WO2017193881A1 - Procédé de préparation de disilane - Google Patents

Procédé de préparation de disilane Download PDF

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Publication number
WO2017193881A1
WO2017193881A1 PCT/CN2017/083418 CN2017083418W WO2017193881A1 WO 2017193881 A1 WO2017193881 A1 WO 2017193881A1 CN 2017083418 W CN2017083418 W CN 2017083418W WO 2017193881 A1 WO2017193881 A1 WO 2017193881A1
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WO
WIPO (PCT)
Prior art keywords
disilane
catalyst
magnesium silicide
ammonium chloride
reaction
Prior art date
Application number
PCT/CN2017/083418
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English (en)
Chinese (zh)
Inventor
黄晓东
Original Assignee
浙江迅鼎半导体材料科技有限公司
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Publication date
Application filed by 浙江迅鼎半导体材料科技有限公司 filed Critical 浙江迅鼎半导体材料科技有限公司
Publication of WO2017193881A1 publication Critical patent/WO2017193881A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/04—Hydrides of silicon

Definitions

  • the invention belongs to the technical field of gas production, and particularly relates to a method for producing monosilane (SiH 4 ), disilane (Si 2 H 6 ), trisilane (Si 3 H 8 ), etc., and particularly to a method for producing disilane.
  • silicon is used to isolate the conductive layers in electronic precision components. Since components, such as chips, have repeatedly pursued precision, and the specification design has become more and more fine, from micron to nanometer, the silicon isolation layer has not been formed by mechanical cutting, but must be formed by vapor phase lamination, so silanes The use of the necessary materials.
  • Disilane is a promising precursor to silicon films. Compared with monosilane, it has the advantages of high deposition rate, low temperature requirement and high film uniformity. It is one of the most attractive specialty gases in the semiconductor industry.
  • the method has high production cost due to low yield, many by-products and expensive equipment.
  • the second method is the trichlorosilane purification method (commonly known as the UCC method).
  • the process of this method firstly reacts silicon powder with hydrogen chloride (commonly known as hydrochloric acid) to form trichlorosilane (Si+3HCl ⁇ HSiCl 3 +H 2 ).
  • trichlorosilane is reacted with hydrogen to form dichlorosilane and hydrogen chloride (HSiCl 3 + H 2 ⁇ H 2 SiCl 2 + HCl) by combining hydrogen with chlorine. Further, by reacting dichlorosilane with hydrogen, hydrogen and chlorine are combined to form monochlorosilane and hydrogen chloride (H 2 SiCl 2 + H 2 ⁇ H 3 SiCl + HCl). Then, the monochlorosilane is further reacted with hydrogen, that is, hydrogen and chlorine are combined to form silicon methane and hydrogen chloride (H 3 SiCl + H 2 ⁇ SiH 4 + HCl). This method can generate silicon methane. However, products such as silane, silane, and the like cannot be produced by this method.
  • a method for producing disilane which comprises reacting magnesium silicide with ammonium chloride as a raw material, and generating disilane gas in the presence of liquid ammonia and a catalyst, the reaction temperature is -10 ° C to 50 ° C, and the reaction pressure is 0.2-1 MPa.
  • the molar ratio of magnesium silicide to ammonium chloride is 1:2-5, and the catalyst is a complex of zinc.
  • reaction pressure is 0.25 to 0.55 MPa.
  • the molar ratio of the magnesium silicide to the ammonium chloride is 1:3.
  • reaction is carried out in a 3-10 M 3 reactor, preferably a 8.4 M 3 reactor.
  • the reactor is equipped with a magnetic stirrer to prevent material leakage.
  • the catalyst is one or more of C 54 H 45 P 3 ZnX 2 , C 68 H 56 Fe 2 P 4 ZnY 2 , C 52 H 48 P 4 ZnCl 2 , C 54 H 52 P 4 ZnCl 2 Where X is F, Cl, Br or I, and Y is Br or I.
  • the disilane gas is stored in a liquid phase in a storage tank by low-temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
  • disilane is the main product of the production process, thereby solving the problem of by-products of large-scale production of disilane, greatly improving the production efficiency of producing high-purity disilane, low energy consumption, and low production cost.
  • the embodiment of the present invention adopts the following manufacturing method: reacting magnesium silicide with ammonium chloride as a raw material, and generating disilane gas in the presence of liquid ammonia and a catalyst, the reaction temperature is -10 ° C to 50 ° C, and the reaction pressure is 0.2- 1 MPa, the molar ratio of the magnesium silicide to the ammonium chloride is 1:2-5, and the catalyst is a complex of zinc.
  • Examples 1-10 of the present invention produced disilane in a yield having industrial applicability.
  • the synthesis reaction is carried out in the presence of liquid ammonia, which means that liquid ammonia is introduced into the reaction vessel at least during the feed, while allowing it to occur partially during the reaction or All vaporization.
  • Disilane is produced in accordance with the above method.
  • the reaction temperature is -10 ° C
  • the reaction pressure is 0.2 MPa
  • the molar ratio of the magnesium silicide to the ammonium chloride is 1:2
  • the catalyst is C 54 H 52 P 4 ZnCl 2
  • the reaction is at 3 M 3
  • the reaction kettle was carried out.
  • Example 1 was repeated except that the reaction temperature was 50 ° C, the reaction pressure was 1 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:5, and the catalyst was C 54 H 45 P 3 ZnX 2 .
  • the reaction was carried out in a 10 M 3 reactor equipped with a magnetic stirrer.
  • Example 1 was repeated except that the reaction temperature was 20 ° C, the reaction pressure was 0.6 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:3.5, and the catalyst was C 52 H 48 P 4 ZnCl 2 The reaction was carried out in a 6.5 M 3 reactor equipped with a magnetic stirrer.
  • Example 1 was repeated except that the reaction pressure was 0.25 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:3, and the catalyst was C 68 H 56 Fe 2 P 4 ZnY 2 . This was carried out in a 8.4 M 3 reactor equipped with a magnetic stirrer.
  • Example 4 was repeated except that the reaction pressure was 0.55 MPa and the catalyst was a mixture of C 54 H 45 P 3 ZnX 2 and C 68 H 56 Fe 2 P 4 ZnY 2 .
  • the disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
  • Example 5 was repeated except that the reaction pressure was 0.4 MPa and the catalyst was a mixture of C 54 H 45 P 3 ZnX 2 and C 52 H 48 P 4 ZnCl 2 , and the pressure in the tank jacket was 10Pa.
  • Example 2 was repeated except that the molar ratio of magnesium silicide to ammonium chloride was 1:3, the catalyst was C 68 H 56 Fe 2 P 4 ZnY 2 , and the reaction was at 8.4 M 3
  • the kettle was placed in a kettle equipped with a magnetic stirrer.
  • the disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
  • Example 3 was repeated, except that the magnesium silicide and ammonium chloride molar ratio of 1: 3, the catalyst is C 68 H 56 Fe 2 P 4 ZnY 2 and C 52 H 48 P 4 ZnCl 2 is The mixture was reacted in a 8.4 M 3 reactor equipped with a magnetic stirrer.
  • the disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
  • the pressure inside the tank jacket is 6 Pa.
  • Example 4 was repeated except that the reaction temperature was 20 ° C and the reaction pressure was 0.6 MPa, and the catalyst was a mixture of C 54 H 45 P 3 ZnX 2 and C 52 H 48 P 4 ZnCl 2 , the disilane
  • the gas is stored in a liquid phase in a storage tank by low temperature decompression, which is a jacketed structure with a -30 ° C glycol cooling medium in the jacket.
  • Example 5 was repeated except that the reaction temperature was -10 ° C, the reaction pressure was 0.3 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:4, and the catalyst was C 54 H 52 P 4 ZnCl. 2. The reaction was carried out in a 8.4 M 3 reactor with a pressure of 2 Pa in the jacket jacket.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne un procédé de fabrication de disilane. On fait réagir du siliciure de magnésium et du chlorure d'ammoniac en tant que matières premières en présence d'ammoniac liquide et d'un catalyseur de manière à produire un gaz de type disilane, la température de réaction étant de -10°C à 50°C, la pression de réaction étant de 0,2-1 MPa, le rapport molaire du siliciure de magnésium au chlorure d'ammoniac étant de 1:2-5 et le catalyseur étant un complexe du zinc. Dans le procédé, le disilane est un produit principal du procédé de production ; ainsi, le problème de sous-produits dans la production à grande échelle du disilane peut être résolu, l'efficacité de production de disilane de haute pureté est considérablement améliorée, la consommation d'énergie est faible et le coût de production est réduit.
PCT/CN2017/083418 2016-05-09 2017-05-08 Procédé de préparation de disilane WO2017193881A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201610299473.5A CN105800616B (zh) 2016-05-09 2016-05-09 一种乙硅烷的制造方法
CN201610299473.5 2016-05-09

Publications (1)

Publication Number Publication Date
WO2017193881A1 true WO2017193881A1 (fr) 2017-11-16

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PCT/CN2017/083418 WO2017193881A1 (fr) 2016-05-09 2017-05-08 Procédé de préparation de disilane

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CN (1) CN105800616B (fr)
WO (1) WO2017193881A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105800616B (zh) * 2016-05-09 2017-03-22 浙江迅鼎半导体材料科技有限公司 一种乙硅烷的制造方法
CN106185949B (zh) * 2016-08-02 2018-03-09 浙江迅鼎半导体材料科技有限公司 一种乙硅烷的制造方法
CN112661161A (zh) * 2020-12-28 2021-04-16 烟台万华电子材料有限公司 一种连续生产高阶硅烷的方法
CN113083166A (zh) * 2021-03-16 2021-07-09 洛阳中硅高科技有限公司 乙硅烷制备设备和制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090241730A1 (en) * 2008-03-31 2009-10-01 Et-Energy Corp. Chemical process for generating energy
CN102502653A (zh) * 2011-12-14 2012-06-20 浙江赛林硅业有限公司 一种生产高纯乙硅烷的系统及其方法
CN104724711A (zh) * 2015-02-02 2015-06-24 上海万寅安全环保科技有限公司 一种硅烷类产品的制造方法
CN105800616A (zh) * 2016-05-09 2016-07-27 浙江迅鼎半导体材料科技有限公司 一种乙硅烷的制造方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102205968A (zh) * 2010-03-31 2011-10-05 天津市泰亨气体有限公司 硅化镁制备硅烷方法工艺技术

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090241730A1 (en) * 2008-03-31 2009-10-01 Et-Energy Corp. Chemical process for generating energy
CN102502653A (zh) * 2011-12-14 2012-06-20 浙江赛林硅业有限公司 一种生产高纯乙硅烷的系统及其方法
CN104724711A (zh) * 2015-02-02 2015-06-24 上海万寅安全环保科技有限公司 一种硅烷类产品的制造方法
CN105800616A (zh) * 2016-05-09 2016-07-27 浙江迅鼎半导体材料科技有限公司 一种乙硅烷的制造方法

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CN105800616A (zh) 2016-07-27

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