CN104134792B - A kind of high voltage height cobalt lithium ion anode material and preparation method thereof - Google Patents
A kind of high voltage height cobalt lithium ion anode material and preparation method thereof Download PDFInfo
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- CN104134792B CN104134792B CN201410328214.1A CN201410328214A CN104134792B CN 104134792 B CN104134792 B CN 104134792B CN 201410328214 A CN201410328214 A CN 201410328214A CN 104134792 B CN104134792 B CN 104134792B
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- lithium ion
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000010405 anode material Substances 0.000 title claims abstract description 21
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 title claims description 23
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 13
- 239000010941 cobalt Substances 0.000 claims abstract description 13
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 5
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 4
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 25
- 239000000654 additive Substances 0.000 claims description 20
- 230000000996 additive effect Effects 0.000 claims description 20
- 229910052751 metal Inorganic materials 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 17
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 15
- 229910052744 lithium Inorganic materials 0.000 claims description 15
- 239000011572 manganese Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 13
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 239000012266 salt solution Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 claims description 10
- 150000002739 metals Chemical class 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- SEVNKUSLDMZOTL-UHFFFAOYSA-H cobalt(2+);manganese(2+);nickel(2+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mn+2].[Co+2].[Ni+2] SEVNKUSLDMZOTL-UHFFFAOYSA-H 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- 229910052748 manganese Inorganic materials 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- -1 Κ O Η Chemical compound 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 150000001868 cobalt Chemical class 0.000 claims description 4
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 4
- 150000002696 manganese Chemical class 0.000 claims description 4
- 150000002815 nickel Chemical class 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- 238000004886 process control Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims description 3
- PXEDJBXQKAGXNJ-QTNFYWBSSA-L disodium L-glutamate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](N)CCC([O-])=O PXEDJBXQKAGXNJ-QTNFYWBSSA-L 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 3
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 3
- 235000013923 monosodium glutamate Nutrition 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 235000011083 sodium citrates Nutrition 0.000 claims description 3
- 229940073490 sodium glutamate Drugs 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims 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 claims description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- 229910013716 LiNi Inorganic materials 0.000 claims description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000011833 salt mixture Substances 0.000 claims 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000004411 aluminium Substances 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 239000000347 magnesium hydroxide Substances 0.000 claims 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 28
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 5
- 238000009938 salting Methods 0.000 description 5
- 229910002651 NO3 Inorganic materials 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 229910032387 LiCoO2 Inorganic materials 0.000 description 3
- 238000001467 acupuncture Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 3
- 229940099596 manganese sulfate Drugs 0.000 description 3
- 239000011702 manganese sulphate Substances 0.000 description 3
- 235000007079 manganese sulphate Nutrition 0.000 description 3
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- 229910005763 Li1.05Co0.8Mn0.2O2 Inorganic materials 0.000 description 1
- 229910002991 LiNi0.5Co0.2Mn0.3O2 Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000006104 solid solution 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
- H01M4/48—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
- 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
- H01M4/52—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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of high voltage height cobalt anode material for lithium-ion batteries and preparation method thereof, its molecular formula is LiNi0.1Co0.8Mn0.1AxO2, wherein: A is one or more in Ti, Mg, Al, Zr element, 0 ＜ x ＜ 0.1.Present invention reduces the content of cobalt element in positive electrode, reducing material cost, preparation technology controllability is good, and lot stability is good, it is easy to production management, can meet on market high voltage, long circulating, height ratio capacity, high magnification, the application demand of lower cost materials.The most significant advantage is that the security performance of material is significantly improved, it is possible to meet the market requirement to high security material.
Description
Technical field
The present invention relates to technical field of lithium ion, particularly to a kind of high voltage height cobalt material and
Preparation method.
Background technology
Lithium ion battery has been widely used in the numbers such as notebook computer, mobile phone, digital camera at present
On product and various electric tool, it is increasingly becoming product indispensable in people's life.In order to meet
Updating and upgrading of a product demand, various product also tends to portability, high efficiency, economization, and this will
Lithium ion battery product is asked to develop to high-energy-density, low cost direction, in recent years in CE market
Use the widest LiCoO2It is limited by cobalt raw material, has been difficult to reduce cost, it is therefore necessary to find
A kind of low cost has higher energy density and the positive pole alternative materials of excellent battery performance simultaneously.
Some material and battery producer are in order to reduce cost both at home and abroad, use LiCoO2With
Li1+nNi0.5+xCo0.2+yMn0.3+zO2Pilot process product or final products are simply mixed use, but this
Mixed method exists that cost is high, process is wayward, discharge voltage and the low deficiency of compacted density, and
And the defect of homogenous material can affect the performance of whole mixing material, therefore final battery in mixing material
Uniformity also be difficult to ensure.A kind of synthesis is described at US7510805 disclosed in 2009
Li1.05Co0.8Mn0.2O2Method, but capacity decline more, it is impossible to meet the requirement of high-capacity battery.
CN102891307A disclosed in 2013 describes a kind of stratum nucleare
Li1+nAwNi0.5+xCo0.2+yMn0.3+zO2, shell be Li1+aCo1-bMbO2Lithium ion battery compound just
Pole material can play good cycle performance and high-temperature behavior under high voltages.But the method cost
Height, technique are complex.
Summary of the invention
The technical problem to be solved is to provide a kind of high voltage height cobalt lithium ion cell positive
Material LiNi0.1Co0.8Mn0.1AxO2And preparation method thereof, present invention reduces cobalt element in positive electrode
Content, reduce material cost, and technique be close with cobalt acid lithium, prepared material capacity is high,
Normal temperature and high temperature cyclic performance is good, multiplying power is high, it is simple to large-scale production.The most significant advantage is material
Security performance be significantly improved.
The present invention solve above-mentioned technical problem be the technical scheme is that a kind of high voltage height cobalt lithium from
Sub-cell positive material, its chemical general formula is LiNi0.1Co0.8Mn0.1AxO2, wherein, A be Ti,
One or more in Mg, Al, Zr element, 0 ＜ x ＜ 0.1.
The preparation method of above-mentioned a kind of high voltage height cobalt lithium ion anode material, comprises the following steps:
1) nickel salt of solubility, cobalt salt, manganese salt and doping metals A salt are configured to salting liquid, stir
Mix and make it fully be uniformly mixed so as to obtain mixing salt solution；Described doping metals A salt is containing metal element A
Salt compounds；Wherein nickel, cobalt, the ratio of three kinds of elements of manganese are 0.1:0.8:0.1；Preferably,
In the described mixing salt solution that preparation obtains, metal cation total concentration is 0.3～2.3mol/L.
2) preparation aqueous slkali and enveloping agent solution respectively, then by the solution mixing prepared or individually with
The speed of 0.1～10L/h pumps in reactor and is stirred, simultaneously by controlling aqueous slkali and complexing
The flow velocity of agent solution makes mixed solution pH value be 9～12, and process control temperature of reaction kettle exists
20 DEG C～100 DEG C, reactor has inert gas or compressed air protection；Mixing speed is
100～800rpm, after the salting liquid prepared all adds reactor, continue stirring and be aged 2～48h,
Then the solidliquid mixture centrifugal filtration obtained is separated, be washed with deionized solids to neutral
After, at 80～200 DEG C, dry 2～12h, obtain required nickel cobalt manganese hydroxide precursor；
3) by described step 2) presoma pre-burning 2～8h at 200～600 DEG C of obtaining, it is cooled to room
After temperature, grind into powder crosses 250 mesh sieves, obtains oxide I；Mix with lithium source and additive A again,
At 800 DEG C～1200 DEG C, calcine 8～30h, be cooled to after room temperature through ground 400 mesh sieves, obtain II.
When oxide I, lithium source and additive A being mixed, it is preferable that the quality in the lithium source of interpolation accounts for herein
The 40%～50% of oxide I mass.
4) by described step 3) II that obtains mixes with additive A, forges at 700 DEG C～1000 DEG C
Burn 8～20h, be cooled to after room temperature through ground 400 mesh sieves, obtain III.
5) by described step 4) III that obtains and lithium source add in solvent, be sufficiently stirred for forming feed liquid,
Again the solution being dissolved with additive A is instilled in described feed liquid, stir, filter and after drying,
Calcine 8～20h at 300 DEG C～900 DEG C, after being cooled to room temperature, cross 400 mesh sieves, obtain the present invention and be combined
Modified high voltage height cobalt lithium ion anode material LiNi0.1Co0.8Mn0.1AxO2.Preferably, described step
Rapid 5), in, the quality in the lithium source of interpolation accounts for the 0.1%～2% of described III gross mass.
A kind of as high voltage height cobalt lithium ion anode material preparation method of the present invention improves, and described 1)
In nickel salt be at least one in nickel sulfate, nickel chloride or nickel nitrate；Cobalt salt is cobaltous sulfate, chlorination
At least one in cobalt or cobalt nitrate；Manganese salt is at least one in manganese sulfate, manganese chloride or manganese nitrate.
A kind of as high voltage height cobalt lithium ion anode material preparation method of the present invention improves, and described 2)
In aqueous slkali be NaOH, Κ O Η, LiOH, Na2CO3In one, concentration is 1～10mol/L；
Enveloping agent solution is in ammonium nitrate, ammoniacal liquor, ammonium sulfate, sodium glutamate, sodium citrate, ammonium chloride
One or more, concentration is 0.01～4mol/L.
As a kind of improvement of high voltage height cobalt lithium ion anode material preparation method of the present invention, described step
Rapid 1) doping metals A salt is the salt compounds containing element A.Described step 3), 4),
5) additive A in also refers to the compound containing element A.Described A is Ti, Mg, Al,
One or more in Zr element.Ti is TiO2Or butyl titanate, Mg is magnesia or hydroxide
Magnesium, Al is in aluminium hydroxide, aluminum fluoride, aluminium isopropoxide, aluminum nitrate, nano aluminium oxide, aluminum phosphate
One, Zr is ZrO2.Described step 3), 4), 5) additive A in three steps is permissible
Identical, it is also possible to different.Described doping metals A salt can be identical with additive A, it is also possible to different.
In preferred embodiment, described step 1) doping metals A salt be aluminum sulfate；Described step
Rapid 3) additive A is Mg (OH)2Or MgO；Step 4) additive A be AlF3；Step
Rapid 5) additive A is Al (NO3)3。
In another preferred embodiment, described step 1) doping metals A salt be aluminum sulfate；
Described step 3) additive A be Mg (OH)2Or MgO；Step 4) additive A be TiO2；
Step 5) additive A be Al (NO3)3。
In another preferred embodiment, described step 1) doping metals A salt be aluminum sulfate；
Described step 3) additive A be Mg (OH)2Or MgO；Step 4) additive A be TiO2；
Step 5) additive A be butyl titanate.
As a kind of improvement of high voltage height cobalt lithium ion anode material preparation method of the present invention, described step
Rapid 3), 5) in, lithium source is at least one in lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate.
As a kind of improvement of high voltage height cobalt lithium ion anode material preparation method of the present invention, described step
Rapid 5), in, solvent is the one in ethanol, deionized water, acetone.
As a kind of improvement of high voltage height cobalt lithium ion anode material of the present invention, step 3), 4) in
The equipment that mixing uses is high mixer, agravic mixing kettle, inclined ball mill, horizontal ball mill, OK
One or more in celestial body grinding machine, Quick ball grinder.
Compared with prior art, the present invention utilizes wet method and pyrogenic process technology, by nickel, cobalt, manganese, doping
The various element permutation and combination in an orderly manner such as element is got up, and forms the firmly microstructure of functionalization, promotees
The material making synthesis is solid solution homogenous material, it is to avoid due to mixing material in homogenous material defect and
The final performance affecting whole mixing material.Simultaneously as employ cheap nickel and manganese takes
The cobalt that cost lattice are higher, reduces production cost, and practical operation is simple, energy consumption is low, be prone to work
Industryization is promoted and is produced and controls.The LiNi of the present invention0.1Co0.8Mn0.1AxO2Lithium electricity positive electrode combines
LiCoO2Material and LiNi0.5Co0.2Mn0.3O2Advantage, be allowed to have both high volume energy density and height
The feature of security, the performance such as material uniformity under high voltages, safety, circulation can be more preferably.
Detailed description of the invention
In order to make the goal of the invention of the present invention, technical scheme and Advantageous Effects become apparent from, below
The method present invention being described in further detail by embodiment, but this is not limitation of the present invention,
Those skilled in the art are according to the basic thought of the present invention, and various modifications may be made or improves, as long as
Without departing from the basic thought of the present invention, the most within the scope of the present invention.
Embodiment 1
1) nickel sulfate, cobaltous sulfate, manganese sulfate are 0.1:0.8:0.1's by Ni, Co, Mn mol ratio
Ratio is dissolved in deionized water and is configured to the salting liquid that metal cation total concentration is 1.2mol/L, solute
Gross weight 200kg, adds 0.2kg aluminum sulfate, and stirring makes it fully be uniformly mixed so as to obtain mixing salt solution.
2) sodium hydroxide solution of 5mol/L and the ammoniacal liquor of 3mol/L are prepared respectively, and in above-mentioned mixing
Solution adds 0.4kg hydrazine hydrate；Then the mixing salt solution for preparing above-mentioned, sodium hydroxide solution,
Three kinds of solution of ammoniacal liquor pump in reactor with the speed of 0.4L/h individually and are stirred, and pass through simultaneously
The flow velocity controlling NaOH and ammonia aqueous solution makes mixed solution pH value be 9.7, and process control is reacted
Still temperature at 45 DEG C, blanketing with inert gas in reactor；Mixing speed is 300rpm, waits to prepare
Described mixing salt solution all add reactor after continue stirring and be aged 12h, then will obtain
Solidliquid mixture centrifugal filtration separates, and is washed with deionized solids to after neutrality, at 120 DEG C
Dry 7h, obtain required nickel cobalt manganese hydroxide precursor.
3) by above-mentioned presoma pre-burning 5h at 400 DEG C, after being cooled to room temperature, grind into powder crosses 250
Mesh sieve, obtains oxide I；Take 100kg oxide I, with 50kg Li2CO3With 0.35kg Mg (OH)2
In agravic mixing kettle, mix 2h, at 1000 DEG C, calcine 18h, be cooled to after room temperature through ground
400 mesh sieves, obtain II.
4) by step 3) prepared by II Yu 0.4kg AlF3In high-speed mixer and mixing 1h, at 900 DEG C
Lower calcining 14h, is cooled to after room temperature through ground 400 mesh sieves, obtains III.
5) by 0.8kg Al (NO3)3It is dissolved in 18L deionized water, standby.Then by step
4) III and the 0.2kg lithium acetate prepared by adds in deionized water, is sufficiently stirred for, instills above-mentioned system
Standby Al (NO3)3Solution, quickly stirs a period of time, filters and dried, forges at 600 DEG C
Burn 10h, cross 400 mesh sieves after being cooled to room temperature, just obtaining composite modified high voltage height cobalt lithium ion
Pole material.
Through 053048 full battery testing 4.4V, battery 1C capacity 170mAh/g, 500 normal temperature
Follow capability retention more than 91% (loop test condition: 1C/1C charge and discharge, lower with), 300 times 45 DEG C
High temperature circulation capability retention more than 92%, acupuncture and overcharge (3C/5V) 4 batteries full by.
Embodiment 2
1) nickel nitrate, cobalt nitrate, manganese nitrate are 0.1:0.8:0.1's by Ni, Co, Mn mol ratio
Ratio is dissolved in deionized water and is configured to the salting liquid that metal cation total concentration is 1.7mol/L, solute
Gross weight 200kg, adds 0.3kg aluminum sulfate, and stirring makes it fully be uniformly mixed so as to obtain mixing salt solution.
2) sodium hydroxide solution of 4mol/L and the sodium glutamate of 4mol/L are prepared respectively, and above-mentioned
Mixed solution adds 0.6kg hydrazine hydrate；Then the mixing salt solution for preparing above-mentioned, NaOH
Solution, three kinds of solution of ammoniacal liquor pump in reactor with the speed of 0.4L/h individually and are stirred, with
Time make mixed solution pH value be 10.8 by controlling the flow velocity of NaOH and ammonia aqueous solution, process
Control temperature of reaction kettle at 65 DEG C, blanketing with inert gas in reactor；Mixing speed is 400rpm,
After the described mixing salt solution prepared all adds reactor, continue stirring and be aged 16h, then will
The solidliquid mixture centrifugal filtration that obtains separates, and is washed with deionized solids to after neutrality,
Dry 9h at 120 DEG C, obtain required nickel cobalt manganese hydroxide precursor.
3) by above-mentioned presoma pre-burning 8h at 600 DEG C, after being cooled to room temperature, grind into powder crosses 250
Mesh sieve, obtains oxide I；Take 100kg oxide I, with 48kg Li2CO3With 0.8kg Mg (OH)2
In agravic mixing kettle, mix 2.5h, at 1020 DEG C, calcine 14h, through grinding after being cooled to room temperature
Cross 400 mesh sieves, obtain II.
4) by step 3) prepared by II Yu 0.32kg TiO2In high-speed mixer and mixing 1h, at 940 DEG C
Lower calcining 10h, is cooled to after room temperature through ground 400 mesh sieves, obtains III.
5) 0.92kg aluminium isopropoxide is dissolved in 22L ethanol, standby.Then by step 4) institute
III and the 0.1kg lithium oxalate of preparation adds in ethanol, is sufficiently stirred for, instills aluminium isopropoxide solution,
It is sufficiently stirred for, instills the Al (NO of above-mentioned preparation3)3Solution, quickly stirs a period of time, is dried
After, at 550 DEG C, calcine 12h, cross 400 mesh sieves after being cooled to room temperature, obtain composite modified height
Voltage height cobalt lithium ion anode material.Test through 053048 full battery 4.4V, battery 1C capacity
169mAh/g, 500 normal temperature follow capability retention more than 90%, 300 45 DEG C of high temperature circulation capacity
Conservation rate more than 91%, acupuncture and overcharge (3C/5V) 4 batteries full by.
Embodiment 3
1) nickel sulfate, cobaltous sulfate, manganese sulfate are 0.1:0.8:0.1's by Ni, Co, Mn mol ratio
Ratio is dissolved in deionized water and is configured to the salting liquid that metal cation total concentration is 1.8mol/L, solute
Gross weight 200kg, adds 0.24kg aluminum sulfate, and stirring makes it fully be uniformly mixed so as to obtain mixing salt solution.
2) sodium hydroxide solution of 5mol/L and the sodium citrate of 5mol/L are prepared respectively, and above-mentioned
Mixed solution adds 0.5kg hydrazine hydrate；Then the mixing salt solution for preparing above-mentioned, NaOH
Solution, three kinds of solution of ammoniacal liquor pump in reactor with the speed of 0.3L/h individually and are stirred, with
Time make mixed solution pH value be 9.4 by controlling the flow velocity of NaOH and ammonia aqueous solution, the most program control
Temperature of reaction kettle processed at 75 DEG C, blanketing with inert gas in reactor；Mixing speed is 500rpm,
After the described mixing salt solution prepared all adds reactor, continue stirring and be aged 10h, then will
The solidliquid mixture centrifugal filtration that obtains separates, and is washed with deionized solids to after neutrality,
Dry 12h at 100 DEG C, obtain required nickel cobalt manganese hydroxide precursor.
3) by above-mentioned presoma pre-burning 6h at 530 DEG C, after being cooled to room temperature, grind into powder crosses 250
Mesh sieve, obtains oxide I；Take 100kg oxide I, with 47kg Li2CO3Exist with 0.5kg MgO
Agravic mixing kettle mixes 2.5h, at 1050 DEG C, calcines 12h, be cooled to after room temperature through ground
400 mesh sieves, obtain II.
4) by step 3) prepared by II Yu 0.26kg TiO2In high-speed mixer and mixing 1h, at 980 DEG C
Lower calcining 10h, is cooled to after room temperature through ground 400 mesh sieves, obtains III.
5) 1.2kg butyl titanate is dissolved in 20L acetone, standby, then by step 4) made
Standby III and 0.1kg lithium hydroxide adds in ethanol, is sufficiently stirred for, instills the metatitanic acid of above-mentioned preparation
Butyl acetate solution, quickly stirs a period of time, after drying, calcines 7h, be cooled to room temperature at 650 DEG C
Rear mistake 400 mesh sieve, obtains composite modified high voltage height cobalt lithium ion anode material.
Test through 053048 full battery 4.4V, battery 1C capacity 171mAh/g, 500 normal temperature
Follow capability retention more than 89%, 300 45 DEG C of high temperature circulation capability retentions more than 90%, acupuncture
With overcharge (3C/5V) 4 batteries full by.
From the point of view of the electrical performance data of embodiment, the high temperature cyclic performance of material is substantially better than similar material
Material, some electrical performance indexes is near or above pure cobalt acid lithium, particularly capacity, safety and high temperature circulation
Performance, is more an advantage over similar LiNi0.1Co0.8Mn0.1O2Material.It it is the energy substituting cobalt that a kind of potentiality are the biggest
The high-performance positive electrode of acid lithium.
As it has been described above, just can preferably realize the present invention.
Claims (6)
1. the preparation method of a high voltage height cobalt lithium ion anode material, it is characterised in that
Described high voltage height cobalt lithium ion anode material chemical formula is LiNi0.1Co0.8Mn0.1AxO2, formula
In 0 ＜ x ＜ 0.1, A is one or more in Ti, Mg, Al, Zr element；Described system
Preparation Method specifically includes following steps:
1) nickel salt of solubility, cobalt salt, manganese salt and doping metals A salt are configured to salt-mixture
Solution；Wherein nickel, cobalt, the ratio of three kinds of elements of manganese are 0.1:0.8:0.1；
2) aqueous slkali and enveloping agent solution are prepared respectively；Then by molten for the described salt-mixture for preparing
Liquid, aqueous slkali and enveloping agent solution mix or individually pump into reaction with the speed of 0.1～10L/h
In still and be stirred, make mixing molten by controlling the flow velocity of aqueous slkali and enveloping agent solution simultaneously
Liquid pH value is 9～12, and process control temperature of reaction kettle, at 20 DEG C～100 DEG C, has in reactor
Inert gas shielding；Mixing speed is 100～800rpm, described mixing salt solution to be prepared
Continue stirring after all adding reactor and be aged 2～48h, the solidliquid mixture that then will obtain
Centrifugal filtration separates, and is washed with deionized solids to after neutrality, dries at 80～200 DEG C
Dry 2～12h, obtain required nickel cobalt manganese hydroxide precursor；
3) by described step 2) the nickel cobalt manganese hydroxide precursor that obtains is at 200～600 DEG C
Pre-burning 2～8h, after being cooled to room temperature, grind into powder crosses 250 mesh sieves, obtains oxide I；Again
Mix with lithium source and additive A, at 800 DEG C～1200 DEG C, calcine 8～30h, be cooled to room
Through ground 400 mesh sieves after temperature, obtain II；
4) by described step 3) II that obtains mixes with additive A, at 700 DEG C～1000 DEG C
Lower calcining 8～20h, is cooled to after room temperature through ground 400 mesh sieves, obtains III；
5) by described step 4) III that obtains and lithium source add in solvent, be sufficiently stirred for being formed
Feed liquid, then the solution being dissolved with additive A is instilled in described feed liquid, stir, filter and
After drying, at 300 DEG C～900 DEG C, calcine 8～20h, after being cooled to room temperature, cross 400 mesh sieves,
Obtain high voltage height cobalt lithium ion anode material LiNi of the present invention0.1Co0.8Mn0.1AxO2；
Wherein, described doping metals A salt and additive A are the change containing metal element A
Compound；Compound containing metal element Ti is TiO2Or butyl titanate；Containing metallic element
The compound of Mg is magnesia or magnesium hydroxide；Compound containing metal element A l is hydroxide
One in aluminium, aluminum fluoride, aluminium isopropoxide, aluminum nitrate, nano aluminium oxide, aluminum phosphate；Contain
The compound of metallic element Zr is ZrO2。
2. according to the preparation method of the high voltage height cobalt lithium ion anode material described in right 1,
It is characterized in that, described step 1) in nickel salt be in nickel sulfate, nickel chloride or nickel nitrate
At least one；Cobalt salt is at least one in cobaltous sulfate, cobalt chloride or cobalt nitrate；Manganese salt is sulphur
At least one in acid manganese, manganese chloride or manganese nitrate.
3. according to the preparation method of the high voltage height cobalt lithium ion anode material described in right 1,
It is characterized in that, described step 2) in aqueous slkali be NaOH, Κ O Η, LiOH, Na2CO3
In one, concentration is 1～10mol/L；Enveloping agent solution be ammonium nitrate, ammoniacal liquor, ammonium sulfate,
One or more in sodium glutamate, sodium citrate, ammonium chloride, concentration is 0.01～4mol/L.
4. according to the preparation method of the high voltage height cobalt lithium ion anode material described in right 1,
It is characterized in that, described step 5) described in solvent be in ethanol, deionized water, acetone
A kind of.
5. according to the preparation method of the high voltage height cobalt lithium ion anode material described in right 1,
It is characterized in that, described step 3), 5) in, described lithium source be lithium carbonate, lithium hydroxide,
At least one in lithium acetate, lithium oxalate；Described step 3) in the quality in lithium source added account for
The 40%～50% of oxide I gross mass, described step 5) in the quality in lithium source added account for institute
State the 0.1%～2% of III gross mass.
6. high voltage height cobalt lithium ion anode material, it is characterised in that use Claims 1 to 5
Any one method prepares.
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| CN105336941A (en) * | 2015-11-16 | 2016-02-17 | 广东邦普循环科技有限公司 | High-voltage LiNixCoyMnzM(1-x-y-z)O2 cathode material, preparation method thereof, cathode and battery |
| CN107293744A (en) * | 2016-04-12 | 2017-10-24 | 河南科隆新能源股份有限公司 | High-voltage monocrystal-like ternary cathode material and preparation method thereof |
| CN108123128A (en) * | 2017-12-25 | 2018-06-05 | 北京理工大学 | Adulterate Al in a kind of surface layer3+NCM tertiary cathode materials preparation method |
| CN109081384B (en) * | 2018-07-10 | 2020-11-20 | 南京航空航天大学 | Composite complexing agent and method for preparing positive electrode precursor material for lithium ion power battery |
| CN112047397B (en) * | 2020-09-15 | 2024-03-22 | 天津市捷威动力工业有限公司 | A high-power ternary material precursor and preparation method |
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