CN112675922A - Titanium dioxide photocatalytic film with three-layer structure and preparation method thereof - Google Patents
Titanium dioxide photocatalytic film with three-layer structure and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of photocatalytic films, and particularly relates to TiO with a three-layer structure2A photocatalytic film and a preparation method thereof. In the photocatalytic film of the invention, the bottom layer is TiO doped with Mo2The film, the middle layer is methylamine lead-iodine perovskite film, and the top layer is TiO doped with Mo2A film; wherein the Mo-doped concentration of the bottom layer and the top layer is the same or different. The invention adopts the vapor deposition technology under the full vacuum environment and utilizes the magnetron sputtering and vacuum evaporation methods to prepare TiO with a three-layer structure2A photocatalytic film. The invention introduces methylamine lead-iodine perovskite type narrow band gap material into Mo-doped TiO2The film is used as an intermediate layer and can generate a large number of electron-hole pairs under visible light; and a plurality of built-in electric fields which can be modulated are implanted into the film by utilizing the Fermi energy level difference between the multiple layers of film layers and the layers, so that the mobility of carriers is effectively improved. Thus obtaining a multilayer TiO with high efficiency light absorption and photocatalytic activity2The film has good practical value.
Description
Technical Field
The invention belongs to the technical field of photocatalytic films, and particularly relates to TiO with a three-layer structure2A photocatalytic film and a preparation method thereof.
Background
The photocatalysis can deeply react at room temperature and can directly use sunlight as a light source to drive the reaction and other unique properties, thereby becoming an ideal environmental pollution treatment technology and a clean energy production technology. Among the numerous photocatalysts, TiO2The optical property is excellent, the light corrosion resistance is strong, the chemical and mechanical properties are stable, the price is low, and no toxicity is caused to human bodies, so that the optical fiber is always favored by people and has wide application prospect. However, due to TiO2With a wide band gap (anatase E)g=3.20 eV), it is determined that it can absorb only ultraviolet light or the ultraviolet portion of sunlight, and therefore, the light absorption range is widened and TiO is increased2The catalytic activity of the photocatalyst is an important task for popularization and application of the photocatalytic technology. Although in relation to TiO2Modification has been studied a lot, but in TiO2In the aspect of multilayer films, corresponding research is still few so far, and only a few research reports are just preliminary attempts on the feasibility of multilayer films. Students with study[1]A metallic molybdenum-doped core-shell structure of TiO was prepared2Particles which have been found to increase the Fermi energy in the core after dopingGrade, and surrounding with a pure TiO with a relatively low Fermi level2And the shell layer forms a micro nano particle with the Fermi level gradually increasing from outside to inside, and the result shows that the nano particle has higher catalytic performance. In addition, relevant foreign research shows that[2]The external electric field can well inhibit the electron-hole recombination, but the electric field generated in the researches basically comes from the external anode bias voltage rather than from the thin film per se, so that the effect is limited in practical application. The research of the face susceptibility and the like shows that[3, 4]A multilayer of doped TiO2In the thin film structure, as the Fermi level is increased along with the increase of the doping amount, a photon-generated carrier can be diffused at an interface under the driving of the Fermi level difference, positive and negative charges are respectively accumulated at two sides of a crystal boundary to form a built-in electric field, and the separation of the photon-generated carrier can be accelerated by the homojunction electric field between the two interfaces.
In general, when narrow bandgap semiconductors and TiO2When combined, the conduction band of the narrow bandgap semiconductor has a specific value to TiO2And the potential is lower, so that when the photo-induced holes are excited by light irradiation, the photo-induced holes move to a valence band with a more negative energy level, and the photo-induced electrons jump to a conduction band with a higher energy level, and finally, the separation of photo-induced electron-hole pairs is realized. Methylamine lead iodide (CH) as a light collecting material3NH3PbI3) The perovskite material has excellent photoelectric characteristics of high absorption coefficient, high carrier mobility, long diffusion length and the like, so that methylamine lead perovskite and TiO are mixed2The combination can obviously improve TiO2Photocatalytic activity. Methylamine lead iodine is however a very unstable material and will decompose in the presence of moisture or at elevated temperatures, making its practical application very difficult. The invention mixes methylamine lead, iodine calcium titanium ore and TiO2The multilayer films are combined, and Mo is sequentially subjected to vapor deposition under a full vacuum environment: TiO 22And CH3NH3PbI3The film layer, the prepared multilayer film has stable chemical property and photocatalytic property compared with pure TiO2The film is greatly improved, the problem of water vapor erosion to methylamine lead iodine perovskite material is solved, and the film is expected to be widely applied in actual life.
Reference documents:
[1] Liu X G,Ou Z Q,Geng DY, Han Z, J J, Jiang, Liu W, Zhang Z D. Influenceof a graphite shell on the thermal and electromagnetic characteristics of FeNi nanoparticles[J]. Carbon, 2010, 48:891-897.
[2]Domaradzki, J., Kaczmarek, D.,Prociow, E.L., et al. Microstructure and optical propertiesof TiO2 thin films prepared by low pressure hot target reactive magnelron sputtering[J]. G. Thin Solid Films, 2006, 513(1-2):269-274.
[3]preparation of multilayer molybdenum-doped TiO by magnetron sputtering2Photoelectric Properties of the film [ D]University of double denier, 2013.
[4] Shenjie, Luo Sheng Tang and Yan Bing, Chinese patent CN 201210350730.5.
Disclosure of Invention
The invention aims to provide a TiO three-layer structure with high-efficiency light absorption efficiency, higher carrier separation capacity and strong practicability2A photocatalytic film and a preparation method thereof.
The invention provides TiO with a three-layer structure2The schematic diagram of the photocatalytic film is shown in FIG. 1. Wherein the bottom layer is TiO doped with Mo2（Mo:TiO2) The film, the middle layer is methylamine lead iodine perovskite (CH)3NH3PbI3) Film, the top layer is TiO doped with Mo2（Mo:TiO2) The film is a molybdenum-doped titanium dioxide-methylamine lead-iodine perovskite-molybdenum-doped titanium dioxide three-layer structure composite film, and is marked as Mo, TiO2-CH3NH3PbI3- Mo:TiO2. The Mo-doped concentration of the bottom layer and the top layer can be the same or different.
In the invention, the bottom layer and the top layer are Mo and TiO2The film may be prepared under the same conditions or under different conditions.
The bottom layer and the top layer are Mo and TiO2In the film, the doping amount of Mo is 0-3% (preferably 0.1-3%) in terms of Mo/Ti atomic ratio; mo doping amount is zero and is expressed as pure TiO2Film, bottom and top Mo-TiO2The doping amount of Mo in the film is not zero at the same time.
The invention provides the TiO with the three-layer structure2The preparation method of the photocatalytic film adopts a vapor deposition technology under a full vacuum environment and utilizes magnetron sputtering and vacuum evaporation to prepare the photocatalytic film with a three-layer structure. All three film layers are prepared in the same vacuum equipment by adopting a vacuum vapor deposition technology, and are not exposed to any atmosphere or water vapor environment, so that the water vapor is prevented from reacting on CH3NH3PbI3Erosion of the perovskite layer. The preparation method comprises the following specific steps:
(1) depositing a layer of Mo-doped TiO on a cleaned substrate2A base film;
(2) depositing methylamine lead iodine perovskite (CH) on the bottom layer film3NH3PbI3) An intermediate layer;
(3) depositing Mo-doped TiO on the intermediate layer2A top film.
Mo-doped TiO of bottom layer and top layer2The preparation of the film adopts a radio frequency magnetron sputtering method and adopts a molybdenum-embedded titanium dioxide ceramic target, wherein the atomic ratio of Mo to Ti is 0-3% (the atomic ratio is 0.1-3%), and the purity is 99.9%. Molybdenum in the molybdenum-embedded titanium dioxide ceramic target is embedded in a sputtering area on the target in a molybdenum sheet form, and the Mo/Ti atomic ratio in the film is controlled by the product of the area ratio of the molybdenum sheet to the titanium dioxide in the sputtering area and the sputtering rate ratio of the molybdenum sheet to the titanium dioxide; the distance between the target and the substrate is 50-75 mm.
Glass or metal is taken as a substrate, Ar ions are used for bombarding a target material during sputtering, and Mo-doped TiO is2Depositing onto a substrate; wherein the temperature of the substrate is 25-400 ℃; oxygen-argon mixed gas is used during radio frequency magnetron sputtering, the total gas pressure is 0.1 Pa-1.0 Pa, wherein O2Partial pressure accounts for 0.1-5.0% of the total air pressure ratio, the sputtering time is 30-120 min, and the sputtering power density is 10-80 kW/m2(when the target diameter is 60 mm, the sputtering power is 28 to 226W).
Preparing the methylamine lead-iodine perovskite film of the middle layer by adopting a vacuum transportation method, and doping Mo into TiO at the bottom layer2Preparing an intermediate layer on the film: thermal evaporation of PbI2On the bottom layer film; the evaporation boat is tantalum boat, PbI of each evaporation2Mass of the powder0.1-0.5 g, evaporation current of 60-150A, and 1-5 min to obtain composite membrane, which is marked as PbI2-Mo：TiO2(ii) a Then the prepared PbI is added2-Mo：TiO2Transferring the film into a sealable glass container in a vacuum chamber, wherein 0.1-1.0 g of CH is disposed in the container at a position opposite to the film3NH3I, sealing a glass container (the glass container is always in a vacuum state), heating to 100-150 ℃, and preserving heat for 20-120 min to obtain the methylamine lead perovskite film; opening the glass container and taking out the film;
finally, sputtering and depositing a top layer to finish the preparation of the whole three-layer structure film.
In the invention, three layers of Mo and TiO are adopted2-CH3NH3PbI3-Mo:TiO2The total thickness of the film is 300 nm-700 nm; wherein the thickness of the bottom layer film is 50 nm-100 nm, the thickness of the intermediate layer methylamine lead iodoperovskite film is 200 nm-500 nm, and the thickness of the top layer film is 50 nm-100 nm.
The invention uses methylamine lead iodide (CH)3NH3PbI3) Introduction of perovskite type narrow band gap material into Mo-doped TiO2The thin film serves as an intermediate layer, and the semiconductor with the narrow band gap can generate a large number of electron-hole pairs under visible light. On the other hand, a plurality of built-in electric fields which can be modulated are implanted in the film by utilizing the Fermi energy level difference between the multilayer film layer and the interlayer, and the mobility of carriers is effectively improved. Thus, a multilayer TiO having high light absorption and photocatalytic activity is obtained2The film has good practical value.
Test results show that the three-layer Mo and TiO prepared by the invention2-CH3NH3PbI3-Mo:TiO2The film has excellent photocatalytic performance under both ultraviolet light and visible light.
The method has good process stability, and is used for preparing the TiO with high photocatalytic performance2A novel method for thin films; has industrial production prospect.
Drawings
FIG. 1 shows three layers of Mo and TiO2-CH3NH3PbI3-Mo:TiO2Film(s)The structure is schematic.
FIG. 2 shows the photocatalytic performance of the three-layer structure film prepared in example 1. Wherein, (a) the photoproduction current curve under the ultraviolet-visible light, the test condition: sample area 1X 1cm2The light source is a xenon lamp, the wavelength range is 200-800 nm, and the power density is 30mW/cm2The irradiation distance is 50 cm; (b) photodegradation curve of organic dye methylene blue under ultraviolet-visible light, test conditions: sample area 1X 1cm2The light source is a xenon lamp, the wavelength range is 200-800 nm, and the power density is 30mW/cm2The irradiation distance was 50 cm. The comparative sample was pure TiO of the same thickness2A film.
Fig. 3 is a graph showing the photocatalytic performance of the three-layer structure film prepared in example 2. Wherein, (a) a photoproduction current curve under ultraviolet-visible light; (b) photodegradation curve of organic dye methylene blue under uv-visible light. The test conditions were the same as in FIG. 2. The comparative sample was Mo of the same thickness: TiO 22A film.
Fig. 4 is a graph showing the photocatalytic performance of the three-layer structure film prepared in example 3. Wherein, (a) a photoproduction current curve under ultraviolet-visible light; (b) photodegradation curve of organic dye methylene blue under UV-visible light. The test conditions were the same as in FIG. 2. The comparative sample was Mo of the same thickness: TiO 22A film.
Detailed Description
Example 1:
the bottom layer and the top layer are sputtered by pure titanium dioxide: by using TiO2The ceramic target has a substrate temperature of 80 deg.C and a total gas pressure of 0.3Pa, wherein O2The partial pressure accounts for 1.0 percent of the total air pressure, the sputtering time is 60min, the sputtering power is 120W, and the sputtering power density is 42.5kW/m2。
Intermediate perovskite layer CH3NH3PbI3Preparation: firstly PbI2Depositing TiO on the bottom layer by using a thermal evaporation method2Above, the sample was placed in a sealable glass container in a vacuum chamber, and CH was placed in a position opposite to the sample3NH3And I, sealing the glass container (in this case, the glass container is in a vacuum state). Keeping the temperature for 60min in an environment of 120 ℃. The preparation conditions were as follows: the evaporation boat isMolybdenum boat, PbI before each evaporation2The amount of (A) is 0.3g, the evaporation current is 100A, the time is 2min, CH3NH3The amount of I was 0.5 g.
The photocurrent density and photocatalytic degradation performance test results of the sample under ultraviolet-visible light are respectively shown in fig. 2(a) and fig. 2 (b). Three-layer TiO2-CH3NH3PbI3-TiO2Photocurrent of the film sample was about 5.7 × 10-4A/cm2Is pure TiO of the same thickness2Thin film (photocurrent about 6X 10)-5A/cm2) 9.5 times of the total weight of the powder. The photocatalytic degradation rate constant of the three-layer sample is-0.016, and the pure TiO with the same thickness2The film is about-0.011, and the photocatalytic degradation rate is pure TiO21.45 times of the film.
Example 2:
the pure titanium dioxide layers of the bottom layer and the top layer are both changed into Mo: TiO 22Layer, wherein the Mo/Ti atomic ratio in the Mo-doped titania ceramic target was about 0.5%, and the other set-up conditions were the same as in example 1.
The photocurrent density and photocatalytic degradation performance test results of the sample under ultraviolet-visible light are shown in fig. 3(a) and fig. 3(b), respectively. Three layers of Mo: TiO 22-CH3NH3PbI3-Mo：TiO2Photocurrent of about 8.2 x 10 for the thin film sample-4A/cm2The thickness is Mo: TiO 22Thin film (photocurrent about 8X 10)-5A/cm2) 10.3 times of that of pure TiO with the same thickness2The film was 13.7 times brighter. The photocatalytic degradation rate constant of the three-layer sample is-0.022, and the thickness of Mo: TiO 22The film was about-0.013, the photocatalytic degradation rate was Mo: TiO 221.7 times of the film is pure TiO 22 times of the film.
Example 3:
mo of the bottom layer and the top layer: TiO 22The sputtering power in the preparation conditions of the layer was changed to 200W, and the sputtering power density was 70.8kW/m2. The other conditions were the same as in example 2.
The photocurrent density and photocatalytic degradation performance test results of the sample under ultraviolet-visible light are shown in fig. 4(a) and fig. 4 (b), respectively. Three layers of Mo: TiO 22-CH3NH3PbI3- Mo：TiO2Photocurrent of about 8.6 x 10 for the thin film sample-4A/cm2The thickness is Mo: TiO 22Thin film (photocurrent about 8X 10)-5A/cm2) 10.8 times of that of pure TiO with the same thickness2The film was 14.3 times light. The photocatalytic degradation rate constant of the three-layer sample is-0.026, and the ratio of Mo: TiO 22The film was about-0.013, the photocatalytic degradation rate was Mo: TiO 222 times of the film is pure TiO22.4 times of the film.
Claims (6)
1. TiO with three-layer structure2The photocatalytic film is characterized in that the bottom layer is TiO doped with Mo2The film, the middle layer is methylamine lead-iodine perovskite film, and the top layer is TiO doped with Mo2A film; wherein the Mo-doped concentration of the bottom layer and the top layer is the same or different.
2. The tri-layer TiO of claim 12The photocatalytic film is characterized in that the bottom layer and the top layer are doped with Mo TiO2In the film, the doping amount of Mo is 0-3% by Mo/Ti atomic ratio; mo doping amount is zero and is expressed as pure TiO2Film, bottom and top Mo-TiO2The doping amount of Mo in the film is not zero at the same time.
3. The tri-layer TiO according to claim 22The photocatalytic film is characterized in that the total thickness of the three layers of films is 300 nm-700 nm; wherein, the thickness of the bottom layer film is 50 nm-100 nm, the thickness of the middle layer film is 200 nm-500 nm, and the thickness of the top layer film is 50 nm-100 nm.
4. A TiO of the three-layer structure as claimed in any of claims 1 to 32The preparation method of the photocatalytic film is characterized in that a vapor deposition technology under a full vacuum environment is adopted, three layers of films are prepared in the same vacuum equipment by utilizing magnetron sputtering and vacuum evaporation, and the preparation method comprises the following specific steps:
(1) depositing a layer of Mo-doped TiO on a cleaned substrate2A base film;
(2) depositing a methylamine lead perovskite interlayer on the bottom layer film;
(3) depositing Mo-doped TiO on the intermediate layer2A top film.
5. The three-layer TiO of claim 42The preparation method of the photocatalytic film is characterized in that the bottom layer and the top layer of the film are prepared by adopting a radio frequency magnetron sputtering method, a molybdenum-embedded titanium dioxide ceramic target is used, molybdenum in the molybdenum-embedded titanium dioxide ceramic target is embedded in a sputtering area on the target in a molybdenum sheet form, and the Mo/Ti atomic ratio in the film is controlled by the product of the area ratio of the molybdenum sheet to the titanium dioxide in the sputtering area and the sputtering rate ratio of the molybdenum sheet to the titanium dioxide in the sputtering area; the distance between the target and the substrate is 50-75 mm;
bombarding the target material with Ar ions during sputtering to mix Mo-doped TiO2Depositing onto a substrate; wherein the temperature of the substrate is 25-400 ℃; oxygen-argon mixed gas is used during radio frequency magnetron sputtering, the total gas pressure is 0.1 Pa-1.0 Pa, wherein O2Partial pressure accounts for 0.1-5.0% of the total air pressure ratio, the sputtering time is 30-120 min, and the sputtering power density is 10-80 kW/m2。
6. The three-layer TiO of claim 52The preparation method of the photocatalytic film is characterized in that the methylamine lead-iodine perovskite film of the middle layer is prepared by a vacuum transportation method; thermal evaporation of PbI2On the bottom layer film; the evaporation boat is tantalum boat, PbI of each evaporation2The mass of the powder is 0.1-0.5 g, the evaporation current is 60-150A, and the time is 1-5 min; then transferring the prepared film into a sealable glass container in a vacuum chamber, wherein 0.1-1.0 g of CH is arranged in the container at the position opposite to the film3NH3And I, sealing the glass container, heating to 100-150 ℃, and preserving heat for 20-120 min to obtain the methylamine lead-iodine perovskite film.
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| CN102836704A (en) * | 2012-09-20 | 2012-12-26 | 复旦大学 | Molybdenum-doped TiO2 photocatalytic film with three-layer structure and preparation method thereof |
| KR101540364B1 (en) * | 2014-11-05 | 2015-07-30 | 한국과학기술연구원 | ZSO-base perovskite solar cell and its preparation method |
| CN105226187A (en) * | 2015-11-15 | 2016-01-06 | 河北工业大学 | Film crystal silicon perovskite heterojunction solar cell and preparation method thereof |
| CN106732807A (en) * | 2016-11-21 | 2017-05-31 | 西北大学 | A kind of organic perovskite composite photocatalysis film of titanium dioxide and preparation and application |
| CN108493340A (en) * | 2018-03-27 | 2018-09-04 | 武汉理工大学 | A kind of method that steam auxiliary prepares perovskite solar cell |
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Patent Citations (5)
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| CN102836704A (en) * | 2012-09-20 | 2012-12-26 | 复旦大学 | Molybdenum-doped TiO2 photocatalytic film with three-layer structure and preparation method thereof |
| KR101540364B1 (en) * | 2014-11-05 | 2015-07-30 | 한국과학기술연구원 | ZSO-base perovskite solar cell and its preparation method |
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