CN101837289A - TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method - Google Patents
TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method Download PDFInfo
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- CN101837289A CN101837289A CN201010213904A CN201010213904A CN101837289A CN 101837289 A CN101837289 A CN 101837289A CN 201010213904 A CN201010213904 A CN 201010213904A CN 201010213904 A CN201010213904 A CN 201010213904A CN 101837289 A CN101837289 A CN 101837289A
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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
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Abstract
The invention discloses a TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method, and relates to a surface modification method of a nano titanium dioxide film photocatalyst. The method solves the problem of low catalysis activity of a traditional immobilized titanium dioxide photocatalyst. The method comprises the following steps that: first, a nano titanium dioxide film is first prapred on a TC4 titanium alloy through an anodic oxidation method; and then the nano titanium dioxide film is put into a tube furnace to be heated to 300 to 600DEG C, the heat is insulated for 1 to 3h, and the film is cooled with the furnace. The method successfully prepares a Ti and V composite oxide, the hydrogen production rate of the obtained modified nano titanium dioxide film photocatalyst in photocatalytic hydrogen production is 1.18 times of that of the titanium dioxide film which does not receive heat treatment, and the photocatalytic hydrogen production performance is improved.
Description
Technical field
The present invention relates to a kind of surface modifying method of nano-titanium dioxide film photocatalyst.
Background technology
Environment and energy crisis are the severe problems that human survival and development are faced.Because the product of combustion of hydrogen is a water, the combustion heat is high and can any pollution not arranged to the border, so Hydrogen Energy is that everybody pays close attention to one of maximum green source at present; And solar energy is a kind of inexhaustible, nexhaustible natural source, utilizes solar photolysis water hydrogen to become people's focus of research at present, and 1972 years Fujishima and Honda find TiO
2Can photolysis water hydrogen, in recent decades, the theory and technology that people produce hydrogen to photocatalysis has carried out going deep into extensive studies, obtained very big progress, but also had some problem demanding prompt solutions, the catalyst of the nano powder powder of process modification has good product hydrogen effect, but owing to reclaim difficulty, both can't reuse, and be discharged in the environment and can pollute again, be emphasis and the difficult point of studying so preparation has high visible immobilization semiconductor light-catalyst active and photostability.
But TiO
2Be wide band gap semiconducter, the energy gap of anatase is 3.2eV, and the energy gap of rutile is 3.0eV, mainly wavelength is just had absorption less than the ultraviolet light of 400nm; Exist light induced electron-hole to shortcomings such as the life-span are short, the photocatalytic process quantum efficiency is low in addition.V
2O
5Energy gap is 2.24eV.Can absorb the sunshine of λ≤564nm, V with this narrow band gap
2O
5TiO with broad-band gap
2Be compound to the utilization rate that has improved light together.V
2O
5/ TiO
2The coupled mode catalyst, be widely used in some industrial important catalytic reactions, comprise the selective oxidation reaction of dimethylbenzene, the ammoxidation reaction of hydrocarbon, the M.R.Bayati of Iranian University of Science and Technology, method with differential arc oxidation (MAO), with pure titanium is matrix, and electrolyte is the NaVO3 of 0.03M, uses AC power, applying voltage is 250 ~ 500V, and having prepared energy gap is the (V of 2.58eV narrow band gap
2O
5) x-(TiO
2) rete of 1-x nanometer sheet structure.Though realized the nanometer and the immobilization of catalyst, but nano particle is disordered structure to be arranged, on nano particle, there are a large amount of crystal boundaries and blemish, these crystal boundaries and blemish meeting trapped electrons, thereby cause light induced electron and hole-recombination probability big, thereby influenced the catalytic activity of photochemical catalyst.
Summary of the invention
The objective of the invention is provides a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method in order to solve the low problem of catalytic activity of existing immobilized titanium dioxide photochemical catalyst.
TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method of the present invention is realized by following steps: one, prepare nano-titanium dioxide film on TC4 titanium matrix: TC4 titanium matrix is carried out preliminary treatment remove surface film oxide, then pretreated TC4 titanium matrix is placed electrolyte as working electrode, the copper sheet conduct is to electrode, the control response voltage is 10 ~ 30V, carry out constant voltage anodic oxidation 20 ~ 120min, promptly obtain nano-titanium dioxide film on TC4 titanium matrix, wherein electrolyte consists of: the NH of 5 ~ 6g/L
4F and volumetric concentration are 2% ~ 5% H
3PO
4Solution, solvent are water; Two, the TC4 titanium matrix after step 1 is handled is put into tube furnace, tube furnace is heated to 300 ~ 600 ℃ then, insulation 1 ~ 3h, cool off i.e. titanium dioxide film photocatalyst after obtaining modification on the TC4 titanium matrix with stove again, promptly finish the TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method.
The present invention realizes the heat treatment surface modification of nano-titanium dioxide film by two-step method, the modifying titanium dioxide film photocatalyst that obtains having the Ti-O-V nanostructured, and wherein, vanadium is with the form and the TiO of vanadic anhydride
2Be combined with each other.The nano-titanium dioxide film of step 1 preparation is the TiO that arranges in order
2Nano-tube array has been realized the ordering and the nanometer of immobilized titanium dioxide film; In tube furnace in the air atmosphere after the heat treatment, V element high temperature (300 ~ 600 ℃) is oxidized to V in the nano-titanium dioxide film that step 1 is obtained through step 2
2O
5, and and TiO
2Be combined with each other, obtained having the modifying titanium dioxide film photocatalyst of Ti-O-V nanostructured.The orderly TiO that arranges
2Nano-tube array is owing to have the pore passage structure of one dimension, electronics transmits along hole wall, has avoided the contact of intergranule, has therefore quickened the transfer rate of electronics, effectively improve the right separative efficiency in light induced electron-hole, thereby improved the photocatalytic activity of nano-titanium dioxide film photocatalyst.
Heat treatment surface modification method preparation technology of the present invention is simple, and preparation process is controlled easily, and V comes from TC4 titanium matrix, then V
2O
5With TiO
2Compound even, can effectively improve the right separative efficiency in light induced electron-hole.
The titanium dioxide film photocatalyst of the present invention after the modification that obtains on the TC4 titanium matrix strengthens the absorption of visible light wave range; The effect of photocatalysis hydrogen production reaches 22.3 μ L/hcm than the hydrogen-producing speed of the photocatalysis hydrogen production of existing nano-titanium dioxide film simultaneously
2, be hydrogen-producing speed (the 18.86 μ L/hcm of the nano-titanium dioxide film of not heat-treating
2) 1.18 times.
Description of drawings
Fig. 1 is the uv-vis spectra spectrogram of the titanium dioxide film photocatalyst after the modification that obtains of the specific embodiment 11 to 14; Fig. 2 is x-ray photoelectron spectroscopy (XPS) spectrogram of the nano-titanium dioxide film photocatalyst after the modification that obtains of the specific embodiment 12; Fig. 3 is the light application time of the nano-titanium dioxide film photocatalyst after the modification that obtains of the specific embodiment 12 and the graph of relation of hydrogen output; Fig. 4 is the SEM shape appearance figure of the nano-titanium dioxide film photocatalyst after the modification that obtains of the specific embodiment 12; Fig. 5 is the Raman spectrum spectrogram of the nano-titanium dioxide film photocatalyst after the modification that obtains of the specific embodiment 12.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: present embodiment TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method is realized by following steps: one, on TC4 titanium matrix, prepare nano-titanium dioxide film: TC4 titanium matrix is carried out preliminary treatment remove surface film oxide, then pretreated TC4 titanium matrix is placed electrolyte as working electrode, the copper sheet conduct is to electrode, the control response voltage is 10 ~ 30V, carry out constant voltage anodic oxidation 20 ~ 120min, promptly obtain nano-titanium dioxide film on TC4 titanium matrix, wherein electrolyte consists of: the NH of 5 ~ 6g/L
4F and volumetric concentration are 2% ~ 5% H
3PO
4Solution, solvent are water; Two, the TC4 titanium matrix after step 1 is handled is put into tube furnace, tube furnace is heated to 300 ~ 600 ℃ then, insulation 1 ~ 3h, cool off i.e. titanium dioxide film photocatalyst after obtaining modification on the TC4 titanium matrix with stove again, promptly finish the TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method.
Present embodiment realizes the heat treatment surface modification of nano-titanium dioxide film by two-step method, the modifying titanium dioxide film photocatalyst that obtains having the Ti-O-V nanostructured, and wherein, vanadium is with the form and the TiO of vanadic anhydride
2Be combined with each other.
Heat treatment surface modification method preparation technology of the present invention is simple, and preparation process is controlled easily, and V comes from TC4 titanium matrix, then V
2O
5With TiO
2Compound even, can effectively improve the right separative efficiency in light induced electron-hole.Titanium dioxide film photocatalyst after the modification that obtains on the TC4 titanium matrix strengthens the absorption of visible light wave range; The effect of photocatalysis hydrogen production reaches 22.3 μ L/hcm than the hydrogen-producing speed of the photocatalysis hydrogen production of existing nano-titanium dioxide film simultaneously
2, be hydrogen-producing speed (the 18.86 μ L/hcm of the nano-titanium dioxide film of not heat-treating
2) 1.18 times.
The specific embodiment two: present embodiment and the specific embodiment one are different is in the step 1 TC4 titanium matrix to be carried out preliminary treatment to remove the concrete operations of surface film oxide and be: with hydrofluoric acid and red fuming nitric acid (RFNA) according to volume ratio be the ratio of 1:1 mix mixed acid solution, then the titanium matrix is immersed in the mixed acid solution, parked 1 ~ 2s in mixed acid solution, take out then, rinse well with deionized water, and then with in the titanium matrix immersion mixed acid solution, parked 1 ~ 2s, take out then, repeat aforesaid operations 1 ~ 4 time.Other step and parameter are identical with the specific embodiment one.
Concrete repetitive operation number of times can be by the light decision that become of titanium matrix surface in the present embodiment.
The specific embodiment three: what present embodiment was different with the specific embodiment one or two is that the control response voltage is 15 ~ 25V in the step 1.Other step and parameter are identical with the specific embodiment one or two.
The specific embodiment four: what present embodiment was different with the specific embodiment one or two is that the control response voltage is 20V in the step 1.Other step and parameter are identical with the specific embodiment one or two.
The specific embodiment five: what present embodiment was different with one of specific embodiment one to four is to carry out constant voltage anodic oxidation 30 ~ 90min in the step 1.Other step and parameter are identical with one of specific embodiment one to four.
The specific embodiment six: what present embodiment was different with one of specific embodiment one to four is to carry out constant voltage anodic oxidation 60min in the step 1.Other step and parameter are identical with one of specific embodiment one to four.
The specific embodiment seven: what present embodiment was different with one of specific embodiment one to six is that electrolyte consists of in the step 1: the NH of 5g/L
4F and volumetric concentration are 3% H
3PO
4Solution.Other step and parameter are identical with one of specific embodiment one to six.
The specific embodiment eight: what present embodiment was different with one of specific embodiment one to seven is tube furnace to be heated to 400 ~ 500 ℃ then in the step 2.Other step and parameter are identical with one of specific embodiment one to seven.
The specific embodiment nine: what present embodiment was different with one of specific embodiment one to eight is to be incubated 1.5 ~ 2.5h in the step 2.Other step and parameter are identical with one of specific embodiment one to eight.
The specific embodiment ten: what present embodiment was different with one of specific embodiment one to eight is to be incubated 2h in the step 2.Other step and parameter are identical with one of specific embodiment one to eight.
The specific embodiment 11: present embodiment TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method is realized by following steps: one, prepare nano-titanium dioxide film on TC4 titanium matrix: TC4 titanium matrix is carried out preliminary treatment remove surface film oxide, then pretreated TC4 titanium matrix is placed electrolyte as working electrode, the copper sheet conduct is to electrode, the control response voltage is 20V, carry out constant voltage anodic oxidation 30min, promptly obtain nano-titanium dioxide film on TC4 titanium matrix, wherein electrolyte consists of: the NH of 5g/L
4F and volumetric concentration are 3% H
3PO
4Solution, solvent are water; Two, the TC4 titanium matrix after step 1 is handled is put into tube furnace, tube furnace is heated to 300 ℃ then, insulation 2h, cool off i.e. titanium dioxide film photocatalyst after obtaining modification on the TC4 titanium matrix with stove again, promptly finish the TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method.
The response area of the TA1 titanium sheet of present embodiment step 1 is 2.5 * 4cm
2, the top of conversion zone is wrapped with sealing with adhesive tape, and purpose is prevent electrolyte soaring.To dropwise required time be 1 ~ 2h to penetration enhancer in the step 2.In the step 1 TA1 titanium sheet being carried out preliminary treatment removes the concrete operations of surface film oxide and is: with hydrofluoric acid and red fuming nitric acid (RFNA) according to volume ratio be the ratio of 1:1 mix mixed acid solution, then the titanium matrix is immersed in the mixed acid solution, parked 1 ~ 2s in mixed acid solution, take out then, rinse well with deionized water, and then the titanium matrix is immersed in the mixed acid solution parked 1 ~ 2s, take out then, repeat aforesaid operations 2 times.
The titanium dioxide film photocatalyst of present embodiment after to the modification that obtains carries out the uv-vis spectra test, and the ultraviolet-visible absorption spectroscopy curve that obtains is shown in curve among Fig. 11; As a comparison, present embodiment obtains nano-titanium dioxide film (without the heat treatment of step 2 tube furnace) to step 1 and carries out the uv-vis spectra test on TA1 titanium sheet, and the ultraviolet-visible absorption spectroscopy curve that obtains is shown in curve among Fig. 15; Contrasted as seen by curve among Fig. 11 and curve 5, the nano-titanium dioxide film photocatalyst behind the heat treatment surface modification of present embodiment has stronger absorption at visible light wave range.
The specific embodiment 12: what present embodiment and the specific embodiment 11 were different is tube furnace to be heated to 400 ℃ then in the step 2.Other step and parameter are identical with the specific embodiment 11.
The nano-titanium dioxide film photocatalyst of present embodiment after to the modification that obtains carries out the uv-vis spectra test, and the ultraviolet-visible absorption spectroscopy curve that obtains is shown in curve among Fig. 12; In the comparison diagram 1 curve 2 and curve 5 as can be known, the nano-titanium dioxide film photocatalyst after the heat treatment surface modification of present embodiment is handled has stronger absorption at visible light wave range.
The nano-titanium dioxide film photocatalyst of present embodiment after obtaining modification on the TC4 titanium matrix carries out x-ray photoelectron spectroscopy (XPS) test, and the xps energy spectrum figure that test obtains is shown in curve among Fig. 22.As a comparison, the nano-titanium dioxide film (structure is a nano-tube array) that the present embodiment step 1 is prepared carries out x-ray photoelectron spectroscopy (XPS) test, and test result is shown in curve among Fig. 21.Curve 1 and curve 2 are as can be known in the comparison diagram 2, nano-titanium dioxide film is through after calcining heat treatment, occurred the peak of pentavalent vanadium V2p3/2 and V2p1/2 respectively at 517.5ev and 524.8eV, can prove on the nano-titanium dioxide film through the nano-tube array structure after the calcining heat treatment to have generated V
2O
5
Present embodiment is carried out the photocatalysis hydrogen production performance test to the nano-titanium dioxide film photocatalyst for preparing, and method of testing is: with the quartz glass tube reactor, and 0.1mol/LNa
2S and 0.02mol/LNa
2SO
3The aqueous solution for the reaction target, under the irradiation of 500W xenon lamp, the hydrogen that collect to produce, the distance of xenon lamp and quartz glass tube is 10cm, the reactivity of evaluation photochemical catalyst.The photocatalytic degradation time that obtains and the relation curve of hydrogen output are shown in curve among Fig. 31, and hydrogen-producing speed is 22.3 μ L/hcm
2As a comparison, present embodiment obtains nano-titanium dioxide film (without the heat treatment of step 2 tube furnace) to step 1 and carries out the test of photocatalytic degradation hydrogen production by water decomposition effect on TA1 titanium sheet, the photocatalytic degradation time that obtains and the relation curve of hydrogen output are shown in curve among Fig. 32.Hydrogen-producing speed is 18.86 μ L/hcm
2By among Fig. 3 as can be known, behind the heat treatment surface modification of present embodiment, it is big that the hydrogen output of its photocatalytic degradation hydrogen production by water decomposition becomes, it is big that hydrogen-producing speed becomes, hydrogen-producing speed is not have 1.18 times of heat treated titanium deoxid film.
The SEM of the nano-titanium dioxide film photocatalyst after the modification that present embodiment prepares (SEM) shape appearance figure as shown in Figure 4, as seen from Figure 4, nano-titanium dioxide film photocatalyst after the modification still has nano-tube array structure, and is structurally ordered.
The nano-titanium dioxide film photocatalyst of present embodiment after to the modification for preparing carries out the Raman spectrum test, test result as shown in Figure 5, " A " expression Detitanium-ore-type among the figure, " R " represents rutile-type.As shown in Figure 5, constitute by Detitanium-ore-type and two kinds of crystal formations of rutile-type through 400 ℃ of calcining post-modification nano-titanium dioxide films.Wherein, at 143cm
-1The peak be the Raman vibration that causes by Detitanium-ore-type O-Ti-O bending mode, be by the flexible Raman vibration that causes of the symmetry of Detitanium-ore-type O-Ti-O key at the 648cm-1 peak.238cm
-1The peak at place is because the Raman that the rocking vibration of rutile titanyl key causes vibrates, and 448cm
-1Vibration frequency then is to belong to rutile O-Ti-O torsional vibration.
The specific embodiment 13: what present embodiment and the specific embodiment 11 were different is tube furnace to be heated to 500 ℃ then in the step 2.Other step and parameter are identical with the specific embodiment 11.
The titanium dioxide film photocatalyst of present embodiment after to the modification that obtains carries out the uv-vis spectra test, and the ultraviolet-visible absorption spectroscopy curve that obtains is shown in curve among Fig. 13; In the comparison diagram 1 curve 3 and curve 5 as can be known, the nano-titanium dioxide film photocatalyst after the heat treatment surface modification of present embodiment is handled has stronger absorption at visible light wave range.
The specific embodiment 14: what present embodiment and the specific embodiment 11 were different is tube furnace to be heated to 500 ℃ then in the step 2.Other step and parameter are identical with the specific embodiment 11.
The titanium dioxide film photocatalyst of present embodiment after to the modification that obtains carries out the uv-vis spectra test, and the ultraviolet-visible absorption spectroscopy curve that obtains is shown in curve among Fig. 14; In the comparison diagram 1 curve 4 and curve 5 as can be known, the nano-titanium dioxide film photocatalyst after the heat treatment surface modification of present embodiment is handled has stronger absorption at visible light wave range.
Claims (10)
1. TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method, it is characterized in that the TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method realizes by following steps: one, on TC4 titanium matrix, prepare nano-titanium dioxide film: TC4 titanium matrix is carried out preliminary treatment remove surface film oxide, then pretreated TC4 titanium matrix is placed electrolyte as working electrode, the copper sheet conduct is to electrode, the control response voltage is 10 ~ 30V, carry out constant voltage anodic oxidation 20 ~ 120min, promptly obtain nano-titanium dioxide film on TC4 titanium matrix, wherein electrolyte consists of: the NH of 5 ~ 6g/L
4F and volumetric concentration are 2% ~ 5% H
3PO
4Solution, solvent are water; Two, the TC4 titanium matrix after step 1 is handled is put into tube furnace, tube furnace is heated to 300 ~ 600 ℃ then, insulation 1 ~ 3h, cool off i.e. titanium dioxide film photocatalyst after obtaining modification on the TC4 titanium matrix with stove again, promptly finish the TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method.
2. a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method according to claim 1, it is characterized in that in the step 1 TC4 titanium matrix carried out preliminary treatment removes the concrete operations of surface film oxide and is: with hydrofluoric acid and red fuming nitric acid (RFNA) according to volume ratio be the ratio of 1:1 mix mixed acid solution, then the titanium matrix is immersed in the mixed acid solution, parked 1 ~ 2s in mixed acid solution, take out then, rinse well with deionized water, and then with in the titanium matrix immersion mixed acid solution, parked 1 ~ 2s, take out then, repeat aforesaid operations 1 ~ 4 time.
3. a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method according to claim 1 and 2 is characterized in that the control response voltage is 15 ~ 25V in the step 1.
4. a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method according to claim 1 and 2 is characterized in that the control response voltage is 20V in the step 1.
5. a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method according to claim 3 is characterized in that carrying out in the step 1 constant voltage anodic oxidation 30 ~ 90min.
6. a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method according to claim 3 is characterized in that carrying out in the step 1 constant voltage anodic oxidation 60min.
7. according to claim 1,2,5 or 6 described a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification methods, it is characterized in that electrolyte consists of in the step 1: the NH of 5g/L
4F and volumetric concentration are 3% H
3PO
4Solution.
8. a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification method according to claim 7 is characterized in that tube furnace being heated to 400 ~ 500 ℃ then in the step 2.
9. according to claim 1,2,5,6 or 8 described a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification methods, it is characterized in that being incubated in the step 2 1.5 ~ 2.5h.
10. according to claim 1,2,5,6 or 8 described a kind of TC4 matrix nano titanium dioxide film photocatalyst heat treatment surface modification methods, it is characterized in that being incubated in the step 2 2h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433787A (en) * | 2019-08-08 | 2019-11-12 | 清远市简一陶瓷有限公司 | A kind of nano-titania photocatalyst and preparation method thereof |
| CN110624560A (en) * | 2019-09-17 | 2019-12-31 | 吉林师范大学 | FeVO for photo-Fenton combined catalysis4/TiO2Porous catalyst membrane layer material and preparation method thereof |
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| CN101140961A (en) * | 2007-10-16 | 2008-03-12 | 哈尔滨工业大学 | Method for in-situ upgrowth titanic oxide thin film electric pole |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433787A (en) * | 2019-08-08 | 2019-11-12 | 清远市简一陶瓷有限公司 | A kind of nano-titania photocatalyst and preparation method thereof |
| CN110624560A (en) * | 2019-09-17 | 2019-12-31 | 吉林师范大学 | FeVO for photo-Fenton combined catalysis4/TiO2Porous catalyst membrane layer material and preparation method thereof |
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Application publication date: 20100922 |