CN110265657A - One type monocrystalline lithium nickel cobalt manganese oxide material and preparation method thereof - Google Patents
One type monocrystalline lithium nickel cobalt manganese oxide material and preparation method thereof Download PDFInfo
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- CN110265657A CN110265657A CN201910334253.5A CN201910334253A CN110265657A CN 110265657 A CN110265657 A CN 110265657A CN 201910334253 A CN201910334253 A CN 201910334253A CN 110265657 A CN110265657 A CN 110265657A
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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
- H01M4/485—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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
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Abstract
The present invention relates to type monocrystalline lithium nickel cobalt manganese oxide material and preparation method thereof, the material general formula is LiaNixCoyMn1‑x‑yMbNcO2·ZdO2, in formula, 1.0≤a≤1.1,0.5≤x≤0.9,0.1≤y≤0.2,0.001≤c≤0.03, Z and LiaNixCoyMn1‑x‑yMbNcO2·ZdO2Mass ratio 0.05%≤d≤0.35%, M and LiaNixCoyMn1‑x‑ yMbNcO2·ZdO2Mass ratio 0.007%≤b≤0.35%.The present invention does not use physical grinding mode, and fluxing agent when a kind of additive is added in mixed once as sintering reduces sintering temperature, simplifies production procedure, make presoma that can be burnt into class monocrystalline pattern；Fluxing agent is added, and makes the reduction of crystal internal stress, more conducively lithium ion insertion and abjection, promotes material capacity.
Description
Technical field
The present invention relates to anode material for lithium ion battery field more particularly to a type monocrystalline lithium nickel cobalt manganese combined oxidations
The preparation method of object material and the material.
Background technique
Tertiary cathode material is due to having many advantages, such as that energy density is high, recycle, and conducive in electric car lightweight,
The mainstream selection of electric car is had become at present.
The secondary spherical particles that most of ternary material currently on the market is 7 μm or more.When being coated with roll-in, sphere holds
It is easily broken, cause uncoated internal particle to be exposed, and then influence the cycle performance of battery, high-temperature storage performance.Secondly
The prolonged convergent-divergent of primary particle causes ball to split to secondary ball particle in the circulating cycle, also influences the cycle performance of battery.Therefore,
Need to develop other lithium nickel cobalt manganese oxide materials.
Application No. is CN200910019746.6 to disclose the preparation method of a type monocrystalline tertiary cathode material, adopt
Presoma class single crystal grain is ground to the method for grinding to be sintered again.Application No. is public in CN201410327608.5
The preparation method for having opened a type monocrystal material, uses and grinds the presoma after oxidation, be sintered after grinding, burns
It is pulverized and sieved to obtain class monocrystal material after knot.It is that class monocrystalline pattern is reached by physical grinding or crushing, does not add
The explanation of fluxing agent.
The method of physical grinding material can generate≤3 μm of material in grinding and increase, and≤3 μm of material is in battery
Meeting super-charge super-discharge deteriorates circulation in cyclic process.And complex process, the high requirements on the equipment when production.
Summary of the invention
The object of the present invention is to provide type monocrystalline lithium nickel cobalt manganese oxide materials and preparation method thereof；Do not make
With the mode of physical grinding, and fluxing agent when a kind of additive is sintering is added in mixed once, reduces sintering temperature,
Simplify production procedure, class monocrystalline pattern can be burnt by making the presoma in certain particle size range.The addition of fluxing agent can make material
The growth temperature of crystal reduces, and makes the reduction of crystal internal stress, keeps crystal form more preferable, more conducively the insertion and abjection of lithium ion, protecting
Capacity is improved while card circulation.And the element of stable crystal form is added in mixing, cladding member is added before double sintering
Usually promote circulation.
In order to achieve the above object, the present invention has following technical scheme:
A type monocrystalline lithium nickel cobalt manganese oxide material of the invention, in which: the material general formula is
LiaNixCoyMn1-x-yMbNcO2·ZdO2, in formula, 1.0≤a≤1.1,0.5≤x≤0.9,0.1≤y≤0.2,0.001≤c≤
0.03, Z and LiaNixCoyMn1-x-yMbNcO2·ZdO2Mass ratio 0.05%≤d≤0.35%, M and LiaNixCoyMn1-x- yMbNcO2·ZdO2Mass ratio 0.007%≤b≤0.35%.
Wherein, the presoma D50 of the material is 1.0~7.0 μm.
Wherein, the material is aspherical primary particle aggregate under electron-microscope scanning.
Wherein, the addition element M of the material is one of B, Mg, Ca, Sr, Ba, and the addition element N of the material is
At least one of Nb, Ta, Zr, Y, Al or a variety of, the addition element Z of the material are at least one of Al, Zr, Ti or more
It plants, wherein the source B H3BO3、B2O3At least one of, the source Mg MgO, Mg (OH)2At least one of, the source Ca CaO, Ca
(OH)2、CaCO3At least one of, the source Sr SrCO3、 Sr(OH)2, at least one of SrO, the source Ba BaCO3、Ba
(OH)2At least one of, the source Nb Nb2O5、NbO2、Nb2O3At least one of, the source Ta Ta2O5、 TaO2、Ta2O3In
At least one, the source Zr ZrO2, the source Y Y2O3、Y(NO3)3、 Y(OH)3At least one of, the source Al Al2O3、Al(OH)3In
One kind, the source Ti TiO2, at least one of isopropyl titanate.
Wherein, the presoma D50 of the material is 1.0-6.0 μm.
Wherein, the presoma is nickel cobalt manganese hydroxide, nickel cobalt manganese oxyhydroxide, nickel cobalt manganese carbonation, nickel cobalt manganese
One of oxide.
Wherein, the lithium source is lithium carbonate, lithium hydroxide, or both mixing.
The preparation method of a type monocrystalline lithium nickel cobalt manganese oxide material of the invention, this method comprise the following steps:
(1) the mixed once process of presoma and lithium salts and addition element M and addition element N,
(2) mixed once sintered process,
(3) sintered broken process,
(4) rear and addition element Z secondary mixed processes are crushed,
(5) mixed double sintering process,
(6) the sieving process after double sintering.
Wherein, the temperature of the once sintered process is 700-970 DEG C, time 5-25h.
Wherein, the double sintering process temperature is 500-700 DEG C, time 3-10h.
Beneficial effect
The present invention improves capacity while guaranteeing circulation compared with prior art.Due to sintering temperature is low,
It can guarantee the cycle characteristics of material.Due to the addition of fluxing agent, makes the reduction of crystal internal stress, keep crystal form more preferable, more conducively lithium
The insertion and abjection of ion promote material capacity.
The production process process of class monocrystalline tertiary cathode material is simplified, reduces temperature sintering, and do not need using machine
Tool external force keeps secondary ball broken, and the primary particle of≤3 μm of reduction improves the yield rate of product, reduces production cost.
The material of the method for the present invention preparation has the advantages that at low cost, capacity is high, circulation is good.
Detailed description of the invention
Fig. 1 is the electron microscope of embodiment 1；
Fig. 2 is the circulation comparison diagram of embodiment 1 and comparative example 2, comparative example 3.
1,1 curve of embodiment；2,2 curve of comparative example；3,3 curve of comparative example.
Specific embodiment
For a further understanding of the present invention, the present invention is made below in conjunction with specification and specific preferred embodiment further
Description, but protection scope not thereby limiting the invention.
Embodiment 1
Select D50 for 3.3 μm of Ni0.6Co0.1Mn0.3(OH)2Presoma and lithium carbonate are pressed 1.06 mole by presoma
Than, and add 0.007% B element, the mixing of 0.015 mole of Zr element.The source B uses H3BO3, the source Zr uses ZrO2.?
It is uniformly mixed in high-speed mixer.Uniformly mixed material is placed in sintering furnace and is warming up to the heating rate of 3 DEG C/min
910 DEG C and keep the temperature 12h.It is cooled to room temperature later with furnace temperature, by being crushed crusher machine.Broken material and 0.15% Al
(source Al is Al2O3) be uniformly mixed, 700 DEG C are warming up to the heating rate of 3 DEG C/min in sintering furnace and keep the temperature 6h.With furnace temperature
It is down to room temperature.Then sieving gets product material.
Above-mentioned finished-product material, acetylene black, KS-6, PVDF are mixed according to the ratio that mass ratio is 9.0 ︰, 0.4 ︰, 0.3 ︰ 0.3
Uniformly, appropriate NMP is added, uniform slurry is made in stirring；Slurry is uniformly applied on aluminium foil, air dry oven baking is put into
After dry, place into 120 DEG C of vacuum oven and be dried in vacuo 12 hours；Going out diameter with sheet-punching machine after natural cooling is 16mm's
Disk is placed on tablet press machine with obtaining positive plate after the pressure compaction of 10MPa by disk.It is anode with homemade positive plate,
Lithium piece is cathode, and Celgard2400 microporous polypropylene membrane is diaphragm, and the LiPF6/EC+DMC (v:v=1:1) of 1mol/L is electrolysis
Liquid is all assembled into CR2016 type button cell in the 0.1ppm glove box below full of argon gas in water content and oxygen content,
Charge-discharge test is carried out in 2.75~4.3V voltage range with the multiplying power of 0.1C, discharge capacity reaches 178.9mAh/ to material for the first time
G, 100 weeks capacity retention ratios of 1C, 2.75-4.3V circulation are 95% to button cell at normal temperature
Electron microscope is shown in that attached drawing 1, capacity see attached list 2, and half-cell circulation is shown in attached drawing 2.
Table 2 is the capacity comparison table of embodiment 1 and comparative example 1
| 0.1CmAh/g | Head effect % | |
| Embodiment 1 | 178.9 | 87.98 |
| Comparative example 1 | 164.9 | 84.04 |
Embodiment 2
Select D50 for 2.0 μm of Ni0.8Co0.1Mn0.1(OH)2Presoma, using lithium hydroxide and 0.15%Sr, (source Sr is
Sr(OH)2), once sintered temperature is 750 DEG C.In addition to the condition, other and embodiment 1 are identical.
Embodiment 3
Select D50 for 6.0 μm of Ni0.5Co0.2Mn0.3(OH)2Presoma, using 0.1%Sr (source Sr is SrO), once
Sintering temperature is 970 DEG C, and in addition to the condition, other and embodiment 1 are identical.
Comparative example 1
In addition to B element is not added, other and embodiment 1 are identical.Its capacity result sees attached list 2.Comparative example 2
In addition to Zr element is not added, other and embodiment 1 are identical.
Comparative example 3
Other are the same as embodiment 1 in addition to the mixing of Al element is not added.
The result shows that the capacity with higher compared with comparative example 1 of embodiment 1, illustrates the addition of synthermal lower fluxing agent
Conducive to the performance of material capacity；Embodiment 1 has similar capacity compared with comparative example 2, but cycle performance is much better than comparative example
2, illustrate that Zr doping has very significant improvement result to cycle performance；Embodiment 1 has similar appearance compared with comparative example 3
Amount, but cycle performance is better than comparative example 3, illustrates to coat the effect that also has greatly improved to cycle performance；Embodiment 1, embodiment
2, the presoma of different-grain diameter, different nickel cobalt manganese ratio is respectively adopted in embodiment 3, illustrates that the method for the present invention is not intended to limit and uses
Presoma.
The Applicant declares that the present invention is explained by the above embodiments, the present invention is made is further described, cannot
Assert that specific implementation of the invention is only limited to these instructions.It should be bright for those skilled in the art
, under the early periods for not departing from present inventive concept, several simple deductions or substitution are made to the present invention, all fall within guarantor of the invention
It protects within range and the open scope.
Claims (10)
1. a type monocrystalline lithium nickel cobalt manganese oxide material, it is characterised in that: the material general formula is LiaNixCoyMn1-x- yMbNcO2·ZdO2, in formula, 1.0≤a≤1.1,0.5≤x≤0.9,0.1≤y≤0.2,0.001≤c≤0.03, Z with
LiaNixCoyMn1-x-yMbNcO2·ZdO2Mass ratio 0.05%≤d≤0.35%, M and LiaNixCoyMn1-x-yMbNcO2·ZdO2Matter
Measure ratio 0.007%≤b≤0.35%.
2. type monocrystalline lithium nickel cobalt manganese oxide material according to claim 1, it is characterised in that: the material
Presoma D50 be 1.0~7.0 μm.
3. type monocrystalline lithium nickel cobalt manganese oxide material according to claim 1, it is characterised in that: the material
It is aspherical primary particle aggregate under electron-microscope scanning.
4. type monocrystalline lithium nickel cobalt manganese oxide material according to claim 1, it is characterised in that: the material
Addition element M be one of B, Mg, Ca, Sr, Ba, the addition element N of the material be in Nb, Ta, Zr, Y, Al at least
One or more, the addition element Z of the material is at least one of Al, Zr, Ti or a variety of, wherein the source B H3BO3、B2O3
At least one of, the source Mg MgO, Mg (OH)2At least one of, the source Ca CaO, Ca (OH)2、CaCO3In at least one
Kind, the source Sr SrCO3、Sr(OH)2, at least one of SrO, the source Ba BaCO3、Ba(OH)2At least one of, the source Nb
Nb2O5、NbO2、Nb2O3At least one of, the source Ta Ta2O5、TaO2、Ta2O3At least one of, the source Zr ZrO2, the source Y
Y2O3、Y(NO3)3、Y(OH)3At least one of, the source Al Al2O3、Al(OH)3One of, the source Ti TiO2, isopropyl titanate
At least one of.
5. type monocrystalline lithium nickel cobalt manganese oxide material according to claim 1, it is characterised in that: the material
Presoma D50 be 1.0-6.0 μm.
6. type monocrystalline lithium nickel cobalt manganese oxide material according to claim 1, it is characterised in that: the forerunner
Body is one of nickel cobalt manganese hydroxide, nickel cobalt manganese oxyhydroxide, nickel cobalt manganese carbonation, nickel, cobalt and manganese oxide.
7. type monocrystalline lithium nickel cobalt manganese oxide material according to claim 1, it is characterised in that: the lithium source
For lithium carbonate, lithium hydroxide, or both mixing.
8. preparation method according to claim 1, it is characterised in that: this method comprises the following steps:
(1) the mixed once process of presoma and lithium salts and addition element M and addition element N,
(2) mixed once sintered process,
(3) sintered broken process,
(4) rear and addition element Z secondary mixed processes are crushed,
(5) mixed double sintering process,
(6) the sieving process after double sintering.
9. preparation method according to claim 8, it is characterised in that: the temperature of the once sintered process is 700-970
DEG C, time 5-25h.
10. preparation method according to claim 8, it is characterised in that: the double sintering process temperature is 500-700
DEG C, time 3-10h.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111710843A (en) * | 2020-06-24 | 2020-09-25 | 河南福森新能源科技有限公司 | Method for manufacturing nickel cobalt lithium manganate serving as high-compaction lithium battery cathode material |
| CN111952581A (en) * | 2020-08-25 | 2020-11-17 | 湖北融通高科先进材料有限公司 | NCM613 single crystal type anode material and preparation method thereof |
| CN112499695A (en) * | 2020-11-26 | 2021-03-16 | 湖南海利锂电科技股份有限公司 | Nickel-cobalt-manganese ternary cathode material and preparation method and application thereof |
| WO2021165282A1 (en) * | 2020-02-17 | 2021-08-26 | Umicore | A method for preparing a positive electrode active material for rechargeable lithium ion batteries |
| CN113422046A (en) * | 2021-06-30 | 2021-09-21 | 湖南杉杉能源科技有限公司 | High-nickel single crystal nickel-cobalt-aluminum ternary cathode material and preparation method thereof |
| CN113955809A (en) * | 2021-12-20 | 2022-01-21 | 河南科隆新能源股份有限公司 | Nickel-cobalt-manganese-lithium aluminate positive electrode material with shell-core structure and preparation method thereof |
| WO2022129083A1 (en) * | 2020-12-15 | 2022-06-23 | Umicore | A positive electrode active material for rechargeable lithium-ion batteries |
| WO2022129077A1 (en) * | 2020-12-15 | 2022-06-23 | Umicore | A positive electrode active material for rechargeable lithium-ion batteries |
| WO2023231083A1 (en) * | 2022-05-31 | 2023-12-07 | 四川大学 | High-nickel layered positive electrode material with radial texture morphology and preparation method therefor |
| CN117374260A (en) * | 2023-12-07 | 2024-01-09 | 河南科隆新能源股份有限公司 | Preparation method of monocrystal-like lithium nickel cobalt manganese composite oxide |
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| CN115103815A (en) * | 2020-02-17 | 2022-09-23 | 尤米科尔公司 | Method for preparing positive electrode active material for rechargeable lithium ion battery |
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| WO2022129083A1 (en) * | 2020-12-15 | 2022-06-23 | Umicore | A positive electrode active material for rechargeable lithium-ion batteries |
| WO2022129077A1 (en) * | 2020-12-15 | 2022-06-23 | Umicore | A positive electrode active material for rechargeable lithium-ion batteries |
| CN113422046A (en) * | 2021-06-30 | 2021-09-21 | 湖南杉杉能源科技有限公司 | High-nickel single crystal nickel-cobalt-aluminum ternary cathode material and preparation method thereof |
| CN113422046B (en) * | 2021-06-30 | 2022-11-01 | 巴斯夫杉杉电池材料有限公司 | High-nickel single crystal nickel-cobalt-aluminum ternary cathode material and preparation method thereof |
| CN113955809B (en) * | 2021-12-20 | 2022-03-11 | 河南科隆新能源股份有限公司 | Nickel-cobalt-manganese-lithium aluminate positive electrode material with shell-core structure and preparation method thereof |
| CN113955809A (en) * | 2021-12-20 | 2022-01-21 | 河南科隆新能源股份有限公司 | Nickel-cobalt-manganese-lithium aluminate positive electrode material with shell-core structure and preparation method thereof |
| WO2023231083A1 (en) * | 2022-05-31 | 2023-12-07 | 四川大学 | High-nickel layered positive electrode material with radial texture morphology and preparation method therefor |
| CN117374260A (en) * | 2023-12-07 | 2024-01-09 | 河南科隆新能源股份有限公司 | Preparation method of monocrystal-like lithium nickel cobalt manganese composite oxide |
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Application publication date: 20190920 |