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Method for synthesizing tantalum-based nitride (nitrogen oxide) nanoparticles, and nanoparticles thereof

A nanoparticle, tantalum-based nitrogen technology, applied in the field of nanomaterials, can solve the problems of difficult raw materials, difficult to achieve industrialization, long reaction time, etc., achieve product quality and high yield, good application and industrialization prospects, and breakthrough safety. Effects of pitfalls and limitations

Inactive Publication Date: 2017-02-15
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] According to literature reports, traditional metal nitride synthesis methods can be roughly divided into the following categories: 1) temperature programming method, the temperature of the nitride precursor is raised by a set program, but due to the high temperature (>750 ° C), the synthesis conditions Harsh, difficult to achieve industrialization
2) Thermal decomposition method, using metal organic compounds or metal organic compound salts to heat and decompose metal nitrides under carrier gas, but it is difficult to synthesize metal organic compounds and their salts for some metals, which has limitations
3) Solid state reaction method, using metal powder, metal oxide, or metal salt as metal source, NaN 3 etc. as nitrogen source, and synthesize metal nitrides after solid-state reaction, but this method requires high pressure, and the nitrogen source used is expensive
4) The ball milling method is to make the raw materials fully mixed and refined and reacted by ball milling under a certain atmosphere, but due to the long reaction time, the raw materials are difficult to completely react, making it difficult to use on a large scale
However, there is no report on the effective realization of controllable nitriding

Method used

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  • Method for synthesizing tantalum-based nitride (nitrogen oxide) nanoparticles, and nanoparticles thereof
  • Method for synthesizing tantalum-based nitride (nitrogen oxide) nanoparticles, and nanoparticles thereof
  • Method for synthesizing tantalum-based nitride (nitrogen oxide) nanoparticles, and nanoparticles thereof

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Experimental program
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Effect test

Embodiment 1

[0043] 0.25g TaCl 5 (0.7mM) was dissolved in 2mL of methanol, then 0.103g of strontium chloride (0.65mM) was added, after dissolution, 0.084g of urea (1.4mM) was added, and stirred at room temperature for 4h to gel. It was roasted at 700° C. for 5 h in a nitrogen flow, and the obtained product was treated with 1 mol / L hydrochloric acid and stirred at room temperature for 48 h. The obtained product was washed several times with ethanol, filtered with suction, and dried at 50°C. Tantalum oxynitride nanoparticles A (TaON) were obtained.

Embodiment 2

[0045] 0.25g TaCl 5 (0.7mM) was dissolved in 2mL of methanol, then 0.103g of strontium chloride (0.65mM) was added, and after dissolution, 0.294g of urea (4.9mM) was added, and stirred at room temperature for 4h to gel. It was roasted at 700° C. for 5 h in a nitrogen flow, and the obtained product was treated with 1 mol / L hydrochloric acid and stirred at room temperature for 48 h. The obtained product was washed several times with ethanol, filtered with suction, and dried at 50°C. Obtain tantalum pentanitride nanoparticles B (Ta 3 N 5 ).

Embodiment 3

[0047] 0.25g TaCl 5 (0.7mM) was dissolved in 2mL of methanol, then 0.103g of strontium chloride (0.65mM) was added, after dissolution, 0.084g of urea (1.4mM) was added, and stirred at room temperature for 4h to gel. It was calcined at 700° C. for 5 h in an argon flow, and the obtained product was treated with 1 mol / L hydrochloric acid and stirred at room temperature for 48 h. The obtained product was washed several times with ethanol, filtered with suction, and dried at 50°C. Tantalum oxynitride nanoparticles C(TaON) were obtained.

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Abstract

The invention belongs to the technical field of nanometer materials, and discloses a method for controllably synthesizing tantalum-based nitride (nitrogen oxide) nanoparticles, and nanoparticles thereof. The method comprises: dissolving a tantalum salt in an organic alcohol, adding an alkaline earth metal salt and an organic nitrogen source, stirring to obtain a precursor, placing into an inert atmosphere, carrying out high temperature calcination, and treating with a hydrochloric acid solution to obtain the tantalum-based nitride (nitrogen oxide) nanoparticles. According to the present invention, the method has advantages of mild condition and environmental protection, and breaks through the safety hazard and the limitation caused by the traditional method using NH3; by simply regulating the nitrogen source consumption, the precise control of the product nitrification degree is achieved; by effectively regulating the density of the empty orbit unoccupied by d in the tantalum, the product has the catalysis property similar to the precious metals; and the obtained nanoparticles have wide application prospects in the fields of benzene hydrogenation, Fischer-Tropsch synthesis, hydrodesulfurization / hydrodenitrification, alcohol decomposition-hydrogen production and other fine chemical industry catalysis reactions, fuel cell electrode catalysis materials, sensors, electrical materials, and other fields.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, in particular to a method for controllably synthesizing tantalum-based nitrogen (oxide) oxide nanoparticles and the nanoparticles. Background technique [0002] Transition metal nitride represented by tantalum nitride has become one of the most promising catalytic materials in the past 10 to 20 years due to its unique noble metal-like electronic structure, catalytic performance, and good thermal stability. Especially in recent years, with the rapid rise of oil prices, the efficient and green utilization of energy and resources has become increasingly popular, and the development of photocatalytic properties and hydrogen-related catalytic reactions of nitrides and nitrogen oxides has further attracted people's attention. . In addition, since the raw materials for the synthesis of such transition metal nitrides and nitrogen oxides are relatively cheap and easy to obtain, it is also of ...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/02
Inventor 高庆生杨晓芸
Owner JINAN UNIVERSITY
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