Nitride high-entropy ceramic fiber and preparation method and application thereof

A technology of ceramic fiber and nitride, applied in the field of nitride high-entropy ceramic fiber and its preparation, can solve the problems of high-entropy ceramic fiber without nitride, high-entropy ceramic without nitride, powder material easily falling off, etc. The effect of spinning efficiency, convenient operation and low cost

Active Publication Date: 2020-08-28
INST OF CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2012, V.Braic et al. from Romania deposited a layer of (TiZrNbHfTa)N coating on the surface of stainless steel by physical vapor deposition, which increased the surface hardness to 33GPa. Compared with traditional metal coatings, the surface hardness increased More than three times (V.Braic, Alina Vladescu, Nanostructured multi-element (TiZrNbHfTa) N and (TiZrNbHfTa) C hard coatings, Surface & Coatings Technology, 211 (2012): 117-121), but the physical vapor deposition method requires higher equipment , can only prepare a single two-dimensional material such as a coating, and its application range is limited; in 2018, East China University of Science and Technology, the University of Tennessee, and Oak Ridge National Laboratory jointly developed a method for preparing high-entropy nitride ceramic powders. method, this method uses metal chloride and urea as raw materials to prepare a single crystal form (VCrNbMoZr)N nanopowder at 800 °C, which shows potential application value in supercapacitors (Tian Jin, Xiahan Sang ,Mechanochemical-Assisted Synthesis of High-Entropy Metal Nitride via a Soft Urea Strategy,2018(30):1707512), but powder materials have problems such as easy to fall off and uneven dispersion in the preparation of devices
[0007] At present, there is no report on nitride high-entropy ceramic fibers, and there is no precedent for applying nitride high-entropy ceramics to the field of photocatalysis

Method used

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  • Nitride high-entropy ceramic fiber and preparation method and application thereof
  • Nitride high-entropy ceramic fiber and preparation method and application thereof
  • Nitride high-entropy ceramic fiber and preparation method and application thereof

Examples

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Embodiment 1

[0055] This example provides a general preparation method for high-entropy ceramic precursors, as follows:

[0056] (1) Obtain metal alkoxides: select transition metal alkoxides containing different types of elements. When M in the metal alkoxides is Hf, Nb, Ta or Mo, the alkoxides are prepared as follows: metal salt MCl n or M(NO 3 ) n Disperse in a solvent, add monohydric alcohol dropwise at -10~5°C, then drop triethylamine, heat to reflux for 1~5h after the dropwise addition, and filter to obtain metal alkoxide solution; among them, metal salt, monohydric alcohol and triethylamine The ratio of ethylamine is 1:(1~2)n:(1~1.5)n; the solvent is n-hexane, n-heptane, toluene, xylene, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, One or more of tert-butyl methyl ether; the monohydric alcohol is selected from one of methanol, ethanol, isopropanol, n-propanol, n-butanol, isobutanol, ethylene glycol methyl ether, and ethylene glycol ether species or several;

[0...

Embodiment 2

[0066] In this embodiment, the following method is used to prepare nitride high-entropy ceramic fibers:

[0067] (1) Preparation of spinnable precursor solution: adopt the method described in Example 1 to prepare a carbide high-entropy ceramic precursor containing Ti, Hf, Ta, Nb, Mo, get 30 g of the high-entropy ceramic precursor, and polymerize Vinylpyrrolidone 10g, ethanol 150g, mixed and stirred to obtain a tan uniform solution;

[0068] (2) Spinning and collection: using compressed air as the gas source, the precursor solution obtained in step (1) is stretched into nanofibers by using an air spinning device, the spinning air pressure is 0.09MPa, and the feed rate is 30mL / h , the receiving distance is 40cm;

[0069] (3) Debinding: place the nanofiber cotton collected in step (2) in a heat treatment device, raise the temperature to 600°C at a heating rate of 1°C / min under a nitrogen atmosphere, and keep it warm for 2 hours to obtain debinding fibers ;

[0070](4) Nitridin...

Embodiment 3

[0073] In this embodiment, the following method is used to prepare nitride high-entropy ceramic fibers:

[0074] (1) Preparation of spinnable precursor solution: adopt the method described in Example 1 to prepare a carbide high-entropy ceramic precursor containing Ti, Hf, Ta, Nb, Mo, get 30 g of the high-entropy ceramic precursor, and polymerize Vinyl butyral 10g, n-propanol 285g, mixed and stirred to obtain a tan uniform solution;

[0075] (2) Spinning and collection: using compressed nitrogen as the gas source, the precursor solution obtained in step (1) was stretched into nanofibers by using an air spinning device, the spinning pressure was 0.06MPa, and the feed rate was 30mL / h , the receiving distance is 40cm;

[0076] (3) Debinding: place the nanofiber cotton collected in step (2) in a heat treatment device, raise the temperature to 600°C at a heating rate of 1.5°C / min under an argon atmosphere, and keep it warm for 2 hours to obtain debinding fiber;

[0077] (4) Nitri...

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Abstract

The invention discloses a nitride high-entropy ceramic fiber and a preparation method and application thereof. The high-entropy ceramic fiber contains Ti, Hf, Ta, Nb and Mo elements, the nitride high-entropy ceramic fiber is in a single crystalline phase, and all the elements are uniformly distributed in a molecular level. The preparation method of the high-entropy ceramic fiber comprises the following steps: uniformly mixing a carbide high-entropy ceramic precursor containing a target metal element, a spinning aid and a solvent to prepare a precursor spinning solution, and then carrying out spinning, degumming and nitriding processes to prepare the nitride high-entropy ceramic fiber. The nitride high-entropy ceramic fiber can be applied to a process for preparing methane by photocatalysisof carbon dioxide.

Description

technical field [0001] The invention belongs to the technical field of high-entropy ceramics, and in particular relates to a nitride high-entropy ceramic fiber and its preparation method and application. Background technique [0002] High-entropy ceramics are single-phase solid-solution ceramics composed of at least five elements, each element content is 5-35%. So far, people's research on high-entropy ceramics is still relatively small. At present, high-entropy ceramics only exist in the form of powder, block and coating, and the research on the performance of high-entropy ceramics is also limited to a few fields. [0003] Nitride high-entropy ceramics are ceramics with a single crystal form composed of at least five metal elements and nitrogen elements. Current research is mainly focused on the preparation of nitride high-entropy ceramic coatings and powders. In 2012, V.Braic et al. from Romania deposited a layer of (TiZrNbHfTa)N coating on the surface of stainless steel ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/622B01J27/24B01J35/06C07C1/02C07C9/04
CPCC04B35/58007C04B35/58014C04B35/58028C04B35/62286B01J27/24B01J35/004B01J35/06C07C1/02C07C2527/24C07C9/04B01J35/1009B01J35/002B01J37/033B01J23/28C07C45/77C07C1/20C07C67/31C04B35/63476C04B35/63424C04B35/63416C04B35/6342C04B35/63444C04B35/6263C04B35/6264C04B35/6325C04B2235/465C04B2235/3239C04B2235/3244C04B2235/3251C04B2235/3256D01F9/08D01D1/02D01D10/02C01B21/0602C01P2002/72C01P2004/04C07C49/92C07C69/732C04B2235/524
Inventor 赵彤李伟叶丽陈凤华孙娅楠
Owner INST OF CHEM CHINESE ACAD OF SCI
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