CN106159219B - A kind of surface cladding LiTi2O4Lithium titanate material and preparation method thereof - Google Patents
A kind of surface cladding LiTi2O4Lithium titanate material and preparation method thereof Download PDFInfo
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- CN106159219B CN106159219B CN201510184211.XA CN201510184211A CN106159219B CN 106159219 B CN106159219 B CN 106159219B CN 201510184211 A CN201510184211 A CN 201510184211A CN 106159219 B CN106159219 B CN 106159219B
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- 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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- 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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- 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
The present invention provides a kind of surface cladding LiTi2O4Lithium titanate material and preparation method thereof.LiTi2O4With stable spinel structure as lithium titanate, it is often more important that LiTi2O4Electronic conductivity is far above lithium titanate, and LiTi2O4Cell parameter it is bigger than lithium titanate, the present invention covers LiTi in lithium titanate bread2O4The high rate performance of lithium titanate material can be effectively improved afterwards, can be suitable for high current charge-discharge, and do not influence the cycle performance of lithium titanate itself.Material prepared good rate capability and cycle performance is excellent according to the method for the present invention.In addition, raw material needed for the invention are cheap, technological process is simple, it is suitble to industrialized production.
Description
The invention belongs to clean energy technology field, it is related to a kind of lithium ion battery negative material and preparation method thereof, it is special
It is not a kind of surface cladding LiTi2O4Lithium titanate material and preparation method thereof.
Background technology
In recent years, lithium ion chargeable battery is of increased attention as Ke Xunhuanliyong clean energy resource,
And it is widely applied on various digital products and the vehicles.It is more and more wider with the range of application, to lithium ion battery
Safety, more stringent requirements are proposed for forthright again and service life.Lithium ion battery currently on the market mostly uses greatly can be embedding
Lithium carbon material is as negative material.But carbon material causes its surface to be easy precipitating metal Li dendrite since intercalation potential is relatively low, from
And pierce through diaphragm and cause internal short-circuit of battery, cause cells burst even to explode.And the lithium titanate with spinel structure
(Li4Ti5O12) it is used as a kind of " zero strain " material, there is good cycle performance, while higher (the 1.55V Li of its intercalation potential+/ Li), Li dendrite will not be precipitated in charge and discharge process, it is safe, it is believed under replacing carbon material to become ideal
Generation lithium cell cathode material.But lithium titanate electronic conductivity is low, high rate performance is poor, is not suitable for high current charge-discharge, leads
It is caused to be applied to the high-power batteries such as electric vehicle field limited.Therefore, improve lithium titanate material conductivity and high rate performance by
Gradually become research hotspot.
Currently, the main method for improving lithium titanate material electronic conductivity includes by its nanosizing, element doping and surface
Cladding.Wherein, by after material nano, material specific surface area is significantly increased, and causes material to be easy to reunite, it is difficult to increase battery slurrying
Degree.Element doping often while improving lithium titanate material, changes the original lattice structure of lithium titanate, is followed so as to cause it
Ring reduced performance.And surface is coated in the case of coating selection improperly, such as various carbon coatings, lithium titanate material can only be improved
The electronic conductance of material, and the carbon-coating on lithium titanate particle surface is to Li+Diffusivity castering action unobvious at interface, or even meeting
Hinder Li+Diffusion at interface；And often specific surface is bigger for carbon-coated lithium titanate material, and group also easily occurs when use
It is poly-.
Invention content
To solve the above-mentioned problems, lithium titanate material conductivity and high rate performance are improved, the present invention uses sol-gal process
LiTi is covered in lithium titanate bread2O4Material.LiTi2O4As the same based material of lithium titanate, with what is stablized as lithium titanate
Spinel structure, it is often more important that LiTi under room temperature2O4The resistivity of pressed powder be 1.8 m Ω cm (Yang Jianwen etc.,
LiTi2O4Progress as negative electrode of lithium ion battery, chemistry notification, the 12nd phase in 2008), i.e., electronic conductivity is 5.56
×104S·cm-1Far above the electronic conductivity (＜ 10 of lithium titanate-13S·cm-1)(Yoshihiro KADOMA,Yusuke
CHIBA,Daisuke YOSHIKAWA,Yuko MITOBE,Naoaki KUMAGAI,and Koichi UI,Influence of
the Carbon Source on the Surface and Electrochemical Characteristics of
Lithium Excess Li4.3Ti5O12Carbon Composite, Electrochemistry, 80 (10), 759-761
(2012)).And LiTi2O4Cell parameter be a=0.8391nm, be more than lithium titanate cell parameter (lithium titanate a=
0.83588nm), after lithium titanate surface forms clad, the insertion and abjection of lithium ion are more advantageous to.Therefore, the present invention exists
Lithium titanate bread covers LiTi2O4The high rate performance of lithium titanate material can be effectively improved afterwards, can be suitable for large current density
Electricity, and the cycle performance of lithium titanate itself is not influenced.In addition, this method is simple for process, it is easy to industrialize.
The present invention provides a kind of surface cladding LiTi2O4Lithium titanate material, the material be surface coat LiTi2O4Titanium
Sour lithium, wherein LiTi2O4The mass percent for accounting for material gross mass was 0%~15% (not including 0%)；It is preferred that 5%~15%.
Wherein, above-mentioned surface coats LiTi2O4Lithium titanate material covered in lithium titanate bread by using sol-gal process
LiTi2O4Material is made.
Specifically, surface of the invention coats LiTi2O4The preparation method of lithium titanate material include the following steps：
(1) according to the cladding substance LiTi of design2O4Mass percent in product (material) weigh lithium titanate,
Lithium source and titanium source；
(2) lithium source weighed up in step (1) is dispersed in dispersant, lithium source dispersion liquid is made；
(3) titanium source weighed up in step (1) is dispersed in dispersant, titanium source dilution is made；
(4) titanium source dilution is added drop-wise in lithium source dispersion liquid and mixed liquor is made, then the lithium titanate that will be weighed up in step (1)
It is added in mixed liquor and stirs evenly, then dry to obtain presoma；
(5) presoma obtained in step (4) is placed in atmosphere furnace, is warming up under inert atmosphere or reducing atmosphere
After 600~800 DEG C of 2~8h of heat preservation, cooled to room temperature coats LiTi to get to surface2O4Lithium titanate material.
Wherein, raw material lithium titanate can be obtained by any method for preparing lithium titanate in this field in step (1), preferred
Preparation method is：
(a) Li in molar ratio:Ti=4~4.1：5 weigh lithium source and titanium dioxide, and to be added ball milling mixing in dispersant uniform,
Mixed slurry drying and screening is obtained into white powder；
(b) white powder obtained by step (a) is placed in atmosphere furnace, is warming up to 700~900 DEG C of heat preservations in air atmosphere
Cooled to room temperature after 4~12h, obtains lithium titanate material.
Wherein, the titanium dioxide crystal form described in step (a) is one kind or combinations thereof in rutile-type or anatase titanium dioxide.
Lithium source described in step (1) and step (a) is respectively selected from lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, nitre
The combination of one or more of sour lithium, lithium citrate or lithium alkylide.
Dispersant described in step (a) is the combination of one or more of water, absolute ethyl alcohol, propyl alcohol or acetone.
Dispersant described in step (2) and step (3) is respectively selected from 50%~80% ethanol water.
Titanium source described in step (1) is in the chloride of butyl titanate, tetraethyl titanate, tetraisopropyl titanate or titanium
One or more of combinations.
Inert atmosphere or reducing atmosphere described in step (5) are one or more of nitrogen, argon gas or hydrogen
Combination.
Surface obtained coats LiTi according to the method described above2O4Lithium titanate material, safety and stability, electronic conductivity is high, times
Rate performance is good (10C/1C capacity retention ratios are more than 85%), can be used for high current charge-discharge, and good cycle (55 DEG C, 3C
After recycling 300 times 90%) capacity retention ratio is more than, and can be used in the high-power batteries such as electric vehicle field.In addition the party is used
Method, required raw material are cheap, technological process is simple, are suitble to industrialized production.
Description of the drawings
Fig. 1 is that the surface prepared by embodiment 1 coats LiTi2O4Charge and discharge of the lithium titanate anode material under 1C multiplying powers
Curve.
Fig. 2 is that the surface prepared by embodiment 1 coats LiTi2O4Lithium titanate anode material and reference example prepare metatitanic acid
Lithium material high rate performance correlation curve.
Fig. 3 is that the surface prepared by embodiment 1 coats LiTi2O4Lithium titanate anode material and reference example prepare metatitanic acid
Lithium material cycle performance correlation curve under 55 DEG C, 3C multiplying powers.
Fig. 4 is that the surface prepared by embodiment 1 coats LiTi2O4Lithium titanate anode material and reference example prepare metatitanic acid
The stereoscan photograph of lithium material.
Specific implementation mode
LiTi is coated to surface provided by the invention with reference to specific embodiment2O4Lithium titanate anode material preparation
Method is described further.But the present invention is not limited in following embodiment.
Reference example：
Li in molar ratio:Ti=4：5 weigh lithium carbonate and anatase titanium dioxide, and that ball milling mixing in absolute ethyl alcohol is added is equal
It is even, mixed slurry is dried to obtain white powder；Gained white powder is placed in atmosphere furnace and is heated up in air atmosphere
Cooled to room temperature obtains lithium titanate material after to 900 DEG C of heat preservation 4h.
Embodiment 1：
Li in molar ratio:Ti=4：5 weigh lithium carbonate and anatase titanium dioxide, and that ball milling mixing in absolute ethyl alcohol is added is equal
It is even, mixed slurry drying and screening is obtained into white powder；Gained white powder is placed in atmosphere furnace in air atmosphere
Cooled to room temperature obtains lithium titanate material after being warming up to 900 DEG C of heat preservation 4h.
By LiTi in synthetic product2O4Design content is that 13wt% weighs lithium titanate, lithium carbonate and butyl titanate；It will claim
Good lithium carbonate is dispersed in 50% ethanol water, and lithium carbonate dispersion liquid is made；The butyl titanate weighed up is equal
It is even to be dispersed in 70% ethanol water, butyl titanate dilution is made；Butyl titanate dilution is added drop-wise to carbonic acid
Mixed liquor is made in lithium dispersion liquid, then the lithium titanate weighed up is added in mixed liquor and is stirred evenly, then drying obtains presoma；
Obtained presoma is placed in atmosphere furnace cooled to room temperature after being warming up to 800 DEG C of heat preservation 4h in a nitrogen atmosphere to obtain
Surface coats LiTi2O4Lithium titanate material, coating mass percent be 13wt%.
Embodiment 2：
Li in molar ratio:Ti=4.05：5, which weigh ball milling in lithium carbonate and rutile titanium dioxide addition absolute ethyl alcohol, mixes
It closes uniformly, mixed slurry drying and screening is obtained into white powder；Gained white powder is placed in atmosphere furnace in air gas
Cooled to room temperature obtains lithium titanate material after being warming up to 900 DEG C of heat preservation 8h under atmosphere.
By LiTi in synthetic product2O4Design content is that 10wt% weighs lithium titanate, lithium hydroxide and tetraethyl titanate；It will
The lithium hydroxide weighed up is dispersed in 50% ethanol water, and lithium hydroxide dispersion liquid is made；The metatitanic acid four that will be weighed up
Ethyl ester is dispersed in 70% ethanol water, and tetraethyl titanate dilution is made；Tetraethyl titanate dilution is added dropwise
To being made mixed liquor in lithium hydroxide dispersion liquid, then the lithium titanate weighed up is added in mixed liquor and is stirred evenly, then dried
To presoma；Obtained presoma is placed in atmosphere furnace after being warming up to 700 DEG C of heat preservation 6h under an argon atmosphere and is naturally cooled to
Room temperature obtains surface cladding LiTi2O4Lithium titanate material, coating mass percent be 10wt%.
Embodiment 3：
Li in molar ratio:Ti=4.1：5 weigh lithium hydroxide and anatase titanium dioxide to be added to the water ball milling mixing uniform,
Mixed slurry drying and screening is obtained into white powder；Gained white powder is placed in atmosphere furnace and is heated up in air atmosphere
Cooled to room temperature obtains lithium titanate material after to 800 DEG C of heat preservation 8h.
By LiTi in synthetic product2O4Design content is that 6wt% weighs lithium titanate, lithium oxalate and tetraisopropyl titanate；It will claim
Good lithium oxalate is dispersed in 50% ethanol water, and lithium oxalate dispersion liquid is made；The tetraisopropyl titanate that will be weighed up
It is dispersed in 70% ethanol water, tetraisopropyl titanate dilution is made；Tetraisopropyl titanate dilution is added dropwise
To being made mixed liquor in lithium oxalate dispersion liquid, then the lithium titanate weighed up is added in mixed liquor and be stirred evenly, then drying obtains
Presoma；Obtained presoma is placed in atmosphere furnace after being warming up to 600 DEG C of heat preservation 8h in a hydrogen atmosphere and naturally cools to room
Temperature obtains surface cladding LiTi2O4Lithium titanate material, coating mass percent be 6wt%.
Embodiment 4：
Li in molar ratio:Ti=4.1：5 weigh lithium hydroxide and anatase titanium dioxide to be added to the water ball milling mixing uniform,
Mixed slurry drying and screening is obtained into white powder；Gained white powder is placed in atmosphere furnace and is heated up in air atmosphere
Cooled to room temperature obtains lithium titanate material after to 700 DEG C of heat preservation 8h.
By LiTi in synthetic product2O4Design content is that 6wt% weighs lithium titanate, lithium acetate and butyl titanate；It will weigh up
Lithium acetate be dispersed in 55% ethanol water, lithium acetate dispersion liquid is made；The butyl titanate weighed up is uniform
It is dispersed in 80% ethanol water, butyl titanate dilution is made；Butyl titanate dilution is added drop-wise to lithium acetate
Mixed liquor is made in dispersion liquid, then the lithium titanate weighed up is added in mixed liquor and is stirred evenly, then drying obtains presoma；
Obtained presoma be placed in atmosphere furnace be warming up in a hydrogen atmosphere 600 DEG C heat preservation 6h after cooled to room temperature obtain table
Bread covers LiTi2O4Lithium titanate material, coating mass percent be 6wt%.
Claims (14)
1. a kind of surface coats LiTi2O4Lithium titanate material, which is characterized in that the material be surface coat LiTi2O4Metatitanic acid
Lithium, wherein LiTi2O4The mass percent for accounting for material gross mass is 0%~15%, but does not include 0%；
Wherein, the lithium titanate material is prepared by the following method：
(1) according to the cladding substance LiTi of design2O4Mass percent in the material weighs lithium titanate, lithium source and titanium source；
(2) lithium source weighed up in step (1) is dispersed in dispersant, lithium source dispersion liquid is made；
(3) titanium source weighed up in step (1) is dispersed in dispersant, titanium source dilution is made；
(4) titanium source dilution is added drop-wise in lithium source dispersion liquid and mixed liquor is made, then the lithium titanate weighed up in step (1) is added
It is stirred evenly in mixed liquor, drying obtains presoma；
(5) presoma obtained in step (4) is placed in atmosphere furnace, 600 is warming up under inert atmosphere or reducing atmosphere
Cooled to room temperature coats LiTi to get to surface after~800 DEG C of 2~8h of heat preservation2O4Lithium titanate material.
2. surface according to claim 1 coats LiTi2O4Lithium titanate material, which is characterized in that the LiTi2O4Quality
Percentage is 5%~15%.
3. surface according to claim 1 or 2 coats LiTi2O4Lithium titanate material, it is characterised in that：Institute in step (1)
The one kind or several of the lithium source stated in lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium nitrate, lithium citrate or lithium alkylide
The combination of kind.
4. surface according to claim 1 or 2 coats LiTi2O4Lithium titanate material, it is characterised in that：Institute in step (2)
The dispersant described in dispersant and step (3) stated independently selected from 50%~80% ethanol water.
5. surface according to claim 1 or 2 coats LiTi2O4Lithium titanate material, it is characterised in that：Institute in step (1)
The titanium source stated is the combination of one or more of chloride of butyl titanate, tetraethyl titanate, tetraisopropyl titanate or titanium.
6. surface according to claim 1 or 2 coats LiTi2O4Lithium titanate material, it is characterised in that：Institute in step (5)
The inert atmosphere or reducing atmosphere stated are the combination of one or more of nitrogen, argon gas or hydrogen.
7. a kind of surface according to claim 1 or 2 coats LiTi2O4Lithium titanate material preparation method, feature exists
In the preparation method comprises the steps of：
(1) according to the cladding substance LiTi of design2O4Mass percent in the material weighs lithium titanate, lithium source and titanium source；
(2) lithium source weighed up in step (1) is dispersed in dispersant, lithium source dispersion liquid is made；
(3) titanium source weighed up in step (1) is dispersed in dispersant, titanium source dilution is made；
(4) titanium source dilution is added drop-wise in lithium source dispersion liquid and mixed liquor is made, then the lithium titanate weighed up in step (1) is added
It is stirred evenly in mixed liquor, drying obtains presoma；
(5) presoma obtained in step (4) is placed in atmosphere furnace, 600 is warming up under inert atmosphere or reducing atmosphere
Cooled to room temperature coats LiTi to get to surface after~800 DEG C of 2~8h of heat preservation2O4Lithium titanate material.
8. preparation method according to claim 7, which is characterized in that the preparation of the raw material lithium titanate in the step (1)
Method is：
(a) Li in molar ratio:Ti=4~4.1：5, which weigh lithium source and titanium dioxide, is added in dispersant that ball milling mixing is uniform, will mix
Slurry drying and screening after conjunction obtains white powder；
(b) white powder obtained by step (a) is placed in atmosphere furnace, be warming up in air atmosphere 700~900 DEG C of heat preservations 4~
Cooled to room temperature after 12h, obtains lithium titanate material.
9. preparation method according to claim 8, it is characterised in that：Titanium dioxide crystal form described in step (a) is gold
One kind in red stone-type or anatase titanium dioxide or combination thereof.
10. preparation method according to claim 7 or 8, it is characterised in that：Lithium source described in step (1) and step (a)
It is respectively selected from one or more of lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium nitrate, lithium citrate or lithium alkylide
Combination.
11. preparation method according to claim 8, it is characterised in that：Dispersant described in step (a) is water, anhydrous
The combination of one or more of ethyl alcohol, propyl alcohol or acetone.
12. preparation method according to claim 7, it is characterised in that：Dispersant described in step (2) and step (3)
Described in dispersant independently selected from 50%~80% ethanol water.
13. preparation method according to claim 7, it is characterised in that：Titanium source described in step (1) is four fourth of metatitanic acid
Ester, tetraethyl titanate, tetraisopropyl titanate or titanium one or more of chloride combination.
14. preparation method according to claim 7, it is characterised in that：Inert atmosphere described in step (5) or reproducibility
Atmosphere is the combination of one or more of nitrogen, argon gas or hydrogen.
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| CN107871864B (en) * | 2017-04-27 | 2020-12-18 | 乳源东阳光磁性材料有限公司 | Titanium modified high-nickel multi-element positive electrode material and preparation method thereof |
| CN107946554A (en) * | 2017-10-26 | 2018-04-20 | 天津普兰能源科技有限公司 | A kind of preparation method of lithium battery lithium titanate anode material |
| CN114583149A (en) * | 2022-03-07 | 2022-06-03 | 北京泰斯利科技有限公司 | Titanium-based negative electrode material with surface coated with low-valence titanium compound in situ and preparation method thereof |
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| CN104377344A (en) * | 2014-09-30 | 2015-02-25 | 李宏斌 | Preparation method and use of LiTi2O4-graphene composite material |
| CN104477979A (en) * | 2014-12-17 | 2015-04-01 | 湖南大学 | Method for preparing LiTi204 powder material |
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| CN104377344A (en) * | 2014-09-30 | 2015-02-25 | 李宏斌 | Preparation method and use of LiTi2O4-graphene composite material |
| CN104477979A (en) * | 2014-12-17 | 2015-04-01 | 湖南大学 | Method for preparing LiTi204 powder material |
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