A kind of hfc/c ceramic precursor polymer and preparation method thereof

A technology of polymers and compounds, applied in the field of polymer materials, can solve problems such as structural characterization of side reactions that cannot be ruled out, few researches on the conversion of hafnium carbide ceramics, and complex reaction processes, etc., to achieve low oxygen content, reduce weight loss, and ensure solubility. Effect

Active Publication Date: 2021-08-31
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For hafnium-containing polymer systems, bifunctional monomers can be used for polymerization, such as diols or diacids reacted with hafnium compounds to construct hafnium oxide polymers, or double carbanogens and dichlorohafnocenes to synthesize hafnium carbon polymers, However, most of the products obtained from these systems are insoluble products, and side reactions cannot be ruled out and structural characterizations are performed. The cracked products often contain hafnium oxide.
In addition, hafnium n-butoxide and hafnium dimethylamino hafnium are used to modify silicon-based polymers, and after cracking, a special structure product with metal components dispersed in silicon-based ceramics is produced. The metal content of this type of system is very low and the same The reaction process is complicated
Soluble hafnium polymers with a clear coordination structure have not been reported so far, and there are few related studies on the transformation of hafnium carbide ceramics

Method used

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  • A kind of hfc/c ceramic precursor polymer and preparation method thereof
  • A kind of hfc/c ceramic precursor polymer and preparation method thereof
  • A kind of hfc/c ceramic precursor polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] 100ml single-mouth flask, 2.0 mmol of tetramethyl alcohol, 2.0 mmol of four-salted seed Yang, 3, 3'-diaminobliphenine, 20 mL of N-methylpyrrolidone, stirring at 25 ° C for ligand exchange polymerization The reaction mixture was added to 120 mL of methanol, and there was a yellow solid precipitation, and the precursor polymer shown in the formula I provided by the present invention was obtained.

[0056] Its nuclear magnetic spectrum and carbon species are respectively figure 1 with figure 2 As shown, it is known that the product structure is correct and is a target product.

[0057] The GPC characterization number average molecular weight is 3750 (the corresponding IN is 4.7), the GPC spectrum is image 3 Indicated.

[0058] The precursor polymer was placed in an argon atmosphere of 1600 ° C for 2 h, resulting in a black ceramic product, ceramic yield of 59.4%, XRD and Raman spectroscopy showed that the product was HFC / C ceramic, and its XRD and Raman spectrum respectively...

Embodiment 2

[0062] The 100ml single-mouth flask was added 1.0 mmol of tetra-plycetol and 1.0 mmol of tetraisopropanol, 2.0 mmol of four-salted seed Yang-3,3'-diaminobliphenylamine, 10 mL of N-methylpyrrolidone and 10 ml of tetrahydrofuran was stirred at 25 ° C for ligand to exchange polymerization at 24 h, and then the reaction mixture was added to 120 mL of methanol, yellow solid precipitation, which was filtered to obtain a precursor polymer shown in the formula I provided by the present invention.

[0063] The GPC characterization number average molecular weight is 4100 (N is 5.1 in accordance with the corresponding I).

[0064] The precursor polymer was placed in an argon atmosphere of 1600 ° C for 2 h, resulting in a black ceramic product, ceramic yield of 61.9%, XRD and Raman spectroscopy showed that the product was HFC / C ceramic.

[0065] Ultra-high temperature performance of the HFC / C ceramic product cannot be detected in the general laboratory, which cannot be melted at 3000 ° C....

Embodiment 3

[0068] The 100ml single-mouth flask was added to 2.0 mmol of tetra-niolfurium and 3.0 mmol of four-salty-3,3'-diaminophenylamine, 10 ml of dimethylformamide and 10 mL of tetrahydrofuran, stirred at 40 ° C The ligand exchanged polymerization was 6 h, followed by adding the reaction mixture to 60 mL of methanol and 60 mL of ethanol, yellow solid precipitation, and filtered to obtain a precursor polymer shown in the formula I provided by the present invention.

[0069] The GPC characterization number average molecular weight is 2460 (N is 3.1 in corresponding I).

[0070] The precursor polymer was placed in an argon atmosphere of 1600 ° C for 2 h, resulting in a black ceramic product, ceramic yield of 57.3%, XRD and Raman spectroscopy showed that the product was HFC / C ceramic.

[0071] Ultra-high temperature performance of the HFC / C ceramic product cannot be detected in the general laboratory, which cannot be melted at 3000 ° C.

[0072] The solubility of the polymer shown in thi...

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Abstract

The invention discloses an HfC / C ceramic precursor polymer material and a preparation method thereof. The polymer has a coordination structure of hafnium and tetraiminetetraphenol, and can be pyrolyzed and converted into HfC / C ceramics at a temperature above 1600° C., and its ceramic yield is not lower than 55 wt%. The preparation method of the polymer is to synthesize the hafnium source compound and the tetraimine tetraphenol monomer through a one-pot polymerization reaction. The polymer precursor prepared by the invention is expected to be used as an impregnated matrix for ceramic matrix composite materials and anti-oxidation carbon / carbon composite materials, so as to improve their ultra-high temperature anti-oxidation properties.

Description

Technical field [0001] The present invention is in the field of polymer materials, in particular to a HfC / C preceramic polymers and preparation method thereof. Background technique [0002] In refractory metal carbide-based ultra-high temperature ceramic to remain relatively stable physical and chemical properties under extreme environmental conditions of high temperature reactive atmosphere and the like, applied to an aircraft heat shield member can improve the oxidation of carbon / carbon composite material and ablation resistance. Hafnium carbide has excellent physical and chemical properties, such as ultra high melting point, high hardness, wear resistance, good electrical and thermal conductivity, and chemical stability, and thus become one of the ultra-high temperature ceramic materials are currently the most attention. Hafnium carbide conventional synthetic methods include solid-state combustion elemental, oxide carbothermal reduction, chemical vapor deposition, etc., th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C04B35/56C04B35/524C04B35/622
CPCC04B35/524C04B35/5622C04B35/622C08G83/008
Inventor 吴雨桓赵彤叶丽韩伟健
Owner INST OF CHEM CHINESE ACAD OF SCI
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