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A kind of preparation method of chemical vapor deposition metal rhenium precursor

A technology of chemical vapor deposition and precursors, applied in chemical instruments and methods, inorganic chemistry, rhenium compounds, etc., can solve the problems of reducing yield and achieve the effect of improving purity, large contact area and high yield

Active Publication Date: 2017-07-28
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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  • A kind of preparation method of chemical vapor deposition metal rhenium precursor

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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: 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: 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; the tube furnace is started, and the temperature is raised from room temperature to 220°C at a heating rate of 5°C / min.

[0034] (3) The temperature of the oil bath is contro...

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 whole system pipeline tightly, and fix the ground joints with stainless steel chucks, 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 is ...

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Abstract

The invention discloses a preparation method of a chemical vapor deposition metal rhenium precursor, which belongs to the technical field of material preparation; the method of the invention combines ReCl 5 React in an oxidizing atmosphere, and perform high-efficiency solid-liquid-gas separation of reactants and products through sand core filter balls, effectively separate reactants, reaction products and waste gas, and simultaneously remove the reaction product ReOCl 4 and ReO 3 Cl is concentrated in the collection container heated by the oil bath. After the reaction is completed, the oxygen is turned off, the inert gas is kept in circulation, and the temperature of the tube furnace is lowered. At the same time, the oil bath is heated to make the ReO 3 Cl volatilizes and enters the rectification unit to collect and purify ReOCl 4 , to obtain high-purity precursor ReOCl for chemical vapor deposition metal rhenium 4 . The method of the present invention has high reaction efficiency, and ReOCl 4 and ReO 3 Cl is separated by rectification, which improves the product ReOCl 4 purity.

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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Patent Type & Authority Patents(China)
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