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Non-stoichiometric oxynitride nano powder and preparation method thereof

A non-stoichiometric, oxynitride technology, applied in nanotechnology and other directions, can solve the problems of prolonged preparation time, slow gas-solid reaction diffusion, etc., and achieve the effect of improving purity, low cost and high product purity

Active Publication Date: 2021-10-08
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the diffusion of the gas-solid reaction in the second step of ammoniation is slow, and the reaction is often limited to the gas-solid contact surface. To increase the yield, it is necessary to stop and grind the powder in the middle of the reaction, which greatly prolongs the preparation time. Therefore, it is necessary to Further explore more efficient preparation and optimization process

Method used

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  • Non-stoichiometric oxynitride nano powder and preparation method thereof
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  • Non-stoichiometric oxynitride nano powder and preparation method thereof

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Effect test

Embodiment 1

[0031] A preparation method of the non-stoichiometric oxynitride nanopowder of the present invention, comprising the following steps:

[0032] (1) 3g of europium trioxide, 3.75g of tantalum pentoxide and 5.45g of urea were added to 50mL of absolute ethanol, and ball milled for 240min to obtain a mixed slurry;

[0033] (2) Drying the mixed slurry obtained in step (1), the drying process is as follows: heat preservation at 60° C. for 24 hours to obtain mixed precursor powder;

[0034](3) Place the mixed precursor powder obtained in step (2) in a crucible, and then calcined in a nitrogen atmosphere at a heating rate of 100°C / min, a temperature of 1100°C, and a holding time of 1min; finally, it was cooled to room temperature with the furnace, that is Get EuTa(O,N) 3 Oxynitride nano powder;

[0035] (4) EuTa(O,N) obtained in step (3) 3 The oxynitride nano powder is subjected to ammoniation annealing treatment in an ammonia atmosphere, that is, the temperature is raised to 1100°C...

Embodiment 2

[0038] A preparation method of the non-stoichiometric oxynitride nanopowder of the present invention, comprising the following steps:

[0039] (1) Add 3 g of europium trioxide powder, 3.75 g of tantalum pentoxide powder and 5.45 g of urea into 50 mL of absolute ethanol, and ball mill for 240 min to obtain a mixed slurry;

[0040] (2) Dry the mixed slurry obtained after ball milling in step (1). The drying process is as follows: heat preservation at 60° C. for 24 hours to obtain mixed precursor powder;

[0041] (3) Place the mixed precursor powder obtained in step (2) in a crucible, and then calcined in a nitrogen atmosphere at a heating rate of 100°C / min, a temperature of 1100°C, and a holding time of 1min; finally, it was cooled to room temperature with the furnace, that is Get EuTa(O,N) 3 Oxynitride nano powder;

[0042] (4) EuTa(O,N) obtained in step (3) 3 The oxynitride nanopowder is subjected to ammoniation annealing treatment in an ammonia atmosphere, that is, the tem...

Embodiment 3

[0044] A preparation method of the non-stoichiometric oxynitride nanopowder of the present invention, comprising the following steps:

[0045] (1) Add 3 g of europium trioxide powder, 3.75 g of tantalum pentoxide powder and 5.45 g of urea into 50 mL of absolute ethanol, and ball mill for 240 min to obtain a mixed slurry;

[0046] (2) Dry the mixed slurry obtained after ball milling in step (1). The drying process is as follows: heat preservation at 60° C. for 24 hours to obtain mixed precursor powder;

[0047] (3) Place the mixed precursor powder obtained in step (2) in a crucible, and then calcined in a nitrogen atmosphere at a heating rate of 100°C / min, a temperature of 1100°C, and a holding time of 1min; finally, it was cooled to room temperature with the furnace, that is Get EuTa(O,N) 3 Oxynitride nano powder;

[0048] (4) EuTa(O,N) obtained in step (3) 3 The oxynitride nano powder is subjected to ammoniation annealing treatment in an ammonia atmosphere, that is, the te...

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Abstract

The invention discloses non-stoichiometric oxynitride nano powder and a preparation method thereof. The preparation method comprises the following steps: firstly, dissolving europium oxide powder, tantalum pentoxide powder and urea in absolute ethyl alcohol, carrying out ball milling to obtain mixed slurry, drying the mixed slurry to obtain mixed precursor powder, calcining the mixed precursor powder in a protective atmosphere to obtain EuTa(O, N)3 oxynitride nano powder, and carrying out ammonification annealing treatment on the EuTa(O, N)3 oxynitride nano powder in an ammonia atmosphere to obtain the oxynitride nano powder EuTaOaNb with the non-stoichiometric ratio, wherein a is more than or equal to 1.5 and less than or equal to 2.5, b is more than or equal to 0.5 and less than or equal to 1.5, and a:bis not equal to 2:1. According to the invention, the method has the advantages of low cost, simple process, high product purity and the like, and the prepared product is good in dielectric property and magnetism.

Description

technical field [0001] The invention relates to the technical field of preparation of high-performance dielectric ceramic materials, in particular to a non-stoichiometric oxynitride nano powder and a low-cost preparation method thereof. Background technique [0002] Rare earth perovskite oxynitrides are a new class of functional materials that have received international attention in recent years. This type of oxynitride is obtained by introducing N atoms and rare earth metal cations into the corresponding binary rare earth perovskite oxide ABOx. The common types are AB(O,N) 3 ,A 2 BO 3 N or A(B,B') 1 (O, N) 3 etc., where A is a rare earth element (such as La, Nd, Pr, Eu, etc.), and B / B' is a transition metal element (such as Ta, Ti, Nb, Mo, Zr, W, etc.). In its crystal structure, B atoms usually form B(O,N) with O / N atoms 6 octahedral with the B atom at the center of the octahedron. Due to the different arrangement of O / N atoms (cis and trans) and B(O,N) 6 Depending...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/626B82Y40/00
CPCC04B35/58007C04B35/58C04B35/62605C04B35/6268B82Y40/00C04B2235/3224C04B2235/3251C04B2235/465Y02E60/36
Inventor 李端李俊生曾良
Owner NAT UNIV OF DEFENSE TECH
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