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Tantalum-based oxynitride nano powder and preparation method thereof

A technology of oxynitride and nanopowder, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc. It can solve the problems of several hours of preparation time, reduced purity of oxynitride, and low nitriding efficiency. problem, to achieve the effect of high current density, good effect and rapid temperature rise

Active Publication Date: 2019-06-25
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method greatly improves the reaction efficiency, but the preparation time still takes hours
At the same time, the slow heating rate of traditional calcination causes nitrogen sources such as urea to decompose completely below the temperature at which oxynitrides are formed, a large amount of nitrogen sources are lost, and the nitriding efficiency is low, which will also lead to a decrease in the purity of oxynitrides in the product

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  • Tantalum-based oxynitride nano powder and preparation method thereof

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preparation example Construction

[0035] The rapid preparation method of a kind of tantalum-based oxynitride nanopowder of the present invention comprises the following steps:

[0036] S1. Dissolving alkaline earth metal salt, tantalum salt and nitrogen source in alcohol, ball milling and drying to obtain a mixed precursor;

[0037] S2. Put the mixed precursor obtained in step S1 into a reaction vessel, and perform discharge plasma calcination under a protective atmosphere to obtain tantalum-based oxynitride nanopowder.

[0038] The present invention adopts the combination of discharge plasma calcination and nitrogen source one-step synthesis method to prepare tantalum-based oxynitride. Due to the Joule effect and electric field effect, the heating is very efficient, and the whole process only takes a few minutes, compared with the traditional preparation method (several hours or even tens of Hours) greatly shorten the preparation time, and the cost is also lower.

Embodiment 1

[0040] A rapid preparation method of a tantalum-based oxynitride nanopowder in this embodiment comprises the following steps:

[0041] S1. Add 3.5g of strontium carbonate, 4.5g of tantalum pentoxide and 4.8g of urea into 35ml of absolute ethanol, and ball mill for 240min to obtain a mixed slurry;

[0042] S2. Drying the mixed slurry obtained after ball milling in step S1. The drying process is as follows: heat preservation at 60° C. for 24 hours to obtain a mixed precursor;

[0043] S3. Put the mixed precursor obtained in step S2 in a reaction container, place the reaction container in a pressureless plasma calcination equipment, and perform discharge plasma calcination in a nitrogen atmosphere, with a heating rate of 300°C / min and a temperature of 1000°C. Time 1min; finally cool to room temperature with the furnace to get SrTaO 2 N oxynitride powder, that is, tantalum-based oxynitride nanopowder, its phase composition and microscopic morphology are as follows figure 2 and ...

Embodiment 2

[0052] A rapid preparation method of a tantalum-based oxynitride nanopowder in this embodiment comprises the following steps:

[0053] S1, 4.8g of barium carbonate, 4.5g of tantalum pentoxide and 4.8g of urea were added to 40ml of absolute ethanol, and ball milled for 240min to obtain a mixed slurry;

[0054] S2. Drying the mixed slurry obtained after ball milling in step S1. The drying process is as follows: heat preservation at 60° C. for 24 hours to obtain a mixed precursor;

[0055] S3. Put the mixed precursor obtained in step S2 in a reaction container, place the reaction container in a pressureless plasma calcination equipment, and perform discharge plasma calcination in a nitrogen atmosphere, with a heating rate of 300°C / min and a temperature of 1000°C. Time 1min; finally cool down to room temperature with the furnace to get BaTaO 2 N oxynitride powder, that is, tantalum-based oxynitride nanopowder, its phase composition and microscopic morphology are as follows Figu...

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Abstract

The invention discloses a preparation method of tantalum-based oxynitride nano powder, and the preparation method comprises the following steps: S1, dissolving an alkaline earth metal salt, a tantalumsalt and a nitrogen source in an alcohol, and performing ball milling and drying to obtain a mixed precursor; and S2, placing the mixed precursor obtained in the step S1 into a reaction container, and performing non-pressure discharge plasma calcination under a protective atmosphere to obtain the tantalum-based oxynitride nano powder. The preparation method of the invention has short preparationperiod, and the purity of the prepared tantalum-based oxynitride nano powder is high.

Description

technical field [0001] The invention relates to the technical field of preparation of high-performance dielectric ceramic materials, in particular to a tantalum-based oxynitride nanopowder and a preparation method thereof. Background technique [0002] Perovskite Oxynitride SrTaO 2 N and BaTaO 2 N has attracted extensive attention from scholars at home and abroad because of its extremely high dielectric constant at room temperature. In the two crystal structures, Ta atoms and O / N atoms constitute Ta(O,N) 6 Octahedral and Ta is located in the center of the octahedron, and the A atom is located between the octahedrons and occupies the eight vertices of the unit cell. Due to the difference in the radius of the A atom and the Ta atom and the various arrangements of the N atoms, Ta(O,N) 6 The octahedron is tilted to different degrees, which changes the bond length and bond angle of Ta-O / N-Ta, and Ta ions deviate from the central position to generate spontaneous polarization. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/626B82Y30/00
Inventor 李端李斌曾良
Owner NAT UNIV OF DEFENSE TECH