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Organometallic polymer ceramic precursor, and preparation method and application thereof

A ceramic precursor and organometallic technology, which is applied in the field of organometallic polymer ceramic precursors and their preparation, can solve the problem of low content of ultra-high temperature resistant component metal materials, low yield of ultra-high temperature resistant ceramics, and conversion efficiency of polymer ceramics. lower problem

Active Publication Date: 2012-06-27
NAT UNIV OF DEFENSE TECH
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  • Abstract
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Problems solved by technology

[0005] At present, the main problems of the ultra-high temperature resistant ceramics prepared by the precursor conversion method are: (1) the solubility of the precursor is poor; (2) the prepared The yield of ultra-high temperature ceramics is too low; (3) The content of ultra-high temperature resistant component metal materials in ceramics is too small
Only people such as Russia Pomogailob have publicly reported that a kind of organometallic polymer containing metal elements has been prepared by the method of vinyl polymerization, and ceramic materials containing higher high temperature resistant components have been prepared after pyrolysis (D. Krutko, M . Borzov, D. Lemenovskii, G. Dzhardimalieva, A. Pomogailob. Synthesis and reactivity of metal-containing monomers. Part 59. Preparation and polymerization transformations of vinyl and isopropenyl derivatives of hafnocene dichloride. Russ. Chem. Bull., Int. Ed ., 2005, 54, 247-251.), but its polymer-ceramic conversion efficiency is low

Method used

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  • Organometallic polymer ceramic precursor, and preparation method and application thereof
  • Organometallic polymer ceramic precursor, and preparation method and application thereof
  • Organometallic polymer ceramic precursor, and preparation method and application thereof

Examples

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reference example 1

[0031] Reference Example 1 Preparation of divinyl zirconocene: Add 29.282 g of dichloro zirconocene into a three-necked flask, add 2000 ml of ether solvent, dissolve, and cool down to -40 o C. Add 0.2 mol of vinyl Grignard reagent to the solution, react at constant temperature for 48 hours, filter after the reaction is completed, remove the solvent under reduced pressure, rinse twice with cold n-pentane, and recrystallize with toluene-n-pentane to obtain white di Vinyl zirconocene, yield 70-90%.

reference example 2

[0032] Reference example 2 Preparation of dipropenyl zirconocene: Add 29.282 g of dichloro zirconocene into a three-necked flask, add 2000 ml of ether solvent, dissolve, and cool down to -40 o C. Add 0.2 mol of propenyl Grignard reagent to the solution, react at constant temperature for 48 hours, filter after the reaction is completed, remove the solvent under reduced pressure, rinse twice with cold n-pentane, and recrystallize with toluene-n-pentane to obtain a white di Propyl zirconocene, yield 60-80%.

[0033] two, Preparation example of polymer containing zirconocene, hafnium and titanium ceramic precursor

Embodiment 1

[0035] Under nitrogen protection, add 0.55 g (0.002 mol) divinylzirconocene (A 2 monomer) and 5 ml toluene at a constant temperature of -20 o C; Add 0.02 g (0.0014 mol) borane (D) dropwise under electromagnetic stirring 3 monomer) pyridine solution (concentration: 2.0 mol / L), reacted for 48 hours, the solution became viscous; added 100 ml of n-pentane, precipitated, filtered, 80 o C is dried, obtains Zr-B-C ceramic precursor polymer pale yellow polymer powder (referring to figure 1 ). Yield 85%.

[0036] The obtained Zr-B-C ceramic precursor polymer is soluble in DMF, NMP, DMAc and DMSO. Through IR, 1 Structural characterization and testing of the precursor polymer by H NMR and TGA, in the IR spectrum, 3095 cm -1 and 2900 cm -1 The positions are the carbon-hydrogen vibration absorption peaks on the precursor polymer ring and the carbon-hydrogen vibration absorption peaks on the methylene on the main chain, respectively, at 1400 cm -1 、1100 cm -1 and 800 cm -1 corre...

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Abstract

The invention relates to an organometallic polymer ceramic precursor, and a preparation method and application thereof. The organometallic polymer ceramic precursor is prepared by copolymerization of a double-bond-containing organometallic zirconium or titanium or hafnium monomer and a boron-containing monomer. By using the organometallic polymer ceramic precursor for preparing M(Zr,Ti,Hf)-B-C ceramic, the ceramic yield is up to 40-60%, and the content of the super-high-temperature-resistant component (ZrC / ZrB2,TiC / TiB2,HfC / HfB2) in the prepared ceramic material is higher than 70 wt%. When being treated at 2000 DEG C for 2 hours, the organometallic polymer ceramic precursor is not subjected to obvious weight loss, thereby having favorable high-temperature resistance.

Description

Technical field [0001] The present invention involves an organic metal polymer ceramic pioneer and its preparation methods and applications. Specifically, it is an organic metal polymeter ceramic pioneer and its preparation methods involving an organic metal polymer containing Ermao (titanium, 铪), as well asIt is used in M (ZR, Ti, HF) -B-C ceramic preparation. Background technique [0002] UHIGH TEMPERAMICS (UHTCS) material is a type of high-temperature-resistant material represented by boronized materials represented by boron bornes and carbides with difficulty melting metals (such as ZR, HF, and TA, etc.).Can run normally.These materials have excellent physical properties, including rare high melting points, high thermal conductivity, high elastic modulus, and maintaining good mechanical properties at high temperatures.Application prospects (S. Levine, E Opila, M. Halbig, Et Al. Evaluation of Ultra-High Temperature Ceramics for AeroPropulsion Use. Journal of the European Ceram...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/08C04B35/515
Inventor 王浩陈兴波王军谢征芳简科王应德高波
Owner NAT UNIV OF DEFENSE TECH
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