CN104979557A - High-rate lithium iron phosphate positive electrode material and battery electrode sheet - Google Patents
High-rate lithium iron phosphate positive electrode material and battery electrode sheet Download PDFInfo
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- CN104979557A CN104979557A CN201510258029.4A CN201510258029A CN104979557A CN 104979557 A CN104979557 A CN 104979557A CN 201510258029 A CN201510258029 A CN 201510258029A CN 104979557 A CN104979557 A CN 104979557A
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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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 present invention discloses a high-rate lithium iron phosphate positive electrode material preparation method and a lithium-ion battery positive electrode sheet of the material. The preparation method comprises: lithium iron phosphate positive electrode material preparing; chemical plating of elemental aluminum on the lithium iron phosphate surface; and lithium iron phosphate-graphene composite material preparing. Compared with the material in the prior art, the composite material of the present invention has the following advantages that: 1, the chemical plating method is used to achieve the molecular-level surface coating; and 2, with the graphene doping, the electric conductivity of the lithium iron phosphate material can be substantially improved, and the material is especially suitable for high-power power lithium-ion batteries.
Description
Technical field
The present invention relates to a kind of preparation method of high magnification lithium iron phosphate positive material, and the positive plate using this high magnification positive electrode to make.
Background technology
Development and the battery performance of positive electrode are closely related, and therefore people are always at the cathode material of development of new.At present extensively the anode material for lithium-ion batteries of research concentrates on transition metal oxide LiMO2(M=Co, Ni, Mn as layer structure of lithium) and the LiMn2O4 of spinel structure.As positive electrode, they differ from one another, and LiCoO2 cost is high, natural resources shortage, and toxicity is large; LiNiO2 prepares difficulty, poor heat stability; LiMn2O4 capacity is lower, and cyclical stability is poor.In order to solve the defect of above material, battery circle has done large quantity research.1997, the LiFePO4 that Padhi etc. report olivine-type has excellent chemical property, wherein LiFePO4 raw material sources are extensive, cheap, non-environmental-pollution, the Heat stability is good of material, the security performance of prepared battery is given prominence to, and becomes the anode material for lithium-ion batteries of new generation of most development and application potentiality.But pure phase LiFePO4 material is because lithium ion diffusion velocity is slow and electron conduction is poor, practical value useless.By coated, ion doping and interpolation metallic conduction powder can improve the conductivity of material; By nanometer or prepare the evolving path that porous material can shorten lithium ion, improve the utilance of lithium ion with this.The coated mode of common carbon causes carbon-coating can only carry out the coated of part to particle, and be difficult to carry out coated to particle completely, this has just shone into certain polarization phenomena, is difficult to the requirement meeting fast charging and discharging performance.
Graphene is a kind of new material risen in recent years, its structure can be understood as the graphite of individual layer, because it has splendid electric conductivity, good electric conductivity is also also existed to lithium ion simultaneously, make it have more outstanding advantage as in additive agent modified material.Due to the two-dimension plane structure that Graphene is special, material can be made to carry out coated in its superficial growth or Graphene to material, form composite material.
Pass through patent retrieval, patent 200910052413.3, lithium ion battery anode material lithium iron phosphate of a kind of Graphene compound and preparation method thereof, use the Graphene of high conductivity as electric conducting material, but owing to there is the not high problem of Graphene Compound Degree, in charge and discharge process, thus there will be polarization phenomena to a certain degree.Patent 201010207516.5, the preparation method of LiFePO 4 material and lithium ion battery and positive plate thereof, prepare composite ferric lithium phosphate material by the method for chemical plating, carries out Surface coating owing to adopting chemical plating method, improve the conductivity of material, but there is the problem of long-range conductivity deficiency.By patent retrieval, also do not find following relevant report: chemical plating metal is carried out and doped graphene combines the conductivity improving LiFePO 4 material in LiFePO4 surface.This composite material has the following advantages: 1. adopt electroless plating method to realize other Surface coating of molecular level; 2. the rare conductivity greatly can improving LiFePO 4 material of doped graphite.
Summary of the invention
The object of the invention there are provided the preparation method of a kind of high magnification LiFePO4 composite material and battery pole piece, comprises the steps: step one, the preparation of lithium iron phosphate positive material or directly use lithium iron phosphate positive material ready-made on the market; Step 2, LiFePO4 surface chemical metal plating aluminium simple substance; Step 3, the preparation of LiFePO4-graphene composite material; Step 4, the positive plate made with above-mentioned positive electrode.
According in the preparation method of a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece, in described step one, lithium iron phosphate positive material can use now common method to carry out synthesizing or directly buying lithium iron phosphate positive material ready-made on the market.If oneself synthesizing iron lithium phosphate, sintering temperature is 600-850 degree, temperature retention time 1-10h, and has argon gas or nitrogen protection gas.
According in the preparation method of a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece, in described step 2, LiFePO4 surface chemical metal plating (for metallic aluminium), comprises following a few sub-steps:
1. prepare metal fused salt electroplate liquid: described metal fused salt electroplate liquid comprises aluminum metal room temperature fused salt;
2. the configuration of activating solution: the chlorate solution containing active metal Pd, Ru or Rh ion is joined ethanol, in propyl alcohol or ethylene glycol, is configured to the activating solution of alcohol-water mixture;
3. the activation of lithium iron phosphate positive material: under nitrogen or argon inert atmosphere, LiFePO 4 material is immersed in above-mentioned activating solution, reflux under inert gas shielding, make reactive metal deposits activated matrix LiFePO 4 material surface, by activation after lithium iron phosphate positive material washing and filtering and vacuumize;
4. under inert gas shielding, by the lithium iron phosphate positive material after activation as in electroplate liquid, control reducing condition, LiFePO4 surface lamination metal simple-substance, described redox reaction temperature is 25-50 degree;
5. wash with the lithium iron phosphate positive material of absolute ethyl alcohol effects on surface plating, by the composite ferric lithium phosphate material vacuum drying after cleaning.
According in the preparation method of a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece, in described step 3, the preparation of LiFePO4/graphene composite material.By composite ferric lithium phosphate material with after fully mixing according to the Graphene of constant weight or graphite oxide, after in inert gas shielding, 500-800 degree calcines a period of time, cooling can obtain high magnification LiFePO 4 material to be prepared.
According in the preparation method of a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece, in described step 4, by above-mentioned composite ferric lithium phosphate material, conductive agent and binding agent according to certain proportioning be mixed even after, be coated on foil surface, dry and i.e. gained battery pole piece after carrying out compacting.
According in a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece, preferably, described inorganic metal aluminium salt comprises aluminum halide, and the content of described aluminum halide accounts for the 20-50% of molten fuse salt total amount; Described organic halogenation salt comprises halogenation quaternary amine, imidazolium halide salt, pyridiniujm, the 30-80% of described organic halogenation salt content station fuse salt total amount; The concentration range of described organic reducing agent in electroplate liquid is 0.005-0.5mol/L, and in described organic reducing agent and described aluminum metal fused salt, the mol ratio of aluminium salt is 0.5-5.0.
According in a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece, preferably, described activating solution also comprises the polymer stabilizer that concentration is not more than 0.01mol/L, and described stabilizer comprises, polyvinyl alcohol or polyethylene glycol.
According in a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece, preferably, cover the 0.1-5.0% that aluminum amount accounts for composite material total amount.
According in a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece, preferably, the preparation method of LiFePO4/graphene composite material, described grapheme material is that the material with carbon element between 1-20 layer forms by individual layer or the number of plies.
According in a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece, preferably, the preparation method of LiFePO4/graphene composite material, raw material uniform mixing method is solid phase or the fully mixing of solid-liquid machinery, liquid phase substance can adopt ethanol or acetone, incorporation time is 2-50h, and wherein Graphene content is between the 0.1-5% of lithium iron phosphate positive material weight.
According in a kind of high magnification LiFePO4 composite material of the present invention and battery pole piece; preferably; the preparation method of LiFePO4/graphene composite material, 550 DEG C of calcining 0.5-5h when there being nitrogen to protect, namely cooling obtains LiFePO4/graphene composite material of the present invention naturally.
The feature of high magnification LiFePO4 composite material of the present invention is, LiFePO4 coated with uniform one deck aluminum metal, and then forms composite material with Graphene, and it is inner or surperficial that Graphene is distributed in lithium iron phosphate particles, forms long-range conductive network.
Beneficial effect of the present invention is as follows: 1. adopt electroless plating method to realize other Surface coating of molecular level; 2. the rare conductivity greatly can improving LiFePO 4 material of doped graphite.
For object of the present invention, in second of the present invention, the invention provides a kind of positive plate of lithium iron phosphate lithium battery, described positive plate comprises above-mentioned composite ferric lithium phosphate material.
For object of the present invention, in 3rd of the present invention, the invention provides a kind of ferric phosphate lithium cell, in described positive plate of iron phosphate lithium battery, comprise above-mentioned composite ferric lithium phosphate material.
Accompanying drawing explanation
Fig. 1 is the XRD diffraction pattern of the high magnification lithium iron phosphate positive material that pole piece of the present invention obtains.
Embodiment
Embodiment one:
Step one: sintering preparation iron phosphate powder: by lithium carbonate; ferric phosphate is as raw material; the ratio of control Li, Fe and PO4 carries out ball milling, using acetone as medium according to 1.05:1:1; ratio of grinding media to material is 5:1; mill after 12h, mixture is placed in 650 DEG C, tube furnace, calcining 8h; logical argon gas is protected, and obtains iron phosphate powder after cooling.
Step 2: preparation aluminum metal Molten Salt Electroplating liquid: inorganic metal aluminium salt is generally aluminium chloride, its content accounts for 25% of fused salt total amount, organic halogenation salt is halogenation quaternary amine, its content accounts for 60% of fused salt total amount, organic solvent is benzene, and its consumption is 0.05mol/L for making trivalent aluminium salt ultimate density, and organic reducing agent is lithium hydride, be 2:1 with organic aluminium salt mol ratio, the concentration of organic reducing agent in electroplate liquid is 0.25mol/L.
Step 3: preparation is containing the chlorate solution of active metal Pd ion: the concentration of chlorate is 0.005mol/L, and the ethanol added is equal with chlorate liquor capacity, to be configured to the alcohol-water mixture of 50%, can stir in preparation process, makes two to mix.
Step 4: the activation of lithium iron phosphate positive material: under argon inert atmosphere; LiFePO 4 material is immersed in above-mentioned activating solution; and add polyethylene glycol stabilized dose; the concentration of stabilizer is 0.005mol/L; stirring and refluxing is carried out under inert gas shielding; control reaction temperature 30-40 degree, make reactive metal deposits on activated matrix LiFePO 4 material surface, by the lithium iron phosphate positive material washing and filtering after activation and vacuumize.
Step 5: LiFePO4 surface lamination metal simple-substance aluminium: under argon shield, the lithium iron phosphate positive material after activation is placed in electroplate liquid, low speed magnetic agitation 3h, material is fully mixed with electroplate liquid, controlling reducing condition temperature is 35-45 DEG C.
Step 6: the preparation of high magnification LiFePO4 composite material: by the LiFePO 4 material of above-mentioned coated metal and according to LiFePO4 weight 2% Graphene carry out mixing 10h; 550 degree of calcining 1.5h when there being nitrogen to protect, namely cooling obtains LiFePO4/graphene composite material of the present invention naturally.
Step 7: above-mentioned LiFePO4/graphene composite material is made into flexible package 503759-800mAh high-multiplying-power battery according to existing common lithium ion battery manufacture craft on the market, and then carry out high rate performance test, test result is as follows:
As can be seen from data, after adopting LiFePO4/graphene composite material of the present invention to make battery, its internal resistance reduces 13.2% than conventional aluminium foil battery, and high rate performance is to being significantly improved.
Claims (8)
1. high magnification lithium iron phosphate positive material and a battery pole piece, comprise the steps: step one, the preparation of lithium iron phosphate positive material or directly use lithium iron phosphate positive material ready-made on the market; Step 2, LiFePO4 surface chemical metal plating aluminium simple substance; Step 3, the preparation of LiFePO4-graphene composite material; Step 4, the positive plate made with above-mentioned positive electrode.
2. high magnification lithium iron phosphate positive material and a battery pole piece, is characterized in that, comprises in described step 2:
Sub-step one: prepare metal fused salt electroplate liquid;
Sub-step two: the configuration of activating solution
Sub-step three: the activation of lithium iron phosphate positive material
Sub-step four: LiFePO4 surface lamination metal simple-substance.
3. a kind of high magnification lithium iron phosphate positive material as claimed in claim 2 and battery pole piece, is characterized in that, the sub-step one described in it prepares metal fused salt electroplate liquid, and described metal fused salt electroplate liquid comprises aluminum metal room temperature fused salt;
The configuration of sub-step two activating solution: the chlorate solution containing active metal Pd, Ru or Rh ion is joined ethanol, in propyl alcohol or ethylene glycol, is configured to the activating solution of alcohol-water mixture;
The activation of sub-step triphosphoric acid iron lithium ion anode material: under nitrogen or argon inert atmosphere, LiFePO 4 material is immersed in above-mentioned activating solution, reflux under inert gas shielding, make reactive metal deposits activated matrix LiFePO 4 material surface, by activation after lithium iron phosphate positive material washing and filtering and vacuumize;
Sub-step four LiFePO4 surface lamination metal simple-substance: under inert gas shielding, by the lithium iron phosphate positive material after activation as in electroplate liquid, control reducing condition, LiFePO4 surface lamination metal simple-substance, described redox reaction temperature is 25-50 degree.
4. a kind of high magnification lithium iron phosphate positive material as claimed in claim 3 and battery pole piece, is characterized in that, in the sub-step one described in it: described inorganic metal aluminium salt comprises aluminum halide, and the content of described aluminum halide accounts for the 20-50% of molten fuse salt total amount; Described organic halogenation salt comprises halogenation quaternary amine, imidazolium halide salt, pyridiniujm, the 30-80% of described organic halogenation salt content station fuse salt total amount; The concentration range of described organic reducing agent in electroplate liquid is 0.005-0.5mol/L, and in described organic reducing agent and described aluminum metal fused salt, the mol ratio of aluminium salt is 0.5-5.0;
In sub-step two: described activating solution also comprises the polymer stabilizer that concentration is not more than 0.01mol/L, described stabilizer comprises, polyvinyl alcohol or polyethylene glycol;
In sub-step four: LiFePO4 covers the 0.1-5.0% that aluminum amount accounts for composite material total amount.
5. a kind of high magnification lithium iron phosphate positive material as claimed in claim 1 and battery pole piece; it is characterized in that; in step 3 described in it; raw material uniform mixing method is solid phase or the fully mixing of solid-liquid machinery; liquid phase substance can adopt ethanol or acetone; incorporation time is 2-50h; wherein Graphene content is between the 0.1-5% of lithium iron phosphate positive material weight; then 550 DEG C of calcining 0.5-5h when there being nitrogen to protect, namely cooling obtains LiFePO4/graphene composite material of the present invention naturally.
6. a kind of high magnification lithium iron phosphate positive material according to claim 1 and battery pole piece, is characterized in that, in the step 3 described in it, grapheme material is that the material with carbon element between 1-20 layer forms by individual layer or the number of plies.
7. high magnification lithium iron phosphate positive material and a battery pole piece, is characterized in that the high magnification lithium iron phosphate positive material that described positive electrode comprises any one in 1-6 and prepares.
8. high magnification lithium iron phosphate positive material and a battery pole piece, is characterized in that the high magnification lithium iron phosphate positive material that described positive plate comprises any one in 1-6 and prepares.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105514432A (en) * | 2016-01-13 | 2016-04-20 | 李震祺 | Lithium iron phosphate composite cathode material and preparation method thereof |
| CN107994219A (en) * | 2017-11-27 | 2018-05-04 | 桑顿新能源科技有限公司 | A kind of metal-doped composite positive pole of graphene coated and preparation method thereof |
| CN111668448A (en) * | 2020-07-14 | 2020-09-15 | 贵州梅岭电源有限公司 | Lithium iron phosphate modified composite material and preparation method thereof |
| CN113517430A (en) * | 2021-09-10 | 2021-10-19 | 蜂巢能源科技有限公司 | Aluminum-coated positive electrode material for inhibiting oxygen release and battery comprising same |
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| CN101562248A (en) * | 2009-06-03 | 2009-10-21 | 龚思源 | Graphite composite lithium ion battery anode material lithium iron phosphate and preparation method thereof |
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| CN101891179A (en) * | 2010-06-23 | 2010-11-24 | 万星光电子(东莞)有限公司 | Preparation method of LiFePO material, lithium ion battery and positive plate thereof |
| CN102306783A (en) * | 2011-09-14 | 2012-01-04 | 哈尔滨工业大学 | Multi-layer graphene/lithium iron phosphate intercalated composite material, preparation method thereof, and lithium ion battery adopting multi-layer grapheme/lithium iron phosphate intercalated composite material as anode material |
| US20140093769A1 (en) * | 2011-05-19 | 2014-04-03 | Northeastern University | Carbon Nanotube-Based Electrode and Rechargeable Battery |
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| CN101562248A (en) * | 2009-06-03 | 2009-10-21 | 龚思源 | Graphite composite lithium ion battery anode material lithium iron phosphate and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105514432A (en) * | 2016-01-13 | 2016-04-20 | 李震祺 | Lithium iron phosphate composite cathode material and preparation method thereof |
| CN107994219A (en) * | 2017-11-27 | 2018-05-04 | 桑顿新能源科技有限公司 | A kind of metal-doped composite positive pole of graphene coated and preparation method thereof |
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| CN111668448A (en) * | 2020-07-14 | 2020-09-15 | 贵州梅岭电源有限公司 | Lithium iron phosphate modified composite material and preparation method thereof |
| CN111668448B (en) * | 2020-07-14 | 2023-02-24 | 贵州梅岭电源有限公司 | Lithium iron phosphate modified composite material and preparation method thereof |
| CN113517430A (en) * | 2021-09-10 | 2021-10-19 | 蜂巢能源科技有限公司 | Aluminum-coated positive electrode material for inhibiting oxygen release and battery comprising same |
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Application publication date: 20151014 |