CN109286001A - A kind of modified lithium nickelate preparation method - Google Patents
A kind of modified lithium nickelate preparation method Download PDFInfo
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- CN109286001A CN109286001A CN201811032185.9A CN201811032185A CN109286001A CN 109286001 A CN109286001 A CN 109286001A CN 201811032185 A CN201811032185 A CN 201811032185A CN 109286001 A CN109286001 A CN 109286001A
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- lithium nickelate
- lithium
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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
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of modified lithium nickelate preparation method of technical field of lithium ion, using coprecipitation by metallic element M Uniform Doped to presoma Ni (OH)2Body phase in, by sintering by Co3O4It is coated to doping type lithium nickelate surface, obtains the lithium nickelate as anode material for lithium-ion batteries;The present invention improves the stability of lithium nickelate internal crystal structure by body phase Uniform Doped, reduces the Li of nickel layer in lithium nickelate crystal+/Ni2+Mixing degree, improve its high rate performance and cycle performance as anode material for lithium-ion batteries, meanwhile being reacted by the residual lithium of surface coated cobaltosic oxide part and doping type lithium nickelate surface and generating cobalt acid lithium, the capacity of lithium nickelate is increased while consuming residual lithium.
Description
Technical field
The present invention relates to technical field of lithium ion, specially a kind of modified lithium nickelate preparation method.
Background technique
Compared with the secondary cells such as traditional plumbic acid, lithium ion battery possesses voltage height, capacity height, and energy density is big, follows
Ring performance is good, many-sided advantage such as environmental-friendly.The performance of lithium ion battery is largely more dependent upon positive electrode.Cobalt acid
When positive electrode of the lithium as lithium ion battery, there are at high cost, thermal stability be poor and the series of negative such as cobalt pollution environment
Problem, it is therefore desirable to develop novel anode material for lithium-ion batteries.
Lithium nickelate is a very outstanding potential alternative materials because its capacity is high and has price advantage.However
The case where easily occurring cationic mixing and surface in the lattice of lithium nickelate there are residual lithiums, thus reduce lithium nickelate cycle performance and
High rate performance.The method of wet process cladding inert compound is provided in patent CN102447105B, improves the electricity of lithium nickelate
Pond performance.However, on the one hand, increase inertia coating, namely the covert total capacity for reducing lithium nickelate;On the other hand,
There is no make improvements the lithium nickel mixing in lithium nickelate body phase to this patent.Therefore, existing lithium ion technology of preparing exists again
Rate performance and the low problem of cycle performance.
Summary of the invention
In view of the above technical problems, the present invention provides a kind of modified lithium nickelate preparation method, and this method effectively improves lithium
The low problem of ion battery positive electrode capacity improves the high rate performance and cycle performance of lithium ion preparation.
The present invention adopts the following technical scheme:
A kind of modified lithium nickelate preparation method, comprising the following steps:
S1: presoma Ni is preparedxM1-x(OH)2, wherein the value range of x is 0.95≤x≤1, and M is metallic element;
S2: the S1 presoma prepared is passed through into batch mixer with lithium salts in proportion and is mixed, and mixed material is sintered, is obtained
To LiNiyM1-yO2, wherein the value range of y is 0.95≤y≤1;
S3: the LiNi that S2 is sinteredyM1-yO2(0.95≤y≤1) and Co3O4It is mixed with planetary ball mill;
S4: the mixed material after ball milling is sintered, and obtains surface cladding LiCoO2/Co3O4LiNizM1-zO2(0.95≤z
≤ 0.999).
Preferably, in S1, nickel source and doped source are prepared by presoma Ni using coprecipitationxM1-x(OH)2, nickel
Source is at least one of nickel sulfate, nickel nitrate, nickel chloride, and doped source is at least one of sulfate, nitrate, chloride, is total to
The preparation condition of the precipitation method are as follows: reaction temperature is 40-60 DEG C, and the ammonia density in precipitating reagent is 4-9mol/L, alkali dense in precipitating reagent
Degree is 2-8mol/L, and the pH of precipitating reagent is 9.8-11.5.
Preferably, in S2, the mixing revolving speed of batch mixer is 400-2000rpm, mixing time 1-4h, Li:(Ni
+ M) molar ratio be 1.01-1.15.
Preferably, in S2, it first is warming up to 400-600 DEG C with the heating rate of 1-6 DEG C/min, is sintered 4-8h;Again
Continue to be warming up to 680-820 DEG C with the heating rate of 1-6 DEG C/min, be sintered 12-20h, the atmosphere of sintering reaction is oxygen or sky
Gas.
Preferably, in S3, planetary ball mill revolving speed is 150-350rpm, and ratio of grinding media to material is (1-3): 1, Ball-milling Time
For 1-4h.
Preferably, in S3, Co (Co3O4): LiNiyM1-yO2Molar ratio be 0.3-1.
Preferably, in S3, the particle size of Co3O4 is between 20-100nm.
Preferably, in S4, sintering is warming up to 650-800 DEG C by the heating rate of 1-6 DEG C/min, sintering time
For 3-6h, the atmosphere of sintering process is oxygen or air atmosphere.
Preferably, in S1, the metal M of doping is Zr, W, Ti, Al, Nb, at least one of Mn.
Preferably, in S1, metal M and presoma NixM1-x(OH)2Molar ratio be 0.1-5.
Compared with prior art, the beneficial effects of the present invention are:
The present invention prepares presoma Ni using coprecipitationxM1-x(OH)2, metal M is uniformly doped to presoma body phase, is kept away
Exempt to improve the stability inside lithium nickelate using lithium nickelate as the lithium nickel mixing inside when anode material of lithium battery;It is logical
Oversintering is by Co3O4It reacts with the residual lithium on surface, forms cobalt acid lithium on lithium nickelate surface, while reducing residual lithium content, subtract
The inertia cladding for having lacked lithium nickelate surface, to improve the total capacity of lithium nickelate;Prepared by the method modified lithium nickelate
As the positive electrode of lithium ion battery, the capacity of lithium ion battery is effectively raised, improves the multiplying power of lithium ion preparation
Performance and cycle performance.
Detailed description of the invention
Fig. 1 is material SEM figure prepared by the embodiment of the present invention 1.
Fig. 2 is material SEM figure prepared by the embodiment of the present invention 2.
Fig. 3 is material SEM figure prepared by the embodiment of the present invention 3.
Fig. 4 is the material SEM figure of comparative example preparation of the present invention.
Fig. 5 is capacity (the 1C multiplying power test after material prepared by comparative example and embodiment 1,2,3 of the present invention is fabricated to battery
Condition)-circulation comparison diagram.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
A kind of modified lithium nickelate preparation method, specifically includes the following steps:
S1: presoma Ni is preparedxM1-x(OH)2, wherein the value range of x is 0.95≤x≤1, and M is metallic element;
Wherein, nickel source and doped source are prepared by presoma Ni using coprecipitationxM1-x(OH)2, nickel source is nickel sulfate, nitric acid
At least one of nickel, nickel chloride, doped source are at least one of sulfate, nitrate, chloride, and the metal M of doping is Zr, W,
At least one of Ti, Al, Nb, Mn, metal M and presoma NixM1-x(OH)2Molar ratio be 0.1-5.
The preparation condition of coprecipitation: reaction temperature is 40-60 DEG C, ammonia density 4-9mol/L, alkali concentration 2-8mol/L, PH
For 9.8-11.5, the crystal structure of specific morphology can be obtained under this condition;Metal M is uniformly doped to presoma body
Phase, M ion occupy the original Ni in part3+Position and stablize the structure on periphery and the oxonium ion on periphery, hence it is evident that reduce the de- of oxygen
It goes, greatly reduces Ni2+Formation, so that lithium nickel inside when reducing using lithium nickelate as anode material of lithium battery is mixed
Row, improves the high rate performance and cycle performance of lithium nickelate.
S2: the S1 presoma prepared is passed through into batch mixer with lithium salts in proportion and is mixed, and mixed material is burnt
Knot, obtains LiNiyM1-yO2, wherein the value range of y is 0.95≤y≤1;
Wherein, the mixing revolving speed of batch mixer is for the molar ratio of 400-2000rpm, mixing time 1-4h, Li:(Ni+M)
1.01-1.15, lithium salts are lithium carbonate or lithium hydroxide, and sintering uses double sintering, and the atmosphere of sintering reaction is oxygen or air,
It first is warming up to 400-600 DEG C with the heating rate of 1-6 DEG C/min, is sintered 4-8h, first step sintering is primarily to decompose hydrogen-oxygen
Change nickel and lithium salts and discharges byproduct gas H2O or CO2;This stage lithium salts and presoma Ni at a lower temperaturexM1-x(OH)2Point
Solution, decomposed at low temperature rate is relatively slow and avoids crystal cleavage caused by the release for decomposing gas;It is further continued for 1-6 DEG C/min's
Heating rate is warming up to 680-820 DEG C, is sintered 12-20h, and second step is sintered primarily to further solid phase reaction, obtains
Lithium nickelate carries out the solid phase reaction of modified lithium nickelate sufficiently, and higher temperature ensure that layer structure
It is formed.
S3: the LiNi that S2 is sinteredyM1-yO2(0.95≤y≤1) and Co3O4It is mixed with planetary ball mill;
Wherein, drum's speed of rotation 150-400rpm, ratio of grinding media to material are (1-3): 1, Ball-milling Time 1-4h, Co (Co3O4):
LiNixMn1-xO2Molar ratio be 0.3-1, Co3O4Particle size between 20-100nm, nanoscale Co3O4In ball action
Lower and LiNiyM1-yO2Mixing can be uniformly dispersed in its surface, ensure that the thickness nanoscale of cladding is controllable and consistency
And uniformity;The slow-speed of revolution is crossed, mixing is uneven, and excessive speeds increase the burden of equipment on one side, easily makes on the other hand
It is damaged at sample topography, selects 150-400rpm reasonably avoiding these two issues.
S4: the mixed material after ball milling is sintered, and obtains surface cladding LiCoO2/Co3O4LiNizM1-zO2(0.95
≤ z≤0.999).
Wherein, sintering is warming up to 650-800 DEG C by the heating rate of 1-6 DEG C/min, sintering time 3-6h, sintered
The atmosphere of journey be oxygen or air atmosphere, 650-800 DEG C at a temperature of, be not only completed cladding, can also realize residual lithium and oxygen
Change cobalt reaction and generate cobalt acid lithium, by being sintered Co3O4It reacts with the residual lithium on surface, forms cobalt acid lithium on lithium nickelate surface,
While reducing residual lithium content, reduce the inertia cladding on lithium nickelate surface, to improve the specific capacity of lithium nickelate.
Embodiment 1
Ni is prepared using coprecipitation0.95Ti0.05(OH)2Presoma;By Ni0.95Ti0.05(OH)2Presoma and lithium salts pass through mixing
After machine mixing, mixed material progress double sintering is obtained into LiNi0.95Ti0.05O2, first segment sintering temperature be 450 DEG C, first
The time of section sintering is 2h, and the temperature of second segment sintering is 720 DEG C, and the time of second segment sintering is 14h;By the production of double sintering
Product LiNi0.95Ti0.05O2The Co for being 40nm with particle size3O4It is mixed with planetary ball mill, Co (Co3O4): LiNi0.95Ti0.05O2
Molar ratio be 0.2, mixing time 2h;The material after ball milling is sintered 6h at 710 DEG C again, obtains LiCoO2/
Co3O4The LiNi of cladding0.95Ti0.05O2。
Embodiment 2
Ni is prepared using coprecipitation0.97W0.03(OH)2Presoma;By Ni0.97W0.03(OH)2Presoma and lithium salts pass through batch mixer
After mixing, mixed material progress double sintering is obtained into LiNi0.97W0.03O2, the temperature of first segment sintering is 550 DEG C, first segment
The time of sintering is 4h, and the temperature of second segment sintering is 710 DEG C, and the time of second segment sintering is 16h;By the product of double sintering
LiNi0.97W0.03O2The Co for being 30nm with particle size3O4It is mixed with planetary ball mill, Co (Co3O4): LiNi0.97W0.03O2Rub
You are than being 0.2, mixing time 1h;The material after ball milling is sintered 5h at 730 DEG C again, obtains LiCoO2/Co3O4Packet
The LiNi covered0.97W0.03O2。
Embodiment 3
Ni is prepared using coprecipitation0.99Zr0.01(OH)2Presoma;By Ni0.99Zr0.01(OH)2Presoma and lithium salts pass through mixing
After machine mixing, mixed material progress double sintering is obtained into LiNi0.99Zr0.01O2, first segment sintering temperature be 490 DEG C, first
The time of section sintering is 5h, and the temperature of second segment sintering is 760 DEG C, and the time of second segment sintering is 13h;By the production of double sintering
Product LiNi0.99Zr0.01O2With the Co for being 25nm with particle size3O4It is mixed with planetary ball mill, Co (Co3O4):
LiNi0.99Zr0.01O2Molar ratio be 0.2, mixing time 3h;Material after ball milling is sintered 3h at 750 DEG C, is obtained
To LiCoO2/Co3O4The LiNi of cladding0.96Zr0.04O2。
Comparative example
Ni (OH) is generated using the precipitation method2, with LiOHH20 is mixed with batch mixer, and is sintered, first in 490 DEG C of temperature
Lower sintering 5h, then 750 DEG C at a temperature of be sintered 12h, obtain LiNiO2。
The experimental data are shown in the following table for the material of the method for above-described embodiment and comparative example preparation:
Embodiment is compared with the physical property of comparative example;
Embodiment is compared with the chemical property of comparative example;
By upper table and attached drawing it is found that positive electrode of the prepared by the method modified lithium nickelate as lithium ion battery, effectively
The capacity for improving lithium ion battery, improve lithium ion preparation high rate performance and cycle performance.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (10)
1. a kind of modified lithium nickelate preparation method, comprising the following steps:
S1: presoma Ni is preparedxM1-x(OH)2, wherein the value range of x is 0.95≤x≤1, and M is metallic element;
S2: the S1 presoma prepared is passed through into batch mixer with lithium salts in proportion and is mixed, and mixed material is sintered, is obtained
To LiNiyM1-yO2, wherein the value range of y is 0.95≤y≤1;
S3: the LiNi that S2 is sinteredyM1-yO2(0.95≤y≤1) and Co3O4It is mixed with planetary ball mill;
S4: the mixed material after ball milling is sintered, and obtains surface cladding LiCoO2/Co3O4LiNizM1-zO2(0.95≤z
≤ 0.999).
2. a kind of modified lithium nickelate preparation method according to claim 1, it is characterised in that: in S1, using co-precipitation
Nickel source and doped source are prepared into presoma Ni by methodxM1-x(OH)2, nickel source be at least one of nickel sulfate, nickel nitrate, nickel chloride,
Doped source is at least one of sulfate, nitrate, chloride, the preparation condition of coprecipitation are as follows: reaction temperature 40-60
DEG C, the ammonia density in precipitating reagent is 4-9mol/L, and alkali concentration is 2-8mol/L in precipitating reagent, and the pH of precipitating reagent is 9.8-11.5.
3. a kind of modified lithium nickelate preparation method according to claim 1, it is characterised in that: in S2, batch mixer is mixed
Material revolving speed is 400-2000rpm, mixing time 1-4h, Li:(Ni+M) molar ratio be 1.01-1.15.
4. a kind of modified lithium nickelate preparation method according to claim 1, it is characterised in that: in S2, first with 1-6 DEG C/
The heating rate of min is warming up to 400-600 DEG C, is sintered 4-8h;It is further continued for being warming up to 680- with the heating rate of 1-6 DEG C/min
820 DEG C, it is sintered 12-20h, the atmosphere of sintering reaction is oxygen or air.
5. a kind of modified lithium nickelate preparation method according to claim 1, it is characterised in that: in S3, planetary ball mill
Revolving speed is 150-350rpm, and ratio of grinding media to material is (1-3): 1, Ball-milling Time 1-4h.
6. a kind of modified lithium nickelate preparation method according to claim 5, it is characterised in that: in S3, Co (Co3O4):
LiNiyM1-yO2Molar ratio be 0.3-1.
7. a kind of modified lithium nickelate preparation method according to claim 1, it is characterised in that: in S3, the partial size of Co3O4
Size is between 20-100nm.
8. a kind of modified lithium nickelate preparation method according to claim 1, it is characterised in that: in S4, sintering passes through 1-6
DEG C/heating rate of min is warming up to 650-800 DEG C, sintering time 3-6h, the atmosphere of sintering process is oxygen or air gas
Atmosphere.
9. a kind of modified lithium nickelate preparation method described in -8 according to claim 1, it is characterised in that: in S1, the gold of doping
Category M is Zr, W, Ti, Al, Nb, at least one of Mn.
10. a kind of modified lithium nickelate preparation method according to claim 9, it is characterised in that: in S1, metal M is with before
Drive body NixM1-x(OH)2Molar ratio be 0.1-5.
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Cited By (5)
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CN112151779A (en) * | 2020-09-18 | 2020-12-29 | 深圳市贝特瑞纳米科技有限公司 | Binary anode composite material and preparation method and application thereof |
CN112614990A (en) * | 2020-12-11 | 2021-04-06 | 格林美股份有限公司 | Nickel-manganese binary composite positive electrode material and preparation method thereof |
CN114426312A (en) * | 2022-01-13 | 2022-05-03 | 南京同宁新材料研究院有限公司 | Method for preparing high-pressure lithium cobaltate by using waste lithium cobaltate |
CN114566641A (en) * | 2022-02-28 | 2022-05-31 | 蜂巢能源科技股份有限公司 | Positive electrode material and preparation method and application thereof |
WO2024012605A1 (en) * | 2022-07-12 | 2024-01-18 | 宁波致良新能源有限公司 | Lithium nickelate positive electrode material and preparation method therefor, and application |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112151779A (en) * | 2020-09-18 | 2020-12-29 | 深圳市贝特瑞纳米科技有限公司 | Binary anode composite material and preparation method and application thereof |
CN112614990A (en) * | 2020-12-11 | 2021-04-06 | 格林美股份有限公司 | Nickel-manganese binary composite positive electrode material and preparation method thereof |
CN114426312A (en) * | 2022-01-13 | 2022-05-03 | 南京同宁新材料研究院有限公司 | Method for preparing high-pressure lithium cobaltate by using waste lithium cobaltate |
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CN114566641B (en) * | 2022-02-28 | 2024-02-23 | 蜂巢能源科技股份有限公司 | Positive electrode material and preparation method and application thereof |
WO2024012605A1 (en) * | 2022-07-12 | 2024-01-18 | 宁波致良新能源有限公司 | Lithium nickelate positive electrode material and preparation method therefor, and application |
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