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Method for preparing precursor for chemical vapor deposition of metallic rhenium

A chemical vapor deposition and precursor technology, used in chemical instruments and methods, inorganic chemistry, rhenium compounds, etc., can solve problems such as reducing yield, and achieve the effects of improving purity, simple control of process parameters, and improving yield

Active Publication Date: 2016-01-20
海朴精密材料(苏州)有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above method is used to prepare ReOCl before adopting 4 , ReOCl 4 Will be with ReO 3 The reaction produces ReCl 3 and ReO 3 Cl, which reduces the yield

Method used

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  • Method for preparing precursor for chemical vapor deposition of metallic rhenium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation method of the precursor for chemical vapor deposition metal rhenium described in this embodiment specifically includes the following steps:

[0027] (1) Weigh 100 powdered ReCl 5 (purity ≥ 99%) placed in the sand core filter ball, spread evenly.

[0028] (2) Put the sand core filter ball in the tube furnace, connect the whole system pipeline tightly, and fix the ground joints with stainless steel chucks to check the air tightness; start the valve to feed nitrogen (≥99.9%), and carry out Cleaning process, nitrogen pressure: 0.1MPa, flow rate: 0.1L / min, clean the entire pipeline for 50 minutes; start the valve to feed high-purity oxygen (≥99.9%), oxygen pressure: 0.1MPa, flow rate: 0.05L / min, inert The flow ratio of gas to oxygen is controlled at 2:1, and the gas is supplied stably for 2 minutes; the tube furnace is started, and the temperature is raised from room temperature to 120°C at a temperature increase rate of 1°C / min.

[0029] (3) The temperature ...

Embodiment 2

[0031] The preparation method of the precursor for chemical vapor deposition metal rhenium described in this embodiment specifically includes the following steps:

[0032] (1) Weigh 200 powdered ReCl 5 (purity ≥ 99%) placed in the sand core filter ball, spread evenly.

[0033] (2) Put the sand core filter ball in the tube furnace, connect the entire system pipeline tightly, and fix the ground joints with stainless steel chucks to check the air tightness; start the valve to feed argon (≥99.9%), Carry out the cleaning process, argon pressure: 0.6MPa, flow rate: 0.5L / min, clean the entire pipeline for 20 minutes; start the valve to feed high-purity oxygen (≥99.9%), oxygen pressure: 0.6MPa, flow rate: 0.1L / min , the flow ratio of inert gas to oxygen is controlled at 5:1, and the gas is supplied stably for 10 minutes; start the tube furnace, and heat up from room temperature to 220°C at a heating rate of 5°C / min.

[0034] (3) The temperature of the oil bath is controlled at 100°C...

Embodiment 3

[0036] The preparation method of the precursor for chemical vapor deposition metal rhenium described in this embodiment specifically includes the following steps:

[0037] (1) Weigh 100 powdered ReCl 5 (purity ≥ 99%) placed in the sand core filter ball, spread evenly.

[0038] (2) Put the sand core filter ball in the tube furnace, connect the entire system pipeline tightly, and fix the ground joints with stainless steel chucks to check the air tightness; start the valve to feed helium (≥99.9%), Carry out the cleaning process, helium pressure: 0.3MPa, flow rate: 2L / min, clean the entire pipeline for 20 minutes; start the valve to feed high-purity oxygen (≥99.9%), oxygen pressure: 0.3MPa, flow rate: 0.5L / min, The flow ratio of inert gas to oxygen is controlled at 4:1, and the gas is supplied stably for 10 minutes; the tube furnace is started, and the temperature is raised from room temperature to 180°C at a heating rate of 3°C / min.

[0039] (3) The temperature of the oil bath ...

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Abstract

The invention discloses a method for preparing a precursor for chemical vapor deposition of metallic rhenium and belongs to the technical field of material preparation. According to the method, ReCl5 is made to react in an oxidizing atmosphere, efficient solid-liquid-gas separation is conducted on reactants and products with a sand core filter bulb so that reactants, reaction products and waste gas can be effectively separated, the reaction products ReOCl4 and ReO3Cl are gathered in a collection vessel heated by an oil bath pan at the same time, oxygen introduction is stopped after reaction ends, circulation of inert gases is maintained, a tube furnace is cooled, the oil bath pan is heated at the same time to enable ReO3Cl to volatilize to enter a rectification unit to be collected, ReOCl4 is purified, and then the high-purity precursor ReOCl4 for chemical vapor deposition of metallic rhenium is obtained. By the adoption of the method, reaction efficiency is high, ReOCl4 and ReO3Cl are separated through rectification, and the purity of the product ReOCl4 is improved.

Description

technical field [0001] The invention discloses a method for preparing a precursor of metal rhenium for chemical vapor deposition, which belongs to the technical field of material preparation and is applied to rhenium-iridium nozzles for aviation. Background technique [0002] Metal rhenium has a high melting point and has excellent high-temperature mechanics, thermal fatigue resistance, wear resistance, corrosion resistance, and catalysis. It is widely used in national defense, aerospace, electronics, and petrochemical industries, such as: thermionic emission materials, high-temperature engine thrust chamber nozzle, etc. However, due to the high melting point of metal rhenium, it is generally processed by powder metallurgy; for metal rhenium tubes used in aviation, due to the harsh working conditions, the material prepared by powder metallurgy has many internal defects, so it is easy to generate cracks and fail, and the effective working time is reduced. . Chemical vapor d...

Claims

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Application Information

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IPC IPC(8): C01G47/00
Inventor 刘科学于晓东王玉天谭成文胡劲王开军张维钧
Owner 海朴精密材料(苏州)有限责任公司
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