JPH10167716A - Purification of silicon - Google Patents

Purification of silicon

Info

Publication number
JPH10167716A
JPH10167716A JP8328451A JP32845196A JPH10167716A JP H10167716 A JPH10167716 A JP H10167716A JP 8328451 A JP8328451 A JP 8328451A JP 32845196 A JP32845196 A JP 32845196A JP H10167716 A JPH10167716 A JP H10167716A
Authority
JP
Japan
Prior art keywords
silicon
filter
electron beam
hearth
melting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
JP8328451A
Other languages
Japanese (ja)
Inventor
Kazuhiro Hanazawa
和浩 花澤
Yasuhiko Sakaguchi
泰彦 阪口
Yoshihide Kato
嘉英 加藤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JFE Steel Corp
Original Assignee
Kawasaki Steel Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kawasaki Steel Corp filed Critical Kawasaki Steel Corp
Priority to JP8328451A priority Critical patent/JPH10167716A/en
Publication of JPH10167716A publication Critical patent/JPH10167716A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy

Landscapes

  • Filtering Materials (AREA)
  • Silicon Compounds (AREA)
  • Photovoltaic Devices (AREA)

Abstract

PROBLEM TO BE SOLVED: To improve efficiency of a silicon purifying process of the latter method and to better the yield of a product, by equipping a melting part with a filter and filtering a molten silicon to effectively remove intervening impurities in electron beam melting in purifying silicon by the electron beam melting. SOLUTION: A raw material silicon 3 is supplied to a hearth 1 and melted by electron beam. A filter 4 is installed in the hearth 1 and intervening impurities 5 are caught. The intervening impurities are caught by the filter 4 and a molten silicon 2 is passed through the filter. A sintered filter of high purity SiC is used as the filter 4 and a material which is stable at a high temperature in high vacuum and has a small amount melted into silicon is proper. For example, carbon and silicon carbide are suitable due to stability at high temperature in high vacuum, a small amount melted into molten silicon of about 100ppm and ready oxidation and removal.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は真空下において電子
ビームを用いて太陽電池用シリコン中のP、Al、Ca
等の不純物を除去するシリコンの精製方法に関するもの
である。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to P, Al, Ca in silicon for solar cells using an electron beam under vacuum.
And a method of purifying silicon for removing impurities such as impurities.

【0002】[0002]

【従来の技術】近年エネルギー源の多様化の要求から太
陽光発電が脚光を浴び、低価格発電装置の実用化に向け
研究開発が盛んに行われている。このような状況の中
で、太陽電池用原料としてシリコンは最も汎用され易い
材料であり、動力用電力供給に使われる材料として最も
重要視されている。
2. Description of the Related Art In recent years, photovoltaic power generation has been in the spotlight due to the demand for diversification of energy sources, and research and development have been actively conducted for practical use of low-cost power generation devices. Under such circumstances, silicon is the most commonly used material as a material for solar cells, and is regarded as the most important material used for power supply for power.

【0003】太陽電池用原料として用いられるシリコン
は、99.9999%(6N)以上の高純度シリコンが
必要とされている。従来、市販の金属シリコン(純度9
9.5%)から上記高純度シリコンを製造する場合に、
電子ビーム溶解により市販の金属シリコン中のP、C
a、Alを同時に除去する技術が開発されている。WO
93/12272国際公開公報には水冷銅バス内の湯面
付近に水冷パイプを設置し、浮遊した介在物を除去する
方法が開示されている。その技術は、 (1)電子ビームの誤操作時に溶損し、水漏れ等の事故
を引き起こす可能性が高い。 (2)主要な介在物としては、Al23 、SiO2
SiCがあげられるが、いずれの場合も密度が、4.0
g/cm3 、2.2g/cm3 、3.2g/cm 3 であ
ることから、溶融シリコンの密度2.5g/cm3 に近
く、浮遊だけでなく沈降することもあるため、本法での
介在物除去は不十分である等の問題があった。
[0003] Silicon used as a raw material for solar cells
Is a high purity silicon of 99.9999% (6N) or more
is necessary. Conventionally, commercially available metallic silicon (purity 9
9.5%) to produce the high-purity silicon.
P, C in commercially available metallic silicon by electron beam melting
Technology for simultaneously removing a and Al has been developed. WO
WO 93/12272 states that the water level in a water-cooled copper bath
Install a water cooling pipe nearby to remove suspended inclusions
A method is disclosed. The technology is as follows: (1) Accidents such as water leakage due to erosion due to incorrect operation of the electron beam
Likely to cause. (2) The main inclusions are AlTwo OThree , SiOTwo ,
SiC is mentioned, and in any case, the density is 4.0.
g / cmThree 2.2g / cmThree 3.2g / cm Three In
Therefore, the density of molten silicon is 2.5 g / cmThree Close to
Not only floating but also sedimentation.
There were problems such as insufficient removal of inclusions.

【0004】[0004]

【発明が解決しようとする課題】電子ビーム溶解の場
合、黒鉛容器又は水冷銅容器が用いられる。この時原料
シリコン中に含有されるか、又は、溶解後に生成する介
在物、例えばSiC、SiO2 、Al23 等がハース
から流出し、次の工程又はさらに後段の工程にまで介在
物が除去されずに残留し、場合によってはC等が飽和溶
解量までしか除去されない、という問題があった。この
ような介在物が電子ビーム溶解と連続化された次工程の
一方向凝固セルに入ると、一方向凝固させたインゴット
の切断除去量が増加し、歩留低下を生ずる。
In the case of electron beam melting, a graphite container or a water-cooled copper container is used. At this time, inclusions contained in the raw silicon or generated after melting, for example, SiC, SiO 2 , Al 2 O 3, etc., flow out of the hearth, and the inclusions are included in the next step or further later steps. There is a problem in that it remains without being removed, and in some cases, C and the like are removed only up to the saturation dissolution amount. When such inclusions enter the unidirectional solidification cell in the next step, which is continuous with the electron beam melting, the amount of cut and removed of the unidirectionally solidified ingot increases, and the yield decreases.

【0005】本発明はこのような電子ビーム溶解におけ
る不純物介在物を効果的に除去し、後段のシリコン精製
工程の効率化を図ると共に、製品の歩留りの向上を図る
ことを目的とする。
It is an object of the present invention to effectively remove such impurity inclusions in the electron beam melting to improve the efficiency of the subsequent silicon refining process and to improve the product yield.

【0006】[0006]

【課題を解決するための手段】本発明は、上記目的を達
成するためになされたもので、電子ビーム溶解にてシリ
コンの精製を行うに当り、溶解部にフィルタを設け、溶
融シリコンを濾過することを特徴とするシリコンの精製
方法である。本発明では溶融シリコンの表面付近のみで
なく、溶融シリコンの断面全域にフィルタを設置する。
DISCLOSURE OF THE INVENTION The present invention has been made to achieve the above-mentioned object. In purifying silicon by electron beam melting, a filter is provided in a melting part to filter molten silicon. This is a method for purifying silicon. In the present invention, the filter is installed not only near the surface of the molten silicon but also over the entire cross section of the molten silicon.

【0007】フィルタとしては、高温、高真空で安定し
ており、シリコンへの溶解量が少ない材料が適切であ
る。例えば炭素、炭化珪素は、高温、高真空で安定であ
り、溶融シリコンへの溶解量も100ppm程度であ
り、酸化除去し易いので適当である。また、炭素、炭化
珪素は電子ビームを直接照射しても溶損することなくシ
リコンの汚染も問題とならない。
As the filter, a material which is stable at high temperature and high vacuum and has a small amount of dissolved in silicon is suitable. For example, carbon and silicon carbide are suitable because they are stable at high temperatures and high vacuums, dissolve in molten silicon at about 100 ppm, and are easily oxidized and removed. In addition, carbon and silicon carbide are not melted even if the electron beam is directly irradiated, and there is no problem of silicon contamination.

【0008】[0008]

【発明の実施の形態】本発明は電子ビームの溶解を行う
ハース内にフィルタを設け、不純物介在物の流出を防止
する。フィルタとしては、炭素又は炭化珪素を主成分と
し、粒状体、球状体、管状体又は不定形のラッシヒリン
グ、等を用いることができ、これらを吹き付けた板状の
形状のフィルタが望ましい。
DESCRIPTION OF THE PREFERRED EMBODIMENTS According to the present invention, a filter is provided in a hearth for dissolving an electron beam to prevent outflow of impurity inclusions. As the filter, a granular body, a spherical body, a tubular body, an irregular Raschig ring, or the like containing carbon or silicon carbide as a main component can be used.

【0009】なお、フィルタ材についてもシリコンへの
汚染防止のため高い純度であることが望まれる。図2に
従来例を示し、図1に実施例の断面図を示した。ハース
1に原料シリコン3が供給され、図示省略した電子ビー
ムによりこれを溶解する。従来は介在物5はハース1か
ら流出する溶融シリコンと共に次の工程の鋳型又は坩堝
11に移される。
It is desired that the filter material has a high purity to prevent contamination of silicon. FIG. 2 shows a conventional example, and FIG. 1 shows a sectional view of the embodiment. The raw material silicon 3 is supplied to the hearth 1 and is melted by an electron beam not shown. Conventionally, the inclusions 5 are transferred together with the molten silicon flowing out of the hearth 1 to the mold or crucible 11 in the next step.

【0010】従来はハース1から流出する溶融シリコン
6と共に介在物5も流出し、次工程の鋳型又は坩堝11
内に入る。そして、これらの介在物は、固体シリコン1
3中に取込まれるか又は溶融シリコン12と共にさらに
次の工程に移行する。また鋳型又は坩堝11内壁に生成
するスカル14も後流工程へ移行することがある。図1
に示す実施例ではハース1内にフィルタ4を設け、介在
物をここで捕護する。フィルタ4としては純度の高いS
iCの焼結フィルタを用いた。介在物はこのフィルタに
捕えられ、溶融シリコンはこれを通過する。
Conventionally, the inclusions 5 also flow out together with the molten silicon 6 flowing out of the hearth 1, and the mold or crucible 11
Get in. And these inclusions are solid silicon 1
3 or move to the next step together with the molten silicon 12. Also, the skull 14 generated on the inner wall of the mold or crucible 11 may shift to the downstream process. FIG.
In the embodiment shown in (1), a filter 4 is provided in the hearth 1, and inclusions are captured here. High purity S for filter 4
An iC sintered filter was used. Inclusions are trapped in the filter and the molten silicon passes through it.

【0011】[0011]

【発明の効果】本発明によれば、電子ビーム溶解におけ
る溶解部にフィルタを設け、不純物介在物を効果的に除
去し、後流のシリコン精製工程の効率化を図ると共に、
製品の歩留りの向上を図ることが可能となった。
According to the present invention, a filter is provided in a melting portion in electron beam melting to effectively remove impurity inclusions, thereby improving the efficiency of the downstream silicon purification step, and
It has become possible to improve the yield of products.

【図面の簡単な説明】[Brief description of the drawings]

【図1】実施例のシリコンの電子ビーム溶解ハースの断
面図である。
FIG. 1 is a sectional view of an electron beam melting hearth of silicon according to an embodiment.

【図2】従来例のシリコンの電子ビーム溶解ハースの断
面図である。
FIG. 2 is a sectional view of a conventional silicon electron beam melting hearth.

【符号の説明】[Explanation of symbols]

1 ハース 2 溶融シリコン 3 原料シリコン 4 フィルタ 5 介在物 6 流出する溶融シリコン 11 鋳型又は坩堝 12 溶融シリコン 13 固体シリコン 14 スカル Reference Signs List 1 hearth 2 molten silicon 3 raw material silicon 4 filter 5 inclusion 6 molten silicon flowing out 11 mold or crucible 12 molten silicon 13 solid silicon 14 skull

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 電子ビーム溶解にてシリコンの精製を行
うに当り、溶解部にフィルタを設け、溶融シリコンを濾
過することを特徴とするシリコンの精製方法。
1. A method for purifying silicon, comprising the steps of: providing a filter in a melting section and filtering molten silicon when purifying silicon by electron beam melting.
JP8328451A 1996-12-09 1996-12-09 Purification of silicon Withdrawn JPH10167716A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP8328451A JPH10167716A (en) 1996-12-09 1996-12-09 Purification of silicon

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP8328451A JPH10167716A (en) 1996-12-09 1996-12-09 Purification of silicon

Publications (1)

Publication Number Publication Date
JPH10167716A true JPH10167716A (en) 1998-06-23

Family

ID=18210426

Family Applications (1)

Application Number Title Priority Date Filing Date
JP8328451A Withdrawn JPH10167716A (en) 1996-12-09 1996-12-09 Purification of silicon

Country Status (1)

Country Link
JP (1) JPH10167716A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013132651A1 (en) 2012-03-09 2013-09-12 新日鉄マテリアルズ株式会社 Silicon refining device
KR101426015B1 (en) * 2008-09-05 2014-08-06 상뜨로 나쇼날 드 라 러쉐르쉐 샹띠피크 Material having a multilayer architecture and intended for being contacted with liquid silicon
CN104649277A (en) * 2013-11-22 2015-05-27 青岛隆盛晶硅科技有限公司 Method for removal of impurity oxygen from polycrystalline silicon ingot base material by electron beam melting
US9783426B2 (en) 2015-10-09 2017-10-10 Milwaukee Silicon Llc Purified silicon, devices and systems for producing same

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101426015B1 (en) * 2008-09-05 2014-08-06 상뜨로 나쇼날 드 라 러쉐르쉐 샹띠피크 Material having a multilayer architecture and intended for being contacted with liquid silicon
WO2013132651A1 (en) 2012-03-09 2013-09-12 新日鉄マテリアルズ株式会社 Silicon refining device
CN104649277A (en) * 2013-11-22 2015-05-27 青岛隆盛晶硅科技有限公司 Method for removal of impurity oxygen from polycrystalline silicon ingot base material by electron beam melting
US9783426B2 (en) 2015-10-09 2017-10-10 Milwaukee Silicon Llc Purified silicon, devices and systems for producing same
US9802827B2 (en) 2015-10-09 2017-10-31 Milwaukee Silicon, Llc Purified silicon, devices and systems for producing same
US10093546B2 (en) 2015-10-09 2018-10-09 Milwaukee Silicon Llc Purified silicon, devices and systems for producing same

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