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Preparation method of HfxTa1-xC alloy precursor and HfxTa1-xC alloy obtained through method

A technology of precursors and alloys, which is applied in the field of preparation of HfxTa1-xC alloy precursors and alloys, can solve the problems that the precursors do not have processability, cannot be used for composite materials, coatings or fiber preparation, etc., and achieves excellent solubility, The effect of improved purity and low equipment requirements

Active Publication Date: 2017-04-26
自贡中天胜新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the uncontrollable reaction between the hafnium-tantalum solution and the carbon source, it can only obtain the insoluble precursor of the powder. The precursor is not processable and cannot be prepared for composite materials, coatings or fibers, and the reaction needs to be in Carried out under high pressure (solvent heat is high pressure reaction), the conditions are relatively harsh

Method used

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  • Preparation method of HfxTa1-xC alloy precursor and HfxTa1-xC alloy obtained through method
  • Preparation method of HfxTa1-xC alloy precursor and HfxTa1-xC alloy obtained through method
  • Preparation method of HfxTa1-xC alloy precursor and HfxTa1-xC alloy obtained through method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Hf in this example 0.2 Ta 0.8 The C precursor is synthesized by the following steps:

[0043] 1. Preparation of hafnium alkoxide: Disperse 1 mol hafnium tetrachloride in 30 mol n-hexane solvent, add 4.5 mol n-propanol dropwise at -5°C, then add 4 mol triethylamine dropwise, heat to reflux for 1 hour after the dropwise addition, and filter to obtain Hafnium alkoxide solution;

[0044] 2. Preparation of polyhafoxane: at room temperature, add 0.5 mol acetylacetone dropwise to the hafnium alkoxide solution obtained in step 1, reflux for 0.5 h after dropping, drop to room temperature, add dropwise a mixture of 0.9 mol water and 4 mol n-propanol liquid, dripped and refluxed for 1 hour, and distilled under reduced pressure to obtain polyhafoxane;

[0045] 3. Preparation of tantalum alkoxide: disperse 4 mol tantalum pentachloride in 240 mol petroleum ether, drop 24 mol n-butanol at -5°C, then drop 20 mol triethylamine, heat and reflux for 1 hour after dropping, filter to obt...

Embodiment 2

[0050] Hf in this example 0.8 Ta 0.2 The C precursor is synthesized by the following steps:

[0051] 1. Preparation of hafnium alkoxide: disperse 4 mol hafnium tetrachloride in 200 mol n-heptane solvent, drop 28 mol isopropanol at 10°C, then drop 20 mol triethylamine, heat and reflux for 5 hours after dropping, and filter to obtain hafnium alkoxide solution;

[0052] 2. Preparation of polyhafoxane: at room temperature, add 4 mol ethyl acetoacetate dropwise to the hafnium alkoxide solution obtained in step 1, reflux for 2 hours after dropping, drop to room temperature, add dropwise a mixture of 6 mol water and 32 mol isopropanol , reflux for 2h after dripping, and distill under reduced pressure to obtain polyhafoxane;

[0053] 3. Preparation of tantalum alkoxide: Disperse 1mol tantalum pentachloride in 40mol ethylene glycol dimethyl ether, drop 9mol isobutanol at 10°C, then drop 6mol triethylamine, heat and reflux for 5h after dropping, filter , to obtain tantalum alkoxide ...

Embodiment 3

[0058] Hf in this example 0.5 Ta 0.5 The C precursor is synthesized by the following steps:

[0059] 1. Preparation of hafnium alkoxide: disperse 1 mol hafnium tetrachloride in 40 mol tert-butyl methyl ether solvent, add 5 mol ethylene glycol monomethyl ether dropwise at 0°C, then add 4.5 mol triethylamine, and heat to reflux for 3 hours after adding , filtered to obtain hafnium alkoxide solution;

[0060] 2. Preparation of polyhafoxane: at 50°C, add 2 mol of acetylacetone dropwise to the hafnium alkoxide solution obtained in step 1, reflux for 5 hours after dropping, drop to 50°C, add dropwise a mixture of 1.2 mol of water and 5 mol of n-propanol Liquid, after dripping, reflux for 3h, and distill under reduced pressure to obtain polyhafoxane;

[0061] 3. Preparation of tantalum alkoxide: Disperse 1 mol of tantalum pentachloride in 40 mol of ethylene glycol diethyl ether, drop in 8 mol of n-propanol at 0°C, then drop in 5.5 mol of triethylamine, heat to reflux for 3 hours aft...

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Abstract

The invention relates to a preparation method of an HfxTa1-xC alloy precursor and an HfxTa1-xC alloy obtained through the method. The method comprises the steps that 1, hafnium tetrachloride is dispersed in a solvent, monobasic alcohol is dripped into the solvent, triethylamine is dripped into the solvent, after monobasic alcohol and triethylamine are completely dripped, reflux is conducted, filtration is conducted, and a hafnium alkoxide solution is obtained; 2, a chelating agent is dropwise added into the hafnium alkoxide solution, after the chelating agent is completely dripped, reflux is conducted, water and monobasic alcohol are added, after the water and monobasic alcohol are completed dripped, reflux is conducted, and polyhafnoxane is obtained through vacuum distillation; 3, tantalum pentachloride is dispersed in the solvent, monobasic alcohol is dripped into the solvent, triethylamine is dripped into the solvent subsequently, after monobasic alcohol and triethylamine are completely dripped, reflux is conducted, filtration is conducted, and a tantalum alkoxide solution is obtained; 4, a chelating agent is dropwise added into the hafnium alkoxide solution, after the chelating agent is completely dripped, reflux is conducted, water and monobasic alcohol are added, after the water and monobasic alcohol are completed dripped, reflux is conducted, and poly tantalum oxane is obtained through vacuum distillation; 5, polyhafnoxane, poly tantalum oxane and allyl phenol are mixed, and a hafnium tantalum alloy precursor is obtained. The prepared alloy precursor is good in solubility and stable storage life and can serve as a fiber reinforced ceramic-based composite material matrix for use.

Description

technical field [0001] The present invention relates to the preparation method of ultra-high temperature ceramic precursor and ceramics, especially relates to Hf x Ta 1-x C alloy precursor and preparation method of the alloy. Background technique [0002] Refractory cermet is a kind of material with ultra-high melting point, which has excellent ablation resistance and erosion resistance, and refractory metal carbide reacts with oxygen to form oxides covering the surface of the material in an oxidizing atmosphere, protecting the material from corrosion. It is further oxidized, so it has high temperature oxidation resistance. [0003] Typical refractory metal carbides are ZrC, HfC, TaC, etc. Among them, the melting point of TaC is 3880°C, and the strong covalent bond-metal bonding method of TaC makes it exhibit good oxidation resistance, thermal shock resistance and chemical corrosion resistance; HfC has a melting point of 3890°C and is the binary metal compound with the hi...

Claims

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Application Information

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IPC IPC(8): C04B35/56C04B35/622C08L85/00C08G79/00
CPCC04B35/5622C04B35/622C04B2235/3839C04B2235/48C04B2235/656C08G79/00C08L85/00C08L2205/025
Inventor 赵彤邱文丰鲁艳叶丽韩伟健
Owner 自贡中天胜新材料科技有限公司
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