CN107331839A - A kind of preparation method of carbon nanotube loaded nano titanium oxide - Google Patents
A kind of preparation method of carbon nanotube loaded nano titanium oxide Download PDFInfo
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- CN107331839A CN107331839A CN201710505827.1A CN201710505827A CN107331839A CN 107331839 A CN107331839 A CN 107331839A CN 201710505827 A CN201710505827 A CN 201710505827A CN 107331839 A CN107331839 A CN 107331839A
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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
- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 relates to a kind of preparation method of carbon nanotube loaded nano titanium oxide.This method is immersed in 20 ~ 200 milligrams of CNTs in 50 ~ 200 milliliters of concentrated nitric acid solutions is handled first；Then CNT is scattered in the mixed solution of deionized water, surfactant and absolute ethyl alcohol simultaneously ultrasonic vibration 3 ~ 24 hours；Then it is 1 by volume ratio under low-temperature condition:10 ~ 100 titanium-containing compound and the mixed solution of ethanol are added drop-wise in above-mentioned mixed liquor dropwise, and are persistently stirred 12 ~ 36 hours at low temperature, obtain precursor solution.It is placed in air dry oven and is dried after high speed centrifugation, obtains precursor powder.It is last that precursor powder is calcined in air or oxygen atmosphere, obtain titanium dioxide composite Nano carbon pipe negative material powder.Titanium dioxide composite Nano carbon pipe negative material prepared by the present invention has high-specific surface area and mechanical strength, and even particle size distribution, excellent electrochemical performance is adapted to industrialized production.
Description
Technical field：
The present invention relates to a kind of preparation method of carbon nanotube loaded nano titanium oxide, belong to lithium ion battery material and prepare skill
Art field.
Technical background
Lithium ion battery is a kind of superior battery system, with operating voltage is high, energy density is high, pollution-free and circulates
The advantages of performance is good, is widely used in the mobile electronic terminal device necks such as portable digital equipment, electric tool and arms equipment
Domain, also has vast potential for future development in terms of electric car, it is considered to be 21 century has weight to national economy and people's lives
Want the new high-tech product of meaning.
In recent years, titanium dioxide（TiO2）Receive much concern, be primarily due to as the negative material of energy-storage battery（1）Dioxy
Change the intercalation potential about 1.75V of titanium, Li dendrite can be prevented effectively from and formed, the security performance of lithium ion battery is improved；（2）In lithium
During ion intercalation/deintercalation, the structure change of titanium dioxide is smaller, the structural stability of height is maintained, with excellent
Cycle performance and service life.But, the relatively low electronic conductance of titanium dioxide, relatively low ionic mobility and relatively low ratio
Capacity (335mAhg-1) it is limited in high-energy-density, the lithium-ion-power cell and energy-storage system of high power density
Application prospect.The TiO of nanosizing2The contact area of electrode surface and electrolyte is increased, the diffusion road of lithium ion is reduced
Footpath and removal lithium embedded depth, significantly improve the actual specific capacity and fast charging and discharging performance of battery.CNT is new as one kind
Fibrous conductive agent, can composite inner formation three-dimensional conductive network structure, play a part of electron propagation ducts,
The internal resistance of cell is reduced, the polarization of battery is alleviated, so as to further improve the chemical property of composite.Low temperature hydrolysis side
Method is a kind of important process route for synthesizing nano titanium oxide, simple, easy to operate and energy large-scale production excellent with equipment
Point.
The content of the invention
In order to improve the fast charging and discharging performance of composite titania material, the present invention is prepared for using low temperature hydrolysis method
The combination electrode material of carbon nanotube loaded nano titanium oxide, both effectively prevent nano titanium oxide during embedding de- lithium
Reunite, the electric conductivity of composite is significantly improved again, and then improve the chemical property of titanium dioxide.
For realize the purpose of the present invention use technical scheme be：
1st, 20 ~ 200 milligrams of CNTs are scattered in 50 milliliters~200 milliliters concentrated nitric acid solutions, processing time 8~20 is small
When.
2nd, the CNT for treating concentrated nitric acid is scattered in deionized water（1~3 milliliter）, surfactant phenmethylol（1
~10 milliliters）And absolute ethyl alcohol（30~100 milliliters）Mixed solution, ultrasonic disperse is after 3~24 hours at room temperature, then is placed in temperature
Spend in the cryogenic box for 1~7 DEG C and stir 12~36 hours, 100~400 revs/min of mixing speed is obtained containing CNT
The mixing solution A of absolute ethyl alcohol.
3rd, the organic compound of soluble titanium is dissolved in absolute ethyl alcohol, obtains the nothing of the organic compound containing soluble titanium
Water-ethanol mixes B solution；The organic compound of titanium and the volume ratio 1 of absolute ethyl alcohol：10~100.
4th, mixing B solution is added dropwise in mixing solution A and obtains mixed solution C, rate of addition is 1 ~ 3 drop/sec.
Concentrated nitric acid solution of the present invention, its concentration is 55~70%.
CNT of the present invention is multi-walled carbon nanotube（MWCNTs）And single-walled carbon nanotube（SWCNTs）In
It is a kind of.
The organic compound of titanium of the present invention is one kind in butyl titanate and isopropyl titanate and titanium tetrachloride.
In carbon nanotube loaded nanometer titanium dioxide composite material of the present invention, the mass fraction of CNT is 5%
~25%.
5th, mixed solution C is placed in the cryogenic box that temperature is 1~7 DEG C and continues to stir 12~36 hours, mixing speed 100
~400 revs/min.After stirring terminates, mixed solution C is separated with supercentrifuge, precursor product is obtained；Centrifugal rotational speed is
3000 ~ 4500 revs/min, centrifugation time is 1 ~ 10 minute.
6th, the precursor product obtained after high speed centrifugation is placed in air dry oven and be dried, obtain presoma
Powder, drying temperature is 50~150 DEG C, 6 ~ 24 hours drying times.
7th, precursor powder is placed in Muffle furnace or atmosphere furnace, the calcinations and sintering under air or oxygen atmosphere：Sintering temperature
Spend for 200~420 DEG C, heating rate is 1~5 DEG C/min, sintering time is 1~6 hour；Room temperature then is cooled to stove, is obtained
To carbon nanotube loaded nano titanium oxide of the present invention.
The inventive method effectively controls the particle diameter of synthesis of titanium dioxide, improves mechanical strength, the machinery branch of titanium dioxide
Support and energy density, improve the high current density charge-discharge performance and cycle performance of titanium dioxide cathode material.Simplify simultaneously
Synthesis technique, reduces production cost, improves the quality of product, it is easy to industrially practice.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum of sample prepared by the embodiment of the present invention 1.
Fig. 2 is the electron scanning micrograph of sample prepared by the embodiment of the present invention 1.
Fig. 3 is the cycle performance curve of sample prepared by the embodiment of the present invention 1.
Fig. 4 is the X ray diffracting spectrum of sample prepared by the embodiment of the present invention 2.
Fig. 5 is the electron scanning micrograph of sample prepared by the embodiment of the present invention 2.
Fig. 6 is the cycle performance curve of sample prepared by the embodiment of the present invention 2.
Embodiment
Below in conjunction with the accompanying drawings and case study on implementation, the present invention will be further described.
Embodiment 1
Titanium dioxide is combined SWNT（TiO2@SWCNTs）.
Weigh 50 milligrams through over-richness for 70% nitric acid treatment after SWCNTs be scattered in 50 milliliters of absolute ethyl alcohols, 8 milliliters
Phenmethylol and 1 ml deionized water mixed solution, ultrasonic vibration are placed in after 5 hours in 4 DEG C of cryogenic boxes, then are persistently stirred 2 hours
After obtain solution A.0.65 milliliter of butyl titanate is dissolved in 10 milliliters of absolute ethyl alcohols, it is molten to obtain B after stirring 20 minutes at room temperature
Liquid.B solution is added drop-wise in solution A dropwise and obtains mixed solution C, 1 drop/sec of rate of addition.Low temperature of the mixed solution C at 4 DEG C
Continue to stir 36 hours in case, 400 revs/min of mixing speed.After stirring terminates, mixed solution is separated with supercentrifuge, is obtained
To precursor product, centrifugal rotational speed is 3000 revs/min, and centrifugation time is 3 minutes.By the forerunner obtained after high speed centrifugation
Body product, which is placed in air dry oven, to be dried, and obtains precursor powder, and drying temperature is 60 DEG C, 24 hours drying times.
Precursor powder is placed in Muffle furnace, calcined under air atmosphere：Risen to 3 DEG C/min of heating rate from room temperature
350 DEG C, calcined 3 hours at 350 DEG C；Room temperature then is cooled to stove, carbon nanotube loaded nanometer two of the present invention is obtained
The composite of titanium oxide.The sample as made from above-mentioned steps is labeled as sample 1.
Fig. 1 is that the present embodiment prepares the X-ray diffracting spectrum of sample 1, from the collection of illustrative plates, and synthesized powder spreads out
Penetrate peak sharp, the standard diffraction peak of diffraction maximum and anatase titania meets very well, without other impurity diffraction maximums.
Fig. 2 is the stereoscan photograph of sample 1, as can be seen from the figure nano-TiO2Particle is uniformly coated on carbon nanometer
The surface of pipe.
Weigh the TiO of sample 1 made from 0.07 gram2@SWCNTs powder, 0.02 gram of conductive black and 0.01 gram of binding agent
PVDF（Kynoar）, it is scattered in N methylpyrrolidone solutions, is applied to after being well mixed on copper foil, it is dry in 110 DEG C of vacuum
Dry 12 hours, TiO is made2@SWCNTs cathode pole pieces.Using 1.0 mol/L LiPF6/ EC/DEC/DMC is electrolyte, wherein
LiPF6For conducting salt, EC (ethylene carbonate)/DEC (diethyl carbonate)/DMC (dimethyl carbonate) is double solvents, three
Volume ratio（EC:DEC:DMC）For 1：1：1.Using metal lithium sheet be to electrode, the polypropylene screens of Cellgard 2300 as barrier film,
Button cell is assembled into above-mentioned negative pole, discharge and recharge is carried out with 1000 mA/g current densities, the voltage range of discharge and recharge is 0.05
~3V。
Fig. 3 is charge and discharge cycles figure, as seen from the figure, and 500 lower TiO are circulated under 25 DEG C, 1000mA/g current densities2@
The specific discharge capacity of SWCNTs composites can still reach 260mAh/g or so, illustrate TiO made from this method2@SWCNTs
Composite has good chemical property.
Embodiment 2
Titanium dioxide is combined multiple-wall carbon nanotube（TiO2@MWCNTs）.
Weigh 45 milligrams and be scattered in 70 milliliters of absolute ethyl alcohols, 10 millis through over-richness for the SWCNTs after 55% nitric acid treatment
Phenmethylol and 1 ml deionized water mixed solution are risen, ultrasonic vibration is placed in after 3 hours in 5 DEG C of cryogenic boxes, then persistently stirring 3 is small
When after obtain solution A.By 0.8 milliliter of metatitanic acid isopropyl titanate in 20 milliliters of absolute ethyl alcohols, B is obtained after stirring 30 minutes at room temperature
Solution.B solution is added drop-wise in solution A dropwise and obtains mixed solution C, 2 drops/sec of rate of addition.Mixed solution C is low at 5 DEG C
Continue to stir 12 hours in incubator, 200 revs/min of mixing speed.After stirring terminates, precursor product is obtained.Use high speed centrifugation
Machine separates precursor product, and centrifugal rotational speed is 4500 revs/min, and centrifugation time is 5 minutes.By what is obtained after high speed centrifugation
Precursor product is placed in air dry oven and is dried, and obtains precursor powder, and drying temperature is 150 DEG C, and drying time 6 is small
When.Precursor powder is placed in Muffle furnace, calcined under air atmosphere：With 3 DEG C/min of heating rate from room temperature liter
To 380 DEG C, calcined 4 hours at 380 DEG C；Room temperature then is cooled to stove, carbon nanotube loaded nanometer of the present invention is obtained
The composite of titanium dioxide.The sample as made from above-mentioned steps is labeled as sample 2.
Fig. 4 is that the present embodiment prepares the X-ray diffracting spectrum of sample 2, from the collection of illustrative plates, and synthesized powder spreads out
Penetrate peak sharp, the standard diffraction peak of diffraction maximum and anatase titania meets very well, without other impurity diffraction maximums.
Fig. 5 is the stereoscan photograph of sample 2, as can be seen from the figure nano-TiO2Particle is uniformly coated on carbon nanometer
The surface of pipe.
Weigh the TiO of sample 2 made from 0.07 gram2@SWCNTs powder, 0.02 gram of conductive black and 0.01 gram of binding agent
PVDF（Kynoar）, it is scattered in N methylpyrrolidone solutions, is applied to after being well mixed on copper foil, it is dry in 120 DEG C of vacuum
Dry 12 hours, TiO is made2@SWCNTs cathode pole pieces.Using 1.0 mol/L LiPF6/ EC/DEC/DMC is electrolyte, wherein
LiPF6For conducting salt, EC (ethylene carbonate)/DEC (diethyl carbonate)/DMC (dimethyl carbonate) is double solvents, three
Volume ratio（EC:DEC:DMC）For 1：1：1.Using metal lithium sheet be to electrode, the polypropylene screens of Cellgard 2300 as barrier film,
Button cell is assembled into above-mentioned negative pole, discharge and recharge is carried out with 5000 mA/g current densities, the voltage range of discharge and recharge is 0.05
~3V。
Fig. 6 is charge and discharge cycles figure, as seen from the figure, and at 25 DEG C, 5000mA/g current densities circulate 1000 lower TiO2@MWCNTs
The specific discharge capacity of composite can still reach 160mAh/g or so, illustrate TiO made from this method2@MWCNTs composite woods
Material has good chemical property.
Claims (8)
1. a kind of preparation method of carbon nanotube loaded nano titanium oxide, it is characterised in that：
1）20~200 milligrams of CNTs are scattered in 50 milliliters~200 milliliters concentrated nitric acid solutions, processing time 8~20 is small
When；
2）The CNT that concentrated nitric acid is treated is scattered in the mixing of deionized water, surfactant phenmethylol and absolute ethyl alcohol
In solution, ultrasonic disperse carries out low temperature hydrolysis after 3~24 hours at room temperature, obtains mixing solution A；
3）The organic compound of soluble titanium is dissolved in absolute ethyl alcohol, obtains mixing B solution；The organic compound of titanium with it is anhydrous
The volume ratio 1 of ethanol：10~100；
4）Mixing B solution is added dropwise in mixing solution A and obtains mixed solution C, rate of addition is 1~3 drop/sec；
5）Mixed solution C is placed in cryogenic box and carries out low-temp reaction, after low-temp reaction terminates, is separated and mixed with supercentrifuge
Solution C, obtains precursor product；
6）Precursor product is placed in air dry oven and is dried, precursor powder is obtained, drying temperature is 50~150
DEG C, 6~24 hours drying times；
7）Precursor powder is placed in Muffle furnace or atmosphere furnace, the calcinations and sintering under air or oxygen atmosphere；Then dropped with stove
Warm to room temperature, obtain described carbon nanotube loaded nano titanium oxide.
2. the preparation method of a kind of titanium dioxide composite Nano carbon pipe according to claim 1, it is characterised in that described
CNT be multi-walled carbon nanotube and single-walled carbon nanotube in one kind.
3. a kind of preparation method of titanium dioxide composite Nano carbon pipe according to claim 1, it is characterised in that step 2）
In described mixed solution, the volume of deionized water, surfactant phenmethylol and absolute ethyl alcohol is respectively 1~3 milliliter, 1
~10 milliliters, 30~100 milliliters.
4. a kind of preparation method of titanium dioxide composite Nano carbon pipe according to claim 1, it is characterised in that step 2）
Described low temperature hydrolysis, its temperature is 1~7 DEG C, and hydrolysis time is 12~36 hours.
5. a kind of preparation method of carbon nanotube loaded nano titanium oxide according to claim 1, it is characterised in that institute
The concentrated nitric acid stated, concentration is 55~70%.
6. a kind of preparation method of carbon nanotube loaded nano titanium oxide according to claim 1, it is characterised in that institute
The titanium-containing compound stated is one kind in butyl titanate, isopropyl titanate and titanium tetrachloride.
7. a kind of preparation method of carbon nanotube loaded nano titanium oxide according to claim 1, it is characterised in that step
Rapid 5）Described low-temp reaction, its temperature is 1~7 DEG C, while stirring 12~36 hours, 100~400 revs/min of mixing speed；
Supercentrifuge is separated, and centrifugal rotational speed is 3000~4500 revs/min, and centrifugation time is 1~10 minute.
8. a kind of preparation method of carbon nanotube loaded nano titanium oxide according to claim 1, it is characterised in that step
Rapid 7）Described calcinations and sintering, sintering temperature is 200~420 DEG C, and heating rate is 1~5 DEG C/min, and sintering time is 1~6
Hour.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108598384A (en) * | 2018-03-19 | 2018-09-28 | 福建翔丰华新能源材料有限公司 | A kind of preparation method of composite aerogel negative material |
| CN109546113A (en) * | 2018-11-15 | 2019-03-29 | 北京长城华冠汽车科技股份有限公司 | A kind of preparation method and lithium-sulfur cell of the phosphorous carbon nano tube compound material of coated by titanium dioxide |
| CN110559691A (en) * | 2019-08-30 | 2019-12-13 | 长江大学 | Reusable carbon-based nano demulsifier and preparation method thereof |
| CN110880589A (en) * | 2019-11-25 | 2020-03-13 | 浙江理工大学 | Carbon nanotube @ titanium dioxide nanocrystal @ carbon composite material and preparation method and application thereof |
| CN111081992A (en) * | 2019-10-12 | 2020-04-28 | 开封大学 | Preparation method of binder-free lithium ion battery negative electrode material |
| CN113582220A (en) * | 2021-06-08 | 2021-11-02 | 湖南师范大学 | TiO 22Preparation method of/carbon composite interlayer |
| CN114709364A (en) * | 2022-03-24 | 2022-07-05 | 惠州锂威新能源科技有限公司 | Preparation method of composite negative electrode material, product of composite negative electrode material, negative electrode sheet and secondary battery |
| CN115057472A (en) * | 2022-06-21 | 2022-09-16 | 中国医学科学院基础医学研究所 | Novel fluorescence sensing system and application thereof in PTP-1B detection |
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| CN108598384A (en) * | 2018-03-19 | 2018-09-28 | 福建翔丰华新能源材料有限公司 | A kind of preparation method of composite aerogel negative material |
| CN109546113A (en) * | 2018-11-15 | 2019-03-29 | 北京长城华冠汽车科技股份有限公司 | A kind of preparation method and lithium-sulfur cell of the phosphorous carbon nano tube compound material of coated by titanium dioxide |
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| CN111081992A (en) * | 2019-10-12 | 2020-04-28 | 开封大学 | Preparation method of binder-free lithium ion battery negative electrode material |
| CN110880589A (en) * | 2019-11-25 | 2020-03-13 | 浙江理工大学 | Carbon nanotube @ titanium dioxide nanocrystal @ carbon composite material and preparation method and application thereof |
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| CN113582220A (en) * | 2021-06-08 | 2021-11-02 | 湖南师范大学 | TiO 22Preparation method of/carbon composite interlayer |
| CN114709364A (en) * | 2022-03-24 | 2022-07-05 | 惠州锂威新能源科技有限公司 | Preparation method of composite negative electrode material, product of composite negative electrode material, negative electrode sheet and secondary battery |
| CN115057472A (en) * | 2022-06-21 | 2022-09-16 | 中国医学科学院基础医学研究所 | Novel fluorescence sensing system and application thereof in PTP-1B detection |
| CN115057472B (en) * | 2022-06-21 | 2023-10-27 | 中国医学科学院基础医学研究所 | Novel fluorescence sensing system and application thereof in PTP-1B detection |
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