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Nanometer hollow structure of multi-metal nitrogen oxide as well as preparation method and application of nanometer hollow structure

A multi-metal oxide and hollow structure technology, applied in the field of nanomaterials, can solve the problems of limited material application, large pH difference, and inability to prepare nano-structured multi-metal oxynitride, and achieve the effect of expanding the scope of application

Active Publication Date: 2015-09-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example Maeda, K.; Teramura, K.; Lu, D. et al, J. Phys. Chem. B, 2006, 110, 13753-13758; Maeda, K.; Teramura, K.; Lu, D. et al , Nature 2006, 440 (7082), 295-295; Japanese Patent JP2005144210-A are all reported (for the preparation process see figure 1 ), first of all, multi-metal oxides containing zinc oxide and gallium oxide should be prepared by co-precipitation, because Zn 2+ , Ga 3+ The precipitation pH of the two ions is very different (the formation of Zn 2+ The pH of the precipitate is about 6, forming Ga 3+ The pH of the precipitation is about 3), and during the co-precipitation process will lead to Ga 3+ Precipitate first and Zn 2+ post-precipitation, so that after the entire co-precipitation is completed, the particle size of the gallium-rich oxide in the multi-metal oxide is precipitated and grown first, which is much larger than the particle size of the zinc-rich oxide, so the manufacturing Large size (200 nanometers to 2 microns) and uneven size distribution of the obtained multi-metal oxide material particles
And the subsequent high-temperature nitriding process requires a temperature above 900°C. At such a high temperature, it must undergo a solid-state reaction process, and the materials in the mixture will undergo severe melting and agglomeration, making the obtained multi-metal nitrogen oxidation. The particle size of the compound is further increased (on the order of 10 microns), so the existing technology cannot produce nanostructured polymetallic oxynitride, which greatly limits the application of this type of material

Method used

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  • Nanometer hollow structure of multi-metal nitrogen oxide as well as preparation method and application of nanometer hollow structure
  • Nanometer hollow structure of multi-metal nitrogen oxide as well as preparation method and application of nanometer hollow structure
  • Nanometer hollow structure of multi-metal nitrogen oxide as well as preparation method and application of nanometer hollow structure

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Experimental program
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Effect test

Embodiment 1

[0063] Embodiment 1 (Ga 0.82 Zn 0.18 )(N 0.82 o 0.18 ) Preparation of hollow nanospheres

[0064] (1) Configure the adsorption solution: 0.005 moles of ZnCl 2 and 0.005 molar GaCl 3 Dissolve in 100mL of DMF to obtain an adsorption solution with a total molar concentration of 0.1M;

[0065] (2) Adsorption: 2 grams of carbon sphere templates (with carboxyl and hydroxyl groups on the surface) with a diameter of 500 nanometers are added to the adsorption solution prepared in step 1), and the content of the carbon sphere template in the adsorption solution is 20g / L. The adsorption solution was sonicated for 30 minutes, stirred and adsorbed at room temperature for 12 hours, and then filtered with a filter membrane with a pore size of 450 nm to obtain carbon spheres adsorbing polymetallic ions, which were placed at 70°C and dried for 40 hours;

[0066] (3) Template removal: put the template dried in step 2) into a tube furnace for heat treatment in air at 800°C for 3 hours, and...

Embodiment 2

[0068] Embodiment 2 (Ga 0.21 Zn 0.79 )(N 0.21 o 0.79 ) Preparation of hollow nanospheres

[0069] (1) Configure the adsorption solution: mix 4.8 moles of Zn(NO 3 ) 2 and 0.2 molar Ga(NO 3 ) 3 Dissolve in 100mL of DMF to obtain an adsorption solution with a total molar concentration of 50M;

[0070] (2) Adsorption: 0.1 g of a carbon sphere template (with carboxyl and hydroxyl groups on the surface) with a diameter of 2 microns is added to the adsorption solution prepared in step 1), and the content of the carbon sphere template in the adsorption solution is 1 g / L. The adsorption solution was sonicated for 30 minutes, stirred and adsorbed at room temperature for 12 hours, and then filtered with a filter membrane with a pore size of 450 nm to obtain carbon spheres adsorbing polymetallic ions, which were placed at 70°C and dried for 40 hours;

[0071] (3) Template removal: Put the template dried in step 2) into a tube furnace for heat treatment in the air environment at 30...

Embodiment 3

[0073] Embodiment 3 (Ga 0.5 Zn 0.5 )(N 0.5 o 0.5 ) Preparation of hollow nanospheres

[0074] (1) Configure the adsorption solution: 0.0009 moles of ZnSO 4 and 0.0001 molar Ga 2 (SO 4 ) 3 Dissolve in 100mL of ethyl acetate to obtain an adsorption solution with a total molar concentration of 0.001M;

[0075] (2) Adsorption: 10 grams of a carbon sphere template (with carboxyl and hydroxyl groups on the surface) with a diameter of 300 nanometers is added to the adsorption solution prepared in step 1), and the content of the carbon sphere template in the adsorption solution is 100 g / L. The adsorption solution was sonicated for 40 minutes, stirred and adsorbed at room temperature for 12 hours, and then filtered with a filter membrane with a pore size of 250 nm to obtain carbon spheres adsorbing polymetallic ions, which were placed at 70°C and dried for 40 hours;

[0076] (3) Template removal: put the template dried in step 2) into a tube furnace for heat treatment in air a...

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Abstract

The invention discloses a nanometer hollow structure of multi-metal nitrogen oxide as well as a preparation method and application of the nanometer hollow structure. The nanometer hollow structure material of the multi-metal nitrogen oxide is prepared and obtained by using a template adsorption method, a multi-metal ion solution and subsequent nitrogen treatment. The nanometer hollow structure of an oxide with multiple metal components is nitrogenized and prepared into the nanometer hollow structure of various nitrogen oxide, such as a solid solution nitrogen oxide (Ga1-xZnx)(N1-xOx), a chemometry nitrogen oxide LaTiO2N, and a mixed nitrogen oxide (Ga1-xZnx)(N1-xOx)-InN. The specific surface area of the nanometer hollow structure is larger than or equal to 50m<2>. g<-1>, which is far larger than the specific surface area (smaller than or equal to 5m<2>. g<-1>) of conventional multi-metal nitrogen oxide; the shell layer thickness of the nanometer hollow structure is smaller than or equal to 20 nanometers; the granule size of the nanometer hollow structure is smaller than or equal to 10 nanometers, which is far smaller than the granule size (micron dimension) of conventional multi-metal nitrogen oxide; therefore, the defects that the multi-metal nitrogen oxide is difficult to realize nanocrystallization and the specific surface area is extremely low are overcome; the use efficiency of a catalyst can be greatly improved, the usage amount of the catalyst is reduced, and the catalyst has good application prospects; in addition, the nanometer hollow structure can also be used for the respects of gas catalysis, gas sensitivity, lithium ion batteries and the like.

Description

technical field [0001] The invention relates to the field of nanomaterials, in particular to a multi-metal oxynitride nano hollow structure and its preparation method and application. Background technique [0002] In recent years, the energy crisis has become increasingly prominent and the environmental problems caused by fossil fuels have become more and more serious. Finding clean new energy is a major issue in the new century. Using semiconductor photocatalysis to produce H from water 2 It is one of the effective ways to obtain clean energy, but most semiconductors are not suitable for photocatalytic hydrolysis of H 2 . Metal nitrides and metal oxynitrides are a new catalyst system. In particular, nitrides and oxynitrides containing multiple metal components, because of the presence of multiple metal components and oxygen and nitrogen, make multi-metal oxynitride not only reduce the bandgap width but also regulate the position of the energy band , so this compound is ...

Claims

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Application Information

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IPC IPC(8): C01B21/082
Inventor 朱丽萍李亚光宋辉楼子瑞肖慕
Owner ZHEJIANG UNIV
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