CN107785563A - Nano-TiO2The preparation method of electrode material - Google Patents

Nano-TiO2The preparation method of electrode material Download PDF

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Publication number
CN107785563A
CN107785563A CN201710823247.7A CN201710823247A CN107785563A CN 107785563 A CN107785563 A CN 107785563A CN 201710823247 A CN201710823247 A CN 201710823247A CN 107785563 A CN107785563 A CN 107785563A
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tio
nano
electrode material
preparation
absolute ethyl
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李志宏
李力强
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Tianjin University
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Tianjin University
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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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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 kind of nano-TiO2As the preparation method of electrode material, using butyl titanate as titanium source, polyvinylpyrrolidone (mass fraction Mr=30000 PVP) is used as suspending agent, by volume absolute ethyl alcohol：Acetic acid：Butyl titanate=15:15:8 ratios mix, and add and compare absolute ethyl alcohol with quality：PVP=4：The solution that 3 ratios mix, obtains precursor solution, high molecular polymer is prepared with electrospinning device, is torn off and is placed in crucible, be heated to 500 DEG C with 2 °/min heating rates, obtain TiO2Fibrous material.The invention provides a kind of cost is cheap, technique is simple, has the TiO of bigger reversible specific capacity, more excellent cycle performance and high rate performance2Electrode material, 500 DEG C of heat treatment TiO2First charge-discharge specific capacity reaches 156mAh/g, obvious charge and discharge platform be present.

Description

Nano-TiO2The preparation method of electrode material
Technical field
The present invention is more particularly to a kind of nano-TiO on electrode material2Preparation method as electrode material.
Background technology
It is increasingly becoming with the fast development of social industrial technology, the problems such as environmental pollution and scarcity of resources of concern Focus, the development of electrochmical power source are faced with unprecedented opportunities and challenges, and with the arriving in electric automobile epoch, lithium ion battery will Large-scale application is obtained, and lithium ion battery negative material is TiO an important factor for influenceing battery performance2Due to its have than Higher discharge platform (1.5~1.8V), the advantages that having a safety feature, it is expected to turn into a kind of new negative electrode of lithium ion battery material Material.Nano-TiO at present2The technology of preparing of material mainly has electrostatic spinning technique, hydro-thermal method, sol-gel method, anodic oxidation Method etc..Low-dimension nano material etc. scope of application is wider, and operating method is simple and easy preparing for electrostatic spinning technique, by grinding Study carefully the property of solution, apply the parameter such as relevant voltage and adjustment spinning environment to realize the various of low-dimension nano material structure Change, and be compared to traditional hydro-thermal method and prepare titania fiber material, more efficient, the microcosmic controllability of material is more convenient, Electrostatic spinning technique prepare high polymer material be it is diversified, it is almost unrestricted, thus utilize electrostatic spinning skill Art prepares the superfine fibre of various high polymer materials and inorganic matter nanofiber can develop application in numerous areas, including electricity Sub- device, nano-form, tissue engineering bracket and high-performance filter, seperation film, vest, drug controlled release, absorption All there is boundless development prospect Deng.
The content of the invention
The purpose of the present invention, is to provide that a kind of technique is simple, energy consumption is low, the nano-TiO of function admirable2As electrode material The preparation method of material, it is compared to traditional hydro-thermal method and prepares titania fiber material, more efficient, material controllability is more By force.
The present invention is achieved by following technical solution.
A kind of nano-TiO2The preparation method of electrode material：TiO is prepared using electrostatic spinning technique2Nanofiber, specific step It is rapid as follows：
(1) using butyl titanate as titanium source, polyvinylpyrrolidone is molten as solvent using absolute ethyl alcohol and acetic acid as suspending agent Butyl titanate is solved, by volume absolute ethyl alcohol：Acetic acid：Butyl titanate=15:15:8, mix 2h；Another extracting container is with anhydrous Ethanol is solvent polyethylene dissolving pyrrolidones, by absolute ethyl alcohol：Polyvinylpyrrolidone mass ratio=4：3, mix 2h； Solution containing polyvinylpyrrolidone is poured into butyl titanate solution, 6h is mixed and obtains precursor solution；
(2) precursor solution for obtaining step (1), is pumped into disposable syringe, the insertion needle at pin hole, is cut The tiling of 30cm × 20cm aluminium foils, which is fixed on, to be received on plate washer；
(3) step (2) described syringe is placed in electrospinning device termination, setting syringe needle is with receiving plate washer distance 15cm, electrode one end is clipped on syringe needle, start high voltage power supply, high molecular polymer is prepared；
(4) high molecular polymer obtained by step (3) is torn off and be placed in crucible, be put into Muffle furnace and be warming up to 500 DEG C, perseverance Warm 3h takes out, and nano-TiO is made2Fibrous material；
(5) by TiO obtained by step (4)2Fibrous material is pressed with conductive carbon black (Super P) and carboxymethyl cellulose (CMC) Mass ratio 8:1:1 mixing, with H2O is that solvent is well mixed, grinds half an hour, and slurry is mixed up；Using copper foil as collector, use Coating machine is by slurry even application on copper foil；Coated electrode slice is put into vacuum drying chamber and is warming up to 120 DEG C of dryings 12 hours；Dried electrode slice is cut into a diameter of 12mm circular electric pole piece with hand microtome, obtains TiO2Electrode material Material.
The polyvinylpyrrolidone mass fraction of the step (1) is Mr=30000 PVP.
The disposable syringe of the step (2) is 5ml, and needle gauge is No. 21.
The step (3) sets syringe needle and receives plate washer apart from being 12cm, starts high voltage power supply and sets 12KV.
The temperature schedule of the step (4) is：Less than 500 DEG C heating rates are 2 DEG C/min, and 180min is incubated in 500 DEG C.
The invention provides a kind of cost is cheap, technique is simple, has bigger reversible specific capacity, more excellent cycle performance With the TiO of high rate performance2Electrode material, 500 DEG C of heat treatment TiO2First charge-discharge specific capacity reaches 156mAh/g, exists obvious Charge and discharge platform.
Brief description of the drawings
Fig. 1 is TiO prepared by the embodiment of the present invention 32X-ray diffraction pattern；
Fig. 2 is TiO prepared by the embodiment of the present invention 32Scanning electron microscope diagram；
Fig. 3 is TiO prepared by the embodiment of the present invention 32Cyclic voltammetry curve figure under 10mV/s sweep speeds；
Fig. 4 is TiO prepared by the embodiment of the present invention 32Cycle performance curve map.
Embodiment
Below by specific embodiment, the invention will be further described.
Embodiment 1
(1) 0.45g polyvinylpyrrolidones (mass fraction Mr=30000 PVP) are weighed with electronic balance and is placed in 100ml In beaker, 7.5ml absolute ethyl alcohols are measured out at twice with 5ml (precision 0.1ml) graduated cylinder and are poured into beaker, be put into A type magnetic force and stir Sub (model A200/ ￠ 8 × 20) is mixed, then it is got up with preservative film plastic packaging and (prevented alcohol from volatilizing), is placed on magnetic stirring apparatus On 2h be stirred at room temperature with 300r/min speed obtain solution A；
3ml absolute ethyl alcohols are measured with 5ml (precision 0.1ml) graduated cylinder to be placed in another 100ml beakers, then with same size Graduated cylinder measures 3ml glacial acetic acids and pours into beaker (glacial acetic acid heating water bath to 60 DEG C of 30min), finally measures 1.6ml metatitanic acids Butyl ester pours into beaker and (accurate measuring is carried out in ventilating kitchen with disposable plastic dropper), is put into A type magnetic stir bar (models A200/ ￠ 8 × 20), it is got up with preservative film plastic packaging, is placed on magnetic stirring apparatus and is stirred at room temperature with 300r/min speed 2h obtains B solution；
B solution is poured into solution A, mixed solution is placed on magnetic stirring apparatus to be stirred at room temperature with 300r/min speed 6h obtains precursor solution.
(2) cut the tiling of 30 × 20cm aluminium foils to be fixed on reception plate washer, it is molten to be pumped into presoma with 5ml disposable syringes Liquid, internal gas is drained, 21# syringe needles are inserted at pin hole, it is 15cm to set syringe needle and receive plate washer distance；
(3) electrode one end is clipped on syringe needle, starts high voltage power supply, voltage is adjusted to 12KV, carries out electrostatic spinning (Static Spinning Silk parameter setting according to solution viscosity is different can suitably adjust), high molecular polymer is prepared；
(4) aluminium foil is removed after the completion of electrostatic spinning, the high molecular polymer that spinning is obtained, which is torn off, to be placed in crucible, is put Enter in Muffle furnace and be heated to 700 DEG C with 2 °/min heating rates, constant temperature 3h takes out, and nano-TiO is made2Fibrous material.
(5) by nano-TiO2Fibrous material, conductive carbon black (Super P) and carboxymethyl cellulose (CMC) press 8:1:1 is mixed Close, with H2O is that solvent is well mixed, grinds half an hour, and slurry is mixed up；Using copper foil as collector, with coating machine by slurry Even application is on copper foil；Coated electrode slice is put into vacuum drying chamber and is warming up to 120 DEG C of dryings 12 hours；With manual Dried electrode slice is cut into a diameter of 12mm circular electric pole piece by slicer, obtains TiO2Electrode material.
Embodiment 2
In embodiment 2 in addition to heating-up temperature is 600 DEG C, other processes are identical with example 1.
Embodiment 3
In embodiment 3 in addition to heating-up temperature is 500 DEG C, other processes are identical with example 1.
TiO2Electrochemical property test is tested by being assembled into button cell, first carries out battery according to the following procedure Assembling：Carried out in the glove box full of argon gas, ensure that water, oxygen content are less than 0.5ppm, using obtained electrode slice as negative pole, gold Category lithium piece is positive pole, and electrolyte uses 1mol/L LiPF6/EC-DMC (1:1volume ratio)/lithium ion battery, barrier film Using 2400 type microporous polypropylene films of Celgard companies.Successively according to anode cover-electrode slice-barrier film-negative plate-pad- The order of shell fragment-negative electrode casing assembles battery, and is sealed battery by battery sealing machine, stands 6 hours and ensures electrolysis liquid energy Enough abundant wetting electrode pieces.Electrochemical property test, voltage start-stop scope are 1-3V to the battery assembled at ambient temperature.Its It is middle that cyclic voltammetry is carried out using electrochemical workstation (CHI 604D, Shanghai Chen Hua)；Using the charge and discharge controlled by computer Electrical measurement test system (Shenzhen Xin Wei electronics corporations, BTS series) carries out constant current charge-discharge performance test.
Fig. 1 is TiO prepared by the embodiment of the present invention 32X-ray diffraction pattern.As shown in figure 1, the TiO obtained2X ray picture Spectrum, where it can be seen that 500 DEG C of heat treatment TiO2There is a stronger characteristic peak at 25.1 °, correspond to TiO2(101) crystal face category Feature peak position in Anatase, figure is and anatase TiO2PDF cards it is consistent.
Fig. 2 is TiO prepared by the embodiment of the present invention 32Scanning electron microscope diagram.It is from scanning figure it may be seen that fine Thread weave in, diameter skewness are tieed up, surface topography has considerable influence to chemical property.
Fig. 3 is TiO prepared by the embodiment of the present invention 32Cyclic voltammetry curve figure under 10mV/s sweep speeds.Such as Fig. 3 Shown, prepared by embodiment 3 TiO2Cyclic voltammetry curve, it was obvious that there is a dioxygen near 1.9V and 1.6V Change reduction peak, that represent respectively is Li+Abjection and insertion, be typical Detitanium-ore-type TiO2Redox peaks.In 2.3V and 2.1V nearby also has a pair of redox peaks, represents TiO2(B) presence of phase, it is consistent with XRD analysis result.
Fig. 4 is TiO prepared by the embodiment of the present invention 32Cycle performance curve map.As shown in figure 4, in order to test electrode material Circulation ability and the charging and discharging capabilities under big multiplying power current density, we are under 0.1A/g current density to three kinds of electrodes Material has done after 20 circulations and has then made powerful charge-discharge test, respectively 0.2,0.5, under 1A/g current density Test the charging and discharging capabilities of electrode material.Charging and discharging curve under three kinds of electrode material different multiplyings, it can be seen that electrode material Material capacity in the case where current density becomes big declines, because as current density increases, electrode is in electrolyte surface meeting Substantial amounts of electrolyte ion is adsorbed, causes interface electrolyte ion concentration to decline rapidly, so as to increase concentration polarization, causes to expand Scattered dynamic performance reduces, and then causes Li+ abjection speed to be affected, secondly, when high current can bring effective abjection Between reduction because the time of the bigger discharge and recharge of multiplying power is fewer, then the coverage of diffusion also receives to a certain extent Influence, so in charging complete, it is likely that there are some lithium ions can not also be completely among negative pole, so capacity can be with Current density increase and reduce.
500 DEG C of heat treatment TiO2Specific discharge capacity is higher, and first charge-discharge specific capacity reaches 156mAh/g, exists and significantly fills Discharge platform, charging and discharging curve is gentle, corresponding typical Anatase.
Show from above-mentioned electro-chemical test, prepared TiO2Nano-fiber material has preferable chemical property, has Prestige is applied in the energy storage devices such as lithium battery.
Above example is only the exemplary description done to the present invention, it should explanation, is not departing from the present invention's In the case of core, any simple deformation, modification or other skilled in the art can not spend creative work Equivalent substitution each falls within protection scope of the present invention.

Claims (5)

  1. A kind of 1. nano-TiO2The preparation method of electrode material, TiO is prepared using electrostatic spinning technique2Nanofiber, specific steps It is as follows：
    (1) using butyl titanate as titanium source, polyvinylpyrrolidone dissolves titanium using absolute ethyl alcohol and acetic acid as suspending agent as solvent Acid butyl ester, by volume absolute ethyl alcohol：Acetic acid：Butyl titanate=15:15:8, mix 2h；Another extracting container is with absolute ethyl alcohol For solvent polyethylene dissolving pyrrolidones, by absolute ethyl alcohol：Polyvinylpyrrolidone mass ratio=4：3, mix 2h；It will contain The solution for having polyvinylpyrrolidone is poured into butyl titanate solution, is mixed 6h and is obtained precursor solution；
    (2) precursor solution for obtaining step (1), is pumped into disposable syringe, the insertion needle at pin hole, cuts 30cm The tiling of × 20cm aluminium foils, which is fixed on, to be received on plate washer；
    (3) step (2) described syringe is placed in electrospinning device termination, it is 15cm to set syringe needle and receive plate washer distance, Electrode one end is clipped on syringe needle, starts high voltage power supply, high molecular polymer is prepared；
    (4) high molecular polymer obtained by step (3) is torn off and be placed in crucible, be put into Muffle furnace and be warming up to 500 DEG C, constant temperature 3h Take out, nano-TiO is made2Fibrous material；
    (5) by TiO obtained by step (4)2Fibrous material and conductive carbon black (Super P) and carboxymethyl cellulose (CMC) are in mass ratio 8:1:1 mixing, with H2O is that solvent is well mixed, grinds half an hour, and slurry is mixed up；Using copper foil as collector, coating machine is used By slurry even application on copper foil；Coated electrode slice is put into vacuum drying chamber and is warming up to 120 DEG C of dryings 12 hours； Dried electrode slice is cut into a diameter of 12mm circular electric pole piece with hand microtome, obtains TiO2Electrode material.
  2. 2. nano-TiO according to claim 12The preparation method of electrode material, it is characterised in that the step (1) is gathered Vinylpyrrolidone mass fraction is Mr=30000 PVP.
  3. 3. nano-TiO according to claim 12Preparation method as electrode material, it is characterised in that the step (2) Disposable syringe be 5ml, needle gauge is No. 21.
  4. 4. nano-TiO according to claim 12Preparation method as electrode material, it is characterised in that the step (3) Syringe needle is set and receives plate washer apart from being 12cm, starts high voltage power supply and 12KV is set.
  5. 5. nano-TiO according to claim 12Preparation method as electrode material, it is characterised in that the step (4) Temperature schedule be：Less than 500 DEG C heating rates are 2 DEG C/min, and 180min is incubated in 500 DEG C.
CN201710823247.7A 2017-09-13 2017-09-13 Nano-TiO2The preparation method of electrode material Pending CN107785563A (en)

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CN110176596A (en) * 2019-06-17 2019-08-27 启东启澳新材料科技发展有限公司 A method of improving lithium battery anode coating material chemical property
CN110846888A (en) * 2019-11-27 2020-02-28 宁波大学 Preparation method of sulfur-doped titanium dioxide nano-fiber
CN112886013A (en) * 2021-01-28 2021-06-01 陕西科技大学 Preparation method of titanium dioxide/carbon nanofiber anode material with multilevel structure
CN113816419A (en) * 2021-08-04 2021-12-21 绿宸新能源科技(苏州)有限公司 Modified titanium dioxide manganese cobaltate composite material and preparation method and application thereof

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CN110846888A (en) * 2019-11-27 2020-02-28 宁波大学 Preparation method of sulfur-doped titanium dioxide nano-fiber
CN112886013A (en) * 2021-01-28 2021-06-01 陕西科技大学 Preparation method of titanium dioxide/carbon nanofiber anode material with multilevel structure
CN112886013B (en) * 2021-01-28 2022-11-08 陕西科技大学 Preparation method of titanium dioxide/carbon nanofiber anode material with multilevel structure
CN113816419A (en) * 2021-08-04 2021-12-21 绿宸新能源科技(苏州)有限公司 Modified titanium dioxide manganese cobaltate composite material and preparation method and application thereof

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