Microsphere of titanium dioxide in dandelion shape, and prepartion method

A dandelion-shaped, titanium dioxide technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of large size, messy shape, complex crystal structure, etc., and achieve good electron migration, short production cycle and intact crystal form Effect

Inactive Publication Date: 2009-01-07
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Journal of the American Ceramic Society (J.Am.Ceram.Soc.2006,89,2660-2663) reported that the flower-shaped titanium dioxide microspheres prepared by the solution method have a three-dimensional structure, but due to the peroxidation treatment on the metal titanium sheet, The obtained product is difficult to separate from the substrate, and the shape is messy, the crystal structure is complex, the size is large, the specific surface area is low, and the yield is low, which is not conducive to further production and application

Method used

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  • Microsphere of titanium dioxide in dandelion shape, and prepartion method
  • Microsphere of titanium dioxide in dandelion shape, and prepartion method
  • Microsphere of titanium dioxide in dandelion shape, and prepartion method

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Preparation containing NaCl 10mol / L and TiCl 3 0.15mol / L mixed solution, the pH value of the solution is 3; put 14ml of the mixed solution into a 20ml autoclave with a polytetrafluoroethylene liner, heat up to 190°C, and the internal vapor pressure is 12× 10 5 Pa, hydrothermal reaction for 4 hours, naturally cooled down to room temperature with the furnace, unloaded the kettle, and washed the product repeatedly with deionized water and ethanol until the reaction solution was neutral; finally, centrifugally filtered and dried, the obtained product was a white powder .

[0018] The product was analyzed by scanning electron microscopy. exist figure 1 As can be seen from the given scanning electron microscope photos, the product is a dandelion-shaped TiO with a diameter of 1.8-2.2um 2 Microspheres, the top of each branch is square, and the side length of the branch is 12-16nm.

[0019] A high-resolution electron microscope test was performed on the sample to analyze i...

Embodiment 2

[0025] Prepare TiCl 3 0.15mol / L solution, the pH value of the solution is 3, put 14ml of the solution into a 20ml autoclave with a polytetrafluoroethylene liner, raise the temperature to 190°C, and the internal vapor pressure is 12×10 5 Pa, hydrothermal reaction for 4 hours, and all the other steps were the same as in Example 1 to obtain a white powder.

[0026] Figure 5 It is the scanning electron micrograph of the product of the present embodiment 2, and the illustration wherein is its independent microsphere electron micrograph.

[0027] exist Figure 5 It can be seen from the electronic scanning photo in: the product of Example 2 is a dandelion-shaped rutile phase with a diameter of 0.3-0.35um, a branch branch diverging from the center, a square cross-section, a side length of 10-18nm, and a branch length of 100-130nm TiO 2 microsphere structure.

Embodiment 3

[0029] Preparation containing NaCl 10mol / L and TiCl 3 0.15mol / L mixed solution, add 0.25ml of 1mol / L NaOH solution to adjust the pH value of the solution to 4.5, put 14ml of this mixed solution into an autoclave with a polytetrafluoroethylene liner with a volume of 20ml, and heat up to 190°C, internal vapor pressure 12×10 5 Pa, hydrothermal reaction for 4 hours, and all the other steps were the same as in Example 1 to obtain a white powder.

[0030] Image 6 Provided is the electronic scanning photo of the product of Example 3.

[0031] exist Image 6 It can be seen from the electronic scanning photo that the product of Example 3 is a dandelion-shaped rutile phase TiO with a diameter of 1.4-1.8um, a cross-section of branches diverging from the center, a side length of 10-18nm, and a branch length of 700-900nm. 2 microsphere structure.

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Abstract

This invention discloses a method for preparing dandelion-shaped TiO2 microsphers. The method comprises: (1) using NaOH solution to adjust the pH of aqueous solution of 0-12 mol / L NaCl and 0.13-0.17 mol / L TiCl3 to 3-8; (2) reacting at 160-210 deg.C under 4-14*105 Pa for 2-7 h; (3) Air-cooling to below 60 deg.C, cleaning, filtering and drying to obtain powder of dandelion-shaped rutile TiO2 microsphers. The microspheres have diameters of 0.2-2.5 mum. The branch sections emanated from the center are squares and have side lengths of 10-18 nm; the lengths of the branch are 0.1-1.2 mum. The method can prepare dandelion-shaped TiO2 microsphers without using a substrate. The product has such advantages as easy collection, short preparation period, good crystal morphology, small sizes and better electron transfer and photoelectric conversion abilities.

Description

Technical field: [0001] The invention belongs to the technical field of nanometer preparation, and in particular relates to a dandelion-shaped titanium dioxide microsphere and a preparation method thereof. Background technique: [0002] Currently on titanium dioxide (TiO 2 ) prepared patents, such as CN1405093 and CN1443601, are all granular titanium dioxide powders. Because the particles are not conducive to electron migration and transport, and the particles are prone to agglomeration and lose part of their activity, which reduces their application efficiency in the fields of photoelectrochemistry and ceramics. "Journal of Materials Chemistry" (J.Mater.Chem.2006, 16, 649-662) pointed out that three-dimensional structure materials have a high specific surface area due to their special morphology, which can make semiconductor materials more widely used in optical applications. Catalysis, dye-sensitized cells, three-dimensional lasers, and increasing the performance of cera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047
Inventor 白雪莲王海千王晓平谢斌侯建国
Owner UNIV OF SCI & TECH OF CHINA
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