CN106025233B - A kind of preparation method of lithium ion battery - Google Patents
A kind of preparation method of lithium ion battery Download PDFInfo
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- CN106025233B CN106025233B CN201610563366.9A CN201610563366A CN106025233B CN 106025233 B CN106025233 B CN 106025233B CN 201610563366 A CN201610563366 A CN 201610563366A CN 106025233 B CN106025233 B CN 106025233B
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- lithium ion
- ion battery
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 102
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical class [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003792 electrolyte Substances 0.000 claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 19
- 239000002608 ionic liquid Substances 0.000 claims abstract description 15
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 15
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 15
- 239000003063 flame retardant Substances 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000007774 positive electrode material Substances 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 26
- 229910052744 lithium Inorganic materials 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 18
- 239000011572 manganese Substances 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 16
- -1 phosphate ester Chemical class 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 11
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 11
- 238000002955 isolation Methods 0.000 claims description 11
- 229910052748 manganese Inorganic materials 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 239000006183 anode active material Substances 0.000 claims description 8
- 239000006258 conductive agent Substances 0.000 claims description 8
- 238000000975 co-precipitation Methods 0.000 claims description 6
- 239000011883 electrode binding agent Substances 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical class CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 5
- 229910001290 LiPF6 Inorganic materials 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 239000003660 carbonate based solvent Substances 0.000 claims description 4
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 4
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- GVIJJXMXTUZIOD-UHFFFAOYSA-N thianthrene Chemical compound C1=CC=C2SC3=CC=CC=C3SC2=C1 GVIJJXMXTUZIOD-UHFFFAOYSA-N 0.000 claims description 4
- DWYMPOCYEZONEA-UHFFFAOYSA-L fluoridophosphate Chemical compound [O-]P([O-])(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-L 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000007086 side reaction Methods 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- 239000002202 Polyethylene glycol Substances 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 229920001223 polyethylene glycol Polymers 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 4
- 229920000049 Carbon (fiber) Polymers 0.000 description 4
- 239000000908 ammonium hydroxide Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000004917 carbon fiber Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 244000248349 Citrus limon Species 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical class N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 2
- 229920000914 Metallic fiber Polymers 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- PRORZGWHZXZQMV-UHFFFAOYSA-N azane;nitric acid Chemical compound N.O[N+]([O-])=O PRORZGWHZXZQMV-UHFFFAOYSA-N 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 125000004386 diacrylate group Chemical group 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229920002313 fluoropolymer Polymers 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 229910021397 glassy carbon Inorganic materials 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 150000002466 imines Chemical class 0.000 description 2
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical group [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- 229940071125 manganese acetate Drugs 0.000 description 2
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical group [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical group O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- BKURQRFQHBUAHF-UHFFFAOYSA-N ethyl(tetrafluoro)-$l^{5}-phosphane Chemical compound CCP(F)(F)(F)F BKURQRFQHBUAHF-UHFFFAOYSA-N 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- ZAUUZASCMSWKGX-UHFFFAOYSA-N manganese nickel Chemical compound [Mn].[Ni] ZAUUZASCMSWKGX-UHFFFAOYSA-N 0.000 description 1
- RHFUXPCCELGMFC-UHFFFAOYSA-N n-(6-cyano-3-hydroxy-2,2-dimethyl-3,4-dihydrochromen-4-yl)-n-phenylmethoxyacetamide Chemical compound OC1C(C)(C)OC2=CC=C(C#N)C=C2C1N(C(=O)C)OCC1=CC=CC=C1 RHFUXPCCELGMFC-UHFFFAOYSA-N 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000011787 zinc oxide Substances 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
-
- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/56—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation methods of lithium ion battery, the lithium ion battery is using modified nickel ion doped as positive electrode active materials, chemical stability is good, capacity is high, it can be good at arranging in pairs or groups with aqueous electrolyte, inhibit the reaction rate of side reaction, the lithium ion battery uses ionic liquid, additive, organic solvent, the electrolyte of fire retardant and lithium salts composition, use temperature range narrow disadvantage when overcoming conventional organic solvents as lithium-ion battery electrolytes, both there is excellent anti-overcharge performance, other chemical properties of battery are not influenced again, in applied at elevated temperature, electrochemical properties are stablized, good flame resistance, average for the first time charged efficiency of the preparation method by lithium ion battery under different discharge-rates, the charging capacity of lithium ion battery is to obtain discharge capacity of the lithium ion battery under different discharge-rates, to handle The chemical conversion of lithium ion battery, partial volume time greatly reduce.
Description
Technical field
The present invention relates to the preparation methods of battery, and in particular to a kind of preparation method of lithium ion battery.
Background technique
Lithium ion battery is the green high-capacity environment-protecting battery occurred the 1990s, has energy density height, environment friend
It gets well, memory-less effect, have extended cycle life, the prominent advantage such as self discharge is few, being not only mobile phone, laptop, portable
The ideal source of the electronic devices miniaturization such as formula measuring instrument, and be currently under industrialization electric car, it is electronic from
The energy-storage battery for power source and the wind energy, solar energy of driving a vehicle.The update of electronic product at this stage and electric car it is fast
Exhibition is hailed, more stringent requirements are proposed to the energy density of lithium ion battery.
With the continuous expansion in lithium ion battery market, safety issue be lithium ion battery market innovation it is important before
It mentions.Carrier of the organic electrolyte as ion motion in lithium ion battery adds mainly for lithium ion secondary battery in high temperature
Hot, excessive charge and discharge, short circuit and high current release a large amount of heat in the case where working long hours, these heats become inflammable electricity
The security risk for solving liquid may cause the problems such as catastrophic thermal breakdown (thermal runaway), burning occur for battery, or even battery caused to be sent out
Raw explosion.
Positive electrode is the important component of lithium ion battery, accounts for the 30%-40% or so of entire battery totle drilling cost.Cause
This, improves the performance of positive electrode and the development reduced its cost for lithium ion battery is extremely crucial.Wherein, it is lithium-rich manganese-based just
Pole material Li1+x(MnM)1-xO2(x≤1/3 M=Ni, Co, Cr, Fe......, 0 <) (is greater than with its high specific discharge capacity
250mAhg-1) it is considered as one of candidate positive electrode of current high energy density cells.
Unmodified nickel ion doped material haves the defects that some to be difficult to overcome.Such as in charge and discharge process, due to nickel manganese
Sour lithium operating voltage is higher, and with electrolyte side reaction can occur for electrode surface, consumes Li+, cause effective lithium to reduce, capacity attenuation
Seriously.In addition, in nickel ion doped crystal, often there is Mn3+, the Mn of material surface3+Easily disproportionation generates Mn2+And it is dissolved in electrolysis
In liquid, material surface is caused to be destroyed, ultimately causes material capacity decaying.
Studies have shown that can effectively inhibit material surface by introducing one layer of stable shell on nickel ion doped surface
Side reaction improves the structural stability of material.Currently, the most common mode for constructing stable shell is exactly coating modification.Wherein,
The substances such as zinc oxide, aluminium oxide, aluminum fluoride are most commonly seen coverings.But the lithium ionic mobility of these substances and electricity
Electron conductivity is often bad, and the high rate performance of material often becomes negatively affected.Moreover, the shell constructed by the method coated
Layer, since shell is entirely different with inner core, due to volume change when charge and discharge, the phenomenon that being easy to appear removing.
It is then desired to find more reasonable means to construct core-shell structure.
Summary of the invention
The present invention provides a kind of preparation method of lithium ion battery, and the lithium ion battery is using modified nickel ion doped as just
Pole active material, chemical stability is good, and capacity is high, can be good at arranging in pairs or groups with aqueous electrolyte, inhibits the reaction speed of side reaction
Rate, the electrolyte which is formed using ionic liquid, additive, organic solvent, fire retardant and lithium salts, overcomes biography
Use temperature range narrow disadvantage when uniting organic solvent as lithium-ion battery electrolytes, both has excellent anti-overcharge performance,
The other chemical properties for not influencing battery again, in applied at elevated temperature, electrochemical properties are stablized, good flame resistance, and the preparation method is logical
Averagely for the first time charged efficiency, the charging capacity of lithium ion battery of the lithium ion battery under different discharge-rates are crossed to obtain lithium
Discharge capacity of the ion battery under different discharge-rates, so that the chemical conversion of lithium ion battery, partial volume time are greatly reduced.
To achieve the goals above, the present invention provides a kind of preparation method of lithium ion battery, which includes such as
Lower step:
(1) lithium battery anode active material is prepared
Using citrate coprecipitation-spray drying-high-temperature roasting method, the chemical formula of the positive electrode active materials is
Li2-x-y-zMnxNiyPbzO2, wherein x=0.31-0.35, y=0.25-0.28, z=0.02-0.04；
(2) electrolyte is prepared
The electrolyte is made of ionic liquid, additive, organic solvent, fire retardant and lithium salts, is specifically included:
55-80 parts of ionic liquid, 10-50 parts of thianthrene, 15-60 parts of carbonate-based solvent, 2-6 parts of phosphate ester flame retardants,
The concentration of lithium salts is 0.75mol/L-1mol/L in the electrolyte；
(3) lithium ion cell positive is prepared
Utilize the lithium battery anode active material of above-mentioned steps (1) preparation, positive conductive agent, positive electrode binder and anode collection
Fluid preparation lithium ion cell positive；
(4) lithium battery early-products are formed
Anode is made in step (3), isolation film and cathode wind and to form core, wherein the isolation film is by the anode
It is isolated with the cathode；
Electrolyte is injected into the core；
Second pressure coefficient is calculated according to the first pressure coefficient in the first pressure coefficient for obtaining the core,
The second pressure coefficient is less than the first pressure coefficient；And
Baking processing is carried out to the core, and pressure is applied to the core using the second pressure coefficient, is obtained
Lithium ion battery early-products.
(5) forming and capacity dividing obtains final lithium ion battery product.
Preferably, in the step (1), specifically comprise the following steps:
(11) corresponding raw material is weighed by the molar ratio of chemical formula, by the solution containing manganese source, nickel source and lead source and contains lemon
The solution of acid ion carries out mixing co-precipitation, and controls mixing condition, obtains precursor pulp；
(12) precursor pulp obtained by step (11) is spray-dried, obtains presoma powder；
(13) presoma powder, lithium source obtained by step (12) are mixed, and mixture high-temperature roasting is obtained positive-active
Material.
Preferably, in the step (2), ionic liquid EMI-BF4(- four fluorophosphoric acid of -3 methylimidazole of 1- ethyl
Salt), EMI-BF6(- 3 methylimidazoles of 1- ethyl-hexafluorophosphate), EMI-TFSI (- two (fluoroform of -3 methylimidazole of 1- ethyl
At least one of base sulphonyl) inferior amine salt), lithium salts LiPF6、LiBF4、LiClO4At least one of.
Preferably, in step (4), the method for the first pressure coefficient for obtaining the core are as follows: to multiple described
Core applies pressure, obtains the maximum pressure coefficient that multiple core are able to bear, and calculates multiple maximum pressure coefficients
Average value, the ratio of the average value of the first pressure coefficient and the maximum pressure coefficient is 80%-100%, described the
The ratio of two pressure coefficients and the first pressure coefficient is 70%-90%.
Preferably, in step (4), the operation of the baking processing are as follows: the core is placed in high-temperature clamp, 70
Baking processing is carried out under conditions of DEG C -90 DEG C.
Preferably, include following sub-step in step (5):
(51) lithium ion battery early-products n are taken, n is the positive integer greater than 4；It is small that the n lithium ion battery is shelved into m
When；
(52) it is charged with the electric current of small flow to it, charging time 2-3h；
(53) lithium ion battery after charging is shelved at a certain temperature, aging；
(54) lithium ion battery is charged to voltage rating by the electric current of flow in, turns constant-voltage charge, until after cut-off current,
Terminate charging；
(55) lithium ion battery after charging is shelved 5-30 minutes；
(56) lithium ion battery is discharged to blanking voltage with different discharge-rates respectively；Held with discharge capacity divided by charging
Amount, obtains for the first time charged efficiency of each lithium ion battery under the discharge-rate, to obtain lithium ion battery in the electric discharge
Average efficiency charged for the first time under multiplying power；
(57) then the lithium ion battery of mass production infuse after liquid by step (51)-(56) progress operation, and general
The lithium ion battery of mass production after charging is discharged to certain voltage, makes at the lithium ion battery produced in enormous quantities
In half state-of-charge；Capacity=mass production lithium ion of the lithium ion battery of mass production under different discharge-rates
Average efficiency charged for the first time under battery charge capacity × difference discharge-rate, forming and capacity dividing terminate.
Preferably, described m hours is 20-40h, and the low current is 0.1C-0.25C, and the middle electric current is 0.25-
0.5C, the discharge-rate are 0.5C-0.8C.
The present invention has the advantage that (1) preparation method of lithium ion battery is living as anode using modified nickel ion doped
Property material, chemical stability is good, and capacity is high, can be good at arranging in pairs or groups with aqueous electrolyte, inhibits the reaction rate of side reaction；
(2) electrolyte that the preparation method of lithium ion battery is formed using ionic liquid, additive, organic solvent, fire retardant and lithium salts,
Use temperature range narrow disadvantage when overcoming conventional organic solvents as lithium-ion battery electrolytes both has excellent anti-mistake
Performance is filled, and does not influence other chemical properties of battery, electrochemical properties are stablized in applied at elevated temperature, good flame resistance；(3) should
Average for the first time charged efficiency, the charging capacity of lithium ion battery of the preparation method by lithium ion battery under different discharge-rates
To obtain discharge capacity of the lithium ion battery under different discharge-rates, thus chemical conversion, partial volume time lithium ion battery
Greatly reduce.
Specific embodiment
Embodiment one
Prepare lithium battery anode active material
Using citrate coprecipitation-spray drying-high-temperature roasting method, the chemical formula of the positive electrode active materials is
Li1.42Mn0.31Ni0.25Pb0.02O2, wherein x=0.31-0.35, y=0.25-0.28, z=0.02-0.04.
Corresponding raw material is weighed by the molar ratio of chemical formula, by the solution containing manganese source, nickel source and lead source and contains citrate
The solution of ion carries out mixing co-precipitation, and controls mixing condition, obtains precursor pulp；Preferably, addition ammonia spirit into
Row co-precipitation；The mixing condition controlled are as follows: mixing speed 500rpm, reaction temperature are room temperature to 85 DEG C, the reaction time >=
4h.Preferably, the concentration of the solution containing citrate ion is 0.5mol/L；Nickel in the solution of nickel source, manganese source and lead source,
The total concentration of manganese and lead ion is 0.5mol/L, and the solid content of the precursor pulp is 50g/L, air inlet temperature when spray drying
Degree is 150 DEG C；The recyclable benefit of the ammonium acetate class or nitric acid ammonium material that gas discharged in spray-drying process condenses
With.
Gained precursor pulp is spray-dried, presoma powder is obtained；Low temperature is carried out to gained presoma powder
The step of heat treatment.The condition of the Low Temperature Heat Treatment are as follows: in 100 DEG C of heat preservation 5h, then be warming up to 300 DEG C of heat preservation 5h.
Gained presoma powder will be walked, lithium source mixes, and mixture high-temperature roasting is obtained positive electrode active materials.Mixture
High-temperature roasting condition are as follows: maturing temperature is 850 DEG C, soaking time 10h.
Wherein, the manganese source is manganese acetate and/or manganese nitrate, and the nickel source is nickel nitrate, and the lead source is plumbi nitras；Institute
Stating the solution containing citrate ion is citric acid solution, the mixed solution of citric acid and ammonium hydroxide, ammonium citrate solution or lemon
At least one of sour ammonium and the mixed solution of ammonium hydroxide；The lithium source is lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate and fluorine
Change at least one of lithium.
Prepare electrolyte
The electrolyte is made of ionic liquid, additive, organic solvent, fire retardant and lithium salts, is specifically included:
55 parts of ionic liquid, 10 parts of thianthrene, 15 parts of carbonate-based solvent, 2 parts of phosphate ester flame retardants, in the electrolyte
The concentration of lithium salts is 0.75mol/L-1mol/L；Preferably, ionic liquid EMI-BF4(- 3 methylimidazoles of 1- ethyl-tetrafluoro phosphorus
Hydrochlorate), EMI-BF6(- 3 methylimidazoles of 1- ethyl-hexafluorophosphate), EMI-TFSI (- two (trifluoro of -3 methylimidazole of 1- ethyl
At least one of sulfonyloxy methyl) inferior amine salt), lithium salts LiPF6、LiBF4、LiClO4At least one of.
Prepare lithium ion cell positive
Lithium battery anode active material, positive conductive agent, positive electrode binder and the anode collection prepared using above-mentioned steps
Body prepares lithium ion cell positive；Preferably, positive conductive agent is selected from conducting polymer, conductive oxide, conductivity ceramics, activity
One of carbon, graphene, carbon black, graphite, carbon fiber, metallic fiber, metal powder and sheet metal are a variety of, anode
The mass percent that conductive agent accounts for positive electrode is 2%.
Preferably, the positive electrode binder can be selected from polyethylene oxide, polypropylene oxide, polyacrylonitrile, polyamides
Imines, polyester, polyethers, fluorinated polymer, poly- divinyl polyethylene glycol, polyethyleneglycol diacrylate, polyethylene glycol diformazan
The mixture and derivative of one of base acrylic acid or above-mentioned polymer.
Preferably, the material of plus plate current-collecting body is selected from vitreous carbon, graphite foil, graphite flake, foamy carbon, carbon felt, carbon cloth, carbon fiber
One of dimension.
Form lithium battery early-products
Obtained anode, isolation film and cathode are wound and to form core, wherein the isolation film bears the anode with described
Pole isolation；Electrolyte is injected into the core；The first pressure coefficient for obtaining the core, according to the first pressure coefficient
Second pressure coefficient is calculated, the second pressure coefficient is less than the first pressure coefficient；And the core is carried out
Baking processing, and pressure is applied to the core using the second pressure coefficient, obtain lithium ion battery early-products.
The method of the first pressure coefficient for obtaining the core are as follows: apply pressure to multiple core, obtain more
The maximum pressure coefficient that a core is able to bear calculates the average value of multiple maximum pressure coefficients, first pressure
The ratio of the average value of force coefficient and the maximum pressure coefficient is 80%, the second pressure coefficient and the first pressure system
Several ratio is 70%.It is described baking processing operation are as follows: the core is placed in high-temperature clamp, under conditions of 70 DEG C into
Row baking processing.
Forming and capacity dividing obtains final lithium ion battery product
Lithium ion battery early-products n are taken, n is the positive integer greater than 4；The n lithium ion battery is shelved m hours；
It is charged with the electric current of small flow to it, charging time 2h；Described m hours is 20h, and the low current is
0.1C, the middle electric current are 0.25C, and the discharge-rate is 0.5C.
Lithium ion battery after charging is shelved at a certain temperature, aging；
Lithium ion battery is charged into voltage rating with the electric current of middle flow, turns constant-voltage charge, until terminating after cut-off current
Charging；
Lithium ion battery after charging is shelved 5 minutes；
Lithium ion battery is discharged to blanking voltage with different discharge-rates respectively；With discharge capacity divided by charging capacity,
For the first time charged efficiency of each lithium ion battery under the discharge-rate is obtained, to obtain lithium ion battery in the discharge-rate
Under average efficiency charged for the first time；
Then the lithium ion battery of mass production has been infused and has carried out operation by above-mentioned steps after liquid, and will be after charging
The lithium ion battery of mass production be discharged to certain voltage, so that the lithium ion battery produced in enormous quantities is in half charged shape
State；Capacity=mass production lithium ion battery of the lithium ion battery of mass production under different discharge-rates, which charges, to be held
Average efficiency charged for the first time under amount × difference discharge-rate, forming and capacity dividing terminate.
Embodiment two
Prepare lithium battery anode active material
Using citrate coprecipitation-spray drying-high-temperature roasting method, the chemical formula of the positive electrode active materials is
Li1.33Mn0.35Ni0.28Pb0.04O2。
Corresponding raw material is weighed by the molar ratio of chemical formula, by the solution containing manganese source, nickel source and lead source and contains citrate
The solution of ion carries out mixing co-precipitation, and controls mixing condition, obtains precursor pulp；Preferably, addition ammonia spirit into
Row co-precipitation；The mixing condition controlled are as follows: mixing speed 1000rpm, reaction temperature are room temperature to 85 DEG C, the reaction time >=
4h.Preferably, the concentration of the solution containing citrate ion is 1.5mol/L；Nickel in the solution of nickel source, manganese source and lead source,
The total concentration of manganese and lead ion is 1mol/L, and the solid content of the precursor pulp is 150g/L, air inlet temperature when spray drying
Degree is 280 DEG C；The recyclable benefit of the ammonium acetate class or nitric acid ammonium material that gas discharged in spray-drying process condenses
With.
Gained precursor pulp is spray-dried, presoma powder is obtained；Low temperature is carried out to gained presoma powder
The step of heat treatment.The condition of the Low Temperature Heat Treatment are as follows: in 300 DEG C of heat preservation 15h, then be warming up to 500 DEG C of heat preservation 15h.
Gained presoma powder will be walked, lithium source mixes, and mixture high-temperature roasting is obtained positive electrode active materials.Mixture
High-temperature roasting condition are as follows: maturing temperature is 900 DEG C, soaking time 20h.
Wherein, the manganese source is manganese acetate and/or manganese nitrate, and the nickel source is nickel nitrate, and the lead source is plumbi nitras；Institute
Stating the solution containing citrate ion is citric acid solution, the mixed solution of citric acid and ammonium hydroxide, ammonium citrate solution or lemon
At least one of sour ammonium and the mixed solution of ammonium hydroxide；The lithium source is lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate and fluorine
Change at least one of lithium.
Prepare electrolyte
The electrolyte is made of ionic liquid, additive, organic solvent, fire retardant and lithium salts, is specifically included:
80 parts of ionic liquid, 50 parts of thianthrene, 60 parts of carbonate-based solvent, 6 parts of phosphate ester flame retardants, in the electrolyte
The concentration of lithium salts is 1mol/L；Preferably, ionic liquid EMI-BF4(- four fluorophosphate of -3 methylimidazole of 1- ethyl), EMI-
BF6(- 3 methylimidazole-two (trimethyl fluoride sulfonyl) of 1- ethyl is sub- by (- 3 methylimidazoles of 1- ethyl-hexafluorophosphate), EMI-TFSI
At least one of amine salt), lithium salts LiPF6、LiBF4、LiClO4At least one of.
Prepare lithium ion cell positive
Lithium battery anode active material, positive conductive agent, positive electrode binder and the anode collection prepared using above-mentioned steps
Body prepares lithium ion cell positive；Preferably, positive conductive agent is selected from conducting polymer, conductive oxide, conductivity ceramics, activity
One of carbon, graphene, carbon black, graphite, carbon fiber, metallic fiber, metal powder and sheet metal are a variety of, anode
The mass percent that conductive agent accounts for positive electrode is 10%.
Preferably, the positive electrode binder can be selected from polyethylene oxide, polypropylene oxide, polyacrylonitrile, polyamides
Imines, polyester, polyethers, fluorinated polymer, poly- divinyl polyethylene glycol, polyethyleneglycol diacrylate, polyethylene glycol diformazan
The mixture and derivative of one of base acrylic acid or above-mentioned polymer.
Preferably, the material of plus plate current-collecting body is selected from vitreous carbon, graphite foil, graphite flake, foamy carbon, carbon felt, carbon cloth, carbon fiber
One of dimension.
Form lithium battery early-products
Obtained anode, isolation film and cathode are wound and to form core, wherein the isolation film bears the anode with described
Pole isolation；Electrolyte is injected into the core；The first pressure coefficient for obtaining the core, according to the first pressure coefficient
Second pressure coefficient is calculated, the second pressure coefficient is less than the first pressure coefficient；And the core is carried out
Baking processing, and pressure is applied to the core using the second pressure coefficient, obtain lithium ion battery early-products.
The method of the first pressure coefficient for obtaining the core are as follows: apply pressure to multiple core, obtain more
The maximum pressure coefficient that a core is able to bear calculates the average value of multiple maximum pressure coefficients, first pressure
The ratio of the average value of force coefficient and the maximum pressure coefficient is 100%, the second pressure coefficient and the first pressure
The ratio of coefficient is 90%.The operation of the baking processing are as follows: the core is placed in high-temperature clamp, under conditions of 90 DEG C
Carry out baking processing.
Forming and capacity dividing obtains final lithium ion battery product
Lithium ion battery early-products n are taken, n is the positive integer greater than 4；The n lithium ion battery is shelved m hours；
It is charged with the electric current of small flow to it, charging time 3h；Described m hours is 40h, and the low current is
0.25C, the middle electric current are 0.5C, and the discharge-rate is 0.8C.
Lithium ion battery after charging is shelved at a certain temperature, aging；
Lithium ion battery is charged into voltage rating with the electric current of middle flow, turns constant-voltage charge, until terminating after cut-off current
Charging；
Lithium ion battery after charging is shelved 30 minutes；
Lithium ion battery is discharged to blanking voltage with different discharge-rates respectively；With discharge capacity divided by charging capacity,
For the first time charged efficiency of each lithium ion battery under the discharge-rate is obtained, to obtain lithium ion battery in the discharge-rate
Under average efficiency charged for the first time；
Then the lithium ion battery of mass production has been infused and has carried out operation by above-mentioned steps after liquid, and will be after charging
The lithium ion battery of mass production be discharged to certain voltage, so that the lithium ion battery produced in enormous quantities is in half charged shape
State；Capacity=mass production lithium ion battery of the lithium ion battery of mass production under different discharge-rates, which charges, to be held
Average efficiency charged for the first time under amount × difference discharge-rate, forming and capacity dividing terminate.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, several equivalent substitute or obvious modifications is made, and performance or use is identical, all should
It is considered as belonging to protection scope of the present invention.
Claims (6)
1. a kind of preparation method of lithium ion battery, the preparation method include the following steps:
(1) lithium battery anode active material is prepared
Using citrate coprecipitation-spray drying-high-temperature roasting method, the chemical formula of the positive electrode active materials is Li2-x-y- zMnxNiyPbzO2, wherein x=0.31-0.35, y=0.25-0.28, z=0.02-0.04；
(2) electrolyte is prepared
The electrolyte is made of ionic liquid, additive, organic solvent, fire retardant and lithium salts, is specifically included:
It is 55-80 parts of ionic liquid, 10-50 parts of thianthrene, 15-60 parts of carbonate-based solvent, 2-6 parts of phosphate ester flame retardants, described
The concentration of lithium salts is 0.75mol/L-1mol/L in electrolyte；
(3) lithium ion cell positive is prepared
Lithium battery anode active material, positive conductive agent, positive electrode binder and the plus plate current-collecting body prepared using above-mentioned steps (1)
Prepare lithium ion cell positive；
(4) lithium battery early-products are formed
Anode is made in step (3), isolation film and cathode wind and to form core, wherein the isolation film is by the anode and institute
State cathode isolation；
Electrolyte is injected into the core；
Second pressure coefficient is calculated according to the first pressure coefficient in the first pressure coefficient for obtaining core, and described second
Pressure coefficient is less than the first pressure coefficient；And
Baking processing carried out to the core, and pressure is applied to the core using the second pressure coefficient, obtain lithium from
Sub- battery early-products；
(5) forming and capacity dividing obtains final lithium ion battery product.
2. the method as described in claim 1, which is characterized in that in the step (1), specifically comprise the following steps:
(11) corresponding raw material is weighed by the molar ratio of chemical formula, by the solution containing manganese source, nickel source and lead source and contains citrate
The solution of ion carries out mixing co-precipitation, and controls mixing condition, obtains precursor pulp；
(12) precursor pulp obtained by step (11) is spray-dried, obtains presoma powder；
(13) presoma powder, lithium source obtained by step (12) are mixed, and mixture high-temperature roasting is obtained positive electrode active materials.
3. method according to claim 2, which is characterized in that in the step (2), ionic liquid EMI-BF4(1- second
- four fluorophosphate of -3 methylimidazole of base), EMI-BF6(- 3 methylimidazoles of 1- ethyl-hexafluorophosphate), EMI-TFSI (1- second
At least one of base -3 methylimidazole-two (trimethyl fluoride sulfonyl) inferior amine salt), lithium salts LiPF6、LiBF4、LiClO4In
It is at least one.
4. method as claimed in claim 3, which is characterized in that in step (4), the first pressure for obtaining the core
The method of coefficient are as follows: apply pressure to multiple core, obtains the maximum pressure coefficient that multiple core are able to bear, meter
Calculate the average value of multiple maximum pressure coefficients, the ratio of the first pressure coefficient and the average value of the maximum pressure coefficient
Being worth is 80%-100%, and the ratio of the second pressure coefficient and the first pressure coefficient is 70%-90%.
5. method as claimed in claim 4, which is characterized in that in step (4), the operation of the baking processing are as follows: by institute
It states core to be placed in high-temperature clamp, carries out baking processing under conditions of 70 DEG C -90 DEG C.
6. method as claimed in claim 5, which is characterized in that include following sub-step in step (5):
(51) lithium ion battery early-products n are taken, n is the positive integer greater than 4；The n lithium ion battery is shelved m hours；
(52) it is charged with the electric current of small flow to it, charging time 2-3h；
(53) lithium ion battery after charging is shelved at a certain temperature, aging；
(54) lithium ion battery is charged to voltage rating by the electric current of flow in, turns constant-voltage charge, until terminating after cut-off current
Charging；
(55) lithium ion battery after charging is shelved 5-30 minutes；
(56) lithium ion battery is discharged to blanking voltage with different discharge-rates respectively；With discharge capacity divided by charging capacity,
For the first time charged efficiency of each lithium ion battery under the discharge-rate is obtained, to obtain lithium ion battery in the discharge-rate
Under average efficiency charged for the first time；
(57) then the lithium ion battery of mass production infuse and carried out operation by step (51)-(56) after liquid, and will charged
After the lithium ion battery of mass production be discharged to certain voltage, so that the lithium ion battery produced in enormous quantities is in half
State-of-charge；Capacity=mass production lithium ion battery of the lithium ion battery of mass production under different discharge-rates
Average efficiency charged for the first time under charging capacity × difference discharge-rate, forming and capacity dividing terminate.
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