroxide nickel cobalt manganese presoma (Ni of preparation0.8Co0.1Mn0.1(OH)2) and lithium carbonate be sufficiently mixed, hydrogen-oxygen
Change nickel cobalt manganese and carbonic acid lithium mixture to fill in alms bowl in saggar, high temperature firing is carried out under the conditions of strong oxygen atmosphere, that is, is existed
It is inserted into miniature crucible in the mixture of hydroxide nickel cobalt manganese and lithium carbonate, is put into sodium peroxide in miniature crucible, installs the above object
The saggar of material, which is put into furnace, carries out high temperature firing.Product after firing is crushed, is crushed, sieving, mixing, sieving, removing iron, packet
Dress, obtains LiNi0.8Co0.1Mn0.1O2Material.The control firing time 24 hours, sintering temperature are 750 DEG C.Control the mixture
In progress high temperature firing in baking apparatus, that is, furnace under the conditions of strong oxygen atmosphere;The strong oxygen atmosphere condition refers to will be loaded on alms bowl
Interior mixture sets active oxygen-increasing device under the conditions of logical oxygen atmosphere in baking apparatus in mixture, and the activity is increased
Oxygen device and being placed in baking apparatus together loaded on the intracorporal mixture of alms bowl carries out under high temperature firing condition that release oxygen be mixed
It closes object high temperature and fires secondary oxygenation, form strong oxygen atmosphere.
It is so-called to form strong oxygen atmosphere, refer to the chemistry in the active automatic aerator of the active oxygen-increasing device in mixture
Oxygenation agent such as sodium peroxide, the oxygen released with the raising sodium peroxide of the firing temperature in baking apparatus with loaded on bowl
Interior mixture comes into full contact with, and under the ambient conditions of logical oxygen, the oxygen concentration of reaction is increased, and is formed to mixture
Secondary oxygenation makes the abundant reaction of hydroxide nickel cobalt manganese presoma and lithium carbonate that the high chemical property of nickel content be prepared excellent
Nickel-cobalt lithium manganate material of the invention.
Raw material specification needed for the present invention is as follows, nickel sulfate, cobaltous sulfate, and manganese sulfate or manganese chloride, lithium carbonate are LITHIUM BATTERY;
Liquid alkaline, technical grade, mass concentration 32%;Ammonium hydroxide, technical grade, mass concentration 20%.
Specific process step process is as follows:
(1) raw material preparation of coprecipitation reaction
The reaction nickel sulfate, cobaltous sulfate, manganese chloride raw material of above-mentioned quality will be bought by market, are sent into raw material storage storage,
It is conveyed into respectively in the nickel sulfate, cobaltous sulfate, manganese chloride feed bin reaction unit in raw material workshop on demand, is reduced and is claimed with electronics
It takes, intermediate storage tank is sent into the example supplying dissolving tank amount of reordering pure water dissolution in mass ratio.Raw material liquid alkaline is sent into former after being bought by market
Expect library storage, be incorporated the dissolving tank amount of reordering pure water in proportion with electronic measuring balance, it is spare to be sent into intermediate storage tank.Ammonium hydroxide is purchased by market
Enter, is sent into ammonia water tank storage.Ammonium hydroxide is configured to the ammonium hydroxide of normal concentration on demand, it is spare to be sent into intermediate storage tank.
(2) prepared by hydroxide nickel cobalt manganese precursor
Each reactant is flowed into each coprecipitated reaction kettle device by setting flow by computer DCS control system respectively, altogether
Heavy reaction is completed in the reaction kettle that several are connected in series, and each reaction kettle, which is controlled by technique requirement by computer DCS, is
System quantitatively feeds nickel, cobalt, manganese mixed solution and ammonium hydroxide.The concentration for controlling sodium hydroxide solution simultaneously is 6.5-7.5mol/l;Institute
Stating and ammonia concn is added is 10Wt%.
Equipped with the pH meter continuously detected in each reaction kettle, computer is carried out according to the pH value of detection and the pH value of setting
Comparison, accurately passes through the specified rate of mass flow controller adjust automatically sodium hydroxide solution using artificial intelligence control algorithm,
Carry out reaction in the pH value range of setting always, it is ensured that the synthesis quality of precursor.It is come out by coprecipitated reaction kettle coprecipitated
Shallow lake reaction slurry removes foreign ion through over cleaning, and cleaning Shi Xianyong dilute alkaline aqueous solution is cleaned, then washed with clear water,
The pH for controlling material is lower than 8.5.The slurry washed, is sent into dry in dryer device, controls drying temperature at 95 DEG C or more,
It is generally 95-100 DEG C, 15-20 hours dry, guarantee that the crystallization water in precursor does not decompose.Scrub raffinate is sent into sewage treatment
It stands, is sent into sewage treatment plant's processing rear outlet up to standard after sloughing ammonia nitrogen ion using ammonia still process method.
(3) nickle cobalt lithium manganate LiNi0.8Co0.1Mn0.1O2Finished product synthesis
Upper step is dried to the hydroxide nickel cobalt manganese precursor of prescribed requirement and above-mentioned lithium carbonate is respectively fed to production vehicle
Between presoma and lithium carbonate device in, the mass ratio for controlling precursor of nickel-cobalt-lithium-manganese-oxide and lithium carbonate is 1:1.05-1.1.It is logical
It crosses after electronics decrement claims accurate dosing and is sent into mixing device, alms bowl is filled after mixing well.It controls each equipped in mixture alms bowl
If being uniformly provided with dry active oxygen-increasing device, it is equipped with and required high temperature in each active automatic aerator for constituting active oxygen-increasing device
The chemical enhancement agent of the matched several mass parts of mixture requisite oxygen gas phase of firing, the activity automatic aerator is miniature crucible,
The chemical enhancement agent is sodium peroxide.
I.e. by the mixture of hydroxide nickel cobalt manganese and lithium carbonate in the alms bowl, in the mixed of hydroxide nickel cobalt manganese and lithium carbonate
It closes in object and is inserted into miniature crucible, control crucible height 45mm, diameter 15mm is uniformly distributed in each alms bowl equipped with 4-6 only miniature earthenware
Crucible, each miniature crucible is interior to be equipped with 3-5 grams of sodium peroxide.The saggar for installing the above material fills alms bowl and is put into progress high temperature burning in furnace
System.It is then fed into progress high temperature firing in roller kilns, maximum temperature section is 750 DEG C.Positive electrode made of being fired as roller kilns
That is LiNi0.8Co0.1Mn0.1O2Nickle cobalt lithium manganate is sent into pulverizer after corundum roller pair breaking crusher machine and is crushed, then through vibrating screen
Sieving reaches LiNi under the sieve of 6-13 microns of granularity requirements0.8Co0.1Mn0.1O2Nickle cobalt lithium manganate, material again through mixing, sieving,
Except iron, packaging obtain LiNi0.8Co0.1Mn0.1O2Nickle cobalt lithium manganate product.Product is sent into product library and stores export trade.
Due in sintering procedure, making have sufficient oxygen atmosphere when material reaction using the method for the present invention,
Ni0.8Co0.1Mn0.1(OH)2And Li2CO3It is able to carry out abundant reaction, in material+trivalent nickel ion can also be stabilized, also have
The residual lithium in surface of material is controlled to effect, final products can play excellent chemical property.
Embodiment 2
Product LiNi prepared by the present embodiment 20.5Co0.2Mn0.3O2For such as table 1 of each performance described in it, product is prepared
Molecular formula is nickel-cobalt lithium manganate material LiNi0.5Co0.2Mn0.3O2, the stoichiometric ratio for controlling nickel cobalt manganese is 5:2:3, preparation side
Method and step are the same as implementation 1.
Claims (5)
1. a kind of preparation method of nickel-cobalt lithium manganate material, using soluble nickel, cobalt, manganese salt as raw material, using coprecipitated reaction process,
It is characterized in that the molecular formula of the nickle cobalt lithium manganate is LiNixCoyMnzO2, wherein x+y+z≤1;
The specific process step that it is prepared is as follows,
1) coprecipitated reaction nickel cobalt manganese presoma processed adds water that nickel sulfate, cobaltous sulfate, manganese sulfate are made mixed in reaction kettle device
Heshui solution is added sodium hydrate aqueous solution and makees precipitating reagent, ammonium hydroxide is added, is total under heating and protective gas existence condition
Heavy reaction, filters to get filtrate and hydroxide nickel cobalt manganese presoma is made in filter residue, filter residue cleaning;Nickel cobalt manganese ratio as needed
The stoichiometric ratio of nickel sulfate, cobaltous sulfate, manganese sulfate in control mixed aqueous solution;Controlling the reaction time is 12-20 hours, instead
Answering temperature is 40-85 DEG C, while controlling ammonia concn in reaction process is 0.75-0.95mol/l, and reaction solution pH is 10.5-
12.5;
2) nickle cobalt lithium manganate product processed is reacted, by the hydroxide nickel cobalt manganese presoma of preparation, drying is dry, after sieving and lithium
Salt stirring is sufficiently mixed as hydroxide nickel cobalt manganese presoma and lithium salt mixture, and hydroxide nickel cobalt manganese presoma and lithium salts are mixed
Object fills alms bowl, and high temperature is fired, is broken, sieving, mixing, sieving, removing iron, being packaged as that anode material nickel cobalt manganic acid lithium is made;Control is burnt
Time 20-36 hours processed, firing temperature was 600-1000 DEG C;
The step 2 hydroxide nickel cobalt manganese presoma and lithium salt mixture fill alms bowl, and high temperature is fired, and are that the control mixture exists
In progress high temperature firing in baking apparatus under the conditions of strong oxygen atmosphere;The strong oxygen atmosphere condition refers to will be loaded on mixed in alms bowl
It closes object and sets active automatic aerator in mixture under the conditions of logical oxygen atmosphere in baking apparatus, by the active automatic aerator and dress
It is placed in progress high temperature firing in baking apparatus together in the intracorporal mixture of alms bowl, releases oxygen, forms secondary oxygenation, is formed strong
Oxygen atmosphere;
The activity automatic aerator includes active oxygen-increasing device and the chemical enhancement agent set on active oxygen-increasing device, the chemical enhancement
Agent is sodium peroxide and/or potassium peroxide and/or potassium permanganate.
2. a kind of preparation method of nickel-cobalt lithium manganate material according to claim 1, activity oxygen-increasing device described in feature
For high-temp-resistant micro crucible.
3. the preparation method of a kind of nickel-cobalt lithium manganate material according to claim 1, it is characterized in that control mixed aqueous solution
In nickel sulfate, cobaltous sulfate, manganese sulfate mass ratio be 1500-1800:580-650:320-380.
4. the preparation method of a kind of nickel-cobalt lithium manganate material according to claim 1, it is characterized in that described in the step 1)
Filter residue cleaning, which refers to, to be first rinsed using dilute alkaline aqueous solution, is then cleaned to the pH of filter residue with deionized water lower than 8.5;It is described
Dilute alkaline aqueous solution is the sodium hydrate aqueous solution that concentration is 0.15-0.35mol/l.
5. the preparation method of a kind of nickel-cobalt lithium manganate material according to claim 1, it is characterized in that the nickle cobalt lithium manganate
Preparation method overall process, be all made of artificial intelligence control;The high temperature is fired to be sintered using roller kilns, controls roller kilns
Roller-way is 25-40 meters a length of.
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CN107799762B (en) * | 2017-09-28 | 2021-01-08 | 华南理工大学 | Preparation method of nickel-cobalt-manganese ternary positive electrode material for improving first discharge efficiency of lithium ion battery |
CN109888269A (en) * | 2018-12-29 | 2019-06-14 | 广东邦普循环科技有限公司 | A kind of pretreated method of ternary material mixing |
CN112624212A (en) * | 2020-12-18 | 2021-04-09 | 江西汉尧富锂科技有限公司 | Carbon-doped nickel hydroxide cobalt manganese material and preparation method thereof |
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CN105870409A (en) * | 2016-04-08 | 2016-08-17 | 浙江新时代海创锂电科技有限公司 | Preparation method of nickel-cobalt-manganese ternary positive electrode material and lithium-ion battery |
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