CN106876633A - A kind of composite diaphragm, lithium battery and preparation method thereof - Google Patents

A kind of composite diaphragm, lithium battery and preparation method thereof Download PDF

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Publication number
CN106876633A
CN106876633A CN201710094521.1A CN201710094521A CN106876633A CN 106876633 A CN106876633 A CN 106876633A CN 201710094521 A CN201710094521 A CN 201710094521A CN 106876633 A CN106876633 A CN 106876633A
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lithium
lithium salt
inorganic
barrier film
salt deposit
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俞浩东
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Beijing WeLion New Energy Technology Co ltd
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Beijing WeLion New Energy Technology Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403—Manufacturing processes of separators, membranes or diaphragms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/058—Construction or manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/44—Fibrous material
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Cell Separators (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention relates to a kind of composite diaphragm, including：Matrix membrane layer；Inorganic lithium salt deposit, the inorganic lithium salt deposit includes indissoluble or is slightly soluble in the inorganic lithium salt of organic electrolyte；Wherein, the inorganic lithium salt deposit is coated in described matrix barrier film layer surface, or, the inorganic lithium salt deposit is embedded in described matrix membrane layer.

Description

A kind of composite diaphragm, lithium battery and preparation method thereof
Technical field
The present invention relates to field of lithium, more particularly to a kind of composite diaphragm, lithium battery and preparation method thereof.
Background technology
With the popularization of electronic product in recent years, as the lithium battery of its power supply, because with light weight, small volume, work Voltage is high, energy density is high, output power, charge efficiency high and the advantages of memory-less effect, is increasingly taken seriously.And In fields such as electric tool, electric automobile and large-scale energy storage, also there is higher and higher wanting to the security and performance of lithium battery Ask.
In the composition of lithium rechargeable battery, positive electrode is one of critical material of battery, is also to determine lithium ion The key factor of battery performance and price.But, due to the electrochemistry of the less stable of current electrolyte, particularly electrolyte Window is narrower, is easily decomposed in high-tension positive electrode surface in charge and discharge process, causes solid electrolyte circle of electrode surface Face (solid electrolyte interface, SEI) film thickness is thickened, and causes the cycle performance of battery poor, performance degradation Seriously.In addition, when high voltage, high current, the surface of another critical component-negative pole of lithium rechargeable battery SEI films easily produce defect, and repairing SEI films can cause battery irreversible capacity；Meanwhile, the SEI films generation of similar patch type is entered One step influences the surface quality of negative pole, increases the inner resistance of battery.
The content of the invention
A kind of composite diaphragm is the embodiment of the invention provides, SEI films stabilization can be made, so as to preferably protect positive negative electricity Pole；And electrolyte can be stablized, prevent electrolyte from being decomposed in positive electrode surface.
On the one hand, a kind of composite diaphragm is the embodiment of the invention provides, including：Matrix membrane layer；Inorganic lithium salt deposit, it is described Inorganic lithium salt deposit includes indissoluble or is slightly soluble in the inorganic lithium salt of organic electrolyte；Wherein, the inorganic lithium salt deposit is coated in described Matrix barrier film layer surface, or, the inorganic lithium salt deposit is embedded in described matrix membrane layer.
In a kind of possible implementation, the inorganic lithium salt include lithium carbonate, lithium metasilicate, lithium metasilicate, lithium nitrate, Lithium acetate, lithium sulfate, lithium sulfite, lithium phosphate, lithium molybdate, the lithium of phosphoric acid hydrogen two, lithium chloride, lithium perchlorate, lithium fluoride, tetrachloro aluminium One or more in sour lithium and lithium metaborate.
In a kind of possible implementation, the inorganic lithium salt deposit also includes ceramic material；The ceramic material includes One or more in aluminum oxide, silica, calcium oxide.
In a kind of possible implementation, the aluminum oxide includes nano aluminium oxide, and the silica includes nanometer Silica；The calcium oxide includes nano calcium oxide.
In a kind of possible implementation, mass ratio >=1 of the inorganic lithium salt and the ceramic material：99.
In a kind of possible implementation, the inorganic lithium salt deposit is coated in described matrix barrier film layer surface and specifically wraps Include：The inorganic lithium salt deposit is coated in the side surface of described matrix membrane layer one or both side surface.
In a kind of possible implementation, the thickness of the inorganic lithium salt deposit is 0.1~50 μm.
In a kind of possible implementation, the thickness of described matrix membrane layer is 1~80 μm.
In a kind of possible implementation, described matrix membrane layer is by polyethylene, polypropylene, microcellular rubber film, polyamides One kind or several in imines, cellulose, Kynoar, ceramics, macromolecule solid electrolyte or inorganic solid electrolyte material Plant composition.
Second aspect, the embodiment of the present invention additionally provides a kind of preparation method of composite diaphragm, comprises the following steps：By Material and the solvent mixing of the inorganic lithium salt deposit on the one hand providing, to obtain mixture；By the mixture be coated on matrix every Film surface, is dried to obtain the composite diaphragm material.
The third aspect, the embodiment of the present invention additionally provides a kind of lithium battery, including positive pole, negative pole, first aspect are provided Barrier film.
Fourth aspect, the embodiment of the present invention additionally provides a kind of preparation method of lithium battery, comprises the following steps：Prepare lithium Anode and negative pole；The barrier film provided using the positive pole, negative pole and first aspect prepares lithium battery, and by chemical conversion.
The composite diaphragm that the embodiment of the invention provides includes indissoluble or is slightly soluble in the inorganic lithium salt of organic electrolyte, in lithium In battery forming process, micro inorganic lithium salt is dissolved in electrolyte so that the SEI films of formation are more stablized, and make in battery During, SEI films are not allowed to be also easy to produce defect, and more preferable protective effect is played to positive and negative electrode；Also, it is micro in electrolyte Inorganic lithium salt can improve the stability of electrolyte, prevent electrolyte from being decomposed on the surface of positive electrode.
Brief description of the drawings
Fig. 1 a are a kind of structural representation of composite diaphragm provided in an embodiment of the present invention；
Fig. 1 c are the structural representation of another composite diaphragm provided in an embodiment of the present invention；
Fig. 1 b are the structural representation of another composite diaphragm provided in an embodiment of the present invention；
Fig. 2 is the performance displaying figure of lithium battery provided in an embodiment of the present invention.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention In accompanying drawing, the technical scheme in the embodiment of the present invention is described, it is clear that described embodiment is a part of the invention Embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making wound The every other embodiment obtained under the premise of the property made work, belongs to the scope of protection of the invention.
The positive electrode for being presently used for lithium ion battery mainly has LiCoO2、LiMn2O4、LiFePO4、LiNi1/3Co1/ 3Mn1/3O2And LiNi0.5Co0.3Mn0.2O2Deng.In recent years, ternary nickel cobalt manganese LiNi0.6Co0.2Mn0.2O2、 LiNi0.8Co0.1Mn0.1O2System and high-tension positive electrode start to cause greatly concern, the product of wherein Ni doping LiNi0.5Mn1.5O4The stable discharging specific capacity of high potential platform and more than 135mAh/g with 4.75V, due to LiNi0.5Mn1.5O4With operating voltage very high, therefore energy density and power density higher can be provided, it is considered to be One kind has application prospect anode material for lithium-ion batteries very much.Additionally, high-tension LiCoO2Positive electrode is also in recent years Study hotspot, its charging voltage can be improved to more than 4.5V.
The stabilization of the stability of positive and negative pole material, particularly positive electrode, and electrolyte stability, to lithium battery Life-span has a major impact.Therefore, a kind of composite diaphragm is the embodiment of the invention provides, SEI films stabilization can be made, so that preferably Protection positive and negative electrode；And electrolyte can be stablized, prevent electrolyte from being decomposed in positive electrode surface；So as to extend lithium battery Service life.
A kind of composite diaphragm is the embodiment of the invention provides, including：Matrix membrane layer 1；Inorganic lithium salt deposit 2；Inorganic lithium salt Layer 2 includes indissoluble or is slightly soluble in the inorganic lithium salt of organic electrolyte.
In one example, as shown in Figure 1a, inorganic lithium salt deposit 2 can be coated in a side surface of matrix membrane layer 1.
It is understood that the side surface that the inorganic lithium salt deposit 2 shown in Fig. 1 a is coated in matrix membrane layer 1 is an act Example explanation, does not constitute and limits.In one example, inorganic lithium salt deposit 2 can be coated in the opposite side table of matrix membrane layer 1 Face.
In one example, as shown in Figure 1 b, inorganic lithium salt deposit 2 can be coated in the both side surface of matrix membrane layer 1.
In one example, as illustrated in figure 1 c, inorganic lithium salt deposit 2 can be embedded in described matrix membrane layer 1.
In one example, inorganic lithium salt can include lithium carbonate, lithium metasilicate, lithium metasilicate, lithium nitrate, lithium acetate, sulphur Sour lithium, lithium sulfite, lithium phosphate, lithium molybdate, the lithium of phosphoric acid hydrogen two, lithium chloride, lithium perchlorate, lithium fluoride, tetrachloro-lithium aluminate and partially One or more in lithium borate.
In one example, inorganic lithium salt deposit 2 also includes ceramic material；Ceramic material includes aluminum oxide, silica, oxygen Change calcium in one or more.
In one example, aluminum oxide includes nano aluminium oxide, and the silica includes nano silicon；The oxygen Changing calcium includes nano calcium oxide.
It should be noted that the inorganic lithium salt and ceramic material in the embodiment of the present invention are the transmission media of lithium ion, Therefore the coating or insertion of inorganic lithium salt deposit 2 will not block transmission channels of the lithium ion in matrix membrane layer 1.Inorganic lithium salt with And ceramic material has chemical stability good and the features such as excellent heat stability, thus inorganic lithium salt and ceramic material coating The security performance of matrix membrane layer 1 can be improved.Although inorganic lithium salt indissoluble is slightly soluble in organic electrolyte, in Organic Electricity Still there is certain solubility in solution liquid, and the inorganic lithium salt for dissolving can stablize electrolyte, and improve electrolyte and electrode Compatibility, improve electrode capacity and cyclical stability；And ceramic material extremely difficult dissolving in the electrolytic solution, it can be ensured that it is inorganic The stability of lithium salts layer 2.Inorganic lithium salt and ceramic material also have non-flammable characteristic, and the inorganic lithium salt of dissolving can also be carried The security of electrolyte high, inorganic lithium salt deposit 2 can improve the security of battery.Additionally, inorganic lithium salt can be potential as one Lithium source, can be continuously replenished battery inside irreversible consumption lithium ion, and then improve battery charge-discharge performance.
In one example, the matter of inorganic lithium salt provided in an embodiment of the present invention and ceramic material in inorganic lithium salt deposit 2 Amount ratio >=1：99.
In one example, the thickness of inorganic lithium salt deposit 2 is 0.1~50 μm.
In one example, the thickness of inorganic lithium salt deposit 2 is 0.1 μm.
In one example, the thickness of inorganic lithium salt deposit 2 is 0.5 μm.
In one example, the thickness of inorganic lithium salt deposit 2 is 1 μm.
In one example, the thickness of inorganic lithium salt deposit 2 is 2 μm.
In one example, the thickness of inorganic lithium salt deposit 2 is 5 μm.
In one example, the thickness of inorganic lithium salt deposit 2 is 10 μm.
In one example, the thickness of inorganic lithium salt deposit 2 is 20 μm.
In one example, the thickness of inorganic lithium salt deposit 2 is 30 μm.
In one example, the thickness of inorganic lithium salt deposit 2 is 49 μm.
In one example, the thickness of described matrix membrane layer 1 is 1~80 μm.
In one example, the thickness of described matrix membrane layer 1 is 1 μm.
In one example, the thickness of described matrix membrane layer 1 is 2 μm.
In one example, the thickness of described matrix membrane layer 1 is 5 μm.
In one example, the thickness of described matrix membrane layer 1 is 10 μm.
In one example, the thickness of described matrix membrane layer 1 is 20 μm.
In one example, the thickness of described matrix membrane layer 1 is 35 μm.
In one example, the thickness of described matrix membrane layer 1 is 60 μm.
In one example, the thickness of described matrix membrane layer 1 is 79 μm.
In one example, matrix membrane layer 1 is by polyethylene, polypropylene, microcellular rubber film, polyimides, cellulose, poly- One or more compositions in vinylidene, ceramics, macromolecule solid electrolyte or inorganic solid electrolyte material.
In one example, ceramic material can be coated in the side surface of matrix membrane layer one, inorganic lithium salt is coated in Another side surface of matrix membrane layer.
The embodiment of the present invention additionally provides a kind of lithium battery, including positive pole, negative pole, functor provided in an embodiment of the present invention Close barrier film.
In one example, the structure of lithium battery can be, positive pole // inorganic lithium salt deposit // matrix membrane layer // negative pole； Or, positive pole // matrix membrane layer // inorganic lithium salt deposit // negative pole.
In one example, the structure of lithium battery can be, positive pole // inorganic lithium salt deposit // matrix membrane layer // inorganic lithium Salt deposit // negative pole.
The embodiment of the present invention additionally provides a kind of preparation method of lithium battery, comprises the following steps：Prepare lithium battery anode And negative pole；Meet barrier film using the positive pole, negative pole and function provided in an embodiment of the present invention.
It is the carbonic acid lithium material and polyvinyladine floride of 100nm by particle size in embodiment 1 (Polyvinylidene Fluoride, PVDF) binding agent and solvent are thoroughly mixed, and to obtain mixture, then use The mixture is carried out single coating by the tape casting in microporous polypropylene membrane, and the thickness of carbonic acid lithium layer is 5 μm, and this is obtained after drying The composite diaphragm for providing is provided.With the composite diaphragm as barrier film, LiNi0.5Mn1.5O4Material is positive active material, according to activity Material is 8.5 with conductive agent, binding agent mass ratio:0.5:1 ratio prepares positive electrode pole piece, thinks lithium metal for negative electrode, Conventional carbonate class mixture is electrolyte, is assembled into button cell.
In embodiment 2, by 1g particle sizes be the carbonic acid lithium material of 100nm, 3g particle sizes be 100nm aluminum oxide Material is thoroughly mixed with PVDF binding agents and solvent, to obtain mixture, is then being gathered the mixture using the tape casting Propylene microcellular film carries out single coating, dries the thickness of rear oxidation aluminium and lithium carbonate material coating for 3 microns, that is, obtain the present invention The composite diaphragm of offer.With the composite diaphragm as barrier film, and positive and negative electrode, the electrolyte that embodiment 1 is provided, it is assembled into button Battery.
In comparative example 1, with microporous polypropylene membrane as barrier film, and positive and negative electrode, the electrolyte that embodiment 1 is provided, It is assembled into button cell.
In comparative example 2, by 2.5g particle sizes for 100nm alumina materials are fully stirred with PVDF binding agents and solvent Mixing is mixed, the mixture is then carried out by single coating in microporous polypropylene membrane using the tape casting, traditional pottery is obtained after drying Porcelain barrier film.With microporous polypropylene membrane as barrier film, and positive and negative electrode, the electrolyte that embodiment 1 is provided, it is assembled into button cell.
Battery performance test is carried out to the battery that embodiment 1, embodiment 2, comparative example 1 and comparative example 2 are provided. Test process can be 2.0V-4.6V for discharge and recharge blanking voltage, and test event includes：Barrier film percent thermal shrinkage test (180 DEG C), Normal temperature volume test (1C charging/1C electric discharges), charge and discharge cycles test (1C charging/1C discharge, and circulate 300 times), low temperature discharge Test (0.3C charging/1C discharge, -10 DEG C).Battery performance test result is as shown in table 1.
The battery performance test Comparative result of table 1
The life test result of battery is as shown in Figure 2, it can be seen that the battery that embodiment 1 and embodiment 2 are provided Life-span is significantly higher than the battery that comparative example 1 and comparative example 2 are provided.
Above-described specific embodiment, has been carried out further to the purpose of the present invention, technical scheme and beneficial effect Describe in detail, should be understood that and the foregoing is only specific embodiment of the invention, be not intended to limit the present invention Protection domain, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc. all should include Within protection scope of the present invention.

Claims (12)

1. a kind of composite diaphragm, it is characterised in that including：
Matrix membrane layer；
Inorganic lithium salt deposit, the inorganic lithium salt deposit includes indissoluble or is slightly soluble in the inorganic lithium salt of organic electrolyte；
Wherein, the inorganic lithium salt deposit is coated in described matrix barrier film layer surface, or, the inorganic lithium salt deposit is embedded in the base Body membrane layer.
2. barrier film according to claim 1, it is characterised in that the inorganic lithium salt includes lithium carbonate, lithium metasilicate, metasilicic acid Lithium, lithium nitrate, lithium acetate, lithium sulfate, lithium sulfite, lithium phosphate, lithium molybdate, the lithium of phosphoric acid hydrogen two, lithium chloride, lithium perchlorate, fluorine Change one or more in lithium, tetrachloro-lithium aluminate and lithium metaborate.
3. barrier film according to claim 1, it is characterised in that the inorganic lithium salt deposit also includes ceramic material；
The ceramic material includes one or more in aluminum oxide, silica, calcium oxide.
4. barrier film according to claim 3, it is characterised in that the aluminum oxide includes nano aluminium oxide, the titanium dioxide Silicon includes nano silicon；The calcium oxide includes nano calcium oxide.
5. barrier film according to claim 3, it is characterised in that the mass ratio of the inorganic lithium salt and the ceramic material >= 1：99.
6. barrier film according to claim 1, it is characterised in that the inorganic lithium salt deposit is coated in described matrix membrane layer table Mask body includes：
The inorganic lithium salt deposit is coated in the side surface of described matrix membrane layer one or both side surface.
7. barrier film according to claim 1, it is characterised in that the thickness of the inorganic lithium salt deposit is 0.1~50 μm.
8. barrier film according to claim 1, it is characterised in that the thickness of described matrix membrane layer is 1~80 μm.
9. barrier film according to claim 1, it is characterised in that described matrix membrane layer is by polyethylene, polypropylene, micropore rubber In glued membrane, polyimides, cellulose, Kynoar, ceramics, macromolecule solid electrolyte or inorganic solid electrolyte material One or more compositions.
10. a kind of preparation method of composite diaphragm, it is characterised in that comprise the following steps：
The material of the inorganic lithium salt deposit described in claim 1-9 and solvent are mixed, to obtain mixture；
The mixture is coated on matrix barrier film layer surface, the composite diaphragm is dried to obtain.
11. a kind of lithium batteries, it is characterised in that including the barrier film described in positive pole, negative pole, claim any one of 1-9.
12. a kind of preparation methods of lithium battery, it is characterised in that comprise the following steps：
Prepare lithium battery anode and negative pole；
Lithium battery is prepared using the barrier film described in the positive pole, negative pole and claim any one of 1-9, and by chemical conversion.
CN201710094521.1A 2017-02-22 2017-02-22 A kind of composite diaphragm, lithium battery and preparation method thereof Pending CN106876633A (en)

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CN108110197A (en) * 2017-12-06 2018-06-01 成都新柯力化工科技有限公司 A kind of lithium battery selective membrane and preparation method thereof
CN108682772A (en) * 2018-03-23 2018-10-19 孙备宽 A kind of lithium ion battery non-porous barrier production method
CN108878751A (en) * 2018-07-03 2018-11-23 宁德卓高新材料科技有限公司 Conductivity ceramics composite diaphragm and solid state battery
CN109004160A (en) * 2018-06-20 2018-12-14 上海恩捷新材料科技股份有限公司 A kind of lithium battery solid electrolyte diaphragm and preparation method thereof
CN109411680A (en) * 2018-10-29 2019-03-01 东莞理工学院 A kind of aramid fiber resin base micropore lithium electric separator and preparation method thereof
CN109428034A (en) * 2017-08-31 2019-03-05 比亚迪股份有限公司 A kind of battery diaphragm and preparation method thereof and lithium ion battery
CN109428037A (en) * 2017-08-31 2019-03-05 比亚迪股份有限公司 A kind of battery diaphragm and preparation method thereof and lithium ion battery
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Application publication date: 20170620