CN108832104A - A kind of preparation method of aluminum fluoride cladding nickel cobalt aluminic acid lithium material - Google Patents
A kind of preparation method of aluminum fluoride cladding nickel cobalt aluminic acid lithium material Download PDFInfo
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- CN108832104A CN108832104A CN201810635944.4A CN201810635944A CN108832104A CN 108832104 A CN108832104 A CN 108832104A CN 201810635944 A CN201810635944 A CN 201810635944A CN 108832104 A CN108832104 A CN 108832104A
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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
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- 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
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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
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- 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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Abstract
The invention discloses a kind of preparation methods of aluminum fluoride cladding nickel cobalt aluminic acid lithium material, are related to battery technology field.Including step：(1) aluminum salt solution is configured；(2) nickel cobalt lithium aluminate solution is configured；(3) fluoride aqueous solution is prepared；(4) secondary species is prepared；(5) end-products are prepared.The present invention is by coating ternary electrode material nickel cobalt lithium aluminate, effectively avoid when charging to high voltage, serious side reaction occurs for ternary material surface and electrolyte, to inhibit structure of the ternary material in charge and discharge process to destroy, electrochemical stability is improved, cycle life is extended；Preparation process of the present invention is simple simultaneously, and preparation process time-consuming is short, and preparation environmental requirement is low, and cost is more cheap.
Description
Technical field
The invention belongs to battery technology fields, more particularly to a kind of preparation of aluminum fluoride cladding nickel cobalt aluminic acid lithium material
Method.
Background technique
Current commercial lithium battery material mainly has cobalt acid lithium, LiMn2O4, LiFePO4, ternary material etc..Wherein ternary
Material specific capacity with higher is high with energy density and power density, operating voltage and stability is good, to become business
The active material of research.However, with electrolyte serious side reaction can occur for ternary material, simultaneously when charging to high voltage
Along with the release of big calorimetric and oxygen, reduced so as to cause poor circulation and thermal stability；Therefore need to ternary material into
Row is modified.
Cladding is that current researcher uses a kind of more surface modifying method, after material is coated, shape
At protective layer the active material in material can be kept apart with electrolyte, so as to substantially reduce electrode and electrolyte
The side reaction of interface；Existing method for coating is not readily available uniform clad and controllable nanoscale cladding substance, packet
Substance after covering and material of main part compatibility are not good enough or are not sufficiently stable, and are easy to fall off so as to cause clad, covered effect is big
It gives a discount.
Summary of the invention
In order to solve the above technical problems, the present invention is achieved by the following technical solutions：
The present invention is the preparation method that a kind of aluminum fluoride coats nickel cobalt aluminic acid lithium material, is included the following steps：
(1) aluminum salt solution is configured；Aluminium salt is added in deionized water and obtains aluminum salt solution after completely dissolution；
(2) nickel cobalt lithium aluminate solution is configured；Nickel cobalt lithium aluminate is added in the aluminum salt solution of step (1) preparation, is persistently stirred
Mixing obtains nickel cobalt lithium aluminate solution for standby；
(3) fluoride aqueous solution is prepared；By in Fluorine source compound solution water, the fluoride aqueous solution of every liter of 1mol is prepared；
(4) secondary species is prepared；Controlling reaction temperature is 50 degrees Celsius；The fluoride aqueous solution of step (3) preparation is added dropwise
Enter in the nickel cobalt lithium aluminate solution prepared in step (2), persistently stir 3-4 hours, secondary species is obtained after suction filtration；
(5) end-products are prepared；Secondary species prepared by step (4) is washed, at 100-120 degrees Celsius after washing
Environment in dry 1-2 hour, calcined in a nitrogen atmosphere 2-5 hour after dry, obtain ultimate production after calcining completion natural cooling
Object is aluminum fluoride cladding nickel cobalt aluminic acid lithium material.
Further, aluminium salt is Al (NO3) in the step (1)3·9H2O；The aluminium salt quality and deionized water volume
Than for 1g：372-373ml.
Further, the stirring rate in the step (2) is 500 turns per minute.
Further, calcining need to carry out in 400-600 degrees Celsius of tube furnace in the step (5).
Further, Fluorine source compound is ammonium fluoride or ammonium acid fluoride in the step (3).
The invention has the advantages that：
1, preparation process of the present invention is simple, and preparation process time-consuming is short, and preparation environmental requirement is simple, low in cost.
2, the present invention is effectively avoided by coating to ternary electrode material nickel cobalt lithium aluminate in the supreme electricity that charges
When pressure, serious side reaction occurs for ternary material surface and electrolyte, to inhibit ternary material in charge and discharge process
Structure is destroyed, and is improved electrochemical stability, is extended cycle life.
Certainly, it implements any of the products of the present invention and does not necessarily require achieving all the advantages described above at the same time.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's all other embodiment obtained without creative efforts belongs to the model that the present invention protects
It encloses.
The present invention is the preparation method that a kind of aluminum fluoride coats nickel cobalt aluminic acid lithium material, is included the following steps：
(1) aluminum salt solution is configured；By aluminium salt Al (NO3)3·9H2O and deionized water press 1g：372-373ml proportion, sufficiently
Aluminum salt solution is obtained after dissolution；
(2) nickel cobalt lithium aluminate solution is configured；Nickel cobalt lithium aluminate is added in the aluminum salt solution of step (1) preparation, with every point
500 turns of clock continue to stir obtained nickel cobalt lithium aluminate solution for standby；
(3) fluoride aqueous solution is prepared；By in ammonium fluoride or ammonium hydrogen fluoride solution water, the fluoride for preparing every liter of 1mol is molten
Liquid；
(4) secondary species is prepared；Controlling reaction temperature is 50 degrees Celsius；The fluoride aqueous solution of step (3) preparation is added dropwise
Enter in the nickel cobalt lithium aluminate solution prepared in step (2), persistently stir 3-4 hours, secondary species is obtained after suction filtration；
(5) end-products are prepared；Secondary species prepared by step (4) is washed, at 100-120 degrees Celsius after washing
Environment in dry 1-2 hour, it is small that 2-5 is persistently calcined in 400-600 degrees Celsius of tube furnace in a nitrogen atmosphere after drying
When, calcining and obtaining end-products after completing natural cooling is aluminum fluoride cladding nickel cobalt aluminic acid lithium material.
Embodiment 1
(1) aluminum salt solution is configured；By the Al (NO3) of aluminium salt 0.1g3·9H2The deionized water of O and 37.2ml is after completely dissolution
Obtain aluminum salt solution；
(2) nickel cobalt lithium aluminate solution is configured；Nickel cobalt lithium aluminate is added in the aluminum salt solution of step (1) preparation, with every point
500 turns of clock continue to stir obtained nickel cobalt lithium aluminate solution for standby；
(3) fluoride aqueous solution is prepared；By in ammonium fluoride solution water, the fluoride aqueous solution of every liter of 1mol is prepared；
(4) secondary species is prepared；Controlling reaction temperature is 50 degrees Celsius, keeps constant temperature；Fluoride prepared by step (3)
Solution is added dropwise in the nickel cobalt lithium aluminate solution prepared in step (2), is persistently stirred 3 hours, and secondary species is obtained after suction filtration；
(5) end-products are prepared；Secondary species prepared by step (4) is washed, in 110 degrees Celsius of ring after washing
It is 1.5 hours dry in border, it is persistently calcined in 400 degrees Celsius of tube furnace 5 hours in a nitrogen atmosphere after dry, calcining is completed
It is aluminum fluoride cladding nickel cobalt aluminic acid lithium material that end-products are obtained after natural cooling.
Embodiment 2
(1) aluminum salt solution is configured；By the Al (NO3) of aluminium salt 0.1g3·9H2The deionized water of O and 37.3ml is after completely dissolution
Obtain aluminum salt solution；
(2) nickel cobalt lithium aluminate solution is configured；Nickel cobalt lithium aluminate is added in the aluminum salt solution of step (1) preparation, with every point
500 turns of clock continue to stir obtained nickel cobalt lithium aluminate solution for standby；
(3) fluoride aqueous solution is prepared；By in ammonium fluoride solution water, the fluoride aqueous solution of every liter of 1mol is prepared；
(4) secondary species is prepared；Controlling reaction temperature is 50 degrees Celsius, keeps constant temperature；Fluoride prepared by step (3)
Solution is added dropwise in the nickel cobalt lithium aluminate solution prepared in step (2), is persistently stirred 4 hours, and secondary species is obtained after suction filtration；
(5) end-products are prepared；Secondary species prepared by step (4) is washed, in 120 degrees Celsius of ring after washing
It is 1 hour dry in border, it is persistently calcined in 500 degrees Celsius of tube furnace 3 hours in a nitrogen atmosphere after dry, calcining is completed certainly
It is aluminum fluoride cladding nickel cobalt aluminic acid lithium material that end-products are so obtained after cooling.
Embodiment 3
(1) aluminum salt solution is configured；By the Al (NO3) of aluminium salt 0.2g3·9H2The deionized water of O and 74.6ml is after completely dissolution
Obtain aluminum salt solution；
(2) nickel cobalt lithium aluminate solution is configured；Nickel cobalt lithium aluminate is added in the aluminum salt solution of step (1) preparation, with every point
500 turns of clock continue to stir obtained nickel cobalt lithium aluminate solution for standby；
(3) fluoride aqueous solution is prepared；By in ammonium fluoride solution water, the fluoride aqueous solution of every liter of 1mol is prepared；
(4) secondary species is prepared；Controlling reaction temperature is 50 degrees Celsius, keeps constant temperature；Fluoride prepared by step (3)
Solution is added dropwise in the nickel cobalt lithium aluminate solution prepared in step (2), is persistently stirred 4 hours, and secondary species is obtained after suction filtration；
(5) end-products are prepared；Secondary species prepared by step (4) is washed, in 100 degrees Celsius of ring after washing
It is 2 hours dry in border, it is persistently calcined in 600 degrees Celsius of tube furnace 2 hours in a nitrogen atmosphere after dry, calcining is completed certainly
It is aluminum fluoride cladding nickel cobalt aluminic acid lithium material that end-products are so obtained after cooling.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (5)
1. a kind of preparation method of aluminum fluoride cladding nickel cobalt aluminic acid lithium material, it is characterised in that：Include the following steps：
(1) aluminum salt solution is configured；Aluminium salt is added in deionized water and obtains aluminum salt solution after completely dissolution；
(2) nickel cobalt lithium aluminate solution is configured；Nickel cobalt lithium aluminate is added in the aluminum salt solution of step (1) preparation, lasting stirring system
Obtain nickel cobalt lithium aluminate solution for standby；
(3) fluoride aqueous solution is prepared；By in Fluorine source compound solution water, the fluoride aqueous solution of every liter of 1mol is prepared；
(4) secondary species is prepared；Controlling reaction temperature is 50 degrees Celsius；Fluoride aqueous solution prepared by step (3) is added dropwise to step
Suddenly it in the nickel cobalt lithium aluminate solution prepared in (2), persistently stirs 3-4 hours, secondary species is obtained after suction filtration；
(5) end-products are prepared；Secondary species prepared by step (4) is washed, in 100-120 degrees Celsius of ring after washing
It is 1-2 hours dry in border, it is calcined in a nitrogen atmosphere 2-5 hours after dry, obtaining end-products after calcining completion natural cooling is
Nickel cobalt aluminic acid lithium material is coated for aluminum fluoride.
2. the preparation method of aluminum fluoride cladding nickel cobalt aluminic acid lithium material according to claim 1, which is characterized in that the step
Suddenly aluminium salt is Al (NO3) in (1)3·9H2O；The aluminium salt quality and deionized water volume ratio are 1g：372-373ml.
3. the preparation method of aluminum fluoride cladding nickel cobalt aluminic acid lithium material according to claim 1, which is characterized in that the step
Suddenly the stirring rate in (2) is 500 turns per minute.
4. the preparation method of aluminum fluoride cladding nickel cobalt aluminic acid lithium material according to claim 1, which is characterized in that the step
Suddenly calcining need to carry out in 400-600 degrees Celsius of tube furnace in (5).
5. the preparation method of aluminum fluoride cladding nickel cobalt aluminic acid lithium material according to claim 1, which is characterized in that the step
Suddenly Fluorine source compound is ammonium fluoride or ammonium acid fluoride in (3).
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| CN201810635944.4A CN108832104A (en) | 2018-06-20 | 2018-06-20 | A kind of preparation method of aluminum fluoride cladding nickel cobalt aluminic acid lithium material |
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| CN201810635944.4A CN108832104A (en) | 2018-06-20 | 2018-06-20 | A kind of preparation method of aluminum fluoride cladding nickel cobalt aluminic acid lithium material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109935809A (en) * | 2019-02-28 | 2019-06-25 | 湖北锂诺新能源科技有限公司 | A kind of preparation method of aluminum fluoride cladding vanadium phosphate cathode material |
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| US20160049655A1 (en) * | 2014-08-15 | 2016-02-18 | Quantumscape Corporation | Doped conversion materials for secondary battery cathodes |
| CN105958017A (en) * | 2016-05-10 | 2016-09-21 | 山东玉皇新能源科技有限公司 | Preparation method for aluminum-fluoride-coated lithium nickel cobalt manganate positive electrode material |
| CN106299353A (en) * | 2015-06-01 | 2017-01-04 | 龙能科技（苏州）有限公司 | Nickel cobalt lithium aluminate composite and its preparation method and application |
| CN106602016A (en) * | 2016-12-21 | 2017-04-26 | 山东玉皇新能源科技有限公司 | Preparation method for ammonium fluoride modified nickel-cobalt-aluminum ternary positive electrode material |
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2018
- 2018-06-20 CN CN201810635944.4A patent/CN108832104A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160049655A1 (en) * | 2014-08-15 | 2016-02-18 | Quantumscape Corporation | Doped conversion materials for secondary battery cathodes |
| CN106299353A (en) * | 2015-06-01 | 2017-01-04 | 龙能科技（苏州）有限公司 | Nickel cobalt lithium aluminate composite and its preparation method and application |
| CN105958017A (en) * | 2016-05-10 | 2016-09-21 | 山东玉皇新能源科技有限公司 | Preparation method for aluminum-fluoride-coated lithium nickel cobalt manganate positive electrode material |
| CN106602016A (en) * | 2016-12-21 | 2017-04-26 | 山东玉皇新能源科技有限公司 | Preparation method for ammonium fluoride modified nickel-cobalt-aluminum ternary positive electrode material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109935809A (en) * | 2019-02-28 | 2019-06-25 | 湖北锂诺新能源科技有限公司 | A kind of preparation method of aluminum fluoride cladding vanadium phosphate cathode material |
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