CN109319830A - Lithium titanate material and preparation method thereof, negative electrode tab, battery - Google Patents
Lithium titanate material and preparation method thereof, negative electrode tab, battery Download PDFInfo
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Abstract
This application discloses a kind of preparation method of lithium titanate material, lithium titanate material, negative electrode tab, battery, preparation method includes: to obtain mixed slurry using wet-mixing mixing lithium source, titanium source and nitrogen source；The dry mixed slurry, obtains the lithium titanate precursor of nitrogen cladding；Nitrogen treatment is carried out to the lithium titanate precursor, obtains nitridation presoma；Carbon coating is carried out to the nitridation presoma, obtains carbon coating presoma；Carbonization treatment is carried out to the carbon coating presoma, obtains nitrogen carbon lithium titanate.The application improves the circulation performance of lithium titanate battery, more effectively maintains the spherical morphology of lithium titanate particle and the processing performance of battery material preparation；And battery flatulence can be prevented, improve the cycle life of battery；In addition, the wet process cladding process in the application is simpler than general sol gel process, and it is at low cost, it is suitable for large-scale industrial production.
Description
Technical field
This application involves energy storage device technical field, especially a kind of lithium titanate material and preparation method thereof, negative electrode tab, electricity
Pond.
Background technique
Compared with the carbon-based negative electrode material of tradition, lithium titanate material is no zero strain material, volume base during removal lithium embedded
This is unchanged, and cycle performance is good.But it is lower that there is also electronic conductivities, poorly conductive, and by the high institute's band of electrode potential
The low problem of the specific energy come, to limit application of the lithium titanate material on lithium ion battery.
Summary of the invention
In view of this, the mesh of the application is to provide a kind of lithium titanate material and preparation method thereof, negative electrode tab, battery, with
Solve the problems, such as that low existing lithium titanate material conductivity, poorly conductive and specific energy are low.
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 lithium titanate material, comprising:
Using wet-mixing mixing lithium source, titanium source and nitrogen source, mixed slurry is obtained；
The dry mixed slurry, obtains the lithium titanate precursor of nitrogen cladding；
Nitrogen treatment is carried out to the lithium titanate precursor, obtains nitridation presoma；
Carbon coating is carried out to the nitridation presoma, obtains carbon coating presoma；
Carbonization treatment is carried out to the carbon coating presoma, obtains nitrogen carbon lithium titanate.
It is optionally, described that mixed slurry is obtained using wet-mixing mixing lithium source, titanium source and nitrogen source, specifically:
The lithium source is dissolved in deionized water, obtains lithium source solution；
The titanium source is dissolved in lithium source solution, obtains lithium titanium mixed solution；
It will be mixed dissolved with the ethanol solution of nitrogen source with the lithium titanium mixed solution, obtain the mixed slurry.
Optionally, the mixing time by when mixing dissolved with the ethanol solution of nitrogen source with the lithium titanium mixed solution is 2
Hour~4 hours.
Optionally, the titanium source is selected from TiO2With one of metatitanic acid or two kinds of mixture；
And/or
The lithium source is selected from one of lithium carbonate, lithium bicarbonate, lithium hydroxide, lithium nitrate and lithium acetate or several
Mixture.
It is optionally, described that nitrogen treatment is carried out to the lithium titanate precursor, specifically:
The lithium titanate precursor is placed in nitrogen atmosphere protection stove and carries out pre-sintering and nitrogen treatment.
Optionally, the nitriding temperature that nitrogen treatment is carried out to the lithium titanate precursor are as follows: 550 DEG C~650 DEG C；Nitrogen
Changing the time is 2 hours~4 hours.
Optionally, the carbon-coated carbon source is selected from one of bitumen, coal tar pitch, asphalt or several
Mixture；
It is described that carbon coating is carried out to the nitridation presoma, specifically:
The nitridation presoma is added in the carbon disulfide dissolved with the carbon source, is stirred until carbon disulfide is waved
It distributes complete.
Optionally, the carbon-coated carbon source is selected from one of sucrose, glucose, phenolic resin or several mixing
Object；
It is described that carbon coating is carried out to the nitridation presoma, specifically:
The nitridation presoma is added in the ethanol water dissolved with the carbon source, is stirred.
The second aspect of the application provides a kind of lithium titanate material, is prepared by preparation method described in any of the above embodiments
It arrives.
The third aspect of the application provides a kind of negative electrode tab, including lithium titanate material as described above.
The fourth aspect of the application provides a kind of battery, including negative electrode tab as described above.
Then preparation method provided by the present application successively carries out it by first preparing the lithium titanate precursor of nitrogen cladding
Nitrogen treatment, carbon coating and carbonization treatment construct electrode material and electrolysis while improving lithium titanate material electric conductivity
Electrochemically stable interface between liquid improves the circulation performance of lithium titanate battery；More effectively maintain lithium titanate particle
The processing performance of spherical morphology and battery material preparation；And dual cladding constructs hydrophobic electrode interface, can prevent electrode material
The crystallization water in material enters electrolyte, while the traces of moisture for also inhibiting electrolyte system is diffused into electrode interface and is catalyzed
Reaction, the electrolyte decomposition generation gas limited in charge and discharge process improve the circulation longevity of battery to prevent battery flatulence
Life；In addition, the wet process cladding process in the application is simpler than general sol gel process, and it is at low cost, it is suitable for large-scale
Industrialized production.
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 of the lithium titanate for the nitrogen carbon dual cladding that 1~embodiment of embodiment 3 obtains；
Fig. 2 shows the SEM figures for the lithium carbonate that comparative example 1 obtains；
The common lithium carbonate that Fig. 3 shows the lithium titanate for the nitrogen carbon dual cladding that embodiment 1 obtains and comparative example 1 obtains
XRD spectrum.
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 lithium titanate material, comprising:
S10: using wet-mixing mixing lithium source, titanium source and nitrogen source, mixed slurry is obtained；
S20: dry mixed slurry obtains the lithium titanate precursor of nitrogen cladding；
S30: carrying out nitrogen treatment to lithium titanate precursor, obtains nitridation presoma；
S40: carbon coating is carried out to nitridation presoma, obtains carbon coating presoma；
S50: carbonization treatment is carried out to carbon coating presoma, obtains nitrogen carbon lithium titanate.
Above-mentioned preparation method, by first prepare nitrogen cladding lithium titanate precursor, then successively it is carried out nitrogen treatment,
Carbon coating and carbonization treatment obtain the lithium titanate modified material of nitrogen carbon dual interface, the particle for the nitrogen carbon lithium titanate prepared
Powder is tiny and is evenly distributed, and while improving lithium titanate material electric conductivity, constructs the electricity between electrode material and electrolyte
Chemical stabilization interface, improves the circulation performance and energy density of lithium titanate battery, and energy density can be improved 5~
10%, more effectively maintain the spherical morphology of lithium titanate particle and the processing performance of battery material preparation；And dual cladding constructs
Hydrophobic electrode interface, can prevent the crystallization water in electrode material from entering electrolyte, while also inhibiting electrolyte system
Traces of moisture is diffused into electrode interface and catalysis reaction occurs, and the electrolyte decomposition limited in charge and discharge process generates gas, thus
Battery flatulence is prevented, the cycle life of battery is also improved；In addition, the wet process cladding process in the application is more solidifying than general colloidal sol
Adhesive process is simple, at low cost, is suitable for large-scale industrial production.
Above-mentioned S10 obtains mixed slurry using wet-mixing mixing lithium source, titanium source and nitrogen source, specifically:
S11: being dissolved in deionized water for lithium source, the two can be made to be sufficiently mixed by stirring, obtain lithium source solution；
S12: being dissolved in lithium source solution for titanium source, the two can be made to be sufficiently mixed by stirring, obtain lithium titanium mixed solution；
S13: it will be mixed dissolved with the ethanol solution of nitrogen source with lithium titanium mixed solution, can mix by stirring, be mixed
Slurry.
Wherein, it can be prepared before S11 dissolved with the ethanol solution of nitrogen source, i.e., nitrogen source is first dissolved in ethanol solution, then into
Row S11.
It is in S13 that mixing time when mixing dissolved with the ethanol solution of nitrogen source with lithium titanium mixed solution is small for 2 hours~4
When, such as 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, so that dissolved with the ethanol solution and lithium titanium mixed solution of nitrogen source
Sufficiently mixed point.
In above-described embodiment, titanium source can be selected from TiO2With one of metatitanic acid or two kinds of mixture；Lithium source choosing
It is such as wherein any from one of lithium carbonate, lithium bicarbonate, lithium hydroxide, lithium nitrate and lithium acetate or several mixtures
Two kinds or three kinds of mixture.
Lithium source, the molar ratio of titanium source can be 4:5 in above-mentioned S10, and nitrogen source can be with the additive amount of mass percent 10%
Addition.
Mixed slurry can be spray-dried by dry mixed slurry in S20, and the inlet temperature that spray drying is arranged is
200 DEG C, outlet temperature is 95 DEG C, and the pressure of compressed air is 0.5MP, certainly, the inlet temperature of spray drying, outlet temperature with
And the pressure of compressed air may be other values, can according to need and is set, as long as drying mixed slurry thoroughly i.e.
It can.
Nitrogen treatment is carried out to lithium titanate precursor in S30, specifically:
Lithium titanate precursor is placed in nitrogen atmosphere protection stove and carries out pre-sintering and nitrogen treatment, such as by lithium titanate precursor
It is placed in the tube furnace of nitrogen protection and carries out pre-sintering and nitrogen treatment, to be sintered under the protection of nitrogen, realize nitridation
Processing.
Specifically, the nitriding temperature of nitrogen treatment is carried out to lithium titanate precursor are as follows: 550 DEG C~650 DEG C, such as 550 DEG C,
580 DEG C, 600 DEG C, 630 DEG C, 650 DEG C etc.；Nitridation time is 2 hours~4 hours, such as 2 hours, 2.5 hours, 3 hours, it is 3.5 small
When, 4 hours etc..Further, the realization that heats up twice can be passed through when nitrogen treatment, it can be warming up to the first heating rate
First temperature, heat preservation at the first time, are then warming up to second temperature again with second heating rate, kept the temperature for the second time, then
Furnace cooling.Wherein, the first temperature can be 200 DEG C~300 DEG C, such as 200 DEG C, 230 DEG C, 240 DEG C, 250 DEG C, 300 DEG C；The
Two temperature are above-mentioned nitriding temperature, are at the first time 0.5 hour~2 hours, such as 0.5 hour, 1 hour, 1.1 hours, it is 1.2 small
When, 1.4 hours, 1.5 hours, 2 hours etc., the second time was 3 hours~4 hours, such as 3 hours, 3.1 hours, 3.3 hours, 3.4
Hour, 3.5 hours, 4 hours etc.；The first heating rate and the second heating rate can be 2 DEG C/min~5 DEG C/min, such as 2 DEG C/
Min, 3 DEG C/min, 4 DEG C/min, 5 DEG C/min etc..
Carbon-coated carbon source is selected from one of bitumen, coal tar pitch, asphalt or several mixing in S40
Object, at this point, carbon coating is carried out to nitridation presoma in S40, specifically:
Nitridation presoma is added in the carbon disulfide dissolved with carbon source, is stirred until carbon disulfide volatilization finishes.
Wherein, in order to guarantee carbon-coated effect, nitridation presoma can be placed in together with the carbon disulfide mixture dissolved with carbon source
In constant temperature blender with magnetic force, it is stirred with specific revolving speed and temperature.
Carbon-coated carbon source can also be selected from one of sucrose, glucose, phenolic resin or several mixing in S40
Object, at this point, carbon coating is carried out to nitridation presoma in S40, specifically:
Nitridation presoma is added in the ethanol water dissolved with carbon source, is stirred, it specifically can be with 500rpm's
Revolving speed stirs 2 hours~6 hours, such as stirring 2 hours, 3 hours, 5 hours, 6 hours, to obtain carbon coating presoma.
In S50, carbonization treatment is carried out to carbon coating presoma, carbon coating presoma can be specifically placed in nitrogen or helium
Carbonization treatment is carried out in the furnace of gas shielded, can be warming up to 780 DEG C~830 in furnace with 3 DEG C/min~5 DEG C/min heating rate
DEG C, such as heating rate is 3 DEG C/min, 3.5 DEG C/min, 4 DEG C/min, 4.5 DEG C/min, 5 DEG C/min, is warming up to 780 DEG C, 790
DEG C, 800 DEG C, 820 DEG C, 830 DEG C etc.；Then 2 hours~4 hours are kept the temperature, such as heat preservation 2 hours, 2.5 hours, 3 hours, it is 3.5 small
When, 4 hours, furnace cooling again later.
In addition, the second aspect of the application provides a kind of lithium titanate material, the preparation as described in any of the above-described embodiment
Method is prepared, which can be applied to the negative electrode material of battery.The third aspect of the application provides one kind
Negative electrode tab, including lithium titanate material as described above.The fourth aspect of the application additionally provides a kind of battery, including as described above
Negative electrode tab.
The feature of the application and performance are described in further detail with reference to embodiments.
Embodiment 1
A kind of preparation method of lithium titanate material, comprising:
S110: raw material mixing: with lithium source, titanium source, 4:5, nitrogen source additive amount are 10% progress mixing in molar ratio, first by 54g
Acetylglucosamine is dissolved in 300ml ethanol solution；Then the LiOH.H2O of 282g (loss on ignition 57.4%) is added
In 1800ml deionized water, after stirring 30 minutes, the TiO2.H2O (loss on ignition 87.5%) of 500g is added, continues 30 points of stirring
Clock obtains lithium titanium mixed solution；The acetyl glucosamine amine aqueous solution of dissolution is poured into above-mentioned lithium titanium mixed solution again, continues to stir
2 hours, obtain mixed slurry.
S120: above-mentioned mixed slurry is spray-dried by spray drying, and setting inlet temperature is 200 DEG C, outlet temperature
It is 95 DEG C, the pressure of compressed air is 0.5MPa, obtains the lithium titanate precursor of nitrogen cladding.
S130: lithium titanate precursor nitridation: above-mentioned lithium titanate precursor is placed in the tube furnace of nitrogen protection in 600 DEG C
Under be pre-sintered and nitrogen treatment, Elevated Temperature Conditions: being first warming up to 200 DEG C with the heating rate of 3 DEG C/min, keep the temperature 30 minutes,
Then 600 DEG C are risen to same heating rate, keeps the temperature 3 hours, furnace cooling obtains nitridation presoma.
S140: it carbon coating: uses pitch as carbon source, 30g bitumen is first dissolved in 300ml carbon disulfide, then
200g is added and nitrogenizes presoma, the stirring temperature in draught cupboard in constant temperature blender with magnetic force with the revolving speed of 500r/min at 80 DEG C
The lower stirring of degree is finished to carbon disulfide volatilization, obtains carbon coating presoma.
S150: the synthesis of nitrogen carbon lithium titanate: carbon coating presoma in S140 is placed in nitrogen or the tube furnace of argon gas protection
Charing process；Elevated Temperature Conditions are that 5 DEG C/min rises to 800 DEG C, keep the temperature 3 hours, furnace cooling can obtain powerful nitrogen carbon metatitanic acid
Lithium material.
Embodiment 2
A kind of preparation method of lithium titanate material, comprising:
S210: raw material mixing: with lithium source, titanium source, 4:5, nitrogen source additive amount are 10% progress mixing in molar ratio, first by 54g
Acetylglucosamine is dissolved in 300ml ethanol solution；Then the lithium carbonate of 282g is added in 1800ml deionized water, stirring 30
After minute, the metatitanic acid of 500g is added, continues stirring 30 minutes, obtains lithium titanium mixed solution；Again by the acetyl glucosamine of dissolution
Amine aqueous solution pours into above-mentioned lithium titanium mixed solution, continues stirring 3 hours, obtains mixed slurry.
S220: above-mentioned mixed slurry is spray-dried by spray drying, and setting inlet temperature is 200 DEG C, outlet temperature
It is 95 DEG C, the pressure of compressed air is 0.5MPa, obtains the lithium titanate precursor of nitrogen cladding.
S230: lithium titanate precursor nitridation: above-mentioned lithium titanate precursor is placed in the tube furnace of nitrogen protection in 550 DEG C
Under be pre-sintered and nitrogen treatment, Elevated Temperature Conditions: being first warming up to 300 DEG C with the heating rate of 2 DEG C/min, keep the temperature 120 minutes,
Then 550 DEG C are risen to same heating rate, keeps the temperature 3.5 hours, furnace cooling obtains nitridation presoma.
S240: carbon coating: using sucrose as carbon source, 30g sucrose be first dissolved in 300ml ethanol water, then plus
Enter 200g nitridation presoma, the whipping temp in draught cupboard in constant temperature blender with magnetic force with the revolving speed of 500r/min at 80 DEG C
Lower stirring 2 hours, obtains carbon coating presoma.
S250: the synthesis of nitrogen carbon lithium titanate: carbon coating presoma in S240 is placed in nitrogen or the tube furnace of argon gas protection
Charing process；Elevated Temperature Conditions are that 5 DEG C/min rises to 780 DEG C, keep the temperature 4 hours, furnace cooling can obtain powerful nitrogen carbon metatitanic acid
Lithium material.
Embodiment 3
A kind of preparation method of lithium titanate material, comprising:
S310: raw material mixing: with lithium source, titanium source, 4:5, nitrogen source additive amount are 10% progress mixing in molar ratio, first by 54g
Acetylglucosamine is dissolved in 300ml ethanol solution；Then the LiOH.H2O of 282g (loss on ignition 57.4%) is added
In 1800ml deionized water, after stirring 30 minutes, the TiO2.H2O (loss on ignition 87.5%) of 500g is added, continues 30 points of stirring
Clock obtains lithium titanium mixed solution；The acetyl glucosamine amine aqueous solution of dissolution is poured into above-mentioned lithium titanium mixed solution again, continues to stir
4 hours, obtain mixed slurry.
S320: above-mentioned mixed slurry is spray-dried by spray drying, and setting inlet temperature is 200 DEG C, outlet temperature
It is 95 DEG C, the pressure of compressed air is 0.5MPa, obtains the lithium titanate precursor of nitrogen cladding.
S330: lithium titanate precursor nitridation: above-mentioned lithium titanate precursor is placed in the tube furnace of nitrogen protection in 650 DEG C
Under be pre-sintered and nitrogen treatment, Elevated Temperature Conditions: being first warming up to 250 DEG C with the heating rate of 5 DEG C/min, keep the temperature 90 minutes,
Then 650 DEG C are risen to same heating rate, keeps the temperature 4 hours, furnace cooling obtains nitridation presoma.
S340: it carbon coating: uses pitch as carbon source, 30g bitumen is first dissolved in 300ml carbon disulfide, then
200g is added and nitrogenizes presoma, the stirring temperature in draught cupboard in constant temperature blender with magnetic force with the revolving speed of 500r/min at 80 DEG C
The lower stirring of degree is finished to carbon disulfide volatilization, obtains carbon coating presoma.
S350: the synthesis of nitrogen carbon lithium titanate: carbon coating presoma in S340 is placed in nitrogen or the tube furnace of argon gas protection
Charing process；Elevated Temperature Conditions are that 3 DEG C/min rises to 830 DEG C, keep the temperature 2 hours, furnace cooling can obtain powerful nitrogen carbon metatitanic acid
Lithium material.
Comparative example 1
A kind of preparation method of lithium titanate material, comprising:
S410: raw material mixing: wherein 4:5 carries out mixing in molar ratio for titanium source, lithium source, does not add nitrogen source.First by 282g's
LiOH.H2O is lithium source (loss on ignition 57.4%), in 1800ml deionized water, adds 500g's after stirring 30 minutes
TiO2.H2O (loss on ignition 87.5%) continues stirring 2 hours.
S420: spray drying: above-mentioned slurry is spray-dried, and setting inlet temperature is 200 DEG C, outlet temperature 95
DEG C, the pressure of compressed air is 0.5MPa；The lithium titanate precursor of nitrogenous cladding can be obtained.
S430: lithium titanate synthesis: above-mentioned presoma is placed in the tube furnace of nitrogen protection, pre-burning is carried out at 800 DEG C
Knot, Elevated Temperature Conditions are 3 DEG C/min to rising to 800 DEG C, keep the temperature 3 hours, then furnace cooling can obtain common lithium titanate material.
The particle obtained using S120 in Malvern ParticleSizer testing example 1, D50 are 5.2um or so, and D99 is
Particle in 12.3um or so, S150, D50 are 9.2um or so, and D99 is 17.3um or so.Tap density meter tests the vibration in S150
Real density is 1.25g/ml；Specific surface area is 9.51m2/g。
Above-mentioned gained nitrogen carbon lithium titanate material is used into scanning electron microscopic observation microscopic appearance, as Figure 1-Figure 2, wherein
Fig. 1 is the SEM figure for the nitrogen carbon lithium titanate that 1~embodiment of embodiment 3 obtains, and Fig. 2 is the SEM figure for the lithium carbonate that comparative example 1 obtains,
It can be seen from Fig. 1, Fig. 2 compared with the common LTO of no cladding (the conventional lithium carbonate of uncoated nitrogen carbon) material, NC-LTO (nitrogen
Carbon lithium titanate) back scattering scanning figure it is obviously clear, the electric conductivity of the lithium titanate material after also illustrating nitrogen carbon dual cladding is bright
It is aobvious to improve.
In addition, by lithium titanate material prepared by nitrogen carbon lithium titanate material, comparative example 1 prepared by above-described embodiment 1 point
It is not mixed with superconduction carbon black binder in the ratio of 90:5:5, prepares negative electrode diaphragm, then dry, slice is prepared into cathode
Piece.Using metal lithium sheet as positive plate, C1garde makees diaphragm, uses 1M LiPF6-EC/DMC (volume ratio 1:1) for electrolysis
Liquid is assembled button cell in the glove box full of argon gas, the performance of each battery is tested using new prestige cell tester, in 0.2C
After discharging for the first time, 0.5C, 1C, 2C, 5C, 10C and 20C charge-discharge magnification and loop test are carried out respectively, the results are shown in Table 1.
Table 1
In conjunction with table 1 and Fig. 3, Fig. 3 is the nitrogen carbon lithium titanate that embodiment 1 obtains and the common lithium carbonate that comparative example 1 obtains
There is bulge (in figure shown in rectangle frame) at 10 ° or so in map in XRD spectrum, becomes unformed after showing pitch charing
Carbon, it is seen that lithium titanate is coated fabulous by carbonizable substance；And other peak shapes of NC-LTO are consistent with the LTO peak shape of no cladding, illustrate nitrogen
There is no the crystal forms for changing LTO for the dual interface of carbon.As can be seen from Table 1, in 0.2C, discharge capacity, embodiment 1 are made for the first time
Standby battery is 174.3mAh/g, and comparative example 1 is 170.1mAh/g, and embodiment 1 is apparently higher than comparative example 1, and 0.5C, 1C,
The discharge capacity for the first time of 2C, 5C, 10C and 20C are even more to be apparently higher than comparative example 1；In addition, in 0.2C, 0.5C, 1C, 2C, 5C, 10C
And in the capacity retention ratio comparison of 20C, embodiment 1 is close compared with comparative example 1.
It can be seen that therefore the lithium titanate material of the preparation method of the application preparation can either effectively improve lithium titanate material
Electric conductivity and high rate performance nor affect on the cycle performance of lithium titanate itself.
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 (11)
1. a kind of preparation method of lithium titanate material characterized by comprising
Using wet-mixing mixing lithium source, titanium source and nitrogen source, mixed slurry is obtained；
The dry mixed slurry, obtains the lithium titanate precursor of nitrogen cladding；
Nitrogen treatment is carried out to the lithium titanate precursor, obtains nitridation presoma；
Carbon coating is carried out to the nitridation presoma, obtains carbon coating presoma；
Carbonization treatment is carried out to the carbon coating presoma, obtains nitrogen carbon lithium titanate.
2. preparation method according to claim 1, which is characterized in that it is described using wet-mixing mixing lithium source, titanium source and
Nitrogen source obtains mixed slurry, specifically:
The lithium source is dissolved in deionized water, obtains lithium source solution；
The titanium source is dissolved in lithium source solution, obtains lithium titanium mixed solution；
It will be mixed dissolved with the ethanol solution of nitrogen source with the lithium titanium mixed solution, obtain the mixed slurry.
3. preparation method according to claim 2, which is characterized in that it is described will be dissolved with the ethanol solution of nitrogen source and the lithium
Mixing time when titanium mixed solution mixes is 2 hours~4 hours.
4. preparation method according to claim 1, which is characterized in that the titanium source is selected from TiO2One of with metatitanic acid
Or two kinds of mixture；
And/or
The lithium source is selected from one of lithium carbonate, lithium bicarbonate, lithium hydroxide, lithium nitrate and lithium acetate or several mixing
Object.
5. preparation method according to claim 1, which is characterized in that described to be carried out at nitridation to the lithium titanate precursor
Reason, specifically:
The lithium titanate precursor is placed in nitrogen atmosphere protection stove and carries out pre-sintering and nitrogen treatment.
6. preparation method according to claim 5, which is characterized in that described to be carried out at nitridation to the lithium titanate precursor
The nitriding temperature of reason are as follows: 550 DEG C~650 DEG C；Nitridation time is 2 hours~4 hours.
7. preparation method according to claim 1, which is characterized in that the carbon-coated carbon source is selected from bitumen, coal
One of pyrobitumen, asphalt or several mixtures；
It is described that carbon coating is carried out to the nitridation presoma, specifically:
The nitridation presoma is added in the carbon disulfide dissolved with the carbon source, is stirred until carbon disulfide is evaporated completely
Finish.
8. preparation method according to claim 1, which is characterized in that the carbon-coated carbon source be selected from sucrose, glucose,
One of phenolic resin or several mixtures；
It is described that carbon coating is carried out to the nitridation presoma, specifically:
The nitridation presoma is added in the ethanol water dissolved with the carbon source, is stirred.
9. a kind of lithium titanate material, which is characterized in that be prepared by the described in any item preparation methods of claim 1-8.
10. a kind of negative electrode tab, which is characterized in that including lithium titanate material as claimed in claim 9.
11. a kind of battery, which is characterized in that including negative electrode tab described in any one of claim 10.
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