CN106887336A - TiO2/BiVO4The preparation method of nano-array optoelectronic pole - Google Patents
TiO2/BiVO4The preparation method of nano-array optoelectronic pole Download PDFInfo
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- CN106887336A CN106887336A CN201710169898.9A CN201710169898A CN106887336A CN 106887336 A CN106887336 A CN 106887336A CN 201710169898 A CN201710169898 A CN 201710169898A CN 106887336 A CN106887336 A CN 106887336A
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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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- 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
- H01G9/0029—Processes of manufacture
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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
- H01G9/2036—Light-sensitive devices comprising an oxide semiconductor electrode comprising mixed oxides, e.g. ZnO covered TiO2 particles
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
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Abstract
The invention discloses a kind of TiO2/BiVO4Nano-array optoelectronic pole preparation method.TiO is prepared by sol-gal process first2Seed Layer colloidal sol；TiO is coated in FTO electro-conductive glass substrates using dip-coating method2Seed Layer, through Overheating Treatment after, by length have TiO2The electro-conductive glass of Seed Layer is placed on TiO2By hydro-thermal process in growth solution, TiO is obtained2Nanometer stick array；Using continuous ionic exchange process by BiVO4Nano-particle deposits to TiO2In nanometer rods, TiO is obtained2/BiVO4Nano-array optoelectronic pole.The preparation process is simple for providing of the invention is easily-controllable, equipment requirement is low.The TiO of preparation2/BiVO4Nano-array optoelectronic pole compares simple TiO2Optoelectronic pole visible absorption strengthens, and PhotoelectrocatalytiPerformance Performance is good.
Description
Technical field
The invention belongs to technical field of material, specially a kind of TiO for photoelectrocatalysis2/BiVO4Nano-array
The preparation method of optoelectronic pole.
Background technology
Energy shortage and problem of environmental pollution are the significant challenges that current mankind faces.In order to maintain mankind's long-run development with
And slow down the further deterioration of environment, finding clean, reproducible new energy turns into relation human survival and sustainable development
Emphasis.Wherein, Hydrogen Energy has gradually attracted the attention of people as a kind of abundance, cleaning and reproducible green energy resource.
In current various hydrogen production process, solar photolysis water hydrogen is to utilize inexhaustible, nexhaustible solar energy for energy
Source, with water as raw material, hydrogen is obtained by being electrolysed, process cleans environmental protection.Additionally, the combustion product of hydrogen is water.Cause
This photolysis water hydrogen is considered as the hydrogen manufacturing approach of most attraction.
1972, Fujishima and Honda was found that illumination TiO2Electrode can be with decomposition water and prepared hydrogen, hereafter, light
The catalyst for solving water hydrogen manufacturing has obtained swift and violent development.At present in the optoelectronic pole material of report, TiO2It is steady with the chemistry that it is higher
The features such as qualitative, non-toxic and wide material sources, become the study hotspot of photocatalytic water catalyst.Wherein, one-dimensional TiO2Nanometer
Material (nano wire, nanometer rods, nanotube etc.) has larger draw ratio, and directly transmission is logical when can be shifted as photoelectron
Road, is a kind of preferable optoelectronic pole material.
However, TiO2There are two main defects in photochemical catalyst：One is energy gap (anatase wider：3.2eV, gold
Red stone 3.0eV), can only can not be by excited by visible light to ultraviolet light response.Two be the recombination rate in electronics and hole pair very
Height, directly influences the performance of photochemical catalyst.Prepare the TiO with appropriate band structure2Matrix composite, can improve TiO2
Photoelectricity hydrolytic hydrogen production performance.BiVO4As a kind of semi-conducting material of new low energy gap, with and TiO2Suitable energy level knot
Structure.Therefore it is proposed that a kind of TiO2/BiVO4The preparation method of nano-array optoelectronic pole, it is intended to improve TiO2Photoelectrocatalysis
Energy.
The content of the invention
It is an object of the invention to propose a kind of TiO2/BiVO4The preparation method of nano-array optoelectronic pole, can improve
TiO2PhotoelectrocatalytiPerformance Performance.
The TiO that the present invention is provided2/BiVO4The preparation method of nano-array optoelectronic pole, comprises the following steps：
Step one：TiO is prepared by sol-gal process2Seed Layer colloidal sol；
Step 2：TiO is coated in FTO electro-conductive glass substrates using dip-coating method2Seed Layer；
Step 3：After through Overheating Treatment, length there is into TiO2The electro-conductive glass of Seed Layer is placed on TiO2Pass through in growth solution
Hydro-thermal process, obtains TiO2Nanometer stick array；
Step 4：Using continuous ionic exchange process by BiVO4Nano-particle deposits to TiO2In nanometer rods, TiO is obtained2/
BiVO4Nano-array optoelectronic pole.
Further, the step one is by ethylene glycol amine (C4H11NO2) and ethanol (C2H5OH) mix, and be added dropwise over
Butyl titanate (C16H36O4Ti), the Seed Layer colloidal sol of 0.2~0.5mol/L is configured.
Further, the step 2 is to complete TiO in FTO electro-conductive glass using dip-coating method2Plated film, at 100 DEG C
After lower drying, to repeat the above steps and carry out second membrane to FTO electro-conductive glass, by FTO electro-conductive glass after membrane terminates twice
1~4h is dried in baking oven is placed.
Further, the step 3 is to be put into TiO after sample is made annealing treatment2In growth solution, hydro-thermal is anti-at 160 DEG C
8~12h is answered, is dried under the conditions of 60 DEG C, obtain TiO2Nanometer rods.
Further, the step 4 is to use continuous ionic exchange process by BiVO4Nano-particle deposits to TiO2Nanometer rods
On.Under normal temperature, by pucherite (BiVO4·5H2O) it is dissolved in EGME (CH3OCH2CH2In OH), be configured to containing 0.005~
0.01mol/L Bi3+Precursor solution.Then, by ammonium metavanadate (NH4VO3) be dissolved in 100 DEG C of hot water, it is configured to contain
0.005~0.01mol/L VO4 3-Precursor solution.Finally, length there is into TiO2The electro-conductive glass of nanometer rods is successively immersed in Bi3 +And VO4 3-Precursor solution in 60s, repetitive cycling 5~15 times.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) preparation process is simple of the invention is easily-controllable, equipment requirement is low.
(2) TiO of the invention2/BiVO4Nano-array optoelectronic pole, it is possible to increase TiO2It is visible light-responded.
(3) TiO of the invention2/BiVO4Nano-array optoelectronic pole, can effectively suppress photo-generate electron-hole and be combined, and promote
Electron hole efficiently separates.
Brief description of the drawings
Fig. 1 is the TiO of gained in embodiments of the invention2/BiVO4The scanning electron microscope image of nano-array optoelectronic pole.
Fig. 2 is the TiO of gained in embodiments of the invention 12/BiVO4Nano-array optoelectronic pole is through UV-Vis spectrophotometry
Photometer test result.
Fig. 3 is the TiO of gained in embodiments of the invention 12/BiVO4Nano-array optoelectronic pole is tested through electrochemical workstation
As a result.
Specific embodiment
The following examples can make those skilled in the art that the present invention is more completely understood, but limit never in any form
The present invention.
Embodiment 1
First, by ethylene glycol amine (C4H11NO2) and ethanol (CH3CH2OH) mix, and be added dropwise over butyl titanate
(C16H36O4Ti), the Seed Layer colloidal sol of 0.2mol/L is configured；Use dipping-pulling method with the speed of 1mm/s in FTO electro-conductive glass
Upper completion TiO2Plated film simultaneously stops 20s in colloidal sol, and after being dried at 100 DEG C, repeat the above steps is carried out to FTO electro-conductive glass
Second membrane, 1h is dried during FTO electro-conductive glass is placed into baking oven after membrane terminates twice；Sample is placed in 450 in Muffle furnace
DEG C when made annealing treatment with 2 DEG C/min, insulation 2h after naturally cool to room temperature；With 1:100 volume ratio is by butyl titanate
(C16H36O4Ti) in instillation concentrated hydrochloric acid (HCl), and length there is into TiO2The electro-conductive glass of Seed Layer is immersed in the mixed growth solution,
Hydro-thermal reaction 8h at 160 DEG C, spontaneously dries under the conditions of 60 DEG C, obtains TiO2Nanometer rods；Using continuous ionic exchange process by BiVO4
Particle deposition is in TiO2In nanometer rods.Under normal temperature, the pucherite (BiVO of 0.007mol/L is configured4·5H2O EGME)
(CH3OCH2CH2OH) solution.At 100 DEG C, the ammonium metavanadate (NH of 0.007mol/L is configured4VO3) aqueous solution.Length there is into TiO2
The electro-conductive glass of nanometer rods is successively immersed in Bi3+And VO4 3-Precursor solution in 60s, repetitive cycling 10 times.Clean and dry
To TiO2/BiVO4Nano-array optoelectronic pole.
Embodiment 2
First, by ethylene glycol amine (C4H11NO2) and ethanol (CH3CH2OH) mix, and be added dropwise over butyl titanate
(C16H36O4Ti), the Seed Layer colloidal sol of 0.3mol/L is configured；Use dipping-pulling method with the speed of 1mm/s in FTO electro-conductive glass
Upper completion TiO2Plated film simultaneously stops 20s in colloidal sol, and after being dried at 100 DEG C, repeat the above steps is carried out to FTO electro-conductive glass
Second membrane, 4h is dried during FTO electro-conductive glass is placed into baking oven after membrane terminates twice；Sample is placed in 450 in Muffle furnace
DEG C when made annealing treatment with 2 DEG C/min, insulation 2h after naturally cool to room temperature；With 1:100 volume ratio is by butyl titanate
(C16H36O4Ti) in instillation concentrated hydrochloric acid (HCl), and length there is into TiO2The electro-conductive glass of Seed Layer is immersed in the mixed growth solution,
Hydro-thermal reaction 10h at 160 DEG C, spontaneously dries under the conditions of 60 DEG C, obtains TiO2Nanometer rods；Using continuous ionic exchange process by BiVO4
Particle deposition is in TiO2In nanometer rods.Under normal temperature, the pucherite (BiVO of 0.005mol/L is configured4·5H2O EGME)
(CH3OCH2CH2OH) solution.At 100 DEG C, the ammonium metavanadate (NH of 0.005mol/L is configured4VO3) aqueous solution.Length there is into TiO2
The electro-conductive glass of nanometer rods is successively immersed in Bi3+And VO4 3-Precursor solution in 60s, repetitive cycling 15 times.Clean and dry
To TiO2/BiVO4Nano-array optoelectronic pole.
Embodiment 3
First, by ethylene glycol amine (C4H11NO2) and ethanol (CH3CH2OH) mix, and be added dropwise over butyl titanate
(C16H36O4Ti), the Seed Layer colloidal sol of 0.5mol/L is configured；Use dipping-pulling method with the speed of 1mm/s in FTO electro-conductive glass
Upper completion TiO2Plated film simultaneously stops 20s in colloidal sol, and after being dried at 100 DEG C, repeat the above steps is carried out to FTO electro-conductive glass
Second membrane, 4h is dried during FTO electro-conductive glass is placed into baking oven after membrane terminates twice；Sample is placed in 450 in Muffle furnace
DEG C when made annealing treatment with 2 DEG C/min, insulation 2h after naturally cool to room temperature；With 1:100 volume ratio is by butyl titanate
(C16H36O4Ti) in instillation concentrated hydrochloric acid (HCl), and length there is into TiO2The electro-conductive glass of Seed Layer is immersed in the mixed growth solution,
Hydro-thermal reaction 12h at 160 DEG C, spontaneously dries under the conditions of 60 DEG C, obtains TiO2Nanometer rods；Using continuous ionic exchange process by BiVO4
Particle deposition is in TiO2In nanometer rods.Under normal temperature, the pucherite (BiVO of 0.01mol/L is configured4·5H2O EGME)
(CH3OCH2CH2OH) solution.At 100 DEG C, the ammonium metavanadate (NH of 0.01mol/L is configured4VO3) aqueous solution.Length there is into TiO2Receive
The electro-conductive glass of rice rod is successively immersed in Bi3+And VO4 3-Precursor solution in 60s, repetitive cycling 5 times.Clean drying is obtained
TiO2/BiVO4Nano-array optoelectronic pole.
The mechanism of action of the invention is：When semiconductor light-catalyst receives light irradiation, absorb wide equal to or more than its forbidden band
The photon of degree causes that electronics is stimulated, and transitting to conduction band from valence band produces light induced electron, and produces light on valence band relevant position
Raw hole, forms photo-generate electron-hole pair.Light induced electron and photohole are respectively provided with very strong oxidability and reducing power.
Photoelectricity is acted on simultaneously under, H2O generates O by Hole oxidation2, and the H in water+It is reduced generation H2。
The TiO that the present invention is obtained2/BiVO4Nano-array composite, growth fraction comparatively dense, and be evenly distributed, sweep
Retouch electron microscopic observation test result as shown in Figure 1.The TiO that the present invention is obtained2/BiVO4Nano-array composite ultraviolet-visible
After spectrophotometer and electrochemical workstation test, extinction reaches 415nm, and photoelectric current reaches 2.51mAcm2(1.23V vs
RHE), test result is distinguished as shown in Figure 2 and Figure 3.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
Should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with scope of the claims
It is defined.
Claims (5)
1.TiO2/BiVO4The preparation method of nano-array optoelectronic pole, it is characterised in that comprise the following steps：
Step one：TiO is prepared by sol-gal process2Seed Layer colloidal sol；
Step 2：TiO is coated in FTO electro-conductive glass substrates using dip-coating method2Seed Layer；
Step 3：After through Overheating Treatment, length there is into TiO2The electro-conductive glass of Seed Layer is placed on TiO2By hydro-thermal in growth solution
Treatment, obtains TiO2Nanometer stick array；
Step 4：Using continuous ionic exchange process by BiVO4Nano-particle deposits to TiO2In nanometer rods, TiO is obtained2/BiVO4Receive
Rice array photoelectric pole.
2. TiO as claimed in claim 12/BiVO4The preparation method of nano-array optoelectronic pole, it is characterised in that the step
One is by ethylene glycol amine (C4H11NO2) and ethanol (C2H5OH) mix, and be added dropwise over butyl titanate (C16H36O4Ti), 0.2 is configured
The Seed Layer colloidal sol of~0.5mol/L.
3. TiO as claimed in claim 12/BiVO4The preparation method of nano-array optoelectronic pole, it is characterised in that the step
Two is to complete TiO in FTO electro-conductive glass using dip-coating method2Plated film, after being dried at 100 DEG C, repeats the above steps to FTO
Electro-conductive glass carries out second membrane, and FTO electro-conductive glass is dried into 1~4h in baking oven is placed after membrane terminates twice.
4. TiO as claimed in claim 12/BiVO4The preparation method of nano-array optoelectronic pole, it is characterised in that the step
Three is to be put into TiO after sample is made annealing treatment2In growth solution, 8~12h of hydro-thermal reaction at 160 DEG C is dried under the conditions of 60 DEG C,
Obtain TiO2Nanometer rods.
5. TiO as claimed in claim 12/BiVO4The preparation method of nano-array optoelectronic pole, it is characterised in that the step
Four is to use continuous ionic exchange process by BiVO4Nano-particle deposits to TiO2In nanometer rods；Under normal temperature, by pucherite
(BiVO4·5H2O) it is dissolved in EGME (CH3OCH2CH2OH in), it is configured to the Bi containing 0.005~0.01mol/L3+Before
Drive liquid solution；Then, by ammonium metavanadate (NH4VO3) be dissolved in 100 DEG C of hot water, it is configured to containing 0.005~0.01mol/L
VO4 3-Precursor solution；Finally, length there is into TiO2The electro-conductive glass of nanometer rods is successively immersed in Bi3+And VO4 3-Presoma it is molten
60s in liquid, repetitive cycling 5~15 times.
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Cited By (5)
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|---|---|---|---|---|
| CN108004526A (en) * | 2017-11-09 | 2018-05-08 | 江苏大学 | A kind of preparation method of phosphorus doping pucherite light anode |
| CN108389727A (en) * | 2018-03-16 | 2018-08-10 | 苏州大学 | Semiconductors coupling heterojunction photovoltaic pole and preparation method thereof |
| CN108686679A (en) * | 2018-05-23 | 2018-10-23 | 西北师范大学 | A kind of preparation method of titanium dioxide/pucherite/bismuth sulfide composite material |
| CN114032552A (en) * | 2021-08-23 | 2022-02-11 | 中山大学 | Titanium dioxide/bismuth vanadate photo-anode and preparation method and application thereof |
| CN114182281A (en) * | 2021-12-10 | 2022-03-15 | 黑龙江省科学院高技术研究院 | Preparation method of mono-crystal-like bismuth vanadate nanorod array with [010] dominant growth orientation |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108004526A (en) * | 2017-11-09 | 2018-05-08 | 江苏大学 | A kind of preparation method of phosphorus doping pucherite light anode |
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| CN108686679A (en) * | 2018-05-23 | 2018-10-23 | 西北师范大学 | A kind of preparation method of titanium dioxide/pucherite/bismuth sulfide composite material |
| CN114032552A (en) * | 2021-08-23 | 2022-02-11 | 中山大学 | Titanium dioxide/bismuth vanadate photo-anode and preparation method and application thereof |
| CN114182281A (en) * | 2021-12-10 | 2022-03-15 | 黑龙江省科学院高技术研究院 | Preparation method of mono-crystal-like bismuth vanadate nanorod array with [010] dominant growth orientation |
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Application publication date: 20170623 |