Method for preparing superfine hollow titanium dioxide nanospheres with diameter smaller than 100 nm

A technology of titanium dioxide and nanospheres, applied in the direction of titanium dioxide, titanium oxide/hydroxide, nanotechnology, etc., can solve problems such as difficult to obtain, and achieve the effect of less reaction steps, low price, and reduced production costs

Active Publication Date: 2016-12-07
XI AN JIAOTONG UNIV +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, the traditional hard template method mainly uses materials such as polymers as template materials. Not only does a large amount of organic solvents and catalysts be used in the template preparation process, but also the resulting templates often have agglomeration, which needs to be alleviated by adding a large amount of surfactants. In order to make the shell material well coated, these templates often need additional surface activation, and this method is difficult to obtain titanium dioxide hollow nanospheres below 100nm, with good monodispersity and controllable particle size and wall thickness (J. Am.Chem.Soc., 2005, 3928; Chem., 2006, 749; J.Colloid.Interface Sci., 2006, 370; Langmuir., 2001, 3579.)

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  • Method for preparing superfine hollow titanium dioxide nanospheres with diameter smaller than 100 nm
  • Method for preparing superfine hollow titanium dioxide nanospheres with diameter smaller than 100 nm
  • Method for preparing superfine hollow titanium dioxide nanospheres with diameter smaller than 100 nm

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preparation example Construction

[0024] The preparation method of ultrafine hollow titanium dioxide nanospheres of the present invention includes the following steps:

[0025] s1. Provide a carbon nanosphere template with a particle size of 20-90nm;

[0026] s2. Disperse the nano-carbon sphere template in step s1 uniformly in absolute ethanol, and add a certain amount of deionized water to form a nano-carbon sphere sol system, and place it in a 60°C water bath with continuous high-speed stirring, then Under these conditions, a dilute solution of tetra-n-butyl titanate diluted with absolute ethanol was added dropwise, reacted for more than 2 hours to obtain CSs@TiO with controllable wall thickness and particle size 2 Sol

[0027] s3, CSs@TiO obtained in step s2 of centrifugation 2 Sol, the separated solids are dried, and then the agglomerates obtained after drying are calcined at a high temperature at a heating rate of 20°C / min or less, and the calcining temperature is 400-800°C, and heat preservation in a muffle fur...

Embodiment 1

[0040] s1. Take 20 mg of carbon nano sphere template with a particle size of 20-40 nm and disperse it in 60 mL of absolute ethanol to form a carbon nano sphere sol;

[0041] s2. Add the above nano carbon sphere sol to 120μL of deionized water, and continuously stir vigorously under the condition of 60℃ in a water bath, and then add dropwise the dilute solution of tetra-n-butyl titanate diluted with absolute ethanol (tetra-n-butyl titanate). 150μL of the original butyl ester solution dissolved in 20mL of absolute ethanol), after adding all the tetra-n-butyl titanate dilute solution, react for 2-10h to obtain nano CSs@TiO with controllable particle size and wall thickness 2 Sol

[0042] s3, the above nano CSs@TiO 2 The sol was centrifuged at a centrifugal speed of 30,000 r / min for 15 minutes to obtain solids;

[0043] s4. Put the above solids in a vacuum oven and treat them at 40°C for 12 hours to obtain dry solids;

[0044] s5. Place the above-mentioned dry solid in a muffle furnace, i...

Embodiment 2

[0047] s1. Take 20 mg of carbon nano sphere template with a particle size of 30-60 nm and disperse it in 60 mL of absolute ethanol to form a carbon nano sphere sol;

[0048] s2. Add the above nano carbon sphere sol to 120μL of deionized water, and continuously stir vigorously under the condition of 60℃ in a water bath, and then add dropwise the dilute solution of tetra-n-butyl titanate diluted with absolute ethanol (tetra-n-butyl titanate). 150μL of the original butyl ester solution dissolved in 20mL of absolute ethanol), after adding all the tetra-n-butyl titanate dilute solution, react for 2-10h to obtain nano CSs@TiO with controllable particle size and wall thickness 2 Sol

[0049] s3, the above nano CSs@TiO 2 The sol was centrifuged at a centrifugal speed of 30,000 r / min for 15 minutes to obtain solids;

[0050] s4. Put the above solids in a vacuum oven and treat them at 40°C for 12 hours to obtain dry solids;

[0051] s5. Place the above-mentioned dry solid in a muffle furnace, i...

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Abstract

The invention provides a method for preparing superfine hollow titanium dioxide nanospheres with diameter smaller than 100 nm. The method comprises the steps of using nanocarbon sphere particles as a template; evenly dispersing the nanocarbon sphere particles (CSs) with different grain sizes in an organic solvent to form a carbon sphere sol system, and then adding a titanic acid tetra-n-butyl solution diluted by the organic solvent dropwise to obtain nano CSs@TiO2 sol with wall thickness and grain size controllable through reaction; conducting centrifugal treatment on the CSs@TiO2 sol, and drying and calcining obtained solid, wherein residues left after calcination are the target product. The hollow titanium dioxide nanospheres with integral form and high monodispersity and capable of being stored stably are prepared, the grain size of the hollow titanium dioxide nanospheres is uniform and controllable under 100 nm, and the wall thickness of the hollow titanium dioxide nanospheres is uniform and controllable under 10 nm; the whole preparing process is easy to operate and high in controllability and repeatability, the template material is widely available, low in price, low in production cost, safe and environmentally friendly, and the method is suitable for large-scale production.

Description

Technical field [0001] The application belongs to the field of preparing nano microspheres, and particularly relates to a method for preparing ultrafine hollow titanium dioxide nanospheres with a diameter of less than 100 nm. Background technique [0002] As a nano-semiconductor material with high specific surface area and low density, hollow titanium dioxide nanospheres not only have good permeability, adsorption characteristics, high stability, non-toxicity, transparency, photocatalytic properties, etc., especially for nano-sized materials smaller than 100nm. Within the limits, the ultrafine hollow titanium dioxide nanospheres have obvious quantum effects and surface effects. It not only involves physics, chemistry, materials, biology and other disciplines, but also has wide application value and prospects in optoelectronic devices, molecular detection, biomedicine and catalysis, such as biocontrollable drug transportation, disease diagnosis, micro-nano containers , Biological...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/08C01G23/053B82Y40/00
CPCC01G23/053C01G23/08C01P2004/34C01P2004/04C01P2004/64
Inventor 沈少华谭余波
Owner XI AN JIAOTONG UNIV
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