CN102169991A - Positive pole material with nuclear shell structure for lithium battery, and preparation method and application thereof - Google Patents

Positive pole material with nuclear shell structure for lithium battery, and preparation method and application thereof Download PDF

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Publication number
CN102169991A
CN102169991A CN2011100628712A CN201110062871A CN102169991A CN 102169991 A CN102169991 A CN 102169991A CN 2011100628712 A CN2011100628712 A CN 2011100628712A CN 201110062871 A CN201110062871 A CN 201110062871A CN 102169991 A CN102169991 A CN 102169991A
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lithium battery
anode material
general formula
nucleocapsid structure
chemical formula
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徐厚宝
何光明
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SICHUAN SIMEI TECHNOLOGY Co Ltd
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SICHUAN SIMEI TECHNOLOGY Co Ltd
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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

The invention discloses a positive pole material with a nuclear shell structure for a lithium battery, and a preparation method thereof. The positive pole material with a nuclear shell structure for a lithium battery has the general formula of LixFeyPO4.z(LiaMbPO4), wherein the nuclear material has the general formula of LixFeyPO4, wherein x is not less than 0.9 and less than 1.0, and y is not less than 0.9 and less than 1.0; the shell material has the general formula of LiaMbPO4, wherein a is not less than 1.15 and not larger than 1.25, and b is not less than 1.15 and not larger than 1.25; M is selected from one of ferrum, cobalt, nickel, manganese, vanadium, niobium, zirconium and titanium; and z is larger than 0 and not larger than 0.3. The invention further discloses a preparation method of the positive pole material with the nuclear shell structure for the lithium battery, which adopts the production technology of dry mixing without the process of drying; therefore, the energy in industrial production can be effectively saved compared with the prior art.

Description

A kind of anode material of lithium battery and its production and application with nucleocapsid structure
Technical field
The present invention relates to technical field of electrochemistry, be specifically related to a kind of anode material of lithium battery and its production and application with nucleocapsid structure.
Background technology
The olivine structural of conventional base metals ionic compound, owing to be subjected to structural restriction, whole ions diffusion and electron conductivity are not good.In order to improve the problem of these bad conductivities, the common practice can be taked molecular energy level to be reduced material microminiaturization or other metallic atom that mixes.Because the condition of these methods is wayward, so manufacturing cost is quite high.At present, this compounds of industrial manufacturing all adopts wet method, must just can carry out sintering after super-dry, has increased energy consumption greatly.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of anode material of lithium battery with nucleocapsid structure and preparation method thereof is proposed, this anode material of lithium battery with nucleocapsid structure is suitable for use as electrode active material, is particularly suitable for the positive active material as secondary cell; This preparation method can effectively reduce energy consumption.
For achieving the above object, the technical solution adopted in the present invention is: a kind of anode material of lithium battery with nucleocapsid structure is provided, it is characterized in that: described anode material of lithium battery with nucleocapsid structure has following general formula:
Li xFe yPO 4·z(Li aM bPO 4)
Wherein, nuclear material has general formula Li xFe yPO 4, 0.9≤x＜1.0,0.9≤y＜1.0; Shell material has general formula Li aM bPO 4, 1.15≤a≤1.25,1.15≤b≤1.25, M is a kind of in chosen from Fe, cobalt, nickel, manganese, vanadium, niobium, zirconium and the titanium; 0＜z≤0.3.
Preferably, the chemical formula of described anode material of lithium battery is: LiFe 0.99PO 40.05 (Li 1.2Fe 1.2PO 4).Wherein, the chemical formula of nuclear material is: LiFe 0.99PO 4The chemical formula of shell material is: Li 1.2Fe 1.2PO 4
Preferably, the chemical formula of described anode material of lithium battery is: LiFe 0.99PO 40.025 (Li 1.2Mn 1.2PO 4).Wherein, the chemical formula of nuclear material is: LiFe 0.99PO 4The chemical formula of shell material is: Li 1.2Mn 1.2PO 4
Preferably, the chemical formula of described anode material of lithium battery is: LiFe 0.99PO 40.02 (Li 1.2Ni 1.2PO 4).Wherein, the chemical formula of nuclear material is: LiFe 0.99PO 4The chemical formula of shell material is: Li 1.2Ni 1.2PO 4
A kind of preparation method of the above-mentioned anode material of lithium battery with nucleocapsid structure comprises that step is as follows: A, take by weighing ferric phosphate, metal phosphate, lithium compound and ball-milling additive according to molar ratio, adopt dry ball milling to make the reaction precursor body; B, there was down under 500～900 ℃ of temperature conditions the constant temperature calcination in this reaction precursor body 5～30 hours in inert gas, makes and have general formula Li xFe yPO 4Z (Li aM bPO 4) the anode material of lithium battery with nucleocapsid structure, wherein, 0.9≤x＜1.0,0.9≤y＜1.0,0＜z≤0.3,1.15≤a≤1.25,1.15≤b≤1.25.
In steps A, contained metallic element is a kind of in iron, cobalt, nickel, manganese, vanadium, niobium, zirconium, the titanium in the described metal phosphate.
A kind of lithium battery is characterized in that: the positive electrode of described lithium battery has following general formula:
Li xFe yPO 4·z(Li aM bPO 4)
Wherein, nuclear material has general formula Li xFe yPO 4, 0.9≤x＜1.0,0.9≤y＜1.0; Shell material has general formula Li aM bPO 4, 1.15≤a≤1.25,1.15≤b≤1.25, M is a kind of in chosen from Fe, cobalt, nickel, manganese, vanadium, niobium, zirconium and the titanium; 0＜z≤0.3.
In sum, have following advantage at anode material of lithium battery with nucleocapsid structure provided by the present invention and preparation method thereof:
1, nuclear material of the present invention has general formula Li xFe yPO 4, 0.9≤x＜1.0,0.9≤y＜1.0 are a kind of materials with cation vacancy; Shell material of the present invention has general formula Li aM bPO 4, 1.15≤a≤1.25,1.15≤b≤1.25 are a kind of materials with anion vacancy; This intracrystalline space has enlarged the evolving path of lithium ion, and diffusion rate increases, plane of crystal and concentration gradient are less, the also easier diffusion of the lithium ion in centre, therefore, nucleocapsid structure energy-accumulating material of the present invention has higher specific capacity and high rate performance.
2, when the nucleocapsid structure energy-accumulating material is applied voltage, oxidation reaction will take place and make host molecule form electric neutrality in central metal.For balance overall molecule valence mumber balance, when forcing peripheral lithium ion to be deviate from, promptly can produce electronics.Similarly, in inert gas environment, central metal is in order to keep structural stable equilibrium's molecule valence mumber, and central metal can carry out reduction reaction and disengage electric current.Carbon powder particles in the nucleocapsid structure energy-accumulating material can increase reversible generation rate on the electrochemistry of nucleocapsid structure energy-accumulating material.
3, this preparation method has adopted dry mixed production technology, does not need through dry run, so can be effectively energy-conservation than prior art in industrial production.
Description of drawings
Fig. 1 is for having general formula LiFe 0.99PO 40.05 (Li 1.2Fe 1.2PO 4) sem photograph of nucleocapsid structure energy-accumulating material.
Fig. 2 has general formula LiFe for using 0.99PO 40.05 (Li 1.2Fe 1.2PO 4) discharge curve of 26650 batteries made of anode material of lithium battery.
Fig. 3 has general formula LiFe for using 0.99PO 40.05 (Li 1.2Fe 1.2PO 4) the multiplying power discharging curve chart of 26650 batteries made of anode material of lithium battery.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described, so that those skilled in the art understands the present invention better.What need point out especially is that in the following description, when perhaps the detailed description of known function and design can desalinate main contents of the present invention, these were described in here and will be left in the basket.
This anode material of lithium battery with nucleocapsid structure has following general formula: Li xFe yPO 4Z (Li aM bPO 4).Wherein, nuclear material has general formula Li xFe yPO 4, 0.9≤x＜1.0,0.9≤y＜1.0; Shell material has general formula Li aM bPO 4, 1.15≤a≤1.25,1.15≤b≤1.25, M is a kind of in chosen from Fe, cobalt, nickel, manganese, vanadium, niobium, zirconium and the titanium; 0＜z≤0.3.
Preferably, the chemical formula of described anode material of lithium battery is: LiFe 0.99PO 40.05 (Li 1.2Fe 1.2PO 4).Wherein, the chemical formula of nuclear material is: LiFe 0.99PO 4The chemical formula of shell material is: Li 1.2Fe 1.2PO 4
Preferably, the chemical formula of described anode material of lithium battery is: LiFe 0.99PO 40.025 (Li 1.2Mn 1.2PO 4).Wherein, the chemical formula of nuclear material is: LiFe 0.99PO 4The chemical formula of shell material is: Li 1.2Mn 1.2PO 4
Preferably, the chemical formula of described anode material of lithium battery is: LiFe 0.99PO 40.02 (Li 1.2Ni 1.2PO 4).Wherein, the chemical formula of nuclear material is: LiFe 0.99PO 4The chemical formula of shell material is: Li 1.2Ni 1.2PO 4
Above-mentioned preparation method with anode material of lithium battery of nucleocapsid structure comprises that step is as follows: A, take by weighing ferric phosphate, metal phosphate, lithium compound and ball-milling additive according to molar ratio, adopt dry ball milling to make the reaction precursor body, contained metallic element is a kind of in iron, cobalt, nickel, manganese, vanadium, niobium, zirconium, the titanium in the described metal phosphate; B, there was down under 500～900 ℃ of temperature conditions the constant temperature calcination in this reaction precursor body 5～30 hours in inert gas, makes and have general formula Li xFe yPO 4Z (Li aM bPO 4) the anode material of lithium battery with nucleocapsid structure, wherein, 0.9≤x＜1.0,0.9≤y＜1.0,0＜z≤0.3,1.15≤a≤1.25,1.15≤b≤1.25.
A kind of lithium battery is characterized in that: the positive electrode of described lithium battery has following general formula: Li xFe yPO 4Z (Li aM bPO 4).Wherein, nuclear material has general formula Li xFe yPO 4, 0.9≤x＜1.0,0.9≤y＜1.0; Shell material has general formula Li aM bPO 4, 1.15≤a≤1.25,1.15≤b≤1.25, M is a kind of in chosen from Fe, cobalt, nickel, manganese, vanadium, niobium, zirconium and the titanium; 0＜z≤0.3.
In heat treatment stages, the reaction precursor body forms olivine crystalline texture by diffusion into the surface, body diffusion in regular turn.When the nucleocapsid structure energy-accumulating material was applied voltage, oxidation reaction will take place and make host molecule form electric neutrality in central metal.For balance overall molecule valence mumber balance, when forcing peripheral lithium ion to be deviate from, promptly can produce electronics.Similarly, in inert gas environment, central metal is in order to keep structural stable equilibrium's molecule valence mumber, and central metal can carry out reduction reaction and disengage electric current.Carbon powder particles in the nucleocapsid structure energy-accumulating material can increase reversible generation rate on the electrochemistry of nucleocapsid structure energy-accumulating material.
Below the solution of the present invention is illustrated:
Embodiment 1
100kg ferric phosphate and 24.5kg lithium carbonate, 8kg starch are placed ball grinder, and dry grinding 8 hours grinds and disperse up hill and dale, then predecessor is placed alumina crucible, put into the inert atmosphere stove, make stove be warming up to 700 ℃, heat treatment 24 hours with 20 ℃/minute speed.Making with the LiFePO4 is the anode material of lithium battery LiFe with nucleocapsid structure of matrix 0.99PO 40.05 (Li 1.2Fe 1.2PO 4).Granularity is D 50=1.5 μ m, specific area is 14.8m 2/ g, the mixed first powder discharge capacity of material can reach about 143mAh/g.
Embodiment 2
100kg ferric phosphate, 3kg manganese phosphate and 25kg lithium carbonate, 8kg starch are placed ball grinder, dry grinding 8 hours, grind up hill and dale and disperse, then predecessor is placed alumina crucible, put into the inert atmosphere stove, make stove be warming up to 700 ℃, heat treatment 24 hours with 20 ℃/minute speed.Making with the LiFePO4 is the anode material of lithium battery LiFe with nucleocapsid structure of matrix 0.99PO 40.025 (Li 1.2Mn 1.2PO 4).Granularity is D 50=1.6 μ m, specific area is 14.2m 2/ g, the mixed first powder discharge capacity of material can reach about 141mAh/g.
Embodiment 3
100kg ferric phosphate, 2kg nickel phosphate and 24.8kg lithium carbonate, 8kg starch are placed ball grinder, dry grinding 8 hours, grind up hill and dale and disperse, then predecessor is placed alumina crucible, put into the inert atmosphere stove, make stove be warming up to 700 ℃, heat treatment 24 hours with 20 ℃/minute speed.Making with the LiFePO4 is the anode material of lithium battery LiFe with nucleocapsid structure of matrix 0.99PO 40.02 (Li 1.2Ni 1.2PO 4).Granularity is D 50=1.8 μ m, specific area is 13.8m 2/ g, the mixed first powder discharge capacity of material can reach about 140mAh/g.
The anode material of lithium battery with nucleocapsid structure and carbon black and polyvinylidene fluoride (PVDF) with embodiment 1 makes are mixed in the nmp solvent with 93: 3: 4 part by weight.Then mixture is coated on the aluminium foil, after 120 ℃ of oven dry, made anodal test piece.Make anodal test piece form 26650 type electrochemical reversible formula batteries in conjunction with the MCMB negative material.With temperature maintenance in room temperature.The result shows that the mixed first powder discharge capacity of material can reach about 143mAh/g, and high rate performance is better, and 1C discharge capacity/0.2C discharge capacity is about 96.6%.
In sum, nucleocapsid structure energy-accumulating material of the present invention and method for making thereof are better than prior art.Electrochemical redox active material of the present invention has splendid electrochemical reversibility.
Although above the illustrative embodiment of the present invention is described; so that the technical staff of present technique neck understands the present invention; but should be clear; the invention is not restricted to the scope of embodiment; to those skilled in the art; as long as various variations appended claim limit and the spirit and scope of the present invention determined in, these variations are conspicuous, all utilize innovation and creation that the present invention conceives all at the row of protection.

Claims (7)

1. anode material of lithium battery with nucleocapsid structure, it is characterized in that: described anode material of lithium battery with nucleocapsid structure has following general formula:
Li xFe yPO 4·z(Li aM bPO 4)
Wherein, nuclear material has general formula Li xFe yPO 4, 0.9≤x＜1.0,0.9≤y＜1.0; Shell material has general formula Li aM bPO 4, 1.15≤a≤1.25,1.15≤b≤1.25, M is a kind of in chosen from Fe, cobalt, nickel, manganese, vanadium, niobium, zirconium and the titanium; 0＜z≤0.3.
2. the anode material of lithium battery with nucleocapsid structure according to claim 1 is characterized in that: the chemical formula of described anode material of lithium battery is:
LiFe 0.99PO 4·0.05(Li 1.2Fe 1.2PO 4)
Wherein, the chemical formula of nuclear material is: LiFe 0.99PO 4The chemical formula of shell material is: Li 1.2Fe 1.2PO 4
3. the anode material of lithium battery with nucleocapsid structure according to claim 1 is characterized in that: the chemical formula of described anode material of lithium battery is:
LiFe 0.99PO 4·0.025(Li 1.2Mn 1.2PO 4)
Wherein, the chemical formula of nuclear material is: LiFe 0.99PO 4The chemical formula of shell material is: Li 1.2Mn 1.2PO 4
4. the anode material of lithium battery with nucleocapsid structure according to claim 1 is characterized in that: the chemical formula of described anode material of lithium battery is:
LiFe 0.99PO 4·0.02(Li 1.2Ni 1.2PO 4)
Wherein, the chemical formula of nuclear material is: LiFe 0.99PO 4The chemical formula of shell material is: Li 1.2Ni 1.2PO 4
5. a claim 1,2,3 or 4 described preparation methods with anode material of lithium battery of nucleocapsid structure, it is characterized in that: described preparation method comprises that step is as follows:
A, take by weighing ferric phosphate, metal phosphate, lithium compound and ball-milling additive, adopt dry ball milling to make the reaction precursor body according to molar ratio;
B, there was down under 500～900 ℃ of temperature conditions the constant temperature calcination in this reaction precursor body 5～30 hours in inert gas, makes and have general formula Li xFe yPO 4Z (Li aM bPO 4) the anode material of lithium battery with nucleocapsid structure, wherein, 0.9≤x＜1.0,0.9≤y＜1.0,0＜z≤0.3,1.15≤a≤1.25,1.15≤b≤1.25.
6. the preparation method with anode material of lithium battery of nucleocapsid structure according to claim 5 is characterized in that: in steps A, contained metallic element is a kind of in iron, cobalt, nickel, manganese, vanadium, niobium, zirconium, the titanium in the described metal phosphate.
7. lithium battery, it is characterized in that: the positive electrode of described lithium battery has following general formula:
Li xFe yPO 4·z(Li aM bPO 4)
Wherein, nuclear material has general formula Li xFe yPO 4, 0.9≤x＜1.0,0.9≤y＜1.0; Shell material has general formula Li aM bPO 4, 1.15≤a≤1.25,1.15≤b≤1.25, M is a kind of in chosen from Fe, cobalt, nickel, manganese, vanadium, niobium, zirconium and the titanium; 0＜z≤0.3.
CN2011100628712A 2011-03-16 2011-03-16 Positive pole material with nuclear shell structure for lithium battery, and preparation method and application thereof Pending CN102169991A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102509791A (en) * 2011-10-21 2012-06-20 北京中科国发科学技术有限公司 Eutectic composite electrochemical active material and preparation method thereof
CN103515594A (en) * 2012-06-26 2014-01-15 中国科学院苏州纳米技术与纳米仿生研究所 Carbon coated lithium manganese phosphate/lithium iron phosphate core-shell structure material as well as preparation method thereof
EP2693539A1 (en) * 2012-08-03 2014-02-05 Samsung SDI Co., Ltd. Positive active material for rechargeable lithium battery, method of preparing the same, and rechargeable lithium battery including the same
CN109920997A (en) * 2019-03-20 2019-06-21 南通百川新材料有限公司 A kind of cobalt phosphate lithium material and preparation method thereof for all-solid-state battery
CN112993227A (en) * 2021-02-23 2021-06-18 雅安锂盛新能企业管理中心(有限合伙) Lithium iron phosphate composite material with long cycle life, positive electrode material and preparation method of lithium iron phosphate composite material
CN114314546A (en) * 2021-12-21 2022-04-12 万向一二三股份公司 Phosphate anode material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060263286A1 (en) * 2004-11-03 2006-11-23 Tatung Company Preparation of olivine Li Fe PO4 cathode materials for lithium batteries via a solution method
CN101262058A (en) * 2008-04-15 2008-09-10 中南大学 An anode material for compound lithium ion battery

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060263286A1 (en) * 2004-11-03 2006-11-23 Tatung Company Preparation of olivine Li Fe PO4 cathode materials for lithium batteries via a solution method
CN101262058A (en) * 2008-04-15 2008-09-10 中南大学 An anode material for compound lithium ion battery

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102509791A (en) * 2011-10-21 2012-06-20 北京中科国发科学技术有限公司 Eutectic composite electrochemical active material and preparation method thereof
CN103515594A (en) * 2012-06-26 2014-01-15 中国科学院苏州纳米技术与纳米仿生研究所 Carbon coated lithium manganese phosphate/lithium iron phosphate core-shell structure material as well as preparation method thereof
CN103515594B (en) * 2012-06-26 2016-04-27 中国科学院苏州纳米技术与纳米仿生研究所 Lithium manganese phosphate/LiFePO4 Core-shell structure material that carbon is coated and preparation method thereof
EP2693539A1 (en) * 2012-08-03 2014-02-05 Samsung SDI Co., Ltd. Positive active material for rechargeable lithium battery, method of preparing the same, and rechargeable lithium battery including the same
US9490483B2 (en) 2012-08-03 2016-11-08 Samsung Sdi Co., Ltd. Positive active material for rechargeable lithium battery, method of preparing same, and rechargeable lithium battery including same
CN109920997A (en) * 2019-03-20 2019-06-21 南通百川新材料有限公司 A kind of cobalt phosphate lithium material and preparation method thereof for all-solid-state battery
CN109920997B (en) * 2019-03-20 2022-11-15 南通百川新材料有限公司 Cobalt lithium phosphate material for all-solid-state battery and manufacturing method thereof
CN112993227A (en) * 2021-02-23 2021-06-18 雅安锂盛新能企业管理中心(有限合伙) Lithium iron phosphate composite material with long cycle life, positive electrode material and preparation method of lithium iron phosphate composite material
CN114314546A (en) * 2021-12-21 2022-04-12 万向一二三股份公司 Phosphate anode material and preparation method thereof

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Application publication date: 20110831