CN104752690A - A lithium ion battery cathode material and a preparing method thereof - Google Patents

A lithium ion battery cathode material and a preparing method thereof Download PDF

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Publication number
CN104752690A
CN104752690A CN201310737340.8A CN201310737340A CN104752690A CN 104752690 A CN104752690 A CN 104752690A CN 201310737340 A CN201310737340 A CN 201310737340A CN 104752690 A CN104752690 A CN 104752690A
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Prior art keywords
lithium
ion batteries
anode material
coating layer
cathode material
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CN201310737340.8A
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陈彦彬
李珊珊
王汝娜
刘亚飞
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Beijing Easpring Material Technology Co Ltd
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Beijing Easpring Material Technology Co Ltd
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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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • 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

The invention discloses a lithium ion battery cathode material and a preparing method thereof, and particularly relates to a phosphate-coated lithium ion battery cathode material and a preparing method thereof. The chemical constitution of a coating layer is M1<a>M2<b>PO4, wherein the M1 is Ni, Mn and Co, and the M2 is Cr, Al, Mg, Fe, Ti, V, Ga, Cu, Zn, Be, Sc, Ca, Sr, Ba, Zr, Li and La. The cathode material can be normally used under a high cut-off voltage for charging (4.4-4.7 V), and has high thermal stability. A lithium ion battery using the cathode material has a higher volume energy density and better cycle performance. The preparing method of the cathode material includes mixing a cathode material core and a salt solution at least comprising Ni, Mn or Co, adding a phosphate, reacting, forming the phosphate coating layer at least comprising the Ni, the Mn or the Co on at least a part of the surface of the cathode material, and performing heat treatment to obtain the lithium ion battery cathode material.

Description

A kind of anode material for lithium-ion batteries and preparation method thereof
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, be specifically related to a kind of anode material for lithium-ion batteries and preparation method thereof.
Background technology
Along with the consumption electronic product such as mobile phone, panel computer is day by day towards lightening future development, more the positive electrode of high-energy-density day by day becomes the focus of Study on Li-ion batteries, and volume energy density=discharge capacity * discharge voltage plateau * compacted density, therefore, the effective means of current raising energy density is exactly improve the charge cutoff voltage of battery, improve discharge capacity, and then improve the volume energy density of battery.
At present, cobalt acid lithium is conventional anode material for lithium-ion batteries, but the gram volume of cobalt acid lithium under more than 4.2V high pressure plays limited, and cycle performance and memory property are not good.Lot of domestic and international document adopts Al with patent discloses 2o 3, ZnO, ZrO 2, TiO 2deng the technology of oxide clad anode material, as patent CN101752558A discloses at cobalt acid lithium/ternary material surface-coated aluminum oxide, patent CN103094557A discloses at cobalt acid lithium coated with zinc oxide, these patents disclose the surface texture stability that can improve positive electrode at cobalt acid lithium oxide coated on surface, improve the cycle performance under battery high voltage, but in practice, these effects improved are very limited, even also can bring counter productive.Because coated metal oxide is non-electroactive materials, it is very poor to lead lithium ion, can sacrifice gram volume and the discharge voltage plateau of cobalt acid lithium, thus sacrifice the energy density of cobalt acid lithium to a certain extent after coated.
In view of this, really be necessary to provide a kind of anode material for lithium-ion batteries, this positive electrode normally can use under higher charging voltage (4.4V ~ 4.7V), and there is higher thermal stability, make the lithium ion battery adopting this positive electrode have higher volume energy density and good cycle performance.
Summary of the invention
An object of the present invention is to provide a kind of anode material for lithium-ion batteries, and this positive electrode normally can use under higher charge cutoff voltage (4.4V ~ 4.7V), and has higher thermal stability.
Another object of the present invention is to provide a kind of preparation method of above-mentioned anode material for lithium-ion batteries.
The invention discloses a kind of anode material for lithium-ion batteries, this positive electrode comprises: composite oxide particle and coating layer.
Above-mentioned combined oxidation cobalt granule is the oxide at least comprising Li and Co, and it has on average forming by following chemical formulation:
(chemical formula 1) Li 1+xco 1-ya yo 2
Wherein, A represents at least one be selected from Mn, Cr, Ni, V, Ti, Al, Ga or Mg, and preferably, 0≤x≤0.1,0≤y≤1.0.
Above-mentioned coating layer comprises the phosphate containing at least one in Li and Ni, Mn or Co, and its surface being arranged at combined oxidation cobalt granule is gone up at least partially; There is on average forming by following chemical formulation:
(chemical formula 2) M1 am2 bpO 4
Wherein, M1 represents at least one be selected from Ni, Mn or Co, M2 represents at least one be selected from Cr, Al, Mg, Fe, Ti, V, Ga, Cu, Zn, Be, Sc, Ca, Sr, Ba, Zr, Li or La, a, b meet: 0 < a≤1.0,0≤b≤1.0, and when M1 is only Co, b ≠ 0.
Above-mentioned anode material for lithium-ion batteries, preferably, the middle particle size range of positive electrode is 5 ~ 20um.
Above-mentioned anode material for lithium-ion batteries, preferably, coating layer quality is 0.1% ~ 10% of positive electrode gross mass.
On the other hand, for realizing object of the present invention, the present invention also provides a kind of preparation method of above-mentioned anode material for lithium-ion batteries, the key step of the method preferably composite oxide particle at least partially on form the adhesion layer of the salt-mixture containing M1 (and M2); Then composite oxide particle at least partially on formed containing the Phosphate coating layer of M1 (and M2); Last heat treatment obtains described anode material for lithium-ion batteries.Wherein, the described Phosphate coating layer at least containing M1 (and M2) has the average composition of following chemical formulation:
(chemical formula 2) M1 am2 bpO 4
Wherein, M1 represents at least one be selected from Ni, Mn or Co, M2 represents at least one be selected from Cr, Al, Mg, Fe, Ti, V, Ga, Cu, Zn, Be, Sc, Ca, Sr, Ba, Zr, Li or La, a, b meet: 0 < a≤1.0,0≤b≤1.0, and when M1 is only Co, b ≠ 0.
According to implementation method provided by the present invention, a kind of preparation of anode material for lithium-ion batteries specifically can comprise following multiple step:
(1) compound concentration is the mixing salt solution of M1, M2 of 0.1 ~ 4mol/L;
(2) fully mix composite oxide particle and mixing salt solution, form Homogeneous phase mixing slurry;
(3) in above-mentioned mixed slurry, phosphate solution is added, abundant stirring reaction;
At (4) 400 ~ 1000 DEG C, heat treatment obtains end product in 0.5 ~ 2 hour.
In above-mentioned preparation method, the M1 described in step (1) represents at least one in Ni, Mn or Co; M2 represents at least one in Cr, Al, Mg, Fe, Ti, V, Ga, Cu, Zn, Be, Sc, Ca, Sr, Ba, Zr, Li or La.
In above-mentioned preparation method, mixing salt solution is preferably one or more in its sulfate, chlorate, nitrate, acetate, acetate.
In above-mentioned preparation method, the composite oxide particle described in step (2) can be the oxide at least comprising Li and Co, and it has on average forming by following chemical formulation:
(chemical formula 1) Li 1+xco 1-ya yo 2
Wherein, A represents at least one be selected from Mn, Cr, Ni, V, Ti, Al, Ga or Mg, and preferably, 0≤x≤0.1,0≤y≤1.0.
In above-mentioned preparation method, preferably, step (2) can be form mixture in mixing salt solution composite oxide particle being joined M1, M2, controls the addition of composite oxides further, makes mixture be muddy.
In above-mentioned preparation method, the phosphate solution described in step (3) comprises the mixing of one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate and triammonium phosphate.
In the present invention, composite oxide particle at least partially on be provided with coating layer, this coating layer comprises the phosphate containing at least one in Li and Ni, Mn or Co, can while the electron transfer between isolated electrolyte and active material, ion be passed through, thus complete the embedding of lithium ion and while deviating from, avoiding electrolyte to decompose at higher voltages.Therefore this positive electrode can have better battery performance and capacity retention energy at higher voltages.
Further, in the present invention, coating layer has good lithium ion conduction performance, can play effective gram volume under high voltages, and can improve discharge voltage plateau, thus improves the volume energy density of battery to a certain extent.
Further, coating layer and composite oxides kernel introduce P-O key in high-temperature sintering process, enhance the structural stability of positive electrode, improve the cycle performance under high pressure.
On the other hand, the preparation method of anode material for lithium-ion batteries provided by the present invention, adopts first solid solution to mix and makes composite oxide particle coated with uniform one deck M1 2+, M2 2+, then add phosphate thus generate coating layer at composite oxide particle surface in situ, thickness can be generated so evenly and continuous print coating layer, avoiding the absorption produced due to solid mixing uneven thus cause coated uneven situation.Therefore method provided by the present invention is more conducive to heavy industrialization application.
Accompanying drawing explanation
Fig. 1 is scanning electron microscopy (SEM1K) figure of the lithium electricity positive electrode of Phosphate coating prepared by embodiment 1.
Fig. 2 is scanning electron microscopy (SEM5K) figure of the lithium electricity positive electrode of Phosphate coating prepared by embodiment 3.
Fig. 3 is the cyclic curve figure of the lithium electricity positive electrode of Phosphate coating prepared by embodiment 3.
specific implementation method
To contribute to understanding the present invention by following embodiment and accompanying drawing, but not limit content of the present invention.
embodiment 1:
A kind of lithium electricity positive electrode that the present embodiment provides, it comprises kernel and coating layer.Inner core is cobalt acid lithium LiCoO 2, wherein particle diameter is 15um, and coating layer structure is LiNi 0.8mn 0.2pO 4, the mass percent accounting for whole positive electrode is 2%, and the thickness of coating layer is 0.5um.
Preparation method is as follows:
Nickelous sulfate, manganese sulfate are dissolved than the ratio of 0.80:0.20 the mixing salt solution obtaining 2.0mol/L according to metal molar, by 100g cobalt acid lithium LiCoO 2join in 30ml mixing salt solution and form a muddy mixture, then mixture is joined (NH 4) 2hPO 4abundant stirring reaction in solution, 400 DEG C of heat treatments obtain LiNi in 2 hours 0.8mn 0.2pO 4coated LiCoO 2lithium electricity positive electrode.
embodiment 2:
A kind of lithium electricity positive electrode that the present embodiment provides, it comprises kernel and coating layer.Inner core is cation doping acid lithium LiCo 0.8ni 0.2o 2, wherein particle diameter is 8um, and coating layer structure is LiNi 0.9al 0.1pO 4, the mass percent accounting for whole positive electrode is 0.1%, and the thickness of coating layer is 0.01um.
Preparation method is as follows:
Nickel chloride, aluminum nitrate are dissolved than the ratio of 0.90:0.10 the mixing salt solution obtaining 4.0mol/L according to metal molar, by 100g cation doping acid lithium LiCo 0.8ni 0.2o 2join in 30ml mixing salt solution and form a muddy mixture, then mixture is joined NH 4h 2pO 4abundant stirring reaction in solution, 500 DEG C of heat treatments obtain LiNi in 1.5 hours 0.9al 0.1pO 4coated LiCo 0.8ni 0.2o 2lithium electricity positive electrode.
embodiment 3:
A kind of lithium electricity positive electrode that the present embodiment provides, it comprises kernel and coating layer.Inner core is cation doping acid lithium LiCo 0.9mg 0.1o 2, wherein particle diameter is 18um, and coating layer structure is LiMn 0.8fe 0.2pO 4, the mass percent accounting for whole positive electrode is 5%, and the thickness of coating layer is 1um.
Preparation method is as follows:
Manganese sulfate, ferric nitrate are dissolved than the ratio of 0.80:0.20 the mixing salt solution obtaining 0.1mol/L according to metal molar, by 100g cation doping acid lithium LiCo 0.9mg 0.1o 2join in 30ml mixing salt solution and form a muddy mixture, then mixture is joined (NH 4) 3pO 4abundant stirring reaction in solution, 800 DEG C of heat treatments obtain LiMn in 1 hour 0.8fe 0.2pO 4coated LiCo 0.9mg 0.1o 2lithium electricity positive electrode.
embodiment 4:
A kind of lithium electricity positive electrode that the present embodiment provides, it comprises kernel and coating layer.Inner core is cobalt acid lithium LiCoO 2, wherein particle diameter is 20um, and coating layer structure is LiNi 0.8mn 0.15v 0.05pO 4, the mass percent accounting for whole positive electrode is 10%, and the thickness of coating layer is 2um.
Preparation method is as follows:
Nickel nitrate, manganese chloride, vanadium chloride are dissolved than the ratio of 0.80:0.15:0.05 the mixing salt solution obtaining 1.5mol/L according to metal molar, by 100g cobalt acid lithium LiCoO 2join in 30ml mixing salt solution and form a muddy mixture, then mixture is joined (NH 4) 2hPO 4abundant stirring reaction in solution, 1000 DEG C of heat treatments obtain LiNi in 0.5 hour 0.8mn 0.15v 0.05pO 4coated LiCoO 2lithium electricity positive electrode.
embodiment 5:
A kind of lithium electricity positive electrode that the present embodiment provides, it comprises kernel and coating layer.Inner core is cation doping acid lithium LiCo 0.85al 0.15o 2, wherein particle diameter is 11um, and coating layer structure is LiNi 0.5mn 0.4mg 0.1pO 4, the mass percent accounting for whole positive electrode is 8%, and the thickness of coating layer is 1.5um.
Preparation method is as follows:
Nickel acetate, manganese nitrate, magnesium chloride are dissolved than the ratio of 0.50:0.40:0.10 the mixing salt solution obtaining 1.0mol/L according to metal molar, by 100g cation doping acid lithium LiCo 0.85al 0.15o 2join in 30ml mixing salt solution and form a muddy mixture, then mixture is joined NH 4h 2pO 4abundant stirring reaction in solution, 600 DEG C of heat treatments obtain LiNi in 1 hour 0.5mn 0.4mg 0.1pO 4coated LiCo 0.85al 0.15o 2lithium electricity positive electrode.

Claims (9)

1. an anode material for lithium-ion batteries, this positive electrode comprises:
Composite oxide particle, it has the average composition of following chemical formulation:
(chemical formula 1) Li 1+xco 1-ya yo 2
Wherein, A represents at least one be selected from Mn, Cr, Ni, V, Ti, Al, Ga or Mg, and 0≤x≤0.1,0≤y≤0.1;
Coating layer, meets going up at least partially of the surface of oxide particle described in being arranged at, and comprises the phosphate containing at least one in Li and Ni, Mn or Co.
2. anode material for lithium-ion batteries according to claim 1, is characterized in that described coating layer has on average forming by following chemical formulation:
(chemical formula 2) M1 am2 bpO 4
Wherein, M1 represents at least one be selected from Ni, Mn or Co, M2 represents at least one be selected from Cr, Al, Mg, Fe, Ti, V, Ga, Cu, Zn, Be, Bi, Sc, Ca, Sr, Ba, Zr, Li or La, a, b meet: 0 < a≤1.0,0≤b≤1.0, and when M1 is only Co, b ≠ 0.
3. anode material for lithium-ion batteries according to claim 1 and 2, is characterized in that described coating layer quality is 0.1% ~ 10% of positive electrode gross mass.
4. anode material for lithium-ion batteries according to claim 1, is characterized in that the middle particle diameter of described positive electrode is 5 ~ 20um.
5. prepare the method for anode material for lithium-ion batteries for one kind, its preparation method comprises, composite oxide particle at least partially on form the adhesion layer of salt-mixture containing M1 (and M2), then composite oxide particle at least partially on formed containing the Phosphate coating layer of M1 (and M2), heat treatment obtains anode material for lithium-ion batteries; Wherein, M1 represents at least one be selected from Ni, Mn or Co, and M2 represents at least one be selected from Cr, Al, Mg, Ti, V, Ga, Cu, Zn, Be, Sc, Ca, Sr, Ba, Zr, Li or La.
6. the method preparing anode material for lithium-ion batteries according to claim 5, is characterized in that described composite oxide particle has the average composition of following chemical formulation:
(chemical formula 1) Li 1+xco 1-ya yo 2
Wherein, A represents at least one be selected from Mn, Cr, Ni, V, Ti, Al, Ga or Mg, and 0≤x≤0.1,0≤y≤1.0.
7. the method preparing anode material for lithium-ion batteries according to claim 5, it is characterized in that described composite oxide particle at least partially on formed in the step of the adhesion layer of the salt-mixture containing M1 (and M2), form slimy mixture to adhere to by described composite oxide particle being distributed in the mixing salt solution containing M1 (and M2).
8. the method preparing anode material for lithium-ion batteries according to claim 5, is characterized in that M1 salt in described mixing salt solution is one or more of the sulfate of Ni, Mn or Co, chlorate, nitrate, acetate or acetate; M2 salt is one or more in the chlorate of Cr, Al, Mg, Ti, V, Ga, Cu, Zn, Be, Sc, Ca, Sr, Ba, Zr, Li or La, nitrate, acetate, acetate.
9. the method preparing anode material for lithium-ion batteries according to claim 5, is characterized in that coating layer quality is 0.1% ~ 10% of anode composite material gross mass.
CN201310737340.8A 2013-12-30 2013-12-30 A lithium ion battery cathode material and a preparing method thereof Pending CN104752690A (en)

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CN110504444A (en) * 2019-08-19 2019-11-26 王杰 Scandium-vanadium-lithium-manganese oxide serving as positive electrode material of lithium battery and preparation method of scandium-vanadium-lithium-manganese oxide
CN110911664A (en) * 2019-11-13 2020-03-24 北京理工大学 High-nickel cathode material with composite surface layer and preparation method and application thereof
CN113629229A (en) * 2021-08-03 2021-11-09 浙江帕瓦新能源股份有限公司 Phosphate-coated wet-method-doped ternary cathode material and preparation method thereof
WO2024007459A1 (en) * 2022-07-08 2024-01-11 广东邦普循环科技有限公司 Phosphorus-containing substance coated positive electrode material, preparation method therefor and use thereof

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Publication number Priority date Publication date Assignee Title
CN110504444A (en) * 2019-08-19 2019-11-26 王杰 Scandium-vanadium-lithium-manganese oxide serving as positive electrode material of lithium battery and preparation method of scandium-vanadium-lithium-manganese oxide
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CN110911664A (en) * 2019-11-13 2020-03-24 北京理工大学 High-nickel cathode material with composite surface layer and preparation method and application thereof
CN113629229A (en) * 2021-08-03 2021-11-09 浙江帕瓦新能源股份有限公司 Phosphate-coated wet-method-doped ternary cathode material and preparation method thereof
CN113629229B (en) * 2021-08-03 2023-02-24 浙江帕瓦新能源股份有限公司 Phosphate-coated wet-method-doped ternary cathode material and preparation method thereof
WO2024007459A1 (en) * 2022-07-08 2024-01-11 广东邦普循环科技有限公司 Phosphorus-containing substance coated positive electrode material, preparation method therefor and use thereof

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Application publication date: 20150701