CN103972495A - Preparation method of lithium ion battery positive pole material lithium nickelate manganate - Google Patents
Preparation method of lithium ion battery positive pole material lithium nickelate manganate Download PDFInfo
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- CN103972495A CN103972495A CN201410208751.2A CN201410208751A CN103972495A CN 103972495 A CN103972495 A CN 103972495A CN 201410208751 A CN201410208751 A CN 201410208751A CN 103972495 A CN103972495 A CN 103972495A
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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
- 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
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- 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
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Abstract
The invention relates to a preparation method of a lithium ion battery positive pole material lithium nickelate manganate. The invention belongs to the technical field of lithium ion batteries. The preparation method comprises the following steps: (1) preparation of metastable-state nickel manganese or nickel manganese oxide nanocrystal powder by mechanical alloying: adding a ball milling medium into Ni and Mn simple substances or oxides according to the stoichiometric proportion, and carrying out mechanical ball milling at the rotation speed of 300-500 r/min according to the grinding medium-to-material ratio of (10-50):1; (2) preparation of nickel manganese oxide presintered precursor: keeping the metastable-state nickel manganese or nickel manganese oxide nanocrystal powder prepared in the step (1) in an air or oxygen atmosphere at the constant temperature of 100-300 DEG C for 3-5 hours; and (3) preparation of lithium ion battery positive pole material lithium nickelate manganate by calcining: mixing a lithium source (2-5% excessive) and the nickel manganese oxide presintered precursor, calcining at 700-900 DEG C for 5-10 hours, cooling, grinding and screening. The method has the advantages of high yield, fewer foreign phases, high specific capacity, favorable loop stability, low energy consumption, low cost, simplified technological conditions, environment friendliness and the like.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to a kind of preparation method of lithium ion battery anode material nickel LiMn2O4.
Background technology
At present, the nickel LiMn2O4 (LiNi of crystallographic system spinel-type
0.5mn
1.5o
4) material is high owing to having voltage platform, energy density is large, Heat stability is good, and raw material resources are abundant, cheap, advantages of environment protection and become a kind of lithium-ion-power cell material that has potentiality.
In the prior art, synthetic nickel LiMn2O4 (LiNi
0.5mn
1.5o
4) method mainly contain solid phase method, coprecipitation, sol-gal process, hydro thermal method, ullrasonic spraying dry heat solution etc.
Due to coprecipitation, sol-gal process complex procedures, production cost is high, easily produces waste water and gas; Hydro thermal method, ullrasonic spraying dry heat solution are high to equipment requirement, complex operation, and technology is also immature; So can be applicable at present the method for suitability for industrialized production is mainly also solid phase method.
Solid phase method is generally a step mixed-sintering method, and the compound that utilizes lithium, nickel, manganese is prepared into after fully mixing high-temperature calcination.Its technique is simple, manufacturing equipment cost is low.Weak point is the oxide material that easily generates inhomogeneous composition, causes material consistency slightly poor, and gram volume is not high; Lithium is close with nickle atom radius, causes the dislocation mixing of Li and Ni in crystal structure, causes the active conversion ratio of material more and more lower, and cyclical stability is bad; And because material granule distribution is wider, there is the technical problems such as properties for follow is bad.
Summary of the invention
The present invention provides a kind of preparation method of lithium ion battery anode material nickel LiMn2O4 for solving the technical problem existing in known technology.
The object of this invention is to provide one, to have productive rate high, and dephasign is few, and specific capacity is high, good cycling stability, and energy consumption is low, and process conditions are simplified, can reduce production costs, the preparation method of the lithium ion battery anode material nickel LiMn2O4 of the features such as environmental friendliness.
The present invention creatively adopts mechanical alloying method to carry out the preparation of lithium ion battery anode material nickel LiMn2O4.Mechanical Alloying be mainly by metal or alloy powder in high energy ball mill by impacting intensely for a long time, collide between powder particle and abrading-ball, make powder particle repeatedly produce cold welding, fracture, cause the diffusion of powder particle Atom, become the method for metastable state ultrafine particle, mechanical activation generates the method for nanocrystalline particle.
The present invention is in conjunction with the advantage of solid phase method and liquid-phase precipitation method, take two step synthetic methods, first adopt mechanical alloying method activate, calcine the Ni, Mn oxide that obtains component homogeneous in air or oxygen atmosphere through mechanical ball milling by nickel, manganese simple substance or its oxide, after add Li source compound again high-temperature calcination make nickel manganate cathode material for lithium.
The technical scheme that the preparation method of lithium ion battery anode material nickel LiMn2O4 of the present invention takes is:
A preparation method for lithium ion battery anode material nickel LiMn2O4, is characterized in that: adopt mechanical alloying method to prepare lithium ion battery anode material nickel LiMn2O4, comprise following processing step:
(1) metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying
By stoichiometric proportion Ni, Mn simple substance or oxide, add ball-milling medium, be under 300-500r/min, the ratio of grinding media to material condition that is 10-50:1 at rotating speed, mechanical ball milling 3-100h, mechanical alloying method makes metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder;
(2) prepare Ni, Mn oxide pre-burning presoma
Metastable state nickel manganese prepared by step (1) or Ni, Mn oxide nanocrystalline powder, be placed in constant temperature under 100-300 DEG C of condition of air or oxygen atmosphere and keep 3-5h, obtains Ni, Mn oxide pre-burning presoma;
Lithium ion battery anode material nickel LiMn2O4 is prepared in calcining
The Li source compound of the excessive 2-5% of stoichiometry is mixed with Ni, Mn oxide pre-burning presoma, in 700-900 DEG C of calcining 5-10h, cool to the furnace and grind the nickel LiMn2O4 product that sieves to obtain after room temperature.
The preparation method of lithium ion battery anode material nickel LiMn2O4 of the present invention can also adopt following technical scheme:
The preparation method of described lithium ion battery anode material nickel LiMn2O4, is characterized in: when metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying, the purity of simple substance Ni is greater than 99.5%, and the purity of simple substance Mn is greater than 99.8%.
The preparation method of described lithium ion battery anode material nickel LiMn2O4, is characterized in: when metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying, the oxide of nickel is NiO or Ni
2o
3, the oxide of manganese is MnO, Mn
2o
3, Mn
3o
4, MnO
2in any one and several.
The preparation method of described lithium ion battery anode material nickel LiMn2O4, is characterized in: when metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying, ball-milling medium is benzinum or absolute ethyl alcohol.
The preparation method of described lithium ion battery anode material nickel LiMn2O4, is characterized in: when lithium ion battery anode material nickel LiMn2O4 is prepared in calcining, Li source compound is Li
2cO
3, LiOHH
2o, LiOH, Li
2o or CH
3cOOLi2H
2the mixture of one or more in O.
The preparation method of described lithium ion battery anode material nickel LiMn2O4, is characterized in: while preparing lithium ion battery anode material nickel LiMn2O4, cool to the furnace to grind to sieve after room temperature and make nickel LiMn2O4 product.
Advantage and good effect that the present invention has are:
The preparation method of lithium ion battery anode material nickel LiMn2O4 is owing to having adopted the brand-new technical scheme of the present invention, and compared with prior art, the present invention has following characteristics:
1. raw material of the present invention is simple substance or oxide, is again solid phase reaction, therefore expect that from former product almost produces without the three wastes, productive rate is high, environmental friendliness, and production cost is low.
2. the solid phase two step synthetic methods in the present invention are compared with a step mixed-sintering method: avoided the mixing of lithium nickel, reduced the generation of dephasign, improved the consistency of product, increased specific capacity and the cyclical stability of material; Another particle diameter distributes and is tending towards evenly, more easily processing.
3. the present invention is owing to having utilized the condition of Mechanical Alloying to prepare metastable state nanocrystalline powder, and active high, follow-up calcining heat is on the low side, has reduced energy consumption.
Brief description of the drawings
Fig. 1 is LiNi prepared by the present invention
0.5mn
1.5o
4the SEM figure of material;
Fig. 2 is LiNi prepared by the present invention
0.5mn
1.5o
4the XRD figure of material;
Fig. 3 is LiNi prepared by the present invention
0.5mn
1.5o
4the first charge-discharge curve of material;
Fig. 4 is LiNi prepared by the present invention
0.5mn
1.5o
4front 100 1C discharge capacity curves of material.
Embodiment
For further understanding summary of the invention of the present invention, Characteristic, hereby exemplify following examples, and coordinate accompanying drawing to be described in detail as follows:
Consult accompanying drawing 1, Fig. 2, Fig. 3 and Fig. 4.
Embodiment 1
A preparation method for lithium ion battery anode material nickel LiMn2O4, the present embodiment obtains 18.30g (0.10mol) LiNi
0.5mn
1.5o
4positive electrode, specifically comprises following processing step:
(1) metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying
Take simple substance Ni2.95g (0.05mol), simple substance Mn8.25g (0.15mol) mixes, and adds 10mL benzinum, is that under 500r/min, the ratio of grinding media to material condition that is 40:1, mechanical ball milling 48h, obtains metastable state nickel manganese nanocrystalline powder at rotating speed.
(2) prepare Ni, Mn oxide pre-burning presoma
Nickel manganese nanocrystalline powder is placed in to 300 DEG C of constant temperature of oxygen atmosphere and keeps 5h, obtain Ni, Mn oxide presoma.
(3) lithium ion battery anode material nickel LiMn2O4 is prepared in calcining
By 4.41g (0.105mol) LiOHH
2o fully mixes with Ni, Mn oxide presoma, in 750 DEG C of high-temperature calcination 10h, cools to the furnace and grinds the LiNi that sieves to obtain after room temperature
0.5mn
1.5o
4product.
Embodiment 2
A preparation method for lithium ion battery anode material nickel LiMn2O4, the present embodiment obtains 36.60g (0.20mol) LiNi
0.5mn
1.5o
4positive electrode, specifically comprises following processing step:
(1) metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying
Take NiO7.50g (0.10mol), simple substance Mn16.50g (0.30mol) mixes, and adds 25mL benzinum, is that under 450r/min, the ratio of grinding media to material condition that is 20:1, mechanical ball milling 48h, obtains metastable state nickel manganese nanocrystalline powder at rotating speed.
(2) prepare Ni, Mn oxide pre-burning presoma
Nickel manganese nanocrystalline powder is placed in to 350 DEG C of constant temperature of oxygen atmosphere and keeps 3h, obtain Ni, Mn oxide presoma.
(3) lithium ion battery anode material nickel LiMn2O4 is prepared in calcining
By 7.70g (0.104mol) Li
2cO
3fully mix with Ni, Mn oxide presoma, in 800 DEG C of high-temperature calcination 8h, cool to the furnace and grind the LiNi that sieves to obtain after room temperature
0.5mn
1.5o
4product.
Embodiment 3
A preparation method for lithium ion battery anode material nickel LiMn2O4, the present embodiment obtains 18.30g (0.10mol) LiNi
0.5mn
1.5o
4positive electrode, specifically comprises following processing step:
(1) metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying
Take simple substance Ni2.95g (0.05mol), Mn
3o
411.44g (0.05mol) mixes, and adds 15mL absolute ethyl alcohol, is that under 450r/min, the ratio of grinding media to material condition that is 40:1, mechanical ball milling 24h, obtains metastable state nickel manganese nanocrystalline powder at rotating speed.
(2) prepare Ni, Mn oxide pre-burning presoma
Nickel manganese nanocrystalline powder is placed in to 300 DEG C of constant temperature of oxygen atmosphere and keeps 4h, obtain Ni, Mn oxide presoma.
(3) lithium ion battery anode material nickel LiMn2O4 is prepared in calcining
By 3.85g (0.052mol) Li
2cO
3fully mix with Ni, Mn oxide presoma, in 800 DEG C of high-temperature calcination 6h, cool to the furnace and grind the LiNi that sieves to obtain after room temperature
0.5mn
1.5o
4product.
Embodiment 4
A preparation method for lithium ion battery anode material nickel LiMn2O4, the present embodiment obtains 36.60g (0.20mol) LiNi
0.5mn
1.5o
4positive electrode, specifically comprises following processing step:
(1) metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying
Take NiO7.50g (0.10mol), Mn
3o
422.88g (0.10mol) mixes, and adds 30mL absolute ethyl alcohol, is that under 450r/min, the ratio of grinding media to material condition that is 20:1, mechanical ball milling 60h, obtains metastable state nickel manganese nanocrystalline powder at rotating speed.
(2) prepare Ni, Mn oxide pre-burning presoma
Nickel manganese nanocrystalline powder is placed in to 350 DEG C of constant temperature of oxygen atmosphere and keeps 4h, obtain Ni, Mn oxide presoma.
(3) lithium ion battery anode material nickel LiMn2O4 is prepared in calcining
By 7.62g (0.103mol) Li
2cO
3fully mix with Ni, Mn oxide presoma, in 800 DEG C of high-temperature calcination 8h, cool to the furnace and grind the LiNi that sieves to obtain after room temperature
0.5mn
1.5o
4product.
Product yield described in the present embodiment has is high, and dephasign is few, and specific capacity is high, good cycling stability, and energy consumption is low, and process conditions are simplified, can reduce production costs, the good effects such as environmental friendliness.
Claims (6)
1. a preparation method for lithium ion battery anode material nickel LiMn2O4, is characterized in that: adopt mechanical alloying method to prepare lithium ion battery anode material nickel LiMn2O4, comprise following processing step:
(1) metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying
Adding Ni, Mn simple substance or oxide by stoichiometric proportion, add ball-milling medium, is under 300-500r/min, the ratio of grinding media to material condition that is 10-50:1 at rotating speed, mechanical ball milling 3-100h, and mechanical alloying method makes metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder;
(2) prepare Ni, Mn oxide pre-burning presoma
Metastable state nickel manganese prepared by step (1) or Ni, Mn oxide nanocrystalline powder, be placed in constant temperature under 100-300 DEG C of condition of air or oxygen atmosphere and keep 3-5h, obtains Ni, Mn oxide pre-burning presoma;
(3) lithium ion battery anode material nickel LiMn2O4 is prepared in calcining
The Li source compound of the excessive 2-5% of stoichiometry is mixed with Ni, Mn oxide pre-burning presoma, in 700-900 DEG C of calcining 5-10h, cool to the furnace and grind the nickel LiMn2O4 product that sieves to obtain after room temperature.
2. the preparation method of lithium ion battery anode material nickel LiMn2O4 according to claim 1, it is characterized in that: when metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying, the purity of simple substance Ni is greater than 99.5%, and the purity of simple substance Mn is greater than 99.8%.
3. the preparation method of lithium ion battery anode material nickel LiMn2O4 according to claim 1, is characterized in that: when metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying, the oxide of nickel is NiO or Ni
2o
3, the oxide of manganese is MnO, Mn
2o
3, Mn
3o
4, MnO
2in any one and several.
4. according to the preparation method of the lithium ion battery anode material nickel LiMn2O4 described in claim 1,2 or 3, it is characterized in that: when metastable state nickel manganese or Ni, Mn oxide nanocrystalline powder are prepared in mechanical alloying, ball-milling medium is benzinum or absolute ethyl alcohol.
5. according to the preparation method of the lithium ion battery anode material nickel LiMn2O4 described in claim 1,2 or 3, it is characterized in that: when lithium ion battery anode material nickel LiMn2O4 is prepared in calcining, Li source compound is Li
2cO
3, LiOHH
2o, LiOH, Li
2o or CH
3cOOLi2H
2the mixture of one or more in O.
6. the preparation method of lithium ion battery anode material nickel LiMn2O4 according to claim 1, is characterized in that: while preparing lithium ion battery anode material nickel LiMn2O4, cool to the furnace to grind to sieve after room temperature and make nickel LiMn2O4 product.
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