JP2000247623A - Method and apparatus for purifying silicon - Google Patents
Method and apparatus for purifying siliconInfo
- Publication number
- JP2000247623A JP2000247623A JP11045960A JP4596099A JP2000247623A JP 2000247623 A JP2000247623 A JP 2000247623A JP 11045960 A JP11045960 A JP 11045960A JP 4596099 A JP4596099 A JP 4596099A JP 2000247623 A JP2000247623 A JP 2000247623A
- Authority
- JP
- Japan
- Prior art keywords
- silicon
- graphite
- melting
- electron beam
- vapor deposition
- 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.)
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Abstract
(57)【要約】
【課題】 シリコンを電子ビーム溶解するに当たり、蒸
着物の落下による汚染を防止し、安定的かつ容易に高純
度な太陽電池用シリコンを得る。
【解決手段】 シリコンを加熱溶解する容器の溶湯表面
積より大きい面積を有し、嵩密度１．７ｇ／ｃｍ3以上
の黒鉛からなる黒鉛製蒸着板を容器の上方を覆って固定
し、この蒸着板に蒸着物を付着保持させつつ電子ビーム
溶解する。
(57) [Problem] To dissolve silicon by electron beam melting, prevent contamination by falling of a deposit, and stably and easily obtain high-purity silicon for solar cells. SOLUTION: A vapor deposition plate made of graphite having an area larger than a surface area of a molten metal of a container for heating and melting silicon and having a bulk density of 1.7 g / cm 3 or more is fixed by covering the upper part of the container. Electron beam melting is performed while depositing and holding the deposited material.
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、シリコンの精製に
関し、とりわけ電子ビーム溶解時の不純物除去効果を高
め、高純度のシリコンが得られるように工夫されたシリ
コンの精製方法および装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to silicon purification, and more particularly to a silicon purification method and apparatus designed to enhance the effect of removing impurities during electron beam melting and obtain high-purity silicon.
【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
陽光発電がエネルギー源として脚光を浴び、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
最も汎用されやすい材料であり、しかも、動力用電力供
給に使われる材料としてシリコンが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 as an energy source due to the demand for diversification of energy sources, and research and development are being actively conducted for practical use of low-cost power generation devices. Under such circumstances, silicon is the most commonly used material as a solar cell material, and silicon 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
の純度は、９９．９９９９％（６Ｎ）以上が必要とされ
ている。従来、市販のシリコン（純度９９．５％）から
上記高純度シリコンを製造するには、Ａｌ、Ｆｅ、Ｔｉ
等の金属不純物元素については固液分配係数の小さいこ
とを利用した一方向凝固精製により除去し、Ｂについて
はＨ2Ｏ、ＣＯ2あるいはＯ2を添加したＡｒプラズマ溶
解により除去する技術が提案されている。[0003] The purity of silicon used as a solar cell raw material is required to be 99.9999% (6N) or more. Conventionally, to produce the high-purity silicon from commercially available silicon (purity 99.5%), Al, Fe, Ti
A technique has been proposed in which metal impurity elements such as are removed by unidirectional solidification purification utilizing the small solid-liquid partition coefficient, and B is removed by Ar plasma dissolution with addition of H 2 O, CO 2 or O 2. ing.
【０００４】一方、最近、電子ビーム溶解により市販の
シリコン中のＰ、Ｃａ、Ａｌ、Ｃ、Ｂの同時除去が可能
であることが報告されており、（ＩＳＩＪ Ｉｎｔｅｒ
ｎａｔｉｏｎａｌ，ｖｏｌ．３２（１９９２）．Ｎｏ．
５ ｐ６３５−６４２）、上記製造工程の簡略化、およ
び効率化が期待されている。電子ビーム溶解法では、り
ん、カルシウム、アルミニウム等の不純物を多量含有す
る蒸発シリコンが炉体天井部に多量蒸着するため、それ
らの落下混入による汚染が品質のバラツキや不純物の除
去速度の低下をもたらし、大きな問題となっていた。そ
こで、本発明者らは特開平７−３０９６１４号公報にて
ステンレス薄板等を移動させながら電子ビーム溶解を行
い蒸着物の落下を防ぐ技術を開示した。On the other hand, it has recently been reported that the simultaneous removal of P, Ca, Al, C, and B in commercially available silicon by electron beam melting is possible.
national, vol. 32 (1992). No.
5 p635-642), and simplification of the above-mentioned manufacturing process and efficiency improvement are expected. In the electron beam melting method, a large amount of evaporated silicon containing impurities such as phosphorus, calcium, and aluminum is deposited on the ceiling of the furnace body, and contamination due to the dropping of the silicon causes variations in quality and a reduction in the removal rate of impurities. Was a big problem. In view of this, the present inventors have disclosed in JP-A-7-309614 a technique for preventing a fall of a deposit by performing electron beam melting while moving a stainless steel plate or the like.
【０００５】しかしながら、ステンレス薄板を大型化し
た場合、炉内の圧力上昇時に時々生じる電子ビームの突
発的な停止や冷却時等に蒸着物が落下することがあり、
太陽電池用シリコンに要求される純度を実生産レベルで
安定して得るためには、蒸着物の落下防止に関する検討
は十分であるとはいえなかった。[0005] However, when the stainless steel sheet is made large, the deposit may fall when the electron beam suddenly stops or cools, which sometimes occurs when the pressure inside the furnace increases.
In order to stably obtain the purity required for silicon for solar cells at the actual production level, studies on preventing falling of the deposits have not been sufficient.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、このような
従来技術の現状に鑑みて、電子ビーム溶解による不純物
の蒸発除去なる利点を活かしてこれを加熱源とし、更に
電子ビーム溶解中の蒸着物の落下による汚染を徹底的に
防止することにより、安定的かつ容易に高純度な太陽電
池用シリコンを得る技術を提供することを目的とするも
のである。SUMMARY OF THE INVENTION In view of the above-mentioned state of the art, the present invention takes advantage of the fact that impurities are removed by evaporation by electron beam melting, and uses this as a heating source. It is an object of the present invention to provide a technique for stably and easily obtaining high-purity silicon for solar cells by thoroughly preventing contamination due to falling objects.
【０００７】[0007]
【課題を解決するための手段】本発明は、前記問題点を
解決するために開発されたもので、蒸着物からの溶融シ
リコンへの汚染を防ぐことを特徴とするものである。SUMMARY OF THE INVENTION The present invention has been developed to solve the above-mentioned problems, and is characterized in that contamination of molten silicon from a deposit is prevented.
【０００８】すなわち、本発明は、シリコンを電子ビー
ム溶解するに当たり、シリコンを加熱溶解する保持容器
の溶湯表面積より大きい黒鉛製蒸着板を容器の上方を覆
って固定し、この蒸着板に蒸着物を付着保持させつつ電
子ビーム溶解することを特徴とするシリコンの精製方法
である。黒鉛製蒸着板を用いるのは、蒸着物を付着保持
する能力に優れているからであり、これを固定するのは
蒸着物が落下するのを防止するためである。That is, according to the present invention, when melting silicon by electron beam, a graphite vapor deposition plate larger than the surface area of the molten metal of a holding vessel for heating and melting silicon is fixed by covering the upper part of the vessel, and the deposit is deposited on the vapor deposition plate. This is a method for purifying silicon, which comprises melting an electron beam while adhering and holding. The reason why the graphite vapor deposition plate is used is that the vapor deposition material has an excellent ability to adhere and hold the vapor deposition material, and is fixed to prevent the vapor deposition material from dropping.
【０００９】本発明は、加熱源が清浄な電子ビームであ
り、雰囲気が高真空である等の電子ビーム溶解の利点を
最大限に生かし、溶解中に発生する不純物を多量含有す
る蒸着物が再びシリコン溶湯中に落下して汚染するのを
防止すれば、シリコンの高純度化を安定的かつ容易に図
ることができるとの考えによって完成されたものであ
る。The present invention makes the most of the advantages of electron beam melting such that the heating source is a clean electron beam and the atmosphere is in a high vacuum. The present invention has been completed based on the idea that the prevention of contamination by dropping into the silicon melt can stably and easily purify silicon.
【００１０】本発明者らは、上述したような蒸着板の大
型化時の蒸着物の落下は、（１）電子ビーム溶解中の電
子ビームの突発的な停止時等に生じる温度変化による蒸
着板の変形、（２）蒸着板の材質とシリコンとの熱膨張
率の大きな差等に主原因があると考え、さらにこれらに
加え、（３）蒸着板の材質は蒸着板自身が高真空中で加
熱されるため、ガス成分の発生による炉内の圧力変動や
シリコンへの汚染のないものとする、（４）蒸着板は太
陽電池用シリコンを安価に大量生産することを考慮する
と、長時間・多数回使用可能であるものとする、との考
えに基づき鋭意研究を行ったところ溶解容器の上方部を
面積が容器の表面積以上である嵩密度１．７ｇ／ｃｍ3
以上の黒鉛製蒸着板を使用すれば上記問題を解決できる
ことを知見した。The inventors of the present invention have found that, as described above, when the vapor deposition plate is increased in size, the vapor deposition material falls due to (1) a temperature change that occurs when the electron beam suddenly stops during melting of the electron beam. It is thought that the main causes are the deformation of (2) the thermal expansion coefficient between the material of the vapor deposition plate and silicon, etc. In addition to these factors, (3) the material of the vapor deposition plate itself is in a high vacuum. Since it is heated, there is no pressure fluctuation in the furnace due to the generation of gas components and no contamination of silicon. (4) Considering that the vapor deposition plate is inexpensive and mass-producing silicon for solar cells, After extensive research based on the idea that it can be used many times, a bulk density of 1.7 g / cm 3 where the area of the upper part of the dissolving vessel is equal to or larger than the surface area of the vessel is obtained.
It has been found that the above problem can be solved by using the above-mentioned graphite vapor deposition plate.
【００１１】ここで、蒸着板は、溶解容器上方部の溶湯
表面積以上の面積をカバーできるものとする。なぜなら
ば、容器上方に不純物を多量に含有する蒸着物が天井に
蒸着し、その蒸着物が溶融したシリコンに落下するた
め、シリコンへの不純物の汚染が避けられないのでこれ
を防止するためである。Here, it is assumed that the vapor deposition plate can cover an area larger than the surface area of the molten metal in the upper part of the melting vessel. This is because, since a deposit containing a large amount of impurities is deposited on the ceiling above the container and the deposited material falls on the molten silicon, contamination of the impurities into the silicon is unavoidable. .
【００１２】ここで、蒸着物を捕捉する蒸着板の材質は
黒鉛とする。なぜならば、黒鉛は、（ａ）上記温度変化
による変形がほとんどない、（ｂ）使用温度領域での熱
膨張率がシリコンとほぼ同等である、（ｃ）炭素は溶融
シリコン中の飽和溶解量が１０〜１００ｐｐｍｗ程度と
非常に低いため溶融シリコンへの汚染がほとんどない、
（ｄ）シリコンと反応して炉体・電子銃内等の圧力低下
をもたらす気体が発生することがない、（ｅ）高融点物
質に比べて安価である、等の優れた特徴を有するためで
ある。Here, the material of the vapor deposition plate for capturing the vapor deposition material is graphite. This is because graphite has (a) almost no deformation due to the above temperature change, (b) a coefficient of thermal expansion in the operating temperature range is almost equal to that of silicon, and (c) carbon has a saturated dissolved amount in molten silicon. There is almost no contamination to molten silicon because it is very low, about 10 to 100 ppmw,
(D) It does not generate a gas that causes a pressure drop in a furnace body or an electron gun due to reaction with silicon, and (e) it is excellent in that it is inexpensive as compared with a high melting point material. is there.
【００１３】また、黒鉛製蒸着板の嵩密度は１．７ｇ／
ｃｍ3以上であることが望ましい。なぜならば、嵩密度
が１．７ｇ／ｃｍ3未満の黒鉛を使用した場合、黒鉛自
身の強度が不足し多量の蒸着物の付着時、あるいは蒸着
板を再利用するための蒸着物剥離時等に黒鉛板が破損す
る可能性が高いためである。加えて、多量の蒸着物の付
着時に蒸着物が落下することも多い。このような場合、
使用黒鉛板量の増加によるコストアップ、品質のバラツ
キや低下を招いてしまう。黒鉛板の表面性状は低密度な
多孔質の方が密着性を考慮するとよいと考えられ易い
が、黒鉛とシリコン蒸着物界面の観察結果も併せて考え
ると、蒸着物の蒸着板への付着は微小な原子の集合によ
り行われているため、黒鉛板の表面を鏡面研磨でもしな
い限り良好な付着能力が得られる。また、上述したよう
に黒鉛板の繰り返し利用を考慮した場合、蒸着物の剥離
作業も容易であり、このときの黒鉛の破壊もほとんど発
生しない。The bulk density of the graphite vapor deposition plate is 1.7 g /
cm 3 or more is desirable. This is because when graphite having a bulk density of less than 1.7 g / cm 3 is used, the strength of the graphite itself is insufficient and a large amount of deposits are adhered, or when deposits are peeled off to reuse a deposition plate. This is because there is a high possibility that the graphite plate will be damaged. In addition, the deposit often drops when a large amount of the deposit is attached. In such a case,
An increase in the amount of graphite plate used leads to an increase in cost and a variation or decrease in quality. It is easy to think that the low-density porous surface properties of the graphite plate should be considered in consideration of the adhesion, but also considering the observation results of the graphite-silicon deposit interface, the adhesion of the deposit on the deposit plate is considered. Since it is performed by the aggregation of minute atoms, good adhesion ability can be obtained unless the surface of the graphite plate is mirror-polished. In addition, when the repeated use of the graphite plate is considered as described above, the work of peeling off the deposited material is easy, and the graphite is hardly broken at this time.
【００１４】[0014]
【発明の実施の形態】本発明で使用される電子ビーム溶
解装置１の一例を示す概略図を図１に示す。原料供給装
置２から３０ｋｇ／ｈの供給速度で連続的に供給された
原料シリコン３を、炉体１５内に設けた内寸１０００ｍ
ｍ×１０００ｍｍ、深さ１００ｍｍの水冷銅ハース４内
で電子銃５から６００ｋＷの電子ビーム６を加熱源とし
て溶解、気化精製した。ついで、オーバーフローした溶
融シリコン７を内寸直径φ６００ｍｍ、深さ５００ｍｍ
の水冷銅ルツボ１０内に半連続的に供給し、ルツボ上方
に配置された電子銃１１から６００ｋＷの電子ビーム１
２を照射しながらインゴット１３の高さが１５０ｍｍと
なるまで一方向凝固を行った。黒鉛製蒸着板２０は嵩密
度が１．７４ｇ／ｃｍ3以上、厚み１０ｍｍである黒鉛
板を使用し、水冷銅ハース４、水冷銅ルツボ１０の両者
をカバーする形で上方に配置した。比較例として黒鉛製
蒸着板に代わりステンレス蒸着板を用いた実験も行っ
た。FIG. 1 is a schematic view showing an example of an electron beam melting apparatus 1 used in the present invention. The raw material silicon 3 continuously supplied at a supply speed of 30 kg / h from the raw material supply device 2 is supplied to a furnace body 15 having an inner size of 1000 m.
In a water-cooled copper hearth 4 having a size of mx 1000 mm and a depth of 100 mm, melting and vaporization and purification were performed using an electron beam 6 of 600 kW from an electron gun 5 as a heating source. Then, the overflowed molten silicon 7 was prepared with an inner diameter of φ600 mm and a depth of 500 mm.
Is supplied semi-continuously into a water-cooled copper crucible 10 and an electron beam 1 of 600 kW is supplied from an electron gun 11 disposed above the crucible.
While irradiating No. 2, unidirectional solidification was performed until the height of the ingot 13 became 150 mm. The graphite vapor deposition plate 20 was a graphite plate having a bulk density of 1.74 g / cm 3 or more and a thickness of 10 mm, and was disposed above the water-cooled copper hearth 4 and the water-cooled copper crucible 10 so as to cover both. As a comparative example, an experiment using a stainless steel evaporated plate instead of the graphite evaporated plate was also performed.
【００１５】以上の条件で得られたシリコンインゴット
中心部における高さ方向のりん濃度をＩＣＰ（Ｉｎｄｕ
ｃｔｉｖｅｌｙ Ｃｏｕｐｌｅｄ Ｐｌａｓｍａ）発光
分析法により分析した。分析サンプルとしては、インゴ
ット中心部の底部から高さ方向に１０ｍｍきざみで５０
×１０×１０ｍｍのシリコン塊を１５個切り出したもの
を用いた。上述の方法で得たＰの分析結果を図２に示
す。図中では、高さ０〜１０ｍｍのサンプルの分析結果
を高さ５ｍｍの位置にプロットした。ここで、同様に原
料シリコン、蒸着シリコン中のりん濃度の分析も行った
結果、それぞれ約３０ｐｐｍｗ、約１５０ｐｐｍｗであ
った。黒鉛製蒸着板を用いた実施例では、シリコン中の
りん濃度は安定しており、溶解中の蒸着物の落下も観察
されなかった。一方、比較例として示したステンレス板
を蒸着板として使用した場合では、分析結果のバラツキ
が非常に大きく、溶解中の観察においても蒸着物の落下
がみられることがわかった。溶解後の炉内観察では、黒
鉛製蒸着板では板の反りも見られず、蒸着シリコンは黒
鉛製蒸着板に捕捉されていた。これに対し、ステンレス
板では板の反りが見られ、蒸着シリコンが落下した痕跡
も観察された。また、黒鉛製蒸着物を再利用するため
の、蒸着シリコンの剥離作業では黒鉛の破損もなく容易
に剥離することができた。ここでは、りんについて述べ
たがアルミニウム、カルシウム等の易揮発性不純物につ
いても同様の傾向が見られた。The phosphorus concentration in the height direction at the center of the silicon ingot obtained under the above conditions is determined by ICP (Indu
(Ctively Coupled Plasma) emission spectrometry. As an analysis sample, 50 in 10 mm increments from the bottom of the center of the ingot in the height direction.
A piece obtained by cutting out 15 silicon chunks of 10 x 10 mm was used. FIG. 2 shows the analysis results of P obtained by the above-described method. In the figure, the analysis result of the sample having a height of 0 to 10 mm is plotted at a position of a height of 5 mm. Here, the analysis of the phosphorus concentration in the raw material silicon and the vapor deposition silicon was also performed, and as a result, they were about 30 ppmw and about 150 ppmw, respectively. In the example using the graphite vapor deposition plate, the phosphorus concentration in silicon was stable, and no drop of the vapor during melting was observed. On the other hand, when the stainless steel plate shown as the comparative example was used as the vapor deposition plate, the analysis results showed a large variation, and it was found that the vapor deposition dropped even during observation during melting. In the furnace observation after melting, no warpage of the graphite vapor deposition plate was observed, and the vapor deposited silicon was captured by the graphite vapor deposition plate. On the other hand, in the case of the stainless steel plate, warpage of the plate was observed, and traces of the deposited silicon dropped were also observed. Moreover, in the stripping operation of the deposited silicon to reuse the graphite deposit, the graphite could be easily separated without damage. Although phosphorus has been described here, a similar tendency was observed for easily volatile impurities such as aluminum and calcium.
【００１６】以上の結果より、本発明を用いればシリコ
ンの高純度化が安定的かつ容易に図られることが明らか
になった。From the above results, it has been clarified that the use of the present invention enables stable and easy purification of silicon.
【００１７】[0017]
【発明の効果】本発明は、シリコンを電子ビーム溶解す
るに当たり、蒸着物からの溶融シリコンへの汚染を防ぐ
ようにしたからシリコンの更なる高純度化が図れ、安定
的かつ容易に高純度なシリコンが得られるようになっ
た。According to the present invention, when silicon is melted with an electron beam, contamination of molten silicon from vapor deposition is prevented, so that the silicon can be further purified, and the silicon can be stably and easily purified. Silicon can now be obtained.
【図１】電子ビーム溶解装置の概略図である。FIG. 1 is a schematic view of an electron beam melting apparatus.
【図２】シリコンインゴット中のりん濃度分布を示すグ
ラフである。FIG. 2 is a graph showing a phosphorus concentration distribution in a silicon ingot.
１ 電子ビーム溶解装置 ２ 原料供給装置 ３ 原料シリコン ４ 水冷銅ハース ５ 電子銃 ６ 電子ビーム ７ 溶融シリコン １０ 水冷銅ルツボ １１ 電子銃 １２ 電子ビーム １３ インゴット １４ 溶湯 １５ 炉体 ２０ 黒鉛製蒸着板 DESCRIPTION OF SYMBOLS 1 Electron beam melting apparatus 2 Raw material supply apparatus 3 Raw material silicon 4 Water-cooled copper hearth 5 Electron gun 6 Electron beam 7 Fused silicon 10 Water-cooled copper crucible 11 Electron gun 12 Electron beam 13 Ingot 14 Molten metal 15 Furnace body 20 Graphite deposition plate
───────────────────────────────────────────────────── フロントページの続き (72)発明者 永瀬 彰博 岡山県倉敷市水島川崎通１丁目（番地な し） 川崎製鉄株式会社水島製鉄所内 (72)発明者 松尾 謙一郎 岡山県倉敷市水島川崎通１丁目（番地な し） 川崎製鉄株式会社水島製鉄所内 Ｆターム(参考） 4G072 AA01 BB01 GG03 GG04 GG05 MM08 NN02 RR30 UU02 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Akihiro Nagase 1-chome, Mizushima-Kawasaki-dori, Kurashiki-shi, Okayama Pref. Chome (without address) Mizushima Works, Kawasaki Steel F-term (reference) 4G072 AA01 BB01 GG03 GG04 GG05 MM08 NN02 RR30 UU02
Claims (3)
り、シリコンを加熱溶解する保持容器の溶湯表面積より
大きい黒鉛製蒸着板を容器の上方を覆って固定し、該蒸
着板に蒸着物を付着保持させつつ電子ビーム溶解するこ
とを特徴とするシリコンの精製方法。When melting silicon by electron beam melting, a graphite vapor deposition plate having a surface area larger than the molten metal surface of a holding container for heating and melting silicon is fixed over the upper part of the container, and the deposition material is adhered and held on the vapor deposition plate. A method for purifying silicon, comprising performing electron beam melting.
ｍ3以上の黒鉛からなることを特徴とする請求項１記載
のシリコンの精製方法。2. The graphite vapor deposition plate has a bulk density of 1.7 g / c.
method for purifying silicon according to claim 1, characterized in that it consists of m 3 or more graphite.
精製装置において、シリコンを加熱溶解する保持容器の
溶湯表面積よりきい大きい黒鉛製蒸着板を容器の上方を
覆って配設固定したことを特徴とするシリコンの精製装
置。3. A silicon refining apparatus for melting silicon by electron beam, wherein a graphite deposition plate having a size larger than a surface area of a molten metal of a holding container for heating and melting silicon is disposed and fixed over the upper part of the container. Purification equipment.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11045960A JP2000247623A (en) | 1999-02-24 | 1999-02-24 | Method and apparatus for purifying silicon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11045960A JP2000247623A (en) | 1999-02-24 | 1999-02-24 | Method and apparatus for purifying silicon |
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|---|---|
| JP2000247623A true JP2000247623A (en) | 2000-09-12 |
Family
ID=12733834
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| JP (1) | JP2000247623A (en) |
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