CN109830677A - Negative electrode material and preparation method thereof, negative electrode tab, battery - Google Patents
Negative electrode material and preparation method thereof, negative electrode tab, battery Download PDFInfo
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- CN109830677A CN109830677A CN201811638304.5A CN201811638304A CN109830677A CN 109830677 A CN109830677 A CN 109830677A CN 201811638304 A CN201811638304 A CN 201811638304A CN 109830677 A CN109830677 A CN 109830677A
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- 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
Abstract
This application discloses a kind of negative electrode material and preparation method thereof, negative electrode tab, battery, preparation method includes preparing lithium titanate；By the lithium titanate, Co3O4It is placed in aqueous solution and mixes, obtain doping mixed liquor；The dry doping mixed liquor, obtains negative electrode material.The preparation method of negative electrode material provided by the present application, by adding Co3O4Obtain modified lithium titanate material, improve the gram volume of lithium titanate material, and when being prepared into lithium titanate battery, chemical stabilization interface between electrode material and electrolyte can be constructed, to ensure that the circulation performance of lithium titanate battery, the spherical morphology of lithium titanate particle and the processing performance of battery preparation are more effectively maintained, thus when overcoming negative electrode material of the lithium titanate separately as lithium ion battery the problem of low capacity, Cycle Difference；Meanwhile this preparation method simple process, mild condition is at low cost, and it is reproducible, it is convenient for large-scale preparation.
Description
Technical field
This application involves energy storage device technical field, especially a kind of negative electrode material and preparation method thereof, negative electrode tab, electricity
Pond.
Background technique
Lithium titanate material is compared with the carbon-based negative electrode material of tradition, for no zero strain material, in the materials'use as battery
When, volume is substantially unchanged during removal lithium embedded, and cycle performance is good.But it is lower that there is also electronic conductivities, poorly conductive, with
And the problem that the specific energy as brought by electrode potential height is low, these problems limit lithium titanate material on lithium ion battery
Application.
Summary of the invention
In view of this, the first purpose of the application is to provide a kind of negative electrode material and preparation method thereof, negative electrode tab, electricity
Pond, to solve the performance of lithium titanate material.
In order to achieve the above objectives, the application adopts the following technical scheme that
The first aspect of the application provides a kind of preparation method of negative electrode material, comprising:
Prepare lithium titanate；
By the lithium titanate, Co3O4It is placed in aqueous solution and mixes, obtain doping mixed liquor；
The dry doping mixed liquor, obtains negative electrode material.
It is optionally, described to prepare lithium titanate, specifically:
Lithium source and titanium source are placed in deionized water and mixed, titanium lithium mixed slurry is obtained；
The dry titanium lithium mixed slurry, obtains lithium titanate precursor；
The lithium titanate precursor is sintered synthesis, obtains the lithium titanate.
Optionally, described lithium source and titanium source are placed in deionized water mixes, and obtains titanium lithium mixed slurry, specifically
Are as follows:
The lithium source is put into the deionized water and is stirred, lithium source solution is obtained；
The titanium source is added in the lithium source solution, and is stirred, obtains the titanium lithium mixed slurry.
Optionally, the titanium source is added in the lithium source solution, and is stirred, obtain the titanium lithium mixed slurry mistake
Cheng Zhong,
Mixing time is 100~200 minutes；
Solid content in the titanium lithium mixed slurry is 15%~25%.
Optionally, the molar ratio of the lithium source and the titanium source is 0.74~0.86；
The titanium source is selected from TiO2With one of metatitanic acid or two kinds of mixture；
The lithium source is selected from one of lithium carbonate, lithium hydroxide, lithium bicarbonate, lithium nitrate, lithium acetate or several
Mixture.
Optionally, the drying titanium lithium mixed slurry, obtains lithium titanate precursor, specifically:
By the dry titanium lithium mixed slurry of spray dried form, the lithium titanate precursor is obtained；
Wherein, the intake air temperature of the spray drying is 180 DEG C~260 DEG C；The air outlet temperature of the spray drying
It is 100 DEG C~110 DEG C；The compressed air of the spray drying is 0.1MPa~0.4MPa.
Optionally, the heating mode when lithium titanate precursor to be sintered to synthesis are as follows: with heating rate for 3
DEG C/min~8 DEG C/min is warming up to 800 DEG C~900 DEG C, keep the temperature 2 hours~4 hours.
Optionally, described by the lithium titanate, Co3O4It is placed in aqueous solution and mixes, obtain doping mixed liquor, specifically:
It disperses the lithium titanate in aqueous solution and stirs, obtain lithium titanate solution；
The Co is added in the lithium titanate solution3O4, continue to stir, until forming viscous paste, obtain the doping
Mixed liquor；
Wherein, the Co3O4Ratio in solid powder is 5%~15%.
Optionally, described by the lithium titanate, Co3O4It is placed in aqueous solution and mixes, obtain doping mixed liquor, specifically:
By the lithium titanate, Co3O4It is placed in aqueous solution, heating stirring is carried out by constant temperature blender with magnetic force, obtain the doping mixing
Liquid.
Optionally, the drying time of the dry doping mixed liquor is 4 hours~10 hours.
The second aspect of the application provides a kind of negative electrode material, prepares shape using preparation method described in any of the above embodiments
At.
The third aspect of the application provides a kind of negative electrode tab, and the material of the negative electrode tab includes cathode material described above
Material.
The fourth aspect of the application provides a kind of battery, including negative electrode tab as described above.
The preparation method of negative electrode material provided by the present application, by adding Co3O4, modified lithium titanate material is obtained, is improved
The gram volume of lithium titanate material, and when being prepared into lithium titanate battery, it is steady that chemistry between electrode material and electrolyte can be constructed
Demarcation face more effectively maintains the spherical morphology of lithium titanate particle to ensure that the circulation performance of lithium titanate battery
With the processing performance of battery preparation, to low capacity when overcoming negative electrode material of the lithium titanate separately as lithium ion battery, follow
The problem of ring difference；Meanwhile this preparation method simple process, mild condition is at low cost, and it is reproducible, it is convenient for large-scale preparation.
Detailed description of the invention
By referring to the drawings to the description of the embodiment of the present application, the above-mentioned and other purpose of the application, feature and
Advantage will be apparent from, in the accompanying drawings:
Fig. 1 shows the SEM figure using the negative electrode material of preparation method provided by the present application preparation；
Fig. 2 shows the SEM figures of negative electrode material prepared by the preparation method using comparative example 1；
Fig. 3 shows the SEM figure of the negative electrode material of the preparation method preparation using comparative example 2；
Fig. 4 is shown the negative electrode material of the preparation method preparation proposed using the application and using the preparation method system of comparative example 2
The XRD spectra of standby negative electrode material.
Specific embodiment
The application is described below based on embodiment, but the application is not restricted to these embodiments.Under
Text is detailed to describe some specific detail sections in the datail description of the application, in order to avoid obscuring the essence of the application,
There is no narrations in detail for well known method, process, process, element.
In addition, it should be understood by one skilled in the art that provided herein attached drawing be provided to explanation purpose, and
What attached drawing was not necessarily drawn to scale.
Unless the context clearly requires otherwise, "include", "comprise" otherwise throughout the specification and claims etc. are similar
Word should be construed as the meaning for including rather than exclusive or exhaustive meaning；That is, be " including but not limited to " contains
Justice.
In the description of the present application, it is to be understood that term " first ", " second " etc. are used for description purposes only, without
It can be interpreted as indication or suggestion relative importance.In addition, in the description of the present application, unless otherwise indicated, the meaning of " multiple "
It is two or more.
This application provides a kind of preparation methods of negative electrode material, comprising:
S100: lithium titanate is prepared；
S200: by lithium titanate, Co3O4It is placed in aqueous solution and mixes, obtain doping mixed liquor；
S300: the dry doping mixed liquor obtains negative electrode material.
Above-mentioned preparation method, by adding Co3O4, modified lithium titanate material is obtained, gram appearance of lithium titanate material is improved
Amount, and when being prepared into lithium titanate battery, chemical stabilization interface between electrode material and electrolyte can be constructed, to ensure that titanium
The circulation performance of acid lithium battery more effectively maintains the spherical morphology of lithium titanate particle and the processability of battery preparation
Can, thus when overcoming lithium titanate separately as lithium ion battery negative material the problem of low capacity, Cycle Difference；Meanwhile it is this
Preparation method simple process, mild condition is at low cost, reproducible, is convenient for large-scale preparation.In addition, use is wet in the application
Method doping, more traditional dry method doping, the doping mixed liquor enabled to is more evenly.
Wherein, lithium titanate precursor is prepared in S100 specifically:
S110: lithium source and titanium source being placed in deionized water and mixed, and obtain titanium lithium mixed slurry；
S120: dry titanium lithium mixed slurry can be specifically dried by way of spray drying, can be set spraying
Dry intake air temperature is 180 DEG C~260 DEG C, such as 180 DEG C, 240 DEG C, 250 DEG C, 260 DEG C；The air outlet temperature of spray drying
Degree is 100 DEG C~110 DEG C, such as 100 DEG C, 105 DEG C, 110 DEG C；The compressed air of spray drying is 0.1MPa~0.4MPa, such as
0.1MPa, 0.15MPa, 0.2MPa, 04MPa etc., obtain lithium titanate precursor；
S130: being sintered synthesis for lithium titanate precursor, specifically, lithium titanate precursor can be placed in air atmosphere
High temperature box furnace be sintered synthesis, obtain lithium titanate.
In view of the solubility of lithium source is lower, in order to be well-dispersed in it in deionized water, S110 of the invention is specific
Are as follows:
S111: lithium source being put into deionized water and is stirred, and mixing time can be 30 minutes, specifically can be according to reality
Border situation determines, so that lithium source sufficiently dissolves, obtains lithium source solution；
S112: titanium source being added in lithium source solution, and is stirred, and mixing time can be 100 minutes~200 minutes,
Such as 100 minutes, 120 minutes, 150 minutes, 180 minutes, 200 minutes, titanium lithium mixed slurry is obtained.
Solid content in above-mentioned lithium titanium mixed solution is 15%~25%, such as 15%, 18%, 20%, 23%, 25%,
To guarantee enough lithium titanate ingredients.
Wherein, titanium source is selected from TiO2With one of metatitanic acid or two kinds of mixture, such as TiO2.H2O；Lithium source is selected from
One of lithium carbonate, lithium hydroxide, lithium bicarbonate, lithium nitrate, lithium acetate or several mixtures.No matter titanium source and lithium source
How to select, the molar ratio of lithium source and titanium source is 0.74~0.86, such as 0.74,0.78,0.80,0.82,0.86.
Lithium titanate precursor is sintered to heating mode when synthesis in above-mentioned S130 are as follows: with heating rate be 3 DEG C/
Min~8 DEG C/min is warming up to 800 DEG C~900 DEG C, such as heating rate is 3 DEG C/min, 5 DEG C/min, 8 DEG C/min, is warming up to
800 DEG C, 820 DEG C, 850 DEG C, 880 DEG C, 900 DEG C etc., keep the temperature 2 hours~4 hours, such as heat preservation 2 hours, 2.5 hours, 3 hours,
3.5 hours, 4 hours etc..
By lithium titanate, Co in S2003O4It is placed in aqueous solution and mixes, obtain doping mixed liquor, specifically:
S210: it disperses lithium titanate in aqueous solution and stirs, dissolve it sufficiently, obtain lithium titanate solution；
S220: Co is added in lithium titanate solution3O4, continue to stir, until forming viscous paste, obtain doping mixed liquor；
Wherein, Co3O4Ratio be 5%~15%, such as 5%, 6%, 10%, 12%, 15%.
Stirring (including the stirring in S21 and S220) in S200 can carry out heating by constant temperature blender with magnetic force and stir
It mixes, so that Co3O4It dissolves as early as possible, obtains doping mixed liquor.
The drying time of dry doping mixed liquor is 4 hours~10 hours in S300, such as 4 hours, 5 hours, 7 hours, it is 8 small
When, 10 hours etc., to improve the performance of negative electrode material.
In order to enable to negative electrode material powder it is tiny and be evenly distributed, after dry doping mixed liquor, be sieved, then
To negative electrode material.
The application also provides a kind of negative electrode material, prepares to be formed using preparation method described in any of the above-described embodiment.In addition,
Present invention also provides a kind of negative electrode tab, the material of the negative electrode tab includes above-mentioned positive electrode.In addition, present invention also provides one
Kind battery, including above-mentioned negative electrode tab.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of preparation method of negative electrode material, comprising:
S11: raw material mixing: according to lithium source, titanium source, 4:5 carries out mixing in molar ratio, firstly, the lithium carbonate for weighing 300g is
Lithium source (purity 99.95%) is put in 4900ml deionized water and stirs 30 minutes, then, adds 925g TiO2.H2The titanium of O
Source (loss on ignition 87.1%) continues stirring 120 minutes, obtains titanium lithium mixed slurry.
S12: spray drying: above-mentioned finely dispersed titanium lithium mixed slurry is spray-dried, and intake air temperature is arranged
It is 260 DEG C, outlet temperature is 110 DEG C or so, compressed air 0.4MPa；Lithium titanate precursor can be obtained.
S13: sintering synthesis: being sintered synthesis for the high temperature box furnace that above-mentioned lithium titanate precursor is placed in air atmosphere,
Heating mode is that 850 DEG C are warming up to the heating rate of 5 DEG C/min, keeps the temperature 2 hours, then furnace cooling obtains lithium titanate.
S14:Co3O4Doping: weighing the lithium titanate material in 90gS13, be scattered in 240ml aqueous solution, stirs 30 minutes
10g Co is added afterwards3O4, continue the heating stirring in constant temperature blender with magnetic force, until forming sticky slurry, obtain doping mixing
Liquid.
S15: negative electrode material: being placed in air dry oven for the doping mixed liquor in S14,4 hours dry, then with 400 mesh
Mesh screen sieving, can obtain high capacity doped with Co3O4Lithium titanate material.
Embodiment 2
Unlike the first embodiment:
In S11, lithium carbonate is replaced by lithium hydroxide, TiO2.H2O is replaced with metatitanic acid, and continues to stir after adding titanium source
100 minutes；
In S12, intake air temperature is 180 DEG C, and outlet temperature is 100 DEG C or so, compressed air 0.2MPa；
In S13, heating mode is that 800 DEG C are warming up to the heating rate of 3 DEG C/min, keeps the temperature 3 hours；
It is 6 hours dry in S15.
Embodiment 3
Unlike the first embodiment:
In S11, continue stirring 200 minutes after adding titanium source；
In S12, intake air temperature is 250 DEG C, and outlet temperature is 105 DEG C or so, compressed air 0.1MPa；
In S13, heating mode is that 900 DEG C are warming up to the heating rate of 8 DEG C/min, keeps the temperature 4 hours；
It is 10 hours dry in S15.
Comparative example 1
A kind of preparation method of negative electrode material, comprising:
S21: raw material mixing: firstly, weighing the lithium carbonate (purity 99.95%) of 200g, it is put in 3200ml deionized water
Middle stirring 30 minutes, then, adds the TiO of 620g2.H2O continues stirring 120 minutes as titanium source (loss on ignition 87.1%).
S22: spray drying: above-mentioned finely dispersed titanium lithium mixed slurry is spray-dried, and intake air temperature is arranged
It is 270 DEG C, outlet temperature is 110 DEG C or so, compressed air 0.4MPa；Lithium titanate precursor can be obtained.
S23: sintering synthesis: being sintered synthesis for the high temperature box furnace that above-mentioned lithium titanate precursor is placed in air atmosphere,
Heating mode is that 850 DEG C are warming up to the heating rate of 5 DEG C/min, keeps the temperature 120 minutes, then furnace cooling obtains lithium titanate.
S24:Co3O4Doping: weighing the lithium titanate material in 90gS23, and 10g Co is added3O4, addition 200g diameter is 3mm
The agate zirconium ball of~5mm using planetary ball mill, inverts 30 minutes after rotating forward 30 minutes, amounts in stainless steel jar mill
Ball milling 60 minutes, obtained mixture was sieved with 400 mesh mesh screens, can be obtained doped with Co3O4Lithium titanate material.
Comparative example 2
A kind of preparation method of negative electrode material, comprising:
S31: raw material mixing: firstly, weighing the lithium carbonate (purity 99.95%) of 150g, it is put in 2460ml deionized water
Middle stirring 30 minutes, then, adds the TiO of 465g2.H2O continues stirring 120 minutes as titanium source (loss on ignition 87.1%).
S22: spray drying: above-mentioned finely dispersed titanium lithium mixed slurry is spray-dried, and intake air temperature is arranged
It is 270 DEG C, outlet temperature is 110 DEG C or so, compressed air 0.4MPa；Lithium titanate precursor can be obtained.
S23: sintering synthesis: being sintered synthesis for the high temperature box furnace that above-mentioned lithium titanate precursor is placed in air atmosphere,
Heating mode is that 850 DEG C are warming up to the heating rate of 5 DEG C/min, keeps the temperature 120 minutes, then furnace cooling, mixed by what is obtained
It closes object to be sieved with 400 mesh mesh screens, obtains lithium titanate, i.e. negative electrode material.
By lithium titanate anode material prepared by above-mentioned comparison case 1 and comparison case 2 and superconduction carbon black binder with 80:
10 ratio mixes difference, negative electrode diaphragm is prepared, using copper foil as collector；Then dry, slice is prepared into negative electrode tab.With
Metal lithium sheet makees diaphragm as positive plate, C1garde, and using 1M LiPF6-EC/DMC (volume ratio 1:1) is electrolyte.?
Button cell is assembled into glove box full of argon gas.Battery performance, the setting of charge and discharge voltage are tested using new prestige cell tester
For 0.1-2.5V, obtaining 1C, discharge capacity is respectively 221.3mAh/g, 185.5mAh/g for the first time.Wherein, 1C and 2C dischargeable capacity
It is shown in Table 1 respectively with loop test result.In addition, the SEM of negative electrode material prepared by embodiment 1, comparative example 1 and comparative example 2 schemes
See that Fig. 1-Fig. 3, Fig. 4 show the XRD spectra of negative electrode material prepared by embodiment 1 and comparative example 2,
Table 1
With reference to Fig. 1-Fig. 4 and table 1, prepared it can be seen from embodiment 1 and comparative example 1 using the preparation method of the application
Negative electrode material it is big compared with the gram volume of the negative electrode material of wet process doping preparation and charge-discharge performance is good；By embodiment 1 with it is right
Ratio 2 is as can be seen that pass through doping Co3O4The gram volume of the lithium titanate significantly improved, and charge-discharge performance is good.
Those skilled in the art will readily recognize that above-mentioned each preferred embodiment can be free under the premise of not conflicting
Ground combination, superposition.
It should be appreciated that above-mentioned embodiment is merely exemplary, and not restrictive, without departing from the basic of the application
In the case where principle, those skilled in the art can be directed to the various apparent or equivalent modification or replace that above-mentioned details is made
It changes, is all included within the scope of claims hereof.
Claims (13)
1. a kind of preparation method of negative electrode material characterized by comprising
Prepare lithium titanate；
By the lithium titanate, Co3O4It is placed in aqueous solution and mixes, obtain doping mixed liquor；
The dry doping mixed liquor, obtains negative electrode material.
2. preparation method according to claim 1, which is characterized in that it is described to prepare lithium titanate, specifically:
Lithium source and titanium source are placed in deionized water and mixed, titanium lithium mixed slurry is obtained；
The dry titanium lithium mixed slurry, obtains lithium titanate precursor；
The lithium titanate precursor is sintered synthesis, obtains the lithium titanate.
3. preparation method according to claim 2, which is characterized in that it is described by lithium source and titanium source be placed in deionized water into
Row mixing, obtains titanium lithium mixed slurry, specifically:
The lithium source is put into the deionized water and is stirred, lithium source solution is obtained；
The titanium source is added in the lithium source solution, and is stirred, obtains the titanium lithium mixed slurry.
4. preparation method according to claim 3, which is characterized in that the titanium source is added in the lithium source solution, and
It is stirred, during obtaining the titanium lithium mixed slurry,
Mixing time is 100~200 minutes；
Solid content in the titanium lithium slurry is 15%~25%.
5. preparation method according to claim 2, which is characterized in that the molar ratio of the lithium source and the titanium source is 0.74
~0.86；
The titanium source is selected from TiO2With one of metatitanic acid or two kinds of mixture；
The lithium source is selected from one of lithium carbonate, lithium hydroxide, lithium bicarbonate, lithium nitrate, lithium acetate or several mixing
Object.
6. preparation method according to claim 2, which is characterized in that the drying titanium lithium mixed slurry obtains titanium
Sour lithium presoma, specifically:
By the dry titanium lithium mixed slurry of spray dried form, the lithium titanate precursor is obtained；
Wherein, the intake air temperature of the spray drying is 180 DEG C~260 DEG C；The air outlet temperature of the spray drying is 100
DEG C~110 DEG C；The compressed air of the spray drying is 0.1MPa~0.4MPa.
7. preparation method according to claim 2, which is characterized in that described that the lithium titanate precursor is sintered conjunction
At when heating mode are as follows: with heating rate be that 3 DEG C/min~8 DEG C/min is warming up to 800 DEG C~900 DEG C, heat preservation 2 hours~4
Hour.
8. preparation method according to claim 1, which is characterized in that described by the lithium titanate, Co3O4It is placed in aqueous solution
In and mix, obtain doping mixed liquor, specifically:
It disperses the lithium titanate in aqueous solution and stirs, obtain lithium titanate solution；
The Co is added in the lithium titanate solution3O4, continue to stir, until forming viscous paste, obtain the doping mixing
Liquid；
Wherein, the Co3O4The ratio for accounting for all solids content is 5%~15%.
9. preparation method according to claim 1, which is characterized in that described by the lithium titanate, Co3O4It is placed in aqueous solution
In and mix, obtain doping mixed liquor, specifically: by the lithium titanate, Co3O4It is placed in aqueous solution, passes through temperature constant magnetic stirring
Device carries out heating stirring, obtains the doping mixed liquor.
10. preparation method according to claim 1, which is characterized in that the drying time of the dry doping mixed liquor is 4
Hour~10 hours.
11. a kind of negative electrode material, which is characterized in that prepare shape using the described in any item preparation methods of the claims 1-10
At.
12. a kind of negative electrode tab, which is characterized in that the material of the negative electrode tab includes negative electrode material described in claim 11.
13. a kind of battery, which is characterized in that including the negative electrode tab described in claim 12.
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Application publication date: 20190531 |