CN110459750A - A kind of cathode material of lithium-ion power battery and preparation method thereof - Google Patents

A kind of cathode material of lithium-ion power battery and preparation method thereof Download PDF

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CN110459750A
CN110459750A CN201910777417.1A CN201910777417A CN110459750A CN 110459750 A CN110459750 A CN 110459750A CN 201910777417 A CN201910777417 A CN 201910777417A CN 110459750 A CN110459750 A CN 110459750A
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lithium
cathode material
ion power
power battery
solution
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CN110459750B (en
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宋婷
张燕
陈晨
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Inner Mongolia Huayang High Tech Material Technology Co ltd
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/058—Construction or manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • 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
    • H01M4/485—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
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The present invention provides a kind of cathode material of lithium-ion power battery and preparation method thereof, this method is the lithium titanate that codope V and Cr is prepared for using sol-gel method, the position the 16d doping for being doped to Ti ion, it is then granulated again using spray drying process, effectively improves initial capacity, cyclical stability and the tap density of lithium titanate.

Description

A kind of cathode material of lithium-ion power battery and preparation method thereof
Technical field
The present invention relates to the technical fields of cathode material of lithium-ion power battery, and in particular to a kind of lithium-ion-power cell Codope lithium titanate anode material and preparation method thereof.
Background technique
Lithium-ion-power cell has many advantages, such as to have extended cycle life high with energy density, is widely used in new-energy automobile Field, but at present due to the more skill of primary study in the problems such as its cruising ability is weak, safety is poor always new energy field Art direction.
Spinel lithium titanate as a kind of negative electrode material being concerned, is had the advantages that 1) lithium titanate is de- Almost zero strain before and after embedding lithium；2) intercalation potential is higher (1.55V), effectively Li dendrite can be avoided to generate, safety is higher；3) have There is very flat voltage platform；4) electrochemical diffusion coefficient and coulombic efficiency are high.
There is the 16d eight in the 8a tetrahedron gap of lithium ion occupy-place and titanium ion occupy-place in spinel lithium titanate structure Face body gap, when selecting Doped ions, it will usually consider which kind of site occupancy Doped ions used more preferably enter, if into The occupy-place of 16d octahedron is then more advantageous to the structure of stable spinel, so as to improve the capacity and cycle performance of electrode material； If causing lithium ion to be extruded into 16d, so that inverse spinel structure is formed, then the electrode obtained material and into 8a occupy-place The capacity and cycle performance of material can be different degrees of decline.
For this purpose, in view of the deficiencies of the prior art, the present invention is based on the chemical property for improving lithium titanate, using in metatitanic acid Codope V and Cr element in lithium, which is easier to enter the position 16d of Ti ion, to effectively improve lithium titanate Initial capacity and cyclical stability.
Summary of the invention
The present invention provides a kind of cathode material of lithium-ion power battery and preparation method thereof, and this method is solidifying using colloidal sol- Glue method is prepared for the lithium titanate of codope, is then granulated using spray drying process again, effectively improves lithium titanate Initial capacity and cyclical stability.
To achieve the above object, one aspect of the present invention provides a kind of cathode material of lithium-ion power battery, the cathode Material is the lithium titanate of dual element codope, and the dual element is transition metal element, described to be doped to Ti doping.
Further, chemical structural formula are as follows: Li4Ti5-x-yVxCryO12, wherein 0 < x≤0.3,0 y≤0.3 <.
Further, the structural formula of the negative electrode material is preferably Li4Ti4.7V0.2Cr0.1O12。
Further, the tap density of the negative electrode material is 1.0-2.0g/cm3, average grain diameter 50-800nm.
Another aspect of the present invention provides the preparation method of cathode material of lithium-ion power battery, includes the following steps:
A, according to molar ratio n (Li): n (Ti): n (V): n (Cr)=4: (5-x-y): x: y weighs a certain amount of titanium source dispersion In solvent, after being uniformly mixed, solution A is obtained；It weighs a certain amount of lithium source to be dissolved in solvent, stirs evenly, obtain To solution B；It weighs a certain amount of vanadium source to be scattered in solvent, after being uniformly mixed, obtains solution C；It weighs a certain amount of Chromium source be scattered in solvent, after being uniformly mixed, obtain solution D, wherein 0 < x≤0.3,0 y≤0.3 <；
B, under the action of stirring, after solution B is slowly added in solution A, then solution C and D is added simultaneously, obtains transparent Colloidal sol, continue stirring until formed gel forged under protective atmosphere in 400-600 DEG C after gained gel drying, grinding It burns, soaking time 2-5h, is then increased to 700-900 DEG C of calcining, soaking time 3-8h is cooled to room temperature, and is obtained through altogether The lithium titanate of doping；
C, the lithium titanate of codope made from a certain amount of step (b) is weighed, deionized water is added, being configured to concentration is 0.1- The slurry is spray-dried after carrying out ball milling, obtains the powder of uniform particle sizes, which is by the slurry of 0.3g/mL Li4Ti5-x-yVxCryO12。
Further, the lithium source is selected from least one of lithium acetate, lithium carbonate, lithium hydroxide, and the titanium source is selected from At least one of isopropyl titanate, butyl titanate, the vanadium source in sodium vanadate, potassium vanadate, ammonium metavanadate at least one Kind, at least one of the chromium source chromic nitrate, chromium chloride, the solvent are deionized water, ethyl alcohol or acetone, the protection gas Atmosphere is selected from nitrogen or argon gas, and the heating rate in the step (b) when calcining is 5-8 DEG C/min.
Further, the inlet temperature of the spray drying is 150-220 DEG C, and outlet temperature is 80-100 DEG C, and pressure is 0.1-0.3MPa。
Further, the ball milling is dry ball milling, time 1-5h.
Another aspect of the present invention provides a kind of lithium ion power cell cathode comprising copper foil and coated on copper foil Negative electrode slurry, the negative electrode slurry include cathode material of lithium-ion power battery above-mentioned.
Another aspect of the present invention provides a kind of lithium-ion-power cell comprising lithium-ion-power cell above-mentioned is negative Pole.
Compared with prior art, the present invention has the advantage that
(1) negative electrode material prepared by the present invention is Ti codope lithium titanates, easily using sol-gel method V and Cr Into Ti the positions 16d carry out codope, wherein V and Cr have synergistic effect, make gained negative electrode material initial capacity with And cyclical stability significantly improves.
(2) present invention is using being finally granulated again using spray drying process, after spray drying, gained particle size It is more uniform, and to be spherical, particle size is uniform, and tap density is high.
(3) slurry is carried out ball milling in advance before spray drying by the present invention, while controlling slurry concentration, so that the vibration of product Real density is higher, and performance is more preferable.
(4) material preparation process is simple, and the electrochemical performance of resulting materials has a good application prospect.
Specific embodiment
For a better understanding of the present invention, next combined with specific embodiments below the present invention is further explained, as described below to be The preferred embodiment of the present invention, it is noted that the contents of the present invention are not limited to following embodiment.
Embodiment 1
The butyl titanate point for weighing 16.33g according to molar ratio n (Li): n (Ti): n (V): n (Cr)=4: 4.8: 0.1: 0.1 It dissipates in 50mL dehydrated alcohol, after being uniformly mixed, obtains solution A；The LiAc for weighing 2.64g is dissolved in 10mL deionization It in water, stirs evenly, obtains solution B；Weigh the Na of 0.184g3VO4It is dissolved in 10mL deionized water, is uniformly mixed Afterwards, solution C is obtained；Weigh the Cr (NO of 0.238g3)3It is dissolved in 10mL deionized water, after being uniformly mixed, obtains molten Liquid D.
Under the action of magnetic agitation, after solution B is slowly added in solution A, then solution C and D is added simultaneously, obtains Bright colloidal sol continues stirring until forming gel, after gained gel drying, grinding, calcines in a nitrogen atmosphere in 500 DEG C, Soaking time is 3h, 5 DEG C/min of heating rate, is then increased to 800 DEG C of calcinings, and soaking time 5h is cooled to room temperature, obtains Lithium titanate through codope.
The lithium titanate for weighing codope made from 4g is scattered in 20mL deionized water, is configured to the slurry that concentration is 0.2g/mL The slurry is spray-dried by material after carrying out ball milling 2h, and wherein inlet temperature is 200 DEG C, and outlet temperature is 90 DEG C, pressure Power is 0.2MPa, obtains the powder of uniform particle sizes, which is Li4Ti4.8V0.1Cr0.1O12。
Embodiment 2
The butyl titanate point for weighing 15.99g according to molar ratio n (Li): n (Ti): n (V): n (Cr)=4: 4.7: 0.2: 0.1 It dissipates in 50mL dehydrated alcohol, after being uniformly mixed, obtains solution A；The LiAc for weighing 2.64g is dissolved in 10mL deionization It in water, stirs evenly, obtains solution B；Weigh the Na of 0.368g3VO4It is dissolved in 10mL deionized water, is uniformly mixed Afterwards, solution C is obtained；Weigh the Cr (NO of 0.238g3)3It is dissolved in 10mL deionized water, after being uniformly mixed, obtains molten Liquid D.
Under the action of magnetic agitation, after solution B is slowly added in solution A, then solution C and D is added simultaneously, obtains Bright colloidal sol continues stirring until forming gel, after gained gel drying, grinding, calcines in a nitrogen atmosphere in 500 DEG C, Soaking time is 3h, 5 DEG C/min of heating rate, is then increased to 800 DEG C of calcinings, and soaking time 5h is cooled to room temperature, obtains Lithium titanate through codope.
The lithium titanate for weighing codope made from 4g is scattered in 20mL deionized water, is configured to the slurry that concentration is 0.2g/mL The slurry is spray-dried by material after carrying out ball milling 2h, and wherein inlet temperature is 200 DEG C, and outlet temperature is 90 DEG C, pressure Power is 0.2MPa, obtains the powder of uniform particle sizes, which is Li4Ti4.7V0.2Cr0.1O12。
Embodiment 3
The butyl titanate point for weighing 15.65g according to molar ratio n (Li): n (Ti): n (V): n (Cr)=4: 4.6: 0.1: 0.3 It dissipates in 50mL dehydrated alcohol, after being uniformly mixed, obtains solution A；The LiAc for weighing 2.64g is dissolved in 10mL deionization It in water, stirs evenly, obtains solution B；Weigh the Na of 0.184g3VO4It is dissolved in 10mL deionized water, is uniformly mixed Afterwards, solution C is obtained；Weigh the Cr (NO of 0.714g3)3It is dissolved in 10mL deionized water, after being uniformly mixed, obtains molten Liquid D.
Under the action of magnetic agitation, after solution B is slowly added in solution A, then solution C and D is added simultaneously, obtains Bright colloidal sol continues stirring until forming gel, after gained gel drying, grinding, calcines in a nitrogen atmosphere in 500 DEG C, Soaking time is 3h, 5 DEG C/min of heating rate, is then increased to 800 DEG C of calcinings, and soaking time 5h is cooled to room temperature, obtains Lithium titanate through codope.
The lithium titanate for weighing codope made from 4g is scattered in 20mL deionized water, is configured to the slurry that concentration is 0.2g/mL The slurry is spray-dried by material after carrying out ball milling 2h, and wherein inlet temperature is 200 DEG C, and outlet temperature is 90 DEG C, pressure Power is 0.2MPa, obtains the powder of uniform particle sizes, which is Li4Ti4.6V0.1Cr0.3O12。
Comparative example 1
It is scattered in 50mL dehydrated alcohol, stirs according to the butyl titanate that molar ratio n (Li): n (Ti)=4: 5 weighs 17g After mixing, solution A is obtained；The LiAc for weighing 2.64g is dissolved in 10mL deionized water, is stirred evenly, is obtained solution B.Under the action of magnetic agitation, after solution B is slowly added in solution A, transparent colloidal sol is obtained, continues stirring until being formed Gel is calcined in 500 DEG C, soaking time 3h in a nitrogen atmosphere after gained gel drying, grinding, and 5 DEG C of heating rate/ Min is then increased to 800 DEG C of calcinings, and soaking time 5h is cooled to room temperature, and obtains spinelle Li4Ti5O12。
Through the foregoing embodiment, the specific test process of the present invention is as follows:, will be obtained in the glove box of argon gas protection Each embodiment composite material does negative electrode material, and the operation preparations such as formulated slurry, coating, drying go out cathode, and lithium piece is done to electrode, Celgard 2400 (PP/PE/PP) makees diaphragm, is dissolved in EC and DMC using the lithium hexafluoro phosphate of 1M as electrolyte, button electricity Pond shell model CR2016 is assembled into lithium battery.In the case where charge-discharge velocity is 0.1C, produced using Shenzhen Xin Wei company CT-4008 type multi-channel battery test instrument battery is tested under constant temperature (25 DEG C) in laboratory.Test number According to the capacity retention ratio after average grain diameter, tap density, initial capacity and 100 circulations including material is made.
After tested, data such as table 1.
If table 1 can be shown in, the Li of codope prepared by the present invention4Ti5O12Composite material various aspects of performance is excellent.And 1 chemical property of comparative example is more weaker in contrast.
The announcement and elaboration of book according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party Formula is changed and is modified.Therefore, the invention is not limited to the specific embodiments disclosed and described above, to of the invention Some equivalent modifications and change should also be as in scope of protection of the claims of the invention.In addition, although making in this specification With some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.

Claims (10)

1. a kind of cathode material of lithium-ion power battery, which is characterized in that the negative electrode material is the metatitanic acid of dual element codope Lithium, the dual element are transition metal element, described to be doped to Ti doping.
2. cathode material of lithium-ion power battery according to claim 1, which is characterized in that its chemical structural formula are as follows: Li4Ti5-x-yVxCryO12, wherein 0 < x≤0.3,0 y≤0.3 <.
3. -2 described in any item cathode material of lithium-ion power battery according to claim 1, which is characterized in that the cathode material The structural formula of material is preferably Li4Ti4.7V0.2Cr0.1O12。
4. cathode material of lithium-ion power battery according to claim 1-3, which is characterized in that the cathode material The tap density of material is 1.0-2.0g/cm3, average grain diameter 50-800nm.
5. a kind of preparation method of cathode material of lithium-ion power battery according to any one of claims 1-4, feature exist In including the following steps:
A, according to molar ratio n (Li): n (Ti): n (V): n (Cr)=4: (5-x-y): x: y weigh a certain amount of titanium source be scattered in it is molten In agent, after being uniformly mixed, solution A is obtained；It weighs a certain amount of lithium source to be dissolved in solvent, stir evenly, obtain molten Liquid B；It weighs a certain amount of vanadium source to be scattered in solvent, after being uniformly mixed, obtains solution C；Weigh a certain amount of chromium Source is scattered in solvent, after being uniformly mixed, obtains solution D, wherein 0 < x≤0.3,0 y≤0.3 <；
B, under the action of stirring, after solution B is slowly added in solution A, then solution C and D is added simultaneously, obtains transparent molten Glue continues stirring until forming gel, after gained gel drying, grinding, calcines, protect in 400-600 DEG C under protective atmosphere The warm time is 2-5h, is then increased to 700-900 DEG C of calcining, and soaking time 3-8h is cooled to room temperature, obtains through codope Lithium titanate；
C, the lithium titanate of codope made from a certain amount of step (b) is weighed, deionized water is added, being configured to concentration is 0.1- The slurry is spray-dried after carrying out ball milling, obtains the powder of uniform particle sizes, which is by the slurry of 0.3g/mL Li4Ti5-x-yVxCryO12。
6. the preparation method of cathode material of lithium-ion power battery according to claim 5, which is characterized in that the lithium source Selected from least one of lithium acetate, lithium carbonate, lithium hydroxide, the titanium source in isopropyl titanate, butyl titanate extremely Few one kind, the vanadium source is at least one of sodium vanadate, potassium vanadate, ammonium metavanadate, the chromium source chromic nitrate, chromium chloride At least one, the solvent be deionized water, ethyl alcohol or acetone, the protective atmosphere be selected from nitrogen or argon gas, the step (b) heating rate in when calcining is 5-8 DEG C/min.
7. according to the preparation method of the described in any item cathode material of lithium-ion power battery of claim 5-6, which is characterized in that The inlet temperature of the spray drying is 150-220 DEG C, and outlet temperature is 80-100 DEG C, pressure 0.1-0.3MPa.
8. according to the preparation method of the described in any item cathode material of lithium-ion power battery of claim 5-7, which is characterized in that The ball milling is dry ball milling, time 1-5h.
9. a kind of lithium ion power cell cathode, which is characterized in that it includes copper foil and coated in the negative electrode slurry on copper foil, institute Stating negative electrode slurry includes cathode material of lithium-ion power battery described in claim 1-8.
10. a kind of lithium-ion-power cell, which is characterized in that it includes lithium ion power cell cathode as claimed in claim 9.
CN201910777417.1A 2019-08-21 2019-08-21 Negative electrode material of lithium ion power battery and preparation method thereof Active CN110459750B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003217583A (en) * 2002-01-18 2003-07-31 Hitachi Maxell Ltd Composite electrode and electrochemical element using the same
CN102714309A (en) * 2009-03-06 2012-10-03 "埃利奥特"有限责任公司 Anode material for electrochemical cells and a method for producing same
CN102153137A (en) * 2011-05-18 2011-08-17 中南大学 Method for preparing spherical lithium titanate from inorganic titanium sources
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