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Mesoporous silica protected ultra-thin ferro-nickel nitride composite material and preparation thereof

A technology of mesoporous silicon dioxide and ferronickel nitride, which is applied in the field of nanomaterials, can solve the problems of limiting the application of ferronickel nitride and increasing the size of ferronickel nitride nanoparticles, achieving mild conditions, improving catalytic performance, Simple and mild preparation method conditions

Active Publication Date: 2018-01-16
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the high-temperature ammoniation process, the precursor nickel-iron hydrotalcite will be seriously agglomerated, making the size of the final nickel-iron nitride nanoparticles larger, and a large number of active sites are shielded, which limits the further application of nickel-iron nitride.

Method used

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  • Mesoporous silica protected ultra-thin ferro-nickel nitride composite material and preparation thereof
  • Mesoporous silica protected ultra-thin ferro-nickel nitride composite material and preparation thereof
  • Mesoporous silica protected ultra-thin ferro-nickel nitride composite material and preparation thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1) The preparation method of nickel-iron hydrotalcite in this example adopts the method recorded in the document C.J.Wang, D.O'Hare,.Synthesis oflayered double hydroxide nanoparticles in a novelmicroemulsion.J.Mater.Chem.2012,22,21125. Proceed as follows:

[0030] 15 mL of n-butanol and 24 mL of N,N-dimethyltetradecyl tertiary amine were placed in the reactor, and stirred at high speed for 10 min to obtain a microemulsion environment. NiCl 2 ·6H 2 O and FeCl 3 ·6H 2 O was added to the reactor at a molar ratio of 3:1, the total amount of metal ions was 6 mmol, and mixed uniformly. The mixed solution was hydrothermally crystallized in a high-closed system at 120°C for 24h. After the reaction, the product was washed by centrifugation with ethanol-water (1:1) mixed solution for at least 5 times, and dried in an oven at 60°C to obtain nickel-iron hydrotalcite

[0031] 2) Nickel-iron hydrotalcite composite NiFe-LDH@SiO protected by mesoporous silica 2 Preparation of: ...

Embodiment 2～3

[0039] Repeat Example 1, the difference is only that the total amount of metal ions of the added nickel salt and iron salt is changed to 3mmol and 9mmol. The diameter of the ultra-thin nickel-iron nitride in the obtained composite catalyst is 18-22nm, the thickness is 2.8-3.2nm, SiO 2 The pore diameter of the mesopore is 2.4-3.2 nm.

Embodiment 4～9

[0041] Repeat Example 1, the only difference being that the nickel salt and the iron salt are changed in molar ratio: 2.2:1, 2.4:1, 2.6:1, 2.8:1, 3.2:1, 3.4:1. After changing the molar ratio of nickel salt and iron salt, the ultrathin nickel-iron nitride composite protected by mesoporous silica cannot be obtained. The result is an ultrathin nickel-iron nitride-nickel-iron alloy composite protected by mesoporous silica.

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Abstract

The invention discloses a mesoporous silica protected ultra-thin ferro-nickel nitride composite material and preparation thereof. The structure of the composite material is Ni3FeN@SiO2, and the composite material comprises an ultra-thin ferro-nickel nitride base layer and mesoporous silica coating the surface of the ultra-thin ferro-nickel nitride base layer. The preparation method comprises the following steps: obtaining a ferro-nickel hydrotalcite precursor through a reverse micro-emulsion method; under the existence of a surface active agent and a silicon source, using a sol-gel method to coat the silica material of a mesoporous structure on the surface of the ferro-nickel hydrotalcite precursor to obtain an original composite material; burning the original composite material in an ammonia gas atmosphere so as to obtain the final mesoporous silica protected ultra-thin ferro-nickel nitride composite material. The preparation method is mild in conditions and applicable generally, andagglomeration in the burning process is avoided; and the obtained mesoporous silica protected ultra-thin ferro-nickel nitride composite material has excellent activity in catalyzed ammonia borane hydrolysis hydrogen production reactions.

Description

technical field [0001] The invention relates to the technical field of nanometer materials, in particular to an ultra-thin nickel-iron nitride composite material protected by mesoporous silicon dioxide and its preparation. Background technique [0002] Transition metal nitrides have good catalytic effects in many important chemical reactions, such as ammonia synthesis, hydrodenitrogenation, hydrodesulfurization and hydrotreating. Recently, thanks to the unique electronic structure and metal properties of transition metal nitrides, scientists have extended the application of transition metal nitrides to energy. The metallic nature of transition metal nitrides makes transition metal nitrides an inexpensive electrode material for many energy conversion and storage devices, such as fuel cells, metal-air batteries, and electrocatalytic water splitting systems. Nickel iron nitride (Ni 3 FeN) is a promising transition metal nitride that can be applied to these reactions. Nickel-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06C01B33/12C01B3/06B01J27/24B01J33/00
Inventor 张铁锐张鑫赵宇飞加晓丹尚露吴骊珠佟振合
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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