Carbide high-entropy ceramic precursor containing rare earth, high-entropy ceramic and preparation method

A ceramic precursor, rare earth carbide technology, applied in the field of high-entropy materials to achieve good storage performance and small viscosity changes

Active Publication Date: 2020-06-19
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

[0008] At present, there is no research report on carbide high-entropy ceramics containing rare earth metals, and the introduction of rare earth metals can not only enrich the types of high-entropy ceramics, but also may make ceramics have certain functions.

Method used

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  • Carbide high-entropy ceramic precursor containing rare earth, high-entropy ceramic and preparation method
  • Carbide high-entropy ceramic precursor containing rare earth, high-entropy ceramic and preparation method
  • Carbide high-entropy ceramic precursor containing rare earth, high-entropy ceramic and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] In this example, the following methods are used to prepare precursors and high-entropy ceramics:

[0052] (1) Obtain metal alkoxide: select metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ta(OPr) 5 and Ti(OPr) 4 , where Hf(OPr) 4 、Ta(OPr) 5 is the metal salt HfCl 4 , TaCl 5 Disperse in n-heptane and ethylene glycol dimethyl ether respectively. At -10°C, add monohydric alcohol n-propanol dropwise, and then drop triethylamine respectively. After the dropwise addition, heat and reflux for 1 hour, and filter separately to obtain metal alkoxides Solution, final vacuum distillation obtains metal alkoxide; Wherein, the ratio of metal salt, monohydric alcohol and triethylamine is respectively 1:4:4, 1:5:6;

[0053] (2) Preparation of metal alkoxide complexes: under the condition of 40°C, the metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ta(OPr) 5 and Ti(OPr) 4Add acetylacetone dropwise, and continue to stir for 0.1h after dropping; the metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ta(OPr) 4 、...

Embodiment 2

[0058] In this example, the following methods are used to prepare precursors and high-entropy ceramics:

[0059] (1) Obtain metal alkoxide: select metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ti(Oi-Pr) 4 , Ta(OCH 2 CH 2 OCH 2 CH 3 ) 5 and Nb(OCH 2 CH 2 OCH 3 ) 5 , where Hf(OPr) 4 , Ta(OCH 2 CH 2 OCH 2 CH 3 ) 5 and Nb(OCH 2 CH 2 OCH 3 ) 5 is the metal salt HfCl 4 , TaCl 5 and NbCl 5 Disperse in n-heptane, n-hexane and ethylene glycol dimethyl ether respectively, at -10°C, drop monohydric alcohol n-propanol, ethylene glycol ethyl ether and ethylene glycol methyl ether, and then drop triethylamine respectively, After the dropwise addition, heat to reflux for 1 hour, filter to obtain the metal alkoxide solution, and finally distill under reduced pressure to obtain the metal alkoxide; wherein, the ratios of metal salt, monohydric alcohol and triethylamine are 1:4:4, 1:5:6, respectively. and 1:6:6;

[0060] (2) Preparation of metal alkoxide complexes: under the cond...

Embodiment 3

[0065] In this example, the following methods are used to prepare precursors and high-entropy ceramics:

[0066] (1) Obtain metal alkoxide: metal alkoxide Zr(OPr) 4 、Hf(OPr) 4 、Ti(Oi-Pr) 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 Separately disperse in toluene, at -5°C, add monohydric alcohol n-propanol, n-propanol, ethylene glycol ethyl ether, ethylene glycol methyl ether dropwise, and then add triethylamine dropwise, heat to reflux for 1 hour after the dropwise addition, Filtrate respectively 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;

[0067] (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 、Ta(OPr)...

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Abstract

The invention discloses a carbide high-entropy ceramic precursor containing rare earth. The precursor comprises at least four transition metal elements and at least one rare earth metal element, and the precursor is dissolved in one or more of 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 transition metal alkoxides, mixing the obtained complex with a compound containing rare earth elements, carrying out co-hydrolysis, and performing reactionwith a carbon source. According to the preparation method of the precursor, the ratio of all the raw materials in the step is finely adjusted, so that all the elements in the precursor are uniformly distributed at a molecular level, all the metal elements are subjected to short-range diffusion in the cracking process, and all the elements can be subjected to solid solution at a relatively low temperature. The preparation of the high-entropy ceramic is different from laser sintering and oxidation reduction in a traditional method, and the high-performance ceramic with a single crystalline phaseand with all elements in a molecular-level uniform distribution state is prepared on the basis of the precursor.

Description

technical field [0001] The invention belongs to the technical field of high-entropy materials, and in particular relates to a rare earth-containing 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 p...

Claims

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Application Information

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IPC IPC(8): C08L61/06C08L85/00C04B35/622C04B35/56
CPCC04B35/56C04B35/5607C04B35/5611C04B35/5622C04B35/5626C04B35/622C04B2235/3817C04B2235/3839C04B2235/3843C04B2235/3847C08L61/06C08L85/00
Inventor 叶丽孙娅楠韩伟健陈凤华赵彤
Owner INST OF CHEM CHINESE ACAD OF SCI
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