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Preparation method of oxide high-entropy ceramic fiber

A technology of ceramic fibers and oxides, which is applied in the field of preparation of oxide high-entropy ceramic fibers, can solve problems such as complex processes, and achieve the effects of simple preparation processes, good flexibility, and improved fiber quality

Active Publication Date: 2021-08-27
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disclosed in CN110204328A is a preparation method of high-entropy oxide ceramic fibers, using MgO, ZnO, NiO, CuO, CaO, CoO, ZrO2, CeO2, Al2O3, Gd2O3, La2O3, Er2O3, Y2O3, Fe2O3, Co3O4, CaCO3 as raw materials A high-entropy oxide ceramic block is prepared; however, it requires mixing the raw materials to make a green body and pretreatment at 500 °C, and then quickly quenching the sample in cold water after being processed in a scintillation furnace, the process is relatively complicated

Method used

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  • Preparation method of oxide high-entropy ceramic fiber
  • Preparation method of oxide high-entropy ceramic fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A kind of preparation method of hafnium polymer precursor, comprises steps as follows:

[0044] (1) Dissolve 60g of hafnium oxychloride octahydrate in 150g of anhydrous methanol, add 15g of acetylacetone after completely dissolving, and after stirring for 1 hour, add 27g of triethylamine dropwise, and continue stirring for 1 hour after the addition is completed, to obtain yellow clear solution;

[0045] (2) Pour the yellow solution obtained in (1) into a round-bottomed flask, and distill under reduced pressure at 38°C to obtain a dry powder mixed with triethylamine hydrochloride and hafnium polyacetylacetonate, which is then placed in a round-bottomed flask Add 200ml of acetone, seal the round bottom flask, and let it stand for 48 hours;

[0046] (3) filter (2) insoluble triethylamine hydrochloride in the round bottom flask, obtain the acetone solution of polyacetylacetonate hafnium, pour it into the round bottom flask and carry out vacuum distillation to dryness, the ...

Embodiment 2

[0048] A method for preparing oxide high-entropy ceramic fibers, comprising the following steps:

[0049] (1) Dissolve 15g of Zr, Hf, Ti, Y, Gd five element precursors in equimolar ratio into 25g of absolute ethanol, add 0.075g of polyethylene oxide (PEO) for magnetic stirring, and continue stirring for 1 After 1 hour, the uniformly stirred solution was left to stand for 1 hour to obtain the desired high-entropy ceramic precursor spinning solution.

[0050] (2) Electrospinning the prepared spinning solution, the spinning voltage is 9kV, the advancing speed of the syringe pump is 1.5ml / h, the ambient humidity is 30%, and the spinning temperature is room temperature.

[0051] (3) Heat-treat the precursor fibers obtained in (2) at 800°C, with a heating rate of 0.5°C / min before 400°C, a heating rate of 1°C / min from 400°C to 800°C, and a holding time of 2 hours. With furnace cooling, the oxide high-entropy ceramic fiber can be obtained.

[0052] The macroscopic picture of the prepa...

Embodiment 3

[0054] A method for preparing oxide high-entropy ceramic fibers, comprising the following steps:

[0055] (1) Dissolve 15g of Zr, Hf, Ti, Y, Gd five element precursors in equimolar ratio into 25g of absolute ethanol, add 0.075g of polyethylene oxide (PEO) for magnetic stirring, and continue stirring for 1 After 1 hour, the uniformly stirred solution was left to stand for 1 hour to obtain the desired high-entropy ceramic precursor spinning solution.

[0056] (2) Electrospinning the prepared spinning solution, the spinning voltage is 9kV, the advancing speed of the syringe pump is 1.5ml / h, the ambient humidity is 30%, and the spinning temperature is room temperature.

[0057] (3) Heat-treat the precursor fibers obtained in (2) at 1000°C, with a heating rate of 0.5°C / min before 400°C, a heating rate of 1°C / min from 400°C to 1000°C, and a holding time of 2 hours. With furnace cooling, the oxide high-entropy ceramic fiber can be obtained.

[0058] The macroscopic picture of the p...

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Abstract

The invention relates to a preparation method of an oxide high-entropy ceramic fiber. The oxide high-entropy ceramic fiber provided by the invention contains five elements of Zr, Hf, Ti, Ce, Y, La, Gd, Er and Sm. The preparation method comprises the following steps: preparing a spinning solution by taking salt or a precursor corresponding to selected elements as a metal source, absolute ethyl alcohol or absolute methanol as a solvent and polyvinylpyrrolidone or polyoxyethylene as a spinning aid, preparing a precursor fiber by an electrostatic spinning method, and carrying out heat treatment on the precursor fiber in air to obtain the oxide high-entropy ceramic fiber. The prepared oxide high-entropy ceramic fiber is uniform in diameter and has good flexibility. Complex heat treatment is not needed, atmosphere protection is not needed, and the preparation process is simple.

Description

Technical field: [0001] The invention relates to a preparation method of an oxide high-entropy ceramic fiber, belonging to the field of high-entropy ceramics. Background technique: [0002] High-entropy ceramics are multi-component single-phase solid solutions composed of 5 to 13 elements with equiatomic ratio or near equiatomic ratio. High-entropy ceramics have many excellent properties due to their thermodynamic high-entropy effects, structural distortion effects, kinetic hysteresis diffusion effects, and performance "cocktail" effects. They are used in thermal protection, catalysis, energy storage, There are broad application prospects in thermocompression and thermoelectricity. [0003] However, the research on high-entropy ceramics at this stage mainly focuses on the research on ceramic powder and bulk, while the research on high-entropy ceramic fibers is less. Ceramic fibers have the advantages of excellent flexibility, large aspect ratio and specific surface area, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/622C04B35/49C04B35/50C04B35/505
CPCC04B35/62231C04B35/6225C04B35/62259C04B35/48C04B35/50C04B35/505C04B2235/6562C04B2235/6567C04B2235/3227C04B2235/3224C04B2235/3225C04B2235/3229C04B2235/3232C04B2235/3244C04B35/64C04B2235/48
Inventor 朱陆益邓哲哲谢永帅王新强张光辉许东
Owner SHANDONG UNIV