CN108336333A - A kind of preparation method of high-voltage lithium ion batteries material and the material of preparation - Google Patents
A kind of preparation method of high-voltage lithium ion batteries material and the material of preparation Download PDFInfo
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- CN108336333A CN108336333A CN201810094558.9A CN201810094558A CN108336333A CN 108336333 A CN108336333 A CN 108336333A CN 201810094558 A CN201810094558 A CN 201810094558A CN 108336333 A CN108336333 A CN 108336333A
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- lithium
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- cobalt
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 28
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 91
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000010941 cobalt Substances 0.000 claims abstract description 51
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 51
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000002253 acid Substances 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 27
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010406 cathode material Substances 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000010936 titanium Substances 0.000 claims abstract description 20
- 239000011159 matrix material Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 14
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 13
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 13
- 239000011777 magnesium Substances 0.000 claims abstract description 13
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 13
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 44
- 150000001875 compounds Chemical class 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- 229910001593 boehmite Inorganic materials 0.000 claims description 4
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 description 14
- 239000010405 anode material Substances 0.000 description 11
- 230000002441 reversible effect Effects 0.000 description 11
- 230000014759 maintenance of location Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 8
- 238000003825 pressing Methods 0.000 description 8
- 239000002033 PVDF binder Substances 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 7
- 239000006229 carbon black Substances 0.000 description 7
- 238000005253 cladding Methods 0.000 description 7
- 239000006258 conductive agent Substances 0.000 description 7
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 238000004088 simulation Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002641 lithium Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Engineering & Computer Science (AREA)
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- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention provides a kind of preparation method of high-voltage lithium ion batteries material, and step includes：Using cobalt oxide and lithium carbonate as presoma, magnesium carbonate is added and is uniformly mixed, carries out first sintering and is crushed, obtain cobalt acid lithium matrix；Aluminum oxide and titanium oxide are added into cobalt acid lithium matrix, is sintered and is crushed for the second time after mixing, obtain lithium cobaltate cathode material.The present invention also provides a kind of high-voltage lithium ion batteries material prepared using the method for the present invention, the average grain diameter of the material is 4~9 μm, and pattern is monocrystalline pattern or aggregate pattern, including cobalt acid lithium matrix and the clad that is coated in cobalt acid lithium；Contain Al and Ti elements in the clad；The chemical formula of the cobalt acid lithium is Li1+xCo1‑yMgyO2, wherein 0.002 ﹤ x≤0.04,0.005≤y ﹤ 0.01.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical fields, and in particular to a kind of high-voltage lithium ion batteries material
Preparation method and this method prepare material.
Background technology
Anode material for lithium-ion batteries is widely used in the electronic equipments such as notebook, mobile phone, digital camera and nobody is mechanical, electrical
On motor-car.Demand with market to anode material for lithium-ion batteries increasingly increases, and market is to high-energy density type and high magnification
The requirement of type cobalt acid lithium is also higher and higher.High-energy density type the main direction of development is high voltage at present, such as 4.35V, 4.4V,
4.45V, wherein application of 4.35V, 4.4V high voltage energy density type cobalt acid lithium material in lithium ion battery substantially at
It is ripe.As the short time such as unmanned plane are large current discharge the increasingly burning hot of electronic product, not only cobalt acid lithium is required to have at normal temperatures
Excellent high rate performance also requires that under low temperature (- 20 DEG C~0 DEG C) and hot conditions excellent chemical property can be possessed.
Under high/low temperature condition, the high current input and output performance of high rate during charging-discharging material and the electric conductivity of material have
It closes, material conductivity includes two kinds：Electron conduction and lithium ion conductive.Material conductivity is improved, DCR, Cai Nengshi are reduced
The fast charging and discharging of existing lithium ion battery.What DCR (i.e. DC internal resistance) was represented is the charged/discharged power capability of battery, very much
High-power applications rely primarily on this parameter, and DCR is smaller, and power capability is stronger, and the performance of high current charge-discharge is better.
The preparation method to cobalt acid lithium material of the prior art, such as application No. is 201610039657.8 Chinese invention is special
Profit discloses a kind of high voltage high-rate type lithium cobaltate positive electrode and preparation method thereof, and the deficiency of preparation method is to utilize
The problem of aluminium alcoholates and this liquid form of the mixed solution of titanate esters carry out secondary cladding, bring be：1. in dry and sintering
Remaining organic solvent consumes oxygen in the process, is easy to capture the oxygen element on cobalt acid lithium surface, destroys cobalt acid lithium surface texture, influences
The surface conductivity of cobalt acid lithium material so that the DCR degradations of material.And solid phase cladding is then not present and destroys cobalt acid lithium surface
The phenomenon that structure, instead surface coated material structurally consummate conductive solid solution can be preferably formed with cobalt acid lithium, promoted
The DCR performances of material；2. sintering require it is harsh, it is especially more demanding to sintering atmosphere, efficiency is low, it is of high cost, to environment not
It is friendly；3. its positive electrode does not have high rate capability and DCR performances under high/low temperature condition.
Invention content
The object of the present invention is to provide a kind of preparation methods of high-voltage lithium ion batteries material, using dry method solid phase packet
It covers, material surface property will not be damaged in cladding or heat treatment process.
It is a further object of the present invention to provide a kind of high-voltage lithium ion batteries materials prepared using the above method.
In order to achieve the above objectives, the technical solution adopted by the present invention is as follows：
A kind of preparation method of high-voltage lithium ion batteries material, step include：
Using cobalt oxide and lithium carbonate as presoma, magnesium carbonate is added and is uniformly mixed, carries out first sintering and is crushed, obtain
To cobalt acid lithium matrix；
Aluminum oxide and titanium oxide are added into cobalt acid lithium matrix, is sintered and is crushed for the second time after mixing,
Obtain lithium cobaltate cathode material.
Further, it is 1 that the cobalt oxide and lithium carbonate, which press Li/Co molar ratios,:1~1.04:1 configuration, magnesium carbonate press Mg/
Co molar ratios are 0.005:1~0.01:1 is added.
Further, the first sintering method is：Under conditions of air atmosphere, 900~1020 DEG C sintering 8~
12h。
Further, the average grain diameter D50 of the broken cobalt acid lithium matrix is 4~9 μm.
Further, the aluminum oxide is 0.001 by Al/Co molar ratios:1~0.002:1 is added, the titanium oxide
It is 0.001 by Ti/Co molar ratios:1~0.003:1 is added.
Further, the aluminum oxide is at least one of alundum (Al2O3), aluminium hydroxide, boehmite；Institute
It includes titanium dioxide to state titanium oxide.
Further, second of sintering method is：Under conditions of air atmosphere, 900~1000 DEG C sintering 2~
10h。
Further, it is mixed using three-dimensional mixer or super mixing machine.
The average grain diameter of a kind of high-voltage lithium ion batteries material prepared using the above method, the material is 4~9 μ
M, pattern are monocrystalline pattern or aggregate pattern, including cobalt acid lithium matrix and the clad that is coated in cobalt acid lithium；The cladding
Contain Al and Ti elements in layer；The chemical formula of the cobalt acid lithium is Li1+xCo1-yMgyO2, wherein 0.002 ﹤ x≤0.04,0.005
≤ y ﹤ 0.01.
Further, the substance of the clad is the compound containing Ti and Al, or for compound containing Ti and contains Alization
Close the mixture of object.
Compared with prior art, solid alumina is added in the cobalt acid lithium matrix of acquisition in preparation method provided by the invention
Compound and titanium oxide carry out the liquid packet of the aluminium alcoholates of solid cladding rather than the prior art and the mixing alcoholic solution of titanate esters
It covers, the advantage is that：1. avoiding liquid from being coated in dry and sintering process generates organic by-products, to material surface structure
It damages.2. reducing the requirement to sintering condition, improve the surface ion and electron conduction of material, promoted platform and
DCR performances；3. solid phase production efficiency is high, production capacity is big, environmentally friendly.This preparation method work simple for process, of low cost, suitable
Industryization mass produces.
Lithium cobaltate cathode material prepared by the present invention has compared with small particle and different-shape, surface electronic conduction and ion
Electric conductivity is excellent, is capable of providing shorter lithium ion diffusion path, is conducive to the raising of capacity and high rate performance.The present invention's
Cobalt acid lithium, Mg2+Replace part Co3+The electric conductivity of material can be improved, reinforces the structural stability in cyclic process, has
Conducive to the raising of high rate performance.Cobalt acid lithium matrix surface has one layer of clad, main component be compound containing Ti and Al,
The mixture of compound containing Ti and the compound containing Al can form solid solution with cobalt acid lithium matrix, and can form gradient on surface and mix
It is miscellaneous, both play the role of physical barriers, it is therefore prevented that the Co under high voltage condition3+Dissolving in the electrolytic solution, and enhance material
Expect surface texture stability in high voltage charge and discharge process, make its still keep under high voltages higher volumetric properties and
High rate performance.In addition, Ti elements react the Li generated with Li extra in cobalt acid lithium2TiO3Compound is that the good of Li ions is led
Body effectively improves the lithium ion conductivity of anode material for lithium-ion batteries, reduces sheet resistance, obtains excellent DCR
Energy.
Lithium cobaltate cathode material DCR performance boosts prepared by the present invention are mainly reflected in the improvement of the following performance of full battery：
1. full battery cryogenic property is promoted：At a lower temperature, discharge capacity of the cell is promoted, and initial discharge voltage is promoted；2. under room temperature
Full battery electric discharge temperature, which rises, to be declined, and storage performance is substantially improved.This lithium cobaltate cathode material electro-chemical test in 3~4.5V, with
35mA/g (0.2C) carries out charge and discharge, and reversible capacity reaches as high as 193.5mAh/g, and 1C capacity retention ratios are up to 99%, 4.4V head
All DCR 10%SOC can be reduced to 35.2 Ω.
Description of the drawings
Fig. 1 is positive electrode SEM figures prepared by the embodiment of the present invention 1.
Fig. 2 is positive electrode SEM figures prepared by the embodiment of the present invention 2.
Fig. 3 is positive electrode SEM figures prepared by the embodiment of the present invention 3.
Fig. 4 is positive electrode SEM figures prepared by the embodiment of the present invention 4.
Fig. 5 is positive electrode SEM figures prepared by the embodiment of the present invention 5.
Fig. 6 is positive electrode SEM figures prepared by the embodiment of the present invention 6.
Specific implementation mode
Features described above and advantage to enable the present invention are clearer and more comprehensible, special embodiment below, and institute's attached drawing is coordinated to make
Detailed description are as follows.
Embodiment 1
The present embodiment provides a kind of preparation methods of high-voltage lithium ion batteries material, and steps are as follows：
(1) Li/Co=1.005 is pressed:Lithium carbonate and cobalt oxide is added in 1 (molar ratio), while pressing Mg/Co=0.01:1 (rubs
That ratio) magnesium carbonate is added；Said mixture is sufficiently mixed using three-dimensional mixer or super mixing machine, is obtained finely dispersed
Once mixture.
(2) once mixture is sintered 10h under conditions of air atmosphere, 960~990 DEG C；The once sintered object of gained is adopted
It is crushed, is sieved with air-flow or high-speed rotating equipment, obtain cobalt acid lithium, control average grain diameter (D50) is 7~9 μm, pattern
For aggregate.
(3) Al/Co=0.0018 is pressed:1 (molar ratio), Ti/Co=0.003:1 (molar ratio) weighs alundum (Al2O3) and two
Above-mentioned cobalt acid lithium is added in titanium dioxide powder, is thoroughly mixed in super mixing machine uniformly, obtains secondary mixture.
(4) secondary mixture is sintered 10h under conditions of air atmosphere, 900~960 DEG C；After Temperature fall
It is crushed using machinery mill, control average grain diameter (D50) is at 7~9 μm, you can obtain the lithium cobaltate cathode material (such as
Shown in Fig. 1).
Using the lithium cobaltate cathode material of preparation as anode material of lithium battery, carbon black is conductive agent, Kynoar (PVDF)
For binder, electrode slice is made, using lithium metal as cathode, is assembled into simulation button cell.At 25 DEG C, 3.0~4.5V 0.2C fill
High rate performance is tested under discharging condition.As can be seen that it is 192.7mAh/g, 1C/0.2C to carry out reversible capability of charging and discharging with 0.2C
Capacity retention ratio 98%, 3.6V platforms conservation rate 99.3%.DCR is 42.3 Ω at 25 DEG C, 3.0~4.4V 10%SOC.
Embodiment 2
The present embodiment provides a kind of preparation methods of high-voltage lithium ion batteries material, and steps are as follows：
(1) Li/Co=1.020 is pressed:Lithium carbonate and cobalt oxide is added in 1 (molar ratio), while pressing Mg/Co=0.005:1 (rubs
That ratio) magnesium carbonate is added；Said mixture is sufficiently mixed using three-dimensional mixer or super mixing machine, is obtained finely dispersed
Once mixture.
(2) once mixture is sintered 8h under conditions of air atmosphere, 1000~1020 DEG C；The once sintered object of gained is adopted
It is crushed, is sieved with air-flow or high-speed rotating equipment, obtain cobalt acid lithium, control average grain diameter (D50) is 7~9 μm, pattern
For monocrystalline pattern.
(3) Al/Co=0.0018 is pressed:1 (molar ratio), Ti/Co=0.003:1 (molar ratio) weighs alundum (Al2O3) and two
Above-mentioned cobalt acid lithium is added in titanium dioxide powder, is thoroughly mixed in super mixing machine uniformly, obtains secondary mixture.
(4) secondary mixture is sintered 10h under conditions of air atmosphere, 900~960 DEG C；After Temperature fall
It is crushed using machinery mill, control average grain diameter (D50) is at 7~9 μm, you can obtain the lithium cobaltate cathode material (such as
Shown in Fig. 2).
Using the lithium cobaltate cathode material of preparation as anode material of lithium battery, carbon black is conductive agent, Kynoar (PVDF)
For binder, electrode slice is made, using lithium metal as cathode, is assembled into simulation button cell.At 25 DEG C, 3.0~4.5V 0.2C fill
High rate performance is tested under discharge stream part.As can be seen that it is 193.1mAh/g, 1C/0.2C to carry out reversible capability of charging and discharging with 0.2C
Capacity retention ratio 97.6%, 3.6V platforms conservation rate 98.9%.DCR is 68.4 Ω at 25 DEG C, 3.0~4.4V 10%SOC.
Embodiment 3
The present embodiment provides a kind of preparation methods of high-voltage lithium ion batteries material, and steps are as follows：
(1) Li/Co=1.005 is pressed:Lithium carbonate and cobalt oxide is added in 1 (molar ratio), while pressing Mg/Co=0.008:1 (rubs
That ratio) magnesium carbonate is added；Said mixture is sufficiently mixed using three-dimensional mixer or super mixing machine, is obtained finely dispersed
Once mixture.
(2) once mixture is sintered 10h under conditions of air atmosphere, 920~980 DEG C；The once sintered object of gained is adopted
It is crushed, is sieved with air-flow or high-speed rotating equipment, obtain cobalt acid lithium, control average grain diameter (D50) is 4~6 μm, pattern
For class monocrystalline pattern.
(3) Al/Co=0.0018 is pressed:1 (molar ratio), Ti/Co=0.002:1 (molar ratio) weighs alundum (Al2O3) and two
Above-mentioned cobalt acid lithium is added in titanium dioxide powder, is thoroughly mixed in super mixing machine uniformly, obtains secondary mixture.
(4) secondary mixture is sintered 2h under conditions of air atmosphere, 900~960 DEG C；Make after Temperature fall
It is crushed with machinery mill, control average grain diameter (D50) is at 5~7 μm, you can obtain described lithium cobaltate cathode material (such as Fig. 3
It is shown).
Using the lithium cobaltate cathode material of preparation as anode material of lithium battery, carbon black is conductive agent, Kynoar (PVDF)
For binder, electrode slice is made, using lithium metal as cathode, is assembled into simulation button cell.At 25 DEG C, 3.0~4.5V 0.2C fill
High rate performance is tested under discharge stream part.As can be seen that it is 193.5mAh/g, 1C/0.2C to carry out reversible capability of charging and discharging with 0.2C
Capacity retention ratio 98.6%, 3.6V platforms conservation rate 99.3%.DCR is 37.8 Ω at 25 DEG C, 3.0~4.4V 10%SOC.
Embodiment 4
The present embodiment provides a kind of preparation methods of high-voltage lithium ion batteries material, and steps are as follows：
(1) Li/Co=1.030 is pressed:Lithium carbonate and cobalt oxide is added in 1 (molar ratio), while pressing Mg/Co=0.005:1 (rubs
That ratio) magnesium carbonate is added；Said mixture is sufficiently mixed using three-dimensional mixer or super mixing machine, is obtained finely dispersed
Once mixture.
(2) once mixture is sintered 10h under conditions of air atmosphere, 920~1000 DEG C；The once sintered object of gained is adopted
It is crushed, is sieved with air-flow or high-speed rotating equipment, obtain cobalt acid lithium, control average grain diameter (D50) is 5~7 μm, pattern
For monocrystalline pattern.
(3) Al/Co=0.0018 is pressed:1 (molar ratio), Ti/Co=0.002:1 (molar ratio) weighs alundum (Al2O3) and two
Above-mentioned cobalt acid lithium is added in titanium dioxide powder, is thoroughly mixed in super mixing machine uniformly, obtains secondary mixture.
(4) secondary mixture is sintered 5h under conditions of air atmosphere, 900~960 DEG C；Make after Temperature fall
It is crushed with machinery mill, control average grain diameter (D50) is at 5~7 μm, you can obtain described lithium cobaltate cathode material (such as Fig. 4
It is shown).
Using the lithium cobaltate cathode material of preparation as anode material of lithium battery, carbon black is conductive agent, Kynoar (PVDF)
For binder, electrode slice is made, using lithium metal as cathode, is assembled into simulation button cell.At 25 DEG C, 3.0~4.5V 0.2C fill
High rate performance is tested under discharge stream part.As can be seen that it is 192.6mAh/g, 1C/0.2C to carry out reversible capability of charging and discharging with 0.2C
Capacity retention ratio 98.4%, 3.6V platforms conservation rate 99.1%.DCR is 45.8 Ω at 25 DEG C, 3.0~4.4V 10%SOC.
Embodiment 5
The present embodiment provides a kind of preparation methods of high-voltage lithium ion batteries material, and steps are as follows：
(1) Li/Co=1.002 is pressed:Lithium carbonate and cobalt oxide is added in 1 (molar ratio), while pressing Mg/Co=0.008:1 (rubs
That ratio) magnesium carbonate is added；Said mixture is sufficiently mixed using three-dimensional mixer or super mixing machine, is obtained finely dispersed
Once mixture.
(2) once mixture is sintered 12h under conditions of air atmosphere, 900 DEG C；The once sintered object of gained uses air-flow
Or high-speed rotating equipment is crushed, sieving, obtains cobalt acid lithium, control average grain diameter (D50) is 4~5.5 μm, and pattern is group
Aggressiveness.
(3) Al/Co=0.001 is pressed:1 (molar ratio), Ti/Co=0.002:1 (molar ratio) weighs boehmite and two
Above-mentioned cobalt acid lithium is added in titanium dioxide powder, is thoroughly mixed in super mixing machine uniformly, obtains secondary mixture.
(4) secondary mixture is sintered 10h under conditions of air atmosphere, 940~960 DEG C；After Temperature fall
It is crushed using machinery mill, control average grain diameter (D50) is at 4~5.5 μm, you can obtain the lithium cobaltate cathode material
(as shown in Figure 5).
Using the lithium cobaltate cathode material of preparation as anode material of lithium battery, carbon black is conductive agent, Kynoar (PVDF)
For binder, electrode slice is made, using lithium metal as cathode, is assembled into simulation button cell.At 25 DEG C, 3.0~4.5V 0.2C fill
High rate performance is tested under discharging condition.As can be seen that it is 193.5mAh/g, 1C/0.2C to carry out reversible capability of charging and discharging with 0.2C
Capacity retention ratio 99.1%, 3.6V platforms conservation rate 99.4%.DCR is 35.2 Ω at 25 DEG C, 3.0~4.4V 10%SOC.
Embodiment 6
The present embodiment provides a kind of preparation methods of high-voltage lithium ion batteries material, and steps are as follows：
(1) Li/Co=1.040 is pressed:Lithium carbonate and cobalt oxide is added in 1 (molar ratio), while pressing Mg/Co=0.005:1 (rubs
That ratio) magnesium carbonate is added；Said mixture is sufficiently mixed using three-dimensional mixer or super mixing machine, is obtained finely dispersed
Once mixture.
(2) once mixture is sintered 10h under conditions of air atmosphere, 980 DEG C；The once sintered object of gained uses air-flow
Or high-speed rotating equipment is crushed, sieving, obtains cobalt acid lithium, control average grain diameter (D50) is 7~8.5 μm, and pattern is single
It is brilliant.
(3) Al/Co=0.001 is pressed:1 (molar ratio) weighs boehmite, by Al/Co=0.001:1 (molar ratio) claims
Aluminium hydroxide is taken, by Ti/Co=0.001:1 (molar ratio) weighs titania powder, and above-mentioned cobalt acid lithium is added, in super mixing
It is thoroughly mixed in machine uniformly, obtains secondary mixture.
(4) secondary mixture is sintered 5h under conditions of air atmosphere, 1000 DEG C；Machine is used after Temperature fall
Tool mill is crushed, and control average grain diameter (D50) is at 7~8.5 μm, you can obtains the lithium cobaltate cathode material (such as Fig. 6 institutes
Show).
Using the lithium cobaltate cathode material of preparation as anode material of lithium battery, carbon black is conductive agent, Kynoar (PVDF)
For binder, electrode slice is made, using lithium metal as cathode, is assembled into simulation button cell.At 25 DEG C, 3.0~4.5V 0.2C fill
High rate performance is tested under discharging condition.As can be seen that it is 187.2mAh/g, 1C/0.2C to carry out reversible capability of charging and discharging with 0.2C
Capacity retention ratio 95.4%, 3.6V platforms conservation rate 98.9%.DCR is 72.8 Ω at 25 DEG C, 3.0~4.4V 10%SOC.
Comparative example 1
As the comparative example of embodiment 1, use announced application No. is 201610039657.8 Chinese invention is special
The method of profit prepares positive electrode, and steps are as follows：
(1) Li/Co=1.005 is pressed:Lithium carbonate and cobalt oxide is added in 1 (molar ratio), while pressing Mg/Co=0.01:1 (rubs
That ratio) magnesium carbonate is added；Said mixture is sufficiently mixed using three-dimensional mixer or super mixing machine, is obtained finely dispersed
Once mixture.
(2) once mixture is sintered 10h under conditions of air atmosphere, 960~990 DEG C；The once sintered object of gained is adopted
It is crushed, is sieved with air-flow or high-speed rotating equipment, obtain cobalt acid lithium, control average grain diameter (D50) is 7~9 μm, pattern
For aggregate.
(3) Al/Co=0.0018 is pressed:1 (molar ratio) takes aluminium isopropoxide to be dissolved in absolute ethyl alcohol, then according to Ti/Co
=0.003:Tetraisopropyl titanate is added in 1 (molar ratio), is stirring evenly and then adding into above-mentioned cobalt acid lithium, is thoroughly mixed, dry
After obtain secondary mixture.
(4) secondary mixture is sintered 10h under conditions of air atmosphere, 980 DEG C；Direct mistake after Temperature fall
Sieve, control average grain diameter (D50) is at 7~9 μm, you can obtains the lithium cobaltate cathode material.
Electrochemical property test：Test method is the same as embodiment 1.After tested, at 25 DEG C, 3.0~4.5V 0.2C charge and discharge items
It is 191.1mAh/g, 1C/0.2C capacity retention ratios 96.6%, the holding of 3.6V platforms to carry out reversible capability of charging and discharging under part with 0.2C
Rate 98.4%.DCR is 130.6 Ω at 25 DEG C, 3.0~4.4V 10%SOC.
Comparative example 2
As the comparative example of embodiment 1, comparative example using announced application No. is 201610039657.8 China
The another method of patent of invention prepares positive electrode, and steps are as follows：
(1) Li/Co=1.005 is pressed:Lithium carbonate and cobalt oxide is added in 1 (molar ratio), while pressing Mg/Co=0.005:1 (rubs
That ratio) magnesium carbonate is added；Said mixture is sufficiently mixed using three-dimensional mixer or super mixing machine, is obtained finely dispersed
Once mixture.
(2) once mixture is sintered 10h under conditions of air atmosphere, 980 DEG C；The once sintered object of gained uses air-flow
Or high-speed rotating equipment is crushed, sieving, obtains cobalt acid lithium, control average grain diameter (D50) is 7~9.5 μm, and pattern is group
Combinate form looks.
(3) Al/Co=0.0018 is pressed:1 (molar ratio), Ti/Co=0.002:1 (molar ratio) weighs alundum (Al2O3) and two
Above-mentioned cobalt acid lithium is added in titanium dioxide powder, is thoroughly mixed in super mixing machine uniformly, obtains secondary mixture.
(4) secondary mixture is sintered 5h under conditions of air atmosphere, 900~960 DEG C；Make after Temperature fall
It is crushed with machinery mill, control average grain diameter (D50) is at 7~9.5 μm, you can obtains two substandard products of cobalt acid lithium.
(5) Al/Co=0.0018 is pressed:1 (molar ratio), weighs aluminium isopropoxide, is dissolved into absolute ethyl alcohol.By above-mentioned cobalt acid
Two substandard products of lithium are added to (solid-to-liquid ratio 2 in the aluminium isopropoxide solution dissolved:1) after, stirring 1h, drying obtains pre-coated cobalt acid
Lithium.The pre-coated cobalt acid lithium is sintered 5h under conditions of air atmosphere, 600~650 DEG C, packaging of being sieved after Temperature fall
It obtains, obtains average grain diameter (D50) at 7~9.5 μm, you can obtain the lithium cobaltate cathode material.
Using the lithium cobaltate cathode material of preparation as anode material of lithium battery, carbon black is conductive agent, Kynoar (PVDF)
For binder, electrode slice is made, using lithium metal as cathode, is assembled into simulation button cell.At 25 DEG C, 3.0~4.5V 0.2C fill
High rate performance is tested under discharging condition.As can be seen that it is 189.7mAh/g, 1C/0.2C to carry out reversible capability of charging and discharging with 0.2C
Capacity retention ratio 95%, 3.6V platforms conservation rate 98.6%.DCR is 135.4 Ω at 25 DEG C, 3.0~4.4V 10%SOC.
The charge-discharge performance test data for the lithium cobaltate cathode material that above-described embodiment and comparative example are prepared is summarized in
Following table：
The charge-discharge performance of 1 lithium cobaltate cathode material of table
As seen from Table 1, the lithium cobaltate cathode material prepared by the present invention shows excellent reversible capacity, higher
Capacity retention ratio and platform conservation rate, and the DCR at 10%SOC shows apparent advantage.And comparative example 1, comparative example 2 are adopted
It is kept with lithium cobaltate cathode material its reversible capacity, the capacity that are prepared application No. is 201610039657.8 existing patented method
The lithium cobaltate cathode material that rate, platform conservation rate are prepared not as good as embodiment 1, and its most important DCR performance obviously deteriorates.
It can thus be seen that the solid cladding that the present invention uses is substantially better than the mixing alcoholic solution of the aluminium alcoholates and titanate esters of the existing patent
Liquid cladding, not only change on pattern, grain size various, be conducive to industrialized production, and it is equal by the improvement of secondary processes
Higher chemical property can be reached, especially novel DCR performances.
The above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited, the ordinary skill of this field
Personnel can be modified or replaced equivalently technical scheme of the present invention, without departing from the spirit and scope of the present invention, this
The protection domain of invention should be subject to described in claims.
Claims (10)
1. a kind of preparation method of high-voltage lithium ion batteries material, step include：
Using cobalt oxide and lithium carbonate as presoma, magnesium carbonate is added and is uniformly mixed, carries out first sintering and is crushed, obtain cobalt
Sour lithium matrix；
Aluminum oxide and titanium oxide are added into cobalt acid lithium matrix, is sintered and is crushed for the second time after mixing, obtained
Lithium cobaltate cathode material.
2. according to the method described in claim 1, it is characterized in that, it is 1 that the cobalt oxide and lithium carbonate, which press Li/Co molar ratios,:1
~1.04:1 configuration, magnesium carbonate are 0.005 by Mg/Co molar ratios:1~0.01:1 is added.
3. according to the method described in claim 1, it is characterized in that, the first sintering method is：In air atmosphere, 900
8~12h is sintered under conditions of~1020 DEG C.
4. according to the method described in claim 1, it is characterized in that, the average grain diameter D50 of the broken cobalt acid lithium matrix is 4
~9 μm.
5. according to the method described in claim 1, it is characterized in that, it is 0.001 that the aluminum oxide, which presses Al/Co molar ratios,:1~
0.002:1 is added, and the titanium oxide is 0.001 by Ti/Co molar ratios:1~0.003:1 is added.
6. according to the method described in claim 1, it is characterized in that, the aluminum oxide is alundum (Al2O3), aluminium hydroxide, one
At least one of boehmite；The titanium oxide includes titanium dioxide.
7. according to the method described in claim 1, it is characterized in that, second of sintering method is：In air atmosphere, 900
2~10h is sintered under conditions of~1000 DEG C.
8. according to the method described in claim 1, it is characterized in that, being mixed using three-dimensional mixer or super mixing machine.
9. a kind of high-voltage lithium ion batteries material prepared using any the methods of the claims 1-8, the material
Average grain diameter be 4~9 μm, pattern is monocrystalline pattern or aggregate pattern, including cobalt acid lithium matrix and is coated in cobalt acid lithium
Clad；Contain Al and Ti elements in the clad；The chemical formula of the cobalt acid lithium is Li1+xCo1-yMgyO2, wherein
0.002 ﹤ x≤0.04,0.005≤y ﹤ 0.01.
10. high-voltage lithium ion batteries material according to claim 9, which is characterized in that the substance of the clad is
Compound containing Ti and Al, or the mixture for compound containing Ti and the compound containing Al.
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| CN109761287A (en) * | 2018-12-29 | 2019-05-17 | 合肥融捷能源材料有限公司 | A kind of high-rate type lithium cobaltate and its preparation method and application |
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| CN112390296A (en) * | 2020-11-12 | 2021-02-23 | 合肥融捷能源材料有限公司 | Low-rate, high-compaction, high-capacity and high-voltage lithium cobaltate material and preparation method and application thereof |
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Application publication date: 20180727 |