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Preparation method of Hf<x>Ta<1-x>C alloy precursor and Hf<x>Ta<1-x>C alloy prepared therefrom

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 prepared for composite materials, coatings or fibers, etc., and achieve excellent solubility, The effect of improving the purity and requiring less equipment

Active Publication Date: 2017-04-26
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

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 Hf&lt;x&gt;Ta&lt;1-x&gt;C alloy precursor and Hf&lt;x&gt;Ta&lt;1-x&gt;C alloy prepared therefrom
  • Preparation method of Hf&lt;x&gt;Ta&lt;1-x&gt;C alloy precursor and Hf&lt;x&gt;Ta&lt;1-x&gt;C alloy prepared therefrom
  • Preparation method of Hf&lt;x&gt;Ta&lt;1-x&gt;C alloy precursor and Hf&lt;x&gt;Ta&lt;1-x&gt;C alloy prepared therefrom

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 of hafnium tetrachloride in 30 mol of n-hexane, add dropwise a mixture of 4.5 mol of n-propanol and 4 mol of triethylamine at -5°C, heat and reflux for 1 hour after the addition, and filter to obtain hafnium alcohol saline solution;

[0044] 2. Preparation of tantalum alkoxide: disperse 4 mol of tantalum pentachloride in 240 mol of ethylene glycol dimethyl ether, drop in a mixture of 24 mol of isopropanol and 24 mol of triethylamine at 10°C, heat and reflux for 5 hours after the addition, and filter to obtain Tantalum alkoxide solution;

[0045] 3. Preparation of hafnium-tantalum polymer precursor by co-hydrolysis: Mix the hafnium alkoxide and tantalum alkoxide solutions obtained in steps 1 and 2, add 2.5mol acetylacetone dropwise at room temperature, reflux for 0.5h after dropping, cool down to room temperature, drop into ...

Embodiment 2

[0049] Hf in this example 0.8 Ta 0.2 The C precursor is synthesized by the following steps:

[0050] 1. Preparation of hafnium alkoxide: disperse 4 mol of hafnium tetrachloride in 200 mol of n-heptane, add dropwise a mixture of 28 mol of isopropanol and 20 mol of triethylamine at 10°C, heat under reflux for 5 hours after the addition, and filter to obtain hafnium alkoxide solution;

[0051] 2. Preparation of tantalum alkoxide: Disperse 1 mol of tantalum pentachloride in 40 mol of xylene, drop in a mixture of 9 mol of n-butanol and 5 mol of triethylamine at -5°C, heat and reflux for 1 hour after the addition, and filter to obtain tantalum alkoxide solution;

[0052] 3. Preparation of hafnium-tantalum polymer precursor by co-hydrolysis: Mix the hafnium alkoxide and tantalum alkoxide solutions obtained in steps 1 and 2, add 5 mol ethyl acetoacetate dropwise at 80°C, reflux for 5 hours after dropping, drop to 50°C, drop Add the mixed solution of 7.5mol water and 40mol n-butano...

Embodiment 3

[0056] Hf in this example 0.5 Ta 0.5 The C precursor is synthesized by the following steps:

[0057] 1. Preparation of hafnium alkoxide: disperse 1 mol of hafnium tetrachloride in 40 mol of toluene, add dropwise a mixture of 5 mol of isobutanol and 4.5 mol of triethylamine at 5°C, heat and reflux for 2 hours after the addition, and filter to obtain hafnium alkoxide solution ;

[0058] 2. Preparation of tantalum alkoxide: disperse 1mol tantalum pentachloride in 50mol ethylene glycol dimethyl ether, add dropwise a mixture of 7mol ethylene glycol monomethyl ether and 5.5mol triethylamine at 3°C, and heat to reflux after the addition 3h, filtered to obtain tantalum alkoxide solution;

[0059]3. Preparation of hafnium-tantalum polymer precursor by co-hydrolysis: Mix the hafnium alkoxide and tantalum alkoxide solutions obtained in steps 1 and 2, add 3 mol of acetylacetone dropwise at room temperature, reflux for 2 hours after dropping, at 80°C, add 2.0 mol of water dropwise Mixe...

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Abstract

The invention relates to a preparation method of an Hf<x>Ta<1-x>C alloy precursor and Hf<x>Ta<1-x>C alloy prepared therefrom. The method includes the following steps: (1) dispersing hafnium tetrachloride in a solvent and dropwise adding a mixture of monohydric alcohol and triethylamine, after the mixture is all added, performing heating reflux and filtering the solution to obtain a hafnium alkoxide solution; (2) dispersing tantalum pentachloride in a solvent and dropwise adding a mixture of monohydric alcohol and triethylamine, after the mixture is all added, performing heating reflux and filtering the solution to obtain a tantalum alkoxide solution; (3) mixing the hafnium alkoxide solution and the tantalum alkoxide solution, dropwise adding a chelating agent, and then performing heating reflux, dropwise adding a mixture of water and monohydric alcohol, after the mixture is all added, performing reflux and pressure reduced distillation to obtain a hafnium and tantalum polymer precursor; and (4) mixing the hafnium and tantalum polymer precursor with allyl phenolic aldehyde to prepare the Hf-Ta alloy precursor. The Hf<x>Ta<1-x>C alloy precursor has good solubility and long stable storage time and can be used as a fiber-reinforced ceramic based composite material substrate.

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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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/56C04B35/622C08L85/00C08G79/00
CPCC04B35/5607C04B35/5622C04B35/622C04B2235/3839C04B2235/48C04B2235/656C08G79/00C08L85/00C08L2205/025
Inventor 赵彤邱文丰鲁艳叶丽韩伟健
Owner INST OF CHEM CHINESE ACAD OF SCI
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