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Nonpolar zirconium carbide liquid-phase ceramic precursor, preparation method therefor and application thereof

A technology of ceramic precursor and zirconium carbide liquid, which is applied in the field of non-polar zirconium carbide liquid phase ceramic precursor and its preparation, can solve the problems of zirconium difficulty and system incompatibility, so as to improve the ceramic production rate and reduce the loss of Zr element , The effect of simple process

Active Publication Date: 2016-01-06
SUZHOU TUNABLE MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The current research on ultra-high temperature ceramic precursors is mainly based on the preparation of refractory metal carbides and boride precursors. Among them, the research on ZrC precursors mainly uses zirconium polyacetylacetonate as the zirconium source, and the obtained precursors are soluble in polar solvents. The polycarbosilane (PCS) used to prepare C / SiC materials is non-polar, and the two systems are not compatible, which makes it difficult to introduce zirconium into the preparation of anti-oxidation C / SiC materials.

Method used

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  • Nonpolar zirconium carbide liquid-phase ceramic precursor, preparation method therefor and application thereof
  • Nonpolar zirconium carbide liquid-phase ceramic precursor, preparation method therefor and application thereof
  • Nonpolar zirconium carbide liquid-phase ceramic precursor, preparation method therefor and application thereof

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Experimental program
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Effect test

Embodiment 1

[0062] Heat 227.5g of propyl zirconate in n-propanol (zirconium content 20.05%, concentration 72%, containing 0.5mol propyl zirconate) to 90°C, add 25g (0.25mol) acetylacetone dropwise, and control the rate of addition, 2 After 1 hour of dropwise addition, the mixture was heated to reflux for 1 hour. Keep heating to reflux, continue to slowly add dropwise a mixed solution of 9.9g (0.55mol) of water and 30g of n-propanol, and then heat to reflux for 2 hours after the dropwise addition is completed for 2 hours. The temperature was lowered to room temperature, and most of the solvent was removed by rotary evaporation to obtain a n-propanol solution of polyziroxane (denoted as PNZ-1). Add 54.7g of divinylbenzene and stir to dissolve, continue rotary steaming at 70℃~75℃ for 0.5h to ensure complete removal of n-propanol solvent, and finally add a small amount of xylene to adjust the solution viscosity to 50~500mpa.s to obtain homogeneous and transparent Precursor solution (referred...

Embodiment 2

[0071] Heat 227.5g of propyl zirconate in n-propanol (zirconium content 20.05%, concentration 72%, containing 0.5mol propyl zirconate) to 90°C, add 50g (0.5mol) acetylacetone dropwise, and control the dropping rate, 2 After 1 hour of dropwise addition, the mixture was heated to reflux for 1 hour. Keep heating to reflux, continue to slowly add dropwise a mixed solution of 8.1 g (0.45 mol) of water and 30 g of n-propanol, and then heat to reflux for 2 hours after the dropwise addition is completed. The temperature was lowered to room temperature, and most of the solvent was removed by rotary evaporation to obtain a n-propanol solution of polyziroxane (referred to as PNZ-2). Add 52.5g of divinylbenzene, stir evenly, further rotary steam at 70℃~75℃ for 0.5h to ensure that the n-propanol solvent is completely removed, and finally add a small amount of xylene to adjust the viscosity of the solution to prepare a homogeneous and transparent precursor solution (denoted as PZC-2). At ...

Embodiment 3

[0078] Heat 227.5g of propyl zirconate in n-propanol (zirconium content 20.05%, concentration 72%, containing 0.5mol propyl zirconate) to 85°C, add 75g (0.75mol) acetylacetone dropwise, and control the rate of addition, 2 After 1 hour of dropwise addition, the mixture was heated to reflux for 1 hour. Keep heating to reflux, continue to slowly add dropwise a mixed solution of 7.2g (0.4mol) of water and 30g of n-propanol, and then heat to reflux for 2 hours after the dropwise addition is completed for 2 hours. The temperature was lowered to room temperature, and most of the solvent was removed by rotary evaporation to obtain a n-propanol solution of polyziroxane (referred to as PNZ-3). Add 50.2 g of divinylbenzene and stir to dissolve, and further rotate steam at 70°C to 75°C for 0.5h to ensure that the n-propanol solvent is completely removed, and finally add a small amount of xylene to adjust the viscosity of the solution to prepare a homogeneous and transparent precursor solu...

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Abstract

The invention relates to a nonpolar zirconium carbide liquid-phase ceramic precursor, a preparation method therefor and application thereof. The preparation method comprises: firstly preparing a nonpolar zirconium polymer-polyzircooxane through coordination protection of propyl zirconate and controllable hydrolysis condensation reaction; and by using the polyzircooxane as a zirconium source and divinyl benzene as a carbon source, compounding the components to obtain the nonpolar zirconium carbide liquid-phase ceramic precursor. The liquid-phase precursor prepared by the invention has the characteristics of polymer resin; the viscosity of the precursor can be controlled between 50 mpa.s and 500 mpa.s by adjusting the solid content, and the manufacturability is good. The zirconium carbide liquid-phase ceramic precursor which is cured and thermally treated can be converted into a pure-phase zirconium carbide ceramic at a relatively low temperature ( for example, 1500 DEG C). The liquid-phase ceramic precursor prepared by the invention is expected to be used as impregnating resin for a ceramic-based composite material and an antioxidant C / C and C / Si composite material so as to improve the ultra-high temperature antioxidant performance of the material and reduce the ablativity of the material.

Description

technical field [0001] The invention relates to a non-polar zirconium carbide liquid-phase ceramic precursor and a preparation method and application thereof. Background technique [0002] In recent years, the development of near-space vehicles has put forward higher requirements for the ablation resistance of carbon / carbon (C / C) and carbon / silicon carbide (C / SiC), two types of lightweight, high-strength, and high-temperature-resistant composite materials. The material is required to have a lower ablation rate or even zero ablation, so that it can be used in various extreme environments such as high-speed long-duration flight, atmospheric re-entry, and trans-atmospheric flight. Studies have shown that introducing carbides and borides of refractory metals such as Zr, Hf, and Ta into C / C and C / SiC composites can effectively improve the ablation resistance of the composites, and obtain oxidation-resistant C / SiC, C / SiC C composite materials greatly expand the application of C / S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/56C04B35/622
Inventor 邱文丰赵彤韩伟健
Owner SUZHOU TUNABLE MATERIALS TECH CO LTD
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