CN102637854B - Preparation method of polyanion cathode material of lithium ion battery - Google Patents
Preparation method of polyanion cathode material of lithium ion battery Download PDFInfo
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- CN102637854B CN102637854B CN201110037904.8A CN201110037904A CN102637854B CN 102637854 B CN102637854 B CN 102637854B CN 201110037904 A CN201110037904 A CN 201110037904A CN 102637854 B CN102637854 B CN 102637854B
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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 relates to a preparation method of a polyanion cathode material of a lithium ion battery. The cathode material is a polyanion compound expressed by LiMx(XOy)z (Formula I). The preparation method comprises the following steps: uniformly stirring and mixing a lithium source, an M source, an X source and an electric conduction additive in a solvent under the protection of an inert atmosphere to obtain slurry; drying the slurry under the protection of an inert atmosphere to obtain a precursor material; sintering the precursor material under the protection of an inert atmosphere to obtain the polyanion compound; and crushing the obtained polyanion compound under the protection of an inert atmosphere. The overall processes of the preparation method are finished under the protection of the inert atmosphere, thus the oxidation of the prepared polyanion compound in the preparation process is effectively prevented, the generation of a mixed phase of the material is inhibited, and the declining of the electrical property of the material is avoided.
Description
Technical field
The present invention relates to lithium ion battery field, and more specifically relate to a kind of preparation method for lithium ion battery polyanionic positive electrode.
Background technology
Lithium ion secondary battery anode material has experienced the LiCoO of layer structure
2, LiNiO
2, spinel structure LiMn
2o
4etc. the development in several stages.LiCoO
2and LiNiO
2theoretical capacity larger (being 274mAh/g), but the restriction of the phase transformation causing due to lithium deintercalation process, actual capacity is 130mAh/g left and right only, LiCoO
2in Co poisonous, expensive, limited its application; And LiNiO
2the preparation of pure phase is very difficult, have a day problem for ion disordering, and thermal stability is very poor; The LiMn of spinelle
2o
4although have the advantage in price, it is its subject matter that the dissolving of Mn causes its high temperature capacity to fail rapidly.Within 1996, play the people such as J.B.Goodenough, C.Masquelier and take the lead in having studied Li
3fe
2(PO
4)
3, Li
3v
2(PO
4)
3, LiFePO
4deng polyanion compound, for positive electrode is introduced new type.Li afterwards
2feSiO
4, Li
2mnSiO
4, LiFeBO
3pay attention to as anode material for lithium-ion batteries also studied person Deng material.
Polyanion compound positive electrode and traditional lamellar structure compound, spinel structure Compound Phase ratio, except oxygen element, also has another nonmetalloid X (X=P, Si, B, S etc.), X forms polyhedron with O and is connected with 0 polyhedron forming with transition metal M (M=Fe, Mn, Ni, Co, Ti, V etc.) by the mode on concurrent, common rib or common limit, thereby M-O polyhedron is separated.This polyhedral having is beneficial to stable framework, and keeps stable in the embedding of lithium ion, while deviating from.
Summary of the invention
The present invention relates to one and prepare polyanion compound positive electrode LiM
x(XO
y)
zthe method of (formula I), wherein 0.5≤x≤1,3≤y≤4,0.5≤z≤1; The method comprises the steps:
By lithium source, M source, X source and conductive additive in solvent, under inert atmosphere protection, be uniformly mixed acquisition slurries;
Under inert atmosphere, to slurry dried, obtain persursor material;
Persursor material carries out sintering under inert atmosphere protection, obtains described polyanion compound; With
The polyanion compound of acquisition is pulverized under inert atmosphere.
According to an aspect of the present invention, the M in above-mentioned formula I is one or more in transition metal Fe, Mn, Ni, Co, Ti and V.
According to another aspect of the present invention, the X in above-mentioned formula I is one or more in P, Si, B and S.
According to a further aspect of the invention, the crystal structure of described polyanion compound is that the polyhedron that M forms with O with X with the polyhedron of O formation is connected by concurrent, altogether rib or coplanar mode.
According to a further aspect of the invention, the lithium source of preparation method's employing of the present invention is selected from the group of following composition: lithium hydroxide, lithium carbonate, lithium acetate, lithium oxalate and lithium dihydrogen phosphate.
According to another aspect of the present invention, the M source of preparation method's employing of the present invention is selected from the group of following composition: oxide, carbonate, hydroxide, oxalates, acetate and phosphate.
According to a further aspect of the invention, the X source of preparation method's employing of the present invention is selected from the group of following composition: the salt that the acid that the salt that oxide, the acid that acid, oxide that oxide is corresponding are corresponding form with lithium hydroxide and oxide are corresponding and the hydroxide of M form.
According to a further aspect of the invention, the solvent of preparation method's employing of the present invention is selected from the group of following composition: pure water, absolute ethyl alcohol, acetone and isobutanol.
According to another aspect of the present invention, the conductive additive of preparation method's employing of the present invention is selected from the group of following composition: graphite, carbon gel, carbon nano-tube, glucose, sucrose, citric acid, polyethylene glycol and polyvinyl alcohol.
According to another aspect of the present invention, the drying mode that preparation method of the present invention adopts comprises that vacuumize, heat drying, freeze drying and/or spraying are dry etc.
According to a further aspect of the invention, the protective atmosphere of preparation method's employing of the present invention is selected from the group of following composition: nitrogen, nitrogen hydrogen mixed gas, argon gas, argon gas hydrogen mixed gas etc.
According to a further aspect of the invention, the pulverizing in material Preparation Method of the present invention completes by the mode such as mechanical crushing, air-flow crushing, thereby obtains the polyanion compound of appropriate particle size.
Preparation method's overall process of the present invention is to complete under inert atmosphere protection, thereby effectively prevents that the polyanion compound of preparation is oxidized in preparation process, has suppressed this material production dephasign, thereby has avoided the decline of material electrical property; And the stability of products quality guarantee and batch consistency.The polyanion compound positive electrode being made by preparation method of the present invention detects M through x-ray photoelectron power spectrum (XPS) and does not have oxidized phenomenon, thereby has the good result of non-oxidation.
Accompanying drawing explanation
Fig. 1 is the XPS collection of illustrative plates of the LiFePO 4 material after the pulverizing prepared of the embodiment of the present invention 1.
Embodiment
Below by specific embodiment, above-mentioned and other advantage of the present invention and feature are specifically described.The object of embodiment is example preparation method of the present invention, and preparation method of the present invention is not limited to these embodiment.
Embodiment 1
1mol lithium dihydrogen phosphate, 0.5mol di-iron trioxide, 30g glucose are added in 250ml water; use can inflated with nitrogen the grinder of protection raw material are stirred; adopt closed nitrogen protection spray drying device to be dried slurries; obtain precursor powder; then by precursor powder 700 ℃ of sintering 16h in the box type furnace that continues logical nitrogen atmosphere, in the airflow milling equipment that possesses the protection of atmosphere gas, pulverize and obtain the LiFePO4 (LiFePO that D50 particle diameter is 3-6 μ m afterwards
4) material.
Then LiFePO4 is made to simulated battery as anode material for lithium-ion batteries, carry out battery performance test.First active material and PVDF, Super-P are distributed to N-methyl in mass ratio than making slurry in pyrrolidone (NMP) at 85: 10: 5, then with scraper plate coating machine, slurry coating is formed on aluminium foil to electrode slice, electrode slice in vacuum drying chamber in 110 ℃ of dry 12h.On electrode slice, stamp out 1cm
2negative pole disk.Battery pack is contained in the glove box that is full of high-purity argon gas and completes.Adopting CR2025 button cell is test model, and take lithium sheet as to electrode, Celgard 2300 polypropylene porous films are barrier film, and electrolyte is 1mol/L LiPF
6the mixed solution of ethylene carbonate (EC)/dimethyl carbonate (DMC) (volume ratio is 1: 1).Current density with 0.1C is carried out charge and discharge cycles test to battery between the voltage of 2.0-4.2V.
Battery performance is tested to discovery, and the 0.1C discharge capacity of LiFePO 4 material reaches 151mAh/g.
LiFePO 4 material is made to XPS (x-ray photoelectron power spectrum) figure, as shown in Figure 1.Can see that from this figure the valence state of iron in the LiFePO 4 material after pulverizing is+divalent, the Fe of do not exist+3 valencys.
1mol lithium dihydrogen phosphate, 1mol ferrous oxalate, 25g citric acid are added in 250ml water; use can inflated with nitrogen the grinder of protection raw material are stirred; adopt closed nitrogen protection spray drying device to be dried slurries, obtain precursor powder, precursor powder is being continued to logical N
2/ H
2720 ℃ of sintering 16h in the box type furnace of (95: 5) mixed atmosphere pulverize and obtain the LiFePO4 (LiFePO that D50 particle diameter is 3-6 μ m afterwards in the airflow milling equipment that possesses nitrogen protection
4) material.Other experimental procedures are identical with embodiment 1 with testing procedure.
Battery performance is tested to discovery, and the 0.1C discharge capacity of LiFePO 4 material reaches 155mAh/g.
Embodiment 3
1mol lithium hydroxide, 1mol ferric phosphate, 28g carbon gel are added in 250ml water; use can inflated with nitrogen the grinder of protection raw material are stirred; adopt closed nitrogen protection spray drying device to be dried slurries; obtain precursor powder; by precursor powder 700 ℃ of sintering 16h in the box type furnace that continues logical Ar atmosphere, in the airflow milling equipment that possesses nitrogen protection, pulverize and obtain the LiFePO4 (LiFePO that D50 particle diameter is 3-6 μ m afterwards
4) material.Other experimental procedures are identical with embodiment 1 with testing procedure.
Battery performance is tested to discovery, and the 0.1C discharge capacity of LiFePO 4 material reaches 153mAh/g.
Embodiment 4
2mol lithium hydroxide, 1mol tetraethyl orthosilicate, 1mol ferrous oxalate, 35g sucrose are added in 250ml water; use can inflated with nitrogen the grinder of protection raw material are stirred; adopt closed nitrogen protection freeze drying equipment to be dried slurries; obtain precursor powder; by precursor powder 750 ℃ of sintering 24h in the box type furnace that continues logical Ar atmosphere, in the airflow milling equipment that possesses the protection of atmosphere gas, pulverize and obtain the ferric metasilicate lithium (Li that D50 particle diameter is 2-8 μ m afterwards
2feSiO
4) material.Other experimental procedures are identical with embodiment 1 with testing procedure.
Battery performance is tested to discovery, and the 0.1C discharge capacity of ferric metasilicate lithium material reaches 133mAh/g.
Embodiment 5
2mol lithium hydroxide, 1mol tetraethyl orthosilicate, 1mol magnesium acetate, 35g sucrose are added in 250ml water; use can inflated with nitrogen the grinder of protection raw material are stirred; adopt closed nitrogen protection freeze drying equipment to be dried slurries; obtain precursor powder; by precursor powder 750 ℃ of sintering 24h in the box type furnace that continues logical Ar atmosphere, in the airflow milling equipment that possesses nitrogen protection, pulverize and obtain the manganese silicate of lithium (LiMnSiO that D50 particle diameter is 2-8 μ m afterwards
4) material.Other experimental procedures are identical with embodiment 1 with testing procedure.
Battery performance is tested to discovery, and the 0.1C discharge capacity of manganese silicate of lithium material reaches 129mAh/g.
Embodiment 6
1mol lithium hydroxide, 1mol ferrous oxalate, 1mol boron oxide, 20g carbon black are added in 250ml water; use can inflated with nitrogen the grinder of protection raw material are stirred; adopt closed nitrogen protection freeze drying equipment to be dried slurries; obtain precursor powder; by precursor powder 600 ℃ of sintering 24h in the box type furnace that continues logical Ar atmosphere, in the airflow milling equipment that possesses nitrogen protection, pulverize and obtain the iron borate lithium (LiFeBO that D50 particle diameter is 2-8 μ m afterwards
3) material.Other experimental procedures are identical with embodiment 1 with testing procedure.
Battery performance is tested to discovery, and the 0.1C discharge capacity of iron borate lithium material reaches 122mAh/g.
Embodiment 7
1mol lithium dihydrogen phosphate, 0.95mol ferrous oxalate, 0.05mol ammonium metavanadate, 25g glucose are added in 250ml water; use can inflated with nitrogen the grinder of protection raw material are stirred; adopt closed nitrogen protection spray drying device to be dried slurries; obtain precursor powder, precursor powder is being continued to logical N
2720 ℃ of sintering 12h in the box type furnace of atmosphere pulverize and obtain the phosphoric acid vanadium iron lithium (LiFe that D50 particle diameter is 3-6 μ m afterwards in the airflow milling equipment that possesses nitrogen protection
0.95v
0.05pO
4) material.Other experimental procedures are identical with embodiment 1 with testing procedure.
Battery performance is tested to discovery, and the 0.1C discharge capacity of LiFePO 4 material reaches 158mAh/g.
Comparative example 1:
1mol lithium dihydrogen phosphate, 0.5mol di-iron trioxide, 30g glucose are added in 250ml water; use grinder that raw material are stirred; adopt open type spray drying device to be dried slurries; obtain precursor powder; then by precursor powder 700 ℃ of sintering 16h in the box type furnace that continues logical nitrogen atmosphere, in the airflow milling equipment without atmosphere protection, pulverize and obtain the LiFePO4 (LiFePO that D50 particle diameter is 3-6 μ m afterwards
4) material.Other experimental procedures are identical with embodiment 1 with testing procedure.
Battery performance is tested to discovery, and the 0.1C discharge capacity of LiFePO 4 material reaches 133mAh/g.
Comparative example 2
1mol lithium dihydrogen phosphate, 1mol ferrous oxalate, 25g citric acid are added in 250ml water, use grinder that raw material are stirred, adopt open spray drying device to be dried slurries, obtain precursor powder, precursor powder is being continued to logical N
2/ H
2720 ℃ of sintering 16h in the box type furnace of (95: 5) mixed atmosphere pulverize and obtain the LiFePO4 (LiFePO that D50 particle diameter is 3-6 μ m afterwards in the airflow milling equipment without atmosphere protection
4) material.Other experimental procedures are identical with embodiment 2 with testing procedure.
Battery performance is tested to discovery, and the 0.1C discharge capacity of LiFePO 4 material reaches 137mAh/g.
Claims (12)
1. a preparation method for anode material for lithium-ion batteries, is characterized in that described positive electrode is the polyanion compound that formula I represents,
LiM
x(XO
y)
zformula I
In formula, 0.5≤x≤1,3≤y≤4,0.5≤z≤1;
Described preparation method comprises the steps:
By lithium source, M source, X source and conductive additive in solvent, under inert atmosphere protection, be uniformly mixed acquisition slurries;
Under inert atmosphere, to slurry dried, obtain persursor material;
Persursor material carries out sintering under inert atmosphere protection, obtains described polyanion compound; With
The polyanion compound of acquisition is pulverized under inert atmosphere.
2. preparation method according to claim 1, is characterized in that M is one or more in transition metal Fe, Mn, Ni, Co, Ti and V.
3. preparation method according to claim 2, is characterized in that X is one or more in P, Si, B and S.
4. preparation method according to claim 3, the crystal structure that it is characterized in that described polyanion compound is that the polyhedron that M forms with O with X with the polyhedron of O formation is connected by concurrent, altogether rib or coplanar mode.
5. preparation method according to claim 4, is characterized in that described lithium source is selected from the group of following composition: lithium hydroxide, lithium carbonate, lithium acetate, lithium oxalate and lithium dihydrogen phosphate.
6. preparation method according to claim 5, is characterized in that described M source is selected from the group of following composition: oxide, carbonate, hydroxide, oxalates, acetate and phosphate.
7. preparation method according to claim 6, is characterized in that described X source is selected from the group of following composition: the salt that the acid that the salt that oxide, the acid that acid, oxide that oxide is corresponding are corresponding form with lithium hydroxide and oxide are corresponding and the hydroxide of M form.
8. preparation method according to claim 7, is characterized in that described solvent is selected from the group of following composition: water, absolute ethyl alcohol, acetone and isobutanol.
9. preparation method according to claim 8, is characterized in that described conductive additive is selected from the group of following composition: graphite, carbon gel, carbon nano-tube, glucose, sucrose, citric acid, polyethylene glycol and polyvinyl alcohol.
10. preparation method according to claim 9, is characterized in that described dryly complete in the following way: vacuumize, heat drying, freeze drying and/or spraying are dry.
11. according to the preparation method described in any one in claim 1-10, it is characterized in that described atmosphere is selected from the group of following composition: nitrogen, nitrogen hydrogen mixed gas, argon gas and argon gas hydrogen mixed gas.
12. preparation methods according to claim 11, is characterized in that described pulverizing is selected from mechanical crushing and/or air-flow crushing.
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| CN103972476A (en) * | 2014-05-16 | 2014-08-06 | 中南大学 | Preparation method of positive electrode material, phosphoric acid oxygen vanadium lithium, of lithium ion battery |
| CN106586999A (en) * | 2015-10-18 | 2017-04-26 | 深圳市沃特玛电池有限公司 | Method for preparing lithium iron phosphate precursor by virtue of vacuum freeze drying |
| CN105261750A (en) * | 2015-11-14 | 2016-01-20 | 合肥国轩高科动力能源有限公司 | Synthetic method for novel anode material, namely manganese lithium stannate, for lithium ion battery |
| CN107464928B (en) * | 2017-07-17 | 2020-06-23 | 上海应用技术大学 | Lithium manganese silicate material for lithium ion battery anode material and preparation method thereof |
| CN112744800B (en) * | 2019-10-30 | 2022-08-26 | 泓辰材料股份有限公司 | Tungsten-doped lithium manganese iron phosphate particles and powder materials for positive electrodes of lithium ion batteries and preparation methods thereof |
| CN111509206A (en) * | 2020-04-23 | 2020-08-07 | 中国科学院过程工程研究所 | Composite lithium-rich cathode material and preparation method and application thereof |
| CN113264516B (en) * | 2021-07-21 | 2021-09-28 | 温州玖源锂电池科技发展有限公司 | Preparation method of lithium iron vanadium phosphate carbon nanotube modified ternary cathode material |
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| FR2937185B1 (en) * | 2008-10-09 | 2011-02-25 | Batscap Sa | ELECTRODE COMPRISING A MODIFIED COMPLEX OXIDE AS ACTIVE MATERIAL. |
| KR100939647B1 (en) * | 2009-01-22 | 2010-02-03 | 한화석유화학 주식회사 | Anion-deficient non-stoichiometric lithium transition metal polyacid compound as electrode active material, method for preparing the same, and electrochemical device using the same |
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| CN1514804A (en) * | 2001-04-10 | 2004-07-21 | �͵�-���ڱ�̫���ܺ������о������빫 | Binary, ternary and quaternary lithium phosphates, method for production thereof and use of the same |
| CN1806356A (en) * | 2003-04-16 | 2006-07-19 | 卡伯特公司 | Method of producing membrane electrode assemblies |
| CN101573812A (en) * | 2006-12-28 | 2009-11-04 | 株式会社杰士汤浅 | Positive electrode material for nonaqueous electrolyte secondary battery, nonaqueous electrolyte secondary battery comprising the same, and method for producing the same |
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