CN103736500B - A kind of Titanium dioxide/cadmium sulfide/titanium dioxide composite film and application thereof - Google Patents
A kind of Titanium dioxide/cadmium sulfide/titanium dioxide composite film and application thereof Download PDFInfo
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- CN103736500B CN103736500B CN201310718449.7A CN201310718449A CN103736500B CN 103736500 B CN103736500 B CN 103736500B CN 201310718449 A CN201310718449 A CN 201310718449A CN 103736500 B CN103736500 B CN 103736500B
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- titanium dioxide
- cadmium sulfide
- titanium
- composite film
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 224
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 106
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 66
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 239000010408 film Substances 0.000 claims abstract description 62
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 26
- 239000010936 titanium Substances 0.000 claims abstract description 26
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000151 deposition Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 23
- 230000008021 deposition Effects 0.000 claims abstract description 21
- 239000010409 thin film Substances 0.000 claims abstract description 21
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 239000002073 nanorod Substances 0.000 claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 11
- 239000002351 wastewater Substances 0.000 claims abstract description 11
- 230000003197 catalytic effect Effects 0.000 claims abstract description 8
- 230000015556 catabolic process Effects 0.000 claims description 15
- 238000006731 degradation reaction Methods 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000005566 electron beam evaporation Methods 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 10
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000010894 electron beam technology Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract 1
- 238000003672 processing method Methods 0.000 abstract 1
- 150000003608 titanium Chemical class 0.000 abstract 1
- 238000004065 wastewater treatment Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 4
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 4
- 229940012189 methyl orange Drugs 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000005518 electrochemistry Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 2
- 239000010815 organic waste Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses a kind of Titanium dioxide/cadmium sulfide/titanium dioxide composite film and application thereof that belong to technical field of waste water processing. The method adopts growth method titanium deposition in substrate, obtain the nano-stick array thin film that discreteness is good, this titanium thin film is annealed 2 hours under 450 DEG C of air conditionses and obtains titanium dioxide nanorod array film, utilizing SILAR method deposition cadmium sulfide nanoparticles to obtain titanium dioxide/cadmium sulfide laminated film on titanic oxide nanorod array, this thin film has good treatment of Organic Wastewater effect under visible light. Depositing layer of titanium dioxide on thin film again with atomic layer deposition method on titanium dioxide/cadmium sulfide laminated film, this titanium dioxide/cadmium sulfide/titania structure is compared the visible ray organic wastewater degraded efficiency of titanium dioxide/cadmium sulfide and is significantly improved. This processing method is simple, and visible light catalytic performance boost is obvious, has wide practical use in wastewater treatment.
Description
Technical field
The invention belongs to technical field of waste water processing, be specifically related to a kind of Titanium dioxide/cadmium sulfide/titanium dioxide composite film and application thereof.
Background technology
Along with the development of society, energy shortage and problem of environmental pollution are day by day serious, and the utilization of regenerative resource is just seemed particularly urgent by people. Catalysis material can utilize reproducible solar energy that the organic pollution in environment is resolved into innocuous substance, it is believed that is the environmental pollution control technique having application prospect most. But for the widely used semiconductor light-catalyst titanium dioxide with inexpensive, nontoxic, chemically stable, high catalytic efficiency, owing to its energy gap is at about 3.0eV, only with only accounting for the sunlight ultraviolet light less than 5%. Improve titanium dioxide and be an up the effective way of its practical application in the utilization ratio of the visible ray accounting for sunlight about 45%.
A kind of effective way by quasiconductor (cadmium sulfide) compound of narrow band gap and titanium dioxide, with Atomic layer deposition method titanium dioxide/cadmium sulfide composite construction titanium deoxid film one layer uniform, fine and close deposited above be then a kind of new effectively promote titanium dioxide/cadmium sulfide composite film visible light when catalytic efficiency degradation of organic substances waste water method.
Summary of the invention
It is an object of the invention to provide a kind of Titanium dioxide/cadmium sulfide/titanium dioxide composite film and application thereof, utilize ald (AtomicLayerDeposition, ALD) method deposition of titanium oxide thin film on titanium dioxide/cadmium sulfide laminated film, thus realizing improving its catalytic efficiency under visible light.
In order to achieve the above object, the technical solution used in the present invention is as follows:
A kind of Titanium dioxide/cadmium sulfide/titanium dioxide composite film, adopts Atomic layer deposition method to deposit layer of titanium dioxide thin film on titanium dioxide/cadmium sulphide membrane, obtains Titanium dioxide/cadmium sulfide/titanium dioxide composite film.
The thickness of above-mentioned titanium deoxid film is 0.65-2nm.
The cycle-index of above-mentioned continuous print Atomic layer deposition method is 20-60 time.
Above-mentioned titanium dioxide/cadmium sulphide membrane is prepared from by the following method:
(1) cleaned electro-conductive glass substrate is fixed on the sample stage of electron beam evaporation deposition machine;
(2) adopting titanium is target, and the chamber of electron beam evaporation deposition machine is evacuated to 3 × 10-8～5 × 10-8The fine vacuum of Torr;
(3) adjusting electron beam incident angle to 65～85 degree, the substrate surface thereof at sample stage grows the thick titanium nano-stick array thin film of 300-600nm;
(4) titanium nano-stick array thin film is annealed 2 hours at 450 DEG C, obtain titanium dioxide nanorod array film;
(5) on titanium dioxide nano-rod thin film, deposit cadmium sulfide nanoparticles by continuous ionic layer adsorption reaction sedimentation, obtain titanium dioxide/cadmium sulphide membrane.
Cleaning in step (1) for carrying out supersound process successively by electricity substrate of glass in acetone, ethanol, deionized water.
Step (3) make sample stage rotate with the speed of 0～10rpm.
The annealing of step (4) uses tube furnace to carry out in air atmosphere.
In step (5), cadmium sulfide nanoparticles is sized to 5nm～30nm.
The application in catalytic degradation organic wastewater of the above-mentioned Titanium dioxide/cadmium sulfide/titanium dioxide composite film.
The invention has the beneficial effects as follows by preparing titanium deoxid film with atomic layer deposition method on titanium dioxide/cadmium sulfide laminated film, preparation Titanium dioxide/cadmium sulfide/titanium dioxide composite film, thus the catalytic performance promoted under the visible light conditions of material system, maximum lift efficiency is up to 100%. The method is simple, cost is low, be effectively improved visible light conditions under catalytic efficiency.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the Titanium dioxide/cadmium sulfide/titanium dioxide composite film of preparation in embodiment 1;
Fig. 2 is the transmission electron microscope photo of the Titanium dioxide/cadmium sulfide/titanium dioxide composite film of preparation in embodiment 2;
Fig. 3 is the degradation rate of the Titanium dioxide/cadmium sulfide/titanium dioxide composite film degradation of organic waste water that different atomic layer deposition cycles number of times obtain under visible ray illumination in 1 hour;
Fig. 4 is the device schematic diagram preparing titanium nano-stick array thin film;
In figure, 1-substrate, 2-deposits thin film, 3-angle of incidence, 4-solid matter, 5-melted material, 6-electron beam.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is illustrated, but protection domain not thereby limiting the invention.
Embodiment 1
(1) by substrate of glass 1 acetone, ethanol, deionized water ultrasonic cleaning one by one and dry;
(2) pretreated substrate of glass 1 is fixed on the sample stage of electron beam evaporation deposition machine;
(3) adopting titanium is target, and target is in Fig. 3 solid matter 4 and melted material 5, and the chamber of electron beam evaporation deposition machine is evacuated to 3 × 10-8～5 × 10-8The fine vacuum of Torr;
(4) adjusting angle of incidence 3 to 85 degree of electron beam 6, and make sample stage static or rotate with the speed of 10rpm, substrate 1 surface thereof at sample stage grows titanium deposition thin film thick for 300nm;
(5) within 2 hours, titanium dioxide nanorod array film is obtained by annealing under titanium nano-stick array thin film in atmosphere 450 DEG C of temperature;
(6) with continuous ionic layer adsorption reaction sedimentation deposit on titanium dioxide nano-rod cadmium sulfide nanoparticles formation titanium dioxide/cadmium sulfide laminated film, cadmium sulfide nanoparticles be sized to 5nm～30nm;
(7) by the titanium deoxid film of the Atomic layer deposition method 2nm that depositing homogeneous is fine and close on titanium dioxide/cadmium sulfide laminated film thickness, the cycle-index of ald is 60 times, obtain Titanium dioxide/cadmium sulfide/titanium dioxide composite film, its transmission electron microscope photo is as shown in Figure 1, show successfully to prepare the laminated film of titanium dioxide (Rutile)/cadmium sulfide (the CdS)/titanium dioxide of Rutile Type, wherein the titanium dioxide of new deposition is amorphous state, and titanium dioxide film layer thickness is 2nm.
(8) preparation Titanium dioxide/cadmium sulfide/titanium dioxide composite film carrying out the Optical Electro-Chemistry test under visible light conditions and the methyl orange simulated wastewater of 10mmol/L is carried out Visible Light Induced Photocatalytic, degradation efficiency is shown in Fig. 3.
Embodiment 2
(1) by substrate of glass 1 acetone, ethanol, deionized water ultrasonic cleaning one by one and dry;
(2) pretreated substrate of glass 1 is fixed on the sample stage of electron beam evaporation deposition machine;
(3) adopting titanium is target, and target is in Fig. 3 solid matter 4 and melted material 5, and the chamber of electron beam evaporation deposition machine is evacuated to 3 × 10-8～5 × 10-8The fine vacuum of Torr;
(4) adjusting angle of incidence 3 to 85 degree of electron beam 6, and make sample stage static or rotate with the speed of 10rpm, substrate 1 surface thereof at sample stage grows titanium deposition thin film thick for 300nm;
(5) within 2 hours, titanium dioxide nanorod array film is obtained by annealing under titanium nano-stick array thin film in atmosphere 450 DEG C of temperature;
(6) with continuous ionic layer adsorption reaction sedimentation deposit on titanium dioxide nano-rod cadmium sulfide nanoparticles formation titanium dioxide/cadmium sulfide laminated film, cadmium sulfide nanoparticles be sized to 5nm～30nm;
(7) by the titanium deoxid film of the Atomic layer deposition method 2.8nm that depositing homogeneous is fine and close on titanium dioxide/cadmium sulfide laminated film thickness, the cycle-index of ald is 80 times, obtain Titanium dioxide/cadmium sulfide/titanium dioxide composite film, its transmission electron microscope photo is as shown in Figure 2, show successfully to prepare the laminated film of titanium dioxide (Rutile)/cadmium sulfide (the CdS)/titanium dioxide of Rutile Type, wherein the titanium dioxide of new deposition is amorphous state, and titanium dioxide film layer thickness is 2.8nm.
(8) preparation Titanium dioxide/cadmium sulfide/titanium dioxide composite film carrying out the Optical Electro-Chemistry test under visible light conditions and the methyl orange simulated wastewater of 10mmol/L is carried out Visible Light Induced Photocatalytic, degradation efficiency is shown in Fig. 3.
Embodiment 3:
(1) by substrate of glass 1 acetone, ethanol, deionized water ultrasonic cleaning one by one and dry;
(2) pretreated substrate of glass 1 is fixed on the sample stage of electron beam evaporation deposition machine;
(3) adopting titanium is target, and target is in Fig. 3 solid matter 4 and melted material 5, and the chamber of electron beam evaporation deposition machine is evacuated to 3 × 10-8～5 × 10-8The fine vacuum of Torr;
(4) adjusting angle of incidence 3 to 85 degree of electron beam 6, and make sample stage static or rotate with the speed of 10rpm, substrate 1 surface thereof at sample stage grows titanium deposition thin film thick for 300nm;
(5) within 2 hours, titanium dioxide nanorod array film is obtained by annealing under titanium nano-stick array thin film in atmosphere 450 DEG C of temperature;
(6) with continuous ionic layer adsorption reaction sedimentation deposit on titanium dioxide nano-rod cadmium sulfide nanoparticles formation titanium dioxide/cadmium sulfide laminated film, cadmium sulfide nanoparticles be sized to 5nm～30nm;
(7) by the titanium deoxid film that the Atomic layer deposition method 0.65nm that depositing homogeneous is fine and close on titanium dioxide/cadmium sulfide laminated film is thick, the cycle-index of ald is 20 times, prepares Titanium dioxide/cadmium sulfide/titanium dioxide composite film;
(8) preparation Titanium dioxide/cadmium sulfide/titanium dioxide composite film carrying out the Optical Electro-Chemistry test under visible light conditions and the methyl orange simulated wastewater of 10mmol/L is carried out Visible Light Induced Photocatalytic, degradation efficiency is shown in Fig. 3.
Embodiment 4: the degradation rate of the Titanium dioxide/cadmium sulfide/titanium dioxide composite film that different ald (ALD) cycle-indexes obtain.
As shown in Figure 3, investigate Titanium dioxide/cadmium sulfide/titanium dioxide composite film that different ALD cycle number of times obtains degradation rate to the methyl orange simulated wastewater of 10mmol/L under visible ray illumination in 1 hour, wherein it is expressed as 0 time without ALD process, for titanium dioxide/cadmium sulphide membrane, and other are Titanium dioxide/cadmium sulfide/titanium dioxide composite film. The titanium deoxid film thickness (nm) of outer layer and the relation of atomic layer deposition cycles number of times are y=0.0336x-0.019, R2=0.9999。
Degradation efficiency by the relatively degradation of organic waste water of the laminated film that different atomic layer deposition cycles number of times obtain, the cycle-index that discovery is not Atomic layer deposition method is more high, the titania coextruded film of new deposition is more thick, its degradation efficiency is more high, but be 20-60 time at atomic layer deposition cycles number of times, that is only degradation efficiency can just be strengthened when the titania coextruded film thickness of new deposition is 0.65-2nm, and when atomic layer deposition cycles number of times reaches 80 times, the titania coextruded film that thickness is 2.8nm of new deposition can reduce its degradation efficiency on the contrary.
Claims (8)
1. a Titanium dioxide/cadmium sulfide/titanium dioxide composite film, it is characterised in that adopt continuous print Atomic layer deposition method to deposit layer of titanium dioxide thin film on titanium dioxide/cadmium sulphide membrane, obtain Titanium dioxide/cadmium sulfide/titanium dioxide composite film;
Described titanium dioxide/cadmium sulphide membrane is specifically prepared from by the following method:
(1) cleaned electro-conductive glass substrate is fixed on the sample stage of electron beam evaporation deposition machine;
(2) adopting titanium is target, and the chamber of electron beam evaporation deposition machine is evacuated to 3 × 10-8～5 × 10-8The fine vacuum of Torr;
(3) adjusting electron beam incident angle to 65～85 degree, the substrate surface thereof at sample stage grows the titanium nano-stick array thin film that 300～600nm is thick;
(4) titanium nano-stick array thin film is annealed 2 hours at 450 DEG C, obtain titanium dioxide nanorod array film;
(5) on titanium dioxide nano-rod thin film, deposit cadmium sulfide nanoparticles by continuous ionic layer adsorption reaction sedimentation, obtain titanium dioxide/cadmium sulphide membrane.
2. Titanium dioxide/cadmium sulfide/titanium dioxide composite film according to claim 1, it is characterised in that the thickness of described titanium deoxid film is 0.65-2nm.
3. Titanium dioxide/cadmium sulfide/titanium dioxide composite film according to claim 1, it is characterised in that the cycle-index of described continuous print Atomic layer deposition method is 20-60 time.
4. Titanium dioxide/cadmium sulfide/titanium dioxide composite film according to claim 1, it is characterised in that clean described in step (1) as electricity substrate of glass being carried out successively in acetone, ethanol, deionized water supersound process.
5. Titanium dioxide/cadmium sulfide/titanium dioxide composite film according to claim 1, it is characterised in that make sample stage rotate with the speed of 0～10rpm in step (3).
6. Titanium dioxide/cadmium sulfide/titanium dioxide composite film according to claim 1, it is characterised in that the described annealing of step (4) uses tube furnace to carry out in air atmosphere.
7. Titanium dioxide/cadmium sulfide/titanium dioxide composite film according to claim 1, it is characterised in that described in step (5), cadmium sulfide nanoparticles is sized to 5nm～30nm.
8. the application in catalytic degradation organic wastewater of the Titanium dioxide/cadmium sulfide/titanium dioxide composite film described in claim 1.
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| CN104916743A (en) * | 2015-06-17 | 2015-09-16 | 许昌学院 | Thermal evaporation method for preparing stoichiometric CdS thin film by using quantum dots as precursors |
| CN108201893B (en) * | 2016-12-20 | 2020-10-09 | 北京大学深圳研究生院 | FeSxThin film, hydrazinophenylene compound, and deposition method and preparation method thereof |
| JP2020054931A (en) * | 2017-01-27 | 2020-04-09 | 国立研究開発法人科学技術振興機構 | Structure and method for manufacturing the same |
| CN109103101B (en) * | 2017-06-21 | 2020-09-29 | 清华大学 | Preparation method of nano-microstructure |
| CN109574190A (en) * | 2018-12-14 | 2019-04-05 | 南京大学盐城环保技术与工程研究院 | A kind of catalyst of catalytic ozonation and preparation method thereof |
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| CN1692979A (en) * | 2005-03-23 | 2005-11-09 | 天津大学 | Photocatalyst used for purifying organic pollutants and its prepn. method |
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