CN108054374A - A kind of negative electrode battery material and preparation method thereof - Google Patents
A kind of negative electrode battery material and preparation method thereof Download PDFInfo
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- CN108054374A CN108054374A CN201711423430.4A CN201711423430A CN108054374A CN 108054374 A CN108054374 A CN 108054374A CN 201711423430 A CN201711423430 A CN 201711423430A CN 108054374 A CN108054374 A CN 108054374A
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Abstract
The invention belongs to power battery technology field more particularly to a kind of negative electrode battery materials, and including nuclear structure and shell structure, it is (0.1 10) that the nuclear structure, which includes mass ratio,：1 modified lithium titanate and modified TiNb2O7, the modified lithium titanate is doped with silver-colored lithium titanate, the modified TiNb2O7For through carbon nano tube modified TiNb2O7；The shell structure is carbon-coating.Compared with the prior art, volumetric properties, cycle performance and high rate performance that the battery of negative material using the present invention has had.
Description
Technical field
The invention belongs to power battery technology fields more particularly to a kind of negative electrode battery material and preparation method thereof.
Background technology
Lithium ion battery, with excellent energy density, high rate performance and long life, is widely applied to move by it
In the equipment such as mobile phone, digital camera and pocket pc, and its application target is just from small type mobile devices to large size
Electric car Vehicular battery series (Vehicular batteries of pure electric vehicle, hybrid electric vehicle and plug-in hybrid electric vehicles etc.) is stored up with energy
Deposit system etc. transformation.
Negative material is an important component for forming lithium ion battery, it is desirable that it can reversibly be embedded in and deviate from
Lithium ion, the performance of negative material largely also determine the quality of battery performance.The lithium titanate conduct of " zero strain "
A kind of negative material being expected to applied to power battery, the corresponding Ti of embedding de- lithium4+/Ti3+Oxidation-reduction pair is compared with Li+/Li
Voltage for 1.5V, the not up to formation current potential of SEI films can avoid certain irreversible capacity, and lithium titanate has three
Dimension passage can quickly be transmitted for lithium ion, and it also there is wider charge and discharge platform, surface not to form passivating film, and its
Charge and discharge platform is very steady, but since its native electronic electrical conductivity is relatively low and lithium ion diffusion velocity is small, causes metatitanic acid
Capacity attenuation is quickly in high magnification high current charge-discharge for lithium material.
In view of this, the present invention is intended to provide a kind of negative electrode battery material and preparation method thereof, the material have nucleocapsid
Structure, core are the lithium titanate for mixing silver and carbon nano tube modified TiNb2O7Mixture, shell is carbon-coating, have preferably follow
Ring performance, volumetric properties and high rate performance.
The content of the invention
It is an object of the present invention to：In view of the deficiencies of the prior art, a kind of negative electrode battery material is provided, the material
Material has nucleocapsid, and core is the mixture of the lithium titanate and carbon nano tube modified TiNb2O7 of mixing silver, and shell is carbon-coating,
With preferable cycle performance, volumetric properties and high rate performance.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of negative electrode battery material, including nuclear structure and shell structure, it is (0.1-10) that the nuclear structure, which includes mass ratio,：
1 modified lithium titanate and modified TiNb2O7, the modified lithium titanate is doped with silver-colored lithium titanate, the modified TiNb2O7For
Through carbon nano tube modified TiNb2O7；The shell structure is carbon-coating.
Wherein, silver is the high substance of electric conductivity, and silver-colored simple substance is combined in lithium titanate, can improve its electrical conductivity, change
It is apt to its high rate charge-discharge performance, specifically, the valence state of lithium titanate main framing can be caused not by adulterating introducing low price element
Balance, so as to generate new gap or increase migration ion concentration, doping can also be by improving the stability of main framing, purposefully
Ground manufactures gap or changes the size of passage, and reduction skeleton and ion intermolecular forces are in favor of the migration of ion, so as to improve material
The ionic conductivity and electron conduction of material.
The lithium ion insertion current potential of titanium niobate material improves material in 1.64V or so while avoiding the formation of SEI films
Energy density, carry out charge and discharge in 1.0V~2.5V, have the reversible capacity of 280mAh/g, far more than the theoretical specific volume of lithium titanate
Amount, but its poor conductivity problems remains unsolved.The present invention, can be in material granule by carbon nano-tube modified on titanium niobate
Between form conducting matrix grain, the electric conductivity of material is improved, so as to improve the cyclical stability of material.
After lithium titanate and titanium niobate are mixed, the electrical conductivity of material can be greatly improved by coated with conductive charcoal, increases electricity
The energy in pond realizes quick charge and discharge.
Therefore, volumetric properties, cycle performance and the high rate performance that the battery of negative material using the present invention has had.
As a kind of improvement of negative electrode battery material of the present invention, the grain size of the nuclear structure is 1 μm -15 μm.
As a kind of improvement of negative electrode battery material of the present invention, the thickness of the shell structure is 500nm-3 μm.
As a kind of improvement of negative electrode battery material of the present invention, in the modified lithium titanate, silver-colored mass percent is
0.1%-2%.The doping of silver is affected to material property, and suitable doping can improve the performance of lithium titanate, but work as and mix
When miscellaneous amount is too big, then the spinel structure of lithium titanate material is destroyed, negative impact is caused to its performance instead.
As a kind of improvement of negative electrode battery material of the present invention, the modified TiNb2O7In, the quality hundred of carbon nanotubes
Divide than being 3%-20%, TiNb2O7With porous structure, and TiNb2O7It is mutually wound with carbon nanotubes.
It is another object of the present invention to provide a kind of preparation method of positive electrode, including at least following steps：
The first step, the preparation of modified lithium titanate：Titanium dioxide, lithium carbonate and silver nitrate are added to according to stoichiometric ratio
In ball grinder, deionized water is added in as dispersant, after ball-milling treatment 8h-15h, is inserted after drying in sintering furnace, in air gas
600-800 DEG C, pre-burning 3-9h is warming up to the heating rate of 1-8 DEG C/min under atmosphere, then is warming up to 820-950 DEG C, calcines 10-
After 25h, cooling obtains modified lithium titanate；
Second step, modified TiNb2O7Preparation：Carbon nanotubes is added in solvent, ultrasonic disperse obtains solution A；Lazy
Under property gas shield, by butyl titanate and NbCl5Stoichiometrically it is added to the water and stirs evenly, obtains solution B；It will be molten
Liquid B is slowly dropped into solution A, is stirred in oil bath and is made evaporation of the solvent, forms colloidal sol, dry, and grinding obtains gel powder,
Then 10-30h is sintered at 800-1000 DEG C, obtains modified TiNb2O7；
3rd step, carbon coating：The modification TiNb that the modified lithium titanate and second step that the first step is obtained obtain2O7By quality
Than homogeneously disperseing in high speed dispersion agent, composite granule is obtained, which is uniformly mixed with carbon source, after high temperature sintering
Obtain negative material
The TiNb prepared using sol-gal process2O7Material has a porous structure, it is various it is mesoporous be linked to be duct, electrolyte into
Li can be reduced after entering+Transmission path, and alleviate lattice deformability.This porous material has very high tap density and excellent
Long circulating performance.And TiNb2O7It is mutually wound with CNT, distribution uniform.Practice have shown that it is added in preparing in materials process
CNT amounts gradually increase, and the particle of material is less and less, and CNT compound in material structure is also more and more.
A kind of improvement of preparation method as positive electrode of the present invention, in the first step, lithium carbonate excess 4wt.%-
8wt.%.Lithium carbonate can volatilize in calcination process, it is therefore desirable to and it is excessive to set,
A kind of improvement of preparation method as positive electrode of the present invention, the carbon nanotubes of second step pass through before use with
Lower processing：Carbon nanotubes is added in mixing inorganic acid, is then heated to reflux in oil bath pan at 60-90 DEG C cold after 1-3h
But, then it is washed with deionized to weakly acidic pH；The inorganic acid that mixes is hydrochloric acid and the mixture of nitric acid, the volume ratio of the two
For (1-5)：1.CNT after functionalization can increase increasing for more oxygen-containing functional groups, especially carboxyl, enhance the hydrophilic of CNT
Property makes its dispersiveness in the solution improve, and provides more active sites and be conducive to material and grown into CNT structures
Core obtains better electric conductivity and material structure.
A kind of improvement of preparation method as positive electrode of the present invention, solvent described in second step for ethyl alcohol, glacial acetic acid and
The mixed solvent of water, the volume ratio of three is (0.5-5)：(0.5-5)：1；Inert gas be nitrogen or argon gas, the temperature of oil bath
For 80-110 DEG C.
A kind of improvement of preparation method as positive electrode of the present invention, carbon source described in the 3rd step are glucose, sucrose, drip
At least one of green grass or young crops, epoxy resin, phenolic resin and furfural resin；Sintering temperature be 600-1100 DEG C, sintering it is lasting when
Between be 2-10h.
Compared with the prior art, this method is simple and practicable, the more uniform negative material of grain size can be made, using the party
Volumetric properties, cycle performance and the high rate performance that the battery of negative material prepared by method has had.
Specific embodiment
Technical scheme is illustrated with specific embodiment below, but protection scope of the present invention is without being limited thereto.
Embodiment 1
A kind of negative electrode battery material is present embodiments provided, including nuclear structure and shell structure, nuclear structure includes mass ratio
For 2：1 modified lithium titanate and modified TiNb2O7, modified lithium titanate is the lithium titanate doped with silver, modified TiNb2O7For through carbon
Nanometer tube modified TiNb2O7；Shell structure is carbon-coating.
The grain size of nuclear structure is 1 μm -15 μm.The thickness of shell structure is 500nm-3 μm.In modified lithium titanate, silver-colored quality
Percentage is 1%.Modified TiNb2O7In, the mass percent of carbon nanotubes is 10%, TiNb2O7With porous structure, and
TiNb2O7It is mutually wound with carbon nanotubes.
Its preparation method includes at least following steps：
The first step, the preparation of modified lithium titanate：By titanium dioxide, lithium carbonate and silver nitrate according to stoichiometric ratio (wherein
Lithium titanate excess 4wt.%) it is added in ball grinder, deionized water is added in as dispersant, after ball-milling treatment 10h, dries postposition
Enter in sintering furnace, be warming up to 700 DEG C, pre-burning 6h in air atmosphere with the heating rate of 4 DEG C/min, then be warming up to 850 DEG C, forge
After burning 14h, cooling obtains modified lithium titanate；
Second step, modified TiNb2O7Preparation：By carbon nanotubes add in solvent in, wherein, solvent for ethyl alcohol, glacial acetic acid and
The mixed solvent of water, the volume ratio of three is 1：1：1 ultrasonic disperse, obtains solution A；Under protection of argon gas, by butyl titanate
And NbCl5Stoichiometrically it is added to the water and stirs evenly, obtains solution B；Solution B is slowly dropped into solution A, in oil bath
In stirred at 90 DEG C and make evaporation of the solvent, form colloidal sol, dry, grinding obtains gel powder, is then sintered at 900 DEG C
20h obtains modified TiNb2O7；
3rd step, carbon coating：The modification TiNb that the modified lithium titanate and second step that the first step is obtained obtain2O7By quality
Than homogeneously disperseing in high speed dispersion agent, composite granule is obtained, which is uniformly mixed with carbon source pitch, at 700 DEG C
Negative material is obtained after lower sintering 4h.
Wherein, the carbon nanotubes of second step passes through following processing before use：Carbon nanotubes is added in mixing inorganic acid,
Then 2h postcoolings are heated to reflux at 70 DEG C in oil bath pan, are then washed with deionized to weakly acidic pH.Wherein, nothing is mixed
Machine acid is hydrochloric acid and the mixture of nitric acid, and the volume ratio of the two is 3：1.
Embodiment 2
A kind of negative electrode battery material is present embodiments provided, including nuclear structure and shell structure, nuclear structure includes mass ratio
For 1：2 modified lithium titanate and modified TiNb2O7, modified lithium titanate is the lithium titanate doped with silver, modified TiNb2O7For through carbon
Nanometer tube modified TiNb2O7；Shell structure is carbon-coating.
The grain size of nuclear structure is 1 μm -15 μm.The thickness of shell structure is 500nm-3 μm.In modified lithium titanate, silver-colored quality
Percentage is 0.5%.Modified TiNb2O7In, the mass percent of carbon nanotubes is 15%, TiNb2O7With porous structure, and
And TiNb2O7It is mutually wound with carbon nanotubes.
Its preparation method includes at least following steps：
The first step, the preparation of modified lithium titanate：By titanium dioxide, lithium carbonate and silver nitrate according to stoichiometric ratio (wherein
Lithium titanate excess 6wt.%) it is added in ball grinder, deionized water is added in as dispersant, after ball-milling treatment 12h, dries postposition
Enter in sintering furnace, be warming up to 650 DEG C, pre-burning 8h in air atmosphere with the heating rate of 6 DEG C/min, then be warming up to 825 DEG C, forge
After burning 18h, cooling obtains modified lithium titanate；
Second step, modified TiNb2O7Preparation：By carbon nanotubes add in solvent in, wherein, solvent for ethyl alcohol, glacial acetic acid and
The mixed solvent of water, the volume ratio of three is 1：2：2 ultrasonic disperses, obtain solution A；Under nitrogen protection, by butyl titanate
And NbCl5Stoichiometrically it is added to the water and stirs evenly, obtains solution B；Solution B is slowly dropped into solution A, in oil bath
In stirred at 100 DEG C and make evaporation of the solvent, form colloidal sol, dry, grinding obtains gel powder, is then sintered at 950 DEG C
15h obtains modified TiNb2O7；
3rd step, carbon coating：The modification TiNb that the modified lithium titanate and second step that the first step is obtained obtain2O7By quality
Than homogeneously disperseing in high speed dispersion agent, composite granule is obtained, which is uniformly mixed with carbon source glucose, 800
Negative material is obtained after being sintered 6h at DEG C.
Wherein, the carbon nanotubes of second step passes through following processing before use：Carbon nanotubes is added in mixing inorganic acid,
Then 1.5h postcoolings are heated to reflux at 80 DEG C in oil bath pan, are then washed with deionized to weakly acidic pH.Wherein, mix
Inorganic acid is hydrochloric acid and the mixture of nitric acid, and the volume ratio of the two is 2：1.
Embodiment 3
A kind of negative electrode battery material is present embodiments provided, including nuclear structure and shell structure, nuclear structure includes mass ratio
For 1：4 modified lithium titanate and modified TiNb2O7, modified lithium titanate is the lithium titanate doped with silver, modified TiNb2O7For through carbon
Nanometer tube modified TiNb2O7；Shell structure is carbon-coating.
The grain size of nuclear structure is 1 μm -15 μm.The thickness of shell structure is 500nm-3 μm.In modified lithium titanate, silver-colored quality
Percentage is 0.8%.Modified TiNb2O7In, the mass percent of carbon nanotubes is 8%, TiNb2O7With porous structure, and
TiNb2O7It is mutually wound with carbon nanotubes.
Its preparation method includes at least following steps：
The first step, the preparation of modified lithium titanate：By titanium dioxide, lithium carbonate and silver nitrate according to stoichiometric ratio (wherein
Lithium titanate excess 7wt.%) it is added in ball grinder, deionized water is added in as dispersant, after ball-milling treatment 14h, dries postposition
Enter in sintering furnace, be warming up to 750 DEG C, pre-burning 4h in air atmosphere with the heating rate of 5 DEG C/min, then be warming up to 870 DEG C, forge
After burning 22h, cooling obtains modified lithium titanate；
Second step, modified TiNb2O7Preparation：By carbon nanotubes add in solvent in, wherein, solvent for ethyl alcohol, glacial acetic acid and
The mixed solvent of water, the volume ratio of three is 2：1：1 ultrasonic disperse, obtains solution A；Under protection of argon gas, by butyl titanate
And NbCl5Stoichiometrically it is added to the water and stirs evenly, obtains solution B；Solution B is slowly dropped into solution A, in oil bath
In stirred at 95 DEG C and make evaporation of the solvent, form colloidal sol, dry, grinding obtains gel powder, is then sintered at 950 DEG C
5h obtains modified TiNb2O7；
3rd step, carbon coating：The modification TiNb that the modified lithium titanate and second step that the first step is obtained obtain2O7By quality
Than homogeneously disperseing in high speed dispersion agent, composite granule is obtained, which is uniformly mixed with carbon source sucrose, at 900 DEG C
Negative material is obtained after lower sintering 8h.
Wherein, the carbon nanotubes of second step passes through following processing before use：Carbon nanotubes is added in mixing inorganic acid,
Then 1.5h postcoolings are heated to reflux at 85 DEG C in oil bath pan, are then washed with deionized to weakly acidic pH.Wherein, mix
Inorganic acid is hydrochloric acid and the mixture of nitric acid, and the volume ratio of the two is 1：1.
Comparative example 1
The negative material that this comparative example provides is spinel type lithium titanate.
By the negative material of embodiment 1 to 3 and comparative example 1 and superconduction carbon, PVDF according to 80:10:10 mass ratio adds in
It into NMP, stirs evenly, obtains the slurry that solid content is 60%, by the slurry coated on copper foil, thickness is 120 μm, is done
Dry, punching obtains pole piece.
The pole piece is put into glove box, using metal lithium sheet as to electrode, PP is membrane, 1mol/L LiPF6/EC+DEC (bodies
Product ratio 1:1) solution is electrolyte, and CR2025 type button cells are assembled into the glove box full of dry argon gas.Obtained electricity
It is S1-S3 and D1 that pond is numbered respectively.
Performance test：Charge-discharge test is constant current charge-discharge, and the voltage ranges of charge and discharge is 1.0~3.0V, charge and discharge
It is 1C that the electric current of electricity, which chooses 300mA/g,.Its capacity for the first time is tested, the test of low current circulation ability takes 0.1C (30mA/g) as Xun Huan
Electric current, test process and step are as follows：(1) 0.1C is discharged to 1.0V；(2) 2min is stood；(3) 0.1C charges to 3.0V；(4) it is quiet
Put 2min；(5) cycle 100 times.The long circulating aptitude tests of high current generally obtain low current using 0.1C first and activate 3 times,
Then cycled 1000 times under 10C multiplying powers.High rate performance test be primarily used to research material fast charging and discharging ability and
The stability of material converted under different multiplying, the multiplying power that material high rate performance is selected during test are followed successively by 5C, 10C, Mei Gebei
Cycle-index is 10 times under rate, and voltage range is still 1~3V.
Table 1：Number is S1-S3 and the test result of the battery of D1.
As can be seen from Table 1, the present invention has preferable volumetric properties, cycle performance and high rate performance.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and changed.Therefore, the invention is not limited in specific embodiment disclosed and described above, to the present invention's
Some modifications and changes should also be as falling into the scope of the claims of the present invention.In addition, it although is used in this specification
Some specific terms, but these terms are merely for convenience of description, do not limit the present invention in any way.
Claims (10)
1. a kind of negative electrode battery material, it is characterised in that：Including nuclear structure and shell structure, the nuclear structure is including mass ratio
(0.1-10)：1 modified lithium titanate and modified TiNb2O7, the modified lithium titanate is doped with silver-colored lithium titanate, the modification
TiNb2O7For through carbon nano tube modified TiNb2O7；The shell structure is carbon-coating.
2. negative electrode battery material according to claim 1, it is characterised in that：The grain size of the nuclear structure is 1 μm of -15 μ
m。
3. negative electrode battery material according to claim 1, it is characterised in that：The thickness of the shell structure is 500nm-3 μ
m。
4. negative electrode battery material according to claim 1, it is characterised in that：In the modified lithium titanate, silver-colored quality
Percentage is 0.1%-2%.
5. negative electrode battery material according to claim 1, it is characterised in that：The modified TiNb2O7In, carbon nanotubes
Mass percent be 3%-20%, TiNb2O7With porous structure, and TiNb2O7It is mutually wound with carbon nanotubes.
6. a kind of preparation method of positive electrode described in any one of claim 1 to 5, which is characterized in that including at least as follows
Step：
The first step, the preparation of modified lithium titanate：Titanium dioxide, lithium carbonate and silver nitrate are added to ball milling according to stoichiometric ratio
In tank, deionized water is added in as dispersant, after ball-milling treatment 8h-15h, is inserted after drying in sintering furnace, in air atmosphere
600-800 DEG C, pre-burning 3-9h is warming up to the heating rate of 1-8 DEG C/min, then is warming up to 820-950 DEG C, after calcining 10-25h,
Cooling, obtains modified lithium titanate；
Second step, modified TiNb2O7Preparation：Carbon nanotubes is added in solvent, ultrasonic disperse obtains solution A；In indifferent gas
Under body protection, by butyl titanate and NbCl5Stoichiometrically it is added to the water and stirs evenly, obtains solution B；By solution B
It is slowly dropped into solution A, stirs in oil bath and makes evaporation of the solvent, form colloidal sol, dry, grinding obtains gel powder, then
10-30h is sintered at 800-1000 DEG C, obtains modified TiNb2O7；
3rd step, carbon coating：The modification TiNb that the modified lithium titanate and second step that the first step is obtained obtain2O7Exist in mass ratio
Homogeneously disperse in high speed dispersion agent, obtain composite granule, which with carbon source is uniformly mixed, is obtained after high temperature sintering
Negative material.
7. the preparation method of positive electrode according to claim 6, which is characterized in that in the first step, lithium carbonate is excessive
4wt.%-8wt.%.
8. the preparation method of positive electrode according to claim 6, which is characterized in that the carbon nanotubes of second step is using
It is preceding to pass through following processing：Carbon nanotubes is added in mixing inorganic acid, is then heated to reflux 1- at 60-90 DEG C in oil bath pan
Then 3h postcoolings are washed with deionized to weakly acidic pH；The mixing inorganic acid is the mixture of hydrochloric acid and nitric acid, the two
Volume ratio is (1-5)：1.
9. the preparation method of positive electrode according to claim 6, which is characterized in that solvent described in second step for ethyl alcohol,
The mixed solvent of glacial acetic acid and water, the volume ratio of three is (0.5-5)：(0.5-5)：1；Inert gas be nitrogen or argon gas, oil
The temperature of bath is 80-110 DEG C.
10. the preparation method of positive electrode according to claim 6, which is characterized in that carbon source described in the 3rd step is grape
At least one of sugar, sucrose, pitch, epoxy resin, phenolic resin and furfural resin；Sintering temperature is 600-1100 DEG C, is burnt
The duration of knot is 2-10h.
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| CN110311100A (en) * | 2019-05-28 | 2019-10-08 | 浙江锋锂新能源科技有限公司 | A kind of solid lithium battery and preparation method thereof |
| TWI743017B (en) * | 2021-05-10 | 2021-10-11 | 台灣中油股份有限公司 | Lithium titanate/titanium niobate core-shell composite material and preparation method thereof |
| CN114300671A (en) * | 2021-12-28 | 2022-04-08 | 蜂巢能源科技股份有限公司 | Graphite composite negative electrode material and preparation method and application thereof |
| US11575122B2 (en) * | 2019-07-29 | 2023-02-07 | GM Global Technology Operations LLC | Electrode with enhanced state of charge estimation |
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| CN109980214B (en) * | 2019-04-26 | 2021-10-01 | 四川昆仑云熙新能源科技有限公司 | Preparation method of carbon nanotube-graphite composite electrode material and lithium ion battery |
| CN110311100A (en) * | 2019-05-28 | 2019-10-08 | 浙江锋锂新能源科技有限公司 | A kind of solid lithium battery and preparation method thereof |
| CN110311100B (en) * | 2019-05-28 | 2022-02-18 | 浙江锋锂新能源科技有限公司 | All-solid-state lithium battery and preparation method thereof |
| US11575122B2 (en) * | 2019-07-29 | 2023-02-07 | GM Global Technology Operations LLC | Electrode with enhanced state of charge estimation |
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| US20220356072A1 (en) * | 2021-05-10 | 2022-11-10 | Cpc Corporation, Taiwan | Lithium titanate/titanium niobate core-shell composite material and preparation method thereof |
| US11746024B2 (en) * | 2021-05-10 | 2023-09-05 | Cpc Corporation, Taiwan | Lithium titanate/titanium niobate core-shell composite material and preparation method thereof |
| CN114300671A (en) * | 2021-12-28 | 2022-04-08 | 蜂巢能源科技股份有限公司 | Graphite composite negative electrode material and preparation method and application thereof |
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