CN103165283A - Method for enhancing electrochemical performance of TiO2 electrode - Google Patents
Method for enhancing electrochemical performance of TiO2 electrode Download PDFInfo
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- CN103165283A CN103165283A CN2013100954532A CN201310095453A CN103165283A CN 103165283 A CN103165283 A CN 103165283A CN 2013100954532 A CN2013100954532 A CN 2013100954532A CN 201310095453 A CN201310095453 A CN 201310095453A CN 103165283 A CN103165283 A CN 103165283A
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Abstract
The invention discloses a simple, convenient, low-cost and high-efficiency method for enhancing the electrochemical performance of a TiO2 electrode. The method is used for reversely applying voltage to the TiO2 electrode, electrochemical reaction treatment is preformed in a two-electrode system by taking neutral, acidic or alkaline solution as electrolyte, a negative electrode of the two-electrode system is the annealed TiO2 electrode, and a positive electrode of the two-electrode system is a carbon rod. In the method, special equipment is omitted, H+ ions in the solution are driven by an electric field, doping and defects are directly led into the TiO2 electrode, the electrochemical performance of the TiO2 electrode is enhanced, TiO2 energy gaps are reduced, the light absorption rate is increased, and electrical conductivity of the electrode is improved. The original TiO2 structure (such as a TiO2 nanotube and a nanowire array) cannot be damaged, so that the TiO2 electrode can be more effectively applied to the field of energy storage, photocatalysis, solar cells, photochromatism and the like.
Description
Technical field
The invention belongs to technical field of electrochemistry, relate to a kind of easy, cheap, strengthen TiO efficiently
2The method of electrode electro Chemical performance.The method can strengthen TiO
2As the energy storage device electrode, the performance of electrode of solar battery and photoelectrocatalysimaterial material can be used as simultaneously good electric conducting material and is applied to other field.
Background technology
Along with global IT application and industrialized fast development, various computers, miniature electronic apparatus and mobile communication equipment are day by day universal, in the urgent need to high performance memory ready power supply.On the other hand, the consumption of fuel-engined vehicle causes energy shortage and serious environmental pollution, and this impels people to design production low energy consumption and low emission electric automobile or mixed power electric car.But secondary cell commonly used because power density is not enough, can't satisfy alone the power requirement of electric automobile at present, needs the ultracapacitor of high power density to be used in conjunction with.Simultaneously, people are seeking new clear energy sources always and are alleviating the method for environmental pollution, as H
2Large energy is emitted in the energy burning and product is water, and water can reuse again and produce H
2, whole cyclic process is without any pollution.But how easy and prepare at an easy rate H
2Be difficult to solve always.TiO
2Owing to having the advantages such as semiconductor property and stable chemical nature, with low cost, environmental protection, be not only a kind of super capacitance electrode material that can be used for electrochemical energy storing device, and be a kind of rising photoelectrocatalysimaterial material, can be applicable to the photoelectrocatalysis decomposition water and prepare H
2Cause the organic substance of environmental pollution with degraded.Therefore, TiO
2As the electrode material of energy storage device, solar cell or photoelectro catalytic system, no matter become in global range is academia or the study hotspot of industrial circle.
Yet, as the TiO of direct use eigenstate
2During as energy storage device electrode or photochemical catalyst electrode, its chemical property is relatively poor.For example, TiO
2When nano particle is prepared into super capacitor electrode, only present lower electric double layer capacitance, capacity is 10-40 μ F/cm
2, this is mainly by eigenstate TiO
2Low conductance property due to.In addition, TiO
2When nano particle was used as photoelectrocatalysielectrode electrode, its efficiency of light absorption was less than 3%, and catalytic efficiency is low.This again with TiO
2Energy gap wider (3.2 eV), only to ultraviolet light have response and the compound factor such as too fast of charge carrier relevant.
As seen, improve TiO
2Conductivity be to strengthen its key as the energy storage device electrode performance.In order to improve TiO
2Conductivity and chemical property, the main employing introduced metal (ZK Zheng at present, et al. Journal of Materials Chemistry 21 (2011) 9079) or the method for nonmetallic inclusion (X Chen, et al. Chemical Reviews 107 (2007) 2891) at TiO
2Produce acceptor or donor state in energy gap, reach thereby reduce energy gap the purpose that improves conductivity.Yet the instability problem of and the thermal and electrochemical compound such as charge carrier that causes due to the introducing of dopant still is difficult to solve (R Asahi, et al. Science 293 (2001) 269).On the other hand, by at TiO
2Introduce oxygen room (Ti in lattice
3+The position) autodoping of generation donor state also can regulate and control its band structure, and this autodoping method can greatly improve TiO
2Visible light is arrived the response of infrared light, its conductivity and electro-chemical activity.But the most effective autodoping method is all at high temperature to carry out (XH Lu, et al. Nano Letters 12 (2012) 1690 so far; XD Jiang, et al. Journal of Physical Chemistry C 116 (2012) 22619) or need long processing procedure (XB Chen, et al. Science 331 (2011) 746).Therefore, find a kind of easy, cheap, TiO of method enhancing efficiently
2Chemical property is the key of dealing with problems.
Summary of the invention
The object of the present invention is to provide a kind of easy, cheap, strengthen TiO efficiently
2The method of electrode electro Chemical performance makes TiO
2Electrode material can satisfy the application requirements in energy storage device, photoelectrocatalysis, solar cell, the field such as photochromic.
The technical solution that realizes the object of the invention is: a kind of easy, cheap, strengthen TiO efficiently
2The method of electrode electro Chemical performance is to prepared TiO
2Electrode carries out reverse making alive to be processed: namely with the TiO of crystalline state
2Electrode is negative electrode, and carbon-point is in two electrode systems of anode, and concentration of electrolyte is 0.1-2 M, carries out electrochemical reaction under normal temperature and processes, and between two electrodes, spacing is 0.5-10 cm, to apply voltage be that 2-10 V and reacting treatment time are 5-360 s.
Described electrolyte is neutrality, acidity or alkaline solution, particular certain cancers, sylvite, ammonium salt, hydrochloric acid, sulfuric acid, phosphoric acid, NaOH or potassium hydroxide solution.
Preparation TiO of the present invention
2The method of electrode can adopt anode oxidation method, hydro thermal method, template, sol-gal process, microemulsion method and vapour deposition process etc., and wherein anode oxidation method can adopt constant voltage oxidizing process and pulse oxidizes method.
Compared with prior art, outstanding advantages of the present invention is that processing method is simple and easy to do, need not special installation: and anode oxidation method prepares TiO
2The time anode opposite, only need TiO
2Change negative electrode into, namely oppositely making alive is processed certain hour and can be significantly improved TiO
2The electrode electro Chemical performance.Due to H in electric field driven solution
+Ion is directly at TiO
2Introduce doping and defective in electrode, greatly reduce TiO
2Energy gap, its chemical property and PhotoelectrocatalytiPerformance Performance and conductivity are improved significantly.This processing method can not destroyed TiO
2Original structure (as TiO
2Nanotube, nano-wire array), make TiO
2Electrode can be applied to energy storage field and photoelectrocatalysis field better to solve energy problem and problem of environmental pollution, simultaneously TiO
2Electrode also can be used as good electric conducting material and is applied to other field.
Description of drawings
Fig. 1 is the untreated TiO of embodiment 1 preparation
2The cyclic voltammetry curve of electrode.
Fig. 2 is the TiO that embodiment 1 processes through reverse making alive
2The cyclic voltammetry curve of electrode.
Fig. 3 is the untreated TiO of embodiment 1 preparation
2The AC impedance curve of electrode.
Fig. 4 is the TiO that embodiment 1 processes through reverse making alive
2The AC impedance curve of electrode.
Fig. 5 is the untreated TiO of embodiment 1 preparation
2The light-catalysed photoelectric current curve of electrode.
Fig. 6 is the TiO that embodiment 1 processes through reverse making alive
2The light-catalysed photoelectric current curve of electrode.
Embodiment
Further illustrate the present invention below by embodiment.
Embodiment 1
Adopt the constant voltage oxidizing process to prepare TiO
2Electrode: take titanium foil as work electrode, carbon-point carries out anodic oxidation in two electrode systems to electrode, and electrolyte is 0.5 wt % NH
4F and 2 vol % H
2The ethylene glycol solution of O.At first, with titanium foil in air 450
° C 20 min that anneal to eliminate structural stress, then use acetone, second alcohol and water ultrasonic cleaning titanium foil 10 min successively.An anodic oxidation is carried out 2 h with constant voltage 60 V, and then ultrasonic 30 min remove oxide-film, again clean successively with acetone, second alcohol and water the titanium foil that leaves pit.Carry out two-step anodization, oxidizing condition is identical with once oxidation again, takes out TiO after oxidation finishes
2Electrode is rinsed well with deionized water, oven dry.The amorphous state TiO for preparing
2Electrode is ordered nano-tube array structure, and the nanotube diameter is 40-60 nm, and thickness is about 12 μ m.With the TiO with the titanium substrate for preparing
2Electrode is put into the tube annealing crystallization, annealing temperature 450
°C。Then, reverse making alive, i.e. crystalline state TiO to anneal
2Electrode is negative electrode, and carbon-point is two electrode systems of anode, is 0.5 M Na at electrolyte
2SO
4Neutral solution in carry out electrochemical reaction, two electrode spacing 2.5 cm, voltage 5 V and reaction time 30 s.
Fig. 1 and Fig. 2 are the TiO that is untreated and processes
2Electrode is swept the cyclic voltammetric that speed is 100 mV/s (CV) curve, as seen from the figure, and the TiO of processing
2Electrode has obvious current response at positive potential, and the area that the CV curve surrounds obviously increases.Fig. 3 and Fig. 4 are the TiO that is untreated and processes
2Electrode is at amplitude 10 mV, the ac impedance spectroscopy (EIS) of test frequency from 100 kHz to 0.1 Hz.The TiO that processes
2In electrode EIS curve, half radius of circle is very little, means very little electrode internal resistance and higher electrode conductivity.With 2 M Li
2SO
4Electrolyte, 0.05 mA/cm
2Current density is carried out charge-discharge test, and voltage range-0.3-0.6 V(Ag/AgCl is reference electrode), untreated TiO
2Electrode discharge is 0.98 mF/cm than electric capacity
2And the TiO that processes
2Electrode reaches 18.5 mF/cm than electric capacity
2Fig. 5 and Fig. 6 are the TiO that is untreated and processes
2The light-catalysed photoelectricity flow graph of electrode.Lower and AM is under the sunlight of 1.5 G at the ultraviolet light (UV) of wavelength 365 nm, untreated TiO
2Electrode photoelectric stream is about respectively 85 μ A and 106 μ A, and the photoelectric current of processing can reach respectively approximately 213 μ A and 225 μ A.
Embodiment 2
Adopt hydro thermal method to prepare TiO
2Electrode: under room temperature, isopropyl titanate is joined according to volume ratio 1:1 with isopropyl alcohol in the acetic acid of pH=2 and mix and stir, then 80
°Approximately l h and vigorous stirring of heating in the C oil bath, after solution is moved in autoclave, after sealing 250
°Place 12h under C.Last ultrasonic dispersion colloid solution is 120
°C heats certain hour, obtains the milky colloid, is applied on the electro-conductive glass that cleans up, and coated area is 1.2 cm
2, oven dry.Oppositely making alive technique is with embodiment 1.Test result shows, hydro thermal method prepares TiO
2The ratio electric capacity of electrode is 63 μ F/cm
2TiO after processing
2Electrode reaches 1.06 mF/cm than electric capacity
2Be that under the sunlight of 1.5 G, hydro thermal method prepares TiO with AM under the UV of wavelength 365 nm
2The photoelectric current of electrode is about respectively 15 μ A and 28 μ A; Photoelectric current after processing can reach respectively approximately 46 μ A and 59 μ A.
Embodiment 3
Adopt template synthesis TiO
2Electrode: template is for (to remove the barrier layer, aperture 60 nm, 20 microns of thickness, area 1.2 cm with the Woelm Alumina of aluminium substrate
2), adopt 0.1 M (NH
4)
2TiF
6Be presoma.To immerse with the Woelm Alumina of aluminium substrate in precursor solution, take out after reaction 1 h, rinse oven dry with deionized water well.Oppositely making alive technique is with embodiment 1.Test result shows, the TiO after processing
2Electrode is 5.89 mF/cm than electric capacity
2Be under the sunlight of 1.5 G with AM under the UV of wavelength 365 nm, its photoelectric current can reach respectively approximately 136 μ A and 163 μ A.
Embodiment 4
The constant voltage oxidizing process prepares TiO
2Electrode is identical with embodiment 1.The annealing in process condition is with embodiment 1.Oppositely making alive technique electrolyte used is 2 M Na
2SO
4Neutral solution, other reverse making alive condition is identical with embodiment 1.Test result shows, the TiO after processing
2Electrode is 20.8 mF/cm than electric capacity
2Be under the sunlight of 1.5 G with AM under the UV of wavelength 365 nm, its photoelectric current can reach respectively approximately 224 μ A and 256 μ A.
Embodiment 5
The constant voltage oxidizing process prepares TiO
2Electrode is identical with embodiment 1.The annealing in process condition is with embodiment 1.Oppositely making alive technique electrolyte used is the acid solution of 0.1 M HCl, and other reverse making alive condition is identical with embodiment 1.Test result shows, the TiO after processing
2Electrode is 15.7 mF/cm than electric capacity
2Be under the sunlight of 1.5 G with AM under the UV of wavelength 365 nm, its photoelectric current can reach respectively approximately 185 μ A and 212 μ A.
Embodiment 6
The constant voltage oxidizing process prepares TiO
2Electrode is identical with embodiment 1.The annealing in process condition is with embodiment 1.Oppositely making alive technique electrolyte used is the alkaline solution of 1 M KOH, and other reverse making alive condition is identical with embodiment 1.Test result shows, the TiO after processing
2Electrode is 18.94 mF/cm than electric capacity
2Be under the sunlight of 1.5 G with AM under the UV of wavelength 365 nm, its photoelectric current can reach respectively approximately 197 μ A and 208 μ A.
Embodiment 7
The constant voltage oxidizing process prepares TiO
2Electrode is identical with embodiment 1.The annealing in process condition is with embodiment 1.Oppositely two electrode spacings in the making alive process are 0.5cm, and applying voltage is 2V, and other reverse making alive process conditions are identical with embodiment 1.Test result shows, the TiO after processing
2Electrode is 4.3 mF/cm than electric capacity
2Be under the sunlight of 1.5 G with AM under the UV of wavelength 365 nm, its photoelectric current can reach respectively approximately 124 μ A and 147 μ A.
Embodiment 8
The constant voltage oxidizing process prepares TiO
2Electrode is identical with embodiment 1.The annealing in process condition is with embodiment 1.Oppositely two electrode spacings in the making alive process are 10cm, and the reaction time is 360 s, and other reverse making alive process conditions are identical with embodiment 1.Test result shows, the TiO after processing
2Electrode is 12.8 mF/cm than electric capacity
2Be under the sunlight of 1.5 G with AM under the UV of wavelength 365 nm, its photoelectric current can reach respectively approximately 164 μ A and 183 μ A.
Embodiment 9
The constant voltage oxidizing process prepares TiO
2Electrode is identical with embodiment 1.The annealing in process condition is with embodiment 1.Oppositely the voltage in the making alive process is 10V, and the reaction time is 5s, and other reverse making alive process conditions are identical with embodiment 1.Test result shows, the TiO after processing
2Electrode is 9.63 mF/cm than electric capacity
2Be under the sunlight of 1.5 G with AM under the UV of wavelength 365 nm, its photoelectric current can reach respectively approximately 152 μ A and 182 μ A.
Embodiment 10
The standby TiO of pulse oxidizes legal system
2The electrolyte of electrode is consistent with embodiment 1 with the pretreating process of titanium foil.Oxidizing process imposes 60V voltage, stops 10s after every oxidation 10s, and total time is 4h.Annealing in process and reverse making alive technique are with embodiment 1.Test result shows, the TiO after processing
2Electrode is 23.5 mF/cm than electric capacity
2Be under the sunlight of 1.5 G with AM under the UV of wavelength 365 nm, its photoelectric current can reach respectively approximately 239 μ A and 251 μ A.
Claims (5)
1. one kind strengthens TiO
2The method of electrode electro Chemical performance is characterized in that TiO
2Electrode carries out reverse making alive to be processed: namely at the TiO with crystalline state
2Electrode is negative electrode, and carbon-point is in two electrode systems of anode, and concentration of electrolyte is 0.1-2 M, carries out electrochemical reaction under normal temperature and processes, and between two electrodes, spacing is 0.5-10 cm, to apply voltage be that 2-10 V and reacting treatment time are 5-360 s.
2. enhancing TiO according to claim 1
2The method of electrode electro Chemical performance is characterized in that described electrolyte is neutrality, acidity or alkaline solution.
3. enhancing TiO according to claim 2
2The method of electrode electro Chemical performance is characterized in that described electrolyte particular certain cancers, sylvite, ammonium salt, hydrochloric acid, sulfuric acid, phosphoric acid, NaOH or potassium hydroxide solution.
4. enhancing TiO according to claim 1
2The method of electrode electro Chemical performance is characterized in that described TiO
2Electrode adopts anode oxidation method, hydro thermal method, template, sol-gal process, microemulsion method or vapour deposition process preparation.
5. enhancing TiO according to claim 4
2The method of electrode electro Chemical performance is characterized in that described anode oxidation method comprises constant voltage oxidizing process or pulse oxidizes method.
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| CN103590087A (en) * | 2013-10-16 | 2014-02-19 | 中国科学院合肥物质科学研究院 | TiO2 nanotube array film with periodically-changing inner aperture and adjustable period and preparation method thereof |
| CN103680978A (en) * | 2013-12-20 | 2014-03-26 | 南京理工大学 | High-specific-volume low-voltage aluminum electrolytic capacitor and manufacturing method thereof |
| CN103924279A (en) * | 2014-04-10 | 2014-07-16 | 北京工业大学 | Method for preparing highly ordered titanium dioxide nanotube array thin film by pulse anodic oxidation |
| CN104658768A (en) * | 2014-12-11 | 2015-05-27 | 湖北大学 | Preparation method of titanic oxide and supercapacitor of titanic oxide |
| CN105448539A (en) * | 2014-08-20 | 2016-03-30 | 南京理工大学 | Method for increase capacitance of TiO2 electrode |
| CN108648927A (en) * | 2018-04-28 | 2018-10-12 | 南京理工大学 | A kind of electrode of super capacitor and preparation method thereof based on titanium oxide nanotubes |
| CN110344097A (en) * | 2019-07-26 | 2019-10-18 | 南京理工大学 | A method of preparing anodic titanium nano flower electrode |
| CN113774426A (en) * | 2021-10-20 | 2021-12-10 | 中国科学技术大学 | Electrocatalyst and preparation method thereof |
| CN114427112A (en) * | 2022-01-27 | 2022-05-03 | 中国人民解放军陆军工程大学 | Method for preparing multi-color photochromic Ag/TiO2 film |
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| CN103590087A (en) * | 2013-10-16 | 2014-02-19 | 中国科学院合肥物质科学研究院 | TiO2 nanotube array film with periodically-changing inner aperture and adjustable period and preparation method thereof |
| CN103590087B (en) * | 2013-10-16 | 2016-03-16 | 中国科学院合肥物质科学研究院 | Internal orifice dimension mechanical periodicity and cycle adjustable TiO 2nano-pipe array thin film and preparation method thereof |
| CN103680978A (en) * | 2013-12-20 | 2014-03-26 | 南京理工大学 | High-specific-volume low-voltage aluminum electrolytic capacitor and manufacturing method thereof |
| CN103680978B (en) * | 2013-12-20 | 2017-04-19 | 南京理工大学 | High-specific-volume low-voltage aluminum electrolytic capacitor and manufacturing method thereof |
| CN103924279B (en) * | 2014-04-10 | 2016-08-24 | 北京工业大学 | A kind of pulse anodic oxidation prepares method prepared by high-sequential titanium dioxide nano-pipe array thin film |
| CN103924279A (en) * | 2014-04-10 | 2014-07-16 | 北京工业大学 | Method for preparing highly ordered titanium dioxide nanotube array thin film by pulse anodic oxidation |
| CN105448539B (en) * | 2014-08-20 | 2017-11-14 | 南京理工大学 | One kind improves TiO2The method of electrode capacitance |
| CN105448539A (en) * | 2014-08-20 | 2016-03-30 | 南京理工大学 | Method for increase capacitance of TiO2 electrode |
| CN104658768A (en) * | 2014-12-11 | 2015-05-27 | 湖北大学 | Preparation method of titanic oxide and supercapacitor of titanic oxide |
| CN104658768B (en) * | 2014-12-11 | 2017-12-22 | 湖北大学 | The preparation method and its ultracapacitor of titanium oxide |
| CN108648927A (en) * | 2018-04-28 | 2018-10-12 | 南京理工大学 | A kind of electrode of super capacitor and preparation method thereof based on titanium oxide nanotubes |
| CN108648927B (en) * | 2018-04-28 | 2020-02-14 | 南京理工大学 | Titanium oxide nanotube-based supercapacitor electrode and preparation method thereof |
| CN110344097A (en) * | 2019-07-26 | 2019-10-18 | 南京理工大学 | A method of preparing anodic titanium nano flower electrode |
| CN110344097B (en) * | 2019-07-26 | 2021-04-27 | 南京理工大学 | Method for preparing anodic titanium oxide nanoflower electrode |
| CN113774426A (en) * | 2021-10-20 | 2021-12-10 | 中国科学技术大学 | Electrocatalyst and preparation method thereof |
| CN113774426B (en) * | 2021-10-20 | 2023-03-10 | 中国科学技术大学 | Electrocatalyst and preparation method thereof |
| CN114427112A (en) * | 2022-01-27 | 2022-05-03 | 中国人民解放军陆军工程大学 | Method for preparing multi-color photochromic Ag/TiO2 film |
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