A kind of zrc/sic/c composite phase ceramic precursor material and preparation method thereof

A technology of multiphase ceramics and precursors, which is applied in the field of ZrC/SiC/C multiphase ceramic precursors and their preparation, can solve the problems of limited reaction activity of zirconocene dichloride, limited amount of zirconium introduced, and long time consumption.

Active Publication Date: 2020-10-23
INST OF CHEM CHINESE ACAD OF SCI
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the limited reactivity of zirconocene dichloride, the process of preparing the precursor in this invention has a high temperature and takes a long time, and the introduction of zirconium is limited

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of zrc/sic/c composite phase ceramic precursor material and preparation method thereof
  • A kind of zrc/sic/c composite phase ceramic precursor material and preparation method thereof
  • A kind of zrc/sic/c composite phase ceramic precursor material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] In this example, the ZrC / SiC / C composite ceramic precursor was prepared by the following method:

[0044] (1) A 100mL dry three-necked bottle, equipped with a rubber stopper, a condenser tube, and a three-way joint, put in a stirring magnet, added 1.46g (5.0mmol) zirconocene dichloride, 0.41g (5.0mmol) polydimethyl For silicon acetylene, vacuumize and fill the system with argon several times to replace the air in the system, then add 10mL of tetrahydrofuran and mix well;

[0045] (2) Cool the reaction flask containing the mixture of step (1) to -60°C, add 4.2mL (10.0mmol) 2.4M n-hexane solution of n-butyllithium dropwise to the reaction flask under stirring, and control the temperature of the system at - 40°C, after the dropwise addition, remove the cooling bath;

[0046] (3) The system in which n-butyllithium was added dropwise in step (2) was raised to 20° C. and continued to stir and react for 24 hours, and a white solid salt was precipitated in the system;

[0047...

Embodiment 2

[0050] In this example, the ZrC / SiC / C composite ceramic precursor was prepared by the following method:

[0051] (1) A 100mL dry three-necked bottle, equipped with a rubber stopper, a condenser tube, and a three-way joint, put it into a stirring magnet, and added 1.46g (5.0mmol) of zirconocene dichloride, 0.82g (10.0mmol) of polydimethyl For silicon acetylene, vacuumize and fill the system with argon several times to replace the air in the system, then add 12mL of tetrahydrofuran and mix well;

[0052] (2) Cool the reaction flask containing the mixture of step (1) to -60°C, add 4.2mL (10.0mmol) 2.4M n-hexane solution of n-butyllithium dropwise to the reaction flask under stirring, and control the temperature of the system at - 40°C, after the dropwise addition, remove the cooling bath;

[0053] (3) The system in which n-butyllithium was added dropwise in step (2) was raised to 20° C. and continued to stir and react for 24 hours, and a white solid salt was precipitated in the ...

Embodiment 3

[0057] This example is based on Example 1. In step (1), the added amount of polydimethylsilylacetylene is adjusted to 0.492g (6.0mmol), the added amount of tetrahydrofuran is 10.4mL, and the rest of the implementation methods are the same as the examples 1. The precursor was cured at 250 °C for 2 h in an argon atmosphere, and then pyrolyzed at 1600 °C for 2 h in an argon atmosphere to obtain a black ceramic product. XRD and elemental analysis showed that the product was a ZrC / SiC / C composite ceramic with a Zr content of 57.5 wt%, Si content is 15.3 wt%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a ZrC / SiC / C composite ceramic precursor material and a preparation method thereof; the precursor is pyrolyzed and converted into a composite ceramic at a temperature of 1600 DEG C, the zirconium content in the composite ceramic is not less than 50 wt%, and the silicon content in the composite ceramic is not less than 10 wt%. The preparation method of the precursor is characterized in that polysilylacetylene, zirconocene dichloride and n-butyllithium are subjected to a one-pot reaction under anhydrous and anaerobic conditions to synthesize the precursor, the zirconocenedichloride is used as a zirconium source, the polysilylacetylene is used as a silicon source, and the n-butyllithium is added at a low temperature to carry out a further reaction to prepare the precursor. The polymer precursor prepared by the method is expected to be used as a dipping matrix of a ceramic-based composite material and a carbon / carbon composite material so as to improve the ultrahigh-temperature oxidation resistance of the ceramic-based composite material and the carbon / carbon composite material.

Description

technical field [0001] The invention belongs to the field of multiphase materials, and in particular relates to a ZrC / SiC / C multiphase ceramic precursor and a preparation method thereof. Background technique [0002] Carbon / carbon composites have low density and excellent thermal and mechanical properties. They have become a good anti-ablation material and high-temperature structural material, and are widely used in aerospace and many civil industries. Although carbon / carbon composites have excellent performance in an inert atmosphere, they are easily oxidized in a high-temperature aerobic environment. With the continuous improvement of application requirements, research on high-temperature oxidation resistance and anti-ablation protection of carbon / carbon composites is of great significance. A large number of studies have shown that the application of ultra-high temperature ceramic refractory metal carbides can improve the oxidation resistance of carbon / carbon composites, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60C04B35/56
CPCC04B35/5622C04B2235/3826C04B2235/422C04B2235/483C08G77/60
Inventor 吴雨桓赵彤叶丽韩伟健
Owner INST OF CHEM CHINESE ACAD OF SCI
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap