CN106207089A - A kind of used as negative electrode of Li-ion battery lithium titanate nano-tube material and preparation method thereof - Google Patents
A kind of used as negative electrode of Li-ion battery lithium titanate nano-tube material and preparation method thereof Download PDFInfo
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- CN106207089A CN106207089A CN201610567687.6A CN201610567687A CN106207089A CN 106207089 A CN106207089 A CN 106207089A CN 201610567687 A CN201610567687 A CN 201610567687A CN 106207089 A CN106207089 A CN 106207089A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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- H—ELECTRICITY
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
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- 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
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Abstract
The invention discloses a kind of used as negative electrode of Li-ion battery lithium titanate nano-tube material and preparation method thereof, it is therefore intended that promote the charge transmission of lithium titanate, to play its high-rate charge-discharge capability.The raw material of lithium titanate nanotube of the present invention is titanium salt: lithium salts Ti: Li=1: 1 ~ 1.5, and its molecular formula is Li4Ti5O12, the caliber of this lithium titanate nanotube is 1 20nm, a length of 50 50nm.Described method is for using dynamic agitation to drive force method, by controlling the presoma titanium salt/ratio of lithium salts, solvent thermal temperature/time, is aided with the programs such as follow-up centrifugal/washing/drying/calcining, obtains lithium titanate nano-tube material.After measured, when the lithium titanate nano-tube material present invention prepared is used as lithium ion battery negative material, it has higher specific discharge capacity and cyclical stability.Meanwhile, the preparation method of the present invention has that reaction temperature is low, react the advantage such as controlled, is suitable for large-scale production, and development prospect is boundless.
Description
Technical field
The present invention relates to Material Field, especially lithium ion battery negative technical field, be specially a kind of lithium ion battery
Negative pole lithium titanate nano-tube material and preparation method.The lithium titanate nano-tube material of the present invention is expected to promote lithium ion battery
Reversible specific capacity, the development for lithium ion battery is significant.
Background technology
Lithium ion battery have voltage height, energy density height, light weight, internal resistance is little, have extended cycle life, memory-less effect and
The advantages such as environmental friendliness, become the focus of research the most both at home and abroad, at information technology, mobile communication, electric automobile, fuel combination
There is huge market potential in the field such as automobile and science and techniques of defence.
Lithium ion battery is mainly made up of positive pole, negative pole, electrolyte and four parts of isolating membrane.It is substantially a kind of lithium
Ion concentration cell, both positive and negative polarity is made up of different Lithium-ion embeding compounds.As the critical material in lithium ion battery, negative
The performance of pole material will directly affect the overall performance of battery.Material with carbon element is also to be the lithium being most widely used at present the earliest simultaneously
Ion battery bears panel material.The Lithium-ion embeding current potential of material with carbon element is low, and specific capacity is high, conducts electricity very well, and good cycle is not allowed
Easily react with organic solvent, and aboundresources, cheap, nontoxic pollution-free.SANYO GS company utilizes high-quality natural stone
Ink at high temperature with appropriate steam effect, improve the ability of its embedding lithium.Sony and Nissan Motor's research show graphite
The defect at alkene surface and edge can receive the substantial amounts of lithium ion of receiving, increases specific capacity.But material with carbon element specific discharge capacity carries
Rise limited space, and it is easily formed Li dendrite at high magnification and low temperature when charging, cause short circuit potential safety hazard, limit it
Popularization and application.
Negative material nanorize is likely significantly improved the chemical property of negative material.First nano material can have
Effect ground reduces Lithium-ion embeding and the time of deintercalation, the fast charging and discharging performance of reinforcing material；The most more grain boundary, can
To provide quick lithium ion transport passage, improve charge-exchange speed；The bigger space of nano material existence can accommodate again
Expanding, the least absolute volume change can reduce the structural instability that in cyclic process, change in volume is brought, bigger
Deformability can bear the stress that change in volume produces, and therefore can be effectively improved the cycle performance of material.
Particularly one-dimensional nano-array relies on its distinctive directive construction, can effectively improve the cycle performance of negative pole with big
Rate charge-discharge performance.This is due to the specific surface area that (1) one-dimensional nano-array is bigger, adds defect and the activity on surface
Site, can improve the specific capacity of material；(2) electrolyte can enter the inside of one-dimensional nano-array, improves active material
With contacting of electrolyte, add the diffusion velocity of lithium ion, improve the high rate charge-discharge performance of material；(3) lithium ion
Embedding and the distance of deintercalation is shorter, one-dimensional nano-array structure enhances electronic conductivity simultaneously, improves the big multiplying power of material
Charge-discharge performance；(4) space in the middle of one-dimensional nano-array can accommodate material expansion in charge and discharge process, decreases material
Rupturing and efflorescence of material, the structure of one-dimensional nano-array is possible to prevent the reunion of material simultaneously, thus is effectively improved circulation
Stability.
Wherein lithium titanate has fabulous high rate charge-discharge performance and has obtained paying close attention to widely.It is brilliant that lithium titanate belongs to point
Stone-type structure, its structure can be the passage of the diffusion offer three-dimensional of lithium ion.During the embedding and abjection of lithium ion, titanium
The varying less of cell parameter of acid lithium, Unit cell volume change is only 0 ~ 0.3%, so lithium titanate is generally otherwise known as " zero
Strain " material.
Extremely low change in volume and sufficient lithium ion duct so that lithium titanate has the most excellent cycle performance with big
Rate charge-discharge performance.But the theoretical specific capacity of lithium titanate electrode is only 175.1 mAh/g, less than the one of commercialization graphite
Half, higher (the 1.55 V vs Li/Li of the current potential of Lithium-ion embeding simultaneously+) so that the open-circuit voltage of whole lithium ion battery is relatively
Low, limit the lithium titanate application as negative material.
Summary of the invention
Present invention aim at: for the problem of above-mentioned existence, it is provided that a kind of used as negative electrode of Li-ion battery lithium titanate nanometer
Tube material and preparation method thereof.Different from existing lithium titanate particle, the present invention proposes a kind of used as negative electrode of Li-ion battery lithium titanate
Nanotube, it has higher specific discharge capacity, and the development to lithium ion battery has important function.Meanwhile, the present invention provides
A kind of preparation method of super used as negative electrode of Li-ion battery lithium titanate nanotube, the method respectively using titanium salt and lithium salts as raw material,
Use dynamic agitation to drive force method, by controlling the presoma titanium salt/ratio of lithium salts, solvent thermal temperature/time, be aided with follow-up
The programs such as centrifugal/washing/drying/calcining, obtain lithium titanate nano-tube material.Through measuring, lithium titanate prepared by the present invention
When nano-tube material is used as lithium ion battery negative material, it has higher specific discharge capacity and cyclical stability.Meanwhile, originally
The preparation method of invention has that reaction temperature is low, react the advantage such as controlled, is suitable for large-scale production, and development prospect is the widest
Wealthy.
To achieve these goals, the present invention adopts the following technical scheme that
A kind of used as negative electrode of Li-ion battery lithium titanate nano-tube material, the raw material of described lithium titanate nanotube is titanium salt: lithium salts
Ti: Li=1: 1 ~ 1.5, its molecular formula is Li4Ti5O12, the caliber of this lithium titanate nanotube is 1-20nm, a length of 50-50nm.
A kind of preparation method of used as negative electrode of Li-ion battery lithium titanate nano-tube material, comprise the steps: with titanium salt and
Lithium salts is raw material, uses dynamic agitation to drive force method, prepares product；Wherein, solvent thermal temperature is 90oC~200oC, solvent thermal
Time is 8h ~ 80h.
Concrete steps include:
(1) respectively according to Ti:Li=1:(1 ~ 1.5) chemical element metering ratio weigh titanium salt and lithium salts；
(2), after titanium salt step 1 weighed and lithium salts mixing, add in solvent, be sufficiently stirred for, be allowed to mix homogeneously, obtain first
Mixture；
(3) the first mixture step 2 obtained is placed in high temperature water heating kettle, and reactor is placed on magnetic agitation in oil bath and adds
Heat, rotating speed 100-500rpm, 90oC~200oUnder C, heat 8h ~ 80h, obtain head product；
(4) head product step 3 obtained utilizes deionized water and hydrochloric acid to be centrifuged successively, washs, is dried, and obtains time product；
(5), during secondary product step 4 obtained puts into (0.1-1) M lithium hydroxide solution, ion exchange, magnetic agitation 10 are carried out
Minute, supersound process 1 hour；
(6) product that step 5 obtains is put into Muffle furnace, 500oC heat treatment 6 hours, obtains end-product.
Further, during described titanium salt is P25, tetraethyl titanate, butyl titanate, isopropyl titanate, titanous chloride.
Plant or multiple.
Further, one or more during described lithium salts is Lithium hydrate, lithium nitrate, lithium sulfate, lithium perchlorate.
Further, in described step 2, solvent is in water, ethanol, isopropanol, the tert-butyl alcohol, DMF
One or more.
Further, in described step 3, the first mixture step 2 obtained is placed in high temperature water heating kettle, uses water
Bath, oil bath, microwave or Ultrasonic Heating, 90oC~200oUnder C, heat 8h ~ 80h.
Further, in described step 6, vacuum drying or nitrogen protection atmosphere is used to be dried, drying time is 1 ~
15h, baking temperature is 400 oC ~700oC。
For foregoing problems, the present invention provides a kind of used as negative electrode of Li-ion battery lithium titanate nano-tube material and preparation side thereof
Method.In the present invention, the principle of lithium titanate nano-tube material height ratio capacity is: the one-dimensional nano-array structure of lithium titanate nanotube
Enhance electronic conductivity, improve the high rate charge-discharge performance of material, with give full play to its high rate charge-discharge performance and
Good cycle performance.
Detailed description of the invention
All features disclosed in this specification, or disclosed all methods or during step, except mutually exclusive
Feature and/or step beyond, all can combine by any way.
Any feature disclosed in this specification, unless specifically stated otherwise, all can by other equivalence or there is similar purpose
Alternative features is replaced.I.e., unless specifically stated otherwise, an example during each feature is a series of equivalence or similar characteristics
?.
Embodiment 1
Synthesize high-purity phase spinel type lithium titanate Li of about 0.4 g4Ti5O12Presoma P25, Lithium hydrate need to be weighed respectively,
Control its stoichiometric proportion Ti:Li=1:1.25.The presoma weighed is placed in hydrothermal reaction kettle, and in hydrothermal reaction kettle
Add 25 mL deionized waters, stir 30 min, make each component mix homogeneously, obtain the first mixture.Then hydrothermal reaction kettle is put
Magnetic agitation heating in oil bath, rotating speed 300rpm, 120oUnder C, heat 24h, obtain head product.For head product, profit successively
It is centrifuged with deionized water and hydrochloric acid, washs, is dried, obtain time product；Secondary product is put into 0.2 M lithium hydroxide solution again
In, carry out ion exchange, magnetic agitation 10 minutes, supersound process 1 hour；Finally put it in Muffle furnace, 500oC heat treatment
2 hours, obtain end-product.
The preparation method of lithium ion battery: by active substance lithium titanate nano-tube material, acetylene black conductor, binding agent
(PVDF) mix with the mass ratio of 80:10:10, instill appropriate N-Methyl pyrrolidone and make uniform black paste.Use scraper
It is coated in aluminum foil current collector uniformly, after 120 C vacuum drying 12h, obtains lithium titanate electrode plate.Hands in argon atmospher
In casing, lithium paper tinsel be negative pole, lithium titanate electrode be positive pole, polypropylene porous film be barrier film, the mixed solution of 1M LiPF6 be electricity
Solve liquid and be assembled into button cell.
Test result: lithium titanate nanotube base lithium ion battery cathode prepared by the present embodiment is at the high rate charge-discharge of 3C
Under, first discharge specific capacity reaches 107 mAh/g；After 100 circulate, capacity maintenance dose is still 70mAh/g；Coulombic efficiency
It is about 100%.
Change Li4Ti5O12Synthesis presoma composition, on the premise of other condition is constant, the lithium titanate nanotube obtained
Base lithium ion battery cathode performance is as shown in table 1 below.
Measurement result under the conditions of table 1 different material and mass ratio
As it can be seen from table 1 change titanium source and lithium source, Li can be directly affected4Ti5O12Specific capacity and coulombic efficiency.This be by
Different with ionic dissociation complexity in the dissolubility of different presomas, and then have impact on the reaction speed of presoma in hydro-thermal reaction
Rate.Meanwhile, suitable titanium lithium ratio, it is also ensured that form stable spinel structure product, utilizes its three-dimensional ion diffusion logical
Road, it is ensured that the specific discharge capacity of system.
Embodiment 2
According to the step described in embodiment 1, use P25 and Lithium hydrate as titanium source and lithium source, keep its chemical element to measure
Ratio is 1:1.25, changes solvent species, solvent thermal temperature and solvent thermal time respectively, on the premise of other condition is constant,
The lithium titanate nanotube base lithium ion battery cathode performance arrived is as shown in table 2 below.
Table 2 different solvents, pH value, solvent thermal temperature and the measurement result under the solvent thermal time
Embodiment 3
According to the step described in embodiment 1 and component, change the dry atmosphere of hydrothermal product, temperature and time respectively, at other
On the premise of condition is constant, testing the lithium titanate nanotube base lithium ion battery cathode performance obtained, test result is such as
Shown in table 3 below.
Measurement result under the conditions of table 3 difference is dry
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, and any
Those familiar with the art in the technical scope that the invention discloses, the change that can readily occur in or replacement, all answer
Contain within protection scope of the present invention.The present invention expands to any new feature disclosed in this manual or any new
Combination, and the arbitrary new method that discloses or the step of process or any new combination.
Claims (7)
1. a used as negative electrode of Li-ion battery lithium titanate nano-tube material, it is characterised in that: described lithium titanate nanotube former
Material is titanium salt: lithium salts Ti: Li=1: 1 ~ 1.5, its molecular formula is Li4Ti5O12, the caliber of this lithium titanate nanotube is 1-20nm, long
Degree is 50-50nm.
2. a preparation method for used as negative electrode of Li-ion battery lithium titanate nano-tube material as claimed in claim 1, its feature
Comprise the steps: in described method
(1) respectively according to Ti:Li=1:(1 ~ 1.5) chemical element metering ratio weigh titanium salt and lithium salts；
(2), after titanium salt step 1 weighed and lithium salts mixing, add in solvent, be sufficiently stirred for, be allowed to mix homogeneously, obtain first
Mixture；
(3) the first mixture step 2 obtained is placed in high temperature water heating kettle, and reactor is placed on magnetic agitation in oil bath and adds
Heat, rotating speed 100-500rpm, 90oC~200oUnder C, heat 8h ~ 80h, obtain head product；
(4) head product step 3 obtained utilizes deionized water and hydrochloric acid to be centrifuged successively, washs, is dried, and obtains time product；
(5), during secondary product step 4 obtained puts into (0.1-1) M lithium hydroxide solution, ion exchange, magnetic agitation 10 are carried out
Minute, supersound process 1 hour；
(6) product that step 5 obtains is put into Muffle furnace, 500oC heat treatment 6 hours, obtains end-product lithium ion battery negative
Use lithium titanate nano-tube material.
The preparation method of used as negative electrode of Li-ion battery lithium titanate nano-tube material the most according to claim 2, its feature exists
In, described titanium salt is one or more in P25, tetraethyl titanate, butyl titanate, isopropyl titanate, titanous chloride..
The preparation method of used as negative electrode of Li-ion battery lithium titanate nanotube the most according to claim 2, it is characterised in that institute
Stating lithium salts is one or more in Lithium hydrate, lithium nitrate, lithium sulfate, lithium perchlorate.
The preparation method of used as negative electrode of Li-ion battery lithium titanate nano-tube material the most according to claim 2, its feature exists
In, in described step 2, solvent is one or more in water, ethanol, isopropanol, the tert-butyl alcohol, DMF.
The preparation method of used as negative electrode of Li-ion battery lithium titanate nano-tube material the most according to claim 2, its feature exists
In, in described step 3, the first mixture step 2 obtained is placed in high temperature water heating kettle, uses water-bath, oil bath, microwave or super
Acoustic heating, 90oC~200oUnder C, heat 8h ~ 80h；In described step 3, the first mixture step 2 obtained is placed in high-temperature water
In hot still, use water-bath, oil bath, microwave or Ultrasonic Heating, 90oC~200oUnder C, heat 8h ~ 80h.
The preparation method of used as negative electrode of Li-ion battery lithium titanate nano-tube material the most according to claim 2, its feature exists
In, in described step 6, use vacuum drying or nitrogen protection atmosphere to be dried, drying time is 1 ~ 15h, and baking temperature is 400 oC ~700oC。
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