JP4140601B2 - Gas rectifying member for single crystal pulling apparatus and manufacturing method thereof - Google Patents
Gas rectifying member for single crystal pulling apparatus and manufacturing method thereof Download PDFInfo
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本発明は、単結晶引き上げ装置を構成するための部材に関し、特に、半導体材料となるチョクラルスキー法による単結晶引き上げ装置に使用されるガス整流部材に関するものである。 The present invention relates to a member for constituting a single crystal pulling apparatus, and more particularly to a gas rectifying member used for a single crystal pulling apparatus based on the Czochralski method as a semiconductor material.
単結晶引き上げ装置は、所謂チョクラルスキー法と称される方法により、雰囲気ガスの存在下で、ルツボ内のシリコン融液からシリコン単結晶を引き上げるもので、例えば、特公昭57−15079号公報にて示されているような「単結晶製造装置」として知られる。この公報に示された装置は、図3に示すように、 「炉体容器1内にその下方より回転軸2が導入され、その回転軸2の端面上に載置台3を介してルツボ4が配される。又該ルツボ4の周りに発熱体5と保温筒6が配され、而してルツボ4内でシリコンが溶融され融液7を得る。一方、炉体容器1の上方には上下に滑動する回転軸9が設けられている。該回転軸9の遊端にシリコンの種結晶8を取付け、回転軸9を種結晶8がルツボ4内の融液7に触れている状態より上方に移動させて、種結晶8の下に続くシリコンの単結晶10を得る。
A single crystal pulling apparatus pulls a silicon single crystal from a silicon melt in a crucible in the presence of an atmospheric gas by a method called a so-called Czochralski method. For example, Japanese Patent Publication No. 57-15079 discloses a single crystal pulling apparatus. It is known as a “single crystal manufacturing apparatus” as shown in FIG. As shown in FIG. 3, the apparatus disclosed in this publication is as follows: “A
単結晶を育成する際、不必要な反応生成ガスが、単結晶10及び融液7の液面で反応しないように、これを排除する必要がある。このためにアルゴン等の不活性ガスを雰囲気ガスとして、炉体容器1の上方より単結晶及び液面に送給し、炉体容器1下部より排出する」
というものである(上記公報の第2欄)。
When growing the single crystal, it is necessary to eliminate unnecessary reaction product gas so that it does not react on the liquid surface of the single crystal 10 and the
(2nd column of the above publication).
この種の単結晶引き上げ装置では、出来上がってくる半導体材料の純度を保つため、ルツボ内のSi溶融液内に不純物が混入しないようにクリーンな雰囲気を形成しておく必要がある。このため、Siを溶融させるルツボ上には、上方より流れる不活性ガスを整流するためのガス整流部材が設置されている。このガスの整流によって、高温下の炉内で発生するSiOガス等の不純物がルツボ内に流入してSi溶融液内に混入するのを防止する。また、Si単結晶の引き上げ速度に影響する引き上げ方向におけるSi単結晶の温度勾配を大きくするためにピータ及びSi溶融液からの輻射熱を遮断する役割もはたしている。 In this type of single crystal pulling apparatus, it is necessary to form a clean atmosphere so that impurities are not mixed into the Si melt in the crucible in order to maintain the purity of the resulting semiconductor material. For this reason, a gas rectifying member for rectifying the inert gas flowing from above is installed on the crucible for melting Si. This gas rectification prevents impurities such as SiO gas generated in the furnace at high temperature from flowing into the crucible and mixing into the Si melt. Moreover, in order to increase the temperature gradient of the Si single crystal in the pulling direction that affects the pulling speed of the Si single crystal, it also plays a role of blocking radiant heat from the Peter and the Si melt.
上記のように、Si単結晶の温度勾配を大きくするためには、融液やルツボからの輻射熱を十分に遮断しなければならない。また、黒鉛材は耐熱性に優れるものであっても、断熱性を十分に発揮し得るものではない。そこで、単結晶引き上げ装置用のガス整流部材は、熱輻射を遮断するために黒鉛を基材とし、断熱材を組み合わせたものが提供されている。例えば、特開平9−183686号公報は
、引き上げ単結晶棒を同軸に囲う円筒とカラーからなり、該カラーは、高純度黒鉛材で形成され、複層に重ね合わせた断熱材がカラー上面を覆うように設けられ
、さらにこの上面は高純度黒鉛材で被覆され、あるいは被覆する高純度黒鉛材の表面には炭化珪素等が被覆されるものである。
As described above, in order to increase the temperature gradient of the Si single crystal, the radiant heat from the melt and the crucible must be sufficiently blocked. Moreover, even if a graphite material is excellent in heat resistance, it cannot fully exhibit heat insulation. Therefore, a gas rectifying member for a single crystal pulling apparatus is provided in which graphite is used as a base material and a heat insulating material is combined in order to block heat radiation. For example, Japanese Patent Application Laid-Open No. 9-183686 is composed of a cylinder and a collar that coaxially surrounds a pulling single crystal rod, and the collar is formed of a high-purity graphite material, and a heat insulating material overlapped on multiple layers covers the upper surface of the collar. Further, the upper surface is coated with a high purity graphite material, or the surface of the high purity graphite material to be coated is coated with silicon carbide or the like.
しかし、ガス整流部材は、加工精度により高価となるばかりか、熱容量も大きくなるという問題があり、更に介合部よりSiOガスが侵入し、次のような化学反応が生じて、断熱材が珪化し、パーティクルの発生の原因となることもあった。 However, the gas rectifying member is not only expensive due to the processing accuracy, but also has a problem that the heat capacity is increased, and further, the SiO gas enters from the interposer and the following chemical reaction occurs, and the heat insulating material is silicified. However, it sometimes causes generation of particles.
SiO+2C→SiC+CO SiO + 2C → SiC + CO
そこで、本発明の目的とするところは、単結晶の引き上げに必要な所望の温 度勾配を与え、かつ単結晶引き上げ装置内の汚染や単結晶の汚染を引き起こすことのない耐久性が高くてコスト低減が可能なガス整流部材を提供することである。 Therefore, the object of the present invention is to provide a desired temperature gradient necessary for pulling a single crystal and to have high durability and cost without causing contamination in the single crystal pulling apparatus or contamination of the single crystal. It is to provide a gas rectifying member that can be reduced.
上記の課題を解決するために請求項1に記載の発明の採った手段を実施形態の説明中において使用する符号を付して説明すると、
「半導体原料を溶融させるルツボ上に設置され、密閉本体に上方より流入する不活性ガスを整流するためのガス整流部材であって、炭素質繊維成形体を基材とし、この基材の表面に熱硬化性樹脂を加熱硬化した後炭化してなる熱硬化性樹脂炭化物を中間層として形成し、さらに、この中間層の表面に熱分解炭素からなる被膜を形成してなり、
炭素質繊維成形体の繊維の1本1本に熱分解炭素の被膜形成が防止されてなることを特徴とする単結晶引き上げ装置用のガス整流部材。」
というものである。
In order to solve the above problems, the means taken by the invention of
“A gas rectifying member installed on a crucible for melting a semiconductor raw material and rectifying an inert gas flowing into the sealed body from above, with a carbonaceous fiber molded body as a base material. A thermosetting resin carbide formed by carbonizing after thermosetting the thermosetting resin is formed as an intermediate layer, and further, a film made of pyrolytic carbon is formed on the surface of the intermediate layer,
A gas rectifying member for a single crystal pulling apparatus, wherein a film of pyrolytic carbon is prevented from being formed on each of the fibers of the carbonaceous fiber molded body. "
That's it.
さらに、請求項2に記載の発明が採った手段は、「半導体原料を溶融させるルツボ上10に設置され、密閉本体50内に上方より流入する不活性ガスを整流するためのガス整流部材60の製造方法であって、
炭素質繊維成形体61を基材とし、この基材の表面に、フェノール樹脂、フラン樹脂、ジビニルベンゼン樹脂、又は縮合多環芳香族化合物とヒドロキシメチル基、ハロメチル基のいずれか少なくとも一種の基を二個以上有する一環又は二環以上の芳香環からなる成る芳香族架橋剤と酸触媒とを組み合わせて成る組成物の中から選ばれる、一種又は二種以上の熱硬化性樹脂を前記炭素繊維質成形体61に塗り付け、
加熱硬化した後、再度塗布して硬化処理をし、
炭化してなる熱硬化性樹脂炭化物を中間層62として形成し、
さらに、この中間層62の表面に熱分解炭素からなる被膜63を形成してなり、
炭素質繊維成形体61の繊維の1本1本に熱分解炭素の被膜形成が防止されてなることを特徴とする単結晶引き上げ装置用のガス整流部材の製造方法。」を特徴とするものである。
Furthermore, the means taken by the invention of
A carbonaceous fiber molded body 61 is used as a base material, and at least one group of a phenol resin, a furan resin, a divinylbenzene resin, or a condensed polycyclic aromatic compound and a hydroxymethyl group or a halomethyl group is formed on the surface of the base material. One or two or more types of thermosetting resins selected from compositions comprising a combination of an aromatic cross-linking agent composed of two or more aromatic rings composed of one or two or more aromatic rings and an acid catalyst. Apply to the molded body 61,
After heat curing, apply and cure again,
Forming a carbonized thermosetting resin carbide as the intermediate layer 62;
Further, a film 63 made of pyrolytic carbon is formed on the surface of the intermediate layer 62,
A method for producing a gas rectifying member for a single crystal pulling apparatus, wherein a film of pyrolytic carbon is prevented from being formed on each of the fibers of the carbonaceous fiber molded body 61 . ".
本発明に係るガス整流部材60は、図1に示すように、半導体原料を溶融させるルツボ10の上方に設置されるものであり、その基材全体を炭素質繊維成形体61によって形成することが必要である。その理由はこのような炭素質繊維成形体61は、熱伝導性が小さく高い断熱性を備えているため、ルツボ10の上方に形成すれば、融液やルツボ10から単結晶に加えられる輻射熱を十分に遮断でき、単結晶の引き上げに必要な所望の温度勾配を得ることができるからである。 As shown in FIG. 1, the gas rectifying member 60 according to the present invention is installed above the crucible 10 for melting the semiconductor raw material, and the entire base material can be formed by the carbonaceous fiber molded body 61. is necessary. The reason is that such a carbonaceous fiber molded body 61 has low heat conductivity and high heat insulation properties. Therefore, if it is formed above the crucible 10, the melt or radiant heat applied from the crucible 10 to the single crystal can be obtained. This is because the desired temperature gradient necessary for pulling up the single crystal can be obtained.
次いで、炭素質繊維成形体61の表面には、熱硬化性樹脂炭化物からなる中間層62を形成する必要がある。そして、この中間層62を形成する熱硬化性樹脂炭化物は、フェノール樹脂、フラン樹脂、ジビニルベンゼン樹脂、又は、縮合多環芳香族化合物とヒドロキシメチル基、ハロメチル基のいずれか少なくとも一種の基を二個以上有する一環または二環以上の芳香環から成る芳香族架橋剤と酸触媒とを組合せて成る組成物の中から選ばれる、一種または二種以上の熱硬化性樹脂を加熱硬化した後炭化して形成される。炭素質繊維成形体61の表面に熱硬化性樹脂炭化物からなる中間層62を形成する理由は、中間層62が存在しないと熱分解炭素の被膜63が形成されにくく、繊維1本1本に熱分解炭素がコーティングされるので、さらに、その上に熱分解炭素の被膜63が形成されることにより重量が増加したり、それに伴う熱容量アップや断熱特性の劣化につながるからである。 Next, an intermediate layer 62 made of a thermosetting resin carbide needs to be formed on the surface of the carbonaceous fiber molded body 61. The thermosetting resin carbide forming the intermediate layer 62 contains at least one group selected from a phenol resin, a furan resin, a divinylbenzene resin, a condensed polycyclic aromatic compound, a hydroxymethyl group, and a halomethyl group. One or two or more thermosetting resins selected from a composition comprising an aromatic crosslinker consisting of one or more aromatic rings composed of one or more aromatic rings and an acid catalyst are heat-cured and then carbonized. Formed. The reason why the intermediate layer 62 made of a thermosetting resin carbide is formed on the surface of the carbonaceous fiber molded body 61 is that if the intermediate layer 62 is not present, the pyrolytic carbon coating 63 is difficult to be formed, and heat is applied to each fiber. Since cracked carbon is coated, the pyrolytic carbon film 63 is further formed on the cracked carbon, thereby increasing the weight, resulting in an increase in heat capacity and deterioration of heat insulation characteristics.
さらに、中間層62として形成された熱硬化性樹脂炭化物の表面には、熱分解炭素からなる被膜63を形成することが必要である。その理由は、熱分解炭素の被膜63の表面層は緻密であるため、耐酸化性、気体不浸透性も極めて向上し、SiOガスやSiガスと熱硬化性樹脂炭化物とが接触して、熱硬化性樹脂炭化物の炭素と反応することを防ぐためである。一方、熱分解炭素からなる被膜63の表面層の熱伝導率は、熱分解炭素沈積面に垂直な方向においては、非常に低いことから、炭素質繊維成形体61の本来の熱伝導率は上昇せず、高断熱性も十分確保されるからである。また、熱硬化性樹脂炭化物からのカーボン落ちの虞もあるため、緻密質な熱分解炭素からなる被膜63でこれらの不都合を防げば、単結晶引き上げ装置100内の汚染や単結晶の汚染を防ぐことができるからである。さらに、熱分解炭素からなる被膜63の表面層は緻密性が高いため、熱硬化性樹脂炭化物からなる中間層62のみならず、炭素質繊維成形体61の機械的強度も向上するだけでなく、耐酸化性及び気体不浸透性も極めて向上するからである。 Further, it is necessary to form a film 63 made of pyrolytic carbon on the surface of the thermosetting resin carbide formed as the intermediate layer 62. The reason is that since the surface layer of the pyrolytic carbon coating 63 is dense, the oxidation resistance and gas impermeability are also greatly improved, and the SiO gas or Si gas and the thermosetting resin carbide come into contact with each other. This is to prevent reaction with carbon of the curable resin carbide. On the other hand, since the thermal conductivity of the surface layer of the coating 63 made of pyrolytic carbon is very low in the direction perpendicular to the pyrolytic carbon deposition surface, the original thermal conductivity of the carbonaceous fiber molded body 61 is increased. This is because high thermal insulation is sufficiently secured. In addition, since there is a risk of carbon dropping from the thermosetting resin carbide, if these disadvantages are prevented by the coating 63 made of dense pyrolytic carbon, contamination in the single crystal pulling apparatus 100 and contamination of the single crystal are prevented. Because it can. Furthermore, since the surface layer of the coating 63 made of pyrolytic carbon has a high density, not only the intermediate layer 62 made of a thermosetting resin carbide but also the mechanical strength of the carbonaceous fiber molded body 61 is improved. This is because the oxidation resistance and gas impermeability are also greatly improved.
本発明に係る単結晶引き上げ装置100用のガス整流部材60は、「半導体原料を溶融させるルツボ10上に設置され、密閉本体50内に上方より流入する不活性ガスを整流するためのガス整流部材60であって、炭素質繊維成形体61を基材とし、この基材の表面に熱硬化性樹脂を加熱硬化した後炭化してなる熱硬化性樹脂炭化物を中間層62として形成し、さらに、この中間層62の表面に熱分解炭素からなる被膜63を形成してなり、炭素質繊維成形体の繊維の1本1本に熱分解炭素の被膜形成が防止されてなること」を特徴とすることにより、炭素質繊維成形体61は高断熱性を備えるので、所望の温度勾配を得ることができ、良質な単結晶が得られる。 また、中間層62には緻密質な熱分解炭素からなる被膜63が堅固に形成されるので、密閉本体50内の汚染や単結晶の汚染を引き起こさないばかりか、ガス整流部材60の珪化を防ぐこともできるので、耐久性が高い低コストの単結晶引き上げ装置用のガス整流部材を得ることができる。 The gas rectifying member 60 for the single crystal pulling apparatus 100 according to the present invention is “a gas rectifying member that is installed on the crucible 10 for melting the semiconductor raw material and rectifies the inert gas flowing from above into the sealed body 50. 60, the carbonaceous fiber molded body 61 is used as a base material, and a thermosetting resin carbide formed by carbonizing the thermosetting resin after heat-curing the thermosetting resin on the surface of the base material is formed as the intermediate layer 62. the intermediate coatings 63 made of pyrolytic carbon on the surface of the layer 62 formed by Ri Na, and characterized in that is prevented film formation of pyrolytic carbon "to one one fiber charcoal predisposition fiber molded body By doing so, since the carbonaceous fiber molded body 61 is provided with high heat insulation, a desired temperature gradient can be obtained and a high-quality single crystal can be obtained. Further, since the coating 63 made of dense pyrolytic carbon is firmly formed on the intermediate layer 62, it does not cause contamination in the sealed body 50 or single crystal, but also prevents silicidation of the gas rectifying member 60. Therefore, it is possible to obtain a gas rectifying member for a single crystal pulling apparatus having high durability and low cost.
次に本発明を、図面に示した実施の形態について説明すると、図1には、本発明に係るガス整流部材60が適用される単結晶引き上げ装置100の縦断面図が示してある。この単結晶引き上げ装置100は、その密閉本体50内に、半導体原料を溶融させるためのルツボ10を回転軸にて回転可能に収容したものであり、このルツボ10の周囲にはこれを加熱するためのヒータ20が配置してある。 そして、ルツボ10の上方には、本発明に係るガス整流部材60が配置してある。 Next, the present invention will be described with reference to the embodiment shown in the drawings. FIG. 1 is a longitudinal sectional view of a single crystal pulling apparatus 100 to which a gas rectifying member 60 according to the present invention is applied. This single crystal pulling apparatus 100 is a device in which a crucible 10 for melting a semiconductor raw material is accommodated in a hermetically sealed main body 50 so as to be rotatable on a rotating shaft, and the crucible 10 is heated around the crucible 10. The heater 20 is arranged. A gas rectifying member 60 according to the present invention is disposed above the crucible 10.
ルツボ10は、溶融した半導体原料と直接接触する部分を、石英ルツボ11とした二重構造のものであり、ヒータ20は、一般的には、所謂黒鉛ヒータが採用されるものであり、図1に示したような位置関係で略一定となるものである。 The crucible 10 has a double structure having a quartz crucible 11 as a portion in direct contact with the molten semiconductor material, and the heater 20 is generally a so-called graphite heater. It becomes substantially constant in the positional relationship as shown in FIG.
ガス整流部材60は、図2に示したように炭素質繊維成形体61を基材として形成され、さらに炭素質繊維成形体61の表面には中間層62として熱硬化性樹脂炭化物が形成され、さらに、この中間層62の表面には、熱分解炭素からなる被膜63が形成される。上記の炭素質繊維成形体61、中間層62を形成する熱硬化性樹脂炭化物及び熱分解炭素からなる被膜63は、以下の実施例にて詳細に示すように製造又は形成されるものである。 As shown in FIG. 2, the gas rectifying member 60 is formed using the carbonaceous fiber molded body 61 as a base material. Further, a thermosetting resin carbide is formed as an intermediate layer 62 on the surface of the carbonaceous fiber molded body 61, Further, a coating 63 made of pyrolytic carbon is formed on the surface of the intermediate layer 62. The carbonaceous fiber molded body 61, the thermosetting resin carbide forming the intermediate layer 62 and the coating 63 made of pyrolytic carbon are manufactured or formed as shown in detail in the following examples.
長径の外径φ340mm、短径の外径φ200mm、厚さ5mm、高さ350mmの逆円錐状の炭素質繊維成形体61を形成した。得られた炭素質繊維成形体61には、熱硬化性樹脂として、軟化点80℃の石油系ピッチのベンゼン可溶分(平均分子量340)とP−キシレングリコールをモル比で1:2の割合で混合し、そこに1wt%のP−トルエンスルホン酸を加えた混合物を用い、これを130℃で40分間反応させた。 An inverted conical carbonaceous fiber molded body 61 having a major outer diameter of 340 mm, a minor outer diameter of 200 mm, a thickness of 5 mm, and a height of 350 mm was formed. The obtained carbonaceous fiber molded body 61 has a 1: 2 molar ratio of a benzene-soluble component (average molecular weight 340) of petroleum-based pitch having a softening point of 80 ° C. and P-xylene glycol as a thermosetting resin. And 1 wt% P-toluenesulfonic acid was added thereto, and this was reacted at 130 ° C. for 40 minutes.
この反応生成物を130℃で溶融させ、前記炭素質繊維成形体61に塗りつけ、180℃で硬化させた後、再度塗布して硬化処理をし、1900℃で焼成した。 This reaction product was melted at 130 ° C., applied to the carbonaceous fiber molded body 61, cured at 180 ° C., then applied again, cured, and baked at 1900 ° C.
表面に熱硬化性樹脂炭化物からなる中間層62が形成された炭素質繊維成形体61をCVD炉内に入れて、蒸着温度2000℃、圧力30Torrの条件下で、水素ガスをキャリアとしてメタンガスを炉内に連続的に供給した。これにより、熱硬化性樹脂炭化物の表面全体に厚さ50μmの熱分解炭素からなる被膜63を形成した。 A carbonaceous fiber molded body 61 having an intermediate layer 62 made of a thermosetting resin carbide formed on the surface is placed in a CVD furnace, and methane gas is heated in a furnace using hydrogen gas as a carrier under conditions of a deposition temperature of 2000 ° C. and a pressure of 30 Torr. Was continuously fed into. Thereby, the film 63 made of pyrolytic carbon having a thickness of 50 μm was formed on the entire surface of the thermosetting resin carbide.
100 単結晶引き上げ装置
10 ルツボ
11 石英ルツボ
20 ヒータ
50 密閉本体
60 ガス整流部材
61 炭素質繊維成形体
62 熱硬化性樹脂炭化物からなる中間層
63 熱分解炭素からなる被膜
DESCRIPTION OF SYMBOLS 100 Single crystal pulling apparatus 10 Crucible 11 Quartz crucible 20 Heater 50 Sealing main body 60 Gas rectifying member 61 Carbonaceous fiber molded body 62 Intermediate layer 63 made of thermosetting resin carbide 63 Film made of pyrolytic carbon
Claims (2)
炭素質繊維成形体の繊維の1本1本に熱分解炭素の被膜形成が防止されてなることを特徴とする単結晶引き上げ装置用のガス整流部材。 A gas rectifying member installed on a crucible for melting a semiconductor raw material and rectifying an inert gas flowing into the sealed body from above, with a carbonaceous fiber molded body as a base material, and heat on the surface of the base material A thermosetting resin carbide formed by heating and curing the curable resin is formed as an intermediate layer, and further, a film made of pyrolytic carbon is formed on the surface of the intermediate layer,
A gas rectifying member for a single crystal pulling apparatus, wherein a film of pyrolytic carbon is prevented from being formed on each of the fibers of the carbonaceous fiber molded body.
炭素質繊維成形体を基材とし、この基材の表面に、フェノール樹脂、フラン樹脂、ジビニルベンゼン樹脂、又は縮合多環芳香族化合物とヒドロキシメチル基、ハロメチル基のいずれか少なくとも一種の基を二個以上有する一環又は二環以上の芳香環からなる成る芳香族架橋剤と酸触媒とを組み合わせて成る組成物の中から選ばれる、一種又は二種以上の熱硬化性樹脂を前記炭素繊維質成形体に塗り付け、
加熱硬化した後、再度塗布して硬化処理をし、
炭化してなる熱硬化性樹脂炭化物を中間層として形成し、
さらに、この中間層の表面に熱分解炭素からなる被膜を形成してなり、
炭素質繊維成形体の繊維の1本1本に熱分解炭素の被膜形成が防止されてなることを特徴とする単結晶引き上げ装置用のガス整流部材の製造方法。 A method for producing a gas rectifying member for rectifying an inert gas which is installed on a crucible for melting a semiconductor raw material and flows into the sealed body from above,
A carbonaceous fiber molded body is used as a base material, and at least one group selected from a phenol resin, a furan resin, a divinylbenzene resin, or a condensed polycyclic aromatic compound and a hydroxymethyl group or a halomethyl group is formed on the surface of the base material. One or more thermosetting resins selected from a composition comprising a combination of an aromatic cross-linking agent comprising one or more aromatic rings composed of one or more aromatic rings and an acid catalyst are formed into the carbon fiber molding. Smear on the body,
After heat curing, apply and cure again,
Forming a carbonized thermosetting resin carbide as an intermediate layer,
Furthermore, a film made of pyrolytic carbon is formed on the surface of this intermediate layer,
Method for producing a gas rectifying member for a single crystal pulling apparatus which is characterized that you made is prevented film formation of pyrolytic carbon to one one fiber of carbonaceous fiber molding.
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JP2004322452A JP4140601B2 (en) | 2004-11-05 | 2004-11-05 | Gas rectifying member for single crystal pulling apparatus and manufacturing method thereof |
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JP03308898A Division JP3637435B2 (en) | 1998-02-16 | 1998-02-16 | Gas rectifier for single crystal pulling device |
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