CN109659497A - A kind of preparation method of the flexible metatitanic acid lithium electrode based on carbon cloth - Google Patents
A kind of preparation method of the flexible metatitanic acid lithium electrode based on carbon cloth Download PDFInfo
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- CN109659497A CN109659497A CN201910094292.2A CN201910094292A CN109659497A CN 109659497 A CN109659497 A CN 109659497A CN 201910094292 A CN201910094292 A CN 201910094292A CN 109659497 A CN109659497 A CN 109659497A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/13—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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- 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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- 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
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
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Abstract
The preparation method of the invention discloses a kind of flexible metatitanic acid lithium electrode based on carbon cloth, the lithium titanate, pattern are nanometer rods matrix structure, and self-assembled growth is on conductive carbon cloth, any binder and conductive carbon black can not be used, flexible lithium ion battery electrode is directly used as.Lithium titanate nanometer rods matrix structure of the present invention, it can be transmitted for the ion in charge and discharge and channel is provided, realize the good high magnification of flexible metatitanic acid lithium electrode, long circulating performance, and still there is excellent chemical property in the state of bending, folding with the flexible lithium ion battery of this flexible metatitanic acid lithium electrode assembling.
Description
Technical field
The present invention relates to field of new-generation energy storage, more particularly to the preparation side of the flexible metatitanic acid lithium electrode based on carbon cloth
Method.
Technical background
With the fast development of electronic technology, more and more electronic equipments are towards lightening and flexibility direction
Developed, such as Samsung and LG are proposed the screen of oneself flexible foldable, and are planning to release folding
The products such as mobile phone.Display component and circuit can all be realized flexible and foldable at present, but maximum challenge is exactly that can fold
Energy storage product.The products such as traditional lithium ion battery, supercapacitor, not only volume is heavy, but also can not fold,
It when volume change is excessive, results even in and short circuit occurs between positive and negative anodes, cause thermal runaway, lead to serious safety problem.Cause
This development in order to adapt to next-generation flexible electronic devices, the developing direction of lithium ion battery also should be towards flexible, folding
Direction is developed.However, from the point of view of current research and development, long-life and powerful flexible lithium ion battery are counted on one's fingers can
Number, seriously hinders the development of flexible lithium ion battery.Therefore, the long-life is developed, high magnification flexible lithium ion battery is compeled in eyebrow
Eyelash.
In the method for production flexible electrode, active material is grown on conductive substrates, such as conductive carbon cloth, is current compare
One of effective method.Carbon cloth is mainly woven by carbon fiber, can provide the structural support to material and effective electronics
Delivering path.It is still one of the problem of currently encountering however, finding high performance lithium ion battery electrode material.
Lithium titanate (Li4Ti5O12) there is defect spinel structure, intercalation potential is 1.55V (vs.Li+/ Li), it is not easy to shape
At SEI film, there is preferable high rate capability.In charge and discharge process, unit cell volume is varied less, referred to as " zero strain material
Material ", therefore lithium titanate has good cyclical stability.But the conductivity of lithium titanate material is very low, limits it applied to lithium
Ion battery electrode materials.
Summary of the invention
The problem of for currently available technology, the present invention provides a kind of flexible metatitanic acid lithium electrode based on carbon cloth
Preparation method, the specific technical proposal is:
On the one hand one, the present invention provides a kind of flexible metatitanic acid lithium electrode based on carbon cloth, the electrode be lithium titanate from
Assembling is grown on carbon cloth and forms.
The lithium titanate is nanometer rods self assembly matrix structure, and the nanorod diameter is about 10-20nm, and nanometer rods it
Between have the gap.
The carbon cloth is worked out by carbon fiber, and carbon fiber surface is smooth, and the carbon fiber diameter is 2.5 to 6 μm.
On the other hand, the present invention provides the preparation methods of the flexible lithium titanate electricity, comprising the following steps:
A certain amount of titanium source is added drop-wise in the mixed liquor of 15mL distilled water and 13mL concentrated hydrochloric acid and obtains titanium source solution, by titanium
Source solution is transferred in reaction kettle, and carbon cloth is added by hydrothermal synthesis and obtains being grown on the titanium dioxide nano thread on carbon cloth；
After obtained titanium dioxide nano thread is used ethyl alcohol and distilled water supersound washing 5min respectively, by being dried in vacuo
To solid titanium dioxide nano wire, the methanol solution of lithium hydroxide is instilled, vacuum drying is placed in tube furnace, at 800 DEG C,
It is calcined in an inert gas atmosphere, obtains the flexible metatitanic acid lithium electrode based on carbon cloth.
The titanium source is one or more of tetrabutyl titanate and isopropyl titanate, as one of technology of the invention
Scheme, the titanium source are the tetrabutyl titanate of 3~0.5g；As one of technical solution of the invention, the isopropanol
The isopropyl titanate of 0.25~0.45g of titanium.
The experiment condition of the hydro-thermal method is 180 DEG C of temperature, and the time is for 24 hours.
The methanol solution of the lithium hydroxide the preparation method comprises the following steps: by lithium hydroxide dissolution in methyl alcohol, the methanol
Volume is 1mL；The molar ratio of lithium ion and the titanium ion in titanium source is 0.75-0.85 in the lithium hydroxide.
The inert atmosphere is one of nitrogen, argon gas and helium.
In another aspect, the present invention provides the purposes of the flexible metatitanic acid lithium electrode based on carbon cloth, including will be based on carbon cloth
Flexible metatitanic acid lithium electrode is as cathode, the nickel ion doped (LiNi coated on Al foil0.5Mn1.5O4) as anode, Celgard
2600 are used as diaphragm, use hexafluoro phosphorus lithium (LiPF6) as the flexible full battery of electrolyte composition.
Unaccounted content can be realized all in accordance with industry routine operation in preparation method of the present invention.
The invention has the benefit that
(1) the flexible metatitanic acid lithium electrode being prepared does not need to add any binder and conductive carbon black, directly available
Do lithium ion cell electrode.
(2) lithium titanate is that nanometer rods matrix structure enhances the electric conductivity of lithium titanate, and wherein the slit between nanometer rods is not
The specific surface area of material can only be increased, increase the contact area of lithium ion and lithium titanate material, and shorten lithium ion
Delivering path enhances its high rate capability.
(3) lithium titanate is to be sintered in inert atmosphere, generates micro Li3+Ion is conducive to the electric conductivity for improving lithium titanate.
(4) this flexible metatitanic acid lithium electrode based on carbon cloth is as cathode, the nickel ion doped coated on Al foil
(LiNi0.5Mn1.5O4) as anode, Celgard 2600 is used as diaphragm, uses hexafluoro phosphorus lithium (LiPF6) formed as electrolyte
Flexible full battery, under bending, folded state, under the charge-discharge magnification of 1C, specific discharge capacity still with higher.
Detailed description of the invention
Fig. 1 is the field emission scanning electron microscope figure of flexible metatitanic acid lithium electrode prepared by embodiment 1.
Fig. 2 is the high-resolution-ration transmission electric-lens figure of flexible metatitanic acid lithium electrode prepared by embodiment 1.
Fig. 3 is the flexible full battery that assembles as cathode of flexible metatitanic acid lithium electrode prepared by embodiment 1 in different bending angles
Charging and discharging curve under degree.
Fig. 4 is the flexible full battery that assembles as cathode of flexible metatitanic acid lithium electrode prepared by embodiment 2 in different bending angles
Charging and discharging curve under degree.
Fig. 5 is the flexible full battery that assembles as cathode of flexible metatitanic acid lithium electrode prepared by embodiment 3 in different bending angles
Charging and discharging curve under degree.
Specific embodiment
Embodiment 1
The tetrabutyl titanate of 0.4g is added drop-wise in the mixed liquor of 15mL distilled water and 13mL concentrated hydrochloric acid, is transferred to reaction kettle
In, carbon cloth is added, hydro-thermal 24 hours at 180 DEG C synthesize the titanium dioxide nano thread being grown on carbon cloth, then use second respectively
Pure and mild distilled water supersound washing 5 minutes, instills methanol (1mL) solution of lithium hydroxide (0.023g) after vacuum drying, vacuum is dry
It is dry to be placed in tube furnace, it at 800 DEG C, is calcined in argon atmosphere, obtains the flexible metatitanic acid lithium electrode based on carbon cloth.
The flexible metatitanic acid lithium electrode prepared in embodiment 1 is characterized.It is right by field emission scanning electron microscope (FE-SEM)
The pattern of material is characterized, and the lithium titanate material as can be seen from Figure 1 prepared is grown on carbon cloth, and has nanometer rods square
Battle array structure.The pattern of material is characterized by high-resolution-ration transmission electric-lens (HR-TEM), system can be further verified from Fig. 2
Standby lithium titanate material has nanometer rods matrix structure, and with the presence of slit between nanometer rods, the diameter of the nanometer rods is 10-
20nm。
Using the flexible metatitanic acid lithium electrode prepared in embodiment 1 as cathode, the nickel ion doped coated on Al foil
(LiNi0.5Mn1.5O4) as anode, Celgard 2600 is used as diaphragm, uses hexafluoro phosphorus lithium (LiPF6) it is used as electrolyte, appearance
It is packaged by dimethyl silicone polymer (PDMS), obtains flexible lithium titanate full battery.The wherein capacity ratio of cathode and anode
For 0.8:1.Electrochemical property test is carried out in the voltage range of 2-3.45V.By carrying out folding different angles to device
(0 °, 90 °, 180 °) carries out charge-discharge performance test to device, it is as shown in Figure 3 to obtain result, it can be seen that prepared by the present invention
The flexible lithium ion battery device of flexible metatitanic acid lithium electrode production is after folding still with the specific discharge capacity of 127.5mAh/g
(under 1C multiplying power).
Embodiment 2
The tetrabutyl titanate of 0.3g is added drop-wise in the mixed liquor of 15mL distilled water and 13mL concentrated hydrochloric acid, is transferred to reaction kettle
In, carbon cloth is added, hydro-thermal 24 hours at 180 DEG C synthesize the titanium dioxide nano thread being grown on carbon cloth, then use second respectively
Pure and mild distilled water supersound washing 5 minutes, instills methanol (1mL) solution of lithium hydroxide (0.017g) after vacuum drying, vacuum is dry
It is dry to be placed in tube furnace, it at 800 DEG C, is calcined in argon atmosphere, obtains the flexible metatitanic acid lithium electrode based on carbon cloth.
Using the flexible metatitanic acid lithium electrode prepared in embodiment 2 as cathode, the nickel ion doped coated on Al foil
(LiNi0.5Mn1.5O4) as anode, Celgard 2600 is used as diaphragm, uses hexafluoro phosphorus lithium (LiPF6) it is used as electrolyte, appearance
It is packaged by dimethyl silicone polymer (PDMS), obtains flexible lithium titanate full battery.The wherein capacity ratio of cathode and anode
For 0.8:1.Electrochemical property test is carried out in the voltage range of 2-3.45V.By carrying out folding different angles to device
(0 °, 90 °, 180 °) carries out charge-discharge performance test to device, it is as shown in Figure 4 to obtain result, it can be seen that prepared by the present invention
The flexible lithium ion battery device of flexible metatitanic acid lithium electrode production is after folding still with the specific discharge capacity of 123.5mAh/g
(under 1C multiplying power).
Embodiment 3
The isopropyl titanate of 0.25g is added drop-wise in the mixed liquor of 15mL distilled water and 13mL concentrated hydrochloric acid, is transferred in reaction kettle,
Carbon cloth is added, hydro-thermal 24 hours at 180 DEG C synthesize the titanium dioxide nano thread being grown on carbon cloth, then use ethyl alcohol respectively
With distilled water supersound washing 5 minutes, methanol (1mL) solution of instillation lithium hydroxide (0.018g) after vacuum drying, vacuum drying
It is placed in tube furnace, at 900 DEG C, is calcined in argon atmosphere, obtain the flexible metatitanic acid lithium electrode based on carbon cloth.
Using the flexible metatitanic acid lithium electrode prepared in embodiment 3 as cathode, the nickel ion doped coated on Al foil
(LiNi0.5Mn1.5O4) as anode, Celgard 2600 is used as diaphragm, uses hexafluoro phosphorus lithium (LiPF6) it is used as electrolyte, appearance
It is packaged by dimethyl silicone polymer (PDMS), obtains flexible lithium titanate full battery.The wherein capacity ratio of cathode and anode
For 0.8:1.Electrochemical property test is carried out in the voltage range of 2-3.45V.By carrying out folding different angles to device
(0 °, 90 °, 180 °) carries out charge-discharge performance test to device, it is as shown in Figure 5 to obtain result, it can be seen that prepared by the present invention
The flexible lithium ion battery device of flexible metatitanic acid lithium electrode production is after folding still with the specific discharge capacity of 119.5mAh/g
(under 1C multiplying power).
Claims (9)
1. a kind of flexible metatitanic acid lithium electrode based on carbon cloth, it is characterised in that: the electrode is lithium titanate self-assembled growth in carbon
Cloth；The lithium carbonate is nanometer rods self assembly matrix structure, and the nanorod diameter is 10-20nm, is had between the nanometer rods
Gap.
2. the flexible metatitanic acid lithium electrode based on carbon cloth as described in claim 1, it is characterised in that: the carbon cloth is compiled by carbon fiber
It makes, carbon fiber surface is smooth, and carbon fiber diameter is 2.5-6 μm.
3. the preparation method of the flexible metatitanic acid lithium electrode based on carbon cloth as described in claim 1, it is characterised in that: including following
Step: a certain amount of titanium source is added drop-wise in the mixed liquor of 15mL distilled water and 13mL concentrated hydrochloric acid and obtains titanium source solution, by titanium source
Solution is transferred in reaction kettle, and carbon cloth is added by hydrothermal synthesis and obtains being grown on the titanium dioxide nano thread on carbon cloth；
Obtained titanium dioxide nano thread is used into ethyl alcohol and distilled water supersound washing after five minutes respectively, is obtained by vacuum drying
Solid titanium dioxide nano wire instills the methanol solution of lithium hydroxide, and vacuum drying is placed in tube furnace, at 800 DEG C,
It is calcined in inert gas atmosphere, obtains the flexible metatitanic acid lithium electrode based on carbon cloth.
4. the preparation method of the flexible metatitanic acid lithium electrode based on carbon cloth as claimed in claim 3, it is characterised in that: the titanium source
For one or more of tetrabutyl titanate and isopropyl titanate.
5. the preparation method of the flexible metatitanic acid lithium electrode based on carbon cloth as claimed in claim 3, it is characterised in that: the hydro-thermal method
Condition be 180 DEG C of temperature, the time is for 24 hours.
6. the preparation method of the flexible metatitanic acid lithium electrode based on carbon cloth as claimed in claim 3, it is characterised in that: the hydrogen-oxygen
In the methanol solution for changing lithium: the molar ratio of lithium ion and the titanium ion in titanium source is 0.75-0.85 in the lithium hydroxide.
7. the preparation method of the flexible metatitanic acid lithium electrode based on carbon cloth as claimed in claim 3, it is characterised in that: the inertia
Atmosphere is one of nitrogen, argon gas and helium.
8. the purposes of the flexible metatitanic acid lithium electrode based on carbon cloth as claimed in claim 1 or 2, it is characterised in that: described to be based on
The flexible metatitanic acid lithium electrode of carbon cloth is used for the cathode of lithium ion battery.
9. the purposes of the flexible metatitanic acid lithium electrode based on carbon cloth as claimed in claim 8, it is characterised in that: including by the base
In carbon cloth flexible metatitanic acid lithium electrode as cathode coated on Al foil nickel ion doped as anode, Celgard 2600 as every
Film uses hexafluoro phosphorus lithium to form flexible full battery as electrolyte.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110396598A (en) * | 2019-07-22 | 2019-11-01 | 广东环境保护工程职业学院 | A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles |
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| JP2018160432A (en) * | 2017-03-24 | 2018-10-11 | 太平洋セメント株式会社 | Negative electrode active material composite for lithium ion secondary battery and method of manufacturing the same |
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| CN110396598A (en) * | 2019-07-22 | 2019-11-01 | 广东环境保护工程职业学院 | A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles |
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