CN105070897A - Lithium titanate material and preparation method thereof, electrode plate using lithium titanate material, and battery - Google Patents
Lithium titanate material and preparation method thereof, electrode plate using lithium titanate material, and battery Download PDFInfo
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- CN105070897A CN105070897A CN201510418331.1A CN201510418331A CN105070897A CN 105070897 A CN105070897 A CN 105070897A CN 201510418331 A CN201510418331 A CN 201510418331A CN 105070897 A CN105070897 A CN 105070897A
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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
- H01M4/36—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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- 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
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Abstract
The invention discloses a preparation method of a lithium titanate material. The preparation method comprises the following steps: (a) mixing a compound of titanium with a solution containing peroxide ions to obtain a precursor solution A; (b) dissolving a lithium source compound into the precursor solution A to obtain a precursor solution B; (c) drying the precursor solution B to obtain a lithium titanate precursor; and (d) sintering the lithium titanate precursor to obtain lithium titanate. The preparation method of the lithium titanate material is simple in preparation technology, low in energy consumption and environment-friendly. In addition, the invention further provides the lithium titanate material prepared by the preparation method of the lithium titanate material, an electrode plate using the lithium titanate material and a battery using the electrode plate.
Description
Technical field
The present invention relates to a kind of preparation method of lithium titanate material, lithium titanate material obtained by this method, apply the electrode plates of this lithium titanate material and apply the lithium ion battery of this electrode plates.
Background technology
Energy density is high because having for lithium ion battery, the characteristic that has extended cycle life and being widely used in each electronic product and electric automobile.The lithium titanate material of spinel structure is as the electrode material of lithium ion battery, little, the Stability Analysis of Structures of change in volume in charge and discharge process and there is the lithium ion diffusion admittance of three-dimensional structure, in addition, the doff lithium potential plateau of lithium titanate material is high, lithium ion is larger than graphite at the intracell diffusion coefficient of lithium titanate, when quick charge and low temperature charging, lithium ion also can not deposit, and therefore lithium titanate material has very excellent cyclic reversibility, fail safe, low temperature charging and the performance of quick charge.But the preparation method of existing lithium titanate material consumes energy high, complicated process of preparation and the cycle performance of obtained lithium titanate material is poor.
Summary of the invention
In view of this, be necessary to provide a kind of energy consumption low and the preparation method of the simple lithium titanate material of technique.
Separately, there is a need to provide a kind of lithium titanate material obtained by the preparation method of above-mentioned lithium titanate material.
Separately, there is a need to provide a kind of electrode plates applying above-mentioned lithium titanate material.
Separately, there is a need to provide a kind of lithium ion battery applying above-mentioned electrode plates.
A preparation method for lithium titanate material, it comprises the steps:
A. the compound of titanium is mixed with the solution containing peroxide radical ion, obtain precursor solution A;
B. Li source compound is dissolved in above-mentioned precursor solution A, obtains precursor solution B;
C. dry described precursor solution B, obtain lithium titanate precursor;
D. sinter described lithium titanate precursor, obtain lithium titanate.
A kind of lithium titanate material obtained by the preparation method of above-mentioned lithium titanate material, this lithium titanate material is by the closely solid micron-sized spherical lithium titanate particle of the nanocrystalline growth in situ of lithium titanate, this lithium titanate particle has spinel structure, the diameter of this lithium titanate particle is 1 ~ 10 μm, and the specific area of this lithium titanate particle is 1 ~ 10m
2/ g, the tap density of this lithium titanate particle is 1.0 ~ 2.5g/cm
3.
A kind of electrode plates, this electrode plates comprises conducting base and is attached to the above-mentioned lithium titanate material of this conducting base.
A kind of lithium ion battery, comprise positive pole, negative pole and electrolyte, the negative or positive electrode of this lithium ion battery comprises above-mentioned lithium titanate material.
The preparation method of lithium titanate material of the present invention is reacted by the compound of hydrogen peroxide and titanium and prepares [Ti (OH)
3o
2]
-ion, and the concentration being controlled precursor solution A by diluent and solvent, then add Li source compound, in the process of heating, drying, promotes that reaction generates the TiO of embedding lithium
2, and balling-up of growing up, then heat treatment obtains the lithium titanate of micron-scale, and this material tap density is large.Preparation technology is simple, low, environmental protection of consuming energy.When using the electrode of the lithium titanate material that obtains of said method for lithium ion battery in addition, the good cycle of this lithium ion battery and specific capacity conservation rate that is stable, electrode material high rate performance that is high, lithium ion battery is excellent.
Accompanying drawing explanation
Fig. 1 is the preparation method of the lithium titanate material of better embodiment of the present invention.
The scanning electron microscope (SEM) photograph of the lithium titanate material of Fig. 2 obtained by embodiment 1.
The X-ray diffractogram of the lithium titanate material of Fig. 3 obtained by embodiment 1.
The lithium titanate material of Fig. 4 obtained by Application Example 1 is as the cycle performance test result curve chart of the lithium ion battery of electrode material.
The lithium titanate material of Fig. 5 obtained by Application Example 1 is as the high rate performance test result curve chart of the lithium ion battery of electrode material.
Main element symbol description
Nothing
Following embodiment will further illustrate the present invention in conjunction with above-mentioned accompanying drawing.
Embodiment
Refer to Fig. 1, the preparation method of lithium titanate material of the present invention, this lithium titanate material is mainly used in the electrode (not shown) of lithium ion battery, and it comprises the steps:
Step S1, mixes the compound of titanium with the solution containing peroxide radical ion, obtains precursor solution A.
Concrete, first peroxide and solvent are mixed according to the ratio preset, obtain mixed solution, then the compound of titanium to be added in this mixed solution and to stir, the compound of titanium is dissolved completely, obtains described precursor solution A.The amount of substance of this peroxide is more than or equal to 1:1 with the ratio of the amount of substance of the titanium elements in the compound of titanium.
Wherein, described peroxide is hydrogen peroxide.Described solvent can be water, is preferably distilled water, deionized water, high purity water or ultra-pure water.The compound of described titanium includes but not limited to one or more in titanium chloride, titanium nitride, titanium carbide and titanyl sulfate.Generate in described precursor solution A and have [Ti (OH)
3o
2]
-ion, generates [Ti (OH)
3o
2]
-the reaction equation of ion is Ti
4++ H
2o
2+ 5OH
-→ [Ti (OH)
3o
2]
-+ 2H
2o.
Step S2, is dissolved in Li source compound in above-mentioned precursor solution A, obtains precursor solution B.
Concrete, first a certain amount of diluent and described solvent to be added in above-mentioned precursor solution A and to mix, then add Li source compound and mix, Li source compound is dissolved completely, obtaining faint yellow emulsus precursor solution B.This diluent and solvent are for regulating the concentration of precursor solution A.Wherein the volume ratio of this diluent solution and solvent is preferably 1:(0.1 ~ 10), in this precursor solution B, elemental lithium is (4 ~ 5) with the ratio of the amount of substance of titanium elements: 5.This diluent can be ketone solution, alcohol solution, ethers solution, arene solution etc., wherein, this ketone solution can be butanone, acetone, methylethylketone etc., this alcohol solution can be absolute ethyl alcohol, ethylene glycol, isopropyl alcohol, methyl alcohol etc., this ethers solution can be ether, expoxy propane etc., and this arene solution can be benzene,toluene,xylene etc.This Li source compound can be selected from but be not limited to one or more in lithium acetate, lithium carbonate, lithium fluoride, lithium hydroxide, lithium oxalate and lithium chloride.
Step S3, dries described precursor solution B, obtains solid lithium titanate precursor, the TiO containing embedding lithium in this lithium titanate precursor
2.
Concrete, adopt the mode of drying above-mentioned precursor solution B, the diluent in precursor liquid B and solvent are all volatilized, obtains the lithium titanate precursor of solid.Wherein, bake out temperature is 60 DEG C ~ 150 DEG C, and drying the time used is more than 10h, drying course can promote [Ti (OH)
3o
2]
-hydrolysis generates TiO
2, concrete hydrolysis equation is: 2 [Ti (OH)
3o
2]
-→ 2TiO
2+ 2H
2o+O
2+ 2OH
-.In the present embodiment, described lithium titanate precursor is white powder.
Step S4, sinters described lithium titanate precursor, obtains lithium titanate.
Concrete, described lithium titanate precursor is placed in stove and sinters 5 ~ 15h under protective atmosphere, wherein sintering temperature is 500 DEG C ~ 900 DEG C.Then naturally cool to room temperature with furnace temperature, namely obtain lithium titanate.This protective atmosphere is the inert gases such as the conventional argon gas used.This lithium titanate is that this micron of spherical lithium titanate particle has spinel structure by the closely solid micron-sized spherical lithium titanate particle (calling the spherical lithium titanate particle of micron in the following text) of the nanocrystalline growth in situ of lithium titanate.The diameter of this micron of spherical lithium titanate particle is 1 ~ 10 μm, and specific area is 1 ~ 10m
2/ g, tap density is 1.0 ~ 2.5g/cm
3.
The preparation method of described lithium titanate material, is reacted by the compound of hydrogenperoxide steam generator and titanium and prepares [Ti (OH)
3o
2]
-, then add the compound of lithium, with [Ti (OH) under heating, drying condition
3o
2]
-reaction, the titanium dioxide of obtained embedding lithium, the titanium dioxide of this embedding lithium has larger particle diameter, can obtain the lithium titanate particle that larger-size micron is spherical, and the tap density of obtained lithium titanate material is larger.
When the lithium titanate material be prepared into utilizing said method is used for the electrode material of lithium ion battery, after this lithium ion battery circulates 500 weeks under the discharge and recharge condition of 10C/10C, the specific capacity conservation rate of the electrode material of battery is more than 90%, and the charge/discharge capacity of 10C is 100.2 ~ 150.1mAh/g.
Below by specific embodiment, the present invention will be further described.
Embodiment 1
By 28ml deionized water, 16ml mass fraction be 20% ~ 30% hydrogen peroxide mix, obtain mixed solution.
The titanium nitride of 0.5g is added in above-mentioned mixed solution, stir and make it dissolve completely, obtain precursor solution A.
By 50ml mass fraction be 99.9% isopropyl alcohol and 100ml deionized water to add in above-mentioned precursor solution A and to mix, then add the lithium fluoride of 0.3g and mix, lithium fluoride is dissolved completely, obtaining faint yellow emulsus precursor solution B.
24h at precursor solution B is placed in 80 DEG C, makes precursor solution B be dried, and obtains the lithium titanate precursor of white.
Described lithium titanate precursor is placed in stove and sinters 7h at argon atmosphere, at 750 DEG C.Then naturally cool to room temperature with furnace temperature, namely obtain lithium titanate material, this lithium titanate material is the lithium titanate particle that micron is spherical.
Embodiment 2
By 40mL deionized water, 12mL mass fraction be 20% ~ 30% hydrogen peroxide mix, obtain mixed solution.
The titanium carbide of 0.25g is added in above-mentioned mixed solution, stir and titanium carbide is dissolved completely, obtain precursor solution A.
By 100ml mass fraction be 99.9% isopropyl alcohol and 100ml deionized water to add in above-mentioned precursor solution A and to mix, then add the lithium hydroxide of 0.3g and mix, lithium hydroxide is dissolved completely, obtaining faint yellow emulsus precursor solution B.
36h at precursor solution B is placed in 80 DEG C, makes precursor solution B be dried, and obtains the lithium titanate precursor of white.
Described lithium titanate precursor is placed in stove and sinters 5h at argon atmosphere, at 700 DEG C.Then naturally cool to room temperature with furnace temperature, namely obtain lithium titanate material, this lithium titanate material is the lithium titanate particle that micron is spherical.
Embodiment 3
By 20mL deionized water, 6mL mass fraction be 20% ~ 30% hydrogen peroxide mix, obtain mixed solution.
The titanium carbide of 0.25g is added in above-mentioned mixed solution, stir and titanium carbide is dissolved completely, obtain precursor solution A.
By 80ml mass fraction be 99.9% ethanol and 50ml deionized water to add in above-mentioned precursor solution A and to mix, then add the lithium acetate of 0.5g and mix, lithium acetate is dissolved completely, obtaining faint yellow emulsus precursor solution B.
36h at precursor solution B is placed in 80 DEG C, makes precursor solution B be dried, and obtains the lithium titanate precursor of white.
Described lithium titanate precursor is placed in stove and sinters 7h at argon atmosphere, at 700 DEG C.Then naturally cool to room temperature with furnace temperature, namely obtain lithium titanate material, this lithium titanate material is the lithium titanate particle that micron is spherical.
Embodiment 4
By 50mL deionized water, 18mL mass fraction be 20% ~ 30% hydrogen peroxide mix, obtain mixed solution.
The titanium chloride of 0.75g is added in above-mentioned mixed solution, stir and titanium chloride is dissolved completely, obtain precursor solution A.
By 150ml mass fraction be 99.9% ethanol and 80ml deionized water to add in above-mentioned precursor solution A and to mix, then add the lithium oxalate of 2.5g and mix, lithium oxalate is dissolved completely, obtaining faint yellow emulsus precursor solution B.
18h at precursor solution B is placed in 150 DEG C, makes precursor solution B be dried, and obtains the lithium titanate precursor of white.
Described lithium titanate precursor is placed in stove and sinters 12h at argon atmosphere, at 800 DEG C.Then naturally cool to room temperature with furnace temperature, namely obtain lithium titanate material, this lithium titanate material is the lithium titanate particle that micron is spherical.
Embodiment 5
By 100mL deionized water, 64mL mass fraction be 20% ~ 30% hydrogen peroxide mix, obtain mixed solution.
The titanyl sulfate of 2g is added in above-mentioned mixed solution, stir and make it dissolve completely, obtain precursor solution A.
By 50ml mass fraction be 99.9% ethanol and 200ml deionized water to add in above-mentioned precursor solution A and to mix, then add the lithium acetate of 1.5g and mix, lithium acetate is dissolved completely, obtaining faint yellow emulsus precursor solution B.
30h at precursor solution B is placed in 120 DEG C, makes precursor solution B be dried, and obtains the lithium titanate precursor of white.
Described lithium titanate precursor is placed in stove and sinters 15h at argon atmosphere, at 800 DEG C.Then naturally cool to room temperature with furnace temperature, namely obtain lithium titanate material, this lithium titanate material is the lithium titanate particle that micron is spherical.
Please consult Fig. 2 ~ 5 further, the lithium titanate material obtained to above-described embodiment 1 is tested, and obtains scanning electron microscope (SEM) photograph, X-ray diffractogram.The cycle performance of test using lithium titanate and lithium sheet as the lithium ion battery of electrode and high rate performance (the method is the method that test that laboratory is commonly used uses the performance of the lithium ion battery of the electrode plates obtained by lithium titanate material), obtain cycle performance test result curve chart and high rate performance test result curve chart respectively.Wherein the electrolyte of this lithium ion battery is with LiPF
6(lithium hexafluoro phosphate) as solute, with volume ratio be the ethylene carbonate of 1:1:1, diethyl carbonate, methyl ethyl carbonate as solvent, the LiPF of configuration
6concentration is the electrolyte of 1mol/L.
As seen from Figure 2, the particle of obtained lithium titanate material is the micron spheric granules of the spinel structure of monodispersed, size uniformity, and the diameter of micron spheric granules is 1 ~ 2 μm.
As shown in Figure 3, obtained lithium titanate material crystalline phase is single and have the spinelle crystal formation lithium titanate of very high crystalline, not containing other any dephasigns.
As seen from Figure 4, use obtained lithium titanate material as the lithium ion battery of electrode, after circulating 350 weeks under 10C/10C discharge and recharge condition, the specific capacity conservation rate of the lithium titanate electrode material of this lithium ion battery is 97.4%, shows very excellent cyclical stability.
As seen from Figure 5, use obtained lithium titanate material as the lithium ion battery of electrode, be 174.5mAh/g in the specific capacity of 0.1C discharge and recharge, the specific capacity of 0.5C discharge and recharge is 160.6mAh/g, the specific capacity of 1C discharge and recharge is 155.7mAh/g, the specific capacity of 2C discharge and recharge is 149.3mAh/g, the specific capacity of 5C discharge and recharge is 130.4mAh/g, the specific capacity of 10C discharge and recharge is 102.5mAh/g, the specific capacity of 20C discharge and recharge is 70.5mAh/g, the specific capacity of 30C discharge and recharge is 54.3mAh/g, shows excellent high rate performance.
A kind of electrode plates (not shown), this electrode plates comprises conducting base and is attached to the above-mentioned lithium titanate material of this conducting base.
A kind of lithium ion battery (not shown), it is in the electronic installations such as mobile phone, computer, electronic reader, electric motor car.This lithium ion battery comprises positive pole, negative pole and electrolyte, and this negative or positive electrode comprises above-mentioned lithium titanate material.
The preparation method of lithium titanate material of the present invention is reacted by the compound of hydrogen peroxide and titanium and prepares [Ti (OH)
3o
2]
-ion, and by the concentration of diluent and solvent adjustment precursor solution A, then add lithium source, in the process of heating, drying, promote that reaction generates the TiO of embedding lithium
2, and balling-up of growing up, then sintering obtains the lithium titanate of micron-scale, and this material tap density is large.Preparation technology is simple, low, environmental protection of consuming energy.When using the electrode of the lithium titanate material that obtains of said method for lithium ion battery in addition, the good cycle of this lithium ion battery and specific capacity conservation rate that is stable, electrode material high rate performance that is high, battery is excellent.
Those skilled in the art will be appreciated that; above execution mode is only used to the present invention is described; and be not used as limitation of the invention; as long as within spirit of the present invention, the appropriate change do above embodiment and change all drop within the scope of protection of present invention.
Claims (10)
1. a preparation method for lithium titanate material, it comprises the steps:
A. the compound of titanium is mixed with the solution containing peroxide radical ion, obtain precursor solution A;
B. Li source compound is dissolved in above-mentioned precursor solution A, obtains precursor solution B;
C. dry described precursor solution B, obtain lithium titanate precursor;
D. sinter described lithium titanate precursor, obtain lithium titanate.
2. the preparation method of lithium titanate material as claimed in claim 1, it is characterized in that: described precursor solution A is by proportionally mixing peroxide with solvent, obtain mixed solution, again the compound of titanium is added mixed solution to be prepared from, wherein, the ratio of the amount of substance of the titanium elements in the amount of substance of peroxide and the compound of titanium is more than or equal to 1:1.
3. the preparation method of lithium titanate material as claimed in claim 2, it is characterized in that: described peroxide is hydrogen peroxide, in described precursor solution B, elemental lithium is (4 ~ 5) with the ratio of the amount of substance of titanium elements: 5.
4. the preparation method of lithium titanate material as claimed in claim 1, is characterized in that: described Li source compound is selected from one or more in lithium acetate, lithium carbonate, lithium fluoride, lithium hydroxide, lithium oxalate and lithium chloride.
5. the preparation method of lithium titanate material as claimed in claim 2, it is characterized in that: described step b is: diluent and described solvent to be added in precursor solution A and to mix, and then Li source compound is mixed with above-mentioned precursor solution A, obtain precursor solution B.
6. the preparation method of lithium titanate material as claimed in claim 5, is characterized in that: described diluent is selected from one or more in ketone solution, alcohol solution, ethers solution and arene solution; Described solvent is deionized water.
7. the preparation method of lithium titanate material as claimed in claim 1, is characterized in that: described step c is:
Dry more than 10h under precursor solution B being placed on the temperature of 60 DEG C ~ 150 DEG C, obtain solid lithium titanate precursor;
Described steps d is: lithium titanate precursor is placed in stove and sinters 5 ~ 15h under protective atmosphere, wherein sintering temperature is 500 ~ 900 DEG C.
8. the lithium titanate material obtained by the preparation method of the lithium titanate material described in claim 1 ~ 7 any one, it is characterized in that: this lithium titanate material is by the closely solid micron-sized spherical lithium titanate particle of the nanocrystalline growth in situ of lithium titanate, this lithium titanate particle has spinel structure, the diameter of this lithium titanate particle is 1 ~ 10 μm, and the specific area of this lithium titanate particle is 1 ~ 10m
2/ g, the tap density of this lithium titanate particle is 1.0 ~ 2.5g/cm
3.
9. an electrode plates, is characterized in that: the lithium titanate material that the preparation method of the lithium titanate material as described in claim 1 ~ 7 any one that this electrode plates comprises conducting base and is attached to this conducting base obtains.
10. a lithium ion battery, it comprises positive pole, negative pole and electrolyte, it is characterized in that: the lithium titanate material that the preparation method of the lithium titanate material that this negative pole or positive pole comprise as described in claim 1 ~ 7 any one obtains.
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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 |
| CN109336169A (en) * | 2018-09-29 | 2019-02-15 | 南京大学射阳高新技术研究院 | A kind of controllable synthesis method of lithium titanate micron-size spherical secondary structure and its application |
| 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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