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A kind of preparation method and device of tungsten pentachloride

A technology of tungsten pentachloride and tungsten tetrachloride, applied in tungsten halide and other directions, can solve problems such as inability to transport, achieve simple daily operation and maintenance, facilitate automatic control, and ensure the effect of air tightness

Active Publication Date: 2021-03-02
湖南省华京粉体材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production process of tungsten pentachloride requires extremely low oxygen and water vapor concentrations to ensure the purity of the product; at the same time, the raw materials for the production of tungsten pentachloride are solid at room temperature and cannot be directly transported through pipelines
How to realize the continuous and efficient preparation of tungsten pentachloride while ensuring the airtightness of the production system is the prerequisite for obtaining electronic grade high-purity tungsten pentachloride. There is no relevant process technology report yet

Method used

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  • A kind of preparation method and device of tungsten pentachloride

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Experimental program
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Effect test

Embodiment 1

[0026] see figure 1 , put 5kg of tungsten tetrachloride into the raw material container 1, the raw material container 1 is connected with the vacuum transition chamber, repeat vacuuming and flushing with nitrogen three times, then open the discharge valve, and open the inert carrier gas at 3L / min at the same time, so that the tungsten tetrachloride The particles fall into the screw feeder 3 under the dual action of gravity and air flow, and are pushed to the heating and sublimation zone by the screw. The heating and sublimation temperature of the material is 450°C, and the obtained tungsten tetrachloride vapor is transported into the mixer 6. Adjust the intake flow rate of chlorine gas to 1.3L / min through the intake valve, so that the preheated chlorine gas and tungsten tetrachloride vapor are fully mixed in the Venturi tube. The mixed gas fully reacts in the labyrinth tube reactor 7, the reaction temperature is 300°C, and the generated steam is collected through condensation....

Embodiment 2

[0030] see figure 1 , put 10kg of tungsten dichloride and tungsten tetrachloride mixture into the raw material container, the raw material container 1 is connected to the vacuum transition chamber, repeat vacuuming and flushing with nitrogen three times, then open the discharge valve, and open the inert carrier gas at 5L / min at the same time, The tungsten tetrachloride particles fall into the screw feeder 3 under the double action of gravity and air flow, and are pushed to the heating and sublimation zone by the screw. Adjust the intake flow rate of chlorine gas to 3L / min through the intake valve, so that the preheated chlorine gas and tungsten tetrachloride vapor are fully mixed in the Venturi tube. The mixed gas fully reacts in the labyrinth tube reactor 7, the reaction temperature is controlled at 500°C, and the generated steam is collected through condensation. Table 2 is the chemical analysis results of the product.

[0031] Table 2 implementation case 2 gained tungsten...

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Abstract

The invention discloses a preparation method of tungsten pentachloride. The preparation method comprises the following steps: feeding tungsten tetrachloride serving as a raw material through a vacuumtransition cavity, conveying the material through a magnetically-driven helical feeder, heating and gasifying the material at the tail end of the feeder, and transporting the material to a Venturi tubular mixer through inert gas flow for efficient mixing with reaction gas; introducing the mixed gas into a reaction chamber, and making the raw material react with the gas at the temperature of 200 to800 DEG C to obtain a tungsten pentachloride crude product. The preparation method is simple in equipment, and is easy to operate. The equipment has high air tightness, and continuous production of high-quality tungsten pentachloride can be realized. An air-tight magnetically-driven helical feeding manner is adopted, so that the airtightness of the system is ensured, and industrial continuous production can be realized. The preparation method has the advantages of simple process flow, low operation difficulty, easiness in daily running and maintenance, and contribution to automatic control.

Description

technical field [0001] The invention relates to a method and a device for preparing tungsten pentachloride through gas phase reaction, belonging to the field of rare material manufacture. Background technique [0002] The chemical vapor deposition CVD process of tungsten is generally used in the electronics industry to form a metal tungsten layer on the surface of the wafer, and to make connecting wires in large-scale integrated circuits or ultra-large-scale integrated circuits. The traditional CVD process uses a large amount of tungsten hexafluoride as a raw material, and after the gas phase deposition chamber is reduced with hydrogen, the tungsten is deposited on the wafer surface, and a large amount of HF gas is generated at the same time. With the advancement of integrated circuit manufacturing technology, the chip manufacturing process has reached the 10nm level, and there is a trend of further development to 7nm and lower 5nm. Because HF is highly corrosive to silicon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/04
CPCC01G41/04
Inventor 彭宁李绍兵薛海涛田吉英李焌源沈季芳吴尔京李春芳
Owner 湖南省华京粉体材料有限公司
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