CN108682846A - Cobalt nickel lithium manganate ternary material and preparation method thereof - Google Patents
Cobalt nickel lithium manganate ternary material and preparation method thereof Download PDFInfo
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- CN108682846A CN108682846A CN201810534535.5A CN201810534535A CN108682846A CN 108682846 A CN108682846 A CN 108682846A CN 201810534535 A CN201810534535 A CN 201810534535A CN 108682846 A CN108682846 A CN 108682846A
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- lithium manganate
- ternary material
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- manganate ternary
- cobalt
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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
A kind of cobalt nickel lithium manganate ternary material and preparation method thereof, is related to lithium battery material field.The preparation method of the cobalt nickel lithium manganate ternary material includes the following steps：Nickel salt, cobalt salt and manganese salt are dissolved in solvent and are mixed to get mixed liquor；The ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise in the mixed liquor of stirring, then centrifugal treating obtains gel at 6000r/min 15000r/min；Gel drying is obtained into powder, stirred evenly after powder and lithium salts are mixed, roast 3 5h after ball milling at 600 750 DEG C.The preparation method of cobalt nickel lithium manganate ternary material provided by the invention is simple for process, easy to operate, can produce on a large scale and prepare the cobalt nickel lithium manganate ternary material with excellent properties.In addition the invention further relates to the cobalt nickel lithium manganate ternary materials that the preparation method of above-mentioned cobalt nickel lithium manganate ternary material is prepared.
Description
Technical field
The present invention relates to a kind of lithium battery material field, and more particularly to a kind of cobalt nickel lithium manganate ternary material and its preparation
Method.
Background technology
Cobalt acid lithium is most widely used lithium battery material at present, but cobalt resource is increasingly deficient and expensive, serious shadow
It rings to its utilization.Cobalt nickel lithium manganate ternary material is with relatively inexpensive nickel and manganese instead of in cobalt acid lithium 2/3rds or more
Cobalt becomes to effectively reduce the cost of material and expand raw material sources by people's extensive concern and research
One of lithium battery material.
The preparation method of current existing cobalt nickel lithium manganate ternary material has raw material is directly mixed or is mixed after roast
Solid phase method, by coprecipitation dry after dissolution of raw material mixed precipitation, using solvent dispersion and mixed raw material gel method, use
Template arranges the template being oriented to etc. a variety of methods to limit raw material, but nickle cobalt lithium manganate three is prepared in above-mentioned method
First material all has certain defect, and if uniform particle diameter is poor, poor circulation etc. cannot meet the needs of using.
Invention content
The purpose of the present invention is to provide a kind of preparation method of cobalt nickel lithium manganate ternary material, with it is simple for process,
Easy to operate, the advantages of capable of producing on a large scale.
Another object of the present invention is to provide a kind of cobalt nickel lithium manganate ternary material, with excellent cycle performance,
Positive electrode be can be used as applied in lithium battery.
The present invention solves its technical problem using following technical scheme to realize.
A kind of preparation method of cobalt nickel lithium manganate ternary material, is prepared by following steps：
Nickel salt, cobalt salt and manganese salt are dissolved in solvent and are mixed to get mixed liquor；
The ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise in the mixed liquor of stirring, then in 6000r/min-
Centrifugal treating obtains gel under 15000r/min；
Gel drying is obtained into powder, stirs evenly after powder and lithium salts are mixed, roasted at 600-750 DEG C after ball milling
3-5h。
Further, in a preferred embodiment of the present invention, nickel in above-mentioned nickel salt, cobalt salt, manganese salt and lithium salts, cobalt, manganese, lithium
Molar ratio is 3-4：1-2：1-2：6-10.
Further, in a preferred embodiment of the present invention, above-mentioned to be added dropwise to the ammonia spirit of ethylene diamine tetra methylene phosphonic acid
After in the mixed liquor of stirring, the pH that mixed liquor is adjusted using ammonium hydroxide is 7-9.
Further, in a preferred embodiment of the present invention, in above-mentioned mixed liquor ethylene diamine tetra methylene phosphonic acid and nickel mole
Than for 1-3：1.
Further, in a preferred embodiment of the present invention, above-mentioned that microwave heating is carried out while centrifugal treating.
Further, in a preferred embodiment of the present invention, above-mentioned microwave heating while centrifugal treating is to 60-80 DEG C.
Further, in a preferred embodiment of the present invention, above-mentioned stir evenly is to stir 20- at 150-250r/min
50min。
Further, in a preferred embodiment of the present invention, above-mentioned ball milling is the ball milling 45-120min at 80-150r/min.
Further, in a preferred embodiment of the present invention, above-mentioned roasting carries out in an inert atmosphere.
It is to use above-mentioned cobalt nickel lithium manganate ternary material the present invention also provides a kind of cobalt nickel lithium manganate ternary material
Preparation method be prepared.
The advantageous effect of the cobalt nickel lithium manganate ternary material of the embodiment of the present invention and preparation method thereof is：The embodiment of the present invention
The preparation method of the cobalt nickel lithium manganate ternary material of offer includes the following steps：Nickel salt, cobalt salt and manganese salt are dissolved in solvent and mixed
Conjunction obtains mixed liquor；The ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise in the mixed liquor of stirring, then in 6000r/
Centrifugal treating obtains gel under min-15000r/min；Gel drying is obtained into powder, is stirred after powder and lithium salts are mixed equal
After even, ball milling 3-5h is roasted at 600-750 DEG C.The preparation method technique letter of cobalt nickel lithium manganate ternary material provided by the invention
It is single, it is easy to operate, it can produce on a large scale and prepare the cobalt nickel lithium manganate ternary material with excellent properties.In addition the present invention is gone back
It is related to the cobalt nickel lithium manganate ternary material that the preparation method of above-mentioned cobalt nickel lithium manganate ternary material is prepared, with excellent
Cycle performance can be used as positive electrode applied in lithium battery.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Cobalt nickel lithium manganate ternary material of the embodiment of the present invention and preparation method thereof is specifically described below.
A kind of preparation method of cobalt nickel lithium manganate ternary material, is prepared by following steps：
Nickel salt, cobalt salt and manganese salt are dissolved in solvent and are mixed to get mixed liquor；Nickel salt, cobalt salt, manganese salt are preferably water solubility
Salt；Solvent is preferably deionized water.
The ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise in the mixed liquor of stirring, then in 6000r/min-
Centrifugal treating obtains gel under 15000r/min；Preferably, the ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise to stirring
After in mixed liquor, the pH that mixed liquor is adjusted using ammonium hydroxide is 7-9；Preferably, ethylene diamine tetra methylene phosphonic acid and nickel in mixed liquor
Molar ratio is 1-3：1；Preferably, the time of centrifugal treating is 1-3h；Preferably, microwave is carried out while centrifugal treating to add
Heat；Preferably, while centrifugal treating microwave heating to 60-80 DEG C.
Gel drying is obtained into powder, stirs evenly after powder and lithium salts are mixed, roasted at 600-750 DEG C after ball milling
3-5h.Preferably, nickel in nickel salt, the cobalt salt, the manganese salt and the lithium salts, cobalt, manganese, lithium molar ratio be 3-4：1-2：1-
2：6-10；Preferably, stir evenly is to stir 20-50min at 150-250r/min；Preferably, ball milling is in 80-150r/
Ball milling 45-120min under min；Preferably, roasting carries out in an inert atmosphere；Inert gas is preferably nitrogen or argon gas；
Preferably, water or organic solvent washing are used at least once before gel drying.
The preparation method of cobalt nickel lithium manganate ternary material provided in an embodiment of the present invention first presses nickel salt, cobalt salt and manganese salt
Proportioning is mixed to get mixed liquor after being dissolved using solvent, is then added to the ammonia spirit of complexing agent ethylene diamine tetra methylene phosphonic acid
Mixed liquor high speed centrifugal treating, obtains finely dispersed gel, finally by after the gel drying with nickel salt ball after mixing
Mill is uniformly dispersed, roasts and obtain finished product, not only simple for process, easy to operate, and can adequately mix raw material uniform, obtains
Cobalt nickel lithium manganate ternary material with excellent cycling performance.
It is to use above-mentioned cobalt nickel lithium manganate ternary material the present invention also provides a kind of cobalt nickel lithium manganate ternary material
Preparation method be prepared, stable structure and uniform particle sizes, have excellent cycle performance, be suitable as lithium battery just
Pole material.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of cobalt nickel lithium manganate ternary material is present embodiments provided, is prepared using following steps：
S11,4 are pressed：2：2：10 molar ratio weighs nickel sulfate, cobaltous sulfate, manganese sulfate and lithium carbonate；By nickel sulfate, sulfuric acid
Cobalt and manganese sulfate are mixed to get mixed liquor after being dissolved in respectively in deionized water.
S12, the ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise in the mixed liquor stirred with 30r/min, makes mixing
The molar ratio of ethylene diamine tetra methylene phosphonic acid and nickel is 3 in liquid：1, the pH that mixed liquor is adjusted using ammonium hydroxide is 8.5, is then existed
Centrifugal treating 1.5h obtains gel under 9000r/min.
S13, gel is dried to obtain powder at 50 DEG C, is stirred at 180r/min after powder and lithium carbonate are mixed
30min is stirred evenly, and then roasts 4.5h in the nitrogen environment at 120r/min after ball milling 60min at 680 DEG C.
Embodiment 2
A kind of cobalt nickel lithium manganate ternary material is present embodiments provided, is prepared using following steps：
S21,3.5 are pressed：1.5：1.5：7.5 molar ratio weighs nickel sulfate, cobaltous sulfate, manganese sulfate and lithium carbonate；By sulfuric acid
Nickel, cobaltous sulfate and manganese sulfate are mixed to get mixed liquor after being dissolved in respectively in deionized water.
S22, the ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise in the mixed liquor stirred with 60r/min, makes mixing
The molar ratio of ethylene diamine tetra methylene phosphonic acid and nickel is 2 in liquid：1, the pH that mixed liquor is adjusted using ammonium hydroxide is 8.1, is then existed
Centrifugal treating 1h obtains gel under 12000r/min.
S23, gel is dried to obtain powder at 60 DEG C, is stirred at 210r/min after powder and lithium carbonate are mixed
25min is stirred evenly, and then roasts 4h in the nitrogen environment at 100r/min after ball milling 90min at 720 DEG C.
Embodiment 3
A kind of cobalt nickel lithium manganate ternary material is present embodiments provided, is prepared using following steps：
S31,3 are pressed：1.1：1.1：6.5 molar ratio weighs nickel sulfate, cobaltous sulfate, manganese sulfate and lithium carbonate；By nickel sulfate,
Cobaltous sulfate and manganese sulfate are mixed to get mixed liquor after being dissolved in respectively in deionized water.
S32, the ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise in the mixed liquor stirred with 40r/min, makes mixing
The molar ratio of ethylene diamine tetra methylene phosphonic acid and nickel is 2.5 in liquid：1, the pH that mixed liquor is adjusted using ammonium hydroxide is 7.3, is then existed
Centrifugal treating 3h obtains gel under 6500r/min, and microwave heating mixed liquor is to 65 DEG C while centrifugal treating.
S33, gel is dried to obtain powder at 55 DEG C, is stirred at 180r/min after powder and lithium carbonate are mixed
35min is stirred evenly, and then roasts 5h in the nitrogen environment at 85r/min after ball milling 110min at 635 DEG C.
Embodiment 4
A kind of cobalt nickel lithium manganate ternary material is present embodiments provided, is prepared using following steps：
S41,3.5 are pressed：1.3：1.3：8.5 molar ratio weighs nickel sulfate, cobaltous sulfate, manganese sulfate and lithium carbonate；By sulfuric acid
Nickel, cobaltous sulfate and manganese sulfate are mixed to get mixed liquor after being dissolved in respectively in deionized water.
S42, the ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise in the mixed liquor stirred with 60r/min, makes mixing
The molar ratio of ethylene diamine tetra methylene phosphonic acid and nickel is 1.5 in liquid：1, the pH that mixed liquor is adjusted using ammonium hydroxide is 8.7, is then existed
Centrifugal treating 2.5h obtains gel under 12500r/min, by mixed liquor microwave heating to 75 DEG C while centrifugal treating.
S43, gel is made after being washed with deionized three times to be dried to obtain powder at 72 DEG C, powder and lithium carbonate is mixed
25min is stirred after conjunction at 160r/min to stir evenly, then the nitrogen at 145r/min after ball milling 55min at 690 DEG C
3.5h is roasted in environment.
The present embodiment 1-4 cobalt nickel lithium manganate ternary materials being prepared are prepared into positive electrode to carry out with 1C multiplying powers
100 charge and discharge cycles tests, capacity retention ratio show it with excellent cycle performance 90% or more.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of cobalt nickel lithium manganate ternary material, which is characterized in that it is prepared by following steps：
Nickel salt, cobalt salt and manganese salt are dissolved in solvent and are mixed to get mixed liquor；
The ammonia spirit of ethylene diamine tetra methylene phosphonic acid is added dropwise in the mixed liquor of stirring, then in 6000r/min-
Centrifugal treating obtains gel under 15000r/min；
The gel drying is obtained into powder, will the powder and lithium salts mix after stir evenly, after ball milling at 600-750 DEG C
Roast 3-5h.
2. the preparation method of cobalt nickel lithium manganate ternary material according to claim 1, which is characterized in that the nickel salt, institute
State nickel in cobalt salt, the manganese salt and the lithium salts, cobalt, manganese, lithium molar ratio be 3-4：1-2：1-2：6-10.
3. the preparation method of cobalt nickel lithium manganate ternary material according to claim 1, which is characterized in that by ethylenediamine tetramethyl
After the ammonia spirit of fork phosphonic acids is added dropwise in the mixed liquor of stirring, the pH that the mixed liquor is adjusted using ammonium hydroxide is 7-9.
4. the preparation method of cobalt nickel lithium manganate ternary material according to claim 1, which is characterized in that in the mixed liquor
Ethylene diamine tetra methylene phosphonic acid and nickel molar ratio be 1-3：1.
5. the preparation method of cobalt nickel lithium manganate ternary material according to claim 1, which is characterized in that at the centrifugation
Microwave heating is carried out while reason.
6. the preparation method of cobalt nickel lithium manganate ternary material according to claim 5, which is characterized in that at the centrifugation
Microwave heating is to 60-80 DEG C while reason.
7. the preparation method of cobalt nickel lithium manganate ternary material according to claim 1, which is characterized in that described to stir evenly
It is to stir 20-50min at 150-250r/min.
8. the preparation method of cobalt nickel lithium manganate ternary material according to claim 6, which is characterized in that the ball milling be
Ball milling 45-120min under 80-150r/min.
9. the preparation method of cobalt nickel lithium manganate ternary material according to claim 6, which is characterized in that the roasting is lazy
It is carried out under property gaseous environment.
10. a kind of cobalt nickel lithium manganate ternary material, which is characterized in that it is using as claimed in any one of claims 1-9 wherein
The preparation method of cobalt nickel lithium manganate ternary material is prepared.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113620351A (en) * | 2021-07-02 | 2021-11-09 | 湖北百杰瑞新材料股份有限公司 | Method for preparing nickel-cobalt-manganese ternary material precursor |
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| CN105794841A (en) * | 2014-12-26 | 2016-07-27 | 财团法人工业技术研究院 | Antibacterial composite material and manufacturing method thereof |
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|---|---|---|---|---|
| CN1711626A (en) * | 2002-11-08 | 2005-12-21 | 福吉米株式会社 | Polishing composition and rinsing composition |
| CN1641914A (en) * | 2004-12-24 | 2005-07-20 | 清华大学 | Lithium ion cell anode material and its preparing method |
| CN103280574A (en) * | 2013-05-29 | 2013-09-04 | 上海电力学院 | Lithium-enriched ternary anode material of power lithium-ion battery and preparation method of lithium-enriched ternary anode material |
| CN105794841A (en) * | 2014-12-26 | 2016-07-27 | 财团法人工业技术研究院 | Antibacterial composite material and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113620351A (en) * | 2021-07-02 | 2021-11-09 | 湖北百杰瑞新材料股份有限公司 | Method for preparing nickel-cobalt-manganese ternary material precursor |
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