CN101635320B - Method for manufacturing titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device - Google Patents
Method for manufacturing titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device Download PDFInfo
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- CN101635320B CN101635320B CN2009100650808A CN200910065080A CN101635320B CN 101635320 B CN101635320 B CN 101635320B CN 2009100650808 A CN2009100650808 A CN 2009100650808A CN 200910065080 A CN200910065080 A CN 200910065080A CN 101635320 B CN101635320 B CN 101635320B
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Abstract
The invention provides a method for manufacturing a titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device, which mainly comprises the steps: preparing colloidal sol, preparing TiO2 mesoporous film by ageing and calcining, plating a molybdenum electrode, and finally obtaining the titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device. The TiO2 mesoporous film ultraviolet photoelectric detection prototype device prepared by the method has simple structure and good photoelectricity response performance for ultraviolet ray. Furthermore, the invention also has the characteristics of high controllable degree, simpler manufacture, easy operation and good repetitiveness, thus forming large-scale production.
Description
Technical field
The invention belongs to technical field of function materials, relate to a kind of manufacture method of titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device.
Background technology
It is strong and be applicable to adverse circumstances good characteristics such as (as hot environments) that the wide bandgap semiconductor ultraviolet light detector has an antijamming capability, have significant application value at scientific research, military affairs, space flight, environmental protection, fire prevention and many industrial control fields. at present, the material that is used to make ultraviolet light detector mainly contains Si, SiC, GaN, ZnO and diamond etc., the technology of Si base ultraviolet detector is ripe relatively, but need subsidiary filter, so there is certain limitation in its practical application.
Great majority research now all concentrates on the semiconductor material with wide forbidden band, with TiO
2As a kind of oxide semiconductor material, energy gap is bigger, visible light is absorbed hardly, and its chemical stability and weatherability is good, and preparation technology is ripe relatively.In recent years, utilize TiO
2Gas-sensitive property, UV absorption and photovoltaic property to be applied to the research of gas sensitive device, photocatalysis and solar cell aspect very active, become the research focus of domestic and international association area.TiO
2Mesopore film is big because of its specific area, have more surface state, bringing into play more and more important effect in fields such as photocatalysis, chemical sensor, luminescent material, electrochromic device and solar cells.So far, employing dc reactive magnetron sputtering technique such as Zhang Liwei has prepared TiO on the ITO quartz substrate
2Film adopts C/TiO
2/ ITO three-decker has been studied anatase TiO
2The ultraviolet light response of film, but the shortcoming of this experiment is a complex structure, is difficult for forming large-scale production.With TiO
2Mesopore film is made the research work of ultraviolet light detector, yet there are no report both at home and abroad.
Summary of the invention
The purpose of this invention is to provide a kind ofly has fine photoelectric response performance and the manufacture method of the titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device that can accomplish scale production to ultraviolet ray.
For achieving the above object, the present invention by the following technical solutions: a kind of manufacture method of titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device, adopt the following steps preparation:
(1) be that 1: 0.003～0.008: 20～80 titanium tetrachloride, blocked polyethers F-127 and absolute ethyl alcohol add in the flask and mix with mass ratio, stirring reaction is 10～20 minutes in ice-water bath, remove ice-water bath then, in flask, add 0.6～3.6ml distilled water, under the normal temperature stirring reaction 4～6 hours colloidal sol;
(2) substrate of glass of cleaning is immersed in the colloidal sol that step (1) makes, slowly lift substrate of glass again, make the surface coverage of substrate of glass that colloidal sol be arranged, the substrate of glass that is coated with colloidal sol was placed in the closed container ageing 24～120 hours, then the substrate of glass after the ageing is calcined in air, the heating rate with 1～2 ℃/min during calcining is warming up to 300～450 ℃, insulation 4～6h, naturally cool to room temperature, obtain transparent TiO
2Mesopore film;
(3) adopt the mode of vacuum sputtering at TiO
2Mesopore film simultaneously plates the molybdenum electrode of two interval 1～3mm, obtains titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device.
During described vacuum sputtering earlier at TiO
2The partition medium that width is 1～3mm pastes in the central authorities of mesopore film, and the mode that adopts Kaufman ion source sputter molybdenum target then is to TiO
2Plate molybdenum electrode on the mesopore film, making the titanium dioxide mesoporous film surface deposition that thickness be arranged is the molybdenum electrode of 30～60nm, throws off to obtain titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device after cutting off medium.
Relative humidity 50～85% in the described closed container, temperature is a room temperature.
Experiment base vacuum degree is 6 * 10 during described Kaufman ion source sputter
-4Pa, vacuum degree 2.2 * 10 during deposit film
-2Pa, argon gas 7.2sccm, plate voltage 1200V, accelerating voltage 100V, line 60mA.
Described partition medium is paper slip, cloth or Polypropylence Sheet.
The TiO of the inventive method preparation
2The mesoporous film ultraviolet photoelectric detection prototype device structure is simpler, the TiO that is adopted
2The mesoscopic structure of mesopore film has good periodicity, the pore passage structure of rule, and bigger specific area is beneficial to O
2On its surface adsorption-desorption takes place, structure is the anatase single crystal kenel, ultraviolet ray is had preferably absorb the TiO that makes at last
2Mesoporous film ultraviolet photoelectric detection prototype device has good photoelectric response performance to ultraviolet ray, and the present invention has also that structure is simple, controllable degree is high, it is simple to make, the characteristics of easy operating, good reproducibility, can form large-scale production.
Titanium tetrachloride is converted into titanium dioxide through the reaction of step 1 through alcoholysis, hydrolysis during preparation; The purpose of ageing: along with the evaporation of absolute ethyl alcohol in the film, the micellar concentration that surfactant is formed increases gradually, after micellar concentration surpasses critical concentration, under the effect of power between hydrogen bond, Van der Waals equimolecular, induces inorganic phase TiO
2Precursor be assembled into the meso-hole structure of long-range order; The purpose of calcining: 1. remove reactants such as surfactant F-127, water and ethanol fully; 2. make TiO
2Be converted into anatase crystal by amorphous state, make it have more excellent photoelectric properties.
Description of drawings
Fig. 1 is TiO
2The little angle XRD figure spectrum of mesopore film;
Fig. 2 is TiO
2The wide-angle XRD figure spectrum of mesopore film;
Fig. 3 is TiO
2The sem photograph in mesopore film front (SEM);
Fig. 4 is TiO
2The sem photograph in mesopore film cross section (SEM);
Fig. 5 is TiO
2The transmission electron microscope picture of mesopore film (TEM);
Fig. 6 is TiO
2The electron diffraction diagram of mesopore film (ED);
Fig. 7 is TiO
2The UV, visible light absorption spectra (uv-vis) of mesopore film;
Fig. 8 is the structural representation of device of the present invention;
(line a) and add light (line b) I-V curve for the dark attitude of device of the present invention for Fig. 9.
Embodiment
Embodiment 1: adopt the following steps preparation:
(1) be that 1: 0.003: 20 titanium tetrachloride, blocked polyethers F-127 (PluronicF-127) and absolute ethyl alcohol adds in the flask and mix with mass ratio, stirring reaction is 10 minutes in ice-water bath, remove ice-water bath then, in flask, add 0.6ml distilled water, under the normal temperature stirring reaction 4 hours colloidal sol;
(2) substrate of glass of cleaning is immersed in the colloidal sol that step (1) makes, slowly lift substrate of glass again, make the surface coverage of substrate of glass that colloidal sol be arranged, the substrate of glass that is coated with colloidal sol was placed in the closed container ageing 24 hours, the relative humidity 50% in the closed container, temperature is a room temperature, then the substrate of glass after the ageing is calcined in air, the heating rate with 1 ℃/min during calcining is warming up to 300 ℃, insulation 4h, naturally cool to room temperature, obtain transparent TiO
2Mesopore film;
(3) adopt the mode of Kaufman ion source sputter at TiO
2Mesopore film simultaneously plates two molybdenum electrodes of 1mm at interval, and experiment base vacuum degree is 6 * 10 during the sputter of Kaufman ion source
-4Pa, vacuum degree 2.2 * 10 during deposit film
-2Pa, argon gas 7.2sccm, plate voltage 1200V, accelerating voltage 100V, line 60mA is earlier at TiO
2The paper slip that width is 1mm pastes in the central authorities of mesopore film, and the mode that adopts Kaufman ion source sputter molybdenum target then is to TiO
2Plate molybdenum electrode on the mesopore film, making the titanium dioxide mesoporous film surface deposition that thickness be arranged is the molybdenum electrode of 30nm, obtains titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device after throwing off paper slip.
Embodiment 2: adopt the following steps preparation:
(1) be that 1: 0.005: 40 titanium tetrachloride, blocked polyethers F-127 (PluronicF-127) and absolute ethyl alcohol adds in the flask and mix with mass ratio, stirring reaction is 15 minutes in ice-water bath, remove ice-water bath then, in flask, add 1.8ml distilled water, under the normal temperature stirring reaction 5 hours colloidal sol;
(2) substrate of glass of cleaning is immersed in the colloidal sol that step (1) makes, slowly lift substrate of glass again, make the surface coverage of substrate of glass that colloidal sol be arranged, the substrate of glass that is coated with colloidal sol was placed in the closed container ageing 60 hours, the relative humidity 70% in the closed container, temperature is a room temperature, then the substrate of glass after the ageing is calcined in air, the heating rate with 1.5 ℃/min during calcining is warming up to 400 ℃, insulation 5h, naturally cool to room temperature, obtain transparent TiO
2Mesopore film;
(3) adopt the mode of Kaufman ion source sputter at TiO
2Mesopore film simultaneously plates two molybdenum electrodes of 2mm at interval, and experiment base vacuum degree is 6 * 10 during the sputter of Kaufman ion source
-4Pa, vacuum degree 2.2 * 10 during deposit film
-2Pa, argon gas 7.2sccm, plate voltage 1200V, accelerating voltage 100V, line 60mA is earlier at TiO
2The paper slip that width is 2mm pastes in the central authorities of mesopore film, and the mode that adopts Kaufman ion source sputter molybdenum target then is to TiO
2Plate molybdenum electrode on the mesopore film, making the titanium dioxide mesoporous film surface deposition that thickness be arranged is the molybdenum electrode of 50nm, obtains titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device after throwing off paper slip.
Embodiment 3:
The preparation of employing following steps:
(1) be that 1: 0.008: 80 titanium tetrachloride, blocked polyethers F-127 (PluronicF-127) and absolute ethyl alcohol adds in the flask and mix with mass ratio, stirring reaction is 20 minutes in ice-water bath, remove ice-water bath then, in flask, add 3.6ml distilled water, under the normal temperature stirring reaction 6 hours colloidal sol;
(2) substrate of glass of cleaning is immersed in the colloidal sol that step (1) makes, slowly lift substrate of glass again, make the surface coverage of substrate of glass that colloidal sol be arranged, the substrate of glass that is coated with colloidal sol was placed in the closed container ageing 120 hours, the relative humidity 85% in the closed container, temperature is a room temperature, then the substrate of glass after the ageing is calcined in air, the heating rate with 2 ℃/min during calcining is warming up to 450 ℃, insulation 6h, naturally cool to room temperature, obtain transparent TiO
2Mesopore film;
(3) adopt the mode of Kaufman ion source sputter at TiO
2Mesopore film simultaneously plates two molybdenum electrodes of 3mm at interval, and experiment base vacuum degree is 6 * 10 during the sputter of Kaufman ion source
-4Pa, vacuum degree 2.2 * 10 during deposit film
-2Pa, argon gas 7.2sccm, plate voltage 1200V, accelerating voltage 100V, line 60mA is earlier at TiO
2The paper slip that width is 3mm pastes in the central authorities of mesopore film, and the mode that adopts Kaufman ion source sputter molybdenum target then is to TiO
2Plate molybdenum electrode on the mesopore film, making the titanium dioxide mesoporous film surface deposition that thickness be arranged is the molybdenum electrode of 60nm, obtains titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device after throwing off paper slip.
The current/voltage characteristic analytical test shows, the Schottky characteristic that device product of the present invention adds when its I-V curve is by dark attitude behind the ultraviolet light changes ohm property (seeing accompanying drawing 9 center line a, line b) into, shows that the ultraviolet photoelectric detection prototype device that the inventive method is made has good photoelectric respone to ultraviolet light; According to scanning electron microscope sem, transmission electron microscope TEM and electronic diffraction ED to TiO
2The observation of mesopore film is seen Fig. 3, Fig. 4 and Fig. 5, as can be known TiO
2The aperture of mesopore film is about 5nm, and the duct regular surfaces is smooth, and thickness is about 500nm; According to the uv-visible absorption spectra (see figure 7) as can be known, the TiO of process of preparing of the present invention
2Mesopore film has very strong absorption to wavelength less than the ultraviolet ray of 400nm; By TiO
2X-ray diffraction XRD of mesopore film (Fig. 1, Fig. 2) and electron diffraction instrument SAED (Fig. 6) as can be seen, TiO
2Mesopore film has good periodicity, and structure is the anatase single crystal kenel.The structure of embodiment 1-3 end product titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device as shown in Figure 8, and is simple in structure.
Test used instrument model:
The model of I-V curve tester is that the semiconductor of U.S.'s Keithley (KEITHLEY) instrument company characterizes instrument (KEITHLEY4200-SCS);
The model of ESEM (SEM) is the JSM-5600LV of Jeol Ltd.;
The model of transmission electron microscope (TEM) and electron diffraction instrument (ED) is the JEM-100CX-II of Jeol Ltd.;
The model of x-ray diffractometer (XRD) is the XPertPro MPD that Dutch Philips produces;
The model of ultraviolet-uisible spectrophotometer is the LAMBDA35 of U.S. PerkinElmer company.
Claims (5)
1. the manufacture method of a titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device is characterized in that adopting the following steps preparation:
(1) be that 1: 0.003～0.008: 20～80 titanium tetrachloride, blocked polyethers F-127 and absolute ethyl alcohol add in the flask and mix with mass ratio, stirring reaction is 10～20 minutes in ice-water bath, remove ice-water bath then, in flask, add 0.6～3.6ml distilled water, under the normal temperature stirring reaction 4～6 hours colloidal sol;
(2) substrate of glass of cleaning is immersed in the colloidal sol that step (1) makes, lift substrate of glass again, make the surface coverage of substrate of glass that colloidal sol be arranged, the substrate of glass that is coated with colloidal sol was placed in the closed container ageing 24～120 hours, then the substrate of glass after the ageing is calcined in air, the heating rate with 1～2 ℃/min during calcining is warming up to 300～450 ℃, insulation 4～6h, naturally cool to room temperature, obtain transparent TiO
2Mesopore film;
(3) adopt the mode of vacuum sputtering at TiO
2Mesopore film simultaneously plates the molybdenum electrode of two interval 1～3mm, obtains titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device.
2. the manufacture method of titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device as claimed in claim 1 is characterized in that: during described vacuum sputtering earlier at TiO
2The partition medium that width is 1～3mm pastes in the central authorities of mesopore film, and the mode that adopts Kaufman ion source sputter molybdenum target then is to TiO
2Plate molybdenum electrode on the mesopore film, making the titanium dioxide mesoporous film surface deposition that thickness be arranged is the molybdenum electrode of 30～60nm, throws off to obtain titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device after cutting off medium.
3. the manufacture method of the titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device of stating as claim 1 or 2, it is characterized in that: the relative humidity 50～85% in the described closed container, temperature is a room temperature.
4. the manufacture method of titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device as claimed in claim 3 is characterized in that: experiment base vacuum degree is 6 * 10 during described Kaufman ion source sputter
-4A, vacuum degree 2.2 * 10 during deposit film
-2Pa, argon gas 7.2sccm, plate voltage 1200V, accelerating voltage 100V, line 60mA.
5. the manufacture method of titanium dioxide mesoporous film ultraviolet photoelectric detection prototype device as claimed in claim 4, it is characterized in that: described partition medium is paper slip, cloth or Polypropylence Sheet.
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| CN101635320B true CN101635320B (en) | 2010-11-17 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102651422A (en) * | 2011-10-10 | 2012-08-29 | 京东方科技集团股份有限公司 | Short wavelength photodetector and manufacturing method thereof |
| CN104810418B (en) * | 2015-03-13 | 2017-08-08 | 纳米新能源（唐山）有限责任公司 | Ultraviolet light sensor based on oxide |
| CN105350068A (en) * | 2015-10-29 | 2016-02-24 | 上海师范大学 | Preparation method of porous monocrystalline TiO2 thin film |
| CN106319319A (en) * | 2016-07-30 | 2017-01-11 | 余姚市巧迪电器厂 | Ceramic die long in service life |
| CN114914318B (en) * | 2022-04-29 | 2023-09-22 | 复旦大学 | Barium titanate@mesoporous titanium dioxide heterojunction two-dimensional film and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1828950A (en) * | 2006-04-04 | 2006-09-06 | 吉林大学 | Metal/semiconductor/metallic structure TiO2 ultraviolet photodetector and preparation |
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|---|---|---|---|---|
| CN1828950A (en) * | 2006-04-04 | 2006-09-06 | 吉林大学 | Metal/semiconductor/metallic structure TiO2 ultraviolet photodetector and preparation |
Non-Patent Citations (4)
| Title |
|---|
| C.Jeffrey Brinker.Evaporation-Induced Self-Assembly Nanostructures Made Easy.《ADVANCED MATERIALS》.1999,第11卷(第7期), |
| C.Jeffrey Brinker.Evaporation-Induced Self-Assembly Nanostructures Made Easy.《ADVANCED MATERIALS》.1999,第11卷(第7期). * |
| Kwang-Suk Jang.Using the effects of pH and moisture to synthesize highly organized mesoporous titania thin films.《CHEM COMM》.2004, |
| Kwang-Suk Jang.Using the effects of pH and moisture to synthesize highly organized mesoporous titania thin films.《CHEM COMM》.2004. * |
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