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Manufacturing method for pure tungsten or molybdenum thin-wall device

A device and thin-wall technology, which is applied in the field of preparation of pure tungsten or molybdenum thin-wall devices, can solve the problems of expensive tungsten fluoride, limited practical application, equipment corrosion, etc., and achieves short processing flow, dense film layer, and deposition speed fast effect

Inactive Publication Date: 2012-07-11
CHINA IRON & STEEL RES INST GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method of preparing metal tungsten products by reactive vapor deposition of tungsten hexafluoride and hydrogen has high deposition purity, simple equipment and fast deposition rate, but due to the raw materials (WF 6 ) and the waste gas (HF) produced are toxic, and the equipment is corroded more seriously, and tungsten fluoride is expensive, which limits its practical application

Method used

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  • Manufacturing method for pure tungsten or molybdenum thin-wall device
  • Manufacturing method for pure tungsten or molybdenum thin-wall device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Use copper material to process pipe fittings with an outer diameter of 50 mm, a wall thickness of 1 mm, and a height of 50 mm. The surface roughness Ra is 0.8, and then the oil on the surface is cleaned and dried. Put the copper pipe fitting template into the vapor deposition chamber, and evacuate the system to a vacuum of 0.5Pa, then preheat the copper pipe fitting to 400°C. Use tungsten hexacarbonyl as the organic source of reaction (gasified at 80°C), 5N hydrogen as the diluent gas, keep the volume flow ratio of tungsten hexacarbonyl and hydrogen at 1:10, and pass the mixed gas into the deposition chamber. Keeping the deposition chamber pressure at 500Pa and the deposition temperature at 400°C, tungsten hexacarbonyl was subjected to thermal dissociation vapor deposition on the red copper template for 4 hours, and then annealed at 900°C for 10 minutes. After the deposition is completed, close the valve of the organic source, and continue to feed hydrogen to keep the d...

Embodiment 2

[0019] Process a crucible with an outer diameter of 5mm, a wall thickness of 1mm, and a height of 50mm with red copper material, and its surface roughness Ra is 1.6, and then the oil stain on the surface is cleaned and dried. Put the copper crucible template into the vapor deposition chamber, and evacuate the system to a vacuum of 2Pa, then preheat the copper crucible to 280°C. Use tungsten hexacarbonyl as the organic source of reaction (gasified at 90°C), 5N hydrogen as the diluent gas, keep the volume flow ratio of tungsten hexacarbonyl and hydrogen at 1:100, and pass the mixed gas into the deposition chamber. The thermal dissociation vapor deposition of tungsten hexacarbonyl on the red copper template was carried out under the condition of maintaining the deposition chamber pressure of 5000Pa and the deposition temperature of 280°C, annealing at 800°C for 20 minutes every 4 hours of deposition, and a total of 182 hours of vapor deposition. After the deposition is completed,...

Embodiment 3

[0021] Use copper material to process pipe fittings with an outer diameter of 5 mm, a wall thickness of 1 mm, and a height of 50 mm. The surface roughness Ra is 3.2, and then the oil on the surface is cleaned and dried. Put the copper pipe fitting template into the vapor deposition chamber, and evacuate the system to a vacuum of 5Pa, then preheat the copper pipe fitting to 360°C. Use tungsten hexacarbonyl as the reactive organic source (gasified at 90°C), 5N nitrogen as the diluent gas, keep the volume flow ratio of tungsten hexacarbonyl and nitrogen at 1:50, and pass the mixed gas into the deposition chamber. Keep the deposition chamber pressure at 10,000 Pa and the deposition temperature at 360°C for thermal dissociation vapor deposition of tungsten hexacarbonyl on the copper template, annealing at 700°C for 30 minutes every 2 hours of deposition, and a total of 142 hours of vapor deposition. After the deposition is completed, close the valve of the organic source, and conti...

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Abstract

The invention discloses a manufacturing method for a pure tungsten or molybdenum thin-wall device, belonging to the technical field of powder metallurgy. The manufacturing method comprises the following process steps of: manufacturing a template of the required device by using a red copper material and keeping the surface clean and dry, wherein the surface roughness Ra of the template is lower than 6.3; placing the template into a vapor deposition chamber; with tungsten hexacarbonyl or molybdenum hexacarbonyl as an reactive organic source and with high-purity hydrogen gas or nitrogen gas as diluent gas, carrying out thermal decomposition vapor deposition on the template under the conditions that the pressure of the vapor deposition chamber is 500-10000Pa and the deposition temperature is 280-420DEG C and carrying out annealing once every 2-4 hours in the deposition process according to the requirement of the deposited wall thickness; after the deposition is finished, closing an organic source valve and continuously introducing the dilute gas and keeping the device cooled to the room temperature; and removing a red copper template matrix from the device of which the template surface is deposited with tungsten or molybdenum by adopting a nitric acid corrosion method to obtain the pure tungsten or molybdenum thin-wall device with the wall thickness being 0.1-3mm. The manufacturing method has the advantages of low deposition temperature, high deposition speed, high purity of deposition film, dense film layer, favorable smoothness of film surface, short process flow and no pollution or corrosion.

Description

technical field [0001] The invention belongs to the technical field of powder metallurgy, in particular to a preparation method of a pure tungsten or molybdenum thin-walled device. technical background [0002] Tungsten and molybdenum are the two most important elements in refractory metals. Because of their high melting points, hydrometallurgy is generally used to make oxides, and then reduced with hydrogen or other reducing agents to obtain metal powders, which are then made into various metal powders by powder metallurgy. Refractory metal processing materials and products. It is difficult to produce special-shaped thin-walled dense metal and its compound devices (such as curved surface and internal thread products) with more complex shapes by ordinary powder metallurgy and mechanical methods, which also greatly limits its application in aviation, aerospace and nuclear industries. applications in the industry. [0003] Chemical vapor deposition (CVD) is a process method ...

Claims

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Application Information

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IPC IPC(8): C23C16/16C23C16/01C23C16/44
Inventor 李一柳学全周武平李金普李楠霍静熊宁石文
Owner CHINA IRON & STEEL RES INST GRP
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