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Preparation method of crucible with tungsten coating

A crucible and coating technology, which is applied in the direction of coating, metal material coating process, gaseous chemical plating, etc., to reduce the risk of heterogeneous nucleation, improve service life, and good bonding performance

Active Publication Date: 2014-12-17
XIAMEN HONGLU TUNGSTEN MOLYBDENUM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the defects of existing powder metallurgy tungsten crucible and molybdenum crucible, to provide a kind of tungsten-containing coating crucible and its preparation method

Method used

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  • Preparation method of crucible with tungsten coating
  • Preparation method of crucible with tungsten coating
  • Preparation method of crucible with tungsten coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] This example is used to prepare the tungsten substrate crucible coated with pure tungsten coating, see figure 1 , the implementation steps are as follows:

[0044] (1) According to the required size, the pure tungsten crucible of the required cylindrical shape is processed and prepared by powder sintering method. The size of the crucible is Φ100mm in outer diameter and 100mm in height.

[0045] (2) Sandblast the surface of the prepared tungsten crucible with 100-mesh alumina for more than ten minutes, clean it with ultra-pure water ultrasonic waves, and then use sodium hydroxide (5mol / L) and deionized water to make lye to the crucible Surface wash, then dry.

[0046] (3) Put the processed substrate into the chemical vapor deposition reaction chamber, and evacuate to 1.0×10 -1 At about Pa, inject nitrogen gas to replenish the pressure of the deposition chamber to normal pressure, repeat three times, then inject hydrogen gas, and raise the temperature under a hydrogen p...

Embodiment 2

[0051] This example is used to prepare the molybdenum alloy substrate crucible coated with pure tungsten coating, see figure 2 , the implementation steps are as follows:

[0052] (1) The TZM molybdenum alloy crucible is prepared by powder metallurgy process, the bottom size of the crucible is 80×80mm, and the height is 80mm.

[0053] (2) Grind the inner wall surface of the processed crucible base material with about 1000# sandpaper, clean it with ultra-pure water ultrasonic waves, and then use sodium hydroxide (1mol / L) and deionized water to make lye to surface the crucible Wash then tumble dry.

[0054] (3) Put the above-mentioned cleaned and dried crucible substrate into the CVD reaction chamber, and evacuate to 1.0×10 -1 At about Pa, inject nitrogen gas to replenish the pressure of the deposition chamber to normal pressure, repeat three times, then inject hydrogen gas, and raise the temperature under a hydrogen protective atmosphere. After the temperature of the inner w...

Embodiment 3

[0059] This example is used to prepare a processed molybdenum crucible coated with a pure tungsten coating, see image 3 , the implementation steps are as follows:

[0060] (1) The rolled molybdenum plate is processed into a molybdenum crucible base material with a diameter of Φ450mm, a height of 600mm and a wall thickness of 1mm by hot spinning process.

[0061] (2) Grind the inner wall surface of the processed molybdenum crucible base material with about 3000# sandpaper, use ultrapure water to clean it ultrasonically, and then use sodium hydroxide (1mol / L) and deionized water to make lye to clean the crucible Surface wash, then tumble dry.

[0062] (3) Put the above-mentioned cleaned and dried molybdenum crucible into the chemical vapor deposition reaction chamber, and evacuate to 1.0×10 -1 At about Pa, inject nitrogen gas to replenish the pressure of the deposition chamber to normal pressure, repeat three times, then inject hydrogen gas, and raise the temperature under a ...

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Abstract

The invention discloses a preparation method of a crucible with a tungsten coating. The preparation method comprises the following steps: (1) a needed pure tungsten, pure molybdenum or molybdenum alloy crucible base material is obtained through a specific processing technology according to a needed size; (2) a certain degree of surface roughening treatment is performed for the obtained crucible base material; and then, the surface is cleaned to remove an oxide layer; and (3) tungsten hexafluoride serves as a raw material, hydrogen serves as reducing gas, and the chemical vapor deposition (CVD) is performed for the surface of the crucible base material under the condition of the base material temperature of 350-600 DEG C to form a tungsten coating layer with the thickness of 0.01-3 mm so as to obtain a crucible product coated with the tungsten coating layer. The CVD tungsten coating layer with high purity and high compactness has excellent metal or nonmetallic solution corrosion resistance, so that the protecting effect on the crucible basal body is achieved, and the service life and the performance of the crucible under such high-temperature environments as metal or nonmetal smelting and crystal growth are prolonged and improved.

Description

technical field [0001] The invention belongs to the technical field of metallurgical materials, and in particular relates to a tungsten-coated crucible and a preparation method thereof. Background technique [0002] Most of the crucibles used in the fields involving rare earth smelting, vacuum evaporation and sapphire crystal growth are made of tungsten and molybdenum. The theoretical density of tungsten is 19.3g / cm 3 , with a melting point of 3410°C. The theoretical density of molybdenum is 10.2g / cm 3 , melting point 2610°C. The currently used tungsten, molybdenum and molybdenum alloy crucibles are mostly obtained by powder metallurgy and pressure processing. [0003] Due to the high hardness and high brittleness of tungsten materials, it is difficult to process them by general casting and forging processes. The tungsten crucibles currently used by powder metallurgy can reach a maximum density of 18.9-19.0g / cm 3 , the highest purity can be about 5N level. Since the si...

Claims

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Application Information

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IPC IPC(8): C23C16/56C23C16/14C23C16/02
Inventor 颜彬游宋久鹏吕延伟刘俊勇于洋
Owner XIAMEN HONGLU TUNGSTEN MOLYBDENUM IND CO LTD
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