CN105680039A - Method for preparing lamellar Co, Ni, Mn and Li battery anode material - Google Patents
Method for preparing lamellar Co, Ni, Mn and Li battery anode material Download PDFInfo
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- CN105680039A CN105680039A CN201610253178.6A CN201610253178A CN105680039A CN 105680039 A CN105680039 A CN 105680039A CN 201610253178 A CN201610253178 A CN 201610253178A CN 105680039 A CN105680039 A CN 105680039A
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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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- 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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- 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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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a LiMn1-x-yNixCoyO2 anode material, in particular to a method for preparing a lamellar Co, Ni, Mn and Li battery anode material. The method comprises the following steps: solid Mn (NO3)2, CoCO3 and Ni (NO3)2.6H2O are mixed and ball-milled; the mixed particles and solid Li2CO3 are mixed, put into a rotary roller inner cavity, thrown out and put into the roller inner cavity again, and a uniformly mixed mixture is obtained; a dispersing agent is added for mechanical activation, then the mixture is dried, and a precursor is obtained; the precursor is presintered in a resistance furnace; grinding is performed after presintering, and then ground materials are put in a rotary roaster; the materials in the roaster move along with rotation of a roaster body, and the Co, Ni, Mn and Li battery anode material is obtained finally. According to the method, first of all, a ball mill is used for ball-milling ternary materials to enable the diameters of the materials to be uniform; then centrifugal force and a fan are adopted, so that the random circulatory motion is achieved for the mixed materials, and objectives of uniformity and no dead angles of material mixing are achieved; then the Co, Ni, Mn and Li battery anode material with good electrochemical performance is obtained by presintering and roasting.
Description
Technical field
The present invention relates to nickel cobalt manganese anode material of lithium battery, specifically the preparation method of stratiform cobalt nickel manganese lithium anode material.
Background technology
In recent years, novel lithium ion composite positive pole quickly grows, especially nickel cobalt manganese lithium anode material, and it becomes the focus of domestic and international experts and scholars research. With business-like LiCoO2Comparing, nickel cobalt manganese lithium anode material has advantage with low cost; With LiNiO2Comparing, nickel cobalt manganese lithium anode material is more easily-synthesized, and cycle performance is relative with heat stability better; Relative spinelle LiMn2O4, nickel cobalt manganese lithium anode material structure in charge and discharge process is more stable, Jahn-Teller effect will not occur, and Mn is ion stabilized, and the dissolving in the electrolytic solution of Mn ion will not occur; With LiFePO4Comparing, nickel cobalt manganese lithium anode material tap density is big, and potential plateau is high.
At present, the preparation method of nickel cobalt manganese lithium anode material includes high temperature solid-state method, coprecipitation, sol-gel process, spray pyrolysis, hydrothermal synthesis method and combustion method etc., but adopt and more remain coprecipitation, the method complicated operation, repeatability are poor and need strict Control release condition, limit industrialized production and the practical application of nickel cobalt manganese lithium anode material to a certain extent.
Summary of the invention
For above-mentioned technical problem, the preparation method that the present invention provides a kind of stratiform cobalt nickel manganese anode material of lithium battery obtaining good electric chemical property, it comprises the following steps:
The technical solution used in the present invention is: the preparation method of stratiform cobalt nickel manganese anode material of lithium battery, and it comprises the following steps:
(1) stoichiometrically by solid-state Mn (NO3)2、CoCO3With Ni (NO3)2·6H2O mixing ball milling, obtain hybrid particles;
(2) again by above-mentioned hybrid particles and solid-state Li2CO3Mixing puts in the drum cavity rotated, and mixture is thrown away from inner chamber by the cylinder of rotation under centrifugal action; The mixture thrown away puts in described drum cavity again; So circulation, mixture being uniformly mixed;
(3) in the mixture of above-mentioned mix homogeneously, add dispersant and carry out mechanical activation;
(4) then the slurry after activation is placed in drying baker inner drying, obtains presoma;
(5) presoma is carried out in resistance furnace pre-burning;
(6) it is ground after pre-burning, then the material after grinding is placed in swinging roaster;
(7) in roaster, material moves along with the rotation of body of heater, finally obtains nickel-cobalt lithium manganate cathode material.
As preferably, described mixture puts in the vertical rotary cylinder inner chamber of high speed rotating from the top down, and the mixture in inner chamber is thrown away from the through hole of downside sidewall by the cylinder of high speed rotating under centrifugal action; Being arranged at the fan on the downside of cylinder and the mixture thrown away is blowed cover on the upside of cylinder from bottom to top, mixture puts in drum cavity after clashing into cover again.
As preferably, adopting the rotating speed of 350 400r/min to carry out during ball milling, Ball-milling Time 45 60min.
As preferably, mechanical activation adopts planetary ball mill, and planetary ball mill adopts the rotating speed of 180--220r/min to carry out mechanical activation, and the time of mechanical activation is 3.5 4.5h.
As preferably, ball material mass ratio during mechanical activation is (8 9): 1.
As preferably, time dry, drying baker keeps the temperature of 60 80 DEG C.
As preferably, calcined temperature is 450--550 DEG C, and the time is 4 5h.
As preferably, the temperature of roasting is 800--900 DEG C, and the time is 9 10h.
As can be known from the above technical solutions, ternary material is carried out ball milling first with ball mill by the present invention so that material particle size is uniform, and recycling centrifugal force and fan make the material of mixing realize random shuttling movement, thus reaching batch mixing uniformly without the purpose at dead angle; And mixture and cover clash into, can make to produce between mixture the adhesive effect of appropriateness, thus lithium ion is uniformly embedded in presoma when ensureing follow-up sintering; Then mixture is carried out mechanical activation, make granular precursor be evenly distributed further, uniform particle sizes; The cobalt nickel lithium manganate cathode material of excellent electrochemical performance is obtained again through pre-burning and roasting.
Detailed description of the invention
The present invention is described more detail below, and illustrative examples and explanation in this present invention are used for explaining the present invention, but not as a limitation of the invention.
The preparation method of stratiform cobalt nickel manganese anode material of lithium battery, it comprises the following steps:
(1) stoichiometrically by solid-state Mn (NO3)2、CoCO3With Ni (NO3)2·6H2O mixing ball milling, during ball milling, ball mill adopts the rotating speed of 350 400r/min to carry out ball milling, Ball-milling Time 45 60min so that ternary material tentatively mixes, and obtains hybrid particles.
(2) again by above-mentioned hybrid particles and solid-state Li2CO3Mixing puts in the drum cavity rotated, and is specifically put into by mixture in the vertical rotary cylinder inner chamber of high speed rotating from the top down, adopts vertical rotary cylinder to be conducive to charging and discharging; Mixture is thrown away from inner chamber by the cylinder rotated under centrifugal action, and in implementation process, the circumferentially arranged several through holes of sidewall on the downside of cylinder, so that the mixture in inner chamber is thrown away from the through hole of downside sidewall by the cylinder of high speed rotating under centrifugal action.
(3) mixture thrown away puts in described drum cavity again, and as preferably, side arranges supply air system under the rollers, such as fan; At cylinder, cover is set; After the mixture thrown away is blowed the cover on the upside of cylinder by fan from bottom to top, mixture puts in drum cavity after clashing into cover again, so circulates, thus reaching batch mixing without dead angle, the mixture being uniformly mixed.
(4) adding dispersant in the mixture of above-mentioned mix homogeneously and carry out mechanical activation, dispersant can adopt dehydrated alcohol etc., is conducive to dispersion, ball milling;Mechanical activation adopts planetary ball mill, and such activation effect is better, and such activation effect is better; Planetary ball mill adopts the rotating speed of 180--220r/min to enter, and the time of activation is 3.5 4.5h. So can improve the interracial contact between material, promote that in subsequent synthetic run, nucleus generates the speed with development growth, plays the effect of grain refinement.
(5) then the slurry after activation is placed in drying baker inner drying, obtains presoma; Time dry, drying baker keeps the temperature of 60 80 DEG C.
(6) being placed in resistance furnace by presoma and carry out pre-burning under compression air atmosphere, calcined temperature is 450--550 DEG C, and the time is 4 5h; Burn-in process happens is that initial chemical course of reaction, and lithium carbonate decomposes, and lithium ion enters in presoma, and water and carbon dioxide are released in reaction. Compression air is adopted to leak water and carbon dioxide by band.
(7) being ground after pre-burning, then the material after grinding is placed in roasting in swinging roaster, the temperature of roasting is 800--900 DEG C, and the time is 9 10h; In roaster, material moves along with the rotation of body of heater, makes material sufficient movement in burner hearth, it is ensured that material is heated evenly, thus the cobalt nickel lithium manganate cathode material of excellent.
Embodiment 1
Stoichiometrically by solid-state Mn (NO3)2、CoCO3、Ni(NO3)2·6H2O mixes and adopts the rotating speed of 350r/min to carry out ball milling, Ball-milling Time 45min; Again by above-mentioned hybrid particles and solid-state Li2CO3Mixture puts in the vertical rotary cylinder inner chamber of high speed rotating from the top down, and the mixture in inner chamber is thrown away from the through hole of downside sidewall by the cylinder of high speed rotating under centrifugal action; After the mixture thrown away is blowed the cover on the upside of cylinder by fan from bottom to top, mixture puts in drum cavity after clashing into cover again, so circulates; After about 10 minutes, mixture is placed in planetary ball mill and adds appropriate dehydrated alcohol, then the rotating speed ball milling 4.5h adopting ball material mass ratio to be 8:1,180/min, then the slurry after ball milling is placed in the drying baker inner drying of 60 DEG C, obtains presoma; Being placed in resistance furnace by presoma and carry out pre-burning under compression air atmosphere, calcined temperature is 450 DEG C, and the time is 5h; Being ground after pre-burning, then be placed in swinging roaster and rotate roasting by the material after grinding, the temperature of roasting is 800 DEG C, and the time is 10h, it is thus achieved that nickel-cobalt lithium manganate cathode material. This material properties test is obtained: at 40 DEG C, the voltage of 2 4.8V, when the discharge and recharge of 60mA/g electric current, the initial capacity of material is 321.43mAh/g, cycle performance is excellent, front 30 loop attenuation rates are only 0.15%, and follow-up 150mA/g is charged, through 30 circulation volumes almost without decay.
Embodiment 2
Stoichiometrically by solid-state Mn (NO3)2、CoCO3、Ni(NO3)2·6H2O mixes and adopts the rotating speed of 380r/min to carry out ball milling, Ball-milling Time 60min; Again by above-mentioned hybrid particles and solid-state Li2CO3Mixture puts in the vertical rotary cylinder inner chamber of high speed rotating from the top down, and the mixture in inner chamber is thrown away from the through hole of downside sidewall by the cylinder of high speed rotating under centrifugal action; After the mixture thrown away is blowed the cover on the upside of cylinder by fan from bottom to top, mixture puts in drum cavity after clashing into cover again, so circulates; After about 12 minutes, mixture is placed in planetary ball mill and adds appropriate dehydrated alcohol, then the rotating speed ball milling 4h adopting ball material mass ratio to be 9:1,200/min, then the slurry after ball milling is placed in the drying baker inner drying of 70 DEG C, obtains presoma;Being placed in resistance furnace by presoma and carry out pre-burning under compression air atmosphere, calcined temperature is 500 DEG C, and the time is 4.5h; Being ground after pre-burning, then be placed in swinging roaster and rotate roasting by the material after grinding, the temperature of roasting is 850 DEG C, and the time is 9.5h, it is thus achieved that nickel-cobalt lithium manganate cathode material. This material properties test is obtained: at 40 DEG C, the voltage of 2 4.8V, when the discharge and recharge of 60mA/g electric current, the initial capacity of material is 337.42mAh/g, cycle performance is excellent, front 30 loop attenuation rates are only 0.11%, and follow-up 150mA/g is charged, through 30 circulation volumes almost without decay.
Embodiment 3
Stoichiometrically by solid-state Mn (NO3)2、CoCO3、Ni(NO3)2·6H2O mixes and adopts the rotating speed of 400r/min to carry out ball milling, Ball-milling Time 50min; Again by above-mentioned hybrid particles and solid-state Li2CO3Mixture puts in the vertical rotary cylinder inner chamber of high speed rotating from the top down, and the mixture in inner chamber is thrown away from the through hole of downside sidewall by the cylinder of high speed rotating under centrifugal action; After the mixture thrown away is blowed the cover on the upside of cylinder by fan from bottom to top, mixture puts in drum cavity after clashing into cover again, so circulates; After about 15 minutes, mixture is placed in planetary ball mill and adds appropriate dehydrated alcohol, then the rotating speed ball milling 3.5h adopting ball material mass ratio to be 8.5:1,220/min, then the slurry after ball milling is placed in the drying baker inner drying of 80 DEG C, obtains presoma; Being placed in resistance furnace by presoma and carry out pre-burning under compression air atmosphere, calcined temperature is 550 DEG C, and the time is 4h; Being ground after pre-burning, then be placed in swinging roaster and rotate roasting by the material after grinding, the temperature of roasting is 900 DEG C, and the time is 9h, it is thus achieved that nickel-cobalt lithium manganate cathode material. This material properties test is obtained: at 40 DEG C, the voltage of 2 4.8V, when the discharge and recharge of 60mA/g electric current, the initial capacity of material is 319.95mAh/g, cycle performance is excellent, front 30 loop attenuation rates are only 0.13%, and follow-up 150mA/g is charged, through 30 circulation volumes almost without decay.
The technical scheme above embodiment of the present invention provided is described in detail, principle and the embodiment of the embodiment of the present invention are set forth by specific case used herein, and the explanation of above example is only applicable to help to understand the principle of the embodiment of the present invention; Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, all will change in detailed description of the invention and range of application, in sum, this specification content should not be construed as limitation of the present invention.
Claims (8)
1. the preparation method of stratiform cobalt nickel manganese anode material of lithium battery, it comprises the following steps:
(1) stoichiometrically by solid-state Mn (NO3)2、CoCO3With Ni (NO3)2·6H2O mixing ball milling, obtain hybrid particles;
(2) again by above-mentioned hybrid particles and solid-state Li2CO3Mixing puts in the drum cavity rotated, and mixture is thrown away from inner chamber by the cylinder of rotation under centrifugal action; The mixture thrown away puts in described drum cavity again; So circulation, mixture being uniformly mixed; In the mixture of above-mentioned mix homogeneously, add dispersant carry out mechanical activation;
(4) then the slurry after activation is placed in drying baker inner drying, obtains presoma;
(5) presoma is carried out in resistance furnace pre-burning;
(6) it is ground after pre-burning, then the material after grinding is placed in swinging roaster;
(7) in roaster, material moves along with the rotation of body of heater, finally obtains cobalt nickel lithium manganate cathode material.
2. preparation method according to claim 1, it is characterised in that: described mixture puts in the vertical rotary cylinder inner chamber of high speed rotating from the top down, and the mixture in inner chamber is thrown away from the through hole of downside sidewall by the cylinder of high speed rotating under centrifugal action; Being arranged at the fan on the downside of cylinder and the mixture thrown away is blowed cover on the upside of cylinder from bottom to top, mixture puts in drum cavity after clashing into cover again.
3. preparation method according to claim 1, it is characterised in that: adopt the rotating speed of 350 400r/min to carry out during ball milling, Ball-milling Time 45 60min.
4. preparation method according to claim 1, it is characterised in that: mechanical activation adopts planetary ball mill, and planetary ball mill adopts the rotating speed of 180--220r/min to carry out mechanical activation, and the time of mechanical activation is 3.5 4.5h.
5. preparation method according to claim 1, it is characterised in that: ball material mass ratio during mechanical activation is (8 9): 1.
6. preparation method according to claim 1, it is characterised in that: time dry, drying baker keeps the temperature of 60 80 DEG C.
7. preparation method according to claim 1, it is characterised in that: calcined temperature is 450--550 DEG C, and the time is 4 5h.
8. preparation method according to claim 7, it is characterised in that: the temperature of roasting is 800--900 DEG C, and the time is 9 10h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610253178.6A CN105680039A (en) | 2016-04-22 | 2016-04-22 | Method for preparing lamellar Co, Ni, Mn and Li battery anode material |
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| CN201610253178.6A CN105680039A (en) | 2016-04-22 | 2016-04-22 | Method for preparing lamellar Co, Ni, Mn and Li battery anode material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106299273A (en) * | 2016-08-22 | 2017-01-04 | 浙江金开来新能源科技有限公司 | A kind of preparation method of titanium cladding nickel cobalt manganese lithium ion power battery cathode material |
| CN109742389A (en) * | 2018-12-10 | 2019-05-10 | 北方奥钛纳米技术有限公司 | Positive electrode and preparation method thereof, positive plate, battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106299273A (en) * | 2016-08-22 | 2017-01-04 | 浙江金开来新能源科技有限公司 | A kind of preparation method of titanium cladding nickel cobalt manganese lithium ion power battery cathode material |
| CN109742389A (en) * | 2018-12-10 | 2019-05-10 | 北方奥钛纳米技术有限公司 | Positive electrode and preparation method thereof, positive plate, battery |
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Application publication date: 20160615 |