CN109686932A - A kind of preparation method by the nickelic tertiary cathode material of polynary coating modification - Google Patents
A kind of preparation method by the nickelic tertiary cathode material of polynary coating modification Download PDFInfo
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- CN109686932A CN109686932A CN201811515799.2A CN201811515799A CN109686932A CN 109686932 A CN109686932 A CN 109686932A CN 201811515799 A CN201811515799 A CN 201811515799A CN 109686932 A CN109686932 A CN 109686932A
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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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- 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 by the nickelic tertiary cathode material of polynary coating modification, comprising the following steps: 1), with nickelic tertiary cathode material LiNixC0yMn1‑x‑yO2(0.6≤x≤0.85,0.05≤y≤0.2) is matrix, and the A of coating containing aluminium and boracic coating B is added, is put into high-speed mixer and uniformly mixes；2) mixture, is subjected to low temperature oxygen-enriched sintering, natural cooling after keeping the temperature 5-10 hours after being warming up to 350-700 DEG C with the rate of 3-7 DEG C/min obtains modified nickelic tertiary cathode material after except iron sieving.The solid phase method that the present invention uses coats nickelic ternary material uniformly by both the above metallic element, the free lithium that can be effectively improved in material, the structure of stable crystal, the corrosion reaction that effective barrier material and battery electrolyte occur；Simple process, it is low for equipment requirements, it is practical, it can mass production.
Description
Technical field
The present invention relates to a kind of preparation methods by the nickelic tertiary cathode material of polynary coating modification, and in particular to a kind of
Mixed solid phase doping, high temperature sintering are crushed solid phase cladding, then the preparation method that low-temperature sintering combines, can prepare high capacity, excellent
The high voltage nickel-cobalt-manganternary ternary anode material of circulation.
Background technique
Lithium ion battery has been promoted in the whole world as New Energy Industry, and nickel-cobalt-manganese ternary is as lithium ion battery
One kind of positive electrode, is always the emphasis studied in industry and developing direction, and to be widely used in digital 3C Product, electronic
Tool, electric vehicle and electric car field.With the high speed development in market, people propose lithium battery higher within 2018
It is required that, it is desirable that next-generation battery product has both safety, consistency, higher capacity, the advantage of the various aspects such as more excellent circulation.And
In view of falling off for subsidy policy, higher price-performance ratio product be also existing market it is urgent.Comprehensively consider nickelic tertiary cathode
The exploitation of material is imperative.
Nickelic ternary dissociates lithium during the sintering process can higher, in air moisture and carbon dioxide is easy reacts generation
Lithium hydroxide and lithium carbonate cause the acidity-basicity ph value of material that can accordingly increase.The easy moisture absorption is at paste during battery pasting,
Influence the process of pole piece.In addition under the action of battery electrolyte, the structure of crystal is easily destroyed and leads to cycle performance
It is deteriorated.And under extreme conditions, bulge, flatulence, the security risks such as on fire are easy to appear.
Coating modification is in the majority with liquid phase method at present, but its complex process, and at high cost, process is uncontrollable, to equipment and production
Environmental requirement is stringent.
Summary of the invention
The technical problem to be solved by the present invention is to overcome lacking for the technology coating modifying of nickelic ternary in the prior art complexity
It falls into, a kind of preparation method by the nickelic tertiary cathode material of polynary coating modification is provided.
In order to solve the above-mentioned technical problems, the present invention provides the following technical solutions:
A kind of preparation method by the nickelic tertiary cathode material of polynary coating modification, comprising the following steps:
1), with nickelic tertiary cathode material LiNixC0yMn1-x-yO2(0.6≤x≤0.85,0.05≤y≤0.2) is matrix,
The A of coating containing aluminium and boracic coating B is added, is put into high-speed mixer and uniformly mixes；
2) mixture, is subjected to low temperature oxygen-enriched sintering, keeps the temperature 5- after being warming up to 350-700 DEG C with the rate of 3-7 DEG C/min
Natural cooling after 10 hours obtains modified nickelic tertiary cathode material after except iron sieving.
Preferably, the mass fraction of the A of coating containing aluminium and boracic coating B are in modified nickelic tertiary cathode material
0.01%-1%.
Further, using ball mill, V-Mixer, cone-type mixer, inclined mixing machine or high speed in the step 1)
Mixing machine is mixed.
Further, atmosphere formula resistance furnace is used in step 2), pusher furnace or roller furnace carry out low temperature oxygen-enriched sintering.
Preferably, the coating containing aluminium A is the aluminium compounds such as nano-grade aluminum hydroxide or aluminium oxide.Boracic coating
B is the boron compounds such as nanoscale boron or boric acid.
Further, the flow of oxygen is 0.6~1.2m when low temperature oxygen-enriched sintering in the step 2)3/h。
The beneficial effects obtained by the present invention are as follows being: the solid phase method that the present invention uses makes nickelic ternary material by both the above
Metallic element uniformly coats, and wherein aluminium coating A can effectively improve the free lithium in material, reduces the soda acid of material
Degree forms layer protecting film, the corrosion reaction that effective barrier material and battery electrolyte occur；Boracic coating B can stablize
The structure of crystal keeps the structure of crystal more complete, significantly improves the processing performance of battery by modified, safety and
Cyclicity has also obtained significantly being promoted.The method simple process, it is low for equipment requirements, it is practical, it can mass production.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the SEM figure of product 1 in the embodiment of the present invention；
Fig. 2 is the half-cell performance test (2.75- that product 1 carries out charge and discharge under 0.5C multiplying power in the embodiment of the present invention
4.3V)。
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
This example is with nickelic tertiary cathode material LiNi0.6Co0.2Mn0.2O2For matrix 5kg, with nano aluminium oxide 9.4g, receive
Meter level boron oxide 24.2g, is put into high-speed mixer and uniformly mixes, and takes out after mixing 30 minutes by 150rpm.Mixed object
Material is put into atmosphere formula resistance furnace low temperature sintering, rose to 680 DEG C by 1.5 hours, keeps the temperature 10 hours, and giving amount of oxygen is 0.8m3/
h.325 meshes point were taken out after natural cooling, obtained product 1.Do SEM scanning electron microscope (referring to Fig. 1)；Simultaneously to half electricity of the product
Pond performance test (2.75-4.3V) carries out charge and discharge (referring to fig. 2) under 0.5C multiplying power.
Example 2:
This example is with nickelic tertiary cathode material LiNi0.6Co0.1Mn0.3O2For matrix 5kg, with alumina in Nano level 9.4g,
Nanoscale boric acid 42.8g, is put into planetary ball mill and uniformly mixes, and takes out after five minutes by 300rpm mixing.Mixed material
It is put into atmosphere formula resistance furnace low temperature sintering, 660 DEG C was risen to by 1.5 hours, keeps the temperature 10 hours, giving amount of oxygen is 0.8m3/h。
325 meshes point were taken out after natural cooling, obtained modified nickelic positive electrode.
Example 3:
This example is with nickelic tertiary cathode material LiNi0.7Co0.1Mn0.2O2For matrix 5kg, match nano-grade aluminum hydroxide
14.4g, nanoscale boric acid 42.8g, are put into inclined mixing machine and uniformly mix, and take out after sixty minutes by 50rpm mixing.Mixed
Material be put into atmosphere formula resistance furnace low temperature sintering, by rising within 1.5 hours 500 DEG C, keep the temperature 10 hours, giving amount of oxygen is
1.2m3/h.325 meshes point were taken out after natural cooling, obtained modified nickelic positive electrode.
Example 4:
This example is with nickelic tertiary cathode material LiNi0.8Co0.1Mn0.1O2For matrix 5kg, with alumina in Nano level 9.4g,
Nanoscale boron 24.2g, is put into high-speed mixer and uniformly mixes, and takes out after twenty minutes by 200rpm mixing.Mixed
Material is put into atmosphere formula resistance furnace low temperature sintering, rose to 400 DEG C by 2 hours, keeps the temperature 10 hours, and giving amount of oxygen is 1.2m3/
h.325 meshes point were taken out after natural cooling, obtained modified nickelic positive electrode.
Conclusion: table 1 is the comparison of product 1 and its matrix object, it is therefore seen that modified greatly reduce the residual lithium of material surface
And pH value, improve battery processability and safety.
The comparison of 1 product 1 of table and its matrix object
| Sample | LiOH% | LiCo3% | Li+ppm | PH | Remarks |
| Product 1 is before modified | 0.176 | 0.097 | 692.6 | 11.98 | It is higher |
| Product 1 is modified | 0.167 | 0.09 | 604 | 11.9 | It reduces |
Fig. 1 can be seen that modified LiNi0.6Co0.2Mn0.2O2Surface forms one layer of uniform clad.Fig. 2 charge and discharge
The 0.5C specific capacity of material is 165.8mAh/g in curve, maintains higher specific discharge capacity.Capacity is possessed after recycling 100 weeks
Rate has good cycle performance by 98.2%, by modified.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (7)
1. a kind of preparation method by the nickelic tertiary cathode material of polynary coating modification, which comprises the following steps:
1), with nickelic tertiary cathode material LiNixC0yMn1-x-yO2(0.6≤x≤0.85,0.05≤y≤0.2) is matrix, is added
The A of coating containing aluminium and boracic coating B, is put into high-speed mixer and uniformly mixes；
2) mixture, is subjected to low temperature oxygen-enriched sintering, it is small that 5-10 is kept the temperature after being warming up to 350-700 DEG C with the rate of 3-7 DEG C/min
When after natural cooling, by except iron sieving after obtain modified nickelic tertiary cathode material.
2. passing through the preparation method of the nickelic tertiary cathode material of polynary coating modification as described in claim 1, which is characterized in that
The mass fraction of the A of coating containing aluminium and boracic coating B are 0.01%-1% in modified nickelic tertiary cathode material.
3. a kind of preparation method by the nickelic tertiary cathode material of polynary coating modification as claimed in claim 1 or 2, special
Sign is, is carried out in the step 1) using ball mill, V-Mixer, cone-type mixer, inclined mixing machine or high-speed mixer
Mixing.
4. passing through the preparation method of the nickelic tertiary cathode material of polynary coating modification as described in claim 1, which is characterized in that
Atmosphere formula resistance furnace is used in step 2), pusher furnace or roller furnace carry out low temperature oxygen-enriched sintering.
5. a kind of preparation method by the nickelic tertiary cathode material of polynary coating modification as described in claim 1, feature
It is, the A of coating containing aluminium is nano-grade aluminum hydroxide or aluminium oxide.
6. a kind of preparation method by the nickelic tertiary cathode material of polynary coating modification as described in claim 1, feature
It is, the boracic coating B is nanoscale boron or boric acid.
7. a kind of preparation method by the nickelic tertiary cathode material of polynary coating modification as described in claim 1, feature
It is, the flow of oxygen is 0.6~1.2m when low temperature oxygen-enriched sintering in the step 2)3/h。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110534717A (en) * | 2019-09-04 | 2019-12-03 | 厦门厦钨新能源材料有限公司 | Positive electrode and preparation method thereof |
| CN111162271A (en) * | 2019-06-12 | 2020-05-15 | 北京当升材料科技股份有限公司 | Multi-element anode material, preparation method thereof and lithium ion battery |
| CN111276691A (en) * | 2020-03-24 | 2020-06-12 | 江门市科恒实业股份有限公司 | High-voltage single-crystal low-cobalt ternary cathode material and preparation method thereof |
| CN111422921A (en) * | 2019-12-31 | 2020-07-17 | 蜂巢能源科技有限公司 | Polycrystalline high-nickel ternary positive electrode material, preparation method thereof, positive plate and lithium ion battery |
| CN111952547A (en) * | 2019-05-16 | 2020-11-17 | 天津国安盟固利新材料科技股份有限公司 | Surface-coated modified lithium ion battery positive electrode material and preparation method thereof |
| CN113830846A (en) * | 2021-11-24 | 2021-12-24 | 湖南长远锂科股份有限公司 | Coating modified cathode material and preparation method thereof |
| CN114400308A (en) * | 2021-12-30 | 2022-04-26 | 浙江浙能中科储能科技有限公司 | Preparation and application method of modified manganese dioxide electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111952547A (en) * | 2019-05-16 | 2020-11-17 | 天津国安盟固利新材料科技股份有限公司 | Surface-coated modified lithium ion battery positive electrode material and preparation method thereof |
| CN111162271A (en) * | 2019-06-12 | 2020-05-15 | 北京当升材料科技股份有限公司 | Multi-element anode material, preparation method thereof and lithium ion battery |
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| CN111276691A (en) * | 2020-03-24 | 2020-06-12 | 江门市科恒实业股份有限公司 | High-voltage single-crystal low-cobalt ternary cathode material and preparation method thereof |
| CN113830846A (en) * | 2021-11-24 | 2021-12-24 | 湖南长远锂科股份有限公司 | Coating modified cathode material and preparation method thereof |
| CN113830846B (en) * | 2021-11-24 | 2022-03-04 | 湖南长远锂科股份有限公司 | Coating modified cathode material and preparation method thereof |
| CN114400308A (en) * | 2021-12-30 | 2022-04-26 | 浙江浙能中科储能科技有限公司 | Preparation and application method of modified manganese dioxide electrode material |
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Application publication date: 20190426 |