Preparation method for microemulsion solvent thermosynthesis monodisperse titanium dioxide nanocrystalline

A titanium dioxide and microemulsion technology, applied in the direction of titanium dioxide, nanostructure manufacturing, titanium oxide/hydroxide, etc., can solve problems such as poor dispersion, and achieve the effects of good crystallinity, good dispersion and good repeatability

Inactive Publication Date: 2010-06-30
ZHEJIANG UNIV
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  • Abstract
  • Description
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Problems solved by technology

Chung-Hsin Lu (Journal of Hazardous Materials 154 (2008) 649-654) etc. synthesized nano-titanium dioxide powder through a microemulsion intermediate, but the particle size of the nano-titanium dioxide produced by the microemulsion solvothermal method is mostly more than 15nm, and the dispersibility is relatively poor, but it is reported that the monodisperse titanium dioxide nanocrystal close to 10nm is synthesized by microemulsion solvothermal method

Method used

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  • Preparation method for microemulsion solvent thermosynthesis monodisperse titanium dioxide nanocrystalline
  • Preparation method for microemulsion solvent thermosynthesis monodisperse titanium dioxide nanocrystalline
  • Preparation method for microemulsion solvent thermosynthesis monodisperse titanium dioxide nanocrystalline

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Embodiment 1

[0031] Accurately measure 10mL of oleic acid and place it in a round-bottomed flask, then add 2ml of butyl carbonate to it, stir evenly at room temperature for 1h to prepare a mixed solution, measure 2ml of deionized water and add it dropwise to the above mixed solution, and stir for 1h . Then the body solution before the reaction is moved into a 180ml stainless steel reaction kettle, and after being sealed, the whole reaction kettle is moved into an oven, the reaction temperature is 300°C, and the time is 0.5h. Centrifuge and wash twice with n-hexane, put the washed product into an oven, and dry it at room temperature for 24 hours to obtain the product for preservation. figure 1 is the X-ray diffraction pattern of the product, which shows that the obtained product is a typical anatase structure. figure 2 It is a transmission electron microscope photograph of the product, and it can be seen that the obtained titanium dioxide nanocrystals are rod and spherical, with a diamete...

Embodiment 2

[0033] Accurately measure 15mL of oleic acid and place it in a round-bottomed flask, then add 5ml of butyl carbonate into it, stir evenly at room temperature for 1h to prepare a mixed solution, measure 4ml of deionized water and add it dropwise to the above mixed solution, and stir for 1h . Then the body solution before the reaction is moved into a 180ml stainless steel reaction kettle, and after being sealed, the whole reaction kettle is moved into an oven. The reaction temperature is 300°C and the time is 1h. Centrifuge and wash twice with alkanes, put the washed product into an oven, and dry it at room temperature for 24 hours to obtain the product for preservation. image 3 is the X-ray diffraction pattern of the product, which shows that the obtained product is a typical titanium oxide anatase structure, and the diffraction peaks are obviously broadened. Figure 4 It is a transmission electron microscope photograph of the product, and it can be seen that the obtained nan...

Embodiment 3

[0035] Accurately measure 20mL of oleic acid and place it in a round-bottomed flask, then add 5ml of butyl carbonate to it, stir evenly at room temperature for 1h to prepare a mixed solution, measure 6ml of deionized water and add it dropwise to the above mixed solution, and stir for 1h . Then the body solution before the reaction is moved into a 180ml stainless steel reaction kettle, and after sealing, the whole reaction kettle is moved into an oven. The reaction temperature is 300°C, and the time is 2h. Centrifuge and wash twice with alkanes, put the washed product into an oven, and dry it at room temperature for 24 hours to obtain the product for preservation. Figure 5 is the X-ray diffraction pattern of the product, which shows that the obtained product is a typical titanium oxide anatase structure, and the diffraction peaks are obviously broadened. Figure 6 It is a transmission electron microscope photograph of the product, and it can be seen that the obtained titanium...

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Abstract

The invention discloses a preparation method for microemulsion solvent thermosynthesis monodisperse titanium dioxide nanocrystalline, which includes the steps as follows: 1) adding 1-10ml of tetrabutyl carbonic acid into 10-20ml of oleic acid to uniformly stir for 1-2 hours under a room temperature; 2) dropping 2-6ml of deionized water to uniformly stir for 1-2 hours under the room temperature to obtain a microemulsion presoma; 3) moving the microemulsion presoma into a stainless steel agitated reactor to seal and heat for 2-8 hours under a reaction temperature of 240-320 DEG C, then cooling to the room temperature through water bath; 4) using alcohol to wash a reaction product centrifugally for 1-2 times, then using normal hexane to wash centrifugally for 1-2 times; and 5) and drying for 24-48 hours under the room temperature to obtain monodisperse titanium dioxide nanocrystalline. The preparation method for microemulsion solvent thermosynthesis monodisperse titanium dioxide nanocrystalline has the characteristics of simple technique, short production period, low cost, and large yield; moreover, the preparation method for microemulsion solvent thermosynthesis monodisperse titanium dioxide nanocrystalline is suitable for large-scale production, etc.

Description

technical field [0001] The invention relates to the field of semiconductor materials, in particular to a method for preparing microemulsion solvothermal synthesis-like monodisperse titanium dioxide nanocrystals. Background technique [0002] As an important semiconductor oxide, titanium dioxide has been widely used in the fields of coatings, additives, photovoltaic cells, gas sensors and photocatalysis due to its white color, non-toxicity and good thermal stability. [0003] In the past ten years, people's research on nano-titanium dioxide has become more and more extensive. The methods for synthesizing nano-titanium dioxide mainly include the following: sol-gel method, microemulsion method, hydrothermal method, solvothermal method, direct oxidation method and chemical vapor deposition method, etc. In recent years, a new synthesis of nanoparticles Methods The microemulsion solvothermal method has been widely used to synthesize new nanomaterials. This method can overcome the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053B82B3/00
Inventor 王智宇刘博俞中平叶波孔伟石欣超翁晶晶
Owner ZHEJIANG UNIV
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