CN106356511A - Preparation method of high-performance nitrogen-doped carbon-coated titanium niobate material and application thereof in lithium ion battery - Google Patents
Preparation method of high-performance nitrogen-doped carbon-coated titanium niobate material and application thereof in lithium ion battery Download PDFInfo
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- CN106356511A CN106356511A CN201610924928.8A CN201610924928A CN106356511A CN 106356511 A CN106356511 A CN 106356511A CN 201610924928 A CN201610924928 A CN 201610924928A CN 106356511 A CN106356511 A CN 106356511A
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- titanium niobate
- niobate material
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- nitrating
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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
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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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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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 invention discloses a preparation method of a high-performance nitrogen-doped carbon-coated titanium niobate material and an application thereof in a lithium ion battery. The preparation method of a titanium niobate material comprises the following steps: (I) dissolving a nitrogen-containing organic matter in a solvent to prepare a nitrogen-containing organic matter solution, adding a titanium niobate material, and performing sufficient stirring and ultrasonic dispersion; (II) preparing a composite precursor of the titanium niobate material and the nitrogen-containing organic matter from the suspension dispersed in the step (I) by a heating-stirring solvent evaporation method or a solvothermal method; and (III) performing heat treatment of the composite precursor obtained in the step (II), and pyrolyzing the organic matter to obtain a titanium niobate material with relatively good conductivity. In the invention, the conductivity of the titanium niobate material is improved through the pyrolysis of the nitrogen-containing organic matter on the particle surface of the titanium niobate material, then the electrochemical performance of titanium niobate is further improved, and the application of titanium niobate in a lithium ion secondary battery is promoted.
Description
Technical field
The invention belongs to energy storage material technical field, it is related to one kind by improving titanium niobate material conductivity and improves material
The method of performance and based on the application in lithium rechargeable battery as negative electrode active material of the material after this improvement.
Background technology
Electric motor car gradually rise and 3c market rapid expansion the material of lithium ion battery is proposed high-energy and
High-power demand, traditional material with carbon element with gradually study the silicon class of maturation, all there are some insoluble problems in stannum class material,
Lithium titanate material has excellent high rate performance and stable charging/discharging voltage platform, but the low theory specific volume of its 175 mah/g
Amount limits it as the material of electrokinetic cell.So needing a kind of high-energy of searching and high-power negative material badly to meet power
The needs of battery.
tinb2o7There are 5 electron transfer electricity to (ti in material4+/ti3+, nb5+/nb3+), there are 387.6 mah/g
Theoretical specific capacity, li+Intercalation electrode potential in 1.64 v, close to li4ti5o12The intercalation potential of material, it can be avoided that
The formation of sei film, improves coulombic efficiency, and higher electrode potential avoids the deposition of lithium metal, improves the peace of battery
Quan Xing.tinb2o7Material 1.0 v ~ 2.5 v(with respect to lithium metal electrode potential) carry out discharge and recharge, actual reversible capacity
280 mah/g can be reached, exceeded well over li4ti5o12Theoretical specific capacity.tinb2o7Outstanding chemical property obtains
The affirmative of well-known scholar both at home and abroad, but still suffer from some technical problems and have to be solved, such as its electric conductivity is poor etc..Therefore, grind
Study carefully and how to improve tinb2o7The electric conductivity of material, thus improving the performance of material further, answers for expanding titanium niobate material
Significant with scope.
Content of the invention
It is an object of the invention to provide a kind of preparation method of titanium niobate material of high-performance nitrating bag carbon and its lithium from
Application in sub- battery, improves the conduction of titanium niobate material by the pyrolysis on titanium niobate material granule surface for the itrogenous organic substance
Property, thus lifting the chemical property of titanium niobate further, and then advance its application in lithium rechargeable battery.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of the titanium niobate material of high-performance nitrating bag carbon, comprises the steps:
First, itrogenous organic substance is dissolved in solvent, prepares itrogenous organic substance solution, titanium niobate material is put into wherein and is filled
Divide stirring and ultrasonic disperse, the mol ratio controlling c, n, ti is 1 ~ 5:1 ~ 3:0.1 ~ 10；
2nd, suspension scattered for step one is prepared titanium niobate material by heated and stirred evaporation solvent method or solvent-thermal method
Composite precursor with itrogenous organic substance；
3rd, the composite precursor that step 2 obtains is carried out heat treatment, after pyrolysis Organic substance, obtain the preferable titanium niobate of electric conductivity
Material.
The titanium niobate material that said method prepares can be applied in lithium ion battery as negative material, described lithium
Ion battery is made up of positive plate, negative plate, barrier film, electrolyte, aluminium shell or aluminum plastic film, and negative plate comprises Copper Foil and bears
Pole slurry, cathode size therein according to 70 ~ 95% titanium niobate material, 2 ~ 10% conductive agent and 3 ~ 20% binding agent matter
Amount percentage ratio composition.
In the present invention, the preparation method of described titanium niobate material does not limit, and can be high temperature solid-state method, solvent-thermal method, colloidal sol
Gel method, spray drying method or method of electrostatic spinning.
In the present invention, the concentration of described itrogenous organic substance solution is 0.1mol/l ~ 5mol/l.
In the present invention, described itrogenous organic substance is cyanamide, carbamide, dicyanodiamine, tripolycyanamide, tetramethyl guanidine, n- methylene
The mixture of one or more of aminoacetonitriles, imido urea.
In the present invention, described solvent is one of water, ethanol, acetonitrile, acetone, dimethylformamide or several mixing
Compound.
In the present invention, the temperature of described heated and stirred evaporation solvent method is 40 ~ 90 DEG C.
In the present invention, the temperature of described solvent-thermal method is 120 ~ 220 DEG C, and the time is 5 ~ 20h.
In the present invention, described heat treatment Muffle furnace, batch-type furnace or tube furnace, heat treatment temperature is 500 ~ 900 DEG C,
Time is 1 ~ 10h, and protective atmosphere is nitrogen or argon.
In the present invention, described conductive agent is one of acetylene black, Ketjen black, CNT, Graphene or super-p
Or wherein several mixture.
The titanium niobate material that the titanium niobate material conductivity that present invention process obtains relatively directly obtains has larger lifting, and
There is excellent circulation and high rate charge-discharge performance, expand the range of titanium niobate material.
Brief description
Fig. 1 is the xrd collection of illustrative plates of the titanium niobate material that embodiment 1 obtains；
Fig. 2 is the scanning electron microscope (SEM) photograph of the titanium niobate material that embodiment 1 obtains；
Fig. 3 is long circulating performance under the multiplying power of 10c for the titanium niobate material that obtains of embodiment 1;
Fig. 4 is the impedance contrast figure of the titanium niobate material that untreated titanium niobate material is obtained with embodiment 1.
Specific embodiment
Below in conjunction with the accompanying drawings technical scheme is further described, but is not limited thereto, every to this
Inventive technique scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should cover
In protection scope of the present invention.
Embodiment 1:
The dicyanodiamine taking 2g is dissolved in the ethanol of 50ml, adds the niobic acid titanium of the high temperature solid-state method preparation of 2g after fully dissolving
Material, stirring ultrasonic 2h, after titanium niobate material is fully dispersed in the solution, in oil bath pan, ethanol therein is evaporated in stirring, and
By the slurry obtaining in air dry oven 50 DEG C fully be dried after obtain composite precursor.Finally presoma is placed in tube furnace
In, 700 DEG C of heat treatment 3h in nitrogen shielding gas, obtain titanium niobate material.
The titanium niobate material that the present embodiment obtains can be applied in the fastening lithium ionic cell of assembling as negative material, its
In cathode size according to 80% titanium niobate material, 5% conductive agent and 15% binding agent mass percent composition.
As shown in Figure 1, the material after process is not changed in compared to the material structure of before processing, is all belonging to monocline knot
Structure.
As shown in Figure 2, the titanium niobate material granule diameter that the present embodiment obtains is in 1 microns.
As seen from Figure 3, after circulating 1000 times, the titanium niobate material that the present embodiment obtains remains to keep 110mah/g left
Right reversible capacity.
As seen from Figure 4, after being processed by itrogenous organic substance, the impedance of material has obvious reduction, and illustrative material is led
Electrical lifting.
Embodiment 2:
The tripolycyanamide taking 2g is dissolved in the ethanol of 40ml, adds the niobic acid titanium of the high temperature solid-state method preparation of 2g after fully dissolving
Material, stirring ultrasonic 2h, after titanium niobate material is fully dispersed in the solution, this suspension are transferred to the polytetrafluoroethyl-ne of 50ml
In alkene reaction kettle, then 180 DEG C of reaction 5h in homogeneous reactor, before being combined after reacted precipitate filtration drying
Drive body.Finally presoma is placed in tube furnace, 700 DEG C of heat treatment 3h in argon shielding gas, obtains titanium niobate material.
Embodiment 3:
The present embodiment is with the difference of embodiment 2: the Organic substance in step one is replaced by cyanamide, carbamide or dicyan two
Amine.
Embodiment 4:
The tripolycyanamide taking 2g is dissolved in the water of 40ml and the mixed solution (volume ratio 1:1) of dimethylformamide, fully dissolves
Add titanium niobate material, stirring the ultrasonic 2h of the high temperature solid-state method preparation of 2g afterwards, treat that titanium niobate material fully divides in the solution
After dissipating, this suspension is transferred in the ptfe autoclave of 50ml, then 150 DEG C of reaction 5h in homogeneous reactor, will
Composite precursor is obtained after reacted precipitate filtration drying.Finally presoma is placed in tube furnace, in nitrogen shielding gas
In 700 DEG C of heat treatment 3h, obtain titanium niobate material.
Embodiment 5:
The present embodiment is with the difference of embodiment 4: the Organic substance in step one is replaced by the mixed of cyanamide and dicyanodiamine
Compound, the two mol ratio is 1:1.
Claims (10)
1. a kind of preparation method of the titanium niobate material of high-performance nitrating bag carbon it is characterised in that described preparation method step such as
Under:
First, itrogenous organic substance is dissolved in solvent, prepares itrogenous organic substance solution, titanium niobate material is put into wherein and is filled
Divide stirring and ultrasonic disperse, the mol ratio controlling c, n, ti is 1 ~ 5:1 ~ 3:0.1 ~ 10；
2nd, suspension scattered for step one is prepared titanium niobate material by heated and stirred evaporation solvent method or solvent-thermal method
Composite precursor with itrogenous organic substance；
3rd, the composite precursor that step 2 obtains is carried out heat treatment, after pyrolysis Organic substance, obtain the preferable titanium niobate of electric conductivity
Material.
2. the preparation method of the titanium niobate material of high-performance nitrating bag carbon according to claim 1 is it is characterised in that described
The concentration of itrogenous organic substance solution is 0.1mol/l ~ 5mol/l.
3. the preparation method of the titanium niobate material of high-performance nitrating bag carbon according to claim 1 and 2 is it is characterised in that institute
State itrogenous organic substance be cyanamide, carbamide, dicyanodiamine, tripolycyanamide, tetramethyl guanidine, n- methylene aminoacetonitriles, in imido urea
The mixture of one or more.
4. the preparation method of the titanium niobate material of high-performance nitrating bag carbon according to claim 1 is it is characterised in that described
Solvent is one of water, ethanol, acetonitrile, acetone, dimethylformamide or several mixture.
5. the preparation method of the titanium niobate material of high-performance nitrating bag carbon according to claim 1 is it is characterised in that described
The temperature of heated and stirred evaporation solvent method is 40 ~ 90 DEG C.
6. the preparation method of the titanium niobate material of high-performance nitrating bag carbon according to claim 1 is it is characterised in that described
The temperature of solvent-thermal method is 120 ~ 220 DEG C, and the time is 5 ~ 20h.
7. the preparation method of the titanium niobate material of high-performance nitrating bag carbon according to claim 1 is it is characterised in that described
Heat treatment temperature is 500 ~ 900 DEG C, and the time is 1 ~ 10h, and protective atmosphere is nitrogen or argon.
8. the titanium niobate material of the high-performance nitrating bag carbon that claim 1-7 any claim prepares can be used as negative pole material
Material is applied in lithium ion battery.
9. the titanium niobate material of high-performance nitrating bag carbon according to claim 8 can be applied in lithium ion as negative material
In battery, described lithium ion battery is made up of positive plate, negative plate, barrier film, electrolyte, aluminium shell or aluminum plastic film, negative pole
Piece comprise Copper Foil and cathode size it is characterised in that described cathode size according to 70 ~ 95% titanium niobate material, 2 ~ 10% conduction
Agent and 3 ~ 20% binding agent mass percent composition.
10. the titanium niobate material of high-performance nitrating bag carbon according to claim 9 can as negative material apply lithium from
It is characterised in that described conductive agent is in acetylene black, Ketjen black, CNT, Graphene or super-p in sub- battery
Plant or wherein several mixture.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610924928.8A CN106356511A (en) | 2016-10-24 | 2016-10-24 | Preparation method of high-performance nitrogen-doped carbon-coated titanium niobate material and application thereof in lithium ion battery |
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| CN201610924928.8A CN106356511A (en) | 2016-10-24 | 2016-10-24 | Preparation method of high-performance nitrogen-doped carbon-coated titanium niobate material and application thereof in lithium ion battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110224111A (en) * | 2019-05-30 | 2019-09-10 | 浙江锋锂新能源科技有限公司 | Titanium niobate material of titanium nitride cladding and preparation method thereof and cathode, battery |
| CN110911666A (en) * | 2019-11-27 | 2020-03-24 | 合肥学院 | Method for synthesizing nitrogen-containing carbon-coated titanium niobate material for negative electrode of lithium battery |
| CN110911679A (en) * | 2019-10-31 | 2020-03-24 | 浙江锋锂新能源科技有限公司 | Modified TiNb2O7Material, modified TiNb2O7Electrode and preparation method |
| CN112551583A (en) * | 2020-12-10 | 2021-03-26 | 哈尔滨工业大学 | Preparation method and application of carbon-coated oxygen-less titanium niobate negative electrode material |
| CN114180571A (en) * | 2020-09-14 | 2022-03-15 | 华中科技大学 | Nitrogen-doped carbon-based lithium storage material and preparation method and application thereof |
| CN114300671A (en) * | 2021-12-28 | 2022-04-08 | 蜂巢能源科技股份有限公司 | Graphite composite negative electrode material and preparation method and application thereof |
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| CN103337631A (en) * | 2013-07-04 | 2013-10-02 | 哈尔滨工程大学 | Carbon-nitrogen co-coating method for improving high rate discharge performance of lithium titanate and inhibiting gas generation |
| CN105470477A (en) * | 2015-11-12 | 2016-04-06 | 南阳师范学院 | Preparation method of high-performance nitrogen-doped and carbon-coated Ti<2>Nb<10>O<29> composite electrode material |
| CN105529465A (en) * | 2016-02-26 | 2016-04-27 | 南阳师范学院 | Nitrogen-doped carbon-coated titanium niobate composite electrode material and preparation method thereof |
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| CN102479950A (en) * | 2010-11-23 | 2012-05-30 | 中国科学院物理研究所 | Titanium niobate composite material, preparation method thereof, and cathode and battery containing the same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110224111A (en) * | 2019-05-30 | 2019-09-10 | 浙江锋锂新能源科技有限公司 | Titanium niobate material of titanium nitride cladding and preparation method thereof and cathode, battery |
| CN110911679A (en) * | 2019-10-31 | 2020-03-24 | 浙江锋锂新能源科技有限公司 | Modified TiNb2O7Material, modified TiNb2O7Electrode and preparation method |
| CN110911666A (en) * | 2019-11-27 | 2020-03-24 | 合肥学院 | Method for synthesizing nitrogen-containing carbon-coated titanium niobate material for negative electrode of lithium battery |
| CN114180571A (en) * | 2020-09-14 | 2022-03-15 | 华中科技大学 | Nitrogen-doped carbon-based lithium storage material and preparation method and application thereof |
| CN114180571B (en) * | 2020-09-14 | 2023-06-16 | 华中科技大学 | Nitrogen-doped carbon-based lithium storage material and preparation method and application thereof |
| CN112551583A (en) * | 2020-12-10 | 2021-03-26 | 哈尔滨工业大学 | Preparation method and application of carbon-coated oxygen-less titanium niobate negative electrode material |
| CN114300671A (en) * | 2021-12-28 | 2022-04-08 | 蜂巢能源科技股份有限公司 | Graphite composite negative electrode material and preparation method and application thereof |
| CN114300671B (en) * | 2021-12-28 | 2024-04-12 | 蜂巢能源科技股份有限公司 | Graphite composite negative electrode material and preparation method and application thereof |
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