CN104282935A - Lithium titanate battery and manufacturing method thereof - Google Patents
Lithium titanate battery and manufacturing method thereof Download PDFInfo
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- 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
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- H01—ELECTRIC ELEMENTS
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- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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- H01M10/00—Secondary cells; Manufacture thereof
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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- 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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- 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
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Abstract
The invention relates to a lithium titanate battery which comprises a positive plate, a negative plate, a diaphragm, electrolyte and an outer package, wherein the positive plate and the negative plate respectively consist of positive and negative current collectors and positive and negative pole materials coating the positive and negative current collectors; the positive pole material comprises a positive active substance, a positive conductive agent and a positive pole adhesive; and the positive active substance refers to an irregular ternary cathode material. Because the irregular ternary material is adopted in the positive pole, and the highest charging potential of a positive pole with high nickel containing ratio is 4.4V, the battery prepared from the material has extremely high specific capacity of larger than 180mAh/g and also has high stability. Moreover, the energy density of a battery cell assembled by matching a high specific capacity positive pole and a lithium titanate negative pole can be 90Wh/kg and is obviously higher than the energy density of the conventional lithium titanate battery.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to a kind of irregular type ternary-lithium titanate type lithium-ions battery and the manufacture method with high-energy-density.
Background technology
The negative material of current commercial lithium ion battery is all adopt graphite-like material with carbon element substantially.Material with carbon element has that thermal stability is high, good conductivity, Lithium-ion embeding deviate from that speed is fast, invertibity advantages of higher, but material with carbon element also exists some shortcomings: first charge-discharge efficiency is low, easily analyse lithium etc. when overcharging, compared with material with carbon element, and lithium titanate (Li
4ti
5o
12) there is obvious advantage: 1) be that a kind of removal lithium embedded close to zero volume inserts material, in charge and discharge process, recurring structure does not change, good cycle; 2) good charge and discharge platform is had; 3) theoretical specific capacity is 175 mAh/g, and actual specific capacity can reach 160 mAh/g, and concentrates on land regions; 4) do not react with electrolyte; 5) prices of raw and semifnished materials are cheap, prepare easier; 6) fast charging and discharging feature (order of magnitude higher than Carbon diffusion system) is possessed; It has possessed the possibility of long-life and high safety, no matter is therefore that its application prospect is all unanimously expected in plug-in hybrid vehicle or scale energy storage field, becomes the study hotspot in worldwide in recent years gradually.But current stage lithium titanate battery does not move towards market, one of them main cause is lithium titanate and common LiFePO 4 of anode material (LiFePO
4), LiMn2O4 (LiMn
2o
4), ternary material (LiNi
1/3co
1/3mn
1/3o
2) to be assembled into lithium ion battery energy density on the low side in collocation, generally only has 50Wh/kg – 75Wh/kg, main cause be lithium titanate anode Lithium-ion embeding, deviate from higher (the vs. Li of potential plateau
+/ Li=1.55V), far above graphite cathode Lithium-ion embeding, deviate from potential plateau (vs. Li
+/ Li=0 V), cause the output voltage of full battery generally to only have 1.7V about-2.5V, well below the 3.2-4.2V adopting graphite cathode lithium ion battery.In addition, above-mentioned LiFePO 4 of anode material (LiFePO
4), LiMn2O4 (LiMn
2o
4), ternary material (LiNi
1/3co
1/3mn
1/3o
2) gram volume generally lower than 160mAh/g, therefore this battery capacity is low, and voltage platform is low, and the low difficult problem of energy density is consistent all undecided.
China Patent Publication No. CN 1529382 A, publication date on September 15th, 2004, name is called the patent of invention of high-power plastic lithium-ion cell, this application case discloses a kind of high-power plastic lithium-ion cell, comprise positive plate, negative plate, dielectric film material, electrolyte material, soft compound package material and plastic casing, positive plate comprises positive electrode, adhesive, DBP, carbon black, aluminium net, negative plate comprises negative material, adhesive, DBP, carbon black, copper mesh, membrane materials for electrolyte comprises adhesive, silicon dioxide, DBP, positive plate, negative plate and dielectric film make unit battery core by heating compound, by superimposed for unit battery core, after adopting composite film material packaging, form assembled battery, draw lug, make assembled battery just, negative pole by ear pole material with just, negative terminal connects, assembled battery is placed in plastics and body, lid and box body are merged by ultrasonic wave, form complete high-power plastic lithium-ion cell.Its weak point is, negative material adopts graphite-like material with carbon element, and first charge-discharge efficiency is low, easily analyse lithium when overcharging.
Summary of the invention
The object of the invention is to negative material in order to solve existing lithium ion battery and adopt graphite-like material with carbon element, first charge-discharge efficiency is low, easily analyse the defect of lithium and a kind of irregular type ternary-lithium titanate type lithium ion battery with high-energy-density is provided when overcharging.
Another object of the present invention is to provide a kind of manufacture method of lithium titanate battery.
To achieve these goals, the present invention is by the following technical solutions:
A kind of lithium titanate battery, comprise positive plate, negative plate, barrier film, electrolyte and external packing, described positive plate, negative plate are made up of positive and negative collector and the positive and negative electrode material be coated on positive and negative electrode collector respectively, positive electrode comprises positive active material, positive conductive agent and positive electrode binder, and described positive active material is LiNi
0.33co
0.33mn
0.33o
2, LiNi
0.5co
0.3mn
0.2o
2, LiNi
0.6co
0.2mn
0.2o
2, LiNi
0.7co
0.15mn
0.15o
2, LiNi
0.8co
0.1mn
0.1o
2in at least one; In positive electrode, the mass percentage of each component is: positive active material 70-92%, positive conductive agent 1-15%, positive electrode binder 1-15%.
In the technical program, irregular type tertiary cathode material LiNi
0.33co
0.33mn
0.33o
2, LiNi
0.5co
0.3mn
0.2o
2, LiNi
0.6co
0.2mn
0.2o
2, LiNi
0.7co
0.15mn
0.15o
2, LiNi
0.8co
0.1mn
0.1o
2with high power capacity, low material cost, more stable, be layered composite structure material, under higher charging voltage, can have higher specific capacity, irregular ternary material is stratiform Li [Li
1/3mn
2/3] O
2, stratiform LiMO
2with spinel-type LiMe
2o
4composite construction;
LiNi
1/3co
1/3mn
1/3o
2under different temperatures and multiplying power, structural change is less, so material has good stability, and LiNi
1/3co
1/3mn
1/3o
2owing to adopting nickel manganese to replace expensive cobalt, material is made to have the price of relative moderate; LiNi
0.5co
0.3mn
0.2o
2what the gram volume of material can be made to play is higher, and improve the volume energy density of battery, capacity is high, and cost performance is good; LiNi
0.7co
0.15mn
0.15o
2improve the content energy of nickel, greatly promote the specific capacity of material, the content reducing cobalt can reduce material cost again, has the features such as specific capacity is high, cycle performance is excellent, high-temperature storage performance is good.
As preferably, negative material comprises negative electrode active material, cathode conductive agent, thickener and negative electrode binder, and described negative electrode active material is lithium titanate Li
4ti
5o
12cathode conductive agent is at least one in superconduction carbon black, crystalline flake graphite, carbon nano-tube, carbon fiber, negative electrode binder is butadiene-styrene rubber, organic olefin(e) acid or carboxylic acid esters, thickener is at least one in polymethacrylates, polyacrylonitrile, CMC, in negative material, the mass percentage of each component is: negative electrode active material, 67-86%, cathode conductive agent 3-15%, negative electrode binder 3-15%, thickener 2-3%.In the technical program, lithium titanate is that a kind of removal lithium embedded close to zero volume inserts material, and in charge and discharge process, recurring structure does not change, good cycle; There is good charge and discharge platform; Theoretical specific capacity is 175 mAh/g, and actual specific capacity can reach 160 mAh/g, and concentrates on land regions; Do not react with electrolyte; The prices of raw and semifnished materials are cheap, prepare easier.
As preferably, the mass ratio between positive active material is 1:1.
As preferably, the solvent of electrolyte is the mixed liquor of organic fluoride ester, organic carbonate, organic nitrile ester, and electrolyte is LiPF
6, LiBOB, LiBF
4, LiODFB, LiN (CF
3sO
2)
2, LiCF
3sO
3in at least one; Wherein, the volume ratio of organic fluoride ester, organic carbonate, organic nitrile ester is 1:2-3:1.5-2, LiPF in electrolyte
6content>=80%.
As preferably, take 1-METHYLPYRROLIDONE as the solvent making slurry, described positive electrode binder is Kynoar, butadiene-styrene rubber, organic olefin(e) acid or carboxylic acid esters, and conductive agent is at least one in superconduction carbon black, crystalline flake graphite, carbon nano-tube, carbon fiber.
As preferably, positive and negative electrode collector all adopts aluminium foil, and the thickness of aluminium foil is 15 ~ 20 μm.
A manufacture method for lithium titanate battery, described manufacture method comprises the following steps:
A) make positive and negative plate: by positive electrode dispersion in organic solvent, obtain anode sizing agent, be coated on plus plate current-collecting body after stirring, after drying at 100 ~ 140 DEG C, roll-in obtains positive plate; Negative material is soluble in water, be coated on after stirring on negative current collector, through roll-in negative plate after drying at 90 ~ 120 DEG C;
B) pole piece baking: above-mentioned pole piece is put into vacuum drying oven 130-150 DEG C of baking 24-36h, continue to vacuumize, control positive and negative electrode pole piece moisture≤200ppm;
C) make battery core: after positive and negative plate cutting step b) obtained, adopt laminated structure or takeup type structure to make battery core according to the order of positive plate, barrier film, negative plate;
D) welding packaging: by the positive and negative plate in battery core respectively by tab welding together, form positive and negative electrode exit, battery core is put into aluminium plastic packaging bag, draw positive and negative lug respectively, heat at tab place, the plastic cement of aluminium plastic bag and tab are fused, and the side of soft-package battery is open state, waits until electrolyte and injects;
E) fluid injection is encapsulated: after high-voltage electrolyte is injected battery core, seal liquid injection port;
F) forming and capacity dividing: by packaged battery preliminary filling, change into, namely obtain having after partial volume the lithium titanate soft package lithium battery of high-energy-density.
As preferably, the thickness in step a) after positive plate roll-in is 100 ~ 300 μm, and compacted density is 2.5 ~ 3.3g/cm
3; Thickness after negative plate roll-in is 60 ~ 200 μm, and compacted density is 1.3 ~ 2.0g/cm
3.
As preferably, be 1000-3000 mPas in the viscosity of anode sizing agent in step a), sieve after stirring, 100-120 order.
The invention has the beneficial effects as follows:
1) owing to have employed irregular type ternary material in positive pole, because the maximum charge current potential of nickeliferous ratio high type positive pole is at 4.4V (vs. Li/Li
+), thus battery prepared by this material has very high specific capacity, is greater than 180mAh/g, has higher stability simultaneously; Adopt height ratio capacity positive pole and the lithium titanate anode energy density of assembling battery core of arranging in pairs or groups to realize 90Wh/kg in the present invention, be significantly higher than existing lithium titanate battery energy density;
2) negative pole adopts lithium titanate material, and in embedding at lithium ion, the de-process of the negative pole of preparation, recurring structure does not change, good cycle; Lithium-ion embeding, deviate from higher (the vs. Li of potential plateau
+/ Li=1.55V), do not exist and analyse lithium problem, fail safe is high;
3) owing to the addition of high voltage bearing organic fluoride ester in electrolyte, make the electrochemical stability that electrolyte and electrode interface keep good under high voltages, comparatively under high charge voltage, negative pole will embed more lithium, can realize the high-energy-density of battery.
Accompanying drawing explanation
Fig. 1 is lithium titanate battery high/low temperature discharge curve prepared by embodiment 1.
Fig. 2 is lithium titanate battery rate discharge curves figure prepared by embodiment 2.
Fig. 3 is lithium titanate battery 55 degree of high temperature circulation curve charts prepared by embodiment 3.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further explained:
Embodiment 1
A manufacture method for lithium titanate battery, described manufacture method comprises the following steps:
A) positive and negative plate is made: the solution first segregation tetrafluoroethene (PVDF) being made into mass fraction 8% with 1-METHYLPYRROLIDONE (NMP), then adds conductive agent, and high speed shear disperses 2 hours, by positive electrode LiNi
0.33co
0.33mn
0.33o
2+ LiNi
0.5co
0.3mn
0.2o
2dispersion in organic solvent, anode sizing agent is obtained after stirring, high speed shear disperses 2 hours, and adding NMP adjusting viscosity is 1000 mPas, after high speed shear disperses 1 hour, anode sizing agent 120 order wire nettings sieve, it is on the aluminium foil of 20 microns that anode sizing agent after sieving is uniformly coated on thickness, 110 DEG C of oven dry, and the anode pole piece after drying is carried out roll-in, thickness after positive plate roll-in is 100 μm, and compacted density is 3.0g/cm
3; The mass percentage controlling each component in anode sizing agent is: positive active material 92%, positive conductive agent 2%, positive electrode binder 6%; Negative material is soluble in water, and coating thickness after cathode size sieves is on the aluminium foil of 20 microns, adopts 110 DEG C to dry pole piece, and the pole piece after drying is carried out roll-in, and the thickness after negative plate roll-in is 100 μm, and compacted density is 1.9g/cm
3; The mass percentage controlling each component is: negative electrode active material 82%, cathode conductive agent 6%, negative electrode binder 10%, thickener 2%; Wherein, positive conductive agent is superconduction carbon black and carbon nano-tube, and mass ratio is 1:1, and positive electrode binder is Kynoar; Cathode conductive agent superconduction carbon black and carbon fiber, mass ratio is 1:1, and negative electrode binder is butadiene-styrene rubber, and thickener is polymethacrylates and polyacrylonitrile, and volume ratio is 1:1;
B) pole piece baking: above-mentioned pole piece is put into vacuum drying oven 130 DEG C baking 36h, continue to vacuumize, control positive and negative electrode pole piece moisture≤200ppm;
C) make battery core: after positive and negative plate cutting step b) obtained, adopt laminated structure or takeup type structure to make battery core according to the order of positive plate, barrier film, negative plate;
D) welding packaging: by the positive and negative plate in battery core respectively by tab welding together, form positive and negative electrode exit, battery core is put into aluminium plastic packaging bag, draw positive and negative lug respectively, heat at tab place, the plastic cement of aluminium plastic bag and tab are fused, and the side of soft-package battery is open state, waits until electrolyte and injects;
E) fluid injection is encapsulated: after high-voltage electrolyte is injected battery core, seal liquid injection port; Wherein, electrolyte is the mixed liquor of organic fluoride ester, organic carbonate, organic nitrile ester, and the volume ratio of organic fluoride ester, organic carbonate, organic nitrile ester is 1:2:1.5; In electrolyte, electrolyte is LiPF
6, LiBOB and LiBF
4, in electrolyte, the mass percent of each component is: 85%LiPF
6, 10%LiBOB, 5%LiBF
4;
F) forming and capacity dividing: preliminary filling, change into and complete so that the system of 0.2C is disposable, constant current charge is to 3.2V, discharge the gas produced in charging process, then 1.0V is discharged to the system of 0.2C, the gas that will produce in battery charge and discharge process after charge and discharge cycles 2 times is discharged, and namely completes the manufacture of lithium titanate ion accumulator of the present invention.
Embodiment 2
A manufacture method for lithium titanate battery, described manufacture method comprises the following steps:
A) positive and negative plate is made: the solution first segregation tetrafluoroethene (PVDF) being made into mass fraction 8% with 1-METHYLPYRROLIDONE (NMP), then adds conductive agent, and high speed shear disperses 2 hours, by positive electrode LiNi
0.33co
0.33mn
0.33o
2+ LiNi
0.6co
0.2mn
0.2o
2dispersion in organic solvent, anode sizing agent is obtained after stirring, high speed shear disperses 2 hours, and adding NMP adjusting viscosity is 2000 mPas, after high speed shear disperses 1 hour, anode sizing agent 100 order wire nettings sieve, it is on the aluminium foil of 15 microns that anode sizing agent after sieving is uniformly coated on thickness, 100 DEG C of oven dry, and the anode pole piece after drying is carried out roll-in, thickness after positive plate roll-in is 200 μm, and compacted density is 2.5g/cm
3; The mass percentage controlling each component in anode sizing agent is: positive active material 90%, positive conductive agent 2%, positive electrode binder 8%; Negative material is soluble in water, and coating thickness after cathode size sieves is on the aluminium foil of 15 microns, dries pole piece with 100 DEG C, and the pole piece after drying is carried out roll-in, and the thickness after negative plate roll-in is 200 μm, and compacted density is 1.3g/cm
3; The mass percentage controlling each component is: negative electrode active material 86%, cathode conductive agent 4%, negative electrode binder 8%, thickener 2%; Wherein, positive conductive agent is crystalline flake graphite and carbon nano-tube, and mass ratio is 1:1, and positive electrode binder is butadiene-styrene rubber; Cathode conductive agent superconduction carbon black and carbon nano-tube, mass ratio is 1:1, and negative electrode binder is acrylic acid, and thickener is polyacrylonitrile and CMC, and volume ratio is 1:1;
B) pole piece baking: above-mentioned pole piece is put into vacuum drying oven 140 DEG C baking 24h, continue to vacuumize, control positive and negative electrode pole piece moisture≤200ppm;
C) make battery core: after positive and negative plate cutting step b) obtained, adopt laminated structure or takeup type structure to make battery core according to the order of positive plate, barrier film, negative plate;
D) welding packaging: by the positive and negative plate in battery core respectively by tab welding together, form positive and negative electrode exit, battery core is put into aluminium plastic packaging bag, draw positive and negative lug respectively, heat at tab place, the plastic cement of aluminium plastic bag and tab are fused, and the side of soft-package battery is open state, waits until electrolyte and injects;
E) fluid injection is encapsulated: after high-voltage electrolyte is injected battery core, seal liquid injection port; Wherein, electrolyte is the mixed liquor of organic fluoride ester, organic carbonate, organic nitrile ester, and the volume ratio of organic fluoride ester, organic carbonate, organic nitrile ester is 1:3:2; In electrolyte, electrolyte is LiPF
6, LiODFB and LiN (CF
3sO
2)
2, in electrolyte, the mass percent of each component is: 90%LiPF
6, 5%LiODFB, 5% LiN (CF
3sO
2)
2;
F) forming and capacity dividing: preliminary filling, change into and complete so that the system of 0.2C is disposable, constant current charge is to 3.2V, discharge the gas produced in charging process, then 1.0V is discharged to the system of 0.2C, the gas that will produce in battery charge and discharge process after charge and discharge cycles 2 times is discharged, and namely completes the manufacture of lithium titanate ion accumulator of the present invention.
Embodiment 3
A manufacture method for lithium titanate battery, described manufacture method comprises the following steps:
A) positive and negative plate is made: the solution first segregation tetrafluoroethene (PVDF) being made into mass fraction 8% with 1-METHYLPYRROLIDONE (NMP), then adds conductive agent, and high speed shear disperses 2 hours, by positive electrode LiNi
0.7co
0.15mn
0.15o
2+ LiNi
0.6co
0.2mn
0.2o
2dispersion in organic solvent, anode sizing agent is obtained after stirring, high speed shear disperses 2 hours, and adding NMP adjusting viscosity is 3000 mPas, after high speed shear disperses 1 hour, anode sizing agent 110 order wire nettings sieve, it is on the aluminium foil of 18 microns that anode sizing agent after sieving is uniformly coated on thickness, 140 DEG C of oven dry, and the anode pole piece after drying is carried out roll-in, thickness after positive plate roll-in is 300 μm, and compacted density is 3.3g/cm
3; The mass percentage controlling each component in anode sizing agent is: positive active material 90%, positive conductive agent 2%, positive electrode binder 8%; Negative material is soluble in water, and coating thickness after cathode size sieves is on the aluminium foil of 18 microns, dries pole piece with 140 DEG C, and the pole piece after drying is carried out roll-in, and the thickness after negative plate roll-in is 300 μm, and compacted density is 2g/cm
3; The mass percentage controlling each component is: negative electrode active material 86%, cathode conductive agent 4%, negative electrode binder 8%, thickener 2%; Wherein, positive conductive agent is carbon nano-tube and carbon fiber, and mass ratio is 1:1, and positive electrode binder is ethyl acetate; Cathode conductive agent superconduction carbon black and carbon nano-tube, mass ratio is 1:1, and negative electrode binder is isoamyl propionate, and thickener is polymethacrylates and CMC, and volume ratio is 1:1;
B) pole piece baking: above-mentioned pole piece is put into vacuum drying oven 150 DEG C baking 30h, continue to vacuumize, control positive and negative electrode pole piece moisture≤200ppm;
C) make battery core: after positive and negative plate cutting step b) obtained, adopt laminated structure or takeup type structure to make battery core according to the order of positive plate, barrier film, negative plate;
D) welding packaging: by the positive and negative plate in battery core respectively by tab welding together, form positive and negative electrode exit, battery core is put into aluminium plastic packaging bag, draw positive and negative lug respectively, heat at tab place, the plastic cement of aluminium plastic bag and tab are fused, and the side of soft-package battery is open state, waits until electrolyte and injects;
E) fluid injection is encapsulated: after high-voltage electrolyte is injected battery core, seal liquid injection port; Wherein, electrolyte is the mixed liquor of organic fluoride ester, organic carbonate, organic nitrile ester, and the volume ratio of organic fluoride ester, organic carbonate, organic nitrile ester is 1:2:2; In electrolyte, electrolyte is LiPF
6, LiCF
3sO
3, in electrolyte, the mass percent of each component is: 90%LiPF
6, 10% LiCF
3sO
3;
F) forming and capacity dividing: preliminary filling, change into and complete so that the system of 0.2C is disposable, constant current charge is to 3.2V, discharge the gas produced in charging process, then 1.0V is discharged to the system of 0.2C, the gas that will produce in battery charge and discharge process after charge and discharge cycles 2 times is discharged, and namely completes the manufacture of lithium titanate ion accumulator of the present invention.
Embodiment 4
A manufacture method for lithium titanate battery, described manufacture method comprises the following steps:
A) positive and negative plate is made: the solution first segregation tetrafluoroethene (PVDF) being made into mass fraction 8% with 1-METHYLPYRROLIDONE (NMP), then adds conductive agent, and high speed shear disperses 2 hours, by positive electrode LiNi
0.33co
0.33mn
0.33o
2+ LiNi
0.8co
0.1mn
0.1o
2dispersion in organic solvent, anode sizing agent is obtained after stirring, high speed shear disperses 2 hours, and adding NMP adjusting viscosity is 3000 mPas, after high speed shear disperses 1 hour, anode sizing agent 110 order wire nettings sieve, it is on the aluminium foil of 18 microns that anode sizing agent after sieving is uniformly coated on thickness, 140 DEG C of oven dry, and the anode pole piece after drying is carried out roll-in, thickness after positive plate roll-in is 300 μm, and compacted density is 3.3g/cm
3; The mass percentage controlling each component in anode sizing agent is: positive active material 92%, positive conductive agent 2%, positive electrode binder 6%; Negative material is soluble in water, and coating thickness after cathode size sieves is on the aluminium foil of 18 microns, dries pole piece with 140 DEG C, and the pole piece after drying is carried out roll-in, and the thickness after negative plate roll-in is 300 μm, and compacted density is 2g/cm
3; The mass percentage controlling each component is: negative electrode active material 86%, cathode conductive agent 4%, negative electrode binder 8%, thickener 2%; Wherein, positive conductive agent is carbon nano-tube and carbon fiber, and mass ratio is 1:1, and positive electrode binder is ethyl acetate; Cathode conductive agent superconduction carbon black and carbon nano-tube, mass ratio is 1:1, and negative electrode binder is isoamyl propionate, and thickener is polymethacrylates and CMC, and volume ratio is 1:1;
B) pole piece baking: above-mentioned pole piece is put into vacuum drying oven 150 DEG C baking 30h, continue to vacuumize, control positive and negative electrode pole piece moisture≤200ppm;
C) make battery core: after positive and negative plate cutting step b) obtained, adopt laminated structure or takeup type structure to make battery core according to the order of positive plate, barrier film, negative plate;
D) welding packaging: by the positive and negative plate in battery core respectively by tab welding together, form positive and negative electrode exit, battery core is put into aluminium plastic packaging bag, draw positive and negative lug respectively, heat at tab place, the plastic cement of aluminium plastic bag and tab are fused, and the side of soft-package battery is open state, waits until electrolyte and injects;
E) fluid injection is encapsulated: after high-voltage electrolyte is injected battery core, seal liquid injection port; Wherein, electrolyte is the mixed liquor of organic fluoride ester, organic carbonate, organic nitrile ester, and the volume ratio of organic fluoride ester, organic carbonate, organic nitrile ester is 1:2:2; In electrolyte, electrolyte is LiPF
6, LiCF
3sO
3, in electrolyte, the mass percent of each component is: 90%LiPF
6, 10% LiCF
3sO
3;
F) forming and capacity dividing: preliminary filling, change into and complete so that the system of 0.2C is disposable, constant current charge is to 3.2V, discharge the gas produced in charging process, then 1.0V is discharged to the system of 0.2C, the gas that will produce in battery charge and discharge process after charge and discharge cycles 2 times is discharged, and namely completes the manufacture of lithium titanate ion accumulator of the present invention.
Embodiment 5
A manufacture method for lithium titanate battery, described manufacture method comprises the following steps:
A) positive and negative plate is made: the solution first segregation tetrafluoroethene (PVDF) being made into mass fraction 8% with 1-METHYLPYRROLIDONE (NMP), then adds conductive agent, and high speed shear disperses 2 hours, by positive electrode LiNi
0.5co
0.3mn
0.2o
2+ LiNi
0.6co
0.2mn
0.2o
2dispersion in organic solvent, anode sizing agent is obtained after stirring, high speed shear disperses 2 hours, and adding NMP adjusting viscosity is 3000 mPas, after high speed shear disperses 1 hour, anode sizing agent 110 order wire nettings sieve, it is on the aluminium foil of 18 microns that anode sizing agent after sieving is uniformly coated on thickness, 140 DEG C of oven dry, and the anode pole piece after drying is carried out roll-in, thickness after positive plate roll-in is 300 μm, and compacted density is 3.3g/cm
3; The mass percentage controlling each component in anode sizing agent is: positive active material 90%, positive conductive agent 2%, positive electrode binder 8%; Negative material is soluble in water, and coating thickness after cathode size sieves is on the aluminium foil of 18 microns, dries pole piece with 140 DEG C, and the pole piece after drying is carried out roll-in, and the thickness after negative plate roll-in is 300 μm, and compacted density is 2g/cm
3; The mass percentage controlling each component is: negative electrode active material 86%, cathode conductive agent 4%, negative electrode binder 8%, thickener 2%; Wherein, positive conductive agent is carbon nano-tube and carbon fiber, and mass ratio is 1:1, and positive electrode binder is ethyl acetate; Cathode conductive agent superconduction carbon black and carbon nano-tube, mass ratio is 1:1, and negative electrode binder is isoamyl propionate, and thickener is polymethacrylates and CMC, and volume ratio is 1:1;
B) pole piece baking: above-mentioned pole piece is put into vacuum drying oven 150 DEG C baking 30h, continue to vacuumize, control positive and negative electrode pole piece moisture≤200ppm;
C) make battery core: after positive and negative plate cutting step b) obtained, adopt laminated structure or takeup type structure to make battery core according to the order of positive plate, barrier film, negative plate;
D) welding packaging: by the positive and negative plate in battery core respectively by tab welding together, form positive and negative electrode exit, battery core is put into aluminium plastic packaging bag, draw positive and negative lug respectively, heat at tab place, the plastic cement of aluminium plastic bag and tab are fused, and the side of soft-package battery is open state, waits until electrolyte and injects;
E) fluid injection is encapsulated: after high-voltage electrolyte is injected battery core, seal liquid injection port; Wherein, electrolyte is the mixed liquor of organic fluoride ester, organic carbonate, organic nitrile ester, and the volume ratio of organic fluoride ester, organic carbonate, organic nitrile ester is 1:2:2; In electrolyte, electrolyte is LiPF
6, LiCF
3sO
3, in electrolyte, the mass percent of each component is: 90%LiPF
6, 10% LiCF
3sO
3;
F) forming and capacity dividing: preliminary filling, change into and complete so that the system of 0.2C is disposable, constant current charge is to 3.2V, discharge the gas produced in charging process, then 1.0V is discharged to the system of 0.2C, the gas that will produce in battery charge and discharge process after charge and discharge cycles 2 times is discharged, and namely completes the manufacture of lithium titanate ion accumulator of the present invention.
Embodiment 6
A manufacture method for lithium titanate battery, described manufacture method comprises the following steps:
A) positive and negative plate is made: the solution first segregation tetrafluoroethene (PVDF) being made into mass fraction 8% with 1-METHYLPYRROLIDONE (NMP), then adds conductive agent, and high speed shear disperses 2 hours, by positive electrode LiNi
0.33co
0.33mn
0.33o
2+ LiNi
0.7co
0.15mn
0.15o
2+ LiNi
0.6co
0.2mn
0.2o
2dispersion in organic solvent, anode sizing agent is obtained after stirring, high speed shear disperses 2 hours, and adding NMP adjusting viscosity is 3000 mPas, after high speed shear disperses 1 hour, anode sizing agent 110 order wire nettings sieve, it is on the aluminium foil of 18 microns that anode sizing agent after sieving is uniformly coated on thickness, 140 DEG C of oven dry, and the anode pole piece after drying is carried out roll-in, thickness after positive plate roll-in is 300 μm, and compacted density is 3.3g/cm
3; The mass percentage controlling each component in anode sizing agent is: positive active material 70%, positive conductive agent 15%, positive electrode binder 15%; Negative material is soluble in water, and coating thickness after cathode size sieves is on the aluminium foil of 18 microns, dries pole piece with 140 DEG C, and the pole piece after drying is carried out roll-in, and the thickness after negative plate roll-in is 300 μm, and compacted density is 2g/cm
3; The mass percentage controlling each component is: negative electrode active material 67%, cathode conductive agent 15%, negative electrode binder 15%, thickener 3%; Wherein, positive conductive agent is carbon nano-tube and carbon fiber, and mass ratio is 1:1, and positive electrode binder is ethyl acetate; Cathode conductive agent superconduction carbon black and carbon nano-tube, mass ratio is 1:1, and negative electrode binder is isoamyl propionate, and thickener is polymethacrylates and CMC, and volume ratio is 1:1;
B) pole piece baking: above-mentioned pole piece is put into vacuum drying oven 150 DEG C baking 30h, continue to vacuumize, control positive and negative electrode pole piece moisture≤200ppm;
C) make battery core: after positive and negative plate cutting step b) obtained, adopt laminated structure or takeup type structure to make battery core according to the order of positive plate, barrier film, negative plate;
D) welding packaging: by the positive and negative plate in battery core respectively by tab welding together, form positive and negative electrode exit, battery core is put into aluminium plastic packaging bag, draw positive and negative lug respectively, heat at tab place, the plastic cement of aluminium plastic bag and tab are fused, and the side of soft-package battery is open state, waits until electrolyte and injects;
E) fluid injection is encapsulated: after high-voltage electrolyte is injected battery core, seal liquid injection port; Wherein, electrolyte is the mixed liquor of organic fluoride ester, organic carbonate, organic nitrile ester, and the volume ratio of organic fluoride ester, organic carbonate, organic nitrile ester is 1:2:2; In electrolyte, electrolyte is LiPF
6, LiCF
3sO
3, in electrolyte, the mass percent of each component is: 90%LiPF
6, 10% LiCF
3sO
3;
F) forming and capacity dividing: preliminary filling, change into and complete so that the system of 0.2C is disposable, constant current charge is to 3.2V, discharge the gas produced in charging process, then 1.0V is discharged to the system of 0.2C, the gas that will produce in battery charge and discharge process after charge and discharge cycles 2 times is discharged, and namely completes the manufacture of lithium titanate ion accumulator of the present invention.
Embodiment 7
A manufacture method for lithium titanate battery, described manufacture method comprises the following steps:
A) positive and negative plate is made: the solution first segregation tetrafluoroethene (PVDF) being made into mass fraction 8% with 1-METHYLPYRROLIDONE (NMP), then adds conductive agent, and high speed shear disperses 2 hours, by positive electrode LiNi
0.33co
0.33mn
0.33o
2+ LiNi
0.5co
0.3mn
0.2o
2+ LiNi
0.6co
0.2mn
0.2o
2+ LiNi
0.7co
0.15mn
0.15o
2+ LiNi
0.8co
0.1mn
0.1o
2dispersion in organic solvent, anode sizing agent is obtained after stirring, high speed shear disperses 2 hours, and adding NMP adjusting viscosity is 2000 mPas, after high speed shear disperses 1 hour, anode sizing agent 100 order wire nettings sieve, it is on the aluminium foil of 15 microns that anode sizing agent after sieving is uniformly coated on thickness, 100 DEG C of oven dry, and the anode pole piece after drying is carried out roll-in, thickness after positive plate roll-in is 200 μm, and compacted density is 2.5g/cm
3; The mass percentage controlling each component in anode sizing agent is: positive active material 90%, positive conductive agent 3%, positive electrode binder 7%; Negative material is soluble in water, and coating thickness after cathode size sieves is on the aluminium foil of 15 microns, dries pole piece with 100 DEG C, and the pole piece after drying is carried out roll-in, and the thickness after negative plate roll-in is 200 μm, and compacted density is 1.3g/cm
3; The mass percentage controlling each component is: negative electrode active material 86%, cathode conductive agent 4%, negative electrode binder 8%, thickener 2%; Wherein, positive conductive agent is crystalline flake graphite and carbon nano-tube, and mass ratio is 1:1, and positive electrode binder is butadiene-styrene rubber; Cathode conductive agent superconduction carbon black and carbon nano-tube, mass ratio is 1:1, and negative electrode binder is acrylic acid, and thickener is polyacrylonitrile and CMC, and volume ratio is 1:1;
B) pole piece baking: above-mentioned pole piece is put into vacuum drying oven 140 DEG C baking 24h, continue to vacuumize, control positive and negative electrode pole piece moisture≤200ppm;
C) make battery core: after positive and negative plate cutting step b) obtained, adopt laminated structure or takeup type structure to make battery core according to the order of positive plate, barrier film, negative plate;
D) welding packaging: by the positive and negative plate in battery core respectively by tab welding together, form positive and negative electrode exit, battery core is put into aluminium plastic packaging bag, draw positive and negative lug respectively, heat at tab place, the plastic cement of aluminium plastic bag and tab are fused, and the side of soft-package battery is open state, waits until electrolyte and injects;
E) fluid injection is encapsulated: after high-voltage electrolyte is injected battery core, seal liquid injection port; Wherein, electrolyte is the mixed liquor of organic fluoride ester, organic carbonate, organic nitrile ester, and the volume ratio of organic fluoride ester, organic carbonate, organic nitrile ester is 1:3:2; In electrolyte, electrolyte is LiPF
6, LiBOB, LiBF
4, LiODFB, LiN (CF
3sO
2)
2with LiCF
3sO
3, in electrolyte, the mass percent of each component is: 80%LiPF
6, 2%LiBOB, 6%LiBF
4, 5%LiODFB, 4%LiN (CF
3sO
2)
2with 3%LiCF
3sO
3;
F) forming and capacity dividing: preliminary filling, change into and complete so that the system of 0.2C is disposable, constant current charge is to 3.2V, discharge the gas produced in charging process, then 1.0V is discharged to the system of 0.2C, the gas that will produce in battery charge and discharge process after charge and discharge cycles 2 times is discharged, and namely completes the manufacture of lithium titanate ion accumulator of the present invention.
By the discharge test of lithium titanate battery at-20 DEG C, 0 DEG C, 25 DEG C, 55 DEG C obtained for embodiment 1, the results are shown in Figure 1;
Lithium titanate battery different multiplying obtained for embodiment 2 is put a test, the results are shown in Figure 2;
Lithium titanate battery obtained for embodiment 3 is done loop test at 55 DEG C, the results are shown in Figure 3.
Claims (9)
1. a lithium titanate battery, comprise positive plate, negative plate, barrier film, electrolyte and external packing, described positive plate, negative plate are made up of positive and negative collector and the positive and negative electrode material be coated on positive and negative electrode collector respectively, it is characterized in that, positive electrode comprises positive active material, positive conductive agent and positive electrode binder, and described positive active material is LiNi
0.33co
0.33mn
0.33o
2, LiNi
0.5co
0.3mn
0.2o
2, LiNi
0.6co
0.2mn
0.2o
2, LiNi
0.7co
0.15mn
0.15o
2, LiNi
0.8co
0.1mn
0.1o
2in at least one; In positive electrode, the mass percentage of each component is: positive active material 70-92%, positive conductive agent 2-15%, positive electrode binder 6-15%.
2. a kind of lithium titanate battery according to claim 1, is characterized in that, negative material comprises negative electrode active material, cathode conductive agent, thickener and negative electrode binder, and described negative electrode active material is lithium titanate Li
4ti
5o
12cathode conductive agent is at least one in superconduction carbon black, crystalline flake graphite, carbon nano-tube, carbon fiber, negative electrode binder is butadiene-styrene rubber, organic olefin(e) acid or carboxylic acid esters, thickener is at least one in polymethacrylates, polyacrylonitrile, CMC, in negative material, the mass percentage of each component is: negative electrode active material, 67-86%, cathode conductive agent 3-15%, negative electrode binder 3-15%, thickener 2-3%.
3. a kind of lithium titanate battery according to claim 1, is characterized in that, the mass ratio between positive active material is 1:1.
4. a kind of lithium titanate battery according to claim 1 and 2, is characterized in that, the solvent of electrolyte is the mixed liquor of organic fluoride ester, organic carbonate, organic nitrile ester, and electrolyte is LiPF
6, LiBOB, LiBF
4, LiODFB, LiN (CF
3sO
2)
2, LiCF
3sO
3in at least one; Wherein, the volume ratio of organic fluoride ester, organic carbonate, organic nitrile ester is 1:2-3:1.5-2, LiPF in electrolyte
6content>=80%.
5. a kind of lithium titanate battery according to claim 1, it is characterized in that, take 1-METHYLPYRROLIDONE as the solvent making slurry, described positive electrode binder is Kynoar; butadiene-styrene rubber, organic olefin(e) acid or carboxylic acid esters, conductive agent is selected from least one in superconduction carbon black, crystalline flake graphite, carbon nano-tube, carbon fiber.
6. a kind of lithium titanate battery according to claim 1 or 2 or 3 or 5, it is characterized in that, positive and negative electrode collector all adopts aluminium foil, and the thickness of aluminium foil is 15 ~ 20 μm.
7. a manufacture method for a kind of lithium titanate battery as claimed in claim 1, is characterized in that, described manufacture method comprises the following steps:
A) make positive and negative plate: by positive electrode dispersion in organic solvent, obtain anode sizing agent, be coated on plus plate current-collecting body after stirring, after drying at 100 ~ 140 DEG C, roll-in obtains positive plate; Negative material is soluble in water, be coated on after stirring on negative current collector, through roll-in negative plate after drying at 90 ~ 120 DEG C;
B) pole piece baking: above-mentioned pole piece is put into vacuum drying oven 130-150 DEG C of baking 24-36h, continue to vacuumize, control positive and negative electrode pole piece moisture≤200ppm;
C) make battery core: after positive and negative plate cutting step b) obtained, adopt laminated structure or takeup type structure to make battery core according to the order of positive plate, barrier film, negative plate;
D) welding packaging: by the positive and negative plate in battery core respectively by tab welding together, form positive and negative electrode exit, battery core is put into aluminium plastic packaging bag, draw positive and negative lug respectively, heat at tab place, the plastic cement of aluminium plastic bag and tab are fused, and the side of soft-package battery is open state, waits until electrolyte and injects;
E) fluid injection is encapsulated: after high-voltage electrolyte is injected battery core, seal liquid injection port;
F) forming and capacity dividing: by packaged battery preliminary filling, change into, namely obtain having after partial volume the lithium titanate soft package lithium battery of high-energy-density.
8. the manufacture method of a kind of lithium titanate battery according to claim 7, is characterized in that, the thickness in step a) after positive plate roll-in is 100 ~ 300 μm, and compacted density is 2.5 ~ 3.3g/cm
3; Thickness after negative plate roll-in is 60 ~ 200 μm, and compacted density is 1.3 ~ 2.0g/cm
3.
9. the manufacture method of a kind of lithium titanate battery according to claim 7, is characterized in that, is 1000-3000 mPas, sieves after stirring, 100-120 order in step a) in the viscosity of anode sizing agent.
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| CN105680052A (en) * | 2016-01-14 | 2016-06-15 | 镇江智联德科技有限公司 | Method for improving performance of conductive agent material of energy storage battery |
| CN106328925A (en) * | 2015-06-30 | 2017-01-11 | 宁德时代新能源科技股份有限公司 | Lithium ion secondary battery and positive pole piece thereof |
| CN107256979A (en) * | 2017-06-22 | 2017-10-17 | 北京圣比和科技有限公司 | A kind of 3V level lithium-ion-power cells and its preparation based on lithium titanate anode |
| CN107974014A (en) * | 2016-10-21 | 2018-05-01 | 苏州今道创业投资有限公司 | A kind of preparation method of metatitanic acid micro-nano mitron/PVDF composite membranes |
| CN108232285A (en) * | 2017-12-30 | 2018-06-29 | 骆驼集团新能源电池有限公司 | A kind of high magnification lithium titanate battery and preparation method thereof |
| CN109119631A (en) * | 2017-06-26 | 2019-01-01 | 宁德时代新能源科技股份有限公司 | Secondary battery |
| CN109119599A (en) * | 2017-06-26 | 2019-01-01 | 宁德时代新能源科技股份有限公司 | Secondary battery and preparation method thereof |
| CN109378520A (en) * | 2018-11-13 | 2019-02-22 | 上海电气国轩新能源科技有限公司 | A kind of nickle cobalt lithium manganate and lithium titanate system battery and preparation method thereof |
| CN110335991A (en) * | 2019-07-15 | 2019-10-15 | 骆驼集团武汉光谷研发中心有限公司 | A kind of long circulation life battery and preparation method thereof |
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| CN106328925A (en) * | 2015-06-30 | 2017-01-11 | 宁德时代新能源科技股份有限公司 | Lithium ion secondary battery and positive pole piece thereof |
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| CN107256979A (en) * | 2017-06-22 | 2017-10-17 | 北京圣比和科技有限公司 | A kind of 3V level lithium-ion-power cells and its preparation based on lithium titanate anode |
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| CN109378520A (en) * | 2018-11-13 | 2019-02-22 | 上海电气国轩新能源科技有限公司 | A kind of nickle cobalt lithium manganate and lithium titanate system battery and preparation method thereof |
| CN109378520B (en) * | 2018-11-13 | 2021-03-26 | 上海电气国轩新能源科技有限公司 | Nickel cobalt lithium manganate and lithium titanate system battery and preparation method thereof |
| CN110335991A (en) * | 2019-07-15 | 2019-10-15 | 骆驼集团武汉光谷研发中心有限公司 | A kind of long circulation life battery and preparation method thereof |
| WO2023221121A1 (en) * | 2022-05-20 | 2023-11-23 | 宁德时代新能源科技股份有限公司 | Non-aqueous electrolyte and secondary battery comprising same, battery module, battery pack, and electric device |
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Address after: 311215 Xiaoshan economic and Technological Development Zone, Zhejiang, No. two road, building No. 118, No. Applicant after: Universal A 1 System Co., Ltd Applicant after: Wanxiang Electric Vehicle Co., Ltd. Applicant after: Wanxiang Group Corporation Address before: 311215 Xiaoshan economic and Technological Development Zone, Zhejiang, No. two road, building No. 118, No. Applicant before: ZHEJIANG WANXIANG YINENG POWER BATTERY CO., LTD. Applicant before: Wanxiang Electric Vehicle Co., Ltd. Applicant before: Wanxiang Group Corporation |
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Free format text: CORRECT: APPLICANT; FROM: ZHEJIANG WANXIANG YINENG POWER BATTERY CO., LTD. TO: WANXIANG A123 SYSTEMS CO., LTD. |
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Address after: 311215 Xiaoshan economic and Technological Development Zone, Zhejiang District, No. two road, building No. 855, No. Applicant after: Wanxiang 123 Co Ltd Applicant after: Wanxiang Electric Vehicle Co., Ltd. Applicant after: Wanxiang Group Corporation Address before: 311215 Xiaoshan economic and Technological Development Zone, Zhejiang, No. two road, building No. 118, No. Applicant before: Universal A 1 System Co., Ltd Applicant before: Wanxiang Electric Vehicle Co., Ltd. Applicant before: Wanxiang Group Corporation |
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Granted publication date: 20180323 Termination date: 20180711 |