Preparation method of anatase TiO2 monocrystal having high-activity (110) face

An anatase, high-activity technology, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problem of no patent report on anatase single crystal, and achieve the goal of inhibiting products from easily crossing or agglomerating, The effect of full utilization of reaction raw materials and strong reproducibility

Inactive Publication Date: 2013-08-14
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, the synthesis of anatase single crystal with (110) face has never been reported in patents.

Method used

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  • Preparation method of anatase TiO2 monocrystal having high-activity (110) face
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  • Preparation method of anatase TiO2 monocrystal having high-activity (110) face

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] This example is used to illustrate the preparation method provided by the present invention.

[0038] (1) Weigh 10 mg of titanium metal powder, add it to the polytetrafluoro reactor liner, add 27ml high-purity water, 0.08ml hydrofluoric acid (aqueous solution with a concentration of 54mol / L) and 1.5 ml of hydrogen peroxide (aqueous solution with a concentration of 30% by weight), and electromagnetically stirred for 10 min to obtain a titanium-containing solution.

[0039] (2) Put the titanium-containing solution prepared in step (1) in a 100 mL autoclave, seal the autoclave, and react at 160° C. for 15 hours.

[0040] (3) After the reaction was completed, the resulting product was washed 8 times with 500 ml of high-purity water, and then washed 3 times with 150 ml of ethanol until its pH value reached 7. The product was dried in an oven for 2 hours.

[0041] (4) Grind the dried product evenly and calcinate at 450°C for 2 hours to obtain anatase TiO with a highly activ...

Embodiment 2

[0044] This example is used to illustrate the preparation method provided by the present invention.

[0045](1) Weigh 10 mg of powder of titanium metal, add it into the polytetrafluoro reactor liner, add 25ml high-purity water, 0.1ml hydrofluoric acid (concentration is the aqueous solution of 56mol / L) and 5ml of hydrogen peroxide (30% by weight aqueous solution), and electromagnetically stirred for 10 minutes to obtain a titanium-containing solution.

[0046] (2) Put the titanium-containing solution prepared in step (1) in a 100 mL autoclave, seal the autoclave, and react at 200° C. for 10 hours.

[0047] (3) After the reaction is completed, the resulting product is washed 5 times with 500 ml of high-purity water, and then 5 times with 200 ml of ethanol until its pH value reaches 7. The product was dried in an oven for 2 hours.

[0048] (4) Grind the dried product evenly and calcinate at 500°C for 3 hours to obtain anatase TiO with a highly active (110) surface 2 single cry...

Embodiment 3

[0051] This example is used to illustrate the preparation method provided by the present invention.

[0052] (1) Weigh 20 mg of titanium metal powder, add it to the polytetrafluoro reactor liner, add 20 ml of high-purity water, 0.5 ml of hydrofluoric acid (aqueous solution with a concentration of 50 mol / L) and 3ml of hydrogen peroxide (30% by weight aqueous solution), and electromagnetically stirred for 10 minutes to obtain a titanium-containing solution.

[0053] (2) Put the titanium-containing solution prepared in step (1) in a 100 mL autoclave, seal the autoclave, and react at 180° C. for 18 hours.

[0054] (3) After the reaction was completed, the resulting product was washed 6 times with 600 ml of high-purity water, and then washed 5 times with 150 ml of ethanol until its pH value reached 7. The product was dried in an oven for 2 hours.

[0055] (4) Grind the dried product evenly, and calcinate it at 600°C for 1 hour to obtain anatase TiO with a highly active (110) surf...

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Abstract

The invention provides a preparation method of an anatase TiO2 monocrystal having a high-activity (110) face. The method comprises the following steps: 1, sequentially adding water, hydrofluoric acid and hydrogen peroxide to titanium powder, and stirring to obtain a titanium-containing solution; 2, reacting the titanium-containing solution in an autoclave at 120-220DEG C for 1-40h; 3, washing a reaction product obtained in step 2 with water and an organic solvent until the pH value is 6.5-7.5, and drying to obtain a solid; and 4, grinding the solid obtained in step 3, and calcining the ground solid at 120-900DEG C for 1-6h to obtain the anatase TiO2 monocrystal having a high-activity face. The preparation method has the advantages of low cost, simplicity, mild reaction, full utilization of above reaction raw materials, no generation of harmful gasses, and strong process repeatability.

Description

technical field [0001] The invention relates to a preparation method of a titanium dioxide material, in particular to an anatase TiO with a highly active (110) face 2 Single crystal preparation method. Background technique [0002] Titanium dioxide is a safe, non-toxic, chemically stable, and low-cost semiconductor oxide, which has a wide range of applications in photocatalysis, sewage treatment, and solar cells. [0003] The application of titanium dioxide is closely related to its crystal structure and surface properties. It has been proved by literature that the order of surface energy of each crystal plane of anatase single crystal is: 1.09J / m 2 ((110) plane)>0.90J / m 2 ((001) plane)>0.53J / m 2 ((100) surface)>0.44J / m 2 ((101) plane) (physical review B, 2002, 65, 119901). During the crystal growth process, the surface energy of the crystal tends to be minimized, and the high-energy surface quickly decreases and disappears, so it is difficult to prepare an an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/16C30B7/14
Inventor 朴玲钰吴谦李永良
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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