CN101871117A - CuxSe/TiO2 nanotube array of p-type semiconductor nano material and preparation method thereof - Google Patents
CuxSe/TiO2 nanotube array of p-type semiconductor nano material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a CuxSe/TiO2 nanotube array of a p-type semiconductor nano material and a preparation method thereof. The method comprises the following steps: putting a TiO2 nanotube array in 5mmol-20mmol of CuSO4 solution; electrodepositing elementary substance Cu on the TiO2 nanotube array by adopting pulse plating in a standard three-electrode system to obtain a Cu/TiO2 compound nanotube array; carrying out electrooxidation in an NaOH alkaline solution for a certain time after deposition is ended to obtain a superfine Cu2O nanowire-modifying TiO2 nanotube array; and then putting the Cu2O/TiO2 nanotube array in a selenium ion solution, and stirring for 30-60 min under light to obtain a copper selenide nanotube array. Based on the superfine Cu2O nanowire-modifying TiO2 nanotube array, the absorption range of TiO2 in a visible light area can be effectively expanded and the compounding probability of an electron hole pair can be reduced, and more photoelectrons and photoholes can be generated under visible light, thereby being more beneficial to Cu2O to react with the selenium ion solution to generate copper selenide. The CuxSe/TiO2 nano material with a novel structure has potential application in the aspects of solar batteries, solar radiation absorbers, nano switches, thermoelectric photoelectric converters, superconductors, air-sensitive sensors and the like.
Description
Technical field
The invention belongs to the nano material chemical field, the p-N-type semiconductorN nano material Cu that is specifically related to a kind of novelty, has outstanding photoelectric properties
xSe/TiO
2Nano-tube array and preparation method thereof.
Background technology
Anonizing prepares Nano tube array of titanium dioxide, and it is big to have specific surface area, and the aperture the is adjustable good characteristic of Denging, the nano tubular structure that it is special has become the research focus of various countries' scientific domain.Anonizing prepares the common inorganic aqueous solution system of electrolytic solution of Nano tube array of titanium dioxide, because various ions travelling speed in the aqueous solution is very fast relatively, the speed of electrochemical anodic oxidation is also quick, can form nano-tube array in the relatively shorter time.But the anodic oxidation voltage that applies generally can only be in the scope of 10～25V, exceed this voltage range and just can not form nano tubular structure, this has limited the caliber of nanotube simultaneously to a certain extent, and the nanotube tube wall for preparing in water solution system is thinner, and is damaged easily.200410021589.X disclose a kind of preparation method of high length-diameter ratio titania nanometer tube array, the solute of its electrolytic solution is fluorochemical and supporting electrolyte, solvent is a water, and add the alcohols additive, and electrolysis under 3～50V voltage conditions, this nanotube pipe is still shorter, have only 250 nanometers long, specific surface area is big inadequately, and can only absorb the light of ultraviolet region, can not make full use of the nature sunlight.Application number is 200910229191.8 invention, adopts the sedimentary method of alternating-current to prepare one dimension Cu
2O/TiO
2The nucleocapsid structure array film, this method has effectively been controlled Cu
2The O particle is at TiO
2Position in the nanotube.And use electro-deposition techniques among the present invention elemental copper is deposited to TiO
2On the nano-tube array, in conjunction with the electrooxidation technology, in basic solution, elemental copper is oxidized to Cu again
2The O nano thread is to make up Cu
2O/TiO
2The heterojunction nano-tube array has obtained the ultra-fine Cu of diameter less than 5nm first
2The TiO that O nanometer silk screen is modified
2Nano-tube array.These nano threads are intertwined and connected mutually and form network structure attached to TiO
2On the nano-tube array, but do not stop up TiO fully
2Nanotube; And enlarged markedly the specific surface area and the adsorptive power of photocatalyst, widened its absorption region at visible region.On this basis, we are again first under illumination condition, with Cu
2O/TiO
2Be substrate,, obtain the copper selenide nanometer flower structure of 3-d modelling with the plasma selenium solution reaction.
Summary of the invention
The object of the present invention is to provide a kind of adsorptive power and electronic conduction ability that can further strengthen Nano tube array of titanium dioxide, widen its absorption region, improve the Cu of its photoelectric transformation efficiency at visible region
xSe/TiO
2The p-N-type semiconductorN nano material novelty of nano-tube array, that have outstanding photoelectric properties and preparation method thereof.
The objective of the invention is to realize in the following manner:
A kind of p-N-type semiconductorN nano material-Cu
xSe/TiO
2Nano-tube array and preparation method thereof may further comprise the steps:
(1) under 25～100V volts DS, be anode with pure titanium or titanium alloy, platinized platinum is a negative electrode, electrolytic preparation titania nanotube in electrolytic solution; Under 400 ℃ of-500 ℃ of aerobic conditions,, make its crystallization become TiO with the Nano tube array of titanium dioxide calcining 4-6h of preparation
2Nano-tube array;
(2) with the TiO of 2cm * 5cm
2Nano-tube array is put 5mmol-20mmolCuSO
4In the solution, adopting the method for pulse plating is being counter electrode with the platinized platinum, and Ag/AgCl is a reference electrode, and the TiO2 nano-tube array is a galvanic deposit elemental copper in the standard three-electrode system of working electrode, and make-and-break voltage is than being-1v :-0.00001v; Make-and-break time ratio is 0.2: 1, obtains Cu/TiO
2The composite nano tube array;
(3) Cu/TiO that adopts step (2) to obtain
2The composite nano tube array is an anode, and platinized platinum is two electrode systems of negative electrode, and interelectrode distance 2cm, voltage are 0.5V, under the no agitation condition in the NaOH of 0.5M-2M basic solution electrooxidation 30min, obtain ultra-fine Cu
2The TiO that the O nano wire is modified
2Nano-tube array.
(4) 0.015g-0.030g Se powder and 18-12gNaOH are put into the beaker of 50ml and added 40ml distilled water, then beaker is placed on continuous heated and stirred on the magnetic stirring apparatus, be made into plasma selenium solution; With the Cu that 2cm * 5cm step (3) obtains
2O/TiO
2Nano-tube array is put into plasma selenium solution, and 30min-60min is stirred in illumination, obtains the Nano tube array of titanium dioxide that copper selenide is modified.
Described electrolytic solution is that the dimethyl sulfoxide (DMSO) or the quality percentage composition of the hydrofluoric acid of 0.5-3% is the NH of 0.25-0.5% by the quality percentage composition
4The alcoholic solution of F is formed.
The present invention is at the TiO based on the preparation of application anonizing
2On it is big that nano-tube array has specific surface area, and the aperture the is adjustable good characteristic of Denging, the method by pulse plating is deposited on TiO with elemental copper
2The nanotube inwall all is oxidized to the ultra-fine Cu of diameter less than 5 nanometers by anodised method with elemental copper again
2O nano wire, these nano threads are intertwined and connected mutually and form network structure attached to TiO
2On the nano-tube array, but do not stop up TiO fully
2Nanotube.This net structure will be very beneficial for the transmission of photo-generated carrier, and has reduced electron-hole pair compound probability.On the basis of this excellent material, the present invention adopts the method for illumination to prepare the copper selenide nanometer flower structure again.Cu
2TiO after the O nano wire is modified
2The nanotube battle array can produce more light induced electron and photohole under visible light light, so more help Cu
2O and plasma selenium solution generation redox reaction generate copper selenide.
3Se+6NaOH→Na
2Se+Na
2SeO
3+H
2O
2(2-X)Cu
2O+4Na
2Se+H
2O+O
2→4Cu
2-xSe+8NaOH
The Cu of conventional art preparation
2O/TiO
2The nanotube battle array is compared, the Cu that the present invention forms
2O/TiO
2The nanotube battle array has huge specific surface area, more helps Cu
2The O nano wire contacts with plasma selenium solution, has accelerated speed of reaction; So just can form copper selenide nanometer flower, see illustrated in figures 1 and 2 with this novel structure.In addition, as important p-N-type semiconductorN material, the Cu of this novel structure
xSe/TiO
2Nano material is at solar cell, the solar radiative absorption device, and nanotube switch, thermoelectric photoelectric commutator, superconductor, there is potential application in aspects such as gas sensor.
Description of drawings
Fig. 1 is the Cu of low power
xThe TiO that Se modifies
2The scanning electron microscope diagram of nano-tube array;
Fig. 2 is the Cu of high power
xThe TiO that Se modifies
2The scanning electron microscope diagram of nano-tube array;
Fig. 3 is Cu
xSe/TiO
2The EDS energy spectrogram of nano-tube array illustrates and contains selenium element and copper;
Fig. 4 modifies TiO for CuSe
2The XRD figure of nano-tube array, explanation are the CuSe crystal;
The TiO that Fig. 5 modifies for CuSe
2The TiO of NTs and unmodified
2Nano-tube array I-V graphic representation, CuSe/TiO
2The saturation photocurrent of NTs is than the TiO of unmodified
2The saturated photogenerated current of nano-tube array is significantly improved, and after having modified CuSe, TiO
2The zero current voltage of nano-tube array has moved on to-0.81 from-0.68V is negative, proves that further material after CuSe modifies can the accelerated material light induced electron and the separating of photohole, and suppresses the compound of light induced electron and photohole;
The TiO that Fig. 6 modifies for CuSe
2The TiO of NTs and unmodified
2Nano-tube array photocurrent response figure, decorations back TiO as seen from the figure
2The photoelectric current of nano-tube array is unmodified TiO
29 times of the resultant photoelectric current of nano-tube array illustrate that the material after modifying has better photovoltaic effect.
Embodiment
Further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
(1) with the substrate material surface polishing, clean up standby;
(2) preparation electrolytic solution: electrolytic solution is that the hydrofluoric acid of 0.5-3% and dimethyl sulfoxide (DMSO) or NH4F quality percentage composition are that the alcoholic solution of 0.25-0.5% is formed by HF quality percentage composition;
(3) under 25～100V volts DS, be anode with pure titanium or titanium alloy, platinized platinum is a negative electrode, electrolytic preparation titanium oxide nanotubes in electrolytic solution;
(4) under 400 ℃ of-500 ℃ of aerobic conditions, the titania nanotube array of above preparation is calcined 4-6h, make its crystallization become TiO
2Nano-tube array;
(5) Cu/TiO that adopts step (4) to obtain
2The composite nano tube array is an anode, and platinized platinum is two electrode systems of negative electrode, and interelectrode distance 2cm, voltage are 0.5V, under the no agitation condition in the NaOH of 0.5M-2M basic solution electrooxidation 30min, obtain ultra-fine Cu
2The TiO that rice noodles are modified in the O
2Nano-tube array;
(6) Cu
xSe/TiO
2The preparation of nano-tube array
1. prepare plasma selenium solution: 0.015g-0.030g Se powder and 18-12gNaOH are put into the beaker of 50ml and added 40ml distilled water, then beaker is placed on continuous heated and stirred on the magnetic stirring apparatus, be made into plasma selenium solution.
2. the Cu that step (5) is obtained
2O/TiO
2Nano-tube array is put into plasma selenium solution, and 30min-60min is stirred in illumination, obtains copper selenide nanometer flower.Test result is seen Fig. 5 and 6.
Claims (3)
1. p N-type semiconductorN nano material Cu
xSe/TiO
2Nano-tube array and preparation method thereof is characterized in that, may further comprise the steps:
(1) under 25～100V volts DS, be anode with pure titanium or titanium alloy, platinized platinum is a negative electrode, electrolytic preparation titania nanotube in electrolytic solution; Under 400 ℃ of-500 ℃ of aerobic conditions,, make its crystallization become TiO with the Nano tube array of titanium dioxide calcining 4-6h of preparation
2Nano-tube array;
(2) with the TiO of 2cm * 5cm
2Nano-tube array is put 5mmol-20mmolCuSO
4In the solution, adopting the method for pulse plating is being counter electrode with the platinized platinum, and Ag/AgCl is a reference electrode, and the TiO2 nano-tube array is a galvanic deposit elemental copper in the standard three-electrode system of working electrode, and make-and-break voltage is than being-1v :-0.00001v; Make-and-break time ratio is 0.2: 1, obtains Cu/TiO
2The composite nano tube array;
(3) Cu/TiO that adopts step (2) to obtain
2The composite nano tube array is an anode, and platinized platinum is two electrode systems of negative electrode, and interelectrode distance 2cm, voltage are 0.5V, under the no agitation condition in the NaOH of 0.5M-2M basic solution electrooxidation 30min, obtain ultra-fine Cu
2The TiO that the O nano wire is modified
2Nano-tube array.
(4) 0.015g-0.030g Se powder and 18-12gNaOH are put into the beaker of 50ml and added 40ml distilled water, then beaker is placed on continuous heated and stirred on the magnetic stirring apparatus, be made into plasma selenium solution; With the Cu that 2cm * 5cm step (3) obtains
2O/TiO
2Nano-tube array is put into plasma selenium solution, and 30min-60min is stirred in illumination, obtains the Nano tube array of titanium dioxide that copper selenide is modified.
2. p N-type semiconductorN nano material Cu according to claim 1
xSe/TiO
2The preparation method of nano-tube array is characterized in that, described electrolytic solution is that the dimethyl sulfoxide (DMSO) or the quality percentage composition of the hydrofluoric acid of 0.5-3% is the NH of 0.25-0.5% by the quality percentage composition
4The alcoholic solution of F is formed.
3. p N-type semiconductorN nano material Cu
xSe/TiO
2Nano-tube array is characterized in that, is the Cu that is prepared by the described method of claim 1
xSe/TiO
2Nano-tube array.
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Cited By (13)
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| CN102544182A (en) * | 2012-01-05 | 2012-07-04 | 西北工业大学 | Surface plasmon resonance rectenna and preparation method therefor |
| CN102965710A (en) * | 2012-11-13 | 2013-03-13 | 同济大学 | Preparation of silver/cadmium sulfide-nanoparticle-comodified titanium dioxide nanotube array |
| CN103391025A (en) * | 2012-05-09 | 2013-11-13 | 中国人民解放军军械工程学院 | Multi-physical-field nanometer generator |
| CN103646989A (en) * | 2013-11-27 | 2014-03-19 | 华东师范大学 | Preparation method of p-n type Cu2O/TiO2 nanowire array composite film |
| CN103774233A (en) * | 2014-01-10 | 2014-05-07 | 陕西师范大学 | Method for preparing Cu2Se single-crystal nanowire of exposing high-energy (III) cubic crystal structure |
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| CN102544182A (en) * | 2012-01-05 | 2012-07-04 | 西北工业大学 | Surface plasmon resonance rectenna and preparation method therefor |
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| CN103879974A (en) * | 2014-04-17 | 2014-06-25 | 哈尔滨工业大学 | Method for preparing copper selenide nanowires by microwave-assisted method |
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