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A kind of carbide high-entropy ceramic precursor and high-entropy ceramic and preparation method

A technology of ceramic precursors and carbides, which is applied in the fields of carbide high-entropy ceramic precursors and high-entropy ceramics and its preparation, which can solve problems such as unfavorable long-term storage and application field restrictions, and achieve the effect of uniform distribution of elements

Active Publication Date: 2021-03-26
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the liquid precursor provided by the patent is a sol, which is not conducive to long-term storage, so it will be limited in the application field

Method used

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  • A kind of carbide high-entropy ceramic precursor and high-entropy ceramic and preparation method
  • A kind of carbide high-entropy ceramic precursor and high-entropy ceramic and preparation method
  • A kind of carbide high-entropy ceramic precursor and high-entropy ceramic and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] In this example, the following methods are used to prepare precursors and high-entropy ceramics:

[0051] (1) Obtain metal alkoxide: select metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ta(OPr) 5 , Mo(OCH 2 CH 2 OCH 2 CH 3 ) 5 and W(OCH 2 CH 2 OCH 3 ) 6 , where Hf(OPr) 4 、Ta(OPr) 5 , Mo(OCH 2 CH 2 OCH 2 CH 3 ) 5 and W(OCH 2 CH 2 OCH 3 ) 6 is the metal salt HfCl 4 , TaCl 5 、MoCl 5 and WCl 6 Disperse in n-heptane respectively, at -10°C, add monohydric alcohol n-propanol, n-propanol, ethylene glycol ethyl ether, ethylene glycol methyl ether dropwise, and then drop triethylamine respectively, heat to reflux after dropping 1h, respectively filter to obtain metal alkoxide solution; wherein, the ratio of metal salt, monohydric alcohol and triethylamine is respectively 1:4:4, 1:5:6, 1:6:5, 1:8:7;

[0052] (2) Preparation of metal alkoxide complexes: under the condition of 40°C, the metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ta(OPr) 5 , Mo(OCH 2 CH 2 OCH 2 CH 3...

Embodiment 2

[0057] In this example, the following methods are used to prepare precursors and high-entropy ceramics:

[0058] (1) Obtain metal alkoxide: select metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ti(Oi-Pr) 4 , Mo(OCH 2 CH 2 OCH 2 CH 3 ) 5 and W(OCH 2 CH 2 OCH 3 ) 6 , where Hf(OPr) 4 , Mo(OCH 2 CH 2 OCH 2 CH 3 ) 5 and W(OCH 2 CH 2 OCH 3 ) 6 Prepared by the method of Example 1;

[0059] (2) Preparation of metal alkoxide complexes: under the condition of 80°C, the metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ti(Oi-Pr) 4 , Mo(OCH 2 CH 2 OCH 2 CH 3 ) 5 , W(OCH 2 CH 2 OCH 3 ) 6 Add acetylacetone dropwise, and continue to stir for 1h after dropping; the metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ti(Oi-Pr) 4 , Mo(OCH 2 CH 2 OCH 2 CH 3 ) 5 , W(OCH 2 CH 2 OCH 3 ) 6 The molar ratio with acetylacetone is respectively 1:1, 1:1, 1:2, 1:1 and 1:2;

[0060] (3) Co-hydrolysis: Mix the metal alkoxide complexes obtained in step (1) uniformly in an equal metal molar ratio, and ...

Embodiment 3

[0064] In this example, the following methods are used to prepare precursors and high-entropy ceramics:

[0065] (1) Obtain metal alkoxide: select metal alkoxide Zr(Oi-Pr) 4 、Hf(Oi-Pr) 4 、Ti(OPr) 4 and Ta(OCH 2 CH 2 OCH 3 ) 5 , where Hf(Oi-Pr) 4 and Ta(OCH 2 CH 2 OCH 3 ) 5 is the metal salt HfCl 4 , TaCl 5 Disperse in xylene and tert-butyl methyl ether respectively. At 0°C, add monohydric alcohol isopropanol and ethylene glycol methyl ether dropwise, and then drop triethylamine respectively. After the dropwise addition, heat to reflux for 2 hours, and filter separately to obtain Metal alkoxide solution; Wherein, the ratio of metal salt, monohydric alcohol and triethylamine is respectively 1:4:4 and 1:10:6;

[0066] (2) Preparation of metal alkoxide complexes: at room temperature, respectively to metal alkoxide Zr(Oi-Pr) 4 、Hf(Oi-Pr) 4 、Ti(OPr) 4 and Ta(OCH 2 CH 2 OCH 3 ) 5 Add ethyl acetoacetate dropwise, and continue to stir for 0.5h after dropping; metal ...

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Abstract

The invention discloses a carbide high-entropy ceramic precursor, a high-entropy ceramic and a preparation method. The precursor comprises at least four of Ti, Zr, Hf, V, Nb, Ta, Mo and W, the amountof substance of each metal element accounts for 5-35% of the total amount of substance of the precursor, and the precursor is dissolved in methanol, ethanol, isopropanol, n-propanol, n-butanol, isobutanol, ethylene glycol monomethyl ether or ethylene glycol ethyl ether. The precursor is prepared by respectively complexing a plurality of metal alkoxides, mixing, co-hydrolyzing and mixing with a carbon source for reaction. According to the preparation method of the precursor, the ratio of the raw materials in the steps is finely adjusted, so that all elements in the precursor are uniformly distributed at the molecular level, all metal elements are in short-range diffusion in the cracking process, and the solid solution temperature of all elements is relatively low. The high-entropy ceramic is high-performance ceramic, which is prepared on the basis of the precursor and has a single crystalline phase, and all elements are uniformly distributed in a molecular level.

Description

technical field [0001] The invention belongs to the technical field of high-entropy materials, and in particular relates to a carbide high-entropy ceramic precursor, high-entropy ceramics and a preparation method. Background technique [0002] High-entropy ceramics are a new type of ceramics that have emerged in recent years. The concept of this ceramic comes from high-entropy alloys, which usually refer to a single-phase solid solution formed by solid-dissolving five or more metal compounds in a (nearly) equimolar ratio. High-entropy ceramics not only enrich the types of ceramics, but also endow materials with rich performance adjustment space due to the novel "high-entropy effect" brought about by the synergy of multiple groups. [0003] The research on carbide high-entropy ceramics is currently mainly focused on transition metal IVB and VB carbide solids. These carbides have rock-salt structure, strong covalent bond characteristics and high melting point, so the required ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L61/06C08L85/00C04B35/56
CPCC04B35/5607C04B35/5611C04B35/5622C04B35/5626C04B2235/48C08L61/06C08L85/00
Inventor 叶丽孙娅楠韩伟健陈凤华赵彤
Owner INST OF CHEM CHINESE ACAD OF SCI