Black titanium dioxide light nano material rich in oxygen vacancy defects as well as preparation method and application thereof

A black titanium dioxide, nanomaterial technology, applied in the direction of titanium dioxide, chemical instruments and methods, titanium oxide/hydroxide, etc., can solve the problem that the reaction cannot be fully carried out, pure black titanium dioxide cannot be obtained, and the carbon content and purity are not clearly given. and other problems, to achieve the effect of flexible and adjustable temperature range, low temperature requirements for preparation environment, and wide application range

Active Publication Date: 2020-11-20
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
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Problems solved by technology

Although this invention is simple, it also has certain defects. The simple physical mixing of ascorbic acid and titanium dioxide cannot ensure that the next step reaction will be fully carried out.
The molecular formula of ascorbic acid is C 6 h 8 o 6 , after grinding it with titanium dioxide, through the patented sintering process, there will be carbon in the product, and it is impossible to get pure black titanium dioxide in the true sense
Moreover, the content and purity of carbon in the product are not clearly given in the patent

Method used

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  • Black titanium dioxide light nano material rich in oxygen vacancy defects as well as preparation method and application thereof
  • Black titanium dioxide light nano material rich in oxygen vacancy defects as well as preparation method and application thereof
  • Black titanium dioxide light nano material rich in oxygen vacancy defects as well as preparation method and application thereof

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preparation example Construction

[0043] The invention discloses a method for preparing a black titanium dioxide nanomaterial rich in oxygen vacancy defects, which comprises the following steps:

[0044] Step 1: dissolving the soluble titanium salt in deionized water, fully stirring to obtain a clear solution, adjusting the pH value of the soluble titanium salt aqueous solution to weak alkalinity (pH=8-10) by adding lye dropwise at room temperature, and obtaining a precipitate, Wash the precipitate with deionized water to remove impurity ions, then add excess hydrogen peroxide solution and stir well. Under the condition of heating at 85° C., excess hydrogen peroxide solution was removed to obtain titanium sol.

[0045] Step 2: Add a reducing agent to the titanium sol, react at 20-100°C for 1-4 hours, filter and centrifuge the reduced product, put it in an oven at 40-80°C for 3-12 hours, and then grind it into powder to obtain titanium precursor gel.

[0046] Step 3: heat-treat the titanium precursor gel cont...

Embodiment 1

[0057] Step 1. Slowly add 0.1mol titanyl sulfate to 500mL deionized water, stir at 600r / min for 4h until the solution is clear and transparent, adjust the pH of the solution to 9 with ammonia water, and obtain a precipitate, filter the precipitate, centrifuge and add 50mL of mass The fraction is 30% hydrogen peroxide aqueous solution, after stirring for 30 minutes, the solution is heated to 85° C., and heated for 10 minutes to remove excess hydrogen peroxide. Cool to room temperature to obtain titanium sol.

[0058] Step 2. Add hydroxylamine hydrochloride to the titanium sol. The molar ratio of hydroxylamine hydrochloride to titanium is 2:1, the reduction temperature is 30°C, and the time is 1h. The zeta potential of the titanium precursor gel containing charged groups is -26.8mV.

[0059] Step 3. Put the titanium precursor gel containing charged groups into a drying oven at a drying temperature of 40° C. for 3 hours to obtain solid particles, which are fully ground into powde...

Embodiment 2

[0062] Step 1. Slowly add 37.94g of titanium tetrachloride (0.2moL) to 1000mL of deionized water, stir at 800r / min for 2h, until the solution is clear and transparent, adjust the pH of the solution to 9 with ammonia water, and obtain a precipitate, filter the precipitate, After centrifugation, add 200 mL of 30% hydrogen peroxide aqueous solution, stir for 1 hour, then heat the solution to 85°C for 20 minutes to remove excess hydrogen peroxide. Cool to room temperature to obtain titanium sol.

[0063] Step 2. Add hydrazine hydrate to the titanium sol, the molar ratio of hydrazine hydrate to titanium is 2.5:1, the reduction temperature is 50°C, and the time is 1h, to obtain a titanium precursor gel containing a charged group of +10.36mV.

[0064] Step 3. Put the titanium precursor gel containing charged groups into a drying oven at a drying temperature of 60° C. for 3 hours to obtain solid particles, which are fully ground into powder.

[0065] Step 4. Under an argon protective...

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Abstract

The invention discloses a titanium dioxide nano material rich in oxygen vacancy defects as well as a preparation method and application thereof, and belongs to the technical field of semiconductor photocatalysts. According to the preparation method, a sol-gel and solid-phase synthesis combined method is adopted, and soluble titanium salt is dissolved and then added into an alkaline solution to obtain a precipitate; the precipitate reacts with a reducing agent to obtain titanium dioxide precursor gel with electronegative groups; and the titanium dioxide precursor gel with electronegative groupsis sintered in inert gas to obtain the pure titanium dioxide nano material rich in oxygen vacancy defects. The oxygen vacancy content of the titanium dioxide nano material rich in oxygen vacancy defects is 8%, the energy band gap is 1.94 eV, and compared with other titanium dioxide, the titanium dioxide nano material has higher photocatalytic activity. The method has the advantages of being green, simple, convenient, high in purity, high in safety, energy-saving, environment-friendly and capable of achieving large-scale mass production, and the material can be applied to the fields of organicdye degradation, gas purification and the like.

Description

technical field [0001] The invention belongs to the technical field of semiconductor photocatalysts, and relates to a black titanium dioxide nanometer material rich in oxygen vacancy defects and a preparation method and application thereof. Background technique [0002] Titanium dioxide (TiO 2 ) As a relatively traditional semiconductor catalyst material, it is widely used in photocatalytic reactions due to its advantages such as low price, abundant earth reserves, strong chemical stability, non-toxicity, and strong reactivity. However, in actual application production, due to its large band gap (3.0eV for rutile phase and 3.2eV for anatase phase), the light utilization rate is relatively low, and only about 5% of the solar spectrum can be used for ultraviolet light and photogenerated light. Electrons and holes are also easily recombined. In order to solve these problems, the researchers performed energy band engineering on TiO 2 Modification is carried out to produce oxy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/08C01G23/053B82Y40/00B01J21/06
CPCC01G23/08C01G23/0532C01G23/0536B82Y40/00B01J21/063B01J35/004C01P2004/64C01P2006/40C01P2002/72C01P2004/04C01P2002/84C01P2002/85
Inventor 杜高辉毕祥孙东峰余愿许并社
Owner SHAANXI UNIV OF SCI & TECH
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