JP2004196643A - Silicon - Google Patents

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Publication number
JP2004196643A
JP2004196643A JP2002383377A JP2002383377A JP2004196643A JP 2004196643 A JP2004196643 A JP 2004196643A JP 2002383377 A JP2002383377 A JP 2002383377A JP 2002383377 A JP2002383377 A JP 2002383377A JP 2004196643 A JP2004196643 A JP 2004196643A
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JP
Japan
Prior art keywords
silicon
purity
silicon tetrachloride
zinc
gas
Prior art date
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Application number
JP2002383377A
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Japanese (ja)
Other versions
JP5087195B2 (en
Inventor
Hideo Yamase
英夫 山瀬
Yutaka Kamaike
豊 蒲池
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Individual
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Priority to JP2002383377A priority Critical patent/JP5087195B2/en
Publication of JP2004196643A publication Critical patent/JP2004196643A/en
Application granted granted Critical
Publication of JP5087195B2 publication Critical patent/JP5087195B2/en
Anticipated expiration legal-status Critical
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a product obtained through highly efficient reduction of silicon tetrachloride with a zinc gas for realizing cost reduction and large-amount supply of high-purity raw material silicon, i.e., the greatest problems in a photovoltaic power generation system which is the most preferable system for energy generation from the standpoint of improving global environment. <P>SOLUTION: A high-purity silicon crystal is produced by heating and evaporating zinc metal and silicon tetrachloride in an evaporator, introducing the evaporated silicon tetrachloride and zinc metal into a reactor by employing an inert gas as a carrier, and carrying out reduction in a gasifying atmosphere. <P>COPYRIGHT: (C)2004,JPO&NCIPI

Description

【0001】
【発明の属する技術分野】
本発明は、高純度亜鉛ガス及び高純度四塩化珪素ガスを反応させる四塩化珪素の亜鉛ガス化還元法により生成された高純度シリコンに関する。
【0002】
【従来の技術】
従来の方式は、TCS(三塩化シラン)を水素ガスにより還元反応を行い高純度シリコンを生成させているが、反応効率が悪く且つ大電力を消費するために、高純度多結晶シリコンで約5,000円/kgと高価となり、太陽電池用としては不適格品が一部使用されているに過ぎない。
【0003】
【発明が解決しようとする課題】
本発明は、高純度亜鉛ガス及び高純度四塩化珪素ガスを、900℃〜1100℃のガス化雰囲気において反応させることにより、高純度シリコン結晶を生成させるものである。
【0004】
【課題を解決するための手段】
上記課題を解決するため、金属亜鉛及び四塩化珪素をそれぞれ加熱蒸発する蒸発器と、蒸発した四塩化珪素及び金属亜鉛を不活性ガスをキャリアとして温度制御、流量制御を行いつつ所定の量を反応器に導入して還元反応を行わせると、請求項1記載の高純度シリコンが生成する。尚、樹枝状結晶もしくは鱗状結晶等の生成割合は、運転条件により変動する。
【0005】
上記で生成した高純度シリコンは大部分が樹枝状結晶や鱗状結晶よりなるが、形状が一定ではなく微粒子や粉体も含む。尚、キャステイング等の後工程での取り扱いの便の為に、難溶解の粉体は篩等で除去後、加熱・融解し固化した塊状の多結晶シリコンとする。
【0006】
【実施例1】
上記0004項により製造した製品の品質を下記に示す。
(1)測定条件:CZキャロットX’tal 4P測定。
(2)抵抗値:N240Ωcm(Top−5%)、Nl60Ωcm(Top−60%)
(3)Bレベル:P1,020Ωcm(Top−5%)、P990Ωcm(Top−60%)
(4)LT:130μ−sec
【0007】
【実施例2】
上記0005項により製造した製品の品質を下記に示す。
(1)測定条件:CZキャロットX’tal 4P測定。
(2)抵抗値:N270Ωcm(Top−5%)、N400Ωcm(Top−60%)
(3)Bレベル:P240Ωcm(Top−5%)、P280Ωcm(Top−60%)
(4)LT:80μ−sec
【実施例3】
上記0004項により製造した製品のサイズにより分別した1例を下記に示す。
(1)測定条件:16メッシュのスクリーンによる。
(2)同スクリーンを通過するものの割合:37%
(3)同スクリーンを通過しないもの割合:63%
[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to high-purity silicon produced by a zinc gasification reduction method of silicon tetrachloride in which high-purity zinc gas and high-purity silicon tetrachloride gas are reacted.
[0002]
[Prior art]
In the conventional method, TCS (silane trichloride) is reduced with hydrogen gas to produce high-purity silicon. However, since the reaction efficiency is low and large power is consumed, about 5% of high-purity polycrystalline silicon is used. It is expensive at 2,000 yen / kg, and only some of the unqualified products are used for solar cells.
[0003]
[Problems to be solved by the invention]
The present invention is to produce high-purity silicon crystals by reacting high-purity zinc gas and high-purity silicon tetrachloride gas in a gasification atmosphere at 900 ° C to 1100 ° C.
[0004]
[Means for Solving the Problems]
In order to solve the above problems, an evaporator for heating and evaporating metal zinc and silicon tetrachloride respectively, and reacting a predetermined amount of the evaporated silicon tetrachloride and metal zinc while performing temperature control and flow rate control using an inert gas as a carrier. The high-purity silicon according to claim 1 is produced when the reaction product is introduced into a vessel to perform a reduction reaction. The rate of formation of dendritic crystals or scale-like crystals varies depending on operating conditions.
[0005]
Most of the high-purity silicon produced above consists of dendritic crystals or scale-like crystals, but the shape is not constant and includes fine particles and powder. In addition, for the convenience of handling in a post-process such as casting, the hardly-dissolved powder is removed by a sieve or the like, and then heated and melted to form a solid polycrystalline silicon.
[0006]
Embodiment 1
The quality of the product manufactured according to the above item 0004 is shown below.
(1) Measurement conditions: CZ carrot X'tal 4P measurement.
(2) Resistance: N240Ωcm (Top-5%), N160Ωcm (Top-60%)
(3) B level: P1,020 Ωcm (Top-5%), P990 Ωcm (Top-60%)
(4) LT: 130 μ-sec
[0007]
Embodiment 2
The quality of the product manufactured according to the above item 0005 is shown below.
(1) Measurement conditions: CZ carrot X'tal 4P measurement.
(2) Resistance value: N270Ωcm (Top-5%), N400Ωcm (Top-60%)
(3) B level: P240Ωcm (Top-5%), P280Ωcm (Top-60%)
(4) LT: 80 μ-sec
Embodiment 3
An example of sorting according to the size of the product manufactured according to the above item 0004 is shown below.
(1) Measurement conditions: 16 mesh screen.
(2) Percentage of those passing through the screen: 37%
(3) Proportion not passing through the screen: 63%

Claims (1)

高純度亜鉛ガス及び高純度四塩化珪素ガスを反応させる四塩化珪素の亜鉛ガス化還元法により生成された、50重量%以上が1mmサイズのスクリーンを通過しない樹枝状結晶もしくは鱗状結晶である一般太陽電池級に使用される抵抗値が「N>0.1Ωcm」もしくは「P>1Ωcm」の高純度多結晶シリコン。A general solar cell which is a dendritic crystal or a scale-like crystal in which 50% by weight or more is produced by a zinc gasification reduction method of silicon tetrachloride which reacts high-purity zinc gas and high-purity silicon tetrachloride gas and does not pass through a 1 mm size screen. High-purity polycrystalline silicon with a resistance value of “N> 0.1 Ωcm” or “P> 1 Ωcm” used for battery grade.
JP2002383377A 2002-12-19 2002-12-19 Method for producing silicon Expired - Lifetime JP5087195B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2002383377A JP5087195B2 (en) 2002-12-19 2002-12-19 Method for producing silicon

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2002383377A JP5087195B2 (en) 2002-12-19 2002-12-19 Method for producing silicon

Publications (2)

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JP2004196643A true JP2004196643A (en) 2004-07-15
JP5087195B2 JP5087195B2 (en) 2012-11-28

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006056767A (en) * 2004-08-17 2006-03-02 Yutaka Kamaike Apparatus and method for producing silicon
JPWO2008153181A1 (en) * 2007-06-15 2010-08-26 ソーラーシリコンテクノロジー株式会社 Reactor for producing silicon raw materials for solar cells

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2773745A (en) * 1954-07-20 1956-12-11 Du Pont Process for the production of pure silicon in a coarse crystalline form
JP2002234719A (en) * 2001-01-31 2002-08-23 Yutaka Kamaike Apparatus for producing silicon material and method therefor
JP2004059416A (en) * 2002-07-31 2004-02-26 Yutaka Kamaike Manufacturing method of silicon

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2773745A (en) * 1954-07-20 1956-12-11 Du Pont Process for the production of pure silicon in a coarse crystalline form
JP2002234719A (en) * 2001-01-31 2002-08-23 Yutaka Kamaike Apparatus for producing silicon material and method therefor
JP2004059416A (en) * 2002-07-31 2004-02-26 Yutaka Kamaike Manufacturing method of silicon

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006056767A (en) * 2004-08-17 2006-03-02 Yutaka Kamaike Apparatus and method for producing silicon
JPWO2008153181A1 (en) * 2007-06-15 2010-08-26 ソーラーシリコンテクノロジー株式会社 Reactor for producing silicon raw materials for solar cells

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