CN101491755B - Preparation method of carbon doped nano titanium dioxide thin film with visible light activity and use thereof - Google Patents
Preparation method of carbon doped nano titanium dioxide thin film with visible light activity and use thereof Download PDFInfo
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- CN101491755B CN101491755B CN2009100469193A CN200910046919A CN101491755B CN 101491755 B CN101491755 B CN 101491755B CN 2009100469193 A CN2009100469193 A CN 2009100469193A CN 200910046919 A CN200910046919 A CN 200910046919A CN 101491755 B CN101491755 B CN 101491755B
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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
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- 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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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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
- 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
- Y02E60/30—Hydrogen technology
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Abstract
The invention discloses a method for preparing a carbon-doped nano titanium dioxide film with visible light activity, and application thereof. The preparation method comprises the following steps: using titanium carbide nano powder as a raw material, a direct-current regulated power supply or a constant potential rectifier as an input device and a suspension of nano titanium carbide as an electrophoresis depositing liquid, electromagnetically stirring the mixture during electrifying, and depositing titanium carbide nano granules on the surface of a substrate to form a TiC film; and thermally treating the formed TiC film by a muffle furnace to form the carbon-containing TiO2 film with the visible light activity when the color of the TiC film changes, wherein the input voltage during electrophoresis depositing is between 10 and 30 volts, and the electrophoresis time is between 0.5 and 10 hours; the electrophoresis depositing liquid adopts the suspension containing 10 to 40 grams per liter of nano titanium carbide; and the thermal treatment temperature is between 350 and 450 DEG C, and the oxidizing time is between 0.5 and 6 hours. Electrophoresis depositing equipment adopted by the method is simple, and the electrophoresis depositing solution can be used repeatedly, so the method can achieve energy conservation and emission reduction during production.
Description
Technical field
The present invention relates to the optically catalytic TiO 2 chemical technology field, relate to a kind of method for preparing carbon-doped nano titanium deoxid film by electrophoretic deposition technique specifically with visible light activity.
Background technology
Found the semiconductor titanium dioxide electrodes since splitting water into hydrogen and oxygen under the UV-irradiation from 1972, titanium dioxide has been subjected in the material field paying attention to very widely.TiO
2Can be used for many aspects such as photocatalysis to degrade organic matter, sterilizing, sewage disposal, air cleaning, light hydrogen production by water decomposition, because TiO
2Energy gap big (3.2eV Detitanium-ore-type, 3.0eV rutile-type), to the absorption difference of visible light, limited its range of application greatly.At present, the nano-TiO of visible light activity
2Preparation method's research become a very active problem of photocatalysis new material exploitation.Usually adopt doping metals or nonmetallic mode to increase its visible light activity, having of reporting at present is nonmetal as C, N, the doping of elements such as S and Fe, Cr, the doping of Sb and the multiple metallic element of rare earth element etc.Wherein, carbon is considered to one of doped chemical of improving its visible light activity.
The carbon-doped nano TiO that has reported
2The preparation method of film has multiple, and the method by gas burner heating Ti metal such as Khan has prepared and has visible light-responded carbonaceous TiO
2Film has improved the absorbent properties of visible light, wideer visible light wave range occurred and has absorbed platform, and the problem of existence is that the method for Khan is difficult to control; Also there is report to utilize CO
2Prepare carbonaceous TiO as the method for reacting gas by splash-proofing sputtering metal Ti target
2Film, we reported once also that the method for sputtered with Ti/C hybrid target prepared carbonaceous TiO
2Film, and the TiC film of anodic oxidation sputter obtains TiO then
2-xC
xMethods such as film.But there are some shortcomings in these methods, as sputter coating energy consumption height, apparatus expensive etc.
Summary of the invention
The object of the invention provides that a kind of equipment is simple, reactant liquor is reusable, the preparation of energy-saving and emission-reduction has the method for the carbon-doped nano titanium deoxid film of visible light activity.
Another object of the present invention has provided above-mentioned application with carbon-doped nano titanium deoxid film of visible light activity.
For achieving the above object, the present invention proposes a kind of preparation method with carbon-doped nano titanium deoxid film of visible light activity, with the titanium carbide nano powder is raw material, pass through D.C. regulated power supply or potentiostat earlier as input equipment, the suspension that utilizes nano titanium carbide is as electrophoretic deposition liquid, and in galvanization, carry out electromagnetic agitation, the titanium carbide nanoparticle deposition forms colored TiC film to substrate surface; The TiC film that forms is heat-treated with muffle furnace,, promptly form to have the carbonaceous TiO of visible light activity when the color of TiC film changes
2Film; Input voltage is 10～30V when regulating electrophoresis, and the control electrophoresis time is 0.5～10 hour; Electrophoretic deposition liquid adopts the suspension of the nano titanium carbide that contains 10～40g/L; Adopt muffle furnace that the titanium carbide film is heat-treated, the control heat treatment temperature is 350～450 ℃, and oxidization time is 0.5～6 hour, causes the color of TiC film to change, and forms to have the carbonaceous TiO of visible light activity
2Film.
Preferably, the control electrophoresis time is 0.5～2 hour among the present invention;
Preferably, the control electrophoretic voltage is 10～13.5V among the present invention;
Preferably, control 350～400 ℃ of heat treatment temperatures among the present invention;
Preferably, control heat treatment time 1.5～3.0 hours among the present invention.
The carbonaceous TiO that the present invention is prepared
2Film has higher visible light activity, can be used for the visible light photocatalysis field.
The carbonaceous TiO that the present invention is prepared
2Film has higher visible light activity, can be used for visible light light hydrogen production by water decomposition field.
The carbonaceous TiO that the present invention is prepared
2Film has higher visible light activity, can be used for area of solar cell.
Preparation method with carbon-doped nano titanium deoxid film of visible light activity provided by the present invention, compared with prior art, have the following advantages: the inventive method adopts electrophoretic deposition equipment simple, and the solution of electrophoretic deposition can use repeatedly, can realize the energy-saving and emission-reduction of production process.
Description of drawings
Fig. 1 is preparation method's process schematic diagram of the present invention.
Fig. 2 is the electric current-time graph of TiC film electrophoresis deposition process under the different electrophoresis input voltages.Wherein:
A. the electrophoresis input voltage is 10.0V;
B. the electrophoresis input voltage is 13.5V.
The carbonaceous TiO of Fig. 3 for making among the embodiment 1
2Short-circuit photocurrent is with the electric current change curve that shines/be in the light under the membrane electrode visible light.
Fig. 4 is the carbonaceous TiO that TiC powder, TiC film and TiC powder after heat treatment obtain
2XRD spectrum.Wherein:
The a.TiC powder;
B. 8 hours TiC film of electrophoretic deposition;
The carbonaceous TiO that the c.TiC powder obtained through 350 ℃ of heat treatments in 2 hours
2
The carbonaceous TiO that the d.TiC powder obtained through 450 ℃ of heat treatments in 2 hours
2
The carbonaceous TiO of Fig. 5 for making among the embodiment 3
2Short-circuit photocurrent is with the electric current change curve that shines/be in the light under the membrane electrode visible light.
Fig. 6 is a carbonaceous TiO
2Electric current-the potential curve of membrane electrode under the illumination of different conditions is penetrated.Wherein:
A. under the light-blocking state;
B. under the visible light state;
C. under the state of white light, photoelectric current numerical value has reduced 10 times.
The specific embodiment
Further describe the present invention by the following examples, but be not limited thereto.
Under the room temperature by electrophoretic deposition method at Ti sheet surface preparation TiC film, to clean back Ti sheet is fixed in the electrolytic cell, the current potential of regulating potentiostat is 10.0V, electrophoretic deposition liquid adopts the titanium carbide suspension that contains 10g/L, electrophoretic deposition 2 hours, the current time change curve of electrophoretic deposition process is shown in a curve among Fig. 2.The TiC film that obtains was heat-treated under 350 ℃ 2 hours in air atmosphere, and at this moment the TiC film changes carbonaceous TiO into
2Film.Fig. 3 illustrates the carbonaceous TiO that is obtained by electrophoretic deposition TiC film in the present embodiment after heat treatment
2The photoelectric current of film can see that the steady short-circuit photoelectric current under visible light is 0.23 μ A/cm
2
Under the room temperature by electrophoretic deposition method at Ti surface preparation TiC film, to clean back Ti sheet is fixed in the electrolytic cell, electrode is adopted metal Pt sheet, regulating D.C. regulated power supply voltage is 30V, and distance between electrodes is 1cm, and electrophoretic deposition liquid adopts the titanium carbide suspension that contains 40g/L, electrophoretic deposition 8 hours, obtain the TiC film, the TiC film that obtains was heat-treated under 450 ℃ 2 hours in air atmosphere, at this moment the TiC film changes carbonaceous TiO into
2Film.The XRD figure of the TiC film that obtains is shown in b curve among Fig. 4.From figure, can be clear that the diffraction maximum of titanium carbide, the substrate surface that deposits to of titanium carbide success is described; The c curve is depicted as the XRD spectrum of the titanium carbide powder after 350 ℃ of heat treatment among while Fig. 4, can see anatase and rutile crystal type TiO
2Generation and the part not have the conversion titanium carbide; The d curve is depicted as the XRD spectrum of the titanium carbide powder after 450 ℃ of heat treatment among Fig. 4, can see that titanium carbide is converted into anatase and rutile crystal type TiO fully
2
Under the room temperature by electrophoretic deposition method at Ti sheet surface preparation TiC film, to clean back Ti sheet is fixed in the electrolytic cell, regulation voltage is 13.5V, electrophoretic deposition liquid adopts the titanium carbide suspension that contains 10g/L, electrophoretic deposition 2 hours, the current time change curve of electrophoretic deposition process is shown in b curve among Fig. 2.The TiC film that obtains was heat-treated under 350 ℃ 2 hours in air atmosphere, and at this moment TiC changes carbonaceous TiO into
2Film.Fig. 5 illustrates the carbonaceous TiO that is obtained by electrophoretic deposition TiC film in the present embodiment after heat treatment
2The photoelectric current of film can see that the photoelectric current under visible light is 0.68 μ A/cm
2Figure 6 shows that prepared carbonaceous TiO in the present embodiment
2Photoelectric current-potential curve under the film different conditions, prepared carbonaceous TiO in the present embodiment as can be seen
2Film has significantly visible light-responded.
Claims (6)
1. preparation method with carbon-doped nano titanium deoxid film of visible light activity, it is characterized in that with the titanium carbide nano powder be raw material, pass through D.C. regulated power supply or potentiostat earlier as input equipment, the suspension that utilizes nano titanium carbide is as electrophoretic deposition liquid, and in galvanization, carry out electromagnetic agitation, the titanium carbide nanoparticle deposition forms colored TiC film to substrate surface; The TiC film that forms is heat-treated with muffle furnace,, promptly form to have the carbonaceous TiO of visible light activity when the color of TiC film changes
2Film; Input voltage is 10～30V when regulating electrophoretic deposition, and the control electrophoresis time is 0.5～10 hour; Electrophoretic deposition liquid adopts the suspension of the nano titanium carbide that contains 10～40g/L; Adopt muffle furnace that the TiC film is heat-treated, the control heat treatment temperature is 350～450 ℃, and oxidization time is 0.5～6 hour, and the color of TiC film changes, and forms to have the carbonaceous TiO of visible light activity
2Film.
2. preparation method as claimed in claim 1, it is characterized in that controlling electrophoresis time is 0.5～2 hour.
3. preparation method as claimed in claim 1, it is characterized in that controlling electrophoretic voltage is 10～13.5V.
4. preparation method as claimed in claim 1 is characterized in that controlling 350～400 ℃ of heat treatment temperatures.
5. preparation method as claimed in claim 1 is characterized in that controlling heat treatment time 1.5～3.0 hours.
According to claim 1 the thin-film material that obtains of method in the application of visible light photocatalysis, light hydrogen production by water decomposition or area of solar cell.
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| CN113145152B (en) * | 2021-02-01 | 2022-05-27 | 重庆工商大学 | Visible light catalysis one-pot multidirectional chemoselectivity N-alkylation method |
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