CN109305698A - A kind of preparation method of unformed lithium ion anode material presoma - Google Patents
A kind of preparation method of unformed lithium ion anode material presoma Download PDFInfo
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- CN109305698A CN109305698A CN201811017392.7A CN201811017392A CN109305698A CN 109305698 A CN109305698 A CN 109305698A CN 201811017392 A CN201811017392 A CN 201811017392A CN 109305698 A CN109305698 A CN 109305698A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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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
- H01M4/50—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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
Abstract
A kind of preparation method of unformed lithium ion anode material presoma, it is that be made into concentration molar ratio be 5:3:2 or the metal mixed solution of other molar ratios to primary raw material by nickel salt, manganese salt and cobalt salt, the importings such as mixed salt solution, complexing agent ammonium hydroxide and precipitating reagent sodium hydroxide has been passed through in the reaction kettle of nitrogen using constant-current flow gauge and have been reacted；First bottom liquid in reaction kettle is heated up before reaction, reaction process controls constant temperature, while detecting pH value of reaction system with pH meter, and control rotating speed of agitator, while nitrogen is constantly passed through in reaction kettle；Granularity is detected using laser particle analyzer, after granularity reaches Spreading requirements, stop importing feed liquid and nitrogen, the spherical unformed lithium ion anode material precursor crystal grain of nanometer that large specific surface area, particle are loose, sintering is high-efficient, processing performance is good can be obtained through certain temperature drying screening in sediment ageing, washing, centrifugation to preparation.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field, before specially a kind of unformed lithium ion anode material
Drive the preparation method of body.
Background technique
Ternary lithium battery technology is anode using ternary material, and cathode is the mixed of artificial graphite and other advanced negative electrode materials
It is fit.Positive ternary material is mainly nickel cobalt manganese, with the relatively low and small in size spy of height ratio capacity, long circulation life, cost
Point in addition, having good synergistic effect between three kinds of elements, therefore is received and is widely applied.In redox energy storage,
Nickel cobalt manganese is main ingredient, and the content by changing nickel cobalt manganese element in material to effectively improve the specific capacity of material is three
The critical issue that first material strides forward forward again.Ternary lithium battery main feature or energy density are big, and voltage is higher, so equally
The battery cell capacity of weight is bigger, and the distance that car is run is also just farther, and speed also can be faster.
In general, tertiary cathode material in the market compared to other lithium electricity positive electrodes have height ratio capacity and it is low at
It is this characteristics of, low but there is also capacity retention ratios, the defects of thermal stability is poor.The unformed ternary prepared using coprecipitation
Presoma can be used for sintering into bigger serface monocrystalline ternary material, be fabricated to high-rate lithium battery be mainly used for unmanned plane and
Electric tool heavy-current discharge and automobile starting power supply use；It can also be used to improve unit volume material energy densities.
The monocrystalline type ternary precursor material sold currently on the market, technique preparation require height, are little particle, size mostly
At 5-6 μm, the grain growth time is too long, and nucleus crystallization degree is high, and particle diameter distribution control is poor, and tap density is high, causes to be fired into
When monocrystal material, there is micro mist, primary particle chip has non-fusion phenomenon of reuniting, and stability is poor, and requires by after baking,
Material processing cost is caused to increase in this way, energy consumption is higher.And the persursor material performance quality prepared is largely determined
Determine the more insoluble technical problem of performance and persursor material producer of tertiary cathode material.
Summary of the invention
The purpose of the present invention is to provide a kind of unformed lithium ion anode material presomas and preparation method thereof, to solve
The problems mentioned above in the background art.
In order to solve the above technical problem, the present invention provides following technical solutions: a kind of unformed lithium ion anode material
Presoma and preparation method thereof, comprising the following steps:
It 1) is that be made into a certain concentration molar ratio be 5:3:2 or Ni to primary raw material by nickel salt, manganese salt and cobalt saltmConMn1-m-n, 0.3≤
M≤1, the metal mixed solution of the molar ratio set in 0≤n≤0.5, using constant-current flow gauge by mixed salt solution, network
Mixture ammonium hydroxide and precipitating reagent sodium hydroxide have been passed through in the reaction kettle of nitrogen with the importing of certain technological means to be reacted；
2) first bottom liquid in reaction kettle being heated up before reaction, reaction process controls constant temperature, while detecting pH value of reaction system with pH meter,
And rotating speed of agitator is controlled, while nitrogen is constantly passed through in reaction kettle；
3) granularity is detected using laser particle analyzer, after granularity reaches Spreading requirements, stops importing feed liquid and nitrogen, to system
Standby sediment is aged, washing, is centrifuged, and it is thin that micron-scale, large specific surface area, particle can be obtained through certain temperature drying screening
Pine, the spherical unformed lithium ion anode material precursor crystal grain of nanometer high-efficient, that processing performance is good of sintering.
According to the above technical scheme, nickel salt, manganese salt and the nickel salt in the step 1) are sulfate, chlorate or nitrate
One of or more than one.Mixed salt solution molar concentration in the step 1) is in 1.0-5.0mol/L.The step
It is rapid 1) in complexing agent ammonia concn be 5-13mol/L, liquid alkaline concentration be 3-13mol/L.Mixed metal salt in the step 1)
Solution, complexing agent ammonium hydroxide and precipitating reagent sodium hydroxide are added mode in reaction kettle and are grade ratio and add.
According to the above technical scheme, reaction temperature is 30 ~ 70 DEG C in the step 2.Reaction system pH in the step 2
Value is 10 ~ 12.Revolving speed is 200 ~ 600r/min in the step 2.
According to the above technical scheme, granularity is 3 ~ 15um in the step 3).Synthesis forerunner described in the step 3)
The size distribution of body is tested by micro- sem observation and Malvern 2000.
Compared with prior art, the beneficial effects obtained by the present invention are as follows being: through the invention coprecipitated determines preparation process can
To be effectively improved the micro-nano size and appearance structure of material property and particle；Different material is uniformly divided in the synthesis process
Dissipate, by different growth mechanisms carry out atomic level on combine, so that it may obtain short growth time, large specific surface area, particle it is loose,
It is sintered high-efficient, excellent electrical property nanometer spherical crystal particle, and technological operation is simple, yield in unit time is high.
Detailed description of the invention
Fig. 1 is the unformed presoma SEM of Ni0.33Co0.33Mn0.33 (OH) 2 photograph that the embodiment of the present invention 1 synthesizes 2um
Piece；
Fig. 2 is the unformed presoma SEM photograph of Ni0.6Co0.2Mn0.2 (OH) 2 that the embodiment of the present invention 2 synthesizes 3 ~ 4um.
Specific embodiment
Above-mentioned attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with the present invention
Embodiment be used to explain the present invention together, be not construed as limiting the invention.Below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described.Obviously, described embodiment is only
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
The present invention provides a kind of technical solution: a kind of unformed lithium ion anode material presoma and preparation method thereof,
Embodiment 1:
A kind of unformed lithium ion anode material presoma and preparation method thereof, comprising the following steps:
It 1) is that primary raw material is made into 2mol/L molar ratio column 1:1:1 nickel cobalt manganese metal salt solution by nickel salt, manganese salt and cobalt salt,
10mol/L sodium hydroxide, 8mol/L ammonium hydroxide are reaction raw materials, are pressed metal mixed solution and ammonium hydroxide and lye with constant-current flow gauge
Corresponding reaction molar ratio cocurrent is added in reactive tank；
2) first bottom liquid in reaction kettle heat up before reaction, 45 DEG C of constant temperature of reaction process control, while pH automatic control be set as 10.5 ~
11, and controlling rotating speed of agitator is 400r/min, entire synthesis process is reacted under inert nitrogen gas protection；
3) granularity is detected using laser particle analyzer, after granularity reaches Spreading requirements 2um, stops importing feed liquid and nitrogen,
It to the ageing of the sediment of preparation, washing, centrifugation, dries and is sieved through 100 DEG C, it is spherical to synthesize microscopic appearance, appearance
Uniformly without agglomerated particle.
Embodiment 2:
A kind of unformed lithium ion anode material presoma and preparation method thereof, comprising the following steps:
It 1) is that primary raw material is made into 1.5mol/L molar ratio column 6:2:2 nickel cobalt manganese metal salt solution by nickel salt, manganese salt and cobalt salt,
8mol/L sodium hydroxide, 8mol/L ammonium hydroxide are reaction raw materials, are pressed metal mixed solution and ammonium hydroxide and lye with constant-current flow gauge
Corresponding reaction molar ratio cocurrent is added in reactive tank；
2) first bottom liquid in reaction kettle heat up before reaction, 55 DEG C of constant temperature of reaction process control, while pH automatic control be set as 11.5 ~
12, and controlling rotating speed of agitator is 300r/min, entire synthesis process is reacted under inert nitrogen gas protection；
3) granularity is detected using laser particle analyzer, after granularity reaches Spreading requirements 3.5um, stops importing feed liquid and nitrogen
Gas is dried and is sieved through 120 DEG C to the ageing of the sediment of preparation, washing, centrifugation, and it is spherical to synthesize microscopic appearance, outside
It sees uniformly without agglomerated particle.
Based on above-mentioned, it is an advantage of the current invention that it is of the invention, it is that primary raw material is made into centainly by nickel salt, manganese salt and cobalt salt
Concentration molar ratio is the metal mixed solution of 5:3:2 or other molar ratios, using constant-current flow gauge by mixed salt solution, network
Mixture ammonium hydroxide and precipitating reagent sodium hydroxide have been passed through in the reaction kettle of nitrogen with the importing of certain technological means to be reacted；Before reaction
First bottom liquid in reaction kettle is heated up, reaction process controls constant temperature, while detecting pH value of reaction system with pH meter, and control agitating paddle
Revolving speed, while nitrogen is constantly passed through in reaction kettle；Granularity is detected using laser particle analyzer, granularity reaches Spreading requirements
Afterwards, stop importing feed liquid and nitrogen, sediment ageing, washing, the centrifugation to preparation can be obtained through certain temperature drying screening
The spherical unformed lithium ion of the nanometer that micron-scale, large specific surface area, particle are loose, sintering is high-efficient, processing performance is good is just
Pole material precursor crystal grain, and technological operation is simple, yield in unit time is high.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to before
Stating embodiment, invention is explained in detail, for those skilled in the art, still can be to aforementioned each
Technical solution documented by embodiment is modified or equivalent replacement of some of the technical features.It is all in the present invention
Spirit and principle within, any modification, equivalent replacement, improvement and so on, should be included in protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of unformed lithium ion anode material presoma, comprising the following steps:
It 1) is that be made into concentration be molar ratio 5:3:2 or Ni to primary raw material by nickel salt, manganese salt and cobalt saltmConMn1-m-n, 0.3≤m≤1,
The molar ratio metal mixed solution set in 0≤n≤0.5, using constant-current flow gauge by mixed salt solution, complexing agent ammonium hydroxide
It has been passed through in the reaction kettle of nitrogen and has been reacted with the importing of precipitating reagent sodium hydroxide；
2) first bottom liquid in reaction kettle being heated up before reaction, reaction process controls constant temperature, while detecting pH value of reaction system with pH meter,
And rotating speed of agitator is controlled, while nitrogen is constantly passed through in reaction kettle；
3) granularity is detected using laser particle analyzer, after granularity reaches Spreading requirements, stops importing feed liquid and nitrogen, to system
Standby sediment ageing, washing, centrifugation, drying screening can be obtained that micron-scale, large specific surface area, particle be loose, sintering
The spherical unformed lithium ion anode material precursor crystal grain of nanometer high-efficient, that processing performance is good.
2. the preparation method of unformed lithium ion anode material presoma according to claim 1, it is characterised in that: described
Nickel salt, manganese salt and nickel salt in step 1) be one of sulfate, chlorate or nitrate or more than one.
3. the preparation method of unformed lithium ion anode material presoma according to claim 1, it is characterised in that: described
Mixed salt solution molar concentration in step 1) is in 1.0-5.0mol/L.
4. the preparation method of unformed lithium ion anode material presoma according to claim 1, it is characterised in that: described
Complexing agent ammonia concn in step 1) is 5-13mol/L, and liquid alkaline concentration is 3-13mol/L.
5. the preparation method of unformed lithium ion anode material presoma according to claim 1, it is characterised in that: described
Mixed salt solution, complexing agent ammonium hydroxide and precipitating reagent sodium hydroxide are added mode in reaction kettle and are grade ratio and add in step 1).
6. the preparation method of unformed lithium ion anode material presoma according to claim 1, it is characterised in that: described
Reaction temperature is 30 ~ 70 DEG C in step 2.
7. the preparation method of unformed lithium ion anode material presoma according to claim 1, it is characterised in that: described
PH value of reaction system is 10 ~ 12 in step 2.
8. the preparation method of unformed lithium ion anode material presoma according to claim 1, it is characterised in that: described
Revolving speed is 200 ~ 600r/min in step 2.
9. the preparation method of unformed lithium ion anode material presoma according to claim 1, it is characterised in that: described
Granularity is 3 ~ 15um in step 3).
10. the preparation method of unformed lithium ion anode material presoma according to claim 1, it is characterised in that: institute
The size distribution for stating synthesis presoma described in step 3) is tested by micro- sem observation and Malvern 2000.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761288A (en) * | 2019-04-09 | 2019-05-17 | 金驰能源材料有限公司 | A kind of preparation method of spherical nickel cobalt manganese persursor material |
| CN112607788A (en) * | 2020-12-14 | 2021-04-06 | 荆门市格林美新材料有限公司 | Method for preparing nickel-cobalt-manganese ternary precursor with narrow particle size distribution |
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| CN106920960A (en) * | 2015-12-28 | 2017-07-04 | 北京有色金属研究总院 | The nickel-cobalt-manganese ternary complex hydroxide and regulation and control construction method of dynamic microstructure |
| CN107342417A (en) * | 2016-12-28 | 2017-11-10 | 杉杉能源（宁夏）有限公司 | A kind of high ni-type precursor of nickel-cobalt-lithium-manganese-oxide with specific morphology and preparation method thereof |
| CN107915263A (en) * | 2017-08-31 | 2018-04-17 | 广东佳纳能源科技有限公司 | A kind of preparation method of small particle ternary anode material precursor |
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2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106920960A (en) * | 2015-12-28 | 2017-07-04 | 北京有色金属研究总院 | The nickel-cobalt-manganese ternary complex hydroxide and regulation and control construction method of dynamic microstructure |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761288A (en) * | 2019-04-09 | 2019-05-17 | 金驰能源材料有限公司 | A kind of preparation method of spherical nickel cobalt manganese persursor material |
| CN112607788A (en) * | 2020-12-14 | 2021-04-06 | 荆门市格林美新材料有限公司 | Method for preparing nickel-cobalt-manganese ternary precursor with narrow particle size distribution |
| CN112607788B (en) * | 2020-12-14 | 2023-11-24 | 荆门市格林美新材料有限公司 | Method for preparing nickel-cobalt-manganese ternary precursor with narrow particle size distribution |
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