CN109244407A - A kind of method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia, aluminium oxide - Google Patents
A kind of method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia, aluminium oxide Download PDFInfo
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- CN109244407A CN109244407A CN201811079859.0A CN201811079859A CN109244407A CN 109244407 A CN109244407 A CN 109244407A CN 201811079859 A CN201811079859 A CN 201811079859A CN 109244407 A CN109244407 A CN 109244407A
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- 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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Abstract
The present invention relates to cell positive material technical fields, the method that cladding nickel-cobalt lithium manganate cathode material is blended in especially a kind of magnesia, aluminium oxide, by magnesia and aluminium oxide are carried out processing nickel-cobalt lithium manganate material using magnesium ion solution and aluminium ion solution blending mode, make it possible to be formed the nickel-cobalt lithium manganate material that magnesia and aluminium oxide coat jointly, the circulating ratio stability for improving nickel-cobalt lithium manganate material, improves the performance of nickel-cobalt lithium manganate cathode material.
Description
Technical field
The present invention relates to cell positive material technical field, cladding nickel cobalt manganese is blended in especially a kind of magnesia, aluminium oxide
The method of sour lithium anode material.
Background technique
Lithium-ion-power cell is generally acknowledged most potential on-vehicle battery both at home and abroad at present, mainly by positive electrode,
The composition such as negative electrode material, diaphragm, electrolyte.Wherein, positive electrode is the important component of lithium ion battery, and determines lithium
The key factor of ion battery performance；Therefore, from the aspect of resource, environmental protection and security performance, lithium ion battery is found
Ideal electrode active material is still the technical problem solved required for those skilled in the art.
Currently, anode material for lithium-ion batteries is mainly by cobalt acid lithium, LiMn2O4, nickle cobalt lithium manganate, LiFePO 4 etc..It is modern
Nian Lai, cobalt nickel lithium manganate ternary material are increasingly subject to attract attention, by the material property, as volume and capacity ratio, weight ratio capacity,
The data test of circulation, safety etc., generally shows nickel-cobalt lithium manganate material as emerging anode material of lithium battery
Some excellent properties, as voltage platform is high, reversible specific capacity is big, stable structure, have a safety feature the advantages that.Although.Nickel cobalt
LiMn2O4 ternary material is quickly grown, but in its practical application, there is also some defects, such as: for the first time coulombic efficiency it is low, times
Rate performance and poor circulation, ingredient and pattern are difficult to control, tap density is low etc..Currently, people mainly pass through reduction sun
Ion mixing improves its coulombic efficiency for the first time, improves its high rate performance by increasing electronic conductivity and plum conductivity,
Increase its tap density by the small particle of preparation morphological rules, specific surface area.Such as Patent No. 201510848444.5
Document disclose using magnesia coat nickel-cobalt lithium manganate cathode material, by directly with nanometer spherical nickel cobalt manganese hydroxide
Presoma is raw material, so that reducing cationic mixing；For another example the document of Patent No. 201510844880.5 discloses use
Alumina-coated nickel-cobalt lithium manganate cathode material, and passing through directly is original with nanometer spherical nickel cobalt manganese hydroxide precursor
Material, so that reducing cationic mixing.Although in the prior art, solving cationic mixing phenomenon, so that positive electrode
Performance is improved, and is that skilled person is continuous for constantly improve for anode material for lithium ion battery performance still
The problem studied and overcome, and the performance for coating the positive electrode of acquisition in the prior art is still undesirable, and by practical
Operation and Experimental Comparison, during short-term cycle charge-discharge, specific capacity is comparatively stable, but with cycle-index
Be continuously increased, it will the reduction for gradually increasing specific capacity causes actual life of positive electrode of preparation to be affected,
Performance is still poor.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of magnesia, aluminium oxide is blended
The method for coating nickel-cobalt lithium manganate cathode material.
It is achieved particular by following technical scheme:
The method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia, aluminium oxide, comprising the following steps:
(1) in water by lithium sulfate, nanometer spherical nickel cobalt manganese hydroxide precursor and polyethylene glycol, using ultrasonic wave added,
Magnetic agitation decentralized processing 2-4h heats evaporating water, crushes, forms uniform intermediate mixture；
(2) intermediate mixture is used into 300-400 DEG C of sintering processes 3-5h, and during the sintering process, is constantly filled with oxygen；Again
It closes oxygen to be filled with, adjustment temperature is 500-600 DEG C of heat treatment 1-2h, obtains nickle cobalt lithium manganate initial material；
(3) nickle cobalt lithium manganate initial material is placed in magnesium ion solution, after impregnating 1-2h, ammonia spirit is added, stirs evenly, mistake
Filter, being placed in temperature is sintering processes 3-5h at 700-800 DEG C, and during the sintering process, is constantly filled with oxygen；
(4) magnesium ion, aluminium ion mixed solution are prepared；The nickel-cobalt lithium manganate material that step (3) sintering is completed is added to mixing
It is uniform using magnetic stirrer in solution, ammonia spirit is added while stirring, clean, filtering, drying to get.
It is preferred that the mixed solution be the magnesium ion solution that magnesium ion molar concentration is 0.07-0.1mol/L and aluminium from
Sub- molar concentration is the aluminium ion solution of 0.1-0.16mol/L, is mixed according to volume ratio for 1:1.
It is preferred that the magnesium ion solution is magnesium chloride solution.
It is preferred that the aluminium ion solution is aluminum nitrate solution.
It is preferred that the lithium sulfate and nanometer spherical nickel cobalt manganese hydroxide precursor molar ratio are 1:0.53-0.56；It is poly-
Ethylene glycol accounts for the 20-30% of total mixture quality.
It is preferred that the mass percent of the ammonia spirit is 10-20%.
Compared with prior art, the technical effect of the invention is embodied in:
By magnesia and aluminium oxide are carried out processing nickle cobalt lithium manganate using magnesium ion solution and aluminium ion solution blending mode
Material makes it possible to be formed the nickel-cobalt lithium manganate material that magnesia and aluminium oxide coat jointly, improves nickel-cobalt lithium manganate material
Circulating ratio stability, improve the performance of nickel-cobalt lithium manganate cathode material.
Especially the material compositions such as lithium sulfate is combined to carry out decentralized processing in water and then be evaporated, crushed, so that
Stock dispersion is uniform, not only facilitates the perfect of material structure, and can aid in improvement material electrochemical cycle performance；Knot
The selection to nickel cobalt manganese hydroxide precursor is closed, so that directly using nanometer spherical material as raw material, so that dispersion is mixed in water
During conjunction, facilitates product component and be uniformly mixed, the mixing of cation is reduced, so that the performance of product is more stable.
Magnesia, aluminium oxide are especially subjected to mixing cladding processing so that the granularity produced is moderate, especially its
Tap density is significantly improved, so that having preferably processing performance in lithium ion battery production process；Coat material
The cost of material is low, covered effect is excellent.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed
Range is not only limited to made description.
Embodiment 1
The method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia, aluminium oxide, comprising the following steps:
(1) in water by lithium sulfate, nanometer spherical nickel cobalt manganese hydroxide precursor and polyethylene glycol, using ultrasonic wave added,
Magnetic agitation decentralized processing 2h heats evaporating water, crushes, forms uniform intermediate mixture；
(2) intermediate mixture is used into 300 DEG C of sintering processes 3h, and during the sintering process, is constantly filled with oxygen；Turn off oxygen
Gas is filled with, and adjustment temperature is 500 DEG C of heat treatment 1h, obtains nickle cobalt lithium manganate initial material；
(3) nickle cobalt lithium manganate initial material is placed in magnesium ion solution, after impregnating 1h, ammonia spirit is added, stirs evenly, filters,
Being placed in temperature is sintering processes 3h at 700 DEG C, and during the sintering process, is constantly filled with oxygen；
(4) magnesium ion, aluminium ion mixed solution are prepared；The nickel-cobalt lithium manganate material that step (3) sintering is completed is added to mixing
It is uniform using magnetic stirrer in solution, ammonia spirit is added while stirring, clean, filtering, drying to get.
The mixed solution is the magnesium ion solution and aluminium ion molar concentration that magnesium ion molar concentration is 0.07mol/L
For the aluminium ion solution of 0.1mol/L, mixed according to volume ratio for 1:1.The magnesium ion solution is magnesium chloride solution.
The aluminium ion solution is aluminum nitrate solution.
The lithium sulfate and nanometer spherical nickel cobalt manganese hydroxide precursor molar ratio is 1:0.53；Polyethylene glycol accounts for always
The 20% of mixture quality.
The mass percent of the ammonia spirit is 10%.
Embodiment 2
The method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia, aluminium oxide, comprising the following steps:
(1) in water by lithium sulfate, nanometer spherical nickel cobalt manganese hydroxide precursor and polyethylene glycol, using ultrasonic wave added,
Magnetic agitation decentralized processing 4h heats evaporating water, crushes, forms uniform intermediate mixture；
(2) intermediate mixture is used into 400 DEG C of sintering processes 5h, and during the sintering process, is constantly filled with oxygen；Turn off oxygen
Gas is filled with, and adjustment temperature is 600 DEG C of heat treatment 2h, obtains nickle cobalt lithium manganate initial material；
(3) nickle cobalt lithium manganate initial material is placed in magnesium ion solution, after impregnating 2h, ammonia spirit is added, stirs evenly, filters,
Being placed in temperature is sintering processes 5h at 800 DEG C, and during the sintering process, is constantly filled with oxygen；
(4) magnesium ion, aluminium ion mixed solution are prepared；The nickel-cobalt lithium manganate material that step (3) sintering is completed is added to mixing
It is uniform using magnetic stirrer in solution, ammonia spirit is added while stirring, clean, filtering, drying to get.
The mixed solution is the magnesium ion solution and aluminium ion molar concentration that magnesium ion molar concentration is 0.1mol/L
For the aluminium ion solution of 0.16mol/L, mixed according to volume ratio for 1:1.The magnesium ion solution is magnesium chloride solution.
The aluminium ion solution is aluminum nitrate solution.
The lithium sulfate and nanometer spherical nickel cobalt manganese hydroxide precursor molar ratio is 1:0.56；Polyethylene glycol accounts for always
The 30% of mixture quality.
The mass percent of the ammonia spirit is 20%.
Embodiment 3
The method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia, aluminium oxide, comprising the following steps:
(1) in water by lithium sulfate, nanometer spherical nickel cobalt manganese hydroxide precursor and polyethylene glycol, using ultrasonic wave added,
Magnetic agitation decentralized processing 3h heats evaporating water, crushes, forms uniform intermediate mixture；
(2) intermediate mixture is used into 350 DEG C of sintering processes 4h, and during the sintering process, is constantly filled with oxygen；Turn off oxygen
Gas is filled with, and adjustment temperature is 550 DEG C of heat treatment 1.5h, obtains nickle cobalt lithium manganate initial material；
(3) nickle cobalt lithium manganate initial material is placed in magnesium ion solution, after impregnating 1.5h, ammonia spirit is added, stirs evenly, mistake
Filter, being placed in temperature is sintering processes 4h at 750 DEG C, and during the sintering process, is constantly filled with oxygen；
(4) magnesium ion, aluminium ion mixed solution are prepared；The nickel-cobalt lithium manganate material that step (3) sintering is completed is added to mixing
It is uniform using magnetic stirrer in solution, ammonia spirit is added while stirring, clean, filtering, drying to get.
The mixed solution is the magnesium ion solution and aluminium ion molar concentration that magnesium ion molar concentration is 0.08mol/L
For the aluminium ion solution of 0.13mol/L, mixed according to volume ratio for 1:1.The magnesium ion solution is magnesium chloride solution.
The aluminium ion solution is aluminum nitrate solution.
The lithium sulfate and nanometer spherical nickel cobalt manganese hydroxide precursor molar ratio is 1:0.55；Polyethylene glycol accounts for always
The 25% of mixture quality.
The mass percent of the ammonia spirit is 15%.
Embodiment 4
The method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia, aluminium oxide, comprising the following steps:
(1) in water by lithium sulfate, nanometer spherical nickel cobalt manganese hydroxide precursor and polyethylene glycol, using ultrasonic wave added,
Magnetic agitation decentralized processing 3h heats evaporating water, crushes, forms uniform intermediate mixture；
(2) intermediate mixture is used into 400 DEG C of sintering processes 3h, and during the sintering process, is constantly filled with oxygen；Turn off oxygen
Gas is filled with, and adjustment temperature is 600 DEG C of heat treatment 1.5h, obtains nickle cobalt lithium manganate initial material；
(3) nickle cobalt lithium manganate initial material is placed in magnesium ion solution, after impregnating 1h, ammonia spirit is added, stirs evenly, filters,
Being placed in temperature is sintering processes 3h at 700 DEG C, and during the sintering process, is constantly filled with oxygen；
(4) magnesium ion, aluminium ion mixed solution are prepared；The nickel-cobalt lithium manganate material that step (3) sintering is completed is added to mixing
It is uniform using magnetic stirrer in solution, ammonia spirit is added while stirring, clean, filtering, drying to get.
The mixed solution is the magnesium ion solution and aluminium ion molar concentration that magnesium ion molar concentration is 0.1mol/L
For the aluminium ion solution of 0.1mol/L, mixed according to volume ratio for 1:1.The magnesium ion solution is magnesium chloride solution.
The aluminium ion solution is aluminum nitrate solution.
The lithium sulfate and nanometer spherical nickel cobalt manganese hydroxide precursor molar ratio is 1:0.54；Polyethylene glycol accounts for always
The 23% of mixture quality.
The mass percent of the ammonia spirit is 17%.
Embodiment 5
The method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia, aluminium oxide, comprising the following steps:
(1) in water by lithium sulfate, nanometer spherical nickel cobalt manganese hydroxide precursor and polyethylene glycol, using ultrasonic wave added,
Magnetic agitation decentralized processing 4h heats evaporating water, crushes, forms uniform intermediate mixture；
(2) intermediate mixture is used into 300 DEG C of sintering processes 4h, and during the sintering process, is constantly filled with oxygen；Turn off oxygen
Gas is filled with, and adjustment temperature is 500 DEG C of heat treatment 2h, obtains nickle cobalt lithium manganate initial material；
(3) nickle cobalt lithium manganate initial material is placed in magnesium ion solution, after impregnating 2h, ammonia spirit is added, stirs evenly, filters,
Being placed in temperature is sintering processes 3h at 700 DEG C, and during the sintering process, is constantly filled with oxygen；
(4) magnesium ion, aluminium ion mixed solution are prepared；The nickel-cobalt lithium manganate material that step (3) sintering is completed is added to mixing
It is uniform using magnetic stirrer in solution, ammonia spirit is added while stirring, clean, filtering, drying to get.
The mixed solution is the magnesium ion solution and aluminium ion molar concentration that magnesium ion molar concentration is 0.07mol/L
For the aluminium ion solution of 0.16mol/L, mixed according to volume ratio for 1:1.The magnesium ion solution is magnesium chloride solution.
The aluminium ion solution is aluminum nitrate solution.
The lithium sulfate and nanometer spherical nickel cobalt manganese hydroxide precursor molar ratio is 1:0.55；Polyethylene glycol accounts for always
The 27% of mixture quality.
The mass percent of the ammonia spirit is 18%.
The positive electrode prepared using embodiment 1-5, is prepared into electrode by the following method:
Using -2 pyrrolidones of organic solvent 1- methyl as solvent, by the electrode material prepared, conductive agent (acetylene black) and bonding
Agent Kynoar is mixed evenly according to mass ratio for 8:1:1, is evenly coated in the aluminum foil current collector that diameter is 14mm,
It in drying box, is dried at 75 DEG C, then uniformly using tablet press machine compacting, electrode to be measured is made.
And battery assembly is carried out to prepared electrode slice using coin shape simulated battery, wherein being lithium metal to electrode
Piece, diaphragm are Celgard2325 composite membrane, and electrolyte is the isometric than ethylene carbonate, dimethyl carbonate of 0.5mol/L
Solution, battery assembly are completed in the glove box full of argon gas.
To the battery being completed, constant current charge-discharge test is done in 2.5-4.3V voltage range, under 2C multiplying power,
As a result as shown in table 1 below:
| First discharge specific capacity (mAh/g) | 50 specific discharge capacities (mAh/g) | 200 specific discharge capacities (mAh/g) | 500 specific discharge capacities (mAh/g) | |
| Embodiment 1 | 186.7 | 184.1 | 178.9 | 158.9 |
| Embodiment 2 | 185.9 | 183.9 | 179.3 | 159.7 |
| Embodiment 3 | 186.2 | 186.8 | 178.8 | 159.2 |
| Embodiment 4 | 186.5 | 186.4 | 178.6 | 159.6 |
| Embodiment 5 | 185.8 | 183.7 | 179.1 | 157.8 |
By the data of table 1 show it can be seen from the invention coat jointly using magnesia and aluminium oxide handle nickel cobalt
Manganate cathode material for lithium improves the property of positive electrode so that the charge-discharge performance of nickel-cobalt lithium manganate cathode material is stablized
Energy index, raw material are easy to get, simple process and low cost.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia, aluminium oxide, which is characterized in that including following step
It is rapid:
(1) in water by lithium sulfate, nanometer spherical nickel cobalt manganese hydroxide precursor and polyethylene glycol, using ultrasonic wave added,
Magnetic agitation decentralized processing 2-4h heats evaporating water, crushes, forms uniform intermediate mixture；
(2) intermediate mixture is used into 300-400 DEG C of sintering processes 3-5h, and during the sintering process, is constantly filled with oxygen；Again
It closes oxygen to be filled with, adjustment temperature is 500-600 DEG C of heat treatment 1-2h, obtains nickle cobalt lithium manganate initial material；
(3) nickle cobalt lithium manganate initial material is placed in magnesium ion solution, after impregnating 1-2h, ammonia spirit is added, stirs evenly, mistake
Filter, being placed in temperature is sintering processes 3-5h at 700-800 DEG C, and during the sintering process, is constantly filled with oxygen；
(4) magnesium ion, aluminium ion mixed solution are prepared；The nickel-cobalt lithium manganate material that step (3) sintering is completed is added to mixing
It is uniform using magnetic stirrer in solution, ammonia spirit is added while stirring, clean, filtering, drying to get.
2. the method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia as described in claim 1, aluminium oxide, feature exist
In the mixed solution is the magnesium ion solution and aluminium ion molar concentration that magnesium ion molar concentration is 0.07-0.1mol/L
For the aluminium ion solution of 0.1-0.16mol/L, mixed according to volume ratio for 1:1.
3. the method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia as claimed in claim 1 or 2, aluminium oxide, special
Sign is that the magnesium ion solution is magnesium chloride solution.
4. the method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia as claimed in claim 2, aluminium oxide, feature exist
In the aluminium ion solution is aluminum nitrate solution.
5. the method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia as described in claim 1, aluminium oxide, feature exist
In the lithium sulfate and nanometer spherical nickel cobalt manganese hydroxide precursor molar ratio are 1:0.53-0.56；Polyethylene glycol accounts for always
The 20-30% of mixture quality.
6. the method that cladding nickel-cobalt lithium manganate cathode material is blended in magnesia as described in claim 1, aluminium oxide, feature exist
In the mass percent of the ammonia spirit is 10-20%.
7. cladding nickle cobalt lithium manganate anode is blended in the magnesia of as the method according to claim 1 to 6 preparation, aluminium oxide
Material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111354936A (en) * | 2020-04-10 | 2020-06-30 | 湖北亿纬动力有限公司 | Core-shell structure cathode material and preparation method and application thereof |
| CN113793935A (en) * | 2021-08-03 | 2021-12-14 | 广东邦普循环科技有限公司 | Preparation method and application of high-performance nickel 55 type modified nickel cobalt lithium manganate material |
| CN114142010A (en) * | 2021-11-26 | 2022-03-04 | 天津巴莫科技有限责任公司 | Magnesium oxide and cerium fluoride composite coated lithium ion battery positive electrode material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105355911A (en) * | 2015-11-28 | 2016-02-24 | 中信大锰矿业有限责任公司大新锰矿分公司 | Preparation method of aluminum oxide coated lithium nickel manganese cobalt cathode material |
| CN106602021A (en) * | 2016-12-22 | 2017-04-26 | 金瑞新材料科技股份有限公司 | Coated positive electrode material of lithium-ion battery and preparation method of positive electrode material |
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2018
- 2018-09-17 CN CN201811079859.0A patent/CN109244407A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105355911A (en) * | 2015-11-28 | 2016-02-24 | 中信大锰矿业有限责任公司大新锰矿分公司 | Preparation method of aluminum oxide coated lithium nickel manganese cobalt cathode material |
| CN106602021A (en) * | 2016-12-22 | 2017-04-26 | 金瑞新材料科技股份有限公司 | Coated positive electrode material of lithium-ion battery and preparation method of positive electrode material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111354936A (en) * | 2020-04-10 | 2020-06-30 | 湖北亿纬动力有限公司 | Core-shell structure cathode material and preparation method and application thereof |
| CN113793935A (en) * | 2021-08-03 | 2021-12-14 | 广东邦普循环科技有限公司 | Preparation method and application of high-performance nickel 55 type modified nickel cobalt lithium manganate material |
| CN113793935B (en) * | 2021-08-03 | 2023-04-11 | 广东邦普循环科技有限公司 | Preparation method and application of high-performance nickel 55 type modified nickel cobalt lithium manganate material |
| CN114142010A (en) * | 2021-11-26 | 2022-03-04 | 天津巴莫科技有限责任公司 | Magnesium oxide and cerium fluoride composite coated lithium ion battery positive electrode material and preparation method thereof |
| CN114142010B (en) * | 2021-11-26 | 2024-05-14 | 天津巴莫科技有限责任公司 | Magnesium oxide and cerium fluoride composite coated lithium ion battery positive electrode material and preparation method thereof |
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