High-concentration anion-doped TiO2 as well as preparation method and application thereof

An anion, high-concentration technology, applied in the direction of titanium oxide/hydroxide, titanium dioxide, etc., can solve the problems of uncontrollable doping amount, low doping amount, high energy consumption, etc., achieve simple operation, increase electronic conductivity, short process effect

Inactive Publication Date: 2021-08-06
CENT SOUTH UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] In view of the defects of low doping amount, uncontrollable doping amount, high energy consumption and high cost in the preparation process of heteroatom-doped titanium dioxide in the prior art, one of the purposes of the present invention is to provide a high doping concentration, doping Preparation method of high-concentration anion-doped titanium dioxide with simple and convenient operation and short cycle with controllable amount

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  • High-concentration anion-doped TiO2 as well as preparation method and application thereof
  • High-concentration anion-doped TiO2 as well as preparation method and application thereof
  • High-concentration anion-doped TiO2 as well as preparation method and application thereof

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Embodiment 1

[0038] 2-NH 2-The MIL-125 precursor was placed in a porcelain boat and heated to 400°C in a muffle furnace at a heating rate of 5°C / min for pre-carbonization for 2h; 2 Heating to 600°C at a heating rate of 10°C / min in a mixed atmosphere of Ar / Ar (hydrogen gas fraction is 5%), and reacting at a constant temperature for 2 hours; after naturally cooling to room temperature, black titanium dioxide powder rich in oxygen vacancies was collected; porcelain boat Put 1.0 g of sublimated sulfur powder into the tube furnace, put the sublimed sulfur in the upper atmosphere port of the tube furnace, and place the black titanium dioxide sample in the lower atmosphere port. In the argon protective gas, the temperature is raised to 500 °C at a heating rate of 10 °C / min, and the temperature is constant for 2 hour; after the reaction was completed, cool to room temperature, and use carbon disulfide (CS 2 ) and deionized (DI) water to remove excess S, and vacuum-dried at 65 °C to obtain high-co...

Embodiment 2

[0044] 2-NH 2 -The MIL-125 precursor was placed in a porcelain boat, heated in a muffle furnace at a heating rate of 5°C / min to 400°C for pre-carbonization for 2h; 2 Heating to 600°C at a heating rate of 10°C / min in a mixed atmosphere of Ar / Ar (hydrogen gas fraction is 5%), and reacting at a constant temperature for 2 hours; after naturally cooling to room temperature, black titanium dioxide powder rich in oxygen vacancies was collected; porcelain boat Put 1.0 g of red phosphorus powder into the tube furnace. The red phosphorus powder is placed in the upper atmosphere port of the tube furnace, and the black titanium dioxide sample is placed in the lower atmosphere port. 2 hours; after the completion of the reaction, cool to room temperature, and use phosphorus tribromide (PBr 3 ) and deionized (DI) water to remove excess phosphorus powder, and vacuum-dried at 65 °C to obtain high-concentration phosphorus-doped titanium dioxide. The resulting phosphorus-doped titanium dioxide...

Embodiment 3

[0046] The anatase precursor was placed in a porcelain boat and heated to 400 °C in a muffle furnace at a heating rate of 5 °C / min for pre-carbonization for 2 h; 2 Heating to 600°C at a heating rate of 10°C / min in a mixed atmosphere of Ar / Ar (hydrogen gas fraction is 5%), and reacting at a constant temperature for 2 hours; after naturally cooling to room temperature, black titanium dioxide powder rich in oxygen vacancies was collected; porcelain boat Put 1.0 g of selenium powder into the tube furnace, place the selenium powder in the upper atmosphere port of the tube furnace, and place the black titanium dioxide sample in the lower atmosphere port. In the argon protective gas, raise the temperature to 500 °C at a heating rate of 10 °C / min, and keep the temperature for 2 hours. ; After the completion of the reaction, cool to room temperature, and use carbon disulfide (CS 2 ) and deionized (DI) water to remove excess elemental selenium, and vacuum-dried at 65 °C to obtain high-c...

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Abstract

The invention provides high-concentration anion-doped TiO2 as well as a preparation method and application thereof, and the preparation method comprises the following steps: pre-carbonizing a titanium source, introducing an oxygen vacancy defect into the pre-carbonized titanium source through a high-temperature hydrogen reduction method, doping through doping source diffusion in a protective atmosphere, washing a doped product, and carrying out drying in vacuum to obtain high-concentration anion doped TiO2, wherein the titanium source is at least one of Ti-MOF, anatase and rutile type TiO2, and the doping source is one of sublimed sulfur, elemental selenium and red phosphorus. According to the preparation method, oxygen vacancy defects are introduced through hydrogen reduction treatment, oxygen vacancies are used for assisting heteroatoms in entering titanium dioxide or Ti-MOF crystal lattices, the high-concentration anion doping level is achieved, the preparation method has the advantages of being short in process, easy to operate, rapid and efficient, and industrial production is facilitated.

Description

technical field [0001] The present invention relates to doped TiO 2 The field of preparation technology, more specifically, relates to high-concentration anion-doped TiO 2 And its preparation method and application. Background technique [0002] Titanium dioxide has attracted much attention in recent years due to its advantages in the migration and intercalation of sodium ions, small volume changes during charge and discharge, low sodium intercalation potential, and semiconductor properties due to its edge-sharing octahedral interstitial positions. Storage is extremely popular. However, the current preparation methods of graphene are complicated and costly, which greatly limits its application. Graphitized carbon has similar structural characteristics to graphene, has excellent electrical and thermal conductivity, and is the most likely material to replace graphene. However, anatase TiO 2 It has low electronic conductivity and slow ion diffusion, which is not conducive ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/047C01G23/08
CPCC01G23/047C01G23/08C01P2002/72C01P2002/78C01P2002/82C01P2002/85C01P2004/03C01P2004/04C01P2006/12C01P2006/14C01P2006/80
Inventor 纪效波邓杏兰邹国强侯红帅
Owner CENT SOUTH UNIV
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