CN108807881A - A kind of body mutually mixes the preparation method of aluminium cobaltosic oxide - Google Patents
A kind of body mutually mixes the preparation method of aluminium cobaltosic oxide Download PDFInfo
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- CN108807881A CN108807881A CN201810490073.1A CN201810490073A CN108807881A CN 108807881 A CN108807881 A CN 108807881A CN 201810490073 A CN201810490073 A CN 201810490073A CN 108807881 A CN108807881 A CN 108807881A
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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
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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
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- 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 invention discloses the preparation methods that a kind of body mutually mixes aluminium cobaltosic oxide, belong to technical field of lithium ion.This method is using certain density cobalt liquor as cobalt source, sodium hydroxide solution is precipitating reagent, ammonia spirit is complexing agent, hydrazine hydrate solution is reducing agent, aluminium salt ethanol solution is that dopant carries out synthetic reaction, in reaction process, participation reaction in reaction kettle is added in aluminium salt ethanol solution by disperseing liquid feeding mode；After synthetic reaction under the conditions of certain pH value, synthetic product is oxidized to hydroxy cobalt oxide using hydrogen peroxide solution, then by mixture washing, dry, calcining, the equally distributed body of aluminium element is obtained and mutually mixes aluminium cobaltosic oxide product, production efficiency is high.It uses the body that the method for the present invention is prepared mutually to mix aluminium cobaltosic oxide product and mixes aluminum amount for 0.5-1%, and aluminium element is uniformly distributed, laser particle size is 15-20 μm, Zhen Shi Mi Du≤2.5g/cm3, specific surface area 1.0-3.0m2/ g, in blocky or spherical pattern.
Description
Technical field
The invention belongs to technical field of lithium ion, specifically a kind of to be used to prepare ion cell anode material lithium cobaltate
The body of lithium mutually mixes the preparation method of aluminium cobaltosic oxide.
Background technology
Using cobalt acid lithium being the lithium ion battery prepared by positive electrode has that light-weight, capacity is big, higher than energy, work is electric
Pressure is high, electric discharge is steady, is suitble to the features such as heavy-current discharge, good cycle, long lifespan, is mainly used in 3C digital domains.
Cobalt acid lithium just develops towards the direction of high voltage, high-pressure solid, high circulation performance, therefore, to the oxidation of raw material four three
The requirement of cobalt is also higher and higher.Co3O4It is a kind of functional material with special construction and performance, conventional Co3O4Market face
Face the present situation of gradually atrophy, big granularity, doping Co3O4The market demand gradually highlight.How research, which prepares the big granularity of high-performance, is mixed
Miscellaneous cobaltosic oxide has become hot spot.
Chinese invention patent（201510881580.4）Disclose a kind of " system of big grain size high-density spherical cobaltic-cobaltous oxide
Preparation Method ", specific method are, by cobalt carbonate made from multiple circulation crystallization, will to pass through segmented heat in cobalt carbonate synthesis phase
It decomposes, makes cobalt carbonate exploded in the low temperature predecomposition stage, form micro channel, in the high temperature thermal decomposition stage, particle surface
Densification, to which big grain size high-density spherical cobaltic-cobaltous oxide be prepared.This method needs multiple in cobalt carbonate synthesis phase
Circulation crystallization, process is cumbersome, is unfavorable for industrialized production.
In view of the above technical problems, the Chinese invention patent of 106587170 A of Publication No. CN discloses a kind of " body phase
The cobaltosic oxide preparation method of rare earth doped element ", this method go out the sediment of doped chemical by Moist chemical synthesis, then by hydrogen
Cobalt oxide is oxidized to hydroxy cobalt oxide, finally by calcining, obtains bulk phase-doped cobaltosic oxide product.But this method for
When mixing the preparation of aluminium cobalt acid lithium, aluminium salt and alkaline reaction speed are fast, there are aluminium and cobalt precipitation it is uneven, so as to cause four oxidation three
The problem of aluminium element is unevenly distributed in cobalt.In addition, the compound of cobalt is very easy to oxidation, the cobalt compound after oxidation can interfere
The fast-growth of synthetic product, therefore, there is also the relatively low problems of production efficiency for this method.
Invention content
The purpose of the invention is to overcome the shortcomings of above-mentioned prior art, provide that a kind of production efficiency is high, four oxidations three
The body that aluminium element is evenly distributed inside cobalt mutually mixes the preparation method of aluminium cobaltosic oxide.
The purpose of the present invention is what is be achieved through the following technical solutions：Using certain density cobalt liquor as cobalt source, hydroxide
Sodium solution is precipitating reagent, and ammonia spirit is complexing agent, and hydrazine hydrate solution is reducing agent, and aluminium salt ethanol solution is that dopant is closed
At reaction, in reaction process, aluminium salt ethanol solution is added in reaction kettle by disperseing liquid feeding mode and participates in reacting；Synthesis
After reaction under the conditions of certain pH value, synthetic product is oxidized to hydroxy cobalt oxide using hydrogen peroxide solution, then will be mixed
Object washing, dry, calcining are closed, the equally distributed body of aluminium element is obtained and mutually mixes aluminium cobaltosic oxide product.Specifically include following step
Suddenly：
A, the preparation of solution
Using cobalt salt as raw material, it is solution A to be configured to the cobalt liquor that cobalt concentration is 1-2mol/L；Compound concentration is the hydrogen of 2-6mol/L
Sodium hydroxide solution is B solution；Compound concentration is the ammonia spirit of 5-10mol/L, and 5-20mL bodies are added in every liter of ammonia spirit
The hydrazine hydrate solution that fraction is 30% is C solution；The hydrogen peroxide solution that compound concentration is 5-10mol/L is solution D；It prepares dense
The aluminium salt ethanol solution that degree is 4-8g/L is E solution；
B, synthetic reaction
So that solution A, B solution and C solution cocurrent is entered reaction kettle, while E solution is added, in the stirring of 200-500r/min
Under reacted, obtain cobalt hydroxide；
C, oxidation reaction
B, solution D are continuously added in cobalt hydroxide in a kettle, are reacted under the stirring of 200-500r/min,
Cobalt hydroxide is set to be changed into hydroxy cobalt oxide；Wherein, reaction temperature is 70-80 DEG C, reaction time 1-2h, and solution D addition is A
0.5-0.6 times of solution addition is 10-11 by adjusting B solution flow control solution ph；
D, it is filtered, washed and dries
After oxidation reaction, material in reaction kettle is filtered, 80-100 DEG C of deionized water pulping and washing, 100-400 DEG C
Lower drying obtains mixing aluminium cobaltosic oxide precursor；
E, it calcines
The calcining of aluminium cobaltosic oxide precursor will be mixed, body is obtained and mutually mixes aluminium cobaltosic oxide product.
As the further preferred of technical solution of the present invention, in step a, cobalt salt is in cobaltous sulfate, cobalt nitrate, cobalt chloride
One or more of mixtures, aluminium salt ethanol solution are the ethanol solution of alchlor or aluminum nitrate.
In synthetic reaction process, a concentration of 5-10g/L of ammonia spirit is controlled, reaction temperature is 70-80 DEG C, solution A flow velocity
For 300L/h, B solution flow velocity is adjusted according to ammonia spirit concentration, and C solution flow velocity is 320-340L/h, and E solution flow rates are 30L/
H, reaction time 15-20h.
In synthetic reaction process, the liquid feeding mode of E solution is that E solution charging lines are divided into 6-9 tiny pipelines,
Each thin charging line liquid outlet is fixed to middle part or the tail portion dispersion liquid feeding of reaction kettle stirrer paddle.
Calcination process is, under the conditions of opening, 4-8h is calcined with 700-800 DEG C of calcination temperature.
Compared with the prior art, the advantageous effect of technical solution of the present invention is：
1. the compound of cobalt is very easy to oxidation, the cobalt compound after oxidation can prevent the quick of synthetic product
Growth, causes the laser particle size of final products to be not easy to grow up, and body of the present invention mutually mixes the preparation method of aluminium cobaltosic oxide,
It is reducing agent by the way that the hydrazine hydrate that volume fraction is 30% is added, cobalt compound can be prevented to aoxidize, and then promotes the quick of product
It grows up, improves production efficiency.
2. mix aluminium cobaltosic oxide with Co deposited synthesis, due to Al (OH)3Solubility product constant at normal temperatures is much
Less than Co (OH)2Solubility product constant, and Al3+It is difficult that complex reaction occurs with ammonium hydroxide, leads to Al in solution3+Settling rate it is remote
Far faster than Co2+, cause that Al elements are unevenly distributed in presoma and granular precursor is difficult to grow up.The present invention uses aluminium salt is molten
In method of the absolute ethyl alcohol as dopant solution, after ethanol solution need are miscible with water, aluminium salt could participate in reacting, and slow down
Al3+Settling rate, solve due to Al (OH)3Solubility product constant is too small and reacts violent, and aluminium cannot be asked with what cobalt was co-precipitated
Topic；And by the way that aluminium salt ethanol solution charging line is divided into 6-9 small sized pipeline, each thin charging line liquid outlet is fixed
In the middle part of to stirring blade or tail portion disperses the method for liquid feeding, makes Al in building-up process3+Reaction kettle can be rapidly and uniformly distributed to
Middle participation reaction ensure that and prepare being uniformly distributed for aluminium element in product.
3, it uses the body that the method for the present invention is prepared mutually to mix aluminium cobaltosic oxide product and mixes aluminum amount for 0.5-1%, and aluminium element
It is uniformly distributed, laser particle size is 15-20 μm, Zhen Shi Mi Du≤2.5g/cm3, specific surface area 1.0-3.0m2/ g, in blocky or class ball
Shape pattern.
Description of the drawings
Fig. 1 is the testing result of the product synthesized using method in the embodiment of the present invention 1；
Fig. 2 is the testing result of the product synthesized using method in the embodiment of the present invention 2；
Fig. 3 is the testing result of the product synthesized using method in the embodiment of the present invention 3.
Specific implementation mode
The preparation method work for mixing the present invention aluminium cobaltosic oxide by specific embodiment below in conjunction with the accompanying drawings is further detailed
It describes in detail bright.
Embodiment 1
The cobalt chloride solution that compound concentration is 1mol/L is solution A；The sodium hydroxide solution that compound concentration is 2mol/L is B molten
Liquid；Compound concentration is the ammonia spirit of 5mol/L, and it is molten that the hydrazine hydrate that 5mL volume fractions are 30% is added in every liter of ammonia spirit
Liquid is C solution；The hydrogen peroxide solution that compound concentration is 5mol/L is solution D；Compound concentration is the anhydrous second of alchlor of 4g/L
Alcoholic solution is E solution.
When synthetic reaction starts, solution A, B solution and C solution cocurrent is made to enter reaction kettle, while by E solution charging lines
It is divided into 6-9 tiny pipelines, each thin charging line liquid outlet is fixed to middle part or the portion of reaction kettle stirrer paddle
It dissipates and E solution is added, reacted under the stirring of 500r/min, it is 8.0 that pH value in reaction is controlled in reaction process, reaction temperature
Degree is 70 DEG C, and solution A flow velocity is 300L/h, and B solution flow velocity is adjusted according to pH value in reaction, and C solution flow velocity is 30L/h, E solution
Flow velocity is 30L/h, and the reaction time, 15h obtained cobalt hydroxide.
After synthetic reaction, B, solution D are continuously added in cobalt hydroxide in a kettle, in the stirring of 500r/min
Oxidation reaction is carried out under state, and cobalt hydroxide is made to be changed into hydroxy cobalt oxide；Wherein, reaction temperature is 70 DEG C, reaction time 1h,
Solution D addition is 0.5 times of solution A addition, is 10 by adjusting B solution flow control solution ph.
After oxidation reaction, material in reaction kettle is filtered, 80 DEG C of deionized water pulping and washings, is done at 200 DEG C
It is dry, it obtains mixing aluminium cobaltosic oxide precursor.
Aluminium cobaltosic oxide precursor will be mixed and calcine 4h under the conditions of not being passed through 800 DEG C of openings of oxidizing gas, obtained
Body mutually mixes aluminium cobaltosic oxide product, and product index is as shown in Figure 1.Prepare using the invention that mix aluminum amount be 0.5% to mix
Aluminium cobaltosic oxide product, and doped chemical is uniformly distributed, laser particle size is 17 μm, Zhen Shi Mi Du≤2.5g/cm3, specific surface
Product 1.0-3.0m2/ g is in bulk morphologies.
Embodiment 2
The cobalt sulfate solution that compound concentration is 1.5mol/L is solution A；The sodium hydroxide solution that compound concentration is 4mol/L is B molten
Liquid；Compound concentration is the ammonia spirit of 8mol/L, and it is molten that the hydrazine hydrate that 15mL volume fractions are 30% is added in every liter of ammonia spirit
Liquid is C solution；The hydrogen peroxide solution that compound concentration is 6mol/L is solution D；Compound concentration is the aluminum nitrate absolute ethyl alcohol of 6g/L
Solution is E solution.
When synthetic reaction starts, solution A, B solution and C solution cocurrent is made to enter reaction kettle, while by E solution charging lines
It is divided into 6-9 tiny pipelines, each thin charging line liquid outlet is fixed to middle part or the portion of reaction kettle stirrer paddle
It dissipates and E solution is added, reacted under the stirring of 400r/min, control control pH value in reaction is 8.5 in reaction process, instead
It is 75 DEG C to answer temperature, and solution A flow velocity is 300L/h, and B solution flow velocity is adjusted according to pH value in reaction, and C solution flow velocity is 40L/h, E
Solution flow rate is 30L/h, reaction time 18h, obtains mixing aluminium cobalt hydroxide.
After synthetic reaction, B, solution D are continuously added in cobalt hydroxide in a kettle, in the stirring of 400r/min
Oxidation reaction is carried out under state, and cobalt hydroxide is made to be changed into hydroxy cobalt oxide；Wherein, reaction temperature is 75 DEG C, the reaction time
1.5h, solution D addition are 0.6 times of solution A addition, are 10.5 by adjusting B solution flow control solution ph.
After oxidation reaction, material in reaction kettle is filtered, 90 DEG C of deionized water pulping and washings, is done at 300 DEG C
It is dry, it obtains mixing aluminium cobaltosic oxide precursor.
Aluminium cobaltosic oxide precursor will be mixed and calcine 6h under the conditions of not being passed through 750 DEG C of openings of oxidizing gas, obtained
Body mutually mixes aluminium cobaltosic oxide product, and product index is as shown in Figure 2.Aluminium 0.75% is mixed using what the method for the present invention had been prepared
Cobaltosic oxide product, and doped chemical is uniformly distributed, and laser particle size is 15-20 μm, Zhen Shi Mi Du≤2.5g/cm3, compare table
Area 1.0-3.0m2/ g, in blocky or spherical pattern.
Embodiment 3
The cobalt nitrate solution that compound concentration is 2mol/L is solution A；The sodium hydroxide solution that compound concentration is 6mol/L is B molten
Liquid；Compound concentration is the ammonia spirit of 10mol/L, and the hydrazine hydrate that 20mL volume fractions are 30% is added in every liter of ammonia spirit
Solution is C solution；The hydrogen peroxide solution that compound concentration is 8mol/L is solution D；Compound concentration is that the alchlor of 8g/L is anhydrous
Ethanol solution is E solution.
When synthetic reaction starts, solution A, B solution and C solution cocurrent is made to enter reaction kettle, while by E solution charging lines
It is divided into 6-9 tiny pipelines, each thin charging line liquid outlet is fixed to middle part or the portion of reaction kettle stirrer paddle
It dissipates and E solution is added, reacted under the stirring of 300r/min, control control pH value in reaction is 9.0 in reaction process, instead
It is 80 DEG C to answer temperature, and solution A flow velocity is 300L/h, and B solution flow velocity is adjusted according to pH value in reaction, and C solution flow velocity is 60L/h, E
Solution flow rate is 30L/h, reaction time 20h, obtains mixing aluminium cobalt hydroxide.
After synthetic reaction, B, solution D are continuously added in cobalt hydroxide in a kettle, in the stirring of 300r/min
Oxidation reaction is carried out under state, and cobalt hydroxide is made to be changed into hydroxy cobalt oxide；Wherein, reaction temperature is 80 DEG C, reaction time 2h,
Solution D addition is 0.55 times of solution A addition, is 11 by adjusting B solution flow control solution ph.
After oxidation reaction, material in reaction kettle is filtered, 100 DEG C of deionized water pulping and washings, is done at 400 DEG C
It is dry, it obtains mixing aluminium cobaltosic oxide precursor.
Aluminium cobaltosic oxide precursor will be mixed and calcine 8h under the conditions of not being passed through 700 DEG C of openings of oxidizing gas, obtained
Body mutually mixes aluminium cobaltosic oxide product, and product index is as shown in Figure 3.Mix aluminium 1% four prepared using the method for the present invention
Co 3 O product, and doped chemical is uniformly distributed, laser particle size is 15-20 μm, Zhen Shi Mi Du≤2.5g/cm3, specific surface area
1.0-3.0m2/ g, in blocky or spherical pattern.
Claims (6)
1. a kind of body mutually mixes the preparation method of aluminium cobaltosic oxide, it is characterized in that, this approach includes the following steps：
A, the preparation of solution
Using cobalt salt as raw material, it is solution A to be configured to the cobalt liquor that cobalt concentration is 1-2mol/L；Compound concentration is the hydrogen of 2-6mol/L
Sodium hydroxide solution is B solution；Compound concentration is the ammonia spirit of 5-10mol/L, and 5-20mL bodies are added in every liter of ammonia spirit
The hydrazine hydrate solution that fraction is 30% is C solution；The hydrogen peroxide solution that compound concentration is 5-10mol/L is solution D；It prepares dense
The aluminium salt ethanol solution that degree is 4-8g/L is E solution；
B, synthetic reaction
So that solution A, B solution and C solution cocurrent is entered reaction kettle, while E solution is added, in the stirring of 200-500r/min
Under reacted, obtain mixing aluminium cobalt hydroxide；
C, oxidation reaction
B, solution D are continuously added in cobalt hydroxide in a kettle, are reacted under the stirring of 200-500r/min,
Cobalt hydroxide is set to be changed into hydroxy cobalt oxide；Wherein, reaction temperature is 70-80 DEG C, reaction time 1-2h, and solution D addition is A
0.5-0.6 times of solution addition is 10-11 by adjusting B solution flow control solution ph；
D, it is filtered, washed and dries
After oxidation reaction, material in reaction kettle is filtered, 80-100 DEG C of deionized water pulping and washing, 100-400 DEG C
Lower drying obtains mixing aluminium cobaltosic oxide precursor；
E, it calcines
The calcining of aluminium cobaltosic oxide precursor will be mixed, body is obtained and mutually mixes aluminium cobaltosic oxide product.
2. a kind of body according to claim 1 mutually mixes the preparation method of aluminium cobaltosic oxide, it is characterised in that：In step a,
The cobalt salt is the mixture of one or more of cobaltous sulfate, cobalt nitrate, cobalt chloride, and aluminium salt ethanol solution is tri-chlorination
The ethanol solution of aluminium or aluminum nitrate.
3. a kind of body according to claim 1 mutually mixes the preparation method of aluminium cobaltosic oxide, it is characterised in that：The synthesis
In reaction process, control pH value in reaction is 8.0 ~ 9.0, and reaction temperature is 70-80 DEG C, and solution A flow velocity is 300L/h, B solution stream
Speed is adjusted according to pH value in reaction, and C solution flow velocity is 30 ~ 60L/h, and E solution flow rates are 30L/h, reaction time 15-20h.
4. mutually mixing the preparation method of aluminium cobaltosic oxide according to a kind of body of claim 1-3 any one of them, it is characterised in that：
In the synthetic reaction process, the liquid feeding mode of E solution is E solution charging lines to be divided into 6-9 tiny pipelines, each
Thin charging line liquid outlet is fixed to middle part or the tail portion dispersion liquid feeding of reaction kettle stirrer paddle.
5. mutually mixing the preparation method of aluminium cobaltosic oxide according to a kind of body of claim 1-3 any one of them, it is characterised in that：
The calcination process is, under the conditions of opening, 4-8h is calcined with 700-800 DEG C of calcination temperature.
6. a kind of body according to claim 4 mutually mixes the preparation method of aluminium cobaltosic oxide, it is characterised in that：The calcining
Process is, under the conditions of opening, 4-8h is calcined with 700-800 DEG C of calcination temperature.
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Cited By (6)
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| CN109896552A (en) * | 2019-02-19 | 2019-06-18 | 湖南中伟新能源科技有限公司 | A kind of preparation method for mixing aluminium lithium ion anode material presoma |
| CN109950482A (en) * | 2019-02-22 | 2019-06-28 | 南通金通储能动力新材料有限公司 | A kind of preparation method of aluminium doping lithium cobaltate cathode material |
| CN110002514A (en) * | 2019-04-23 | 2019-07-12 | 金川集团股份有限公司 | A kind of preparation method of rare earth doped element cobaltosic oxide |
| CN110002512A (en) * | 2019-04-23 | 2019-07-12 | 金川集团股份有限公司 | A kind of preparation method for mixing magnesium cobaltosic oxide |
| CN110078133A (en) * | 2019-04-29 | 2019-08-02 | 湖南雅城新材料有限公司 | Spherical cobaltosic oxide of a kind of aluminium doping and the preparation method and application thereof |
| CN114204008A (en) * | 2021-11-23 | 2022-03-18 | 格林美（江苏）钴业股份有限公司 | Preparation method of high-voltage lithium cobalt oxide positive electrode material |
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| CN109950482A (en) * | 2019-02-22 | 2019-06-28 | 南通金通储能动力新材料有限公司 | A kind of preparation method of aluminium doping lithium cobaltate cathode material |
| CN109950482B (en) * | 2019-02-22 | 2022-06-07 | 南通金通储能动力新材料有限公司 | Preparation method of aluminum-doped lithium cobaltate cathode material |
| CN110002514A (en) * | 2019-04-23 | 2019-07-12 | 金川集团股份有限公司 | A kind of preparation method of rare earth doped element cobaltosic oxide |
| CN110002512A (en) * | 2019-04-23 | 2019-07-12 | 金川集团股份有限公司 | A kind of preparation method for mixing magnesium cobaltosic oxide |
| CN110002514B (en) * | 2019-04-23 | 2021-06-29 | 金川集团股份有限公司 | Preparation method of rare earth element-doped cobaltosic oxide |
| CN110078133A (en) * | 2019-04-29 | 2019-08-02 | 湖南雅城新材料有限公司 | Spherical cobaltosic oxide of a kind of aluminium doping and the preparation method and application thereof |
| CN110078133B (en) * | 2019-04-29 | 2021-10-12 | 湖南雅城新材料有限公司 | Aluminum-doped spheroidal cobaltosic oxide and preparation method and application thereof |
| CN114204008A (en) * | 2021-11-23 | 2022-03-18 | 格林美（江苏）钴业股份有限公司 | Preparation method of high-voltage lithium cobalt oxide positive electrode material |
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