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Preparation method and application of gallium-indium-zinc ternary nitrogen oxide

A nitrogen oxide, gallium indium zinc technology, applied in the field of chemistry, can solve the problems of less than 5% solar energy utilization rate, energy waste, affecting the catalytic effect, etc., to improve the photocatalytic complete water splitting activity, good crystallinity, and ensure uniformity. sexual effect

Active Publication Date: 2019-05-14
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

The two have many things in common. Both GaN and ZnO are UV-responsive semiconductors. Their band gaps are 3.4eV and 3.2eV respectively, and their utilization rate of solar energy is less than 5%.
The advantage of the high-temperature sintering method is that the method is relatively simple. It only needs to mix and nitride the raw materials, but it also has certain disadvantages. Long-term high-temperature sintering and volatilization lead to a decrease in the zinc content of the solid solution, especially the content of Zn close to the surface layer is even close to zero.
However, as we all know, the catalytic reaction is a surface reaction, such a result will not only reduce its visible light application range, but will certainly affect the catalytic effect
In addition, the composition of the obtained product is not particularly uniform by simply nitriding the precursor, which will also affect the photocatalytic activity and reproducibility of the sample.

Method used

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  • Preparation method and application of gallium-indium-zinc ternary nitrogen oxide
  • Preparation method and application of gallium-indium-zinc ternary nitrogen oxide
  • Preparation method and application of gallium-indium-zinc ternary nitrogen oxide

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preparation example Construction

[0033] In order to optimize the preparation process of this type of material, the present invention provides a preparation method of nano-core-shell gallium indium zinc oxynitride. By using solvothermal-refrigeration-calcination technology, the metal precursor can be prepared into nano At the same time, creatively using the characteristic that In has a relatively faster evaporation rate than Zn, it is embedded in a large number of Zn vacancies in the surface layer during the nitriding process, thus forming a core-shell structure with different internal and external components. Calculations prove that the structure can promote the separation of photogenerated carriers, and then obtain excellent photocatalytic activity.

[0034] A method for preparing a gallium indium zinc ternary oxynitride with a core-shell structure, comprising the following steps:

[0035] (1) with Ga(NO 3 ) 3 ·xH 2 O, In(NO 3 ) 3 ·xH 2 O and Zn(Ac) 2 2H 2 O was used as the source of gallium, indium ...

Embodiment 1

[0040] This embodiment includes the following steps:

[0041] (1) 1.25mmol Ga(NO3)3 xH2O, 1.25mmol In(NO3)3 xH2O and 2.5mmol Zn(Ac)2 2H2O were added to reaction glass bottles filled with 4mL ethanolamine and 0.1mL acetic acid respectively, Using solvothermal method, keep at 60°C for 2 hours, transfer to corundum porcelain boat, seal with aluminum foil, transfer to low temperature (0-2°C) and keep for 1 week;

[0042] (2) Put the gel-like precursor obtained by keeping the low temperature for a long time in step (1) in a muffle furnace, raise the temperature to 500°C at a rate of 3°C / min, and bake at this temperature for 10h, and then follow the furnace Cool to room temperature to obtain light yellow GIZO fluffy powder;

[0043] (3) the GIZO powder that step (2) obtains is transferred in the tube furnace, in 200sccm ammonia gas (NH 3 ) at a flow rate of 5°C / min to 850°C and held for 10 hours, and then cooled to room temperature at a rate of 3°C / min to obtain GIZNO nanomaterial...

Embodiment 2

[0045] This embodiment includes the following steps:

[0046] (1) 1.25mmol Ga(NO 3 ) 3 ·xH 2 O, 1.25mmol In(NO 3 ) 3 ·xH 2 O and 2.5mmol Zn(Ac) 2 2H 2 O was added to reaction glass bottles filled with 4mL ethanolamine and 0.1mL acetic acid respectively, and kept at 50°C for 1h by solvothermal method, then transferred to a corundum porcelain boat, sealed with aluminum foil, and then transferred to a low temperature (0~ 2°C) for 1 week;

[0047] (2) Put the gel-like precursor obtained by keeping the low temperature for a long time in step (1) in a muffle furnace, raise the temperature to 600°C at a rate of 3°C / min, and bake at this temperature for 8 hours, and then follow the furnace Cool to room temperature to obtain light yellow GIZO fluffy powder;

[0048] (3) the GIZO powder that step (2) obtains is transferred in the tube furnace, in 200sccm ammonia gas (NH 3 ) at a flow rate of 5°C / min to a certain temperature T°C (T=600) for 12 hours, and then cooled to room tem...

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Abstract

The invention discloses a preparation method of gallium-indium-zinc ternary nitrogen oxide. Ga(NO3)3*xH2O, Zn(Ac)2*2H2O, In(NO3)3*XH2O serve as a gallium source, a zinc source and an indium source, ethanol amine and a small amount of acetic acid serve as solvents, uniform precursor mixed solution is acquired by a solvent thermal method, a precursor is placed in a low-temperature environment for along time and is gel-like, the precursor is roasted at high temperature to obtain faint yellow gallium-indium-zinc oxide (GIZO), and finally, high-temperature nitridation is performed in ammonia atmosphere to prepare a grayish-green GIZNO nano-material. The prepared GIZNO has an obvious core-shell structure, density functional theory (DFT) calculation proves that the core-shell structure can effectively promote separation of photon-generated carriers in the photocatalytic water splitting process, and photocatalytic water splitting can be efficiently performed. 1wt% of rhodium (Rh) is loaded toserve as a co-catalyst, under the irradiation condition of visible light (lambda>=420nm), photocatalytic water splitting hydrogen production rate is 603 micromoles h<-1> g<-1>, oxygen production rateis 274 micromoles h<-1> g<-1>, the apparent quantum efficiency of a 430nm position reaches 3.5%, and a good application prospect is shown.

Description

technical field [0001] The invention belongs to the field of chemistry and relates to the technical field of photocatalytic nano material preparation, in particular to a preparation method and application of a nano-core-shell gallium indium zinc ternary nitrogen oxide. Background technique [0002] In 2005, Domen et al prepared GaN / ZnO photocatalyst by direct nitriding solid solution method, and conducted in-depth analysis on its synthesis method, characterization results, material modification and other aspects. This is the first nitride solid solution photocatalyst that decomposes pure water under visible light, and it is also a very efficient photocatalyst that can decompose pure water using visible light. Gallium nitride has a hexagonal wurtzite structure and is currently mainly used in semiconductor lighting and is the core component of light-emitting diodes. The application of zinc oxide is relatively wide, its band gap and exciton binding energy are large, and it has...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/02C01B3/04B82Y30/00B82Y40/00
CPCY02E60/36
Inventor 刘茂昌符文龙薛飞
Owner XI AN JIAOTONG UNIV
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