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Preparation method of visible light catalyst of surface nitrogen modified titanium dioxide nano-particles based on ALD technology

A technology of titanium dioxide and nanoparticles, which is applied in the field of preparation of new nano-functional materials and photocatalysis, can solve problems such as unsatisfactory nitrogen doping effects, and achieve the effects of enhanced visible light catalytic performance, improved utilization rate, and improved degradation rate

Active Publication Date: 2017-01-04
NANJING UNIV
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] The existing method of doping titanium dioxide with nitrogen based on ALD technology is to use ammonia gas as a nitrogen source and introduce it into ALD to deposit TiO 2 Nitrogen doping is achieved in the process, but the effect of nitrogen doping is not ideal

Method used

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  • Preparation method of visible light catalyst of surface nitrogen modified titanium dioxide nano-particles based on ALD technology
  • Preparation method of visible light catalyst of surface nitrogen modified titanium dioxide nano-particles based on ALD technology
  • Preparation method of visible light catalyst of surface nitrogen modified titanium dioxide nano-particles based on ALD technology

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Experimental program
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Effect test

Embodiment 1

[0026] Using commercial titanium dioxide powder (P25) as a carrier, it was directly transferred into the ALD reaction chamber through the powder sample tank, and the surface was coated with TiN deposition for 20, 50 and 100 cycles by plasma-enhanced atomic layer deposition (PEALD). The specific deposition parameters are as follows: the growth temperature is 360 o C; using titanium tetrachloride (TiCl 4 ) and ammonia plasma as titanium source and nitrogen source, respectively; 150 sccm of high-purity nitrogen and 50 sccm of high-purity argon were used as carrier gases; the growth cycle parameters were 0.1s TiCl 4 -4s N 2 -21.5s ammonia plasma -6s N 2 Cleaning; the flow rate of ammonia gas is 150 sccm, and the plasma power is 2500 W.

[0027] figure 1 The XRD patterns of the P25 powder and the P25 powder deposited with different cycles of PEALD on the surface, it can be seen that all samples show similar diffraction peaks, corresponding to the anatase phase of titanium dioxi...

Embodiment 2

[0030] Using commercial titanium dioxide powder (P25) as a support, plasma-enhanced atomic layer deposition (PEALD) was used at 360 o50 cycles of TiN were deposited on the P25 surface at C. Titanium tetrachloride and ammonia plasma are used as titanium source and nitrogen source, and the carrier gas is 150 sccm of high-purity nitrogen and 50 sccm of high-purity argon, respectively; the growth cycle parameter is 0.1s TiCl 4 -4sN 2 -21.5s ammonia plasma -6sN 2 Cleaning; the flow rate of ammonia gas is 150 sccm, and the plasma power is 2500 W.

[0031] Use the above-mentioned surface-modified P25 powder to degrade 4 mg / L methyl orange solution, using 100 mg P25 powder per 100 mL methyl orange solution. Catalyzed under visible light for 2 h, the degradation rate of methyl orange was measured, and then the solution was centrifuged to recover P25 powder. o C annealed for two hours to remove methyl orange adsorbed on the catalyst surface, and then photocatalytically degrade methy...

Embodiment 3

[0033] Using commercial titanium dioxide powder (P25) as a support, plasma-enhanced atomic layer deposition (PEALD) was used at 360 o 50 cycles of TiN were deposited on the P25 surface at C. In order to enhance the wrapping performance of TiN on titanium dioxide particles, the pulse time of titanium tetrachloride was extended to 2s, and other parameters were as in Example 1.

[0034] Use the above-mentioned surface-modified P25 powder to degrade 4 mg / L of methyl orange solution, and use 100 mg of P25 powder per 100 mL of methyl orange solution. The time curve of this P25 sample degrading methyl orange under visible light is as follows Figure 7 shown. It can be found that the extended TiCl 4 After the pulse time, the catalytic effect of the surface N-modified P25 powder on methyl orange was greatly improved, and the photocatalytic degradation rate was as high as 94% in 2 h.

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Abstract

The invention discloses a preparation method of a visible light catalyst of surface nitrogen modified titanium dioxide nano-particles based on the ALD technology. The method comprises the steps that firstly, titanium dioxide power is transferred into an ALD reaction room, and an ultrathin TiN film is deposited and wrapped on the surface of the titanium dioxide power, wherein wrapping parameters are reaction room temperature which ranges from 100 DEG C to 500 DEG C; a titanium source which is titanium tetrachloride or tetradimethylamino titanium or titanium isopropylate; a nitrogen source which is ammonia gas or ammonia gas plasma; carrier gas, wherein high-purity nitrogen or argon is used as the carrier gas for the titanium source, the flow is 50-200 sccm, argon is used as the carrier gas for the nitrogen source, and the flow is 50-200 sccm; pulsing and cleaning time, wherein the pulse of the titanium source is 0.1-10 s, high-purity nitrogen is used for cleaning for 2-60 s immediately after each time of inorganic source pulsing, the pulse of the nitrogen source is 5-60 s, and high-purity nitrogen is used for cleaning for 2-60 s immediately to wash off reaction byproducts and residual reaction sources. The method is simple and easy to implement, and the visible light catalytic performance of products is remarkably enhanced.

Description

technical field [0001] The invention relates to a method for preparing a high-efficiency visible light catalyst by using atomic layer deposition technology, and belongs to the field of preparation of new nanometer functional materials and photocatalysis. Background technique [0002] With the continuous development and progress of human society, the problem of environmental pollution is becoming more and more serious. TiO 2 Due to the advantages of low price, safety and non-toxicity, good stability, and high catalytic activity, it has been widely and deeply studied as a photocatalytic material. But due to TiO 2 It is a wide bandgap (3.2 eV) semiconductor material, which can only absorb less than 5% of the ultraviolet light in sunlight, while 50% of the solar spectrum is visible light, so TiO 2 The absorption efficiency of most of the visible light in sunlight is very low, and its application is greatly limited. In order to make full use of sunlight, the doping modificati...

Claims

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Application Information

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IPC IPC(8): B01J27/24
CPCB01J27/24B01J37/349B01J35/39
Inventor 李爱东曹燕强赵希瑞陈君吴迪
Owner NANJING UNIV
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