CN104659332B - High-magnification lithium iron phosphate battery positive electrode and manufacturing method thereof - Google Patents
High-magnification lithium iron phosphate battery positive electrode and manufacturing method thereof Download PDFInfo
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- CN104659332B CN104659332B CN201510089370.1A CN201510089370A CN104659332B CN 104659332 B CN104659332 B CN 104659332B CN 201510089370 A CN201510089370 A CN 201510089370A CN 104659332 B CN104659332 B CN 104659332B
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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
- 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
- H01M4/139—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
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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
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Cell Electrode Carriers And Collectors (AREA)
Abstract
The invention discloses a high-magnification lithium iron phosphate battery positive electrode. The high-magnification lithium iron phosphate battery positive electrode is characterized in that a current collector main body of the electrode is made from perforated foamed nickel with a three-dimensional conductive frame structure; the surface of the conductive frame of foamed nickel is coated with an electro-conductive protecting layer; the porosity of the foamed nickel is 50% to 98% and preferably 85% to 95%; the perforation rate of the foamed nickel is larger than 98%; the protecting layer is a pvdf or polyacrylic acid conductive coating which contains 5% to 95% of conductive particles; the conductive particles are one of conductive carbon black, graphite and aluminum powder of which the particle size is smaller than 5 micrometers.
Description
Technical field
The present invention relates to field of lithium ion battery, particularly relate to a kind of high rate lithium iron phosphate cell positive pole and manufacture method thereof.
Technical background
Along with market is for the improving constantly of performance requirement of lithium ion battery, current most of lithium battery manufacturing firm is all to manufacture high-multiplying-power battery electrode by adding more conductive agent and thinner electrode coating thickness in electrode coating, LiFePO 4 material particularly with low conductivity, very thin LiFePO4 coating layer thickness makes the volume of electrode current collecting body take ratio to be greatly increased, reduce the loading of active substance thus reduce the whole volume of battery.Due to electrochemical reaction originally as a kind of three-dimensional mass transport process, understood compared with currently used paper tinsel class such as Copper Foil, aluminium foil by basic electrochemistry general knowledge, use metal foam as the collector of lithium ion battery, significantly improve capacity and the multiplying power discharging property of lithium ion battery.Owing to there is the three-dimensional pore space of porous in foam metal, so that in active substance is filled in this hole rather than be only applied to its surface as paper tinsel body collector.And after in the porous three-dimensional pore space that active substance is filled in foam metal, not only increase filling rate, and due to the three dimensional pore structures of foam metal itself and porous be more beneficial for electric current density be uniformly distributed with electrolyte permeability, be uniformly distributed, such that it is able to improve the active material utilization of lithium ion battery, improve capacity and the multiplying power discharging property of lithium ion battery.Conversely, for metal foil, active substance can only be distributed in the surface of collector.The electric energy changing into chemical energy passes to active substance mainly by collector, active substance near collector and the active substance away from collector are widely different in the distribution of electric energy, the closer to collector, its allocated electric energy is the most uniform while of the most, further away from collector, its allocated electric energy is the fewest.It can be seen that the metal foil that affluxion body in lithium ion batteries uses result in the input of lithium ion battery active substance and output and the inhomogeneities of energy in conversion process, have influence on the raising of active material utilization.The general aluminium of lithium battery anode collector, making three-dimensional conductive collector needs through-hole foam aluminum, as shown in CN200610154100 patent.And the foamed aluminium material being used for battery not yet realizes commercialization, the foam metal of large-scale commercial has foam copper and nickel foam, the lowest being not suitable for of the oxidizing potential of copper is cooked plus plate current-collecting body, and the theoretical oxidation current potential of nickel is about 3.8V, restriction voltage 3.65V close to LiFePO4, but due to the irrational state of nickel surface in actual application, cause its oxidizing potential to reduce, so pure foam nickel be not applied in the LiFePO4 system lithium battery of commercialization.
Summary of the invention
It is an object of the invention to provide a kind of contact internal resistance effectively reducing electrode active material and collector, improve high rate lithium iron phosphate cell positive pole and the manufacture method thereof of the combination property of electrode.
For achieving the above object, the technical solution used in the present invention is:
A kind of high rate lithium iron phosphate cell positive pole, is characterized in that: the collector main body of electrode is to have the through-hole foam nickel of three-dimensional conductive framing structure, and nickel foam conducting matrix grain surface-coated have can the protective layer of electronic conduction.
Described collector main body is the nickel foam with three-dimensional conductive framing structure, and the porosity of nickel foam is 50～98%, preferably 85%～95%, and through-hole rate is more than 98%.
Described protective layer is pvdf or the polyacrylic conductive coating containing 5%～95% conducting particles；Conducting particles is the one that particle diameter is less than in the conductive black of 5um, graphite and aluminium powder.
Comprise the following steps prepared: by containing 5% ~ 95% high-purity aluminium powder of D50 < 5um and the pvdf powder of 5% ~ 95% stir after join in NMP or diethyl ether solution and be sufficiently mixed, it is coated on the through-hole foam nickel of porosity 50% ~ 98% by vertical slurry technique, and by continuous tunnel furnace preliminarily dried at 90 ~ 110 DEG C；Nickel foam after coating is placed in vacuum drying oven and shelves with 150 DEG C ~ 250 DEG C temperature evacuation, make conductive protection coating fully be combined with through-hole foam nickel；With conventional pulping way, LiFePO4, conductive agent and aqueous binders are made electrode slurry again, are coated on the above-mentioned nickel foam collector processed by slurry technique equally, evacuation the most again with continuous twin rollers to roller to design thickness.
Comprise the following steps prepared: aqueous adhesive is fully dissolved and is scattered in deionized water, add the conductive black of the D50=5um of the solid content of 5% ~ 95%, it is sufficiently mixed stirring, it is coated on the through-hole foam nickel of porosity 50 ~ 98% by vertical slurry technique, and by continuous tunnel furnace preliminarily dried at 50 ~ 120 DEG C；Nickel foam after coating is placed in vacuum drying oven and shelves with 90 ~ 120 DEG C of temperature evacuation, make conductive protection coating fully be combined with nickel foam；With current conventional pulping way in industry, LiFePO4, conductive agent and oiliness binding agent pvdf are made electrode slurry again, be coated on the above-mentioned nickel foam collector processed by slurry technique equally, evacuation the most again with continuous twin rollers to roller to design thickness.
Described conductive agent selects one or more in super_P, acetylene black and electrically conductive graphite, and aqueous binders selects one or more in la135, CMC and SBR.
The preparation method of high rate lithium iron phosphate cell positive pole, it is characterized in that: comprise the following steps: by containing 90% high-purity aluminium powder of D50=5um and the pvdf powder of 10% stir with dry method after add nmp solution be sufficiently mixed stirring to viscosity 400cp, on the through-hole foam nickel of the 25ppi being coated on the suitable thickness of porosity about 95% by vertical slurry technique, and by continuous tunnel furnace preliminarily dried at 110 DEG C；Nickel foam after coating is placed in vacuum drying oven and shelves 8h with 200 DEG C of temperature evacuation, make conductive protection coating fully be combined with nickel foam；The LA133 binding agent deionized water of LiFePO4, the conductive black of 3%, the electrically conductive graphite of 1% and 5% of 91% is sufficiently stirred for regulation again to conventional viscosity, i.e. make electrode slurry with convention stir pulping way, it is coated on the above-mentioned nickel foam collector processed by slurry technique equally, after 80 DEG C of preliminarily drieds at evacuation 120 DEG C be dried more than 8h, then with continuous twin rollers to roller to design thickness.
La135 bonding agent is scattered in the deionized water of 90% design flow, add the conductive black of the D50=5um of the solid content of 90%, it is sufficiently mixed stirring and adds deionized water to viscosity about 250cp, on the through-hole foam nickel of the 25ppi being coated on the suitable thickness of porosity about 95% by vertical slurry technique, and by continuous tunnel furnace preliminarily dried at 80 DEG C；Nickel foam after coating is placed in vacuum drying oven and shelves 8h with 120 DEG C of temperature evacuation, make conductive protection coating fully be combined with nickel foam；The pvdf binding agent NMP of LiFePO4, the conductive black of 3%, the electrically conductive graphite of 1% and 5% of 91% is sufficiently stirred for regulation again to regulation viscosity, i.e. make electrode slurry with convention stir pulping way, it is coated on the above-mentioned nickel foam collector processed by slurry technique equally, after 110 DEG C of preliminarily drieds at evacuation 120 DEG C be dried more than 8h, then with continuous twin rollers to roller to design thickness.
For making nickel foam be possibly realized for iron phosphate lithium positive pole collector, the present invention has drawn solution below by lot of experiments.The theoretical oxidation current potential being understood nickel by above-mentioned technical background summary is about 3.8V, restriction voltage 3.65V close to LiFePO4, but due to the irrational state of nickel surface in actual application, its oxidizing potential is caused to reduce, so pure foam nickel be not applied in the LiFePO4 system lithium battery of commercialization.Owing to have employed conductive protection coating nickel coating skeleton surface in the present invention; on the one hand the etch of electrolyte clean state non-ideal to nickel surface has been isolated; simultaneously because bonding agent is preferable with the battery positive electrode active material compatibility in protective coating; effectively reduce the contact internal resistance of electrode active material and collector, improve the combination property of electrode.So a protective coating of good performance is the key factor that foam nickel electrode is applied.And how making conductive protecting layer and nickel foam metal be firmly combined with is the importance of the present invention.Owing in Production Process of Lithium Battery, the dispersant of positive pole LiFePO4 is generally divided into two kinds, a kind of is the oleaginous system with NMP as representative, and representational bonding agent has pvdf etc.；Another kind is water-based system, and i.e. with water as dispersant, representing bonding agent is polyacrylate, such as La135 etc.；Above-mentioned bonding agent all can completely cut off contacting of collector and battery electrolyte solvent, thus protects collector conducting matrix grain.In a preferred embodiment of the invention, nickel foam i.e. uses above-mentioned bonding agent to be combined with nickel foam by conducting particles, is formed and the conductive protecting layer of electrolyte solvent isolation, provides again three-dimensional conductive skeleton simultaneously.The compound mode of above-mentioned bonding agent and nickel foam can select current slurry technique or spraying coating process, preferably slurry technique in industry.Nickel foam and the compound of LiFePO 4 material may be used without above two technique (slurry and spraying).The dispersant of conductive protection coating and LiFePO 4 material should be avoided selecting same type, because this would likely result in the problem that follow-up LiFePO 4 material compound tense conductive protection coating is dissolved and destroys.The composition of certain conductive protection coating and manufacturing process are including but not limited to above-mentioned processing mode.Described above the most preferably illustrates the technical key point of the present invention; any add protective layer on nickel foam surface and be applied to the way of iron phosphate lithium positive pole system and belong to the content of present invention protection, below in conjunction with being embodied as case to describe the innovation of the present invention in detail.
Accompanying drawing explanation
Fig. 1 is the high rate performance figure containing high magnification iron phosphate lithium positive pole battery
Fig. 2 is the cycle performance figure containing high magnification iron phosphate lithium positive pole battery.
Detailed description of the invention
The present invention and result of implementation is specifically introduced below with nonrestrictive embodiment.
Example 1, by containing 90% high-purity aluminium powder of D50=5um and the pvdf powder of 10% stir with dry method after add nmp solution several times and be sufficiently mixed stirring to viscosity about 400cp, on the through-hole foam nickel of the 25ppi being coated on the suitable thickness of porosity about 95% by vertical slurry technique, and by continuous tunnel furnace preliminarily dried at 110 DEG C.Nickel foam after coating is placed in vacuum drying oven and shelves about 8h with 200 DEG C of temperature evacuation, make conductive protection coating fully be combined with nickel foam.The proportioning deionized water of the LA133 binding agent of LiFePO4,3% conductive black, 1% electrically conductive graphite and 5% of 91% is sufficiently stirred for regulation again to conventional viscosity, i.e. make electrode slurry with convention stir pulping way, it is coated on the above-mentioned nickel foam collector processed by slurry technique equally, after 80 DEG C of preliminarily drieds at evacuation 120 DEG C be dried more than 8h, then with continuous twin rollers to roller to design thickness.
Example 2, La135 bonding agent is scattered in the deionized water of 90% design flow, add the conductive black of the D50=5um of the solid content of 90% several times, it is sufficiently mixed stirring and adds deionized water to viscosity about 250cp, on the through-hole foam nickel of the 25ppi being coated on the suitable thickness of porosity about 95% by vertical slurry technique, and by continuous tunnel furnace preliminarily dried at 80 DEG C.Nickel foam after coating is placed in vacuum drying oven and shelves about 8h with 120 DEG C of temperature evacuation, make conductive protection coating fully be combined with nickel foam.Proportioning NMP of the pvdf binding agent of LiFePO4,3% conductive black, 1% electrically conductive graphite and 5% of 91% is sufficiently stirred for regulation again to conventional viscosity, i.e. make electrode slurry with convention stir pulping way, it is coated on the above-mentioned nickel foam collector processed by slurry technique equally, after 110 DEG C of preliminarily drieds at evacuation 120 DEG C be dried more than 8h, then with continuous twin rollers to roller to design thickness.
It is assembled into 1220 button cells by die-cut for the electrode of said method manufacture; the high rate performance and the cycle performance that record are as shown below; it can be seen that 3C discharges up to the 87% of rated capacity; even if the multiplying power discharging with 10C; the capacity of battery still can reach the 78% of rated capacity; discharge curve is the mildest simultaneously; demonstrate the multiplying power property that three-diemsnional electrode is excellent; after circulating 500 times, capability retention reaches 97.4%; only decay 2.6%; foam nickel electrode after visible conductive protective film cladding has good stability, demonstrates excellent using value.
Embodiment described above is only to be described preferred implementation of the present utility model; not design of the present utility model and protection domain are defined; on the premise of without departing from this utility model design concept; various modification that in this area, the technical solution of the utility model is made by ordinary skill technical staff and improvement, all should fall into protection domain of the present utility model.
Claims (1)
1. a high rate lithium iron phosphate cell manufacturing method for anode, is characterized in that: comprise the following steps: by containing 90% D50High-purity aluminium powder of=5 μm and the pvdf powder of 10% add nmp solution and are sufficiently mixed stirring to viscosity 400cP after stirring with dry method, on the through-hole foam nickel of the 25PPI being coated on the suitable thickness that porosity is 95% by vertical slurry technique, and by continuous tunnel furnace preliminarily dried at 110 DEG C；Nickel foam after coating is placed in vacuum drying oven and shelves 8h with 200 DEG C of temperature evacuation, make conductive protection coating fully be combined with nickel foam, the nickel foam collector that formation processed；The LA133 binding agent deionized water of LiFePO4, the conductive black of 3%, the electrically conductive graphite of 1% and 5% of 91% is sufficiently stirred for regulation again to conventional viscosity, i.e. make electrode slurry with convention stir pulping way, it is coated on the above-mentioned nickel foam collector processed by slurry technique equally, after 80 DEG C of preliminarily drieds at evacuation 120 DEG C be dried more than 8h, then with continuous twin rollers to roller to design thickness.
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Families Citing this family (9)
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| CN104909434B (en) * | 2015-06-02 | 2017-08-29 | 吉林大学 | A kind of preparation method of LiFePO4 three-diemsnional electrode |
| US20180034038A1 (en) * | 2015-06-04 | 2018-02-01 | Eoplex Limited | Lead carrier structure and packages formed therefrom without die attach pads |
| CN106025341A (en) * | 2016-06-27 | 2016-10-12 | 国润金华（北京）国际投资管理有限公司 | Lithium-ion power battery capable of being quickly charged and discharged and long in service life |
| CN108511681B (en) * | 2017-12-11 | 2024-04-09 | 吉安市优特利科技有限公司 | Electrode plate, preparation method thereof and battery |
| CN108390041A (en) * | 2018-02-28 | 2018-08-10 | 石河子大学 | Foamed nickel current collector LiFePO4/graphene composite material electrode slice and preparation method thereof |
| CN108808001B (en) * | 2018-06-11 | 2020-11-17 | 安徽正熹标王新能源有限公司 | Multi-element composite conductive layer and preparation method thereof |
| CN111384360B (en) | 2018-12-27 | 2022-02-22 | 财团法人工业技术研究院 | Metal ion battery |
| CN112310406B (en) * | 2020-10-29 | 2022-09-06 | 欣旺达电动汽车电池有限公司 | Flexible current collector and preparation method thereof, pole piece and battery |
| CN112928239A (en) * | 2021-03-31 | 2021-06-08 | 神华准能资源综合开发有限公司 | Preparation method of foam material molded lithium iron phosphate electrode and battery |
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| US5723232A (en) * | 1995-04-24 | 1998-03-03 | Sharp Kabushiki Kaisha | Carbon electrode for nonaqueous secondary battery and nonaqueous battery using the same |
| CN102292851A (en) * | 2009-01-26 | 2011-12-21 | 丰田自动车株式会社 | Positive electrode for lithium secondary battery, and process for producing same |
| CN102332359A (en) * | 2010-06-30 | 2012-01-25 | 大尼克株式会社 | Electrode for electrochemical device and manufacturing approach thereof |
| CN102593424A (en) * | 2012-03-05 | 2012-07-18 | 中南大学 | Method for preparing anode of lithium ion battery |
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- 2015-02-27 CN CN201510089370.1A patent/CN104659332B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5723232A (en) * | 1995-04-24 | 1998-03-03 | Sharp Kabushiki Kaisha | Carbon electrode for nonaqueous secondary battery and nonaqueous battery using the same |
| CN102292851A (en) * | 2009-01-26 | 2011-12-21 | 丰田自动车株式会社 | Positive electrode for lithium secondary battery, and process for producing same |
| CN102332359A (en) * | 2010-06-30 | 2012-01-25 | 大尼克株式会社 | Electrode for electrochemical device and manufacturing approach thereof |
| CN102593424A (en) * | 2012-03-05 | 2012-07-18 | 中南大学 | Method for preparing anode of lithium ion battery |
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