CN105316797A - Preparation of titanium dioxide nanofiber modified with nitrogen-doped mesoporous carbon - Google Patents
Preparation of titanium dioxide nanofiber modified with nitrogen-doped mesoporous carbon Download PDFInfo
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- CN105316797A CN105316797A CN201410381101.8A CN201410381101A CN105316797A CN 105316797 A CN105316797 A CN 105316797A CN 201410381101 A CN201410381101 A CN 201410381101A CN 105316797 A CN105316797 A CN 105316797A
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- mesoporous carbon
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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 titanium dioxide nanofiber modified with nitrogen-doped mesoporous carbon and formed through electrostatic spinning, that is to say, the TiO2 nanofiber modified with the nitrogen-doped mesoporous carbon is obtained through an electrostatic spinning method, and the average thickness is 250 nm. The nanofiber comprises multi-crystal-phase TiO2 of which the interior is communicated and a large number of mesoporous structures in the nitrogen-doped carbon. After 100 cycles at the electric current density of 33mAg<1>, the TiO2 nanofiber modified with the nitrogen-doped mesoporous carbon still has the high capacitance of 264 mAh/g. The TiO2 nanofiber modified with the nitrogen-doped mesoporous carbon can be applied to cathode materials of lithium ion batteries.
Description
Art
The present invention relates to the preparation method of the titania fiber that a kind of N doping mesoporous carbon is modified, more particularly relate to the preparation process of organic-inorganic composition, the i.e. solution such as ethanol of butyl titanate, acetic acid, join after agitation in the ethanolic solution of polyvinylpyrrolidone, add 1-ethyl-3-methylimidazole dicyandiamide salt further, obtain the solution of composition electrostatic spinning, obtain titanium dioxide/polymer composite fiber further by electrospinning device, and at high temperature carbonization obtains N doping mesoporous carbon titania fiber.This titania fiber with meso-hole structure has good chemical property, can be used for the positive electrode of lithium ion battery.
Background technology
Ultracapacitor is a kind of not only stable but also the novel energy-storing element of environmental protection, the advantage such as have that the charging interval is short, long service life, power density are high, safety coefficient is high, energy-conserving and environment-protective, low-temperature characteristics are good.The application of ultracapacitor in modern science and technology, industry, aerospace industry is all very extensive, it represent the once breakthrough of high energy storage technology.
TiO2 is a kind of wide bandgap semiconductor, and its energy gap is 3.2eV, just can show photocatalytic activity be only less than the exciting of 387nm ultraviolet light at wavelength under, but this part ultraviolet light only account for reach ground surface sunlight 3% ~ 4%.In order to expand the spectral response range of TiO2 material, people have attempted a large amount of method of modifying, as noble metal loading, ion doping, composite semiconductor and finishing etc., wherein N element doping not only makes material have obvious visible light activity, and can also keep very high ultraviolet light activity. and the research of material structure optimization aspect mainly concentrates on the preparations and applicatio of high-specific surface area, ordered mesoporous material.
Bibliographical information is had to adopt static state deposition legal system for foramen magnum-mesoporous TiO2 material; Take Woelm Alumina as template, adopt sol-gal process to prepare titania nanotube etc.
There is the weak points such as the poor heat stability of meso-hole structure in current known titanium dioxide nanofiber technology of preparing.
Purport of the present invention effectively utilizes carbon-based material high-specific surface area, and the titanium dioxide nanofiber with the modification of N doping mesoporous carbon of preparation has good chemical property, can be used for the positive electrode of lithium ion battery.
Summary of the invention
The butyl titanate of certain mass ratio, acetic acid, polyvinylpyrrolidone and 1-ethyl-3-methylimidazole dicyandiamide salt are stirred under ethanol is solvent, obtain the solution of composition electrostatic spinning, obtain titanium dioxide/polymer composite fiber by electrospinning device, and at high temperature carbonization obtains N doping mesoporous carbon titania fiber.
the technical solution adopted for the present invention to solve the technical problems is:
By butyl titanate, acetic acid and ethanol according to the mixing of certain quality proportioning, then stir into homogeneous phase solution A; Polyvinylpyrrolidone is dissolved in ethanolic solution, then adds 0.3mL1-ethyl-3-methylimidazole dicyandiamide salt composition homogeneous phase solution B, finally two kinds of solution A, B are mixed composition electrostatic spinning solution mutually.By electrostatic spinning solution by electrospinning device spinning under certain straight alternating voltage and flow velocity, obtain titanium dioxide/polymer composite fiber, and dry under uniform temperature in atmosphere, the fiber high-temperature roasting carbonization in a nitrogen atmosphere further of acquisition.Final acquisition has the mesoporous carbon titania fiber of carbon doping.
The present invention utilizes the characterization method such as X-ray diffraction (XRD), scanning electronic microscope (SEM) to analyze prepared sample.
the invention has the beneficial effects as follows:
The titania fiber that a kind N doping mesoporous carbon of the present invention is modified, average thickness is 250nm.Nanofiber comprises the polycrystalline phase TiO that inside communicates
2with a large amount of meso-hole structure in nitrogen-doped carbon.At 33mAg
1after lower 100 circulations of current density, the TiO of N doping mesoporous carbon decorations
2nanofiber still has the high-capacitance of 264mAh/g, and this fiber is applicable to lithium ion anode process.Method of operating is simple, with low cost, can repeat.
Accompanying drawing explanation
The TiO that Fig. 1 is modified by N doping mesoporous carbon
2the scanning electron microscope (SEM) photograph of nanofiber, can find out that the thickness of N doping mesoporous carbon titania fiber is at about 250nm.
Fig. 2 is the TiO that N doping mesoporous carbon is modified
2the big angle XRD collection of illustrative plates of nanofiber.Show titanium dioxide once anatase crystalline structure after high temperature cabonization.
The TiO that Fig. 3 N doping mesoporous carbon is modified
2nitrogen adsorption-the desorption curve of nanofiber and pore size distribution curve figure.Sample has meso-hole structure.
The TiO that Fig. 4 N doping mesoporous carbon is modified
2the cycle performance figure of nanofiber, as seen at 33mAg
1after lower 100 circulations of current density, the TiO of N doping mesoporous carbon decorations
2nanofiber still has the high-capacitance of 264mAh/g.
The TiO of Fig. 5 N doping mesoporous carbon decorations
2the discharge and recharge collection of illustrative plates of nanofiber after 20 circulations.
The TiO that Fig. 6 N doping mesoporous carbon is modified
2the large current discharging capability figure of nanofiber
Detailed description of the invention
Below by way of specific embodiment, also the invention will be further described by reference to the accompanying drawings, but the present invention is not limited to following examples.
Described method if no special instructions, is conventional method.Described material if no special instructions, all can be bought from open commercial sources and obtain.
embodiment 1
1.0 grams of butyl titanates and 1.0 grams of acetic acid join in 5 grams of ethanolic solutions, form solution A after stirring.0.2 gram of polyvinylpyrrolidone is dissolved in 5 grams of ethanolic solutions, and then adds 0.1 gram of 1-ethyl-3-methylimidazole dicyandiamide salt, after stirring, form solution B.After two kinds of solution are stirred further, composition electrostatic spinning solution.Then ready electrostatic spinning solution is mixed, stir 30min gently, what be then injected into stainless steel has in the syringe of 18 rule metallic nozzle.Solution is carried out electrostatic spinning experiment with the speed of 0.2mL/h under the straight alternating voltage of 5kV, from the nipple top 20cm place of syringe, collects nanofiber on aluminium foil.The Electrospun nano-fibers that obtains first stablizes 5h at 200 DEG C in atmosphere, and then lower 500 DEG C of Ar gas atmosphere carries out carbonization treatment.Heating and cooling speed is 1 DEG C/min.Finally obtain the titania fiber of N doping mesoporous carbon.
embodiment 2
1.0 grams of butyl titanates and 1.5 grams of acetic acid join in 15 grams of ethanolic solutions, form solution A after stirring.0.35 gram of polyvinylpyrrolidone is dissolved in 10 grams of ethanolic solutions, and then adds 0.2 gram of 1-ethyl-3-methylimidazole dicyandiamide salt, after stirring, form solution B.After two kinds of solution are stirred further, composition electrostatic spinning solution.Then ready electrostatic spinning solution is mixed, stir 30min gently, what be then injected into stainless steel has in the syringe of 18 rule metallic nozzle.Solution is carried out electrostatic spinning experiment with the speed of 0.35mL/h under the straight alternating voltage of 15kV, from the nipple top 20cm place of syringe, collects nanofiber on aluminium foil.The Electrospun nano-fibers that obtains first stablizes 5h at 250 DEG C in atmosphere, and then lower 600 DEG C of Ar gas atmosphere carries out carbonization treatment.Heating and cooling speed is 1 DEG C/min.Finally obtain the titania fiber of N doping mesoporous carbon.
embodiment 3
1.0 grams of butyl titanates and 3.0 grams of acetic acid join in 25 grams of ethanolic solutions, form solution A after stirring.0.5 gram of polyvinylpyrrolidone is dissolved in 25 grams of ethanolic solutions, and then adds 0.3 gram of 1-ethyl-3-methylimidazole dicyandiamide salt, after stirring, form solution B.After two kinds of solution are stirred further, composition electrostatic spinning solution.Then ready electrostatic spinning solution is mixed, stir 30min gently, what be then injected into stainless steel has in the syringe of 18 rule metallic nozzle.Solution is carried out electrostatic spinning experiment with the speed of 0.5mL/h under the straight alternating voltage of 20kV, from the nipple top 20cm place of syringe, collects nanofiber on aluminium foil.The Electrospun nano-fibers that obtains first stablizes 5h at 300 DEG C in atmosphere, and then lower 800 DEG C of Ar gas atmosphere carries out carbonization treatment.Heating and cooling speed is 1 DEG C/min.Finally obtain the titania fiber of N doping mesoporous carbon.
Claims (5)
1. the present invention relates to a kind of preparation method with the titanium dioxide nanofiber that N doping mesoporous carbon is modified by electrostatic spinning, be primarily characterized in that butyl titanate, the solution such as the ethanol of acetic acid, join after agitation in the ethanolic solution of polyvinylpyrrolidone, add 1-ethyl-3-methylimidazole dicyandiamide salt further, obtain the solution of composition electrostatic spinning, then the solution of electrostatic spinning is obtained titanium dioxide/polymer composite fiber by electrospinning device, and in atmosphere after drying, high-temperature carbonization in a nitrogen atmosphere, finally obtain the titania fiber that N doping mesoporous carbon is modified.
2. a kind of preparation method with the titanium dioxide nanofiber that N doping mesoporous carbon is modified by electrostatic spinning according to claim 1, is primarily characterized in that the quality of butyl titanate, acetic acid, ethanol, polyvinylpyrrolidone and 1-ethyl-3-methylimidazole dicyandiamide salt than scope at 1:1-3:10-50:0.2-0.5:0.1-0.3.
3. a kind of preparation method with the titanium dioxide nanofiber that N doping mesoporous carbon is modified by electrostatic spinning according to claim 1, is primarily characterized in that the DC voltage 5KV-20KV of electrostatic spinning, flow velocity 0.2-0.5 ml/hour.
4. a kind of preparation method with the titanium dioxide nanofiber that N doping mesoporous carbon is modified by electrostatic spinning according to claim 1, after being primarily characterized in that spinning, titanium dioxide/aerial baking temperature of polymer composite fiber is between 200-300 degree.
5. according to claim 1 a kind ofly have by electrostatic spinning the preparation method of titanium dioxide nanofiber that N doping mesoporous carbon modifies, and is primarily characterized in that the temperature of the titanium dioxide/high temperature cabonization of polymer composite fiber in nitrogen after spinning is between 500-800 degree.
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| CN108950734B (en) * | 2018-08-24 | 2020-12-29 | 济南大学 | Gully-shaped MoO3Synthetic method of (2) and product thereof |
| CN109023558A (en) * | 2018-09-26 | 2018-12-18 | 南通大学 | A kind of electrostatic spinning apparatus and electrospinning process for realizing carbon material N doping |
| CN109023558B (en) * | 2018-09-26 | 2021-01-12 | 南通大学 | Electrostatic spinning device and electrostatic spinning method for realizing nitrogen doping of carbon material |
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