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WO2017018771A1 - Procédé de préparation de tétrasilane et de pentasilane - Google Patents

Procédé de préparation de tétrasilane et de pentasilane Download PDF

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Publication number
WO2017018771A1
WO2017018771A1 PCT/KR2016/008140 KR2016008140W WO2017018771A1 WO 2017018771 A1 WO2017018771 A1 WO 2017018771A1 KR 2016008140 W KR2016008140 W KR 2016008140W WO 2017018771 A1 WO2017018771 A1 WO 2017018771A1
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Prior art keywords
silane
tetrasilane
pyrolysis
pentasilane
trisilane
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Ceased
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PCT/KR2016/008140
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English (en)
Korean (ko)
Inventor
송영하
권삼봉
김성수
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SK Materials Co Ltd
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SK Materials Co Ltd
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02—Silicon compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02—Silicon compounds
    • C07F7/08—Compounds having one or more C—Si linkages

Definitions

  • the present invention relates to a method for producing tetrasilane and pentasilane having high added value as silicon for semiconductors in high yield.
  • the higher silane has a lower decomposition temperature than the lower silane, thereby lowering the temperature of the process of forming the thin film, and when the thin film is formed at the same temperature using the lower silane, the silicon thin film growth rate is faster than that of the lower silane. Homogeneous membrane deposition is possible.
  • higher order silane is expected to be widely used in the semiconductor field in the future.
  • a higher silane may be prepared using a reducing agent such as lithium aluminum hydride (LiAlH 4 ) on a hexachloro disilane or hexaethoxydisilane solvent.
  • a reducing agent such as lithium aluminum hydride (LiAlH 4 ) on a hexachloro disilane or hexaethoxydisilane solvent.
  • this method has a high price of hexadiclodisilane and a reducing agent, and it is difficult to separate organosilicon compounds produced as a by-product.
  • Another method is the production of higher silanes such as tetrasilane, as well as lower silanes such as disilane and trisilane, from monosilanes using the electric discharge method.
  • the method has been reported to obtain a higher yield of higher order silanes, such as tetrasilane, but it is difficult to develop the device for commercial production, it is still difficult to use in the actual manufacturing process.
  • US Patent No. 6027705 proposes a method for producing trisilane or higher silane, and pyrolyzing monosilane by continuously connecting two pyrolysis reactors.
  • this method is complicated to operate, low in yield, and difficult to apply to the actual process.
  • U.S. Patent No. 70609494 describes a method for producing trisilane by pyrolyzing disilane, but due to the reversible reaction mechanism, the yield of higher silane is low, and monosilane and disilane are excessively decomposed.
  • the production economy is low due to the generation of more by-products such as solid silicon powder than the amount converted to higher silane, and the continuous process is impossible due to the blockage of the line due to deposition of a large amount of product in the reactor or accumulation in the process line.
  • the main object of the present invention is to produce a higher-order silane which can economically and efficiently produce high-order silanes, particularly tetrasilane or pentasilane, useful for silicon precursors for semiconductors by thermally decomposing trisilane to solve the above problems. To provide.
  • Tetrasilane or pentasilane production method (a) pyrolysis step of pyrolyzing pure trisilane in a pyrolysis reactor; (b) removing the solid particles to remove the solid particles produced in the pyrolysis product; (c) a condensation step of liquefying and collecting silanes other than hydrogen from the pyrolysis product from which the solid particles are removed; (d) a first separation step of separating the lower silane having a silicon number of 3 or less from the liquefied silanes; (e) a second separation step of separating tetrasilane and pentasilane from the mixture from which the lower silane is removed; Characterized in that it comprises a.
  • the trisilane in step (a) is mixed with the diluent gas is introduced into the pyrolysis reactor, the diluent gas is helium, nitrogen, argon, hydrogen or a mixture thereof, the raw silane gas and dilution
  • the mixing ratio of the gas is characterized in that it is adjusted at a ratio of 50:50 ⁇ 1: 99% by volume.
  • the trisilane is introduced into the reactor at a temperature of 300 ° C or less, preferably 280 to 300 ° C.
  • reaction temperature is 300 °C to 400 °C, it is characterized in that more preferably 325 °C to 375 °C.
  • the pressure of the pyrolysis reactor is 1 bar to 3 bar, characterized in that the space velocity of the trisilane is 50 to 500 hr -1 .
  • the method for producing tetrasilane and pentasilane according to the present invention it is possible to improve the yield of tetrasilane and pentasilane at several times compared to the existing method even at low temperature, so that it is possible to manufacture a large amount of high value-added high-order silane with high economic efficiency. It works.
  • FIG. 1 is a schematic view of a high-order silane manufacturing process according to an embodiment of the present invention.
  • FIG. 2 is a graph showing the conversion rate of monosilane according to the pyrolysis reaction temperature during monosilane pyrolysis.
  • 3 is a graph showing the yield of the product according to the pyrolysis reaction temperature during monosilane pyrolysis.
  • 5 is a graph showing the yield of the product according to the pyrolysis reaction temperature during disilane pyrolysis.
  • FIG. 6 is a graph showing the conversion rate of trisilane according to the pyrolysis reaction temperature according to an embodiment of the present invention.
  • FIG. 7 is a graph showing the yield of the product according to the pyrolysis reaction temperature during trisilane pyrolysis according to an embodiment of the present invention.
  • higher order silane means a silane having a silicon number of 4 or more
  • low order silane means a silane having a silicon number of 4 or less
  • raw material silane refers to a silane compound introduced into a pyrolysis reactor and pyrolyzed to produce higher silane. Examples are monosilane, disilane, trisilane and the like.
  • Raw silane gas is intended to indicate that the silane is maintained in gaseous form.
  • the present invention is characterized in that pyrolysis is performed using trisilane, not monosilane or disilane, as a raw material for pyrolysis reaction in order to produce higher silanes such as tetrasilane and / or pentasilane.
  • FIG. 1 is a schematic diagram of a manufacturing process of tetrasilane and pentasilane according to an embodiment of the present invention.
  • trisilane is supplied to a pyrolysis reactor 100 to perform pyrolysis, and then the resulting pyrolysis product is transferred to a solid particle separator 200 to remove solid particles.
  • Silanes other than hydrogen generated lower silane, unreacted substance and higher silane
  • the higher silane is separated and transferred to the second separation unit 500.
  • the unreacted material (including the generated lower silane) from which the higher silane is recovered is separated, the trisilane is transferred to the pyrolysis reactor 100, and the remaining lower silane is separated and recovered from the third separation unit 400, and then used for other purposes. Collect and save.
  • the higher silane separated and recovered in the second separation unit 500 is purified by tetrasilane and pentasilane in the purification units 600 and 700, respectively, and filled in the charging units 610 and 710, respectively.
  • the manufacturing process is as follows.
  • the raw material silane is introduced into a pyrolysis reactor to perform pyrolysis of the raw material silane.
  • the raw material silane may be introduced in the form of gas and may be pyrolyzed without dilution gas, but is generally introduced into the reactor as the diluent gas.
  • the diluent gas may be helium (He), nitrogen (N 2), argon (Ar) gas, or a mixed gas in which hydrogen (H 2) is mixed in the inert gas, and the raw silane gas and the dilution gas are 50: 50 to 1: 99. It is used by adjusting the ratio of volume%.
  • the pyrolysis reaction temperature may be performed at 300 ° C to 375 ° C, preferably 325 ° C to 375 ° C. More preferably, it may be a temperature of 350 °C to 375 °C.
  • the pyrolysis reactor may be a tubular reactor composed of one or more tubes, but is not limited thereto.
  • the pyrolysis temperature is less than 300 °C, the yield of the desired higher silane is very low, if the pyrolysis temperature is higher than 400 °C, the production of solid particles is too high, if the temperature exceeds 400 °C tetrasilane and pentasilane Yield is reduced.
  • the trisilane gas when introduced into the pyrolysis reactor, it may be introduced at a temperature of 300 ° C. or less, preferably preheated to 280 ° C. to 300 ° C. When the preheating temperature exceeds 300 ° C., the pyrolysis reaction occurs in advance, which is not appropriate.
  • the pressure in the reactor during the pyrolysis reaction can be any of atmospheric pressure, pressurization and reduced pressure, but carrying out the reaction under pressure is economically advantageous in terms of separation efficiency, cooling cost and device size.
  • the reaction pressure is in the range of 1 or 3 bar, preferably 1 to 1.5 bar. Increasing the reaction pressure increases the conversion and yield, but in the case of trisilane having a low vapor pressure, an apparatus investment cost for the feeder increases.
  • the space velocity of the raw material silane gas from the reactors in the range of from 50 to 500hr -1, preferably in the range of 100 to 150hr -1.
  • the gas space velocity (SV) refers to the value divided by the reactor volume passing the volume of raw gas per hour flowing into the pyrolysis reactor measured at the reactor inlet. Also called space velocity.
  • SV gas space velocity
  • Increasing the gas space velocity has the advantage of reducing the amount of solid particles, but the amount of recycled unreacted raw silane gas is greatly increased, the volume of the reactor is increased, there is a disadvantage that the operating cost increases.
  • Such pyrolysis may be carried out by conventional methods used in the art, and the temperature inside the reactor may be raised or maintained using an electrical method or other known methods.
  • the said raw material silane is aimed at higher silane, it is preferable that it is trisilane rather than monosilane and disilane.
  • Pyrolysis using trisilane as a raw material has the advantage that the reaction temperature can be further lowered than that of conventional monosilane or disilane, and the yield of higher silane is several times higher than that of monosilane or disilane. It can increase by several orders of magnitude.
  • the pyrolysis gas produced as a result of performing pyrolysis of the raw silane gas in the reactor as described above includes unreacted material, lower silane, higher silane, hydrogen (boiling point 253 ° C.) and several hundred micron sized solid particles at sub-micron. .
  • the unreacted product may be trisilane (boiling point 53 ° C.), monosilane (boiling point ⁇ 112 ° C.) or disilane (boiling point 14 ° C.), and the higher silane is a silane having a silicon number of 4 or more including tetrasilane and pentasilane. .
  • the raw silane may be decomposed to produce lower silanes lower than the raw silane.
  • the resulting pyrolysis product is obtained to remove solid particles contained in the pyrolysis product.
  • the removal of solid particles in the pyrolysis product not only eliminates process troubles caused by the solid particles in subsequent process steps, but also leads to problems in semiconductor processes where higher order silane gas is used as the final product contains sub-micron particles. It can prevent.
  • Removal of the solid particles may be used without limitation as long as it is a known method for removing solid particles in a gas stream in the art. For example, it is possible to capture and remove solid particles by using a cyclone or a metal filter. Particularly, particles smaller than 0.1 micron are difficult to be removed by a metal filter. Additional traps can be installed to remove solid particles. At this time, the filter can be periodically recycled and reused.
  • the solid particles may be removed by passing a gas including the solid particles through a washing tower spraying an aqueous solution dissolving water or the solid particles. In this case, a separate adsorption tower may be installed for removal of an aqueous solution dissolving water and solid particles generated in the washing tower.
  • the higher silane, the unreacted raw material silane and the lower silane are separated from the pyrolysis product from which the solid particles are removed to recover the higher silane.
  • the lower silane produced during the pyrolysis process is also separated together with the unreacted material.
  • the separation method of the higher order silane and the unreacted raw material may be separated using their physical properties, and preferably, the boiling point difference of these compounds may be separated, but is not limited thereto.
  • tetrasilane or pentasilane is separated and recovered from the recovered higher silane.
  • the method of separating tetrasilane or pentasilane from higher silanes can be separated using their physical properties, similar to the method of separating unreacted substances from higher silanes, and preferably separated using the boiling point difference of these compounds. May be, but is not limited to.
  • the tetrasilane or pentasilane separated in this way may be liquefied and collected, and may further include a purification step and a collecting step to obtain a final target product, and the unreacted raw material separated from the higher silane is recovered to recover the above-described pyrolysis reactor. By recirculating, the loss of raw silane can be minimized.
  • the unreacted raw material silane When the unreacted raw material silane is recycled, it may be directly recycled to a pyrolysis reactor, or may be recycled to each unreacted raw material tank.
  • the reaction temperature was experimented using a reactor consisting of a 300 ⁇ 450 °C tubular reactor. At this time, the pressure was 1 bar (absolute pressure), and the space velocity was 120 h -1 based on the total gas flow rate including the diluent gas.
  • Trisilane was used as the reaction raw material silane gas, high purity nitrogen was used as the diluent gas, and the flow rate was supplied at a total flow rate of 95 ml / min including the diluent gas.
  • the dilution ratio was adjusted to a nitrogen: trisilane volume ratio of 7: 3.
  • the column filled with gas chromatography (Varian, CP3800) connected on-line to the reactor (Porapak Q, 100 ⁇ 120mesh, 6′X 1/8 ′′ x 2.0mm, CP914534) , Varian), and the product was analyzed by a Thermal Conductivity Detector (TCD).
  • gas chromatography Variarian, CP3800
  • Porapak Q 100 ⁇ 120mesh, 6′X 1/8 ′′ x 2.0mm, CP914534
  • Varian Thermal Conductivity Detector
  • Conversion and yield of each reactant was calculated by weight.
  • the conversion rate of the product is expressed as a percentage of (weight of the reacted raw silane gas) / (weight of the fed raw silane gas), and the selectivity is (weight of each generated component) / (reacted raw silane). Weight of gas) as a percentage. Yield was calculated as conversion x selectivity.
  • Example 2 The same method as in Example 1 was carried out, but pyrolysis was performed using disilane as the raw silane gas.
  • the pyrolysis temperature of the reaction proceeds after 400 °C to increase the monosilane conversion, from 430 °C to increase the temperature of the monosilane The conversion rate increased linearly.
  • tetrasilane Only tetrasilane was produced as a product of the higher silane, and no pentasilane was detected in the reaction product.
  • the amount of tetrasilane produced began to be significant at about 430 ° C., but the production of tetrasilane was less than 1 wt% at 450 ° C., and most of the pyrolysis products were disilane.
  • the monosilane conversion increased linearly in proportion to the yield of disilane, trisilane, and tetrasilane, and the monosilane conversion was almost increased to solid particles. It was due to the increase in the rate of conversion.
  • the conversion rate of the raw material silane into solid particles at 385 ° C is about 8 wt%, whereas at 400 ° C, the rate of conversion of the raw material silane to solid particles increases to 22 wt%.
  • Example 1 using trisilane as the raw silane gas, pentasilane was not only produced, but the yield was higher than that of tetrasilane, compared to Comparative Examples 1 and 2 using monosilane or disilane as the raw silane gas. .
  • the yields of higher silanes such as tetrasilane and pentasilane are several to several tens of times higher than those of Comparative Examples 1 and 2.
  • the yield decreases with increasing pyrolysis temperature at 375 ° C. as a peak for both tetrasilane and pentasilane. This is different from the tetrasilane production in FIG. 3 and FIG. 5, which show a tendency to gradually increase as temperature increases to 450 ° C. and 400 ° C., respectively.
  • the yield graph according to has a maximum at about 375 ° C.
  • the conversion rate to solid particles increases with temperature as the solid particles start to form around 350 ° C. and then increase very rapidly after 375 ° C.
  • the yield of tetrasilane and pentasilane is maximized at the initial stage of the rapid increase in the generation of solid particles, and thus the tetrasilane and the amount of solid particles are not high enough to affect the operation of the process. Since the yield of pentasilane is maximum, it is efficient because the yield of higher silane can be increased while reducing the amount of raw material silane recycled in process.
  • the present invention enables economic and efficient production of high value-added high-order silanes, particularly tetrasilane or pentasilane, in higher yields compared to existing processes, and thus the high-order silanes can be widely used in the semiconductor industry as semiconductor film forming materials. I think there will be.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention concerne un procédé de préparation, d'un silane d'ordre supérieur, qui permet la préparation économique et efficace d'un silane d'ordre supérieur, de haute valeur ajoutée, particulièrement de tétrasilane ou de pentasilane, en un rendement élevé comparé à un procédé existant. Plus spécifiquement, la présente invention concerne un procédé de préparation d'un silane d'ordre supérieur en utilisant du trisilane comme matériau pour du silane pour décomposition thermique.
PCT/KR2016/008140 2015-07-27 2016-07-26 Procédé de préparation de tétrasilane et de pentasilane Ceased WO2017018771A1 (fr)

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KR1020150106035A KR101758113B1 (ko) 2015-07-27 2015-07-27 테트라실란 및 펜타실란의 제조방법

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020077177A1 (fr) 2018-10-11 2020-04-16 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procédé de production de silanes supérieurs enrichis en isomère
DE102020211833A1 (de) 2020-09-22 2022-03-24 Evonik Operations Gmbh Verfahren zur Herstellung oligomerer Hydridosilane aus SiH4

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI683788B (zh) * 2018-08-16 2020-02-01 台灣特品化學股份有限公司 高效率的高階矽烷轉化合成及純化回收方法

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JP2719211B2 (ja) * 1989-12-13 1998-02-25 昭和電工株式会社 高次シランの製造法
JPH11260729A (ja) * 1998-01-08 1999-09-24 Showa Denko Kk 高次シランの製造法
JP2008536784A (ja) * 2005-04-05 2008-09-11 ボルテツクス・インコーポレイテツド Ｓｉ２ｈ６およびより高次のシランを製造するためのシステムおよび方法
KR101231370B1 (ko) * 2012-06-13 2013-02-07 오씨아이머티리얼즈 주식회사 모노실란의 열분해에 의한 디실란의 제조방법 및 제조장치

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US7906094B2 (en) 2007-01-18 2011-03-15 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method for producing a high purity trisilane product from the pyrolysis of disilane

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JPH11260729A (ja) * 1998-01-08 1999-09-24 Showa Denko Kk 高次シランの製造法
JP2008536784A (ja) * 2005-04-05 2008-09-11 ボルテツクス・インコーポレイテツド Ｓｉ２ｈ６およびより高次のシランを製造するためのシステムおよび方法
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020077177A1 (fr) 2018-10-11 2020-04-16 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procédé de production de silanes supérieurs enrichis en isomère
US11230474B2 (en) 2018-10-11 2022-01-25 L'Air Liquide, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Process for producing isomer enriched higher silanes
DE102020211833A1 (de) 2020-09-22 2022-03-24 Evonik Operations Gmbh Verfahren zur Herstellung oligomerer Hydridosilane aus SiH4
WO2022063680A1 (fr) 2020-09-22 2022-03-31 Evonik Operations Gmbh Procédé pour la préparation d'hydrosilanes oligomères à partir de sih4

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TW201710271A (zh) 2017-03-16
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TWI602824B (zh) 2017-10-21

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