CN103489935B - Nitrogen-doped titanium dioxide light electrode of responding to visible light and infrared light and preparation method thereof - Google Patents
Nitrogen-doped titanium dioxide light electrode of responding to visible light and infrared light and preparation method thereof Download PDFInfo
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- CN103489935B CN103489935B CN201310444406.4A CN201310444406A CN103489935B CN 103489935 B CN103489935 B CN 103489935B CN 201310444406 A CN201310444406 A CN 201310444406A CN 103489935 B CN103489935 B CN 103489935B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/127—Sunlight; Visible light
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/128—Infra-red light
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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- Y02E10/00—Energy generation through renewable energy sources
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- Y02E10/542—Dye sensitized solar cells
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
Nitrogen-doped titanium dioxide light electrode that the invention discloses a kind of responding to visible light and infrared light and preparation method thereof, belong to new forms of energy field of new and electrochemistry, photoelectrocatalysis field, photoelectricity is very: the obtained the maximum absorption of the ultraviolet-visible absorption spectroscopy figure of described nitrogen-doped titanium dioxide light electrode is 1769nm, arrives near infrared region to the absorption peak of sunlight.Preparation method comprises the following steps successively: titanium substrate pretreatment; The configuration of electrolyte; Titanium sheet is placed in electrolyte as anode, platinized platinum as negative electrode, and be 15 ~ 100V anodic oxygenization, 20 ~ 120min in direct voltage, anode oxidation process at room temperature carries out, then cleaning, drying; By above-mentioned titanium sheet optoelectronic pole calcining.The present invention is nitrogen-doped titanium dioxide light electrode of a kind of energy responding to visible light and infrared light and preparation method thereof, and reach near infrared region to the response spectrum scope of sunlight, obtained the maximum absorption appears at 1769 nanometers.
Description
Technical field
The invention belongs to new forms of energy field of new and electrochemistry, photoelectrocatalysis field.
Background technology
Titanium dioxide (TiO
2) as a kind of novel high-performance just material, harmless to human non-toxic, acid and alkali-resistance, corrosion-resistant, catalytic activity is high, cheap, has broad application prospects in fields such as solar energy sensitized cells, semiconductor, sensing material, fluid purification, energy storage hydrogen manufacturing.
The energy gap of titanium dioxide (anatase) is 3.2ev, be only less than or equal to the UV-irradiation of 387.5nm at wavelength under, shows higher photocatalytic activity.In whole sunlight, the ultraviolet portion that wavelength is less than 400nm accounts for 7%, the visible light part of 0.4-0.76um accounts for 50%, the infrared light being greater than 0.76um accounts for 43%, infrared light comprise again near-infrared (0.76-2.5um), in infrared (2.5-25um) and far red light (>25um), the sunlight wavelength scope that ground can detect is 295-2500nm, and therefore, titanium dioxide is very low to the utilance of sunlight.In order to overcome the above problems, researchers carry out doping vario-property to titanium dioxide, widen the absorbing wavelength scope of titanium dioxide, improve the utilance to sunlight.
Summary of the invention
The object of the invention is to: in order to solve the absorbing wavelength narrow range of existing titanium dioxide to light, the problem of responding to visible light and infrared light hardly, and nitrogen-doped titanium dioxide light electrode of a kind of energy responding to visible light and infrared light and preparation method thereof is provided, arrive near infrared region to the response range of sunlight, obtained the maximum absorption appears at 1769nm.
The object of the invention is realized by following technical proposals:
A nitrogen-doped titanium dioxide light electrode for responding to visible light and infrared light, described nitrogen-doped titanium dioxide light electrode obtained the maximum absorption in ultraviolet-visible absorption spectroscopy figure is 1769nm, arrives near infrared region to the absorption of sunlight.
A preparation method for the nitrogen-doped titanium dioxide light electrode of responding to visible light and infrared light, comprises the following steps successively:
(1) titanium substrate pretreatment.
Preliminary treatment mainly comprises cleaning by degreasing and chemical polishing two parts, with acetone, absolute ethyl alcohol and deionized water, cleaning by degreasing is carried out to it successively, mainly in order to remove the oil substances of titanium substrate surface, to avoid the impact introduced impurity in anode oxidation process and reduce titanium dioxide crystal degree; Carry out chemical polishing in order to make prepare optoelectronic pole surface evenly.
(2) configuration of electrolyte: electrolyte is mixed for ethylene glycol with all the other mutually by the deionized water of 5 ~ 30wt%, the nitric acid of 5 ~ 30wt%; Described nitric acid is the nitric acid meter of 67.5% by mass percentage, and ethylene glycol is by analytical reagent.
The conductivity of the content major effect electrolyte of water in electrolyte, nitric acid not only provides nitrogenous source wherein, affects the conductivity of electrolyte simultaneously, and ethylene glycol mainly affects the viscosity of electrolyte, water content is higher, will improve the conductivity of electrolyte, optoelectronic pole surface will there will be avalanche, and nitric acid content is higher, corrosiveness strengthens, can not microcellular structure be formed, thus affect optoelectronic pole specific area, and then affect catalytic activity and the optoelectronic pole surface topography of whole optoelectronic pole.
(3) titanium sheet is placed in electrolyte as anode, platinized platinum as negative electrode, be 15 ~ 100V anodic oxygenization, 20 ~ 120min in direct voltage, anode oxidation process at room temperature carries out, then cleaning, drying; In anode oxidation process, oxidation voltage and oxidization time play key effect to whole anode oxidation process.Oxidation voltage directly affects nitrogen in optoelectronic pole and mixes the microscopic appearance on effect and optoelectronic pole surface, oxidation voltage is too low, can not puncture the dielectric layer of titanium Surface Creation, thus affects the electric conductivity of optoelectronic pole, and anodic oxidation voltage is too high, collapse directly causing optoelectronic pole surface microstructure; And oxidization time mainly affects the thickness of titanium oxide film layer on whole optoelectronic pole, thus impact is to the utilization ratio of light and conversion ratio, rete is too thin, sunlight can not be made full use of, and the too thick direct increase optoelectronic pole skin resistance of rete, thus the separation of electron hole and the electric conductivity of optoelectronic pole can be affected.
(4) by above-mentioned titanium sheet optoelectronic pole calcining 1 ~ 5h, temperature is 350 ~ 650 DEG C, and takes out cooling subsequently, the nitrogen-doped titanium dioxide light electrode of namely meet with a response visible ray and infrared light.In the process, calcination time and calcining heat directly affect degree of crystallinity and the crystalline phase conversion of titanium dioxide, in this temperature range and time range, titanium dioxide can be good at changing into the highest Detitanium-ore-type of photocatalytic activity from unformed, the rutile-type simultaneously avoiding photocatalytic activity lower produces, when temperature is higher than 650 DEG C, titanium dioxide crystal form is mainly based on the rutile that catalytic activity is lower, the too high photocatalytic activity that will reduce optoelectronic pole of temperature, when temperature is lower than 350 DEG C, the transition temperature of anatase titanium dioxide can not be reached.Calcination time major effect titanium dioxide crystal integrity degree, calcination time is too short, will cause titanium dioxide imperfect crystal, thus affect photocatalytic activity.
As aforesaid further selection, the preparation method of the nitrogen-doped titanium dioxide light electrode of responding to visible light and infrared light, comprises the following steps successively:
(1) titanium substrate pretreatment;
(2) configuration of electrolyte: electrolyte is mixed for ethylene glycol with all the other mutually by the deionized water of 10 ~ 20wt%, the nitric acid of 10 ~ 20wt%;
(3) titanium sheet is placed in electrolyte as anode, platinized platinum as negative electrode, be 30 ~ 60V anodic oxygenization, 50 ~ 90min in direct voltage, anode oxidation process at room temperature carries out, then cleaning, drying;
(4) by above-mentioned titanium sheet optoelectronic pole calcining 2 ~ 4h, temperature is 400 ~ 600 DEG C, and takes out cooling subsequently, the nitrogen-doped titanium dioxide light electrode of namely meet with a response visible ray and infrared light.
As aforesaid selection, described titanium substrate pretreatment is for carry out chemical polishing and ungrease treatment successively by titanium sheet.
As aforesaid selection, described chemical polishing is the titanium sheet of purity >99.9% be placed in by the hydrofluoric acid of 5 ~ 35vol%, the nitric acid of 35 ~ 65vol% and polishing fluid polishing 10 ~ 30s that all the other mix for deionization aqueous phase;
As aforesaid selection, described ungrease treatment is by titanium sheet respectively at acetone, absolute ethyl alcohol, deionized water for ultrasonic 15min, ultrasonic power 720W, more repeatedly rinses with deionized water, dries.
Beneficial effect of the present invention: the present invention adopts and grow nitrogen-doped titanium dioxide light electrode in titanium substrate, titanium deoxid film and substrate are that chemical bond is connected, in conjunction with firm, the film prepared is even, harmless to human non-toxic, acid and alkali-resistance, corrosion-resistant, through long period of soaking, titanium dioxide film can not come off.The nitrogen of the visible ray that the present invention prepares and infrared optical response mixes titanium dioxide photoelectrode mainly Detitanium-ore-type, and anatase crystal face, mainly based on 101 crystal faces that photocatalytic activity is the highest, can show very high photocatalytic activity under sunlight.
Accompanying drawing explanation
Fig. 1 is the visible ray prepared of execution mode 5 and the titanium dioxide photoelectrode of infrared optical response, respectively the percent of decolourization figure of photoelectric catalysis degrading methyl orange under sunlight and ultraviolet light.
Fig. 2 is the percent of decolourization figure of the titanium dioxide photoelectrode photo-catalytic degradation of methyl-orange under ultraviolet light of the visible ray prepared of execution mode 1,2,3,4 and infrared optical response.
Fig. 3 is the ultraviolet-visible absorption spectroscopy figure that execution mode 5 obtains optoelectronic pole, as shown in Figure 3.
Embodiment
Following non-limiting examples is for illustration of the present invention.
embodiment 1:
The preparation of the nitrogen-doped titanium dioxide light electrode of responding to visible light and infrared light:
1. high-purity titanium sheet (>99.9%) is cut into 3 × 4cm size, is placed in by HF, HNO
3, H
2in the O chemical brightening solution that 1:4:5 forms by volume, polishing 10 ~ 30s;
2. titanium sheet is carried out respectively in acetone, ethanol, deionized water ultrasonic degreasing cleaning 15min, ultrasonic power is 720W, 25 DEG C of oven dry;
3. the configuration of electrolyte: electrolyte is mixed for ethylene glycol with all the other mutually by the deionized water of 30wt%, the nitric acid of 30wt%;
4. titanium sheet being placed in electrolyte as anode, platinized platinum as negative electrode, is 100V anodic oxygen 2h in direct voltage, and anode oxidation process at room temperature carries out, and then takes out and washes out surperficial electrolyte with deionized water, 25 DEG C of oven dry;
5. above-mentioned titanium sheet optoelectronic pole is placed in resistance furnace, is warming up to 650 DEG C, calcining at constant temperature 5 hours, obtain the nitrogen-doped titanium dioxide light electrode of responding to visible light and infrared light.
embodiment 2:
Other steps of present embodiment and parameter identical with embodiment one, with embodiment one difference be: in step 3 electrolyte by the deionized water of 10wt%, the nitric acid of 10wt% and all the other mix mutually for ethylene glycol.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
embodiment 3:
Other steps of present embodiment and parameter identical with embodiment two, with execution mode two difference be: in step 4, oxidation voltage is 60V, oxidization time is 50min.
embodiment 4:
Other steps of present embodiment and parameter identical with embodiment three, with execution mode three difference be: in step 5, calcination time is 2 hours, calcining heat is 400 DEG C.
As shown in Figure 2: as can be seen from the figure, different case study on implementation, photoelectrocatalysis effect is different, but show higher photoelectrocatalysis effect on the whole, from execution mode 1 to execution mode 4, photoelectrocatalysis effect improves constantly, and optoelectronic pole catalytic performance is progressively optimized simultaneously.
embodiment 5:
(1) present embodiment concrete steps are as follows:
1. high-purity titanium sheet (>99.9%) is cut into 3 × 4cm size, is placed in by HF, HNO
3, H
2in the O chemical brightening solution that 1:4:5 forms by volume, polishing 10 ~ 30s;
2. by titanium sheet respectively at acetone, carry out in absolute ethyl alcohol, deionized water ultrasonic degreasing cleaning 15min, ultrasonic power is 720W, 25 DEG C of oven dry;
3. the configuration of electrolyte: electrolyte is mixed for ethylene glycol with all the other mutually by the deionized water of 5wt%, the nitric acid of 5wt%;
4. titanium sheet being placed in electrolyte as anode, platinized platinum as negative electrode, is 15V anodic oxygen 20min in direct voltage, and anode oxidation process carries out at room temperature, then takes out and washes out surperficial electrolyte with deionized water, 25 DEG C of oven dry;
5. above-mentioned titanium sheet optoelectronic pole is placed in resistance furnace, is warming up to 350 DEG C, calcining at constant temperature 1 hour, obtain the nitrogen-doped titanium dioxide light electrode of responding to visible light and infrared light.
(2) optoelectronic pole photoelectric catalysis degrading methyl orange
be that the nitrogen-doped titanium dioxide light electrode of the responding to visible light of 3cm × 4cm and infrared light is as positive pole using effective area, carbon-point is negative pole, and immersing 40ml concentration is in the methyl orange solution of 20mg/L, applies 1V bias voltage, use ultraviolet light and solar light irradiation respectively, carry out photoelectric catalysis degrading;
with the absorbance change of ultraviolet-visible spectrophotometer test solution after timing sampling.The percent of decolourization figure of photoelectric catalysis degrading methyl orange as shown in Figure 1.The ultraviolet-visible absorption spectroscopy figure of optoelectronic pole, as shown in Figure 3.
Fig. 1: carry out photoelectric catalysis degrading methyl orange test discovery respectively by mixing titanium dioxide photoelectrode to nitrogen under ultraviolet light and the sun, optoelectronic pole prepared by the present invention under sunlight to the percent of decolourization of methyl orange with under UV-irradiation, all can reaching good decolorizing effect, visible ray sunlight or near infrared light can be responded well from macroscopically demonstrating this optoelectronic pole.
Fig. 3: this figure is from the angle of spectral absorption, explaining the optoelectronic pole that the present invention relates to can responding to visible light and near infrared light, at near infrared region, wavelength obtained the maximum absorption reaches 1769nm, and can totally linearization visible-range, also explain the present invention simultaneously theoretically and show higher photoelectric catalytically active under sunlight.
Claims (8)
1. a nitrogen-doped titanium dioxide light electrode for responding to visible light and infrared light, is characterized in that: described photoelectricity very titanium substrate grows the optoelectronic pole of nitrogen-doped titanium dioxide film; The absorption of described nitrogen-doped titanium dioxide light electrode pair sunlight arrives near infrared region, and the scope of ultraviolet-visible-infrared absorption spectroscopy contains 250-2500nm region, and maximum absorption band is at 1769nm place.
2. a preparation method for the nitrogen-doped titanium dioxide light electrode of responding to visible light and infrared light, is characterized in that comprising the following steps successively:
(1) titanium substrate pretreatment;
(2) configuration of electrolyte: electrolyte is mixed for ethylene glycol with all the other mutually by the deionized water of 5 ~ 30wt%, the nitric acid of 5 ~ 30wt%;
(3) titanium sheet is placed in electrolyte as anode, platinized platinum as negative electrode, be 15 ~ 100V anodic oxygenization, 20 ~ 120min in direct voltage, anode oxidation process at room temperature carries out, then cleaning, drying;
(4) by above-mentioned titanium sheet optoelectronic pole calcining 1 ~ 5h, temperature is 350 ~ 650 DEG C, and takes out cooling subsequently, the nitrogen-doped titanium dioxide light electrode of namely meet with a response visible ray and infrared light.
3. the preparation method of the nitrogen-doped titanium dioxide light electrode of responding to visible light as claimed in claim 2 and infrared light, is characterized in that comprising the following steps successively:
(1) titanium substrate pretreatment;
(2) configuration of electrolyte: electrolyte is mixed for ethylene glycol with all the other mutually by the deionized water of 10 ~ 20wt%, the nitric acid of 10 ~ 20wt%;
(3) titanium sheet is placed in electrolyte as anode, platinized platinum as negative electrode, be 15 ~ 100V anodic oxygenization, 20 ~ 120min in direct voltage, anode oxidation process at room temperature carries out, then cleaning, drying;
(4) by above-mentioned titanium sheet optoelectronic pole calcining 1 ~ 5h, temperature is 350 ~ 650 DEG C, and takes out cooling subsequently, the nitrogen-doped titanium dioxide light electrode of namely meet with a response visible ray and infrared light.
4. the preparation method of the nitrogen-doped titanium dioxide light electrode of responding to visible light as claimed in claim 3 and infrared light, is characterized in that comprising the following steps successively:
(1) titanium substrate pretreatment;
(2) configuration of electrolyte: electrolyte is mixed for ethylene glycol with all the other mutually by the deionized water of 10 ~ 20wt%, the nitric acid of 10 ~ 20wt%;
(3) titanium sheet is placed in electrolyte as anode, platinized platinum as negative electrode, be 30 ~ 60V anodic oxygenization, 50 ~ 90min in direct voltage, anode oxidation process at room temperature carries out, then cleaning, drying;
(4) by above-mentioned titanium sheet optoelectronic pole calcining 1 ~ 5h, temperature is 350 ~ 650 DEG C, and takes out cooling subsequently, the nitrogen-doped titanium dioxide light electrode of namely meet with a response visible ray and infrared light.
5. the preparation method of the nitrogen-doped titanium dioxide light electrode of responding to visible light as claimed in claim 4 and infrared light, is characterized in that comprising the following steps successively:
(1) titanium substrate pretreatment;
(2) configuration of electrolyte: electrolyte is mixed for ethylene glycol with all the other mutually by the deionized water of 10 ~ 20wt%, the nitric acid of 10 ~ 20wt%;
(3) titanium sheet is placed in electrolyte as anode, platinized platinum as negative electrode, be 30 ~ 60V anodic oxygenization, 50 ~ 90min in direct voltage, anode oxidation process at room temperature carries out, then cleaning, drying;
(4) by above-mentioned titanium sheet optoelectronic pole calcining 2 ~ 4h, temperature is 400 ~ 600 DEG C, and takes out cooling subsequently, the nitrogen-doped titanium dioxide light electrode of namely meet with a response visible ray and infrared light.
6. the preparation method of the responding to visible light as described in claim 2,3,4 or 5 and the nitrogen-doped titanium dioxide light electrode of infrared light, is characterized in that: described titanium substrate pretreatment is for carry out chemical polishing and ungrease treatment successively by titanium sheet.
7. the preparation method of the nitrogen-doped titanium dioxide light electrode of responding to visible light as claimed in claim 6 and infrared light, is characterized in that: described chemical polishing is the titanium sheet of purity >99.9% be placed in by the hydrofluoric acid of 5 ~ 35vol%, the nitric acid of 35 ~ 65vol% and polishing fluid polishing 10 ~ 30s that all the other mix for deionization aqueous phase.
8. the preparation method of the nitrogen-doped titanium dioxide light electrode of responding to visible light as claimed in claim 7 and infrared light, it is characterized in that: described ungrease treatment is respectively at acetone, absolute ethyl alcohol, deionized water for ultrasonic 15min by titanium sheet, ultrasonic power 720W, repeatedly rinse with deionized water again, dry.
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| CN109750339A (en) * | 2019-03-25 | 2019-05-14 | 四川农业大学 | With absorption visible light and near-infrared mixing appearance structure optoelectronic pole and preparation method |
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