CN106920920A - A kind of composite negative pole pole piece and preparation method thereof, mobile base station lithium ion battery - Google Patents
A kind of composite negative pole pole piece and preparation method thereof, mobile base station lithium ion battery Download PDFInfo
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- CN106920920A CN106920920A CN201710134540.2A CN201710134540A CN106920920A CN 106920920 A CN106920920 A CN 106920920A CN 201710134540 A CN201710134540 A CN 201710134540A CN 106920920 A CN106920920 A CN 106920920A
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- 239000002131 composite material Substances 0.000 title claims abstract description 39
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000007773 negative electrode material Substances 0.000 claims abstract description 58
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000011230 binding agent Substances 0.000 claims description 29
- 239000002002 slurry Substances 0.000 claims description 26
- 239000006258 conductive agent Substances 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 239000011149 active material Substances 0.000 claims description 15
- -1 nitrogen phosphorus compound Chemical class 0.000 claims description 15
- 238000001704 evaporation Methods 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 229910021389 graphene Inorganic materials 0.000 claims description 9
- LLYXJBROWQDVMI-UHFFFAOYSA-N 2-chloro-4-nitrotoluene Chemical group CC1=CC=C([N+]([O-])=O)C=C1Cl LLYXJBROWQDVMI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- DEAAQMGATPGXLJ-UHFFFAOYSA-N [N].[P].[Cl] Chemical compound [N].[P].[Cl] DEAAQMGATPGXLJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000005829 trimerization reaction Methods 0.000 claims description 4
- LSEFCHWGJNHZNT-UHFFFAOYSA-M methyl(triphenyl)phosphanium;bromide Chemical compound [Br-].C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(C)C1=CC=CC=C1 LSEFCHWGJNHZNT-UHFFFAOYSA-M 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 1
- 239000010410 layer Substances 0.000 description 120
- 239000003792 electrolyte Substances 0.000 description 26
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 21
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 20
- 230000004888 barrier function Effects 0.000 description 13
- 238000012360 testing method Methods 0.000 description 11
- 229920000049 Carbon (fiber) Polymers 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- 239000004917 carbon fiber Substances 0.000 description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 229910001290 LiPF6 Inorganic materials 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 229910052493 LiFePO4 Inorganic materials 0.000 description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 6
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000009834 vaporization Methods 0.000 description 5
- 230000008016 vaporization Effects 0.000 description 5
- 238000001467 acupuncture Methods 0.000 description 4
- 239000011889 copper foil Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 239000007770 graphite material Substances 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000010025 steaming Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 239000002918 waste heat Substances 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- LIAWCKFOFPPVGF-UHFFFAOYSA-N 2-ethyladamantane Chemical group C1C(C2)CC3CC1C(CC)C2C3 LIAWCKFOFPPVGF-UHFFFAOYSA-N 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- YAFOVCNAQTZDQB-UHFFFAOYSA-N octyl diphenyl phosphate Chemical compound C=1C=CC=CC=1OP(=O)(OCCCCCCCC)OC1=CC=CC=C1 YAFOVCNAQTZDQB-UHFFFAOYSA-N 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
Classifications
-
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- H01M10/60—Heating or cooling; Temperature control
- H01M10/65—Means for temperature control structurally associated with the cells
- H01M10/654—Means for temperature control structurally associated with the cells located inside the innermost case of the cells, e.g. mandrels, electrodes or electrolytes
-
- 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
-
- 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
-
- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
-
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2220/00—Batteries for particular applications
- H01M2220/10—Batteries in stationary systems, e.g. emergency power source in plant
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of composite negative pole pole piece and preparation method thereof, mobile base station lithium ion battery, belong to technical field of lithium ion.Composite negative pole pole piece in the present invention, including negative current collector, negative electrode active material layer, negative electrode active material layer surface are provided with red phosphorus layer.Red phosphorus layer can give full play to the gram volume of lithium ion battery negative material, improve electrochemical stability.
Description
Technical field
The present invention relates to a kind of composite negative pole pole piece and preparation method thereof, mobile base station lithium ion battery, belong to lithium from
Sub- field of batteries.
Background technology
Lithium ion battery negative material used is mainly graphite material in the market, but graphite material has gram volume
Low defect, easily causes relatively low by the energy density of its obtained lithium ion battery.Composite negative pole pole piece of the prior art
There is lithium ion battery energy density in the negative electrode active material layer set including collector and in collection liquid surface, the composite pole piece
Low defect.Although thering is the silicon-carbon cathode using high power capacity, tin base cathode and its alloy material of cathode to substitute graphite material
Technology, but there is the defects such as cycle performance difference in these novel anode materials, it is difficult to industrialization.In addition, in the prior art
Graphite material also to there is high rate performance low, it is impossible to meet the requirement of high power charging-discharging.
The content of the invention
The purpose of the present invention aims to provide a kind of composite negative pole pole piece, to improve the specific capacity and high rate performance of negative plate.
The purpose of the present invention another purpose is to provide a kind of preparation method of above-mentioned composite negative pole pole piece.
The purpose of the present invention another purpose is to provide a kind of using above-mentioned composite negative pole and the mobile base station lithium of piece
Ion battery.
To achieve these goals, the technical scheme of composite negative pole pole piece of the invention is as follows：
A kind of composite negative pole pole piece, including negative current collector, negative electrode active material layer, above-mentioned negative electrode active material layer surface
It is provided with red phosphorus layer.
Relation between above-mentioned negative current collector and negative electrode active material layer can be such as negative plate of the prior art, negative pole
Collection liquid surface sets negative electrode active material layer.It can also be following structure：Between negative current collector and negative electrode active material layer
It is provided with conductive radiating layer.I.e. negative current collector surface sets conductive radiating layer, and conductive radiator layer surface sets negative electrode active material
Matter layer.
The thickness ratio of above-mentioned conductive radiating layer, negative electrode active material layer and red phosphorus layer is (1~5)：(80~200)：(1~
3)。
Above-mentioned negative electrode active material layer includes：Negative material, conductive agent and binding agent；The negative material, conductive agent
And the mass ratio of binding agent is (90~95)：(1~3)：(2~4).
Above-mentioned negative material is carbon material.Above-mentioned conductive agent is the one kind in CNT, Graphene and carbon fiber.
Above-mentioned conductive radiating layer can use conductive radiating layer of the prior art, and such as application publication number be
The disclosed functional layer set on negative current collector surface of the patent of invention of CN106099041A.Following side can also be used
Case：Above-mentioned conductive radiating layer includes：Nitrogen phosphorus compound, conductive agent and conductive radiator layer binder；The nitrogen phosphorus compound, lead
The mass ratio of electric agent and conductive radiator layer binder is (80~90)：(5~10)：(5~10).Above-mentioned nitrogen phosphorus compound is poly-
One kind in ammonium phosphate, melamine, methyltriphenylphosphonium bromide, four poly- phosphorus nitrogen chlorine, trimerization phosphorus nitrogen chlorine.
Above-mentioned conductive agent is the one kind in CNT, Graphene and carbon fiber.
Above-mentioned carbon fiber is gas-phase growth of carbon fibre.
The preparation method of above-mentioned composite negative pole pole piece, comprises the following steps：
1) active material slurry is coated in negative current collector surface, drying forms negative electrode active material layer；
Or conductive radiator slurry is coated in negative current collector surface, drying forms conductive radiating layer, then in conduction
Radiating layer surface coating active material slurry, drying forms negative electrode active material layer；The conductive radiator slurry is closed by nitrogen phosphatization
Thing, conductive agent, conductive radiator layer binder are well mixed with organic solvent and are obtained；
2) in step 1) obtained by negative electrode active material layer surface evaporation red phosphorus formed red phosphorus layer, obtain final product.
Above-mentioned steps 1) in dispersant be deionized water or redistilled water.
Above-mentioned steps 1) in organic solvent be 1-METHYLPYRROLIDONE, carbon tetrachloride, tetrahydrofuran, N-N- dimethyl methyls
One kind in acid amides, acetone, N-N- dimethylacetylamides, dichloromethane, dichloroethanes, toluene, ethyl acetate, n-hexane.It is excellent
Elect 1-METHYLPYRROLIDONE as.
Above-mentioned steps 1) in negative material, conductive agent and binding agent mass ratio be (90~95)：(1~3)：(2~
4)。
Above-mentioned steps 1) in negative material be carbon material.Preferably graphite.
Above-mentioned steps 1) in conductive agent be CNT, Graphene and carbon fiber in one kind.
Above-mentioned steps 1) in carbon fiber be gas-phase growth of carbon fibre.
Above-mentioned steps 1) in binding agent be LA132.
Above-mentioned steps 1) in the used solvent of mixing be distilled water.Negative material, conductive agent, binding agent and distilled water
Mass ratio is (90~95)：(1~3)：(2~4)：150.
Above-mentioned steps 1) mass ratio of nitrogen phosphorus compound, conductive agent and conductive radiator layer binder in conductive radiator slurry
It is (80~90)：(5~10)：(5~10).
Above-mentioned steps 1) in nitrogen phosphorus compound be APP, melamine, methyltriphenylphosphonium bromide, four poly- phosphorus nitrogen
One kind in chlorine, trimerization phosphorus nitrogen chlorine.
Above-mentioned steps 1) in conductive agent be CNT, Graphene and carbon fiber in one kind.
Above-mentioned steps 1) in carbon fiber for vapor phase growth carbon fiber.
Above-mentioned steps 1) in nitrogen phosphorus compound, conductive agent and conductive radiator layer binder are well mixed solvent used
It is 1-METHYLPYRROLIDONE.
Above-mentioned steps 1) in conductive radiator layer binder is first added to 1-METHYLPYRROLIDONE, be subsequently adding conductive agent and
Nitrogen phosphorus compound.
Above-mentioned steps 1) in nitrogen phosphorus compound, conductive agent, conductive radiator layer binder and 1-METHYLPYRROLIDONE matter
Amount is than being (80~90)：(5~10)：(5~10)：200.
Above-mentioned steps 1) in nitrogen phosphorus compound, conductive agent, conductive radiator layer binder and 1-METHYLPYRROLIDONE by height
Fast dispersion mixing is uniform, obtains the conductive radiator slurry that viscosity is 500~2000mPas.
Above-mentioned conductive radiator layer binder is Kynoar.
Above-mentioned steps 1) in negative current collector be one kind in Copper Foil or copper mesh.When from copper mesh, the porosity of copper mesh
It is 40~60%.Negative pole currect collecting body thickness is 6~15 μm.Thickness is preferably 10 μm.
Above-mentioned steps 1) in conductive radiator slurry is sprayed on by negative current collector surface using gravure application, through drying
Obtain conductive radiating layer.The thickness of conductive radiating layer is 1~5 μm.Thickness is preferably (1~10) μm.
Above-mentioned steps 1) in drying be in 85 DEG C of 6~24h of drying.
Above-mentioned steps 1) in active material slurry is coated in by step 2 by coating machine) in formed conductive radiating layer table
Face, through being dried to obtain negative electrode active material layer.The thickness of negative electrode active material layer is 80~200 μm.Thickness is preferably 100~
150μm。
Above-mentioned steps 1) in drying be in 85 DEG C of drying (6~24) h.
Above-mentioned steps 2) in operation be to carry out in a vacuum furnace, using vaporization condensation process heating red phosphorus, to be deposited in it negative
Pole active material layer surface forms red phosphorus layer.The thickness of red phosphorus layer is 1~3 μm.Thickness is preferably 1~2 μm.
The thickness ratio of above-mentioned negative current collector, conductive radiating layer, negative electrode active material layer and red phosphorus layer is (6~15)：(1
~5)：(80~200)：(1~3).
The temperature of above-mentioned evaporation red phosphorus is (300~400) DEG C, and evaporation time is (10~120) min.
A kind of mobile base station lithium ion battery, including above-mentioned composite negative pole pole piece.
The electrolyte that electrolyte used by above-mentioned mobile base station lithium ion battery is used is LiPF6, the concentration of electrolyte
It is 1~1.5mol/L, solvent is the mixed liquor of ethylene carbonate (EC) and diethyl carbonate (DEC), and the volume ratio of EC and DEC is
1:1。
Barrier film used by above-mentioned mobile base station lithium ion battery is Celgard 2400.
Also include additive in above-mentioned electrolyte, the additive is cresyl diphenyl phosphate, diphenyl octyl phosphate, fluorine
For the one kind in propene carbonate.Additive mass percent in the electrolytic solution is 0.1%~0.5%.
Beneficial effects of the present invention：
Composite negative pole pole piece of the invention is provided with red phosphorus layer, and red phosphorus forms C- with the carbon in negative electrode active material layer
P chemical bonds, improve the embedded quantity of lithium ion in charge and discharge process, so as to improve the energy density of pole piece and its lithium ion battery.
Further, composite negative plate of the invention sets conductive radiating layer on negative current collector surface, in battery temperature
When too high, conductive radiating layer absorbs waste heat, and used as reaction entropy, spontaneously response chemically reacts, on negative current collector surface
Passivation layer is formed with negative electrode active material layer surface.Further, the conductive agent for containing in conductive radiating layer can in time by heat
Amount is passed, and prevents local temperature too high, reduces the thermal runaway of pole piece.Further, the present invention is steam using vapour deposition method
Can be entrained between graphite and graphite red phosphorus and its pole piece by condensation method, and be evenly distributed, can give full play to lithium from
The gram volume of sub- cell negative electrode material；Red phosphorus has compatibility higher with electrolyte lithium hexafluoro phosphate simultaneously, such that it is able to drop
The generation of low side reaction, improves the cycle performance of battery.
Brief description of the drawings
Fig. 1 compares figure for embodiment 1~3 with the lithium ion battery curve of double curvature of comparative example.
Specific embodiment
Embodiment 1
Composite negative pole pole piece in the present embodiment includes being cascading conduction on negative current collector two sides from inside to outside
Heat dissipating layer, negative electrode active material layer and red phosphorus layer.
Negative current collector is 10 μm of Copper Foil.Conductive radiating layer thickness is 3 μm.Negative electrode active material layer is 120 μm.Red phosphorus
Thickness degree is 2 μm.
Conductive radiating layer is uniformly mixed and is bonded together and constitutes by following material：8g binding agents Kynoar, 8g lead
Electric agent CNT, 85g nitrogen phosphorus compound APPs.
Negative electrode active material layer is uniformly mixed and is bonded together and constitutes by following material：94g Delaniums, 2g carbon nanometer
Pipe, 3g LA132 binding agents.
The preparation method of composite negative pole pole piece comprises the following steps in the present embodiment：
1) mixing is equal in 94g Delaniums, 2g CNTs, 3g LA132 binding agents being added into 150g redistilled waters
It is even, active material slurry is obtained；
2) 8g Kynoar is added in 200g 1-METHYLPYRROLIDONEs and is stirred, be subsequently adding 8g carbon nanometer
Pipe and 85g APPs, carry out high speed dispersion, obtain the conductive radiator slurry of 1000mPas；
3) by step 2) obtained by conductive radiator slurry two of negative current collector are sprayed on by gravure application
Surface, 85 DEG C dry 12h, and two sides conductive radiating layer is formed on negative current collector surface；
4) by step 1) in obtained active material slurry be coated in step 3) in the conductive radiator layer surface that is formed, 85
DEG C 12h is dried, negative electrode active material layer is formed in conductive radiator layer surface；
5) in step 4) obtained by two surfaces of negative electrode active material layer be deposited with red phosphorus layer successively, obtain final product；Specifically, steaming
Plating is in a vacuum furnace, its surface for being deposited in negative electrode active material layer is formed red phosphorus using vaporization condensation process heating red phosphorus
Layer, during evaporation, heating-up temperature is 350 DEG C, and evaporation time is 60min.
Mobile base station in the present embodiment includes above-mentioned composite negative pole pole piece, anode pole piece, barrier film, electricity with lithium ion battery
Solution liquid.It is positive electrode that LiFePO4 is selected in anode pole piece.
The electrolyte that electrolyte used by above-mentioned mobile base station lithium ion battery is used is LiPF6, the concentration of electrolyte
It is 1.3mol/L, solvent is the mixed liquor of ethylene carbonate (EC) and diethyl carbonate (DEC), and the volume ratio of EC and DEC is 1:
1.Barrier film is the films of Celgard 2400, prepares 5AH soft-package batteries.
Embodiment 2
Composite negative pole pole piece in the present embodiment includes being cascading conduction on negative current collector two sides from inside to outside
Heat dissipating layer, negative electrode active material layer and red phosphorus layer.
Negative current collector is 10 μm of copper mesh.The porosity of copper mesh is 50%.Conductive radiating layer thickness is 1 μm.Negative pole is lived
Property material layer be 80 μm.Red phosphorus thickness degree is 1 μm.
Conductive radiating layer is made up of the following raw material：5g binding agents Kynoar, 5g conductive agents Graphene, 80g nitrogen phosphatizations
Compound APP.
Negative electrode active material layer is made up of the following raw material：90g Delaniums, 3g Graphenes, 4g LA132 binding agents.
The preparation method of composite negative pole pole piece comprises the following steps in the present embodiment：
1) mixing is equal in 90g Delaniums, 3g Graphenes, 4g LA132 binding agents being added into 150g redistilled waters
It is even, active material slurry is obtained；
2) 5g Kynoar is added in 200g 1-METHYLPYRROLIDONEs and is stirred, be subsequently adding 5g Graphenes
With 80g APPs, high speed dispersion is carried out, obtain the conductive radiator slurry of 500mPas；
3) by step 2) obtained by conductive radiator slurry two of negative current collector are sprayed on by gravure application
Surface, 85 DEG C dry 6h, and two sides conductive radiating layer is formed on negative current collector surface；
4) by step 1) in obtained active material slurry be coated in step 3) in the conductive radiator layer surface that is formed, 85
DEG C 6h is dried, negative electrode active material layer is formed in conductive radiator layer surface；
5) in step 4) obtained by two surfaces of negative electrode active material layer be deposited with red phosphorus layer successively, obtain final product；Specifically, steaming
Plating is in a vacuum furnace, it is deposited in negative electrode active material layer surface using vaporization condensation process heating red phosphorus and form red phosphorus layer,
During evaporation, heating-up temperature is 300 DEG C, and evaporation time is 10min.
Mobile base station in the present embodiment includes above-mentioned composite negative pole pole piece, anode pole piece, barrier film, electricity with lithium ion battery
Solution liquid.It is positive electrode that LiFePO4 is selected in anode pole piece.
The electrolyte that electrolyte used by above-mentioned mobile base station lithium ion battery is used is LiPF6, the concentration of electrolyte
It is 1.3mol/L, solvent is the mixed liquor of ethylene carbonate (EC) and diethyl carbonate (DEC), and the volume ratio of EC and DEC is 1:
1.Barrier film is the films of Celgard 2400, prepares 5AH soft-package batteries.
Embodiment 3
Composite negative pole pole piece in the present embodiment includes being cascading conduction on negative current collector two sides from inside to outside
Heat dissipating layer, negative electrode active material layer and red phosphorus layer.
Negative current collector is 15 μm of Copper Foil.Conductive radiating layer thickness is 5 μm.Negative electrode active material layer is 200 μm.Red phosphorus
Thickness degree is 3 μm.
Conductive radiating layer is made up of the following raw material：10g binding agents Kynoar, 10g conductive agents gas-phase growth of carbon fibre,
90g nitrogen phosphorus compound APPs.
Negative electrode active material layer is made up of the following raw material：95g Delaniums, 1g gas-phase growth of carbon fibre, 2gLA132 are bonded
Agent.
The preparation method of composite negative pole pole piece comprises the following steps in the present embodiment：
1) 95g Delaniums, 1g gas-phase growth of carbon fibre, 2g LA132 binding agents are added in 150g redistilled waters
It is well mixed, active material slurry is obtained；
2) 10g Kynoar is added in 200g 1-METHYLPYRROLIDONEs and is stirred, be subsequently adding 10g gas phases
Grown carbon fiber and 90g APPs, carry out high speed dispersion, obtain the conductive radiator slurry of 2000mPas；
3) by step 2) obtained by conductive radiator slurry two of negative current collector are sprayed on by gravure application
Surface, 85 DEG C dry 24h, and two sides conductive radiating layer is formed on negative current collector surface；
4) by step 1) in obtained active material slurry be coated in step 3) in the conductive radiator layer surface that is formed, 85
DEG C 24h is dried, negative electrode active material layer is formed in conductive radiator layer surface；
5) in step 4) obtained by two surfaces of negative electrode active material layer be deposited with red phosphorus layer successively, obtain final product；Specifically, steaming
Plating is in a vacuum furnace, it is deposited in negative electrode active material layer surface using vaporization condensation process heating red phosphorus and form red phosphorus layer,
During evaporation, heating-up temperature is 400 DEG C, and evaporation time is 120min.
Mobile base station in the present embodiment includes above-mentioned composite negative pole pole piece, anode pole piece, barrier film, electricity with lithium ion battery
Solution liquid.It is positive electrode that LiFePO4 is selected in anode pole piece.
The electrolyte that electrolyte used by above-mentioned mobile base station lithium ion battery is used is LiPF6, the concentration of electrolyte
It is 1.3mol/L, solvent is the mixed liquor of ethylene carbonate (EC) and diethyl carbonate (DEC), and the volume ratio of EC and DEC is 1:
1.Barrier film is the films of Celgard 2400, prepares 5AH soft-package batteries.
Embodiment 4
Composite negative pole pole piece in the present embodiment includes being cascading negative pole on negative current collector two sides from inside to outside
Active material layer and red phosphorus layer.
Negative current collector is 10 μm of Copper Foil.Negative electrode active material layer is 120 μm.Red phosphorus thickness degree is 2 μm.
Negative electrode active material layer is made up of the following raw material：94g Delaniums, 2g CNTs, 3g LA132 binding agents.
The preparation method of composite negative pole pole piece comprises the following steps in the present embodiment：
1) mixing is equal in 94g Delaniums, 2g CNTs, 3g LA132 binding agents being added into 150g redistilled waters
It is even, active material slurry is obtained；
2) by step 1) in obtained active material slurry the two of negative current collector is sprayed on by gravure application
Individual surface, 85 DEG C dry 12h, and negative electrode active material layer is formed in conductive radiator layer surface；
3) in step 2) obtained by two surfaces of negative electrode active material layer be deposited with red phosphorus layer successively, obtain final product；Specifically, steaming
Plating is in a vacuum furnace, it is deposited in negative electrode active material layer surface using vaporization condensation process heating red phosphorus and form red phosphorus layer,
During evaporation, heating-up temperature is 350 DEG C, and evaporation time is 60min.
Mobile base station in the present embodiment includes above-mentioned composite negative pole pole piece, anode pole piece, barrier film, electricity with lithium ion battery
Solution liquid.It is positive electrode that LiFePO4 is selected in anode pole piece.
The electrolyte that electrolyte used by above-mentioned mobile base station lithium ion battery is used is LiPF6, the concentration of electrolyte
It is 1.3mol/L, solvent is the mixed liquor of ethylene carbonate (EC) and diethyl carbonate (DEC), and the volume ratio of EC and DEC is 1:
1.Barrier film is the films of Celgard 2400, prepares 5AH soft-package batteries.
Comparative example 1
Cathode pole piece in comparative example 1 includes negative current collector and negative electrode active material layer.The thickness of negative electrode active material layer
Spend is 120 μm.
Negative current collector and negative electrode active material layer material composition and content in comparative example 1 is identical with embodiment 1,
The preparation method of negative current collector and negative electrode active material layer in comparative example 2 is identical with the preparation method of each layer in embodiment 1.
Lithium ion battery in comparative example 1 includes above-mentioned composite negative pole pole piece, anode pole piece, barrier film, electrolyte.Positive pole pole
It is positive electrode that LiFePO4 is selected in piece.
The electrolyte that electrolyte used by above-mentioned lithium ion battery is used is LiPF6, the concentration of electrolyte is 1.3mol/L,
Solvent is the mixed liquor of ethylene carbonate (EC) and diethyl carbonate (DEC), and the volume ratio of EC and DEC is 1:1.Barrier film is
The films of Celgard 2400, prepare 5AH soft-package batteries.
Comparative example 2
Cathode pole piece in comparative example 2 includes negative current collector, conductive radiating layer and negative electrode active material layer.Conductive radiator
Thickness degree is 3 μm.The thickness of negative electrode active material layer is 120 μm.
Negative current collector, conductive radiating layer and negative electrode active material layer material composition and content and implementation in comparative example 2
It is identical in example 1, preparation method and the implementation of negative current collector, conductive radiating layer and negative electrode active material layer in comparative example 2
The preparation method of each layer is identical in example 1.
Lithium ion battery in comparative example 2 includes above-mentioned composite negative pole pole piece, anode pole piece, barrier film, electrolyte.Positive pole pole
It is positive electrode that LiFePO4 is selected in piece.
The electrolyte that electrolyte used by above-mentioned lithium ion battery is used is LiPF6, the concentration of electrolyte is 1.3mol/L,
Solvent is the mixed liquor of ethylene carbonate (EC) and diethyl carbonate (DEC), and the volume ratio of EC and DEC is 1:1.Barrier film is
The films of Celgard 2400, prepare 5AH soft-package batteries.
Test example
1) DC internal resistance test and acupuncture short-circuit test：
DC internal resistance is tested：Lithium ion battery prepared by Example 1~4 and comparative example, method of testing：Reference
《Freedom CAR battery testing handbooks》.
Acupuncture short-circuit test：Lithium ion battery prepared by Example 1~4 and comparative example, method of testing：With reference to UL2054
Safety standard testing standard.
DC internal resistance is tested and the result and Performance comparision of acupuncture short-circuit test see the table below 1.
Lithium ion battery direct-current internal resistance test and the result and property of acupuncture short-circuit test prepared by the embodiment of table 1 and comparative example
Can compare
| Project | DC internal resistance (m Ω) | Safety loading coefficient |
| Embodiment 1 | 4.17 | 9/10 |
| Embodiment 2 | 4.21 | 8/10 |
| Embodiment 3 | 4.23 | 8/10 |
| Embodiment 4 | 4.97 | 7/10 |
| Comparative example 1 | 6.85 | 4/10 |
| Comparative example 2 | 6.97 | 3/10 |
As can be seen from Table 1, the security performance of embodiment is substantially better than comparative example, and reason is：When battery temperature is raised,
The waste heat of battery can be quickly absorbed, used as reaction entropy, spontaneously response chemical reaction, protects in graphite surface Surface Creation
Sheath, the continuation that on the one hand can effectively suppress the temperature of battery is raised, and side reaction occurs and avoids height under reducing hot conditions
SEI mass reduction under the conditions of temperature, it is to avoid the thermal runaway of material occurs；On the other hand graphite active layer can be passivated, from root
The potential safety hazard of battery is controlled, the security of battery is ensured.
2) energy density and its loop test
, with rate of charge as 1.0C, discharge-rate is 1.0C to lithium ion battery prepared by Example 1~4 and comparative example,
Charging/discharging voltage scope 2.5V-3.65V, temperature is 25 ± 3 DEG C of 500 cycle performances for testing its lithium ion battery.While with
Rate of charge is that 0.3C and discharge-rate calculate discharge capacity and mean voltage, and weighs battery weight, is calculated afterwards
The mass energy density of lithium ion battery.
The embodiment of table 2 compares with the chemical property of comparative example
By Fig. 1 and table 2 as can be seen that the cycle performance and energy density of embodiment are substantially better than comparative example, its reason
It is that red phosphorus is deposited on its cathode pole piece surface using vapour deposition method, forms C-P chemical bonds, lithium ion is embedding in raising charge and discharge process
Enter amount, so as to improve the energy density of pole piece and its lithium ion battery；Red phosphorus can be entrained in by graphite using vapour deposition method simultaneously
Between graphite and its pole piece, and it is evenly distributed, the gram volume of lithium ion battery negative material can be given full play to；Simultaneously
Red phosphorus has compatibility higher with electrolyte lithium hexafluoro phosphate, and its cyclicity is improved such that it is able to reduce side reaction
Energy.
Claims (9)
1. a kind of composite negative pole pole piece, including negative current collector, negative electrode active material layer, it is characterised in that the negative electrode active
Material layer surface is provided with red phosphorus layer.
2. composite negative pole pole piece as claimed in claim 1, it is characterised in that the negative current collector and negative electrode active material layer
Between be provided with conductive radiating layer, the conductive radiating layer includes nitrogen phosphorus compound, conductive agent and conductive radiator layer binder；
The mass ratio of the nitrogen phosphorus compound, conductive agent and conductive radiator layer binder is (80~90)：(5~10)：(5~10).
3. composite negative pole pole piece as claimed in claim 2, it is characterised in that the nitrogen phosphorus compound is APP, trimerization
One kind in cyanamide, methyltriphenylphosphonium bromide, four poly- phosphorus nitrogen chlorine, trimerization phosphorus nitrogen chlorine.
4. composite negative pole pole piece as claimed in claim 2, it is characterised in that the conductive agent is CNT, Graphene, carbon
One kind in fiber.
5. composite negative pole pole piece as claimed in claim 2, it is characterised in that the conductive radiating layer, negative electrode active material layer
It is (1~5) with the thickness ratio of red phosphorus layer：(80~200)：(1~3).
6. composite negative pole pole piece as claimed in claim 1, it is characterised in that the negative electrode active material layer includes negative pole material
Material, conductive agent and binding agent；The mass ratio of the negative material, conductive agent and binding agent is (90~95)：(1~3)：(2
~4).
7. a kind of preparation method of composite negative pole pole piece as claimed in claim 1, it is characterised in that comprise the following steps：
1) active material slurry is coated in negative current collector surface, drying forms negative electrode active material layer；
Or conductive radiator slurry is coated in negative current collector surface, drying forms conductive radiating layer, then in conductive radiator
Layer surface coats active material slurry, and drying forms negative electrode active material layer；The conductive radiator slurry by nitrogen phosphorus compound, lead
Electric agent, conductive radiator layer binder are well mixed with organic solvent and are obtained；
2) in step 1) obtained by negative electrode active material layer surface evaporation red phosphorus formed red phosphorus layer, obtain final product.
8. the preparation method of composite negative pole pole piece as claimed in claim 7, it is characterised in that the temperature of evaporation red phosphorus is 300
~400 DEG C, evaporation time is 10~120min.
9. a kind of mobile base station lithium ion battery, it is characterised in that the mobile base station includes such as right with lithium ion battery
It is required that the composite negative pole pole piece described in 1.
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