CN101037226A - Novel Titanium dioxide, preparation method and application thereof - Google Patents
Novel Titanium dioxide, preparation method and application thereof Download PDFInfo
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- CN101037226A CN101037226A CN 200710054099 CN200710054099A CN101037226A CN 101037226 A CN101037226 A CN 101037226A CN 200710054099 CN200710054099 CN 200710054099 CN 200710054099 A CN200710054099 A CN 200710054099A CN 101037226 A CN101037226 A CN 101037226A
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Abstract
The present invention discloses a novel titanium dioxide, a preparation method and the application of the same, which is characterized in that: (1)the crystallographic form is anatase structure with a specific surface area of 50~70 m2/g; (2)the crystal lattice contains steady single-electron-trapped oxygen vacancies and Ti3+ crystal lattice defect; (3) a visible light absorption property and a visible light photoluminescent property are possessed; (4)a p-type semiconductor photoelectrochemistry response is presented under the irradiation of visible light, and a n-type semiconductor photoelectrochemistry response is presented under the irradiation of ultraviolet light. The titanium dioxide is prepared by nanotube titanic acid which is subjected to heat treatment for 0.5~72 hours at 400~700 DEG C and then is cooled. The novel titanium dioxide can be used as photoelectric switch material. The present invention has a simple preparation method, a convenient operation, a low cost, and is adapted to mass production.
Description
Technical field
The invention belongs to technical field of nano material, relate to a kind of Novel Titanium dioxide, preparation method and application thereof.
Background technology
Nano titanium oxide has broad application prospects at aspect such as aspect catalysis and the environment protection, and can be applicable to industrial sectors such as daily product, coating, electronics, so nano titanium oxide shows huge market outlook.People are the range of application of expansion titanium dioxide in recent years, attempt obtaining with different preparation methods the titanium dioxide of different crystal forms and pattern.As: utilize the precipitator method with TiCl
4For presoma is prepared globular anatase titanium dioxide [J.AM.Ceram.Soc.1997,80:743-749] by pure pyrolysis method.Utilize the mixed crystal that can prepare anatase octahedrite and rutile of oxidation reduction process preparation, specific surface is 80m
2/ g[Mater Lett.1998,34:290-293], the titanium dioxide with special property of development of new becomes the focus of people's research.The nanotube metatitanic acid is as a kind of novel monodimension nanometer material, because it has nano tubular structure, and bigger specific surface area, people are synthetic to it, big quantity research has been carried out in structure, character and application.In the preparation method of existing titanium dioxide, also do not utilize the nanotube metatitanic acid to have the report of special light electrical property titanium dioxide by the thermal treatment preparation.
Summary of the invention
The purpose of this invention is to provide a kind of novel titanium dioxide.
Further aim of the present invention provides the preparation method of the Novel Titanium dioxide that a kind of technology is simple, easy to operate, cost is low, be suitable for producing in enormous quantities.
Another object of the present invention provides the application of a kind of Novel Titanium dioxide on the preparation photoelectric switch material.
For achieving the above object, the present invention by the following technical solutions: a kind of Novel Titanium dioxide,
(1), crystal formation is anatase structured, specific surface area is 50～70m
2/ g;
(2), contain stable constraint single electron oxygen room and Ti in the lattice
3+Lattice imperfection;
(3), has visible absorption and visible fluorescence character;
(4), under radiation of visible light, show p N-type semiconductorN photoelectrochemistry response, under UV-irradiation, show as the response of n N-type semiconductorN photoelectrochemistry.
The preparation method of Novel Titanium dioxide: be warming up to 400～700 ℃ according to the constant temperature rise rate, the nanotube metatitanic acid is heat-treated 0.5～72h, cooling promptly gets product.
The described naturally cooling that is cooled to.
Thermal treatment temp is preferably 500～600 ℃, and heat treatment time is preferably 2～8h.
Novel Titanium dioxide can be used on the preparation photoelectric switch material.
The preparation method of nanotube metatitanic acid:
Titanium dioxide or metatitanic acid slurry are mixed with strong base solution, in the oil bath under 70～150 ℃ temperature reflux 5～60 hours, cooling-sedimentation, incline and supernatant liquor, being washed with distilled water to pH value is 6～8, the product that filtration obtains soaked in the dilute solution of strong acid 5～72 hours, promptly obtained the nanotube metatitanic acid.
The present invention is to be the thermal treatment presoma with the nanotube metatitanic acid, 400～700 ℃ of following thermal treatments 0.5～72 hour, prepares a kind of novel anatase titanium dioxide by naturally cooling then, and this titanium dioxide specific surface area is big, and specific surface area is 50～70m
2/ g, crystal formation is an anatase crystal, and contains a large amount of stable lattice imperfections in the titanium dioxide crystal lattice: constraint single electron oxygen room (single-electron-trappedoxygen vacancy, SETOV) and Ti
3+, just because of containing stable SETOV and Ti
3+Lattice imperfection, new Ti O of the present invention
2(anatase) demonstrate some special photoelectric properties: promptly have visible absorption and visible fluorescence character, under visible light, show as the photoelectrochemistry response of p N-type semiconductorN under the irradiation, and, therefore can be used as photoelectric switch material in the next photoelectrochemistry response that shows as the n N-type semiconductorN of UV-irradiation; Preparation technology of the present invention is simple, easy to operate, cost is low, is suitable for producing in enormous quantities.
Description of drawings
Fig. 1 is X-ray powder diffraction (XRD) figure of embodiment 2;
Fig. 2 is high-resolution-ration transmission electric-lens (HRTEM) figure of embodiment 2;
Fig. 3 is electron paramagnetic resonance (ESR) figure of embodiment 2;
Fig. 4 is the ultraviolet-visible diffused reflection spectrum of embodiment 2;
Fig. 5 is the fluorescence spectrum of embodiment 2;
Fig. 6 is X-ray powder diffraction (XRD) figure of embodiment 3;
Fig. 7 is X-ray powder diffraction (XRD) figure of embodiment 4;
Fig. 8 is the photoelectric current-bias voltage figure of titanium dioxide of the present invention under radiation of visible light;
Fig. 9 is the photoelectric current-bias voltage figure of titanium dioxide of the present invention under UV-irradiation;
Figure 10 for titanium dioxide of the present invention keep bias voltage be-during 0.4ev, the photoelectricity behavior outcome of the variable semi-conductor Novel Titanium dioxide of n/p type.
The XRD analysis instrument is X ' pert pro type x-ray diffractometer (XRD, Dutch Philips Company), adopt CuK α line excitaton source, λ=0.15418366nm, voltage 40kV, electric current 40mA, sample Product can be powder and place the pressing of sample stage groove or sample dispersion to drip on slide in acetone, dry in the air Become film, direct-detection after doing.
It is JEM-2010 type high-resolution-ration transmission electric-lens that HRTEM analyzes instrument.
It is Switzerland ESP300E electron spin resonanceapparatus that ESR analyzes used instrument.
It is Japanese Shimadzu U3010 ultraviolet-visible scattered reflection instrument that UV-Vis analyzes used instrument.
The used instrument of spectrofluorimetry is SPEX F212 XRF.
The photoelectrochemical behaviour evaluation is finished at DJS-292 type potentiostat, and visible light source is the xenon lamp of 500W, and by the edge filter of infrared-filtered device and 420nm, measuring light intensity through light intensity meter is 0.6 mW/cm2, ultraviolet source is the black light lamp of 8W, measuring light intensity through light intensity meter is 0.7mW/cm2。
Embodiment
Embodiment 1, it is in the polytetrafluoroethylcontainer container in 40% the NaOH solution that 3g titanium dioxide (P25 type) is slowly joined 300ml concentration, place oil bath to heat up 118 ℃, reflux 24h, cooling-sedimentation, inclining supernatant liquor, be washed with distilled water to PH=8.0, filter, use the salt acid soak 5 hours of 0.1mol/L then, filter, wash, be drying to obtain presoma nanotube metatitanic acid.
As shown in Figure 1, to turn out to be product of the present invention be anatase structured to X-ray diffraction analysis; As shown in Figure 2, high-resolution-ration transmission electric-lens (HRTEM) is analyzed in the lattice turn out to be product of the present invention and is contained a large amount of lattice imperfections; As shown in Figure 3, the electron paramagnetic resonance analysis confirms to contain stable constraint single electron oxygen room and Ti in the product lattice of the present invention
3+Lattice imperfection; UV, visible light diffused reflection spectrum and fluorescence spectrum shown in Figure 5 show that this Novel Titanium dioxide has visible absorption and visible fluorescence as shown in Figure 4.
Shown in Fig. 8,9, with P25 (n N-type semiconductorN) as reference, at visible light (λ 〉=420nm, E
PhotonUnder=2.95eV) the irradiation, Novel Titanium dioxide shows as the p N-type semiconductorN, at (λ 〉=365nm, the E of UV-light
PhotonUnder=3.40eV) the irradiation, novel sharp titanium dioxide shows as the n N-type semiconductorN, and the semiconductor type of novel anatase octahedrite can be by light guide ,+0.1V＞V
BiasBeing the p type under visible light during＞-0.7V, is the n type under UV-light.
As shown in figure 10, at fixed bias V
BiasDuring=-0.4V, the variable semi-conductive photoelectrochemistry behavior of n/p type.As can be seen from the figure under visible light radiation, the mensuration electric current reaches a stable negative value through 40s, and the increment of electric current is for negative, and what show demonstration this moment is the behavior of p N-type semiconductorN, keep closing visible light source suddenly behind the 2-3min, the electric current of dark attitude is got back to the level before the illumination again.When UV-light is shone working electrode, electric current reach very soon one stable on the occasion of, the increment of electric current (is photoelectric current I
PhotoValue) for just, show the time n N-type semiconductorN behavior that shows this moment, keep closing visible light source suddenly behind the 2-3min, the electric current of dark attitude is got back to the level before the illumination again.Therefore, this special type material can be used for the photoswitc material.
Claims (5)
1, a kind of Novel Titanium dioxide is characterized in that,
(1), crystal formation is anatase structured, specific surface area is 50～70m
2/ g;
(2), contain stable constraint single electron oxygen room and Ti in the lattice
3+Lattice imperfection;
(3), has visible absorption and visible fluorescence character;
(4), under radiation of visible light, show p N-type semiconductorN photoelectrochemistry response, under UV-irradiation, show as the response of n N-type semiconductorN photoelectrochemistry.
2, the preparation method of Novel Titanium dioxide is characterized in that, is warming up to 400～700 ℃ according to the constant temperature rise rate, and the nanotube metatitanic acid is heat-treated 0.5～72h, and cooling promptly gets product.
3, as the preparation method of Novel Titanium dioxide as described in claims 2, it is characterized in that the described naturally cooling that is cooled to.
4, as the preparation method of Novel Titanium dioxide as described in claims 3, it is characterized in that thermal treatment temp is 500～600 ℃, heat treatment time is 2～8h.
5, the application of Novel Titanium dioxide on the preparation photoelectric switch material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279762B (en) * | 2008-05-26 | 2010-06-02 | 武汉理工大学 | Preparation of fusiform anatase TiO2 nanocrystalline material |
| CN103334142A (en) * | 2013-06-17 | 2013-10-02 | 华中科技大学 | Preparation method of autodoped modified high-conductivity TiO2 nanotube array |
| CN103626225A (en) * | 2013-10-25 | 2014-03-12 | 河南大学 | Anatase titanium dioxide nanocrystal containing single-electron-trapped oxygen vacancies and with exposed {001} face and preparation method thereof |
| CN106582593A (en) * | 2016-12-15 | 2017-04-26 | 河南师范大学 | Method for synthesizing rutile phase titania photocatalyst containing electron-trapped oxygen vacancies |
| CN110038560A (en) * | 2019-04-28 | 2019-07-23 | 河南大学 | A kind of sea urchin shape hollow platinum/titanium dioxide nano material, preparation method and application of oxygen-containing vacancy |
-
2007
- 2007-03-23 CN CN 200710054099 patent/CN101037226A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279762B (en) * | 2008-05-26 | 2010-06-02 | 武汉理工大学 | Preparation of fusiform anatase TiO2 nanocrystalline material |
| CN103334142A (en) * | 2013-06-17 | 2013-10-02 | 华中科技大学 | Preparation method of autodoped modified high-conductivity TiO2 nanotube array |
| CN103626225A (en) * | 2013-10-25 | 2014-03-12 | 河南大学 | Anatase titanium dioxide nanocrystal containing single-electron-trapped oxygen vacancies and with exposed {001} face and preparation method thereof |
| CN103626225B (en) * | 2013-10-25 | 2015-08-26 | 河南大学 | A kind of expose that { 001} face anatase titania is nanocrystalline and preparation method thereof containing constraint single electron Lacking oxygen |
| CN106582593A (en) * | 2016-12-15 | 2017-04-26 | 河南师范大学 | Method for synthesizing rutile phase titania photocatalyst containing electron-trapped oxygen vacancies |
| CN106582593B (en) * | 2016-12-15 | 2020-04-28 | 河南师范大学 | Synthetic method of rutile phase titanium dioxide photocatalyst containing bound electron oxygen vacancy |
| CN110038560A (en) * | 2019-04-28 | 2019-07-23 | 河南大学 | A kind of sea urchin shape hollow platinum/titanium dioxide nano material, preparation method and application of oxygen-containing vacancy |
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