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Ultrahigh-temperature ceramic precursor capable of being subjected to melt spinning as well as preparation method and application thereof

A technology of ultra-high temperature ceramics and ceramic precursors, applied in the field of ceramic materials, can solve the problems of poor melting performance, poor ultra-high temperature performance, lack of anti-oxidation components, etc., and achieve good flexibility, good solubility, and excellent melting performance. Effect

Active Publication Date: 2022-02-18
NAT UNIV OF DEFENSE TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention provides a melt-spinning ultra-high temperature ceramic precursor and its preparation method and application, which are used to overcome the lack of antioxidant components, Defects such as poor ultra-high temperature performance and poor melting performance

Method used

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  • Ultrahigh-temperature ceramic precursor capable of being subjected to melt spinning as well as preparation method and application thereof
  • Ultrahigh-temperature ceramic precursor capable of being subjected to melt spinning as well as preparation method and application thereof
  • Ultrahigh-temperature ceramic precursor capable of being subjected to melt spinning as well as preparation method and application thereof

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preparation example Construction

[0024] The present invention proposes a method for preparing a melt-spinning ultra-high temperature ceramic precursor, comprising the following steps:

[0025] S1: Weighing Cp in proportion 2 ZrCl 2 and reducing metal filings, the Cp 2 ZrCl 2 and reducing metal filings are added to the first reaction solvent, heated and kept warm, filtered after cooling, and the equivalent active species Cp 2 Zr(II) solution;

[0026] Preferably, the Cp 2 ZrCl 2 The reaction molar ratio with reducing metal shavings is 1:3~10. In order to make Cl replaced more fully, the present invention uses excessive reducing metal shavings (Cp 2 ZrCl 2 The reaction ratio with reducing metal shavings is 1:2), among which 1:6 is better, which ensures sufficient reaction and does not cause large waste.

[0027] Preferably, the reducing metal scrap is Mg scrap; the first reaction solvent is one of anhydrous tetrahydrofuran (THF) and anhydrous N,N-dimethylformamide (DMF). When a common solvent containi...

Embodiment 1

[0041] This embodiment provides a method for preparing a melt-spinnable ultra-high temperature ceramic precursor, comprising the following steps:

[0042] S1: Weigh Cp at a molar ratio of 1:6 2 ZrCl 2 and Mg filings, the Cp 2 ZrCl 2 and Mg scraps were added to anhydrous THF, heated to 60°C for 4 hours, cooled and filtered to remove excess Mg scraps to obtain the black-purple equivalent active species Cp 2 Zr(II) solution.

[0043] S2: Press Cp 2 Zr(Ⅱ) solution and ClCH 2 (CH 3 ) 2 Si-NH-Si(CH 3 ) 2 CH 2 The molar ratio of Cl is 5:4 to weigh ClCH 2 (CH 3 ) 2 Si-NH-Si(CH 3 ) 2 CH 2 Cl, take xylene equivalent to the above-mentioned anhydrous THF, and ClCH 2 (CH 3 ) 2 Si-NH-Si(CH 3 ) 2 CH 2 Cl and xylene are added to Cp 2 In the Zr(II) solution, stir well at room temperature, raise the temperature from room temperature to 60°C and keep it at 60°C for 10h, then raise the temperature from 60°C to 130°C and keep it at 130°C for 6h, after cooling, filter to remo...

Embodiment 2

[0049] This embodiment provides a method for preparing a melt-spinnable ultra-high temperature ceramic precursor, comprising the following steps:

[0050] S1: Same as Example 1.

[0051] S2: Same as Example 1.

[0052] S3: heating the oligomer precursor to 200° C. to make it into a molten state, reacting at 200° C. for 3 hours, and cooling to room temperature to obtain a crude product of the PZCSN ceramic precursor.

[0053] S4: Same as Example 1.

[0054] By changing the reaction time, explore the effect of melting reaction time on the structure and properties of PZCSN ceramic precursors, and found that increasing the reaction time, the softening point of the resinous precursor is 72.2-88.6 ° C, indicating that increasing the reaction time has a significant effect on the softening point of the polymer precursor Little effect, meanwhile, its ceramic yield increased to 53.62wt%. The obtained precursor is melt-spun at 130° C., and the obtained fibrils have a diameter of about...

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Abstract

The invention discloses an ultrahigh-temperature ceramic precursor capable of realizing melt spinning as well as a preparation method and application thereof. The preparation method comprises the following steps: firstly, reacting Cp2ZrCl2 with reducing metal to generate an equivalent active species Cp2Zr (II); then adding 1,3-bis(chloromethyl) tetramethyldisilazane and a second reaction solvent into the Cp2Zr (II), and carrying out solution reaction through a heating procedure to obtain an oligomer; and heating the oligomer so that the oligomer reacts in a molten state to obtain the PZCSN ceramic precursor. The preparation method provided by the invention is simple in process and suitable for large-scale production. The ceramic precursor prepared by the preparation method is a linear polymer with a Zr-C-Si-N main chain structure, contains antioxidant components such as Si, N and the like, has a softening point of 80.8-89.2 DEG C, has good solubility in solvents such as toluene, xylene, THF, DMF and the like, has excellent melting performance, and can be used for preparing ultrahigh-temperature ceramic fibers.

Description

technical field [0001] The invention relates to the technical field of ceramic materials, in particular to a melt-spinning ultra-high temperature ceramic precursor and its preparation method and application. Background technique [0002] Ultra-high temperature ceramics have excellent properties such as high temperature resistance, oxidation resistance and chemical inertness, but their application is limited due to the intrinsic brittle fracture of ceramics. Ultra-high temperature ceramic fibers have a thermal expansion coefficient and comprehensive properties similar to those of ultra-high-temperature ceramic substrates, and are an important material for strengthening and toughening ultra-high-temperature ceramics. [0003] At present, the preparation methods of ultra-high temperature ceramic fibers mainly include chemical gas phase reaction method, sol-gel method and organic precursor conversion method. Among them, the organic precursor conversion method can effectively co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C04B35/515C04B35/622
CPCC08G77/60C04B35/515C04B35/62272
Inventor 韩成高强王小宙王应德
Owner NAT UNIV OF DEFENSE TECH
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