CN102468361B - Method for manufacturing photoelectrocatalysis double-function electrode with wide wave range response - Google Patents
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Abstract
The invention relates to a method for manufacturing a photoelectrocatalysis double-function electrode with wide wave range response. The method comprises the following steps of: loading CdS on a TiO2 nano tube (TiO2 NTs) which is vertically grown on a metal titanium substrate and used as a carrier to achieve good photocatalysis performance in a visible light range, loading an antimony-doped SnO2 coating on one side of TiO2 NTs/CdS to achieve good electrocatalysis performance, and constructing to obtain a CdS/TiO2 NTs/SnO2 double-function electrode with a microstructure. Compared with the prior art, the invention has the advantages that the electrode has the excellent photocatalysis performance in an ultraviolet-visible light wide wave range and excellent electrocatalysis performance, and can treat environmental pollutant efficiently and stably.
Description
Technical field
The present invention relates to materials chemistry field, especially relate to a kind of preparation method with the photoelectrocatalysis bifunctional electrodes of wide ripple range response.
Background technology
In recent years, along with rapid development of economy, a large amount of environmental problems that occur have structure of matter complexity and the feature large to life entity toxic action.Photochemical oxidation technology and electrochemical oxidation technology are because the two can both produce the OH free radical of strong oxidizing property by different approach, it has the features such as oxidability is strong, controllability is high, reaction condition is gentle, and becomes the advanced oxidation treatment technology of processing environment problem.Therefore, these two kinds of technical advantage complementations, organic assembling are integral, give full play to advantage separately, obtain the effect of " 1+1 > 2 ", significant.
In numerous semiconductor light-catalysts, TiO
2high with its photocatalytic activity, oxidability is strong, nontoxic, cost is low and gain great popularity, and is current most popular photochemical catalyst.But TiO
2band structure determined that photocatalysis technology exists limitation in extension process.Its greater band gap, spectral response range narrow (Eg=3.2eV), can only utilize the ultraviolet region that accounts for less than 5% in sunlight.Utilize efficiently natural energy resources-solar energy to solve environmental energy problem, the photochemical catalyst that seek environmental friendliness, has a superperformance is the inexorable trend that application is moved towards in photocatalysis basic research.
By at TiO
2in the compound narrow gap semiconductor method of widening photochemical catalyst light absorption bands of a spectrum be TiO
2a kind of important means of Visible-light Irradiation, its concrete principle can be summarized as different can level semiconductors between the transporting with separated of photo-generated carrier.In numerous compound systems, TiO
2the research of-CdS system is paid close attention to the most.CdS is a kind of narrow bandgap semiconductor material (Eg=2.4eV), and in some recent research work, people attempt CdS nanoparticle deposition at TiO
2film surface, during illumination, the electron transfer being stimulated on CdS is to TiO
2conduction band on, the valence band of CdS is still stayed in hole, it is effectively separated that light induced electron and hole obtain, and the absorbing wavelength of system is widened to visual field.But because this CdS nano particle is at TiO
2dispersion on film is even not, and is difficult to obtain comparatively ideal photocatalytic activity.Compare TiO with common film
2nanotube is due to the special construction of its high-sequential, array arrangement, and have larger specific area, surface can, adsorption capacity and avtive spot.Select TiO
2nanotube is carrier, and Chemical assembly CdS nano particle in pipe can further improve the photocatalysis performance of catalyst.
Meanwhile, mix the SnO of antimony
2be a kind of good eelctro-catalyst, its oxygen evolution potential is high, the toxicity intermediate product that degradation process produces can by very soon, catalytic oxidation thoroughly, be a kind of efficient anode material, be suitable for the By Electro-catalytic Oxidation Process of organic pollution.Just based on above-mentioned to titania nanotube and SnO
2the characteristic understanding of electrode, this patent proposes a kind of like this thinking, and by catalytic oxidation and two kinds of senior oxidation technology combinations of photochemical catalytic oxidation, organic assembling is integral, and can realize the photoelectric-synergetic effect in same course of reaction.
Summary of the invention
Object of the present invention is exactly to provide a kind of preparation method simultaneously with photoelectrocatalysis bifunctional electrodes in order to overcome the defect of above-mentioned prior art existence within the scope of wide ripple.
Object of the present invention can be achieved through the following technical solutions:
A preparation method with the photoelectrocatalysis bifunctional electrodes of wide ripple range response, with the TiO of vertical growth in metallic titanium matrix
2nanotube is carrier, in nanotube, the CdS-loaded sensitizer of one side is widened photochemical catalyst in the absorption band of visibility region, at another side tin supported antimony colloidal sol, obtain good electrocatalysis characteristic, finally construct and obtain thering is the CdS/TiO that the wide ripple scope of ultraviolet-visible absorbs
2nTs/SnO
2bifunctional electrodes.
Specifically comprise the following steps:
(1) prepare respectively CdCl
2and Na
2the S precursor aqueous solution, and add surfactant;
(2) with titanium base TiO
2nanotube is carrier, utilizes vacuum impregnation and method of chemical immersion at TiO
2in nanotube, inject successively CdCl
2and Na
2s solution, in two kinds of solution, circulation is flooded respectively afterwards, can obtain having the TiO of microstructure
2nTs/CdS;
(3) by SnCl
4.5H
2o is dissolved in the absolute ethyl alcohol that contains concentrated hydrochloric acid, and magnetic agitation, to settled solution, adds SbCl in whipping process
3, after fully stirring, lucifuge is placed precipitation 8-24h, obtains tin antimony colloidal sol, then at TiO
2the wherein one side tin coating antimony colloidal sol of NTs/CdS, dries and repeats 3-5 time for 40-60 ℃ after applying, and obtains having the CdS/TiO of microstructure
2nTs/SnO
2;
(4) CdS/TiO step (3) being prepared
2nTs/SnO
2heat-treat, obtain having photoelectrocatalysis bifunctional electrodes.
CdCl in described step (1)
2the concentration of the precursor aqueous solution is 0.01mol/L-0.1mol/L, Na
2the concentration of the S precursor aqueous solution is 0.01mol/L-0.1mol/L, and surfactant is trisiloxanes, and addition is overall solution volume 0.5 ‰-1 ‰.
TiO in described step (2)
2nanotube diameter is 50nm-100nm, and thickness is 1 μ m-2 μ m.
In described step (2) with vacuum impregnation and and method of chemical immersion load step: at TiO
2in nanotube, fill CdCl
2and Na
2the S precursor aqueous solution, repeats 3-5 time, then by TiO
2nanotube is immersed in respectively CdCl
2and Na
2in the S precursor aqueous solution, each dip time is 20-50s, after each taking-up, surface solution is wiped away dry, this process that circulates 10-20 time.
In described step (2), vacuum impregnation refers to and utilizes vacuum pump to TiO
2nanotube vacuumizes, and makes to manage interior vacuum degree and reaches 0.09Mpa, CdCl
2and Na
2the S precursor aqueous solution is under ambient pressure in ascending pipe.
In described step (3), concentrated hydrochloric acid is that concentration is the hydrochloric acid of 37.5wt%, and the volume ratio of concentrated hydrochloric acid and absolute ethyl alcohol is 1: 10, SnCl
45H
2the concentration of O is 0.25mol/L～0.5mol/L, SnCl in the tin antimony colloidal sol obtaining
45H
2o and SbCl
3mass ratio be 10～20: 1.
In described step (4), heat treatment adopts nitrogen atmosphere, and controlling heating rate is 1～2 ℃/min, and treatment temperature is risen to 400 ℃-600 ℃, and after heat treatment 1-3h, controlling rate of temperature fall is 1～2 ℃/min, is down to room temperature.
Described bifunctional electrodes can respond the light in ultraviolet light and visible wavelength range.
Compared with prior art, operation principle of the present invention is semi-conductively can be with matching principle, simultaneously in conjunction with novel effectively microstructure design, the CdS/TiO finally obtaining by photoelectric-synergetic effect
2nTs/SnO
2bifunctional electrodes, not only has the photoresponse in the wide ripple scope of ultraviolet-visible, also has efficient, stable electrocatalysis characteristic, adopts this narrow bandgap semiconductor material of CdS (Eg=2.4eV) to carry out sensitization TiO as sensitizer
2, during illumination, the electron transfer being stimulated on CdS is to TiO
2conduction band on, the valence band of CdS is still stayed in hole, it is effectively separated that light induced electron and hole obtain, and the absorbing wavelength of system is widened to visual field.Selection has the more TiO of bigger serface
2nanotube is carrier, and Chemical assembly CdS nano particle in pipe is conducive to further improve the photocatalysis performance of catalyst; On the other hand, mix the SnO of antimony
2be a kind of good eelctro-catalyst, its oxygen evolution potential is high, strong to the degradation capability of organic pollution.By at TiO
2the one side load of NTs/CdS has the SnO of good electrical catalytic performance
2layer, the CdS/TiO finally obtaining
2nTs/SnO
2bifunctional electrodes, not only has the photoresponse of wide ripple scope, also has efficient, stable electrocatalysis characteristic, specifically comprises following advantage:
(1) CdS/TiO that the present invention prepares
2nTs/SnO
2electrode, one side is within the scope of the wide ripple of ultraviolet-visible, to have the CdS material of excellent photocatalytic activity, another side is to have excellent conductivity and the SnO of electro catalytic activity
2material, it is difunctional that electrode integral has possessed optical, electrical catalysis, in degradation of contaminant is processed, can carry out photoelectrocatalysioxidization oxidization simultaneously, has photoelectric-synergetic effect.
(2) to have adopted the orderly Nano tube array of titanium dioxide standing on Titanium base be carrier in the present invention, Chemical assembly semiconductor sensitizer in pipe.This nano-tube array high-sequential, physical and chemical performance is stable, and very large specific area and free space can be provided.Its porous pipe type structure has good dispersive property and template effect for photosensitizer, is more conducive to improve photocatalytic activity, and titania nanotube has guaranteed the highlight catalytic active of system at ultraviolet region.
(3) the present invention has adopted CdS to carry out sensitization TiO as sensitizer
2, to widen photochemical catalyst in the absorption band of visibility region.Because CdS is a kind of narrow bandgap semiconductor material (Eg=2.5eV), when irradiating the excitation energy of light, be not enough to excite TiO
2when in time, but can excite CdS, due to TiO
2conduction band higher than the current potential of CdS, make the electronics being stimulated on CdS more easily move to TiO
2conduction band on, excite the hole of generation still to stay in the valence band of CdS, it is effectively separated that light induced electron and hole obtain, and the absorbing wavelength of system is widened to visual field.
(4) the present invention has adopted the SnO that mixes antimony
2as eelctro-catalyst, its oxygen evolution potential is high, the toxicity intermediate product that degradation process produces can by very soon, catalytic oxidation thoroughly, be a kind of efficient anode material, be suitable for the By Electro-catalytic Oxidation Process of organic pollution.By at TiO
2the one side of NTs/CdS is constructed SnO
2layer can be brought into play the advantage separately of bi-material simultaneously, reaches the optoelectronic integration effect of " 1+1 > 2 ".
Accompanying drawing explanation
Fig. 1 is the upright stereoscan photograph of Nano tube array of titanium dioxide in order of carrier titanium base that the present invention adopts;
Fig. 2 is the TiO that embodiment 1 prepares
2the stereoscan photograph of NTs/CdS;
Fig. 3 is the CdS/TiO that embodiment 1 prepares
2nTs/SnO
2load has SnO
2the stereoscan photograph of coating.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Preparation 0.01mol/L CdCl
2with 0.01mol/L Na
2the precursor solution of S, adds trisiloxane surfactant wherein, and addition is overall solution volume 0.5 ‰.Adopting vacuum impregnation, is 50nm at diameter, and thickness is the TiO of 1 μ m
2in nanotube, fill 0.05mol/L CdCl
2with 0.05mol/L Na
2s precursor solution, repeats after 3 times, and nanotube is immersed in respectively in two kinds of solution, and each dip time is 30s, after each taking-up, surface solution is wiped away dry, this process that circulates 15 times.
By 10gSnCl
45H
2o is dissolved in the 50mL absolute ethyl alcohol that contains 5mL concentrated hydrochloric acid, is stirred well to clarification, then adds 0.5g SbCl
3, be stirred well to clarification, place lucifuge place precipitation 8 hours, obtain SnCl
45H
2o and SbCl
3the mass ratio tin antimony colloidal sol that is 20: 1.At TiO
2the wherein one side tin coating antimony colloidal sol of NTs/CdS, repetitive coatings after drying, totally 5 times, after being dried, being put in 500 ℃ of heat treatment times in Muffle furnace is 3h.
Fig. 1 and Fig. 2 are respectively the TiO selecting in embodiment 1
2nano-tube support and the TiO preparing according to embodiment 1 condition
2nTs/CdS photochemical catalyst shape appearance figure can be found out TiO from Fig. 1
2nano-tube array is closely arranged, and pore-size distribution is compared with homogeneous, and average caliber is about 60nm; After finding out in Fig. 2 that CdS nano particle is in filling full nanotube completely, at nanotube oral thermometer face, mutually pile up formation film.Fig. 3 is the CdS/TiO preparing
2nTs/SnO
2photochemical catalyst SnO
2the stereoscan photograph of coating, as can be seen from Figure 3: SnO
2at TiO
2nTs/CdS surface forms the fine and close and uniform rete of one deck.
Embodiment 2
Preparation 0.05mol/L CdCl
2with 0.05mol/L Na
2the precursor solution of S, adds trisiloxane surfactant wherein, and addition is overall solution volume 0.8 ‰.Adopting vacuum impregnation, is 60nm at diameter, and thickness is the TiO of 1 μ m
2two kinds of precursor solution of load respectively in nanotube, repeat after 3 times, and nanotube is immersed in respectively in two kinds of solution, and each dip time is 30s, after each taking-up, surface solution is wiped away dry, this process that circulates 15 times.
By 7.5gSnCl
45H
2o is dissolved in the 75mL absolute ethyl alcohol that contains 7.5mL concentrated hydrochloric acid, is stirred well to clarification, then adds 0.5g SbCl
3, be stirred well to clarification, place lucifuge place precipitation 12 hours, obtain SnCl
45H
2o and SbCl
3the mass ratio tin antimony colloidal sol that is 15: 1.At TiO
2the wherein one side tin coating antimony colloidal sol of NTs/CdS, repetitive coatings after drying, totally 3 times, after being dried, being put in 500 ℃ of heat treatment times in Muffle furnace is 2h.
Embodiment 3
Preparation 0.05mol/L CdCl
2with 0.05mol/L Na
2the precursor solution of S, adds trisiloxane surfactant wherein, and addition is overall solution volume 1 ‰.Adopting vacuum impregnation, is 80nm at diameter, and thickness is the TiO of 2 μ m
2two kinds of precursor solution of load respectively in nanotube, repeat after 3 times, and nanotube is immersed in respectively in two kinds of solution, and each dip time is 30s, after each taking-up, surface solution is wiped away dry, this process that circulates 15 times.
By 5gSnCl
45H
2o is dissolved in the 100mL absolute ethyl alcohol that contains 10mL concentrated hydrochloric acid, is stirred well to clarification, then adds 0.5g SbCl
3, be stirred well to clarification, place lucifuge place precipitation 16 hours, obtain SnCl
45H
2o and SbCl
3the concentration ratio tin antimony colloidal sol that is 10: 1.At TiO
2the wherein one side tin coating antimony colloidal sol of NTs/CdS, repetitive coatings after drying, totally 5 times, after being dried, being put in 500 ℃ of heat treatment times in Muffle furnace is 3h.
Embodiment 4
A preparation method with photoelectrocatalysis bifunctional electrodes, with the TiO of vertical growth in metallic titanium matrix
2nanotube is carrier, and in nanotube, the CdS-loaded sensitizer of one side is widened photochemical catalyst in the absorption band of visibility region, at another side tin supported antimony colloidal sol, obtains good electrocatalysis characteristic, finally constructs the CdS/TiO that obtains having microstructure
2nTs/SnO
2bifunctional electrodes, specifically comprises the following steps:
(1) CdCl that compound concentration is 0.1mol/L respectively
2na with concentration 0.1mol/L
2the S precursor aqueous solution, and to add surfactant trisiloxanes, addition be overall solution volume 0.8 ‰;
(2) take diameter as 100nm, thickness is the titanium base TiO of 2 μ m
2nanotube is carrier, utilizes vacuum pump to TiO
2nanotube vacuumizes, and makes to manage interior vacuum degree and reaches 0.09Mpa, CdCl
2and Na
2the S precursor aqueous solution is under ambient pressure in ascending pipe, at TiO
2in nanotube, fill CdCl
2and Na
2the S precursor aqueous solution, repeats 20 times, then by TiO
2nanotube is immersed in respectively CdCl
2and Na
2in the S precursor aqueous solution, each dip time is 50s, after each taking-up, surface solution is wiped away dry, and this process that circulates 20 times, can obtain having the TiO of microstructure
2nTs/CdS;
(3) by 10g SnCl
45H
2it is that in the mixed solvent that is mixed with of the concentrated hydrochloric acid of 37.5wt% and the absolute ethyl alcohol of 100mL, magnetic agitation, to settled solution, adds the SbCl of 1g in whipping process that O is dissolved in 10mL concentration
3, after fully stirring, lucifuge is placed precipitation 24h, obtains SnCl
45H
2o and SbCl
3the mass ratio tin antimony colloidal sol that is 10: 1.At TiO
2the one side tin coating antimony colloidal sol of NTs/CdS, controls temperature and is 60 ℃ and dry and repetitive coatings 5 times, obtains having the CdS/TiO of microstructure
2nTs/SnO
2;
(4) CdS/TiO step (3) being prepared
2nTs/SnO
2heat-treat, under nitrogen atmosphere, controlling heating rate is 1 ℃/min, and treatment temperature is risen to 600 ℃, and after heat treatment 3h, controlling rate of temperature fall is 1 ℃/min, is down to room temperature and obtains having photoelectrocatalysis bifunctional electrodes.
Claims (7)
1. a preparation method with the photoelectrocatalysis bifunctional electrodes of wide ripple range response, is characterized in that, the method comprises the following steps:
(1) prepare respectively CdCl
2and Na
2the S precursor aqueous solution, and add surfactant;
(2) with titanium base TiO
2nanotube is carrier, utilizes vacuum impregnation and method of chemical immersion at TiO
2in nanotube, inject successively CdCl
2and Na
2s solution, in two kinds of solution, circulation is flooded respectively afterwards, can obtain having the TiO of microstructure
2nTs/CdS;
(3) by SnCl
45H
2o is dissolved in the absolute ethyl alcohol that contains concentrated hydrochloric acid, and magnetic agitation, to settled solution, adds SbCl in whipping process
3, after fully stirring, lucifuge is placed precipitation 8-24h, obtains tin antimony colloidal sol, then at TiO
2the wherein one side tin coating antimony colloidal sol of NTs/CdS, dries and repeats 3-5 time for 40-60 ℃ after applying, and obtains having the CdS/TiO of microstructure
2nTs/SnO
2;
(4) CdS/TiO step (3) being prepared
2nTs/SnO
2heat-treat, obtain having photoelectrocatalysis bifunctional electrodes.
2. a kind of preparation method with the photoelectrocatalysis bifunctional electrodes of wide ripple range response according to claim 1, is characterized in that, CdCl in described step (1)
2the concentration of the precursor aqueous solution is 0.01mol/L-0.1mol/L, Na
2the concentration of the S precursor aqueous solution is 0.01mol/L-0.1mol/L, and surfactant is trisiloxanes, and addition is overall solution volume 0.5 ‰-1 ‰.
3. a kind of preparation method with the photoelectrocatalysis bifunctional electrodes of wide ripple range response according to claim 1, is characterized in that, TiO in described step (2)
2nanotube diameter is 50nm-100nm, and thickness is 1 μ m-2 μ m.
4. a kind of preparation method with the photoelectrocatalysis bifunctional electrodes of wide ripple range response according to claim 1, is characterized in that, in described step (2), vacuum impregnation and method of chemical immersion comprise the following steps: at TiO
2in nanotube, fill CdCl
2and Na
2the S precursor aqueous solution, repeats 3-5 time, then by TiO
2nanotube is immersed in respectively CdCl
2and Na
2in the S precursor aqueous solution, each dip time is 20-50s, after each taking-up, surface solution is wiped away dry, this process that circulates 10-20 time.
5. according to a kind of preparation method with the photoelectrocatalysis bifunctional electrodes of wide ripple range response described in claim 1 or 4, it is characterized in that, in described step (2), vacuum impregnation refers to and utilizes vacuum pump to TiO
2nanotube vacuumizes, and makes to manage interior vacuum degree and reaches 0.09Mpa, CdCl
2and Na
2the S precursor aqueous solution is under ambient pressure in ascending pipe.
6. a kind of preparation method with the photoelectrocatalysis bifunctional electrodes of wide ripple range response according to claim 1, it is characterized in that, in described step (3), concentrated hydrochloric acid is the hydrochloric acid of concentration 37.5wt%, and the volume ratio of concentrated hydrochloric acid and absolute ethyl alcohol is 1 ︰ 10, SnCl
45H
2the concentration of O is 0.25mol/L～0.5mol/L, SnCl in the tin antimony colloidal sol obtaining
45H
2o and SbCl
3mass ratio be 10～20:1.
7. a kind of preparation method with the photoelectrocatalysis bifunctional electrodes of wide ripple range response according to claim 1, it is characterized in that, in described step (4), heat treatment adopts nitrogen atmosphere, controlling heating rate is 1～2 ℃/min, treatment temperature is risen to 400 ℃-600 ℃, after heat treatment 1-3h, controlling rate of temperature fall is 1～2 ℃/min, is down to room temperature.
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| CN104176795B (en) * | 2014-08-28 | 2016-01-20 | 扬州大学 | The preparation method of the titania nanotube of load macropore titanium tetrachloride |
| RU2624620C1 (en) * | 2016-04-14 | 2017-07-04 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский государственный университет" (СПбГУ) | METHOD FOR PRODUCING PHOTOCATALYST BASED ON NANO-HETEROSTRUCTURAL SEMICONDUCTOR CdS-WO3-TiO2 |
| CN115814785B (en) * | 2022-11-18 | 2024-04-26 | 同济大学 | TiO (TiO) with visible light response nano Au modified crystal face heterojunction2Photoelectrode, construction and application thereof |
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| CN101786005A (en) * | 2010-02-04 | 2010-07-28 | 上海交通大学 | Method for preparing cadmium sulfide-titanium dioxide nano-tube composite catalyst |
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