CN105819501A - Double-layer rutile titanium dioxide nano-structure and preparation method thereof - Google Patents
Double-layer rutile titanium dioxide nano-structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a double-layer rutile titanium dioxide nano-structure and its preparation method. The double-layer rutile titanium dioxide nano-structure is composed of a layer of titanium dioxide nanorod thin-film on a FTO conducting glass substrate and a layer of titanium dioxide nanoflower which grows on the titanium dioxide nanorod thin-film. The preparation method comprises the following steps: mixing concentrated hydrochloric acid and distilled water to form a solution A; stirring while dropwise adding butyl titanate into the solution A, and continuously stirring the solution for 3-5 min to form a mixed solution B; pouring the mixed solution B into a high pressure autoclave which stows FTO conducting glass; and placing the high pressure autoclave in an environment of 140-160 DEG C and reacting for 12-20 h, washing and drying to obtain the double-layer rutile titanium dioxide nano-structure, wherein the FTO conducting glass leans against a teflon inner-wall and the conducting plane faces upwards. The preparation method has the following advantages: the raw materials are cheap and easily available; cost is low; and the synthetic process is simple and easy to realize.
Description
Technical field
The present invention relates to inorganic nano material synthesis field, be specifically related to a kind of double-deck rutile titanium dioxide nanostructured and preparation method thereof.
Background technology
Titanium dioxide is a kind of oxide with essential industry purposes, due to its have stable chemical nature, with low cost, nontoxic, the advantage such as be widely used, of increased attention in the field such as photocatalysis and opto-electronic conversion.Meanwhile, dimension and the size of nano material has become material preparation and the key factor of application.Titanium dioxide nanorod array film has the orderly regularity of height, has the electron propagation ducts of excellence, and three-dimensional titanium dioxide nanostructure has bigger specific surface area；These photoelectric transformation efficiencies being very beneficial for improving titanium dioxide nano material.
The method preparing titanium dioxide nanostructure at present mainly has hydro-thermal method, sol-gal process, chemical vapour deposition technique, anodizing etc..In numerous methods, hydro-thermal method is simple to operate because of it, and condition is easy to control, has unique advantage preparing nano titanium oxide configuration aspects.Such as, Chinese patent 201310044229.0 adds pyrohydrolytic method by one and prepares rutile type nano titanic oxide, and its preparation method operation is simply easily controlled；Chinese patent 201110352461.1 is prepared for a kind of octahedral nano titanium dioxide by a kind of hydro-thermal method, and its method is simple to operation, and condition is easily achieved.Prepare monolayer titanium dioxide nanostructure by hydro-thermal method at present to be easier to realize, but, by the double-deck rutile titanium dioxide nanostructured of hydro-thermal method one step preparation, there is not been reported.
Summary of the invention
Present invention aim at providing a kind of double-deck rutile titanium dioxide nanostructured with large specific surface area and simple hydrothermal preparing process thereof.
A kind of double-deck rutile titanium dioxide nanostructured that the present invention provides is to be layer of titanium dioxide nano-rod film in FTO Conducting Glass, is layer of titanium dioxide nano flower on titanium dioxide nano-rod thin film.
The present invention also provides for the preparation method of a kind of described double-deck rutile titanium dioxide nanostructured, has steps of:
(1) concentrated hydrochloric acid is mixed with distilled water 1:1 by volume stirring, form solution A；
(2) agitating solution A, is added drop-wise to butyl titanate in solution A simultaneously, and butyl titanate continues stirring and forms mixed solution B in 3 ~ 5 minutes after dripping；Wherein butyl titanate is 0.5 ~ 1.1:50 with the volume ratio of above-mentioned solution A；
(3) being poured into by mixed solution B in the autoclave being placed with FTO electro-conductive glass (thickness 1.1mm, surface resistance: 14ohm/sq, light transmittance: 90%), wherein FTO electro-conductive glass leans against politef inwall, and inclination angle is 0 ~ 60 °, and conducting surface is upward；
(4) obtain product after above-mentioned autoclave being placed in the baking oven of 140 ~ 160 DEG C reaction 12 ~ 20 hours, by product distilled water rinse three times, be placed under room temperature environment and be dried, obtain double-deck rutile titanium dioxide nanostructured.
It is further preferred that in step (2), butyl titanate is 0.9:50 with the volume ratio of solution A.
It is further preferred that in step (3), FTO electro-conductive glass leans to politef inwall with the inclination angle of 30 °, and conducting surface is upward.
Step (2) obtains in mixed solution B, solution is controlled in acid condition, thus inhibit the generation of anatase titanium dioxide, making reaction be conducive to the direction towards generating rutile titanium dioxide to carry out, the microscopic appearance of the double-decker titanium dioxide that butyl titanate is prepared time different from the volume ratio of solution A is different；
In step (3), the FTO of FTO electro-conductive glass faces up, and this advantageously forms the generation of the nano flower-like titanium dioxide in prepared double-decker；
Reactor in step (3) and (4) is band teflon-lined stainless steel cauldron；The purity of heretofore described concentrated hydrochloric acid and butyl titanate is analytical pure.
Beneficial effects of the present invention:
(1) hydro-thermal method conventional during the present invention uses nano material synthetic technology, the cheaper starting materials of preparation method provided by the present invention is easy to get, low cost, need not use any catalyst or surfactant in building-up process, and synthesis technique the most easily realizes.
(2) titanium dioxide prepared by the present invention is double-deck rutile type nano structure, this structure is made up of the titanium oxide nanoflower of a regular orderly titanium dioxide nano-rod thin film of layer height and one layer of novel in shape, compared with monolayer titanium dioxide nano-rod thin film, there is bigger specific surface area.
Accompanying drawing explanation
Fig. 1 is double-deck rutile titanium dioxide nanostructured.In figure: 1 is titanium oxide nanoflower；2 is titanium dioxide nano-rod thin film；3 is FTO electro-conductive glass.
Fig. 2 is the scanning electron microscope (SEM) photograph of embodiment 1 gained bilayer rutile titanium dioxide nanostructured.
Fig. 3 is the scanning electron microscope (SEM) photograph of embodiment 2 gained bilayer rutile titanium dioxide nanostructured.
Fig. 4 is the scanning electron microscope (SEM) photograph of embodiment 3 gained bilayer rutile titanium dioxide nanostructured.
Fig. 5 is the scanning electron microscope (SEM) photograph of embodiment 4 gained bilayer rutile titanium dioxide nanostructured.
Fig. 6 is the X ray diffracting spectrum of embodiment 1-4 gained bilayer rutile titanium dioxide nanostructured.In figure: 1 is the X ray diffracting spectrum of embodiment 1；2 is the X ray diffracting spectrum of embodiment 2；3 is the X ray diffracting spectrum of embodiment 3；4 is the X ray diffracting spectrum of embodiment 4.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated, but is not limited to the following example, should include the full content in claims.
Embodiment 1-6: double-deck rutile titanium dioxide nanostructured preparation process:
(1) first concentrated hydrochloric acid is configured solution A with distilled water 1:1 by volume；
(2) agitating solution A on one side, is added drop-wise to butyl titanate in 50mL solution A, and butyl titanate continues agitating solution 3 ~ 5 minutes after dripping, and forms solution B；
(3) solution B being poured in 100mL band teflon-lined autoclave, be placed with the FTO electro-conductive glass of cleaning in autoclave, FTO electro-conductive glass leans to polytetrafluoroethyllining lining inwall with 0 ~ 60 ° of inclination angle；
(4) obtain product after described autoclave being placed in the baking oven of 140 ~ 160 DEG C reaction 12 ~ 20 hours, by product distilled water rinse three times, be placed at room temperature 25 DEG C and be dried, obtain described double-deck rutile titanium dioxide nanostructured.
(5) products therefrom x-ray powder diffraction instrument (XRD) and scanning electron microscope (SEM) being characterized, wherein tube voltage and the electric current of XRD is respectively 40kV and 40mA.SEM's is the scanning electron microscope that model is JSM-7001F that produced of Amada Co., Ltd..
The preparation condition parameter of embodiment 1-6 is as shown in the table
| Condition | Butyl titanate consumption (mL) | Reaction temperature (DEG C) | FTO angle of inclination (°) | Response time (h) |
| Embodiment one | 0.5 | 155 | 0 | 15 |
| Embodiment two | 0.7 | 160 | 45 | 12 |
| Embodiment three | 0.8 | 150 | 30 | 18 |
| Embodiment four | 0.9 | 145 | 30 | 20 |
| Embodiment five | 0.6 | 140 | 60 | 15 |
| Embodiment six | 1.1 | 150 | 15 | 18 |
Implementation result
Implementation result of the present invention: product is accredited as rutile titanium dioxide through X-ray powder diffraction；X-ray diffraction result is as shown in Figure 6；The microscopic appearance of embodiment 1-4 product is obtained by scanning electron microscope result, and its microscopic appearance is two-layer titanium dioxide nanostructured as shown in Figure 2-5.
Embodiment described above only have expressed embodiments of the present invention; it describes more concrete and detailed; but therefore can not be interpreted as the restriction to the scope of the claims of the present invention; in every case the technical scheme using the form of equivalent or equivalent transformation to be obtained, all should fall within the scope and spirit of the invention.
Claims (4)
1. a double-deck rutile titanium dioxide nanostructured, it is characterised in that: it is layer of titanium dioxide nano-rod film in FTO Conducting Glass, is layer of titanium dioxide nano flower on titanium dioxide nano-rod thin film.
2. the preparation method of the double-deck rutile titanium dioxide nanostructured described in a claim 1, it is characterised in that have steps of:
(1) concentrated hydrochloric acid is mixed with distilled water 1:1 by volume stirring, form solution A；
(2) agitating solution A, is added drop-wise to butyl titanate in solution A simultaneously, and butyl titanate continues stirring and forms mixed solution B in 3 ~ 5 minutes after dripping；Wherein butyl titanate is 0.5 ~ 1.1:50 with the volume ratio of above-mentioned solution A；
(3) being poured into by mixed solution B in the autoclave being placed with FTO electro-conductive glass, wherein FTO electro-conductive glass leans against politef inwall, and inclination angle is 0 ~ 60 °, and conducting surface is upward；
(4) obtain product after above-mentioned autoclave being placed in the baking oven of 140 ~ 160 DEG C reaction 12 ~ 20 hours, by product distilled water rinse three times, be placed under room temperature environment and be dried, obtain double-deck rutile titanium dioxide nanostructured.
Preparation method the most according to claim 2, it is characterised in that: in step (2), butyl titanate is 0.9:50 with the volume ratio of solution A.
Preparation method the most according to claim 2, it is characterised in that: in step (3), FTO electro-conductive glass leans to politef inwall with the inclination angle of 30 °, and conducting surface is upward.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107159178A (en) * | 2016-12-19 | 2017-09-15 | 广东工业大学 | A kind of TiO of graphene modified2The preparation method of membranaceous compound and its application in photocatalysis degradation organic contaminant |
| CN108751739A (en) * | 2018-06-05 | 2018-11-06 | 青岛科技大学 | A kind of TiO2Nanometer rods and the staggered film of spike cluster and preparation method thereof |
| CN109020257A (en) * | 2018-07-25 | 2018-12-18 | 沈阳航空航天大学 | A kind of preparation method of self assembly secondary structure TiOx nano array |
| CN110252352A (en) * | 2019-05-23 | 2019-09-20 | 广东工业大学 | A kind of carbon quantum dot modification bismuth tungstate/ordered big hole fluorine-doped tin oxide composite photo-catalyst and its preparation method and application |
| CN114314764A (en) * | 2021-12-16 | 2022-04-12 | 浙江工商大学 | Electrode for degrading bisphenol A in high-chloride system and preparation and application thereof |
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| CN101916670A (en) * | 2010-08-25 | 2010-12-15 | 广东工业大学 | Titanium dioxide nanoflower film photoanode and preparation method thereof |
| CN103030177A (en) * | 2012-12-25 | 2013-04-10 | 王滨 | Preparation method of titanium oxide nanoflower film |
| CN103643254A (en) * | 2013-11-08 | 2014-03-19 | 江苏大学 | Method for synthesizing titanium dioxide/bismuth oxychloride composite electrode on FTO |
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2015
- 2015-01-05 CN CN201510002458.5A patent/CN105819501A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101916670A (en) * | 2010-08-25 | 2010-12-15 | 广东工业大学 | Titanium dioxide nanoflower film photoanode and preparation method thereof |
| CN103030177A (en) * | 2012-12-25 | 2013-04-10 | 王滨 | Preparation method of titanium oxide nanoflower film |
| CN103643254A (en) * | 2013-11-08 | 2014-03-19 | 江苏大学 | Method for synthesizing titanium dioxide/bismuth oxychloride composite electrode on FTO |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107159178A (en) * | 2016-12-19 | 2017-09-15 | 广东工业大学 | A kind of TiO of graphene modified2The preparation method of membranaceous compound and its application in photocatalysis degradation organic contaminant |
| CN108751739A (en) * | 2018-06-05 | 2018-11-06 | 青岛科技大学 | A kind of TiO2Nanometer rods and the staggered film of spike cluster and preparation method thereof |
| CN108751739B (en) * | 2018-06-05 | 2021-06-15 | 青岛科技大学 | TiO22Nanorod and spike-shaped rod bundle staggered array film and preparation method thereof |
| CN109020257A (en) * | 2018-07-25 | 2018-12-18 | 沈阳航空航天大学 | A kind of preparation method of self assembly secondary structure TiOx nano array |
| CN110252352A (en) * | 2019-05-23 | 2019-09-20 | 广东工业大学 | A kind of carbon quantum dot modification bismuth tungstate/ordered big hole fluorine-doped tin oxide composite photo-catalyst and its preparation method and application |
| CN110252352B (en) * | 2019-05-23 | 2022-05-10 | 广东工业大学 | Carbon quantum dot modified bismuth tungstate/ordered macroporous fluorine-doped tin oxide composite photocatalyst and preparation method and application thereof |
| CN114314764A (en) * | 2021-12-16 | 2022-04-12 | 浙江工商大学 | Electrode for degrading bisphenol A in high-chloride system and preparation and application thereof |
| CN114314764B (en) * | 2021-12-16 | 2022-12-06 | 浙江工商大学 | Electrode for degrading bisphenol A in high-chlorine salt system and preparation and application thereof |
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Application publication date: 20160803 |