CN106676565A - Fe2-xTixO3/FTO photo-anode preparing technology and treatment method capable of improving photocurrent density of photo-anode - Google Patents
Fe2-xTixO3/FTO photo-anode preparing technology and treatment method capable of improving photocurrent density of photo-anode Download PDFInfo
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Abstract
The invention discloses a Fe2-xTixO3/FTO photo-anode preparing technology and a treatment method capable of improving photocurrent density of a photo-anode. According to the Fe2-xTixO3/FTO photo-anode preparing technology, a photo-anode precursor is prepared in hydrothermal environment with solubility trivalent ferric salt and alkali metal nitrates serving as a titanium source in an organic titanium solution and FTO conductive glass serving as a carrier, and the treatment method is adopted for treating the precursor; through the photoelectricity test, it shows that after the photo-anode is prepared through the technology, the photocurrent density of Ar-Fe2-xTixO3/FTO is 2.6 0mA/cm<2> at 1.23eV, the photocurrent density of Air-Fe2O3/FTO is 0.12 mA/cm<2> at 1.23eV, and the photocurrent density is improved by more than 21 times. Therefore, according to the prepared photo-anode and the treatment method of the photo-anode, the advanced technical means with the low energy consumption and the efficient water decomposition is achieved, the good industrial application prospect is achieved, and the technology and the method can be used for relieving the global increasingly-strained energy supply situation at present.
Description
Technical field
The invention belongs to solar cell material preparing technical field, and in particular to a kind of Fe2-xTixO3 growth in situ is arrived
Light anode is prepared on the tin ash (electro-conductive glass, referred to as " FTO ") of Fluorin doped, the light anode can be with after special handling
Greatly improve the processing method of density of photocurrent.
Background technology
Our economy is set easily to be produced unstable by the impact of rise in price the strong depend-ence of Fossil fuel
Increase, and the excessive of Fossil fuel uses aggravation air pollution and global warming.Therefore, exploitation cleaning, reproducible replacement
Fossil fuel is a very urgent problem, and in various alternative energy sources strategy, hydrogen is by acknowledged for optimal new
The energy.How its not only nontoxic pollution-free, calorific value is high, and raw material sources are extensive, then the production hydrogen of efficient stable low energy consumption
Have become the significant problem in the puzzlement world.It is considered as optimal hydrogen source method to decompose Aquatic product hydrogen.It is known that
Water decomposition reaction by decomposition Aquatic product hydrogen and decompose Aquatic product two half-reactions of oxygen constitute, through countries in the world scientist for many years
Research find water decomposition chemical reaction face a dynamics problem, that is, decompose Aquatic product oxygen be determine reaction speed control
Step；This single step reaction carry out required for activation energy it is higher, for Optical Electro-Chemistry decomposition water reaction needed for apply overpotential compared with
Height, and the density of photocurrent for producing is relatively low, thus causes photoelectric decomposition Aquatic product hydrogen to there is a problem of high energy consumption.Based on this, I adopts
Fe2-xTixO3/FTO light anodes are prepared with the preparation method of hydro-thermal reaction and produces oxygen come water decomposition, using the special place of the present invention
Reason method makes its density of photocurrent be greatly enhanced processing Fe2-xTixO3/FTO light anodes, the photoelectricity of low energy consumption after being
Decomposition water provides a kind of significant method.
The content of the invention
The Fe2O3 light anode density of photocurrent prepared in order to solve prior art is relatively low, it is impossible to efficient photoelectric decomposition
The problem of Aquatic product oxygen, the present invention has made intensive studies to the mechanism of photoelectrolysis Aquatic product oxygen, is paying substantial amounts of original labor
After dynamic, and then complete the present invention.
A kind of Fe2-xTixO3/FTO light anodes technology of preparing of the present invention and improve the process of its density of photocurrent
Method, wherein Fe2-xTixO3/FTO light anodes technology of preparing are by ferric nitrate, ferric chloride, ferric acetate, iron sulfate
The one kind of one kind in a kind of and sodium nitrate, potassium nitrate in titanium tetrachloride, butyl titanate, three isopropyl titanates is done titanium source and is existed
FTO electro-conductive glass is used as preparing in the thermal and hydric environment of carrier.Processing method of the present invention is above-mentioned preparing
500~800 DEG C are calcined under a kind of Fe2-xTixO3/FTO light anodes atmosphere first in air, oxygen or nitrogen, oxygen gaseous mixture
Calcining 1~5 hour, waits and drops to after room temperature again in nitrogen, argon, 300~400 DEG C of heating 10~60 under a kind of atmosphere in helium
Minute, wait drop to after room temperature take out sample obtained Fe2-xTixO3/FTO light anodes to be prepared of the invention.The present invention
(argon) Ar-Fe2-xTixO3/FTO after the handling process of the present invention is electric at 1.23 electron-volts (eV) for the light anode of preparation
The density of photocurrent of pressure is 2.60 milliamperes/centimetre 2 (mA/cm2), and (air) Air-Fe2O3/FTO is under 1.23eV voltages
Density of photocurrent be 0.12mA/cm2, density of photocurrent improve exceeded 21 times.
Therefore the light anode and its processing method that prepared by the present invention is a kind of with the elder generation for realizing low energy consumption high-efficiency decomposition water
Enter one of technological means, with good prospects for commercial application, can be to alleviate the energy supply of current whole world growing tension
General layout.
A kind of Fe2-xTixO3/FTO light anodes technology of preparing of the present invention and improve the process of its density of photocurrent
Method, its step is as follows：
(1) to the one kind filled in 3~5 grams of ferric nitrate, ferric chloride, ferric acetate, iron sulfate and 5~10 grams of sodium nitrates,
80~120 ml deionized waters are added in a kind of beaker of the solid particle in potassium nitrate, stirs complete to dissolving；
(2) titanium tetrachloride, butyl titanate are taken, 0.5~2 milliliter of solution of the one kind in three isopropyl titanates is added thereto to 50
A kind of~200 milliliters of ethanol, the organic solvent in methanol, are uniformly mixed；
(3) 500~1000 microlitres of solution are taken out from step (2) to be added in step (1), is stirred 10~40 minutes；
(4) the FTO slice, thin pieces for reducing good certain area are put into into ultrasound wave in water to clean 20~40 minutes, in placing into ethanol
Ultrasound wave is cleaned 20~40 minutes, is placed into ultrasound wave in acetone solvent and is cleaned 20~40 minutes, finally with high pure nitrogen or argon
A kind of FTO slice, thin pieces dried up after cleaning in gas；
(5) the teflin tape stainless steel lining bottom that 25~40 milliliters of solution in step (3) is added to 50 milliliters is taken
In reactor, then FTO electro-conductive glass slice, thin pieces cleaned in step (4) are put in above-mentioned reactor, wherein FTO conduction glass
The conduction of glass slice, thin piece faces down and leans to reactor wall with 30~60 degree of placements；
(6) reactor of step (5) is transferred in electric drying oven with forced convection, reaction temperature is controlled at 90~110 DEG C,
10~15 hours response time.Upper Fe2-xTixO3/FTO pieces have been grown when reaction finishes to be taken out when temperature of reaction kettle is down to room temperature
Son, deionized water rinses multiple, is then placed in being dried 8~12 hours in 50~80 DEG C of electric drying oven with forced convections；
(7) Fe2-xTixO3/FTO slice, thin pieces prepared by step (6) are calcined into 500~800 DEG C of calcinings 1~5 in high temperature furnace
Hour；
(8) will in step (7) burnt Fe2-xTixO3/FTO slice, thin pieces again in nitrogen, argon, in helium
300~400 DEG C are heated 10~60 minutes under kind of atmosphere, wait dropping to take out after room temperature sample and obtained of the invention to be prepared
Fe2-xTixO3/FTO light anodes.
The CHI760E electrochemical workstations of Jing Shanghai occasion China production and 300 watts of xenon lamps test of Beijing Zhong Jiaojin sources production,
Using three-electrode system, (platinum electrode is used as to electrode；Saturation silver/silver chloride electrode is used as reference electrode；Prepare
Fe2-xTixO3/FTO light anodes are used as working electrode).The present invention prepare light anode through the present invention handling process after,
Density of photocurrent of the Ar-Fe2-xTixO3/FTO under 1.23eV voltages is 2.60mA/cm2, and Air-Fe2O3/FTO exists
Density of photocurrent under 1.23eV voltages is 0.12mA/cm2, and density of photocurrent is improved and exceeded 21 times.
The present invention greatly improves can the efficiency of photoelectrocatalysiss decomposition water, because relatively low overpotential causes disappearing for the energy
Consumption is less, further meets industrialized requirement, is that sustainable production hydrogen energy source solves the problems, such as kinetics.Therefore originally
Invention is a very significant innovation and creation.
Description of the drawings
Fig. 1：A () and (b) is respectively the X-ray diffractometer of corresponding A ir-Fe2O3/FTO and Ar-Fe2-xTixO3/FTO
(XRD) phenogram.
Fig. 2：Air-Fe2O3/FTO and Ar-Fe2-xTixO3/FTO Flied emissions tunnel scanning electron microscope diagram
(FESEM)。
Fig. 3：A () and (b) is respectively the solid violet of corresponding A ir-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO
Outward-visible absorption spectra figure (UV-vis DRS).
Fig. 4：(a) and (b) be respectively by Air-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO solid it is ultraviolet-
The energy band diagram that visible absorption spectra figure (UV-vis) conversion is obtained.
Fig. 5：It is Air-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO that embodiment 3 and embodiment 4 are prepared
Photoelectron spectroscopy figure (XPS).
Fig. 6：The photoelectric properties phenogram of light anode prepared by different embodiments；A () is pure Fe2O3 prepared by embodiment 1
The anode photocurrent curve obtained after calcining under air atmosphere；(b) be under the pure Fe2O3 argon gas atmospheres of embodiment 2 calcination processing it
Anode photocurrent curve afterwards；C () is that anode photoelectric current is bent after calcining under the Fe2O3 air atmospheres that the Ti of embodiment 3 adulterates
Line；D () is the anode photocurrent curve after the Fe2O3 argon gas atmosphere calcination processings of the Ti doping of embodiment 4.
Fig. 7：The photoelectric properties phenogram of light anode prepared by different embodiments；A () is the Ti doping of embodiment 5
Anode photocurrent curve after Fe2O3 argon gas atmosphere calcination processings；B () is the Fe2O3 nitrogen atmospheres of the Ti doping of embodiment 4
Anode photocurrent curve after calcination processing.
Specific embodiment
Below by specific embodiment, the present invention is described in detail, but the purposes of these exemplary embodiments and
Purpose is only used for enumerating the present invention, not constitutes any type of any restriction to the real protection scope of the present invention, more non-to incite somebody to action
Protection scope of the present invention is confined to this.
Embodiment 1
(1) to filling 4.0545 grams of ferric chlorides (purity >=99.0%) and 8.4992 grams of sodium nitrates (purity >=99.5%)
100 ml deionized waters are added in the beaker of solid particle, stirs complete to dissolving；
(2) the FTO slice, thin pieces for reducing good certain area are put into into ultrasound wave in water to clean 30 minutes, place into ultrasound in ethanol
Ripple is cleaned 30 minutes, is placed into ultrasound wave in acetone solvent and is cleaned 30 minutes, finally dries up the FTO pieces after cleaning with high pure nitrogen
Son；
(3) reaction that 35 milliliters of solution in step (1) is added to 50 milliliters of teflin tape stainless steel lining bottom is taken
In kettle, then FTO slice, thin pieces cleaned in step (2) are put in above-mentioned reactor, wherein the conduction of FTO electro-conductive glass slice, thin piece
Face down and lean to the 45 degree of placements of reactor wall；
(4) reactor of step (3) is transferred in electric drying oven with forced convection, reaction temperature is controlled at 100 DEG C, reaction
12 hours time, the FTO slice, thin pieces for having grown upper Fe2O3 are taken out when temperature of reaction kettle is down to room temperature when reaction is finished, use deionization
Water is rinsed well, is then placed in being dried 10 hours in 60 DEG C of electric drying oven with forced convections；
(5) the Fe2O3/FTO slice, thin pieces for preparing step (4) are calcined 2 hours for 700 DEG C in high temperature furnace, are waited and are dropped to after room temperature
Take out sample obtained it is of the invention to be prepared Air (air)-Fe2O3/FTO light anodes, be labeled as Air-Fe2O3/FTO；
Through Optical Electro-Chemistry test, density of photocurrent is 0.12mA/cm2 under the voltage of 1.23eV.
Embodiment 2
(1) step (1)~(5) are with embodiment 1；
(6) Air (the air)-Fe2O3/FTO slice, thin pieces for preparing step (5) calcine under an argon atmosphere again 350 DEG C of calcinings
30 minutes, wait drop to take out after room temperature sample obtained it is of the invention to be prepared Ar (argon)-Fe2O3/FTO light anodes, mark
It is designated as Ar-Fe2O3/FTO；Through Optical Electro-Chemistry test, density of photocurrent is 0.42mA/cm2 under the voltage of 1.23eV.
Embodiment 3
(1) to filling 4.0545 grams of iron chloride (purity >=99.0%) and 8.4992 grams of sodium nitrates (purity >=99.5%) are solid
100 ml deionized waters are added in the beaker of body granule, stirs complete to dissolving；
(2) take 1 milliliter of titanium tetrachloride (purity >=99.5%) solution to be added thereto to 100 milliliters of dehydrated alcohol (ethanol contains
Amount >=99.5%), it is uniformly mixed；
(3) 750 microlitres of solution are taken out from step (2) to be added in step (1), is stirred 30 minutes；
(4) the FTO slice, thin pieces for reducing good certain area are put into into ultrasound wave in water to clean 30 minutes, place into ultrasound in ethanol
Ripple is cleaned 30 minutes, is placed into ultrasound wave in acetone solvent and is cleaned 30 minutes, finally dries up the FTO pieces after cleaning with high pure nitrogen
Son；
(5) reaction that 35 milliliters of solution in step (3) is added to 50 milliliters of teflin tape stainless steel lining bottom is taken
In kettle, then FTO slice, thin pieces cleaned in step (4) are put in above-mentioned reactor, the conduction of wherein FTO slice, thin pieces faces down tiltedly
By the 45 degree of placements of reactor wall；
(6) reactor of step (5) is transferred in electric drying oven with forced convection, reaction temperature is controlled at 100 DEG C, reaction
12 hours time.The FTO slice, thin pieces for having grown upper Fe2-xTixO3 are taken out when temperature of reaction kettle is down to room temperature when reaction is finished, is spent
Ionized water is rinsed well, is then placed in being dried 10 hours in 60 DEG C of electric drying oven with forced convections；
(7) Fe2-xTixO3/FTO slice, thin pieces prepared by step (6) are calcined into 700 DEG C in high temperature furnace to calcine 2 hours, waits drop
To after room temperature take out sample obtained it is of the invention to be prepared Air (air)-Fe2-xTixO3/FTO light anodes, be labeled as
Air-Fe2-xTixO3/FTO；Through Optical Electro-Chemistry test, density of photocurrent is 1.54mA/cm2 under the voltage of 1.23eV.
Embodiment 4
(2) step (1)~(6) are with embodiment 3；
(7) FeTiO3/F slice, thin pieces prepared by step (6) are calcined into 700 DEG C in high temperature furnace to calcine 2 hours, waits and drop to room temperature
After take out sample；
(8) will burnt Fe2-xTixO3/FTO slice, thin pieces 350 DEG C of heating 30 under an argon atmosphere again in step (7)
Minute, wait drop to after room temperature take out sample obtained it is of the invention to be prepared Ar (argon)-Fe2-xTixO3/FTO light anodes,
It is labeled as Ar-Fe2-xTixO3/FTO；Through Optical Electro-Chemistry test, density of photocurrent is 2.60mA/ under the voltage of 1.23eV
cm2。
Embodiment 5
(1) step (1)~(6) are with embodiment 3；
(7) Fe2-xTixO3/FTO slice, thin pieces prepared by step (6) are calcined into 700 DEG C in high temperature furnace to calcine 2 hours, waits drop
Sample is taken out to after room temperature；
(8) will burnt Fe2-xTixO3/FTO slice, thin pieces 350 DEG C of heating 30 in a nitrogen atmosphere again in step (7)
Minute, wait drop to after room temperature take out sample obtained it is of the invention to be prepared N2 (nitrogen)-Fe2-xTixO3/FTO light anodes,
It is labeled as N2-Fe2-xTixO3/FTO；Through Optical Electro-Chemistry test, density of photocurrent is 2.60mA/ under the voltage of 1.23eV
cm2。
Hereinafter contrast test is carried out to light anode prepared by embodiment 1-5, obtain following result.
Fig. 1：A () and (b) are respectively that the X-ray of corresponding A ir-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO is spread out
The phenogram of instrument (XRD) is penetrated, (a) and (b) all demonstrates what the light anode of preparation was made up of the Fe2O3 that FTO and Ti adulterates.By
It is too small in the shared ratios in system of Ti, therefore can not be shown in XRD spectra.By the comparison of (a) and (b),
There is no significant change in the crystallinity of Air-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO.
Fig. 2：Air-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO Flied emissions tunnel scanning electron microscope diagram
(FESEM)；(A) and (C) is the stereoscan photograph of Air-Fe2-xTixO3/FTO in figure；(B) and (D) is Ar-Fe2- in figure
The stereoscan photograph of xTixO3/FTO.Compare the nanometer rods it can be seen that Ar-Fe2-xTixO3/FTO arrays from (A) and (B)
Length will increased than Air-Fe2-xTixO3/FTO, (B) with (D) it can be seen that the cause of Ar-Fe2-xTixO3/FTO arrays
Density is higher than Air-Fe2-xTixO3/FTO arrays.
Fig. 3：A () and (b) is respectively the solid violet of corresponding A ir-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO
Outward-visible absorption spectra figure (UV-vis DRS), by (a) and (b) relatively can be seen that Air-Fe2-xTixO3/FTO and
The initial absorption wavelength of both Ar-Fe2-xTixO3/FTO be all 750 nanometers (nm) left and right, but in whole spectral region
The intensity of the absworption peak of Ar-Fe2-xTixO3/FTO occurs in that red shift apparently higher than Air-Fe2-xTixO3/FTO, this be by
What the dimensional effect of array nanometer rods caused.
Fig. 4：(a) and (b) be respectively by Air-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO solid it is ultraviolet-
The energy band diagram that visible absorption spectra figure (UV-vis) conversion is obtained.Air-Fe2- relatively can be seen that by (a) and (b)
There is no significant change in the bandwidth of xTixO3/FTO and Ar-Fe2-xTixO3/FTO, be 1.95 electron-volts
(eV)。
Fig. 5：It is Air-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO that embodiment 3 and embodiment 4 are prepared
Photoelectron spectroscopy figure (XPS).All (a) in wherein Fig. 5 is the Air-Fe2-xTixO3/FTO light that embodiment 3 is prepared
Anode, all (b) in Fig. 5 is the Ar-Fe2-xTixO3/FTO light anodes that embodiment 4 is prepared.From Fig. 5 A
Survey figures can draw, in two kinds of light anodes of Air-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO Fe, O are contained,
Tri- kinds of elements of C, and it is not found the presence of Ti.This is because the doping of Ti is relatively low caused.C comes from test environment.
Fe 2p figures from Fig. 5 B in two kinds of light anodes of Air-Fe2-xTixO3/FTO and Ar-Fe2-xTixO3/FTO as can be seen that have
The peak of Fe 2p3/2, Fe 2p1/2 and Fe3+, illustrates Fe in the form of Fe2O3.Fe2+ peaks represent oxygen defect, explanation
Oxygen defects of the Air-Fe2-xTixO3/FTO compared with Ar-Fe2-xTixO3/FTO is more.From the O 1s peaks of Fig. 5 C it can also be seen that in knot
Closing can represent oxygen defect for the peak at 531.8eV positions, show Air-Fe2-xTixO3/FTO compared with Ar-Fe2-xTixO3/FTO's
Oxygen defect is more.Draw from the Ti 2p of Fig. 5 D, Ti is present in light anode prepared by embodiment 3 and embodiment 4 really.
Fig. 6：The photoelectric properties phenogram of light anode prepared by different embodiments.A () is pure Fe2O3 prepared by embodiment 1
The anode photocurrent curve obtained after calcining under air atmosphere；(b) be under the pure Fe2O3 argon gas atmospheres of embodiment 2 calcination processing it
Anode photocurrent curve afterwards；C () is that anode photoelectric current is bent after calcining under the Fe2O3 air atmospheres that the Ti of embodiment 3 adulterates
Line；D () is the anode photocurrent curve after the Fe2O3 argon gas atmosphere calcination processings of the Ti doping of embodiment 4.By (a) and
C the comparison of () can be seen that the Fe2O3 that Ti adulterates is significantly improved than the density of photocurrent of pure Fe2O3, by (b) and (d)
Comparison can be seen that pure Fe2O3 and Ti doping Fe2O3 after argon gas atmosphere calcination processing density of photocurrent obtain
The raising for becoming apparent from.
Fig. 7：The photoelectric properties phenogram of light anode prepared by different embodiments.A () is the Ti doping of embodiment 5
Anode photocurrent curve after Fe2O3 argon gas atmosphere calcination processings；B () is the Fe2O3 nitrogen atmospheres of the Ti doping of embodiment 4
Anode photocurrent curve after calcination processing.Can be seen that the species of noble gases to light anode by the comparison of (a) and (b)
The impact of density of photocurrent is not obvious.
Example is to sum up prepared, we draw conclusion further below：
(1) the iron sesquioxide Fe2O3 that a small amount of titanium source formation titanium (Ti) doping is introduced in preparation process can be notable
Improve density of photocurrent.
(2) density of photocurrent can significantly be improved by last inert gas shielding heating in preparation process, but
It is that impact of the species of noble gases to light anode density of photocurrent is simultaneously little.
Claims (6)
1. a kind of Fe2-xTixO3/ FTO light anodes technology of preparing and improve the processing method of its density of photocurrent, it is characterised in that
Its step is as follows：
(1) 80~120 milliliters are added in a kind of and 5~10 grams of nitrate solid particles the beaker filled in 3~5 grams of iron salt
Deionized water, stirs complete to dissolving；
(2) take 0.5~2 milliliter of solution of titaniferous Organic substance and be added thereto to 50~200 milliliters of organic solvents, be uniformly mixed；
(3) 500~1000 microlitres of solution are taken out from step (2) to be added in step (1), is stirred 10~40 minutes；
(4) the FTO slice, thin pieces for reducing good certain area are put into into ultrasound wave in water to clean 20~40 minutes, place into ultrasound in ethanol
Ripple is cleaned 20~40 minutes, is placed into ultrasound wave in acetone solvent and is cleaned 20~40 minutes, finally with high pure nitrogen or argon
It is a kind of dry up cleaning after FTO slice, thin pieces；
(5) reaction that 25~40 milliliters of solution in step (3) is added to 50 milliliters of teflin tape stainless steel lining bottom is taken
In kettle, then FTO electro-conductive glass slice, thin pieces cleaned in step (4) are put in above-mentioned reactor, wherein FTO electro-conductive glass piece
The conduction of son faces down and leans to reactor wall with 30~60 degree of placements；
(6) reactor of step (5) is transferred in electric drying oven with forced convection, reaction temperature is controlled at 90~110 DEG C, reaction
10~15 hours time.Upper Fe has been grown when reaction finishes to be taken out when temperature of reaction kettle is down to room temperature2-xTixO3/ FTO slice, thin pieces, use
Deionized water rinsing repeatedly, is then placed in being dried 8~12 hours in 50~80 DEG C of electric drying oven with forced convections；
(7) Fe for preparing step (6)2-xTixO3/ FTO slice, thin pieces are calcined 500~800 DEG C in high temperature furnace and are calcined 1~5 hour；
(8) will in step (7) burnt Fe2-xTixO3/ FTO slice, thin pieces again under inert gas atmosphere 300~400 DEG C plus
Heat 10~60 minutes, wait drop to after room temperature take out sample obtained Fe to be prepared of the invention2-xTixO3/ FTO light anodes.
2. Fe as claimed in claim 12-xTixO3/ FTO light anodes technology of preparing and improve the process side of its density of photocurrent
Method, it is characterised in that the iron salt in described step (1) is the one kind in ferric nitrate, ferric chloride, ferric acetate, iron sulfate.
3. Fe as claimed in claim 12-xTixO3/ FTO light anodes technology of preparing and improve the process side of its density of photocurrent
Method, it is characterised in that the nitrate in described step (1) is the one kind in sodium nitrate, potassium nitrate.
4. Fe as claimed in claim 12-xTixO3/ FTO light anodes technology of preparing and improve the process side of its density of photocurrent
Method, it is characterised in that the titaniferous Organic substance in described step (2) is titanium tetrachloride, butyl titanate, in three isopropyl titanates
It is a kind of.
5. Fe as claimed in claim 12-xTixO3/ FTO light anodes technology of preparing and improve the process side of its density of photocurrent
Method, it is characterised in that the organic solvent in described step (2) be ethanol, the one kind in methanol.
6. Fe as claimed in claim 12-xTixO3/ FTO light anodes technology of preparing and improve the process side of its density of photocurrent
Method, it is characterised in that the noble gases in described step (8) be nitrogen, argon, the one kind in helium.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107805822A (en) * | 2017-09-30 | 2018-03-16 | 华南理工大学 | A kind of Ti Fe2O3/ Co Pi complex light electrodes and preparation method thereof |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104617355A (en) * | 2013-11-04 | 2015-05-13 | 中国科学院大连化学物理研究所 | Alpha-Fe2O3 photo-anode and preparation method thereof |
| CN105597784A (en) * | 2015-12-29 | 2016-05-25 | 浙江工商大学 | MoS2-doped iron oxide photocatalytic thin film and preparation method as well as application thereof to treatment of phenolic waste water |
| CN105597723A (en) * | 2014-10-28 | 2016-05-25 | 西安圣合通环保科技有限公司 | Supported TiO2 photocatalyst preparation method |
| CN105601124A (en) * | 2016-01-08 | 2016-05-25 | 福州大学 | Method for preparing porous alpha-Fe2O3 photo-anode |
| CN105837194A (en) * | 2016-03-21 | 2016-08-10 | 国家纳米科学中心 | Titanium-doped alpha-iron oxide photo-anode, and preparation method and application thereof |
| CN106119882A (en) * | 2016-07-29 | 2016-11-16 | 苏州大学 | The preparation of iron titanate/iron sesquioxide complex light electrode and surface modifying method |
| CN107326385A (en) * | 2017-06-16 | 2017-11-07 | 中国科学院化学研究所 | A kind of preparation method of boron doping di-iron trioxide optoelectronic pole |
-
2016
- 2016-12-09 CN CN201611221187.3A patent/CN106676565B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104617355A (en) * | 2013-11-04 | 2015-05-13 | 中国科学院大连化学物理研究所 | Alpha-Fe2O3 photo-anode and preparation method thereof |
| CN105597723A (en) * | 2014-10-28 | 2016-05-25 | 西安圣合通环保科技有限公司 | Supported TiO2 photocatalyst preparation method |
| CN105597784A (en) * | 2015-12-29 | 2016-05-25 | 浙江工商大学 | MoS2-doped iron oxide photocatalytic thin film and preparation method as well as application thereof to treatment of phenolic waste water |
| CN105601124A (en) * | 2016-01-08 | 2016-05-25 | 福州大学 | Method for preparing porous alpha-Fe2O3 photo-anode |
| CN105837194A (en) * | 2016-03-21 | 2016-08-10 | 国家纳米科学中心 | Titanium-doped alpha-iron oxide photo-anode, and preparation method and application thereof |
| CN106119882A (en) * | 2016-07-29 | 2016-11-16 | 苏州大学 | The preparation of iron titanate/iron sesquioxide complex light electrode and surface modifying method |
| CN107326385A (en) * | 2017-06-16 | 2017-11-07 | 中国科学院化学研究所 | A kind of preparation method of boron doping di-iron trioxide optoelectronic pole |
Cited By (14)
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|---|---|---|---|---|
| CN107805822A (en) * | 2017-09-30 | 2018-03-16 | 华南理工大学 | A kind of Ti Fe2O3/ Co Pi complex light electrodes and preparation method thereof |
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| WO2023082384A1 (en) * | 2021-11-09 | 2023-05-19 | 东莞理工学院 | Anode material for photoelectric degradation of tetracycline, and preparation method therefor |
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