CN105070897B - Lithium titanate material and preparation method thereof, the electrode plates using it, battery - Google Patents
Lithium titanate material and preparation method thereof, the electrode plates using it, battery Download PDFInfo
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- CN105070897B CN105070897B CN201510418331.1A CN201510418331A CN105070897B CN 105070897 B CN105070897 B CN 105070897B CN 201510418331 A CN201510418331 A CN 201510418331A CN 105070897 B CN105070897 B CN 105070897B
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- H—ELECTRICITY
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- 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
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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- H—ELECTRICITY
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- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
A kind of preparation method of lithium titanate material, it comprises the following steps:A. the compound of titanium is mixed with the solution containing peroxide radical ion, obtains precursor solution A;B. Li source compound is dissolved in above-mentioned precursor solution A, obtains precursor solution B;C. the precursor solution B is dried, obtains lithium titanate precursor;D. the lithium titanate precursor is sintered, obtains lithium titanate.The preparation method preparation technology of the lithium titanate material is simple, power consumption is low, environmentally friendly.In addition, the present invention also provides a kind of lithium titanate material as made from the preparation method of the lithium titanate material, a kind of electrode plates of the application lithium titanate material, a kind of battery of the application electrode plates.
Description
Technical field
The present invention relates to a kind of preparation method of lithium titanate material, lithium titanate material obtained by this method, using the titanium
The lithium ion battery of the electrode plates and application of sour the lithium material electrode plates.
Background technology
Lithium ion battery is widely used in each electronic product because of characteristic that is high with energy density, having extended cycle life
In electric automobile.Electrode material of the lithium titanate material of spinel structure as lithium ion battery, the body in charge and discharge process
Product changes small, Stability Analysis of Structures and the lithium ion diffusion admittance with three-dimensional structure, in addition, the embedding de- lithium current potential of lithium titanate material
Platform is high, and lithium ion is bigger than graphite in the intracell diffusion coefficient of lithium titanate, when quick charge and low temperature are charged, lithium ion
It will not deposit, therefore lithium titanate material has very excellent cyclic reversibility, security, low temperature charging and quick charge
Performance.However, the preparation method power consumption of existing lithium titanate material is high, preparation technology is complicated and obtained lithium titanate material
Cycle performance is poor.
The content of the invention
In view of this, it is necessary to provide that a kind of energy consumption is low and the preparation method of the simple lithium titanate material of technique.
A kind of lithium titanate material as made from the preparation method of above-mentioned lithium titanate material is provided in addition, there is a need to.
A kind of electrode plates using above-mentioned lithium titanate material are provided in addition, there is a need to.
A kind of lithium ion battery using above-mentioned electrode plates is provided in addition, there is a need to.
A kind of preparation method of lithium titanate material, it comprises the following steps:
A. the compound of titanium is mixed with the solution containing peroxide radical ion, obtains precursor solution A;
B. Li source compound is dissolved in above-mentioned precursor solution A, obtains precursor solution B;
C. the precursor solution B is dried, obtains lithium titanate precursor;
D. the lithium titanate precursor is sintered, obtains lithium titanate.
A kind of lithium titanate material as made from the preparation method of above-mentioned lithium titanate material, the lithium titanate material are by lithium titanate
The close solid micron-sized spherical lithium titanate particle that nanocrystalline growth in situ forms, the lithium titanate particle have spinelle knot
Structure, a diameter of 1~10 μm of the lithium titanate particle, the specific surface area of the lithium titanate particle is 1~10m2/ g, the lithium titanate particle
Tap density be 1.0~2.5g/cm3。
A kind of electrode plates, the electrode plates include conducting base and are attached to the above-mentioned lithium titanate material of the conducting base
Material.
A kind of lithium ion battery, including positive pole, negative pole and electrolyte, the negative or positive electrode of the lithium ion battery is including upper
State lithium titanate material.
[Ti is prepared by the reaction of the compound of hydrogen peroxide and titanium in the preparation method of the lithium titanate material of the present invention
(OH)3O2]-Ion, and by the concentration of diluent and solvent control precursor solution A, then add Li source compound, adding
During heat drying, reaction is promoted to generate the TiO of embedding lithium2, and balling-up of growing up, it is subsequently heat-treated to obtain the metatitanic acid of micron-scale
Lithium, the material tap density are big.Preparation technology is simple, power consumption is low, environmentally friendly.Use lithium titanate material made from the above method in addition
During electrode for lithium ion battery, the good cycle of the lithium ion battery and stably, the specific capacity conservation rate of electrode material
Height, the high rate performance of lithium ion battery are excellent.
Brief description of the drawings
Fig. 1 is the preparation method of the lithium titanate material of better embodiment of the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of the lithium titanate material obtained by embodiment 1.
Fig. 3 is the X-ray diffractogram of the lithium titanate material obtained by embodiment 1.
Fig. 4 is cycle performance of the lithium titanate material as the lithium ion battery of electrode material obtained by Application Example 1
Test result curve map.
Fig. 5 is high rate performance of the lithium titanate material as the lithium ion battery of electrode material obtained by Application Example 1
Test result curve map.
Main element symbol description
Nothing
Following embodiment will combine above-mentioned accompanying drawing and further illustrate the present invention.
Embodiment
Referring to Fig. 1, the preparation method of the lithium titanate material of the present invention, the lithium titanate material are mainly used in lithium ion battery
Electrode (not shown) in, it comprises the following steps:
Step S1, the compound of titanium is mixed with the solution containing peroxide radical ion, obtains precursor solution A.
Specifically, be first well mixed peroxide and solvent according to default ratio, mixed solution is obtained, then by titanium
Compound is added in the mixed solution and stirred, and is completely dissolved the compound of titanium, obtains the precursor solution A.The peroxide
The ratio of the amount of the material of the amount of the material of compound and the titanium elements in the compound of titanium is more than or equal to 1:1.
Wherein, the peroxide is hydrogen peroxide.The solvent can be water, preferably distilled water, deionized water, height
Pure water or ultra-pure water.The compound of the titanium include but is not limited in titanium chloride, titanium nitride, titanium carbide and titanyl sulfate one
Kind is several.Being generated in the precursor solution A has [Ti (OH)3O2]-Ion, generate [Ti (OH)3O2]-The reactional equation of ion
Formula is Ti4++H2O2+5OH-→[Ti(OH)3O2]-+2H2O。
Step S2, Li source compound is dissolved in above-mentioned precursor solution A, obtains precursor solution B.
Specifically, first a certain amount of diluent and the solvent are added in above-mentioned precursor solution A and be well mixed, so
Li source compound is added afterwards and is well mixed, and is completely dissolved Li source compound, is obtained faint yellow emulsus precursor solution B.Should
Diluent and solvent are used for the concentration for adjusting precursor solution A.Wherein the volume ratio of the diluent solution and solvent is preferably 1:
(0.1~10), the ratio of the amount of the material of elemental lithium and titanium elements is (4~5) in precursor solution B:5.The diluent can be with
For ketone solution, alcohol solution, ethers solution, arene solution etc., wherein, the ketone solution can be butanone, acetone, first
Ethyl ketone etc., the alcohol solution can be absolute ethyl alcohol, ethylene glycol, isopropanol, methanol etc., and the ethers solution can be ether, ring
Ethylene Oxide etc., the arene solution can be benzene,toluene,xylene etc..The Li source compound may be selected from but be not limited to acetic acid
One or more in lithium, lithium carbonate, lithium fluoride, lithium hydroxide, lithium oxalate and lithium chloride.
Step S3, the precursor solution B is dried, obtains solid lithium titanate precursor, is contained in the lithium titanate precursor
The TiO of embedding lithium2。
Specifically, by the way of above-mentioned precursor solution B is dried, make diluent in precursor liquid B and solvent complete
Portion volatilizees, and obtains the lithium titanate precursor of solid.Wherein, drying temperature be 60 DEG C~150 DEG C, the time used in drying be 10h with
On, drying course can promote [Ti (OH)3O2]-Hydrolysis generation TiO2, specifically hydrolyzing equation is:2[Ti(OH)3O2]-→
2TiO2+2H2O+O2+2OH-.In the present embodiment, the lithium titanate precursor is white powder.
Step S4, the lithium titanate precursor is sintered, obtains lithium titanate.
Specifically, the lithium titanate precursor is placed in stove 5~15h of sintering, wherein sintering temperature under protective atmosphere
For 500 DEG C~900 DEG C.Then room temperature is naturally cooled to furnace temperature, that is, obtains lithium titanate.The protective atmosphere is conventional use of argon
The inert gases such as gas.The lithium titanate is the close solid micron-sized spherical metatitanic acid formed by the nanocrystalline growth in situ of lithium titanate
Lithium particle (calls the spherical lithium titanate particle of micron in the following text), and this micron of spherical lithium titanate particle has spinel structure.This micron spherical
A diameter of 1~10 μm of lithium titanate particle, specific surface area are 1~10m2/ g, tap density are 1.0~2.5g/cm3。
The preparation method of the lithium titanate material, [Ti is prepared by the reaction of the compound of hydrogenperoxide steam generator and titanium
(OH)3O2]-, add the compound of lithium, under the conditions of heating, drying with [Ti (OH)3O2]-Reaction, the dioxy of obtained embedding lithium
Change titanium, the titanium dioxide of the embedding lithium has larger particle diameter, can obtain the spherical lithium titanate particle of larger-size micron, and
The tap density of obtained lithium titanate material is larger.
When the lithium titanate material being prepared into using the above method is used for into the electrode material of lithium ion battery, the lithium-ion electric
After pond circulates 500 weeks under the conditions of 10C/10C discharge and recharge, the specific capacity conservation rate of the electrode material of battery more than 90%,
10C charge/discharge capacity is 100.2~150.1mAh/g.
Below by specific embodiment, the present invention will be further described.
Embodiment 1
28ml deionized waters, the hydrogen peroxide that 16ml mass fractions are 20%~30% are well mixed, obtain mixed solution.
0.5g titanium nitride is added in above-mentioned mixed solution, stirring is completely dissolved it, obtains precursor solution A.
Isopropanol and 100ml deionized waters that 50ml mass fractions are 99.9% are added in above-mentioned precursor solution A simultaneously
It is well mixed, it is subsequently added into 0.3g lithium fluoride and is well mixed, be completely dissolved lithium fluoride, obtains faint yellow emulsus presoma
Solution B.
Precursor solution B is placed in 24h at 80 DEG C, is oven-dried precursor solution B, obtains the lithium titanate forerunner of white
Body.
The lithium titanate precursor is placed in stove and sinters 7h at argon atmosphere, 750 DEG C.Then it is natural with furnace temperature
Room temperature is cooled to, that is, obtains lithium titanate material, the lithium titanate material is the spherical lithium titanate particle of micron.
Embodiment 2
40mL deionized waters, the hydrogen peroxide that 12mL mass fractions are 20%~30% are well mixed, obtain mixed solution.
0.25g titanium carbide is added in above-mentioned mixed solution, stirring is completely dissolved titanium carbide, obtains precursor solution
A。
Isopropanol and 100ml deionized waters that 100ml mass fractions are 99.9% are added in above-mentioned precursor solution A simultaneously
It is well mixed, it is subsequently added into 0.3g lithium hydroxide and is well mixed, be completely dissolved lithium hydroxide, before obtains faint yellow emulsus
Drive liquid solution B.
Precursor solution B is placed in 36h at 80 DEG C, is oven-dried precursor solution B, obtains the lithium titanate forerunner of white
Body.
The lithium titanate precursor is placed in stove and sinters 5h at argon atmosphere, 700 DEG C.Then it is natural with furnace temperature
Room temperature is cooled to, that is, obtains lithium titanate material, the lithium titanate material is the spherical lithium titanate particle of micron.
Embodiment 3
20mL deionized waters, the hydrogen peroxide that 6mL mass fractions are 20%~30% are well mixed, obtain mixed solution.
0.25g titanium carbide is added in above-mentioned mixed solution, stirring is completely dissolved titanium carbide, obtains precursor solution
A。
Ethanol and 50ml deionized waters that 80ml mass fractions are 99.9% are added in above-mentioned precursor solution A and mixed
Uniformly, it is subsequently added into 0.5g lithium acetate and is well mixed, be completely dissolved lithium acetate, obtains faint yellow emulsus precursor solution
B。
Precursor solution B is placed in 36h at 80 DEG C, is oven-dried precursor solution B, obtains the lithium titanate forerunner of white
Body.
The lithium titanate precursor is placed in stove and sinters 7h at argon atmosphere, 700 DEG C.Then it is natural with furnace temperature
Room temperature is cooled to, that is, obtains lithium titanate material, the lithium titanate material is the spherical lithium titanate particle of micron.
Embodiment 4
50mL deionized waters, the hydrogen peroxide that 18mL mass fractions are 20%~30% are well mixed, obtain mixed solution.
0.75g titanium chloride is added in above-mentioned mixed solution, stirring is completely dissolved titanium chloride, obtains precursor solution
A。
Ethanol and 80ml deionized waters that 150ml mass fractions are 99.9% are added in above-mentioned precursor solution A and mixed
Close uniformly, be subsequently added into 2.5g lithium oxalate and be well mixed, be completely dissolved lithium oxalate, it is molten to obtain faint yellow emulsus presoma
Liquid B.
Precursor solution B is placed in 18h at 150 DEG C, is oven-dried precursor solution B, obtains the lithium titanate forerunner of white
Body.
The lithium titanate precursor is placed in stove and sinters 12h at argon atmosphere, 800 DEG C.Then with furnace temperature certainly
Room temperature so is cooled to, that is, obtains lithium titanate material, the lithium titanate material is the spherical lithium titanate particle of micron.
Embodiment 5
100mL deionized waters, the hydrogen peroxide that 64mL mass fractions are 20%~30% are well mixed, obtain mixing molten
Liquid.
2g titanyl sulfate is added in above-mentioned mixed solution, stirring is completely dissolved it, obtains precursor solution A.
Ethanol and 200ml deionized waters that 50ml mass fractions are 99.9% are added in above-mentioned precursor solution A and mixed
Close uniformly, be subsequently added into 1.5g lithium acetate and be well mixed, be completely dissolved lithium acetate, it is molten to obtain faint yellow emulsus presoma
Liquid B.
Precursor solution B is placed in 30h at 120 DEG C, is oven-dried precursor solution B, obtains the lithium titanate forerunner of white
Body.
The lithium titanate precursor is placed in stove and sinters 15h at argon atmosphere, 800 DEG C.Then with furnace temperature certainly
Room temperature so is cooled to, that is, obtains lithium titanate material, the lithium titanate material is the spherical lithium titanate particle of micron.
Further referring to Fig. 2~5, lithium titanate material made from above-described embodiment 1 is tested, obtains ESEM
Figure, X-ray diffractogram.Testing (should as the cycle performance and high rate performance of the lithium ion battery of electrode using lithium titanate and lithium piece
Method is the side of the performance for the lithium ion battery that the test that laboratory is commonly used uses the electrode plates as made from lithium titanate material
Method), respectively obtain cycle performance test result curve map and high rate performance test result curve map.The wherein lithium ion battery
Electrolyte is with LiPF6(lithium hexafluoro phosphate) is used as solute, using volume ratio as 1:1:1 ethylene carbonate, diethyl carbonate, carbon
Sour methyl ethyl ester is as solvent, the LiPF of configuration6Concentration is 1mol/L electrolyte.
As seen from Figure 2, the particle of obtained lithium titanate material is monodispersed, size uniformity spinel-type knot
The micron spheric granules of structure, and a diameter of 1~2 μm of micron spheric granules.
From the figure 3, it may be seen that obtained lithium titanate material crystalline phase is single and with the spinelle crystal formation titanium of very high crystalline
Sour lithium, other any dephasigns are not contained.
As seen from Figure 4, filled using obtained lithium titanate material as the lithium ion battery of electrode in 10C/10C
After 350 weeks are circulated under discharging condition, the specific capacity conservation rate of the lithium titanate electrode material of the lithium ion battery is 97.4%, performance
Go out very excellent cyclical stability.
As seen from Figure 5, using obtained lithium titanate material as the lithium ion battery of electrode, in 0.1C discharge and recharges
Specific capacity be 174.5mAh/g, the specific capacity of 0.5C discharge and recharges is 160.6mAh/g, and the specific capacity of 1C discharge and recharges is
The specific capacity of 155.7mAh/g, 2C discharge and recharge is 149.3mAh/g, and the specific capacities of 5C discharge and recharges is 130.4mAh/g, 10C charge and discharges
The specific capacity of electricity is 102.5mAh/g, and the specific capacity of 20C discharge and recharges is 70.5mAh/g, and the specific capacity of 30C discharge and recharges is
54.3mAh/g, show excellent high rate performance.
A kind of electrode plates (not shown), the electrode plates include conducting base and are attached to the above-mentioned titanium of the conducting base
Sour lithium material.
A kind of lithium ion battery (not shown), it is used in the electronic installations such as mobile phone, computer, electronic reader, electric car.
The lithium ion battery includes positive pole, negative pole and electrolyte, and the negative or positive electrode includes above-mentioned lithium titanate material.
[Ti is prepared by the reaction of the compound of hydrogen peroxide and titanium in the preparation method of the lithium titanate material of the present invention
(OH)3O2]-Ion, and by the concentration of diluent and solvent adjustment precursor solution A, lithium source is then added, in heating, drying
During, promote reaction to generate the TiO of embedding lithium2, and balling-up of growing up, then sinter and obtain the lithium titanate of micron-scale, the material
Expect that tap density is big.Preparation technology is simple, power consumption is low, environmentally friendly.It is used for lithium using lithium titanate material made from the above method in addition
During the electrode of ion battery, the good cycle of the lithium ion battery and stably, the specific capacity conservation rate of electrode material is high, battery
High rate performance it is excellent.
Those skilled in the art it should be appreciated that the embodiment of the above be intended merely to explanation the present invention,
And be not used as limitation of the invention, as long as within the spirit of the present invention, above example is made
It is appropriate to change and change all to fall within the scope of protection of present invention.
Claims (9)
1. a kind of preparation method of lithium titanate material, it comprises the following steps:
A. peroxide is proportionally mixed with solvent, obtains the solution containing peroxide radical ion, by the compound of titanium and institute
The solution mixing containing peroxide radical ion is stated, obtains precursor solution A, the compound of the titanium is selected from titanium chloride, titanium nitride, carbon
Change the one or more in titanium and titanyl sulfate, the peroxide is hydrogen peroxide, and being generated in the precursor solution A has
[Ti(OH)3O2]-Ion, generate [Ti (OH)3O2]-The reaction equation of ion is Ti4++H2O2+5OH-→[Ti(OH)3O2]-+
2H2O;
B. diluent and the solvent are added in precursor solution A and mixed, then by Li source compound be dissolved in it is above-mentioned before
Drive in liquid solution A, obtain precursor solution B, the volume ratio of the diluent and the solvent is 1:0.1-1:10, the solvent
For water, one or more of the diluent in ketone solution, alcohol solution, ethers solution and arene solution;
C. the precursor solution B is dried, obtains lithium titanate precursor;
D. the lithium titanate precursor is sintered, obtains lithium titanate.
2. the preparation method of lithium titanate material as claimed in claim 1, it is characterised in that:The amount and titanium of the material of peroxide
Compound in titanium elements material amount ratio be more than or equal to 1:1.
3. the preparation method of lithium titanate material as claimed in claim 2, it is characterised in that:Lithium member in the precursor solution B
Element and the ratio of the amount of the material of titanium elements are (4~5):5.
4. the preparation method of lithium titanate material as claimed in claim 1, it is characterised in that:The Li source compound is selected from acetic acid
One or more in lithium, lithium carbonate, lithium fluoride, lithium hydroxide, lithium oxalate and lithium chloride.
5. the preparation method of lithium titanate material as claimed in claim 1, it is characterised in that:The solvent be distilled water, go from
Sub- water, high purity water or ultra-pure water.
6. the preparation method of lithium titanate material as claimed in claim 1, it is characterised in that:The step c is:
More than 10h is dried at a temperature of precursor solution B is placed on into 60 DEG C~150 DEG C, obtains solid lithium titanate precursor;
The step d is:Lithium titanate precursor is placed in stove into 5~15h of sintering, wherein sintering temperature under protective atmosphere is
500~900 DEG C.
7. lithium titanate material made from a kind of preparation method of lithium titanate material as described in claim 1~6 any one, its
It is characterised by:The lithium titanate material is the close solid micron-sized spherical metatitanic acid formed by the nanocrystalline growth in situ of lithium titanate
Lithium particle, the lithium titanate particle have spinel structure, a diameter of 1~10 μm of the lithium titanate particle, the lithium titanate particle
Specific surface area is 1~10m2/ g, the tap density of the lithium titanate particle is 1.0~2.5g/cm3。
A kind of 8. electrode plates, it is characterised in that:The electrode plates include conducting base and be attached to the conducting base as power
Profit requires lithium titanate material made from the preparation method of the lithium titanate material described in 1~6 any one.
9. a kind of lithium ion battery, it includes positive pole, negative pole and electrolyte, it is characterised in that:The negative pole or positive pole are included such as
Lithium titanate material made from the preparation method of lithium titanate material described in claim 1~6 any one.
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CN108649189B (en) * | 2018-03-23 | 2021-02-12 | 浙江大学 | Titanium carbide/carbon core-shell nanowire array loaded nitrogen-doped lithium titanate composite material and preparation method and application thereof |
CN109336169B (en) * | 2018-09-29 | 2020-10-09 | 南京大学射阳高新技术研究院 | Controllable synthesis method and application of lithium titanate micron-sized spherical secondary structure |
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