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Method and system for preparing disilane by reacting polymetallic silicide and ammonium chloride

A technology of multiple metals and silicides, applied in silicon compounds, chemical instruments and methods, non-metallic elements, etc., can solve the problems of high energy consumption, waste of resources, and high production costs for raw material synthesis, so as to improve synthesis efficiency and ensure uniformity , the effect of improving the feasibility

Active Publication Date: 2022-02-08
烟台万华电子材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing disilane preparation methods are mainly due to factors such as low yield and many types of reaction by-products, which lead to high production costs, or due to the limitation of scarcity of raw materials, large-scale production cannot be achieved.
Among them, most of the products obtained by the reaction of magnesium silicide and ammonium chloride in liquid ammonia are monosilane, and about 3-5% of disilane can only be used as a by-product due to the small amount, and the cost of recovering disilane for purification is high , if the by-product of disilane is ignored, it will cause waste of resources
At present, the yield of disilane has been improved by adding additives and adjusting the reaction temperature, but there are still phenomena such as high energy consumption for raw material synthesis and difficulty in adjusting the ratio of monosilane to disilane production, which limits its use as a large-scale production of disilane. possibility

Method used

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  • Method and system for preparing disilane by reacting polymetallic silicide and ammonium chloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Send silicon powder, magnesium powder and lithium powder into the fusion coating machine for pretreatment. The pretreatment process conditions are: the raw materials enter the mixer, the mixing time is 1 hour, and the speed is 40r / min; then transfer to the vibrator, The rotation speed is 350r / min, the temperature is controlled not to exceed 60°C, and the treatment time is 3h.

[0056] The pretreated material is sent to a silicide synthesis device, and synthesized at a synthesis temperature of 500° C. to obtain a multi-element metal silicide. After testing, the proportion of element components in the obtained multi-component metal silicide is: Si 33.3%, Mg 50%, Li 16.7%, the percentage is mole percentage, and the obtained multi-component metal silicide is Mg 1.5 Li 0.5 Si.

[0057] Then put the multi-metal silicide into the reactor, and input liquid ammonia into the reactor to disperse the multi-metal silicide to obtain a suspension, and input the ammonium chloride sol...

Embodiment 2

[0062] Send silicon powder, magnesium powder and lithium powder into the fusion coating machine for pretreatment. The pretreatment process conditions are: the raw materials enter the mixer, the mixing time is 1 hour, and the speed is 40r / min; then transfer to the vibrator, The rotation speed is 350r / min, the temperature is controlled not to exceed 60°C, and the treatment time is 4h.

[0063] The pretreated material is sent to a silicide synthesis device, and synthesized at a synthesis temperature of 475° C. to obtain a multi-element metal silicide. After testing, the proportion of element components in the obtained multi-component metal silicide is: Si 33.3%, Mg 50%, Li 16.7%, the percentage is mole percentage, and the obtained multi-component metal silicide is Mg 1.5 Li 0.5 Si.

[0064] Then put the multi-metal silicide into the reactor, and input liquid ammonia into the reactor to disperse the multi-metal silicide to obtain a suspension, and input the ammonium chloride sol...

Embodiment 3

[0069] Send silicon powder, magnesium powder and lithium powder into the fusion coating machine for pretreatment. The pretreatment process conditions are: the raw materials enter the mixer, the mixing time is 1 hour, and the speed is 40r / min; then transfer to the vibrator, The rotation speed is 350r / min, the temperature is controlled not to exceed 60°C, and the treatment time is 5h.

[0070] The pretreated material is sent to a silicide synthesis device, and synthesized at a synthesis temperature of 525° C. to obtain a multi-element metal silicide. After testing, the proportion of element components in the obtained multi-component metal silicide is: Si 33.3%, Mg 50%, Li 16.7%, the percentage is mole percentage, and the obtained multi-component metal silicide is Mg 1.5 Li 0.5 Si.

[0071] Then put the multi-metal silicide into the reactor, and input liquid ammonia into the reactor to disperse the multi-metal silicide to obtain a suspension, and input the ammonium chloride sol...

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Abstract

The invention provides a method and system for preparing disilane by reacting multi-metal silicide and ammonium chloride. The method provided by the invention can solve the shortcomings of the traditional magnesium silicide method, can obtain disilane with high yield, and can be applied to large-scale production of disilane industrialized production. The invention provides a method for preparing disilane by reacting a multi-element metal silicide with ammonium chloride, comprising the following steps: 1) passing the raw materials used for synthesizing the multi-element metal silicide into a fusion coating machine for pretreatment, after pretreatment The obtained material is sent to the silicide synthesis device to react to generate the multi-element metal silicide; 2) adding the multi-element metal silicide and ammonium chloride solution into the reactor to react in the presence of liquid ammonia to obtain the product material; 3) adding The product material is sent to the impurity separation device to remove the hydrogen and residual ammonia after the ammonia gas is removed through the condensation reflux device, and then the product material is sent to the silane separation device to separate and obtain crude monosilane and disilane.

Description

technical field [0001] The invention relates to the technical field of disilane production, and further relates to a technology for preparing disilane gas with high yield by chemical reaction in an anhydrous environment, in particular to a method and a device system for preparing disilane by reacting multi-element metal silicide and ammonium chloride. Background technique [0002] Disilane is a compound of silicon and hydrogen, and it is an important silicon source gas in the advanced semiconductor manufacturing process. Compared with monosilane, disilane has the advantages of fast deposition rate, low deposition temperature, and high uniformity of deposited film. With the development of semiconductor manufacturing process and market growth, it will become an indispensable electronic special gas. However, the existing disilane preparation methods are mainly due to factors such as low yield and many types of reaction by-products, which lead to high production costs, or due to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/04
CPCC01B33/04C01B33/043
Inventor 王耀西陈刚军
Owner 烟台万华电子材料有限公司