CN106395890A - Vanadium-doped titanium dioxide ultrathin hollow structure microsphere and one-step hydrothermal synthesis method thereof and application thereof - Google Patents
Vanadium-doped titanium dioxide ultrathin hollow structure microsphere and one-step hydrothermal synthesis method thereof and application thereof Download PDFInfo
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- CN106395890A CN106395890A CN201610192689.1A CN201610192689A CN106395890A CN 106395890 A CN106395890 A CN 106395890A CN 201610192689 A CN201610192689 A CN 201610192689A CN 106395890 A CN106395890 A CN 106395890A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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Abstract
The invention belongs to the field of preparation of inorganic semiconductor nano materials, and discloses a vanadium-doped titanium dioxide ultrathin hollow structure microsphere, a one-step hydrothermal synthesis method thereof and an application thereof. Sodium metavanadate, titanium oxysulfate, urea and water according to the mass proportions of 0.01-0.1:1:1-8 are added into a high-pressure kettle with polytetrafluoroethylene lining and react for 8-16 hours at the reaction temperature of 120-200 DEG C. The reaction product is cooled, washed, dried and then calcined at 300-500 DEG C to obtain the vanadium-doped titanium dioxide ultrathin hollow structure microsphere. The method, the process and requirements for required equipment are simple, and the obtained product is relatively novel in morphology; the operation is easy and safe, the cost is low, and the large-scale production can be realized.
Description
Technical field
The invention belongs to inorganic semiconductor nanometer material preparation field, it is related specifically to a kind of vanadium doping titanium dioxide
Ultra-thin hollow structure microsphere and one step hydrothermal synthesis method and application.
Background technology
Titanium dioxide is a kind of important multifunctional inorganic material, and it has, and granule is little, and specific surface area is big, magnetic
By force, absorbent properties are good, absorb the advantages of UV resistance is strong, and surface activity is big, dispersive property is strong.Titanium dioxide
Suspension fluidity good stability obtained by titanium, and harmless, therefore in photocatalysis, ultraviolet absorber, prevent
Skin protection cosmeticss, air cleaning, fine ceramics, high-effect light-sensitive catalyst, solaode and air-sensitive pass
There is extensive and potential application prospect in the fields such as sensing unit.
Choi et al. (The Journal of Physical Chemistry, 1994,98:13669-1367) in research metal
Element doping is to quantum yardstick (2-4nm) anatase TiO2During the impact of photocatalytic activity, find that mixing V can improve
Photocatalytic activity under its ultraviolet radiation, and mix V and result in TiO2Optical absorption edge red shift, but they
Do not study its visible light catalysis activity.K.Iketan et al. (Materials Science and Engineering
B,2004,108:187-193) with sol-Gel method is prepared for V doping TiO2Thin film.But it is special not produce
Appearance structure.Shi Keyu etc. (catalysis journal, 2,002 23 (4):301-403) by butyl titanate through acidic hydrolysises
Obtain TiO2Colloidal sol, is added to after colloidal sol is mixed with phenol in normal heptane disperse medium, then Deca formalin
Solution, is prepared for polymer and TiO by inverse suspension polymerization and so-gel process2Complex microsphere,
But this method is excessively complicated, and cost is higher, and is unfavorable for industrialized production.2015, patent
CN104860348A adopts solvent-thermal method, realizes the titanium dioxide of one pot process nucleocapsid structure, but its granule
Larger, and easily agglomerate into bulky grain.
Prepare titanium dioxide method a lot of from solution, also have the preparation of a lot of different-shapes, including graininess,
The structures such as bar-shaped, tubulose.Synthesis hollow-core construction adopts template mostly, typically first in the surface of mould material bag
Cover Shell Materials, then mould material is removed by the method for dissolving or sintering, obtain hollow-core construction.Abroad also
There is some other TiO2The report of tiny balloon preparation method.But, generally it is both needed in these preparation methoies
Want inorganic material or Organic substance as pore creating material and auxiliary agent, and afterwards, these pore creating materials or auxiliary agent are removed ability
Generate hollow or meso-hole structure.Take a broad view of these TiO2Hollow ball preparation method, all has high cost, system
Standby process complexity and the shortcoming being difficult to large-scale production.
Content of the invention
In order to overcome shortcoming and defect present in prior art, the primary and foremost purpose of the present invention is to provide a kind of vanadium
One one-step hydro-thermal synthesis method of titania-doped ultra-thin hollow structure microsphere.
It is still another object of the present invention to provide the ultra-thin hollow structure of vanadium doping titanium dioxide of said method synthesis
Microsphere.
A further object of the present invention is to provide the application of the ultra-thin hollow structure microsphere of above-mentioned vanadium doping titanium dioxide.
The object of the invention is achieved through the following technical solutions：
A kind of one one-step hydro-thermal synthesis method of the ultra-thin hollow structure microsphere of vanadium doping titanium dioxide, according to operation step
Suddenly：
(1) sodium metavanadate, titanyl sulfate and carbamide are added to in teflon-lined autoclave,
Add water, reacted；
(2) cool down after reaction terminates, filter, wash, be dried；
(3) obtain vanadium doping titanium dioxide ultra-thin hollow structure microsphere after calcining.
The amount of the material of the described sodium metavanadate of step (1), titanyl sulfate and carbamide is than for 0.01～0.1:1:1～8.
The addition of the described water of step (1) is polytetrafluoroethyllining lining volume
The temperature of the described reaction of step (1) is 120～200 DEG C, and the time is 8～16h.
Washing described in step (2) is to adopt distilled water, absolute ethanol washing successively.
The temperature of the described dry run of step (2) is 60～80 DEG C, and drying time is 10～15h.
The temperature of the described calcining of step (3) is 300～500 DEG C, calcination time 3～5h.
The vanadium doping titanium dioxide ultra-thin hollow structure microsphere of said method synthesis.
Above-mentioned vanadium doping titanium dioxide ultra-thin hollow structure microsphere can be applicable to photocatalysis, photoelectron and sensing
In the fields such as device.
Compared with prior art, the present invention has advantages below and beneficial effect：The method of the present invention, technique with
And equipment needed thereby requires simply, products therefrom pattern is more novel；And processing ease, safety, low cost simultaneously,
Can be with large-scale production.
Brief description
Fig. 1 is the XRD (X-ray of the vanadium doping titanium dioxide ultra-thin hollow microsphere structure prepared by embodiment
Diffraction) figure, the XRD figure of wherein a, b, c, d of in figure respectively embodiment 1,2,3,4.
Fig. 2 is ultra-thin hollow microsphere structure SEM (scanning electron microscope) of embodiment 1 vanadium doping titanium dioxide
Figure, the upper right corner is EDX (energy dispersion X-ray spectrum) figure.
Fig. 3 is that ultra-thin hollow microsphere structure SEM of embodiment 2 vanadium doping titanium dioxide is schemed, and the upper right corner is EDX
Figure.
Fig. 4 is that ultra-thin hollow microsphere structure SEM of embodiment 3 vanadium doping titanium dioxide is schemed, and the upper right corner is EDX
Figure.
Fig. 5 is that ultra-thin hollow microsphere structure SEM of embodiment 4 vanadium doping titanium dioxide is schemed, and the upper right corner is EDX
Figure.
Specific implementation method
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to
This.
Embodiment 1
Weigh sodium metavanadate, titanyl sulfate and urea quality and be respectively 0.0153g, 2.000g, 0.7508g, its
The amount of middle material is than respectively wherein sodium metavanadate：Titanyl sulfate：Carbamide=0.01:1:1；By taken sodium metavanadate,
Titanyl sulfate adds, with carbamide, the water adding 65ml in the autoclave with polytetrafluoroethyllining lining (100ml),
10h is reacted at 140 DEG C；After the cooling of question response kettle, then filter, adopt distilled water and dehydrated alcohol successively
Washing, then is placed in 60 DEG C of baking ovens, drying time 12h；Finally it is placed in 300 DEG C of Muffle furnaces, calcine 4h,
Obtain vanadium doping titanium dioxide ultra-thin hollow structure microsphere.Gained vanadium doping titanium dioxide ultra-thin hollow structure microsphere
XRD (X-ray diffraction) figure as shown in figure 1, products obtained therefrom v element is completely into anatase TiO2Knot
In structure；SEM (scanning electron microscope) figure as shown in Fig. 2 products obtained therefrom mean diameter is in 0.8-1.5um,
There is ultra-thin hollow structure.Therefore the vanadium doping dioxy with ultra-thin hollow structure can be prepared by this method
Change titanium ultra-thin hollow structure microsphere, there is compared with other existing identical technologies of preparation method, technique and required
Equipment requirements are simple, and products therefrom pattern is more novel；And processing ease, safety, low cost simultaneously is permissible
The advantages of large-scale production.
Embodiment 2
Weigh sodium metavanadate, titanyl sulfate and urea quality and be respectively 0.0304g, 2.000g, 3.0032g, its
The amount of middle material is than respectively wherein sodium metavanadate：Titanyl sulfate：Carbamide=0.02:1:4；By taken sodium metavanadate,
Titanyl sulfate adds, with carbamide, the water adding 65ml in the autoclave with polytetrafluoroethyllining lining (100ml),
10h is reacted at 170 DEG C；After the cooling of question response kettle, then filter.Adopt distilled water and dehydrated alcohol successively
Washing, then is placed in 60 DEG C of baking ovens, drying time 12h；Finally it is placed in 400 DEG C of Muffle furnaces, calcine 4h,
Obtain vanadium doping titanium dioxide ultra-thin hollow structure microsphere.Gained vanadium doping titanium dioxide ultra-thin hollow structure microsphere
XRD (X-ray diffraction) figure as shown in figure 1, products obtained therefrom v element is completely into anatase TiO2Knot
In structure.SEM (scanning electron microscope) figure is as shown in Figure 3.Products obtained therefrom mean diameter in 0.8-1.5um,
There is ultra-thin hollow structure.Therefore the vanadium doping dioxy with ultra-thin hollow structure can be prepared by this method
Change titanium ultra-thin hollow structure microsphere, there is compared with other existing identical technologies of preparation method, technique and required
Equipment requirements are simple, and products therefrom pattern is more novel；And processing ease, safety, low cost simultaneously is permissible
The advantages of large-scale production.
Embodiment 3
Weigh sodium metavanadate, titanyl sulfate and urea quality and be respectively 0.1525g, 2.000g, 6.0064g, its
The amount of middle material is than respectively wherein sodium metavanadate：Titanyl sulfate：Carbamide=0.1:1:8；By taken sodium metavanadate,
Titanyl sulfate adds, with carbamide, the water adding 65ml in the autoclave with polytetrafluoroethyllining lining (100ml),
16h is reacted at 120 DEG C；After the cooling of question response kettle, then filter, adopt distilled water and dehydrated alcohol successively
Washing, then is placed in 80 DEG C of baking ovens, drying time 10h；Finally it is placed in 400 DEG C of Muffle furnaces, calcine 3h,
Obtain vanadium doping titanium dioxide ultra-thin hollow structure microsphere.Gained vanadium doping titanium dioxide ultra-thin hollow structure microsphere
XRD (X-ray diffraction) figure as shown in figure 1, products obtained therefrom v element is completely into anatase TiO2Knot
In structure.SEM (scanning electron microscope) figure as shown in figure 4, products obtained therefrom mean diameter is in 0.8-1.5um,
There is ultra-thin hollow structure.Therefore the vanadium doping dioxy with ultra-thin hollow structure can be prepared by this method
Change titanium ultra-thin hollow structure microsphere, there is compared with other existing identical technologies of preparation method, technique and required
Equipment requirements are simple, and products therefrom pattern is more novel；And processing ease, safety, low cost simultaneously is permissible
The advantages of large-scale production.
Embodiment 4
Weigh sodium metavanadate, titanyl sulfate and urea quality and be respectively 0.1525g, 2.000g, 3.0032g, its
The amount of middle material is than respectively wherein sodium metavanadate：Titanyl sulfate：Carbamide=0.1:1:4；By taken sodium metavanadate,
Titanyl sulfate adds, with carbamide, the water adding 65ml in the autoclave with polytetrafluoroethyllining lining (100ml),
8h is reacted at 200 DEG C；After the cooling of question response kettle, then filter, washed using distilled water and dehydrated alcohol successively
Wash, then be placed in 60 DEG C of baking ovens, drying time 15h；Finally it is placed in 500 DEG C of Muffle furnaces, calcine 5h, obtain
To vanadium doping titanium dioxide ultra-thin hollow structure microsphere.Gained vanadium doping titanium dioxide ultra-thin hollow structure microsphere
XRD (X-ray diffraction) figure is as shown in figure 1, products obtained therefrom v element is completely into anatase TiO2Structure
In.SEM (scanning electron microscope) figure as shown in figure 5, products obtained therefrom mean diameter is in 0.8-1.5um,
There is ultra-thin hollow structure.Therefore the vanadium doping dioxy with ultra-thin hollow structure can be prepared by this method
Change titanium ultra-thin hollow structure microsphere, there is compared with other existing identical technologies of preparation method, technique and required
Equipment requirements are simple, and products therefrom pattern is more novel；And processing ease, safety, low cost simultaneously is permissible
The advantages of large-scale production.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not subject to above-mentioned enforcement
The restriction of example, the change made, modifies, replaces under other any spirit without departing from the present invention and principle
Generation, combination, simplification, all should be equivalent substitute mode, are included within protection scope of the present invention.
Claims (9)
1. a kind of ultra-thin hollow structure microsphere of vanadium doping titanium dioxide an one-step hydro-thermal synthesis method it is characterised in that
According to operating procedure：
(1) sodium metavanadate, titanyl sulfate and carbamide are added to in teflon-lined autoclave,
Add water, reacted；
(2) cool down after reaction terminates, filter, wash, be dried；
(3) obtain vanadium doping titanium dioxide ultra-thin hollow structure microsphere after calcining.
2. a step hydro-thermal of the ultra-thin hollow structure microsphere of a kind of vanadium doping titanium dioxide according to claim 1
Synthetic method it is characterised in that：The amount of the material of the described sodium metavanadate of step (1), titanyl sulfate and carbamide
Than for 0.01～0.1:1:1～8.
3. a step hydro-thermal of the ultra-thin hollow structure microsphere of a kind of vanadium doping titanium dioxide according to claim 1
Synthetic method it is characterised in that：The addition of the described water of step (1) is polytetrafluoroethyllining lining volume
4. a step hydro-thermal of the ultra-thin hollow structure microsphere of a kind of vanadium doping titanium dioxide according to claim 1
Synthetic method it is characterised in that：The temperature of the described reaction of step (1) be 120～200 DEG C, the time be 8～
16h.
5. a step hydro-thermal of the ultra-thin hollow structure microsphere of a kind of vanadium doping titanium dioxide according to claim 1
Synthetic method it is characterised in that：Washing described in step (2) is to be washed using distilled water, dehydrated alcohol successively
Wash.
6. a step hydro-thermal of the ultra-thin hollow structure microsphere of a kind of vanadium doping titanium dioxide according to claim 1
Synthetic method it is characterised in that：The temperature of the described dry run of step (2) is 60～80 DEG C, drying time
For 10～15h.
7. a step hydro-thermal of the ultra-thin hollow structure microsphere of a kind of vanadium doping titanium dioxide according to claim 1
Synthetic method it is characterised in that：The temperature of the described calcining of step (3) is 300～500 DEG C, and calcination time is
3～5h.
8. the ultra-thin hollow structure of vanadium doping titanium dioxide according to the synthesis of claim 1～7 any one methods described
Microsphere.
9. the ultra-thin hollow structure microsphere of vanadium doping titanium dioxide according to claim 8 is in photocatalysis, photoelectricity
Application in son and sensor field.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107176646A (en) * | 2017-06-15 | 2017-09-19 | 陕西科技大学 | A kind of optical drive is used for the preparation method of the microrobot of environment remediation |
| CN115301225A (en) * | 2022-08-01 | 2022-11-08 | 电子科技大学长三角研究院(湖州) | Preparation method and application of bismuth/titanium dioxide photocatalytic degradation material with hollow microsphere structure |
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| CN107176646A (en) * | 2017-06-15 | 2017-09-19 | 陕西科技大学 | A kind of optical drive is used for the preparation method of the microrobot of environment remediation |
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| CN115301225A (en) * | 2022-08-01 | 2022-11-08 | 电子科技大学长三角研究院(湖州) | Preparation method and application of bismuth/titanium dioxide photocatalytic degradation material with hollow microsphere structure |
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Application publication date: 20170215 |