JP2000247623A - Method for refining silicon and apparatus therefor - Google Patents

Method for refining silicon and apparatus therefor

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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
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Prior art keywords
silicon
electron beam
graphite
vapor deposition
plate
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Inventor
Kazuhiro Hanazawa
Yoshihide Kato
Kenichiro Matsuo
Akihiro Nagase
嘉英 加藤
謙一郎 松尾
彰博 永瀬
和浩 花澤
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Kawasaki Steel Corp
川崎製鉄株式会社
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Abstract

PROBLEM TO BE SOLVED: To prevent the contamination by the drops of vapor depositions and to stably and easily obtain high-purity silicon by fixing a graphite vapor deposition plate larger than a silicon molten metal surface area so as to provide a covering above a vessel and subjecting the silicon to electron beam dissolution while adhering and holding the vapor deposition matter on this vapor deposition plate. SOLUTION: The raw material silicon 3 supplied from a raw material supply device 2 of an electron beam dissolution apparatus 1 is dissolved, vaporized and refined by using the electron beam 6 from an electron gun 5 in a water-cooled copper hearth 4 disposed in a furnace casing 15. The overflowing molten silicon 7 is then semicontinuously supplied into a water cooled copper crucible 10 and while the silicon is irradiated with the electron beam 12 from the electron gun 11 above the crucible, an ingot 13 is unidirectionally solidified. The vapor deposition plate 20 made of graphite formed by using a graphite plate of >=1.74 g/cm3 bulk density and 10 mm in thickness is disposed above the water-cooled copper hearth 4 and the water cooled copper crucible 10 in the form of covering the silicon melt in both thereof. The vapor deposition matter is adhered and held on this plate, by which the contamination by the fall of the vapor deposition matter is prevented.

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、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。 The present invention relates to relates to the purification of silicon, especially enhances the impurity removal effect during electron beam melting, relates to the purification method and device of silicon high purity silicon has been devised so as to obtain.

【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。 The limelight as an energy source is solar power from the request of the diversification of the Prior Art In recent years energy sources, research and development for practical use of low-cost power generation apparatus has been actively carried out. 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。 Under such circumstances, silicon is likely to be the most generic material, moreover, silicon is the most important as a material used for power for power supply as a raw material for solar cells.

【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。 [0003] The purity of silicon used as a raw material for solar cells is required 99.9999% (6N) or more. 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 Conventionally, the production of the high purity silicon from commercially available silicon (purity 99.5%) is, 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H 2 O、CO 2あるいはO 2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。 Was removed by unidirectional solidification purified using it small solid-liquid distribution coefficient for the metal impurity elements etc., a technique for removing by Ar plasma melting with the addition of H 2 O, CO 2 or O 2 have been proposed for B 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 On the other hand, recently, it has been reported that the electron beam melting is possible P in commercial silicon, Ca, Al, C, simultaneous removal of B, (ISIJ Inter
national,vol. national, vol. 32(1992). 32 (1992). No. 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。 5 p635-642), simplification of the manufacturing process, and the efficiency is expected. 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。 The electron beam melting method, phosphorus, calcium, the impurity a large amount containing vaporized silicon to aluminum such as a large amount deposited furnace ceiling, contamination by their falling contamination leads to reduction in the removal rate of quality variations and impurities , it has been a major problem. 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。 Accordingly, the present inventors have disclosed a technique for preventing the falling of the deposit performed electron beam melting while moving the stainless steel sheet or the like in Japanese Unexamined 7-309614 JP.

【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、 However, when the size of the stainless steel sheet, may sudden stop or deposit in the cooling or the like sometimes occur electron beam when the pressure rises in the furnace falls,
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。 In order to be able to stabilize the purity required for silicon for solar cells in actual production levels, Study fall prevention of the deposit was not said to be 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 It is an object of the present invention, in view of the current state of the prior art, which was a heat source by utilizing the advantage that the evaporation the removal of impurities by electron beam melting, further deposition in an electron beam melting by thoroughly prevent contamination due to falling of an object, it is an object to provide a technique to obtain a stable and readily silicon for high purity solar cell.

【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。 The present invention SUMMARY OF] has been developed to solve the above problems, it is characterized in that to prevent contamination of the molten silicon from the deposit.

【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。 Namely, the present invention is a silicon Upon electron beam melting, the graphite deposition plate larger than the molten metal surface area of ​​the holding container for heating and melting the silicon and secured over the top of the container, the deposit on the deposition plate while adhering holding a method for purifying silicon, characterized in that the electron beam melting. 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。 To use a graphite deposition plate is because an excellent ability to adhere retain deposits, is to prevent the deposit from falling to fix this.

【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, heat source is clean electron beam, taking advantage of electron beam melting of equal atmosphere is a high vacuum maximally, deposit a large amount containing impurities generated during the dissolution again if prevent contamination to fall into the silicon melt, it has been completed by the belief that the purity of the silicon can be achieved stably and easily.

【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/cm 3 [0010] The present inventors have found that falling of deposit at the time of enlargement of the deposition plate as described above, (1) the deposition plate due to temperature changes that occur in sudden stop or the like of the electron beam in the electron beam melting deformation, (2) considered to have thermal expansion coefficient primary cause large differentially in the material and the silicon deposition plate, further in addition to these, (3) the material of the deposition plate is deposited plate itself in high vacuum to be heated, and having no contamination of the pressure fluctuations and the silicon in the furnace due to the generation of gas components, considering the (4) deposition plate to inexpensively mass produce solar silicon, long- shall many times can be used, the upper part of the extensive dissolution vessels was studied based on the idea that it measures more than the surface area of the container the bulk density 1.7 g / cm 3
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。 Using the above graphite deposition plate was found that can solve the above problems.

【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。 [0011] Here, the deposition plate is assumed to cover the molten metal surface over the area of ​​the melting vessel upper portion. 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。 Because deposits containing impurities in a large amount is deposited on the ceiling to the container upwards, to fall into the silicon where the deposit is melted, it is to prevent this since contamination of impurities into the silicon can not be avoided .

【0012】ここで、蒸着物を捕捉する蒸着板の材質は黒鉛とする。 [0012] Here, the material of the deposition plate to capture deposit is graphite. 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、 Because graphite, (a) there is little deformation by the change in temperature, (b) the coefficient of thermal expansion in the use temperature range is substantially equal to the silicon, carbon saturation dissolution amount of the molten silicon (c) there is little contamination of the molten silicon for very low and about 10~100ppmw,
(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。 (D) gas resulting in pressure drop by reacting with silicon or the like furnace body, an electron gun in does not occur, in order to have a cheap and is excellent characteristics etc. as compared to (e) a refractory material is there.

【0013】また、黒鉛製蒸着板の嵩密度は1.7g/ [0013] In addition, the bulk density of the graphite deposition plate is 1.7g /
cm 3以上であることが望ましい。 It is desirably cm 3 or more. なぜならば、嵩密度が1.7g/cm 3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。 This is because, if the bulk density were used graphite less than 1.7 g / cm 3, when deposition of a large amount of deposit strength of the graphite itself is insufficient, or the deposition plate upon deposit peeling for recycling, etc. there is a high possibility that the graphite plate is damaged. 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。 In addition, the deposit during deposition of a large amount of deposit is often dropped. このような場合、 In such a case,
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。 Cost due to increased use graphite plate amount, which leads to variations and lower quality. 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。 Surface properties of the graphite plate is easily considered good towards low-density porous to consider the adhesiveness, when considering the graphite and silicon deposit surface observation results together, adhering to the deposition plate of the deposit is because it is made by a set of small atomic, good adhesion ability can be obtained as long as the surface of the graphite plate is not in mirror polishing. 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。 Further, in consideration of reuse of the graphite plate as described above, it is easy to peel work deposit, hardly occur even destruction of the graphite 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。 A schematic diagram showing an example of electron beam melting device 1 used in the Detailed Description of the Invention The present invention is shown in FIG. 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 The material silicon 3 from the raw material supply unit 2 is continuously supplied at a feed rate of 30kg / h, provided the furnace body 15 inner dimensions 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。 m × 1000 mm, dissolved from the electron gun 5 in a water-cooled copper hearth within 4 depth 100mm electron beam 6 of 600kW as a heat source, the vaporized purification. 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 Then, it overflowed molten silicon 7 inner dimension diameter Fai600mm, depth 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 Of water cooled copper crucible 10 and semi-continuously fed, electron beam 600kW from the electron gun 11 disposed in the crucible above 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。 The height of 2 ingot 13 while irradiating is performed directionally solidified until 150 mm. 黒鉛製蒸着板20は嵩密度が1.74g/cm 3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。 Graphite deposition plate 20 a bulk density of 1.74 g / cm 3 or more, using a graphite plate as the thickness of 10 mm, water-cooled copper hearth 4, and arranged above in a manner to cover both the water-cooled copper crucible 10. 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。 Experiments were also performed using alternative stainless deposition plate graphite deposition plate as a comparative example.

【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 [0015] The phosphorus concentration in the height direction in the silicon ingot center was obtained under the above conditions ICP (Indu
ctively Coupled Plasma)発光分析法により分析した。 It was analyzed by ctively Coupled Plasma) emission spectrometry. 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 The analytical sample, with 10mm increments in the height direction from the bottom of the ingot central portion 50
×10×10mmのシリコン塊を15個切り出したものを用いた。 × silicon mass 10 × 10 mm was used as the cut out 15. 上述の方法で得たPの分析結果を図2に示す。 The analysis of P was obtained in the manner described above is shown in FIG. 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。 In the figure, it plots the analysis results of the sample height 0~10mm at a height of 5 mm. 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。 Here, similarly the raw material silicon, phosphorus concentration results analysis was also carried out in during deposition silicon, respectively about 30 ppmw, was about 150 ppmw. 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。 In embodiments using graphite deposition plate, phosphorus concentration in the silicon was not observed fall stable and deposit in the dissolution. 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。 On the other hand, in the case of using a stainless steel plate shown as a comparative example as a deposition plate, the analysis result of the variation is very large, fall also deposit in the observation in the dissolution was found to be seen. 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。 The dissolution after the furnace observation, the graphite deposition plate was not observed warp of the plate, depositing the silicon had been trapped in graphite deposition plate. 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。 In contrast, in the stainless steel plate was observed warping of the plate, depositing the silicon was also observed the traces falling. 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。 Further, in order to reuse the graphite deposit it could be easily peeled without breakage of the graphite in the peeling operation of the deposition silicon. 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。 Is described here phosphorus aluminum, similar tendency for volatile impurities such as calcium were observed.

【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。 [0016] From the above results, highly purified silicon was found to be achieved stably and easily by using the present invention.

【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, a silicon Upon electron beam melting, it is so arranged to prevent contamination of the molten silicon from the deposit Hakare is further highly purified silicon, stable and easily high purity silicon has become thus obtained.

【図面の簡単な説明】 BRIEF DESCRIPTION OF THE DRAWINGS

【図1】電子ビーム溶解装置の概略図である。 1 is a schematic view of an electron beam melting device.

【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。 2 is a graph showing the phosphorus concentration distribution in the silicon ingot.

【符号の説明】 DESCRIPTION OF SYMBOLS

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 1 electron beam melting apparatus 2 raw material supply device 3 material silicon 4 water-cooled copper hearth 5 electron gun 6 the electron beam 7 molten silicon 10 water-cooled copper crucible 11 electron gun 12 the electron beam 13 ingot 14 melt 15 furnace body 20 made of 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 ────────────────────────────────────────────────── ─── of the front page continued (72) inventor Nagase Akihiro Kurashiki, Okayama Prefecture Mizushimakawasakidori 1-chome (address teeth) Kawasaki Steel in the Corporation Mizushima Works (72) inventor Kenichiro Matsuo Kurashiki, Okayama Prefecture Mizushimakawasakidori 1 chome (address teeth) Kawasaki Steel Corporation Mizushima Works in the F-term (reference) 4G072 AA01 BB01 GG03 GG04 GG05 MM08 NN02 RR30 UU02

Claims (3)

    【特許請求の範囲】 [The claims]
  1. 【請求項1】 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、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。 The method according to claim 1 silicon Upon electron beam melting, the graphite deposition plate larger than the molten metal surface area of ​​the holding container for heating and melting the silicon and secured over the top of the container, while adhering hold the deposit in the vapor deposition plate method for purifying silicon, characterized in that the electron beam melting.
  2. 【請求項2】 前記黒鉛製蒸着板が嵩密度1.7g/c Wherein said graphite deposition plate bulk density 1.7 g / c
    3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。 method for purifying silicon according to claim 1, characterized in that it consists of m 3 or more graphite.
  3. 【請求項3】 シリコンを電子ビーム溶解するシリコン精製装置において、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。 In the 3. A silicon silicon purifying apparatus for electron beam melting, silicon, characterized in that silicon was the heard large graphite deposition plate from the molten metal surface area of ​​the holding vessel to be dissolved by heating arrangement secured over the top of the container of purification equipment.
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