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JP2004196642A - Apparatus and method for preparing silicon - Google Patents

Apparatus and method for preparing silicon Download PDF

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Publication number
JP2004196642A
JP2004196642A JP2002383376A JP2002383376A JP2004196642A JP 2004196642 A JP2004196642 A JP 2004196642A JP 2002383376 A JP2002383376 A JP 2002383376A JP 2002383376 A JP2002383376 A JP 2002383376A JP 2004196642 A JP2004196642 A JP 2004196642A
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Prior art keywords
gas
purity
zinc
silicon
silicon tetrachloride
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JP2002383376A
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Japanese (ja)
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JP4497813B2 (en
Inventor
Hideo Yamase
英夫 山瀬
Yutaka Kamaike
豊 蒲池
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an apparatus for preparing high-purity silicon through a gas-phase zinc reduction method wherein the reaction is stably carried out by locating the inlets for introducing raw material gases into the reaction apparatus at different heights and by introducing an appropriate inert gas, and a preparation method. <P>SOLUTION: The inlet for introducing a zinc gas and the inlet for introducing a silicon tetrachloride gas are located at the upper and lower parts of the reaction apparatus, respectively. The reduction reaction is stably carried out by introducing the raw material gases through these inlets and introducing the inert gas into the outlet side, the zinc gas side, etc., of the reaction apparatus. Product quality is improved by improving the purity of the raw materials by passing the raw material gases to be introduced through the silicon. <P>COPYRIGHT: (C)2004,JPO&NCIPI

Description

【0001】
【発明の属する技術分野】
本発明は、高純度シリコンの製造方法に関し、さらに詳しくは原料として四塩化珪素及び金属亜鉛を蒸発気化して使用し、気相において還元反応を行う反応装置の構造に関する。
【0002】
【従来の技術】
従来の亜鉛還元法による高純度シリコンの製造は、溶融亜鉛中に四塩化珪素ガスを導入する方式であるため、液〜ガス間で反応が行われ、その結果として安定した品質の高純度シリコンを得ることが出来なかった。
【0003】
【発明が解決しようとする課題】
本発明の課題は、気相法亜鉛還元法による高純度シリコン製造用反応装置において、気相状態では相対的に軽い亜鉛ガスを上部より、相対的に重い四塩化珪素ガスを下部より導入することにより、安定した品質の高純度シリコンを得ることが出来る装置および方法を提供することにある。
【0004】
反応装置内において、原料ガスの導入部より進むにしたがって反応が進み生成物により詰まり易くなるので、出口側より不活性ガスの導入を行う。
【0005】
反応装置内において、原料ガスの導入部より進むにしたがって反応が進み生成物により詰まり易くなるので、出口側の温度を高めに設定して運転する。
【0006】
亜鉛雰囲気の部分へ四塩化珪素ガスが送られると、そこで部分的な反応が行われて固形物が生じ、詰まりなどの不都合を生じるために、亜鉛ガス雰囲気の所に不活性ガスを導入して四塩化珪素ガス雰囲気の部分より高めに運転する。
【0007】
【課題を解決するための手段】
上記課題を解決するため、本願で特許請求される発明は以下の通りである。
(1)高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応装置において、高純度亜鉛ガスの導入口を高純度四塩化珪素ガスの導入口に対して相対的に上部に配置した高純度シリコン製造装置。
(2)上記(1)記載の装置を用い、安定した還元反応を行わせることを特徴とする高純度シリコンの製造方法。
(3)高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応装置において、不活性ガスの導入を原料ガスの導入側に対して反対側となる反応装置の出口側より導入する高純度シリコン製造装置。
(4)高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応装置内において、原料導入側よりも出口側の温度を高く設定することにより、生成したシリコンによる反応装置内部の詰まりを防止する高純度シリコンの製造方法。
(5)高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応システムにおいて、原料として供給する亜鉛ガス中に四塩化珪素ガスが混入しないように、起動時や停止時を除く定常運転時には、亜鉛ガスが存在する亜鉛蒸発器及び亜鉛ガス過熱器に不活性ガスを導入し、四塩化珪素ガス側には不活性ガスを導入しない高純度シリコンの製造方法。
(6)高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応システムにおいて、原料として供給する亜鉛ガス又は四塩化珪素ガスの純度を改善する為に、それぞれがガス化した後、反応装置へ導入されるまでの間に高純度シリコンを設けた高純度シリコンの製造方法。
(7)上記6項において純度を改善するために設ける高純度シリコンとして、反応装置で生成する高純度シリコン結晶の中の粒径が小さいものを使用する高純度シリコンの製造方法。
【0008】
【発明の実施の形態】
【実施例1】
図1は、本発明装置の実施例を示す説明図である。
反応装置▲1▼への亜鉛ガスの導入口は上部の▲2▼、四塩化珪素ガスの導入口は下部の▲3▼に設置する。反応装置▲1▼の大きさが30cm(▲4▼)の時、導入口▲2▼及び▲3▼は反応装置の中心よりそれぞれ5〜10cmの位置に取り付ける。
【図面の簡単な説明】
【図1】本発明による反応装置の例
【符号の説明】
▲1▼・・・反応装置 ▲2▼・・・亜鉛ガス導入口
▲3▼・・・四塩化珪素ガス導入口 ▲4▼・・・反応装置の大きさ
[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for producing high-purity silicon, and more particularly, to a structure of a reactor for performing a reduction reaction in a gas phase by using silicon tetrachloride and metal zinc as raw materials by evaporating them.
[0002]
[Prior art]
Since the production of high-purity silicon by the conventional zinc reduction method is a method in which silicon tetrachloride gas is introduced into molten zinc, a reaction takes place between liquid and gas, and as a result, high-purity silicon of stable quality is produced. I couldn't get it.
[0003]
[Problems to be solved by the invention]
An object of the present invention is to introduce a relatively light zinc gas from an upper part and a relatively heavy silicon tetrachloride gas from a lower part in a gas phase in a reactor for producing high-purity silicon by a vapor phase zinc reduction method. Accordingly, an object of the present invention is to provide an apparatus and a method capable of obtaining high-purity silicon of stable quality.
[0004]
In the reaction device, the reaction proceeds as it proceeds from the introduction portion of the raw material gas, and the reaction product tends to be clogged. Therefore, the inert gas is introduced from the outlet side.
[0005]
In the reactor, the reaction proceeds as it proceeds from the inlet of the raw material gas, and the product is easily clogged. Therefore, the reactor is operated with the outlet temperature set at a higher temperature.
[0006]
When silicon tetrachloride gas is sent to a portion of the zinc atmosphere, a partial reaction takes place there to generate a solid, which causes inconvenience such as clogging. Operate higher than the silicon tetrachloride gas atmosphere.
[0007]
[Means for Solving the Problems]
The invention claimed in the present application to solve the above problems is as follows.
(1) In a reaction apparatus relating to a zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas, an inlet of high-purity zinc gas is connected to an inlet of high-purity silicon tetrachloride gas. High-purity silicon production equipment located relatively above.
(2) A method for producing high-purity silicon, wherein a stable reduction reaction is performed using the apparatus according to (1).
(3) In a reaction apparatus related to a zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas, a reaction apparatus in which the introduction of an inert gas is on the opposite side to the introduction side of a raw material gas. High-purity silicon production equipment introduced from the outlet side of
(4) Silicon produced by setting the temperature on the outlet side higher than on the material introduction side in a reactor related to the zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas A method for producing high-purity silicon, which prevents clogging inside a reactor by the above method.
(5) In the reaction system relating to the zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas, at the time of startup, silicon tetrachloride gas is not mixed into zinc gas supplied as a raw material. A method for producing high-purity silicon in which an inert gas is introduced into a zinc evaporator and a zinc gas superheater in which zinc gas is present, and no inert gas is introduced into a silicon tetrachloride gas side, during normal operation except when the gas is stopped.
(6) In a reaction system related to a zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas, in order to improve the purity of zinc gas or silicon tetrachloride gas supplied as a raw material, A method for producing high-purity silicon in which high-purity silicon is provided after gasification is performed and before it is introduced into a reaction apparatus.
(7) A method for producing high-purity silicon using a high-purity silicon crystal having a small particle diameter in a high-purity silicon crystal generated in a reactor as the high-purity silicon provided in 6 above for improving the purity.
[0008]
BEST MODE FOR CARRYING OUT THE INVENTION
Embodiment 1
FIG. 1 is an explanatory view showing an embodiment of the device of the present invention.
The inlet for the zinc gas into the reactor (1) is located at the upper (2), and the inlet for the silicon tetrachloride gas is located at the lower (3). When the size of the reactor (1) is 30 cm (4), the inlets (2) and (3) are respectively mounted at positions 5 to 10 cm from the center of the reactor.
[Brief description of the drawings]
FIG. 1 shows an example of a reactor according to the present invention.
{Circle around (1)} Reactor {2} ... Inlet for zinc gas {3} ... Inlet for silicon tetrachloride gas {4} ... Reactor size

Claims (7)

高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応装置において、高純度亜鉛ガスの導入口を高純度四塩化珪素ガスの導入口に対して相対的に上部に配置した高純度シリコン製造装置。In a reactor related to a zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas, the inlet of the high-purity zinc gas is relatively positioned with respect to the inlet of the high-purity silicon tetrachloride gas. High-purity silicon production equipment placed at the top. 高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応装置において、不活性ガスの導入を原料ガスの導入側に対して反対側となる反応装置の出口側より導入する高純度シリコン製造装置。In the reactor related to the zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas, an inert gas is introduced on the outlet side of the reactor opposite to the source gas introduction side. High-purity silicon production equipment to be introduced. 高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応装置内において、原料導入側よりも出口側の温度を高く設定することにより、生成したシリコンによる反応装置内部の詰まりを防止する高純度シリコンの製造方法。In the reactor related to the zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas, the reactor on the outlet side is set higher than the raw material introduction side, so that the reactor using the generated silicon A method for producing high-purity silicon that prevents internal clogging. 高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応システムにおいて、原料として供給する亜鉛ガス中に四塩化珪素ガスが混入しないように、起動時や停止時を除く定常運転時には、亜鉛ガスが存在する亜鉛蒸発器及び亜鉛ガス過熱器に不活性ガスを導入し、四塩化珪素ガス側には不活性ガスを導入しない高純度シリコンの製造方法。In a reaction system related to the zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas, at the time of starting and stopping so that silicon tetrachloride gas is not mixed into the zinc gas supplied as a raw material. A method for producing high-purity silicon in which an inert gas is introduced into a zinc evaporator and a zinc gas superheater in which zinc gas is present during normal operation except for the inert gas, and no inert gas is introduced into the silicon tetrachloride gas side. 高純度亜鉛ガス及び高純度四塩化珪素ガスを使用した四塩化珪素の亜鉛還元法に係わる反応システムにおいて、原料として供給する亜鉛ガス又は四塩化珪素ガスの純度を改善する為に、それぞれがガス化した後、反応装置へ導入されるまでの間に高純度シリコンを設けた高純度シリコンの製造方法。In a reaction system related to the zinc reduction method of silicon tetrachloride using high-purity zinc gas and high-purity silicon tetrachloride gas, in order to improve the purity of the zinc gas or silicon tetrachloride gas supplied as a raw material, each is gasified. After that, a method for producing high-purity silicon in which high-purity silicon is provided before being introduced into a reaction apparatus. 請求項5において純度を改善するために設ける高純度シリコンとして、反応装置で生成する高純度シリコン結晶の中の粒径が小さいものを使用する高純度シリコンの製造方法。6. A method for producing high-purity silicon, comprising using high-purity silicon having a small particle size among high-purity silicon crystals generated in a reactor as the high-purity silicon provided in order to improve the purity. 請求項1及び/もしくは請求項2記載の装置を用いて、安定した還元反応を行わせることを特徴とする高純度シリコンの製造方法。A method for producing high-purity silicon, wherein a stable reduction reaction is performed using the apparatus according to claim 1.
JP2002383376A 2002-12-19 2002-12-19 Method for producing silicon Expired - Lifetime JP4497813B2 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007217262A (en) * 2006-02-14 2007-08-30 Kinotech Corp Apparatus for manufacturing silicon
US7553468B2 (en) * 2007-03-12 2009-06-30 Chisso Corporation Method for producing solid product
WO2010134544A1 (en) * 2009-05-22 2010-11-25 旭硝子株式会社 Device for producing silicon and process for producing silicon

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002234719A (en) * 2001-01-31 2002-08-23 Yutaka Kamaike Apparatus for producing silicon material and method therefor
JP2002274832A (en) * 2001-03-16 2002-09-25 Yutaka Kamaike Apparatus and method for manufacturing silicon raw material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002234719A (en) * 2001-01-31 2002-08-23 Yutaka Kamaike Apparatus for producing silicon material and method therefor
JP2002274832A (en) * 2001-03-16 2002-09-25 Yutaka Kamaike Apparatus and method for manufacturing silicon raw material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007217262A (en) * 2006-02-14 2007-08-30 Kinotech Corp Apparatus for manufacturing silicon
US7553468B2 (en) * 2007-03-12 2009-06-30 Chisso Corporation Method for producing solid product
CN101264889B (en) * 2007-03-12 2012-01-04 Jnc株式会社 Method and apparatus for producing solid product
US8657956B2 (en) 2007-03-12 2014-02-25 Jnc Corporation Apparatus for producing solid product
WO2010134544A1 (en) * 2009-05-22 2010-11-25 旭硝子株式会社 Device for producing silicon and process for producing silicon
JPWO2010134544A1 (en) * 2009-05-22 2012-11-12 旭硝子株式会社 Silicon manufacturing apparatus and silicon manufacturing method

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