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JP2007107030A - Electrode short-circuit prevention method and short-circuit prevention plate - Google Patents

Electrode short-circuit prevention method and short-circuit prevention plate Download PDF

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JP2007107030A
JP2007107030A JP2005297001A JP2005297001A JP2007107030A JP 2007107030 A JP2007107030 A JP 2007107030A JP 2005297001 A JP2005297001 A JP 2005297001A JP 2005297001 A JP2005297001 A JP 2005297001A JP 2007107030 A JP2007107030 A JP 2007107030A
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circuit prevention
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JP4905638B2 (en
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Shunichi Hasegawa
俊一 長谷川
Naoki Hatakeyama
直紀 畠山
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Mitsubishi Materials Polycrystalline Silicon Corp
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Abstract

【課題】多結晶シリコンの製造反応炉に設置された電極まわりの液滴の流下を阻止し、液滴の析出と堆積による短絡を防止する。
【解決手段】多結晶シリコンの製造反応炉に設置された電極に板材を装着し、該板材が電極まわりに張り出すように設けることを特徴とする電極の短絡防止方法、および、側方に開口する凹部を有する板材によって形成されており、該凹部が電極の軸まわりに装入されることによって該板材が電極まわりに張り出して装着され、電極まわりの液滴の流下を阻止することを特徴とする電極の短絡防止板。
【選択図】図１Disclosed is a method for preventing a liquid crystal from flowing down around an electrode installed in a reactor for producing polycrystalline silicon and preventing a short circuit due to deposition and deposition of the liquid droplet.
A method for preventing a short circuit of an electrode, wherein a plate material is attached to an electrode installed in a reactor for producing polycrystalline silicon, and the plate material is provided so as to project around the electrode, and a side opening is provided. Characterized in that it is formed by a plate material having a concave portion, and that the concave portion is inserted around the axis of the electrode so that the plate material is mounted around the electrode and prevents the liquid droplet from flowing around the electrode. Electrode short-circuit prevention plate.
[Selection] Figure 1

Description

本発明は、シーメンス法による多結晶シリコン製造炉に設置される電極の短絡を防止する手段に関する。 The present invention relates to a means for preventing a short circuit of electrodes installed in a polycrystalline silicon manufacturing furnace by the Siemens method.

半導体級多結晶シリコンは従来から主にシーメンス法によって製造されている。この製造装置の一例を図３に示す。図に示するように、反応炉１０は炉底２０を覆うようにベルジャ３０が設けられており、内部が密閉されている。炉内には種棒となる逆Ｕ字型のシリコン芯材（シード）５０が複数本立設されており、該芯材５０の両基端部は炉底部の電極６０にホルダー６１を介して支えられている。炉底２０には、炉内の芯材に向かって原料ガスを供給するノルズ７０が設けらてれいる。ノズル７０の個数は複数のシリコン芯材５０に対して均一に原料ガスが供給されるように配置されている。これらのノズル７０は原料ガスの供給管路９０に接続しており、供給管路９０は流量調整弁９２を介して原料ガスの供給源に通じている。原料ガスは供給管路９０を経てノズル７０に送られ、炉内に供給される。また、反応炉１０には排ガスの排出口９３が設けられており、排出口９３は排出管路９４に接続している。 Semiconductor grade polycrystalline silicon has heretofore been produced mainly by the Siemens method. An example of this manufacturing apparatus is shown in FIG. As shown in the figure, the reaction furnace 10 is provided with a bell jar 30 so as to cover the furnace bottom 20, and the inside is sealed. A plurality of inverted U-shaped silicon cores (seed) 50 serving as seed rods are erected in the furnace, and both base ends of the core material 50 are supported by electrodes 60 at the bottom of the furnace via holders 61. It has been. The furnace bottom 20 is provided with a NORZ 70 for supplying a raw material gas toward the core material in the furnace. The number of nozzles 70 is arranged so that the source gas is uniformly supplied to the plurality of silicon core members 50. The nozzles 70 are connected to a source gas supply line 90, and the supply line 90 communicates with a source gas supply source via a flow rate adjusting valve 92. The source gas is sent to the nozzle 70 through the supply pipe line 90 and supplied into the furnace. The reaction furnace 10 is provided with an exhaust gas outlet 93, and the outlet 93 is connected to the exhaust pipe 94.

シリコン芯材５０は電極６０およびホルダー６１を通じて通電され、表面が１０００℃以上に赤熱される。炉内に供給された原料ガスは、赤熱したシリコン芯材１１の表面に接触して熱分解ないし水素還元され、シード５０の表面に多結晶シリコンを析出する。この反応が進行して多結晶シリコン棒に成長する（特許文献１）。 The silicon core member 50 is energized through the electrode 60 and the holder 61, and the surface is red-heated to 1000 ° C. or higher. The source gas supplied into the furnace comes into contact with the surface of the red-hot silicon core 11 and is thermally decomposed or reduced with hydrogen to deposit polycrystalline silicon on the surface of the seed 50. This reaction proceeds to grow into a polycrystalline silicon rod (Patent Document 1).

このように、シリコン芯材には電極およびホルダーを通じて大量の電流が流れるので、炉底に設けられている電極は反応炉本体に対して絶縁を確保する必要がある。そこで、電極と反応炉との間には絶縁材が設けられている。さらに、電極は赤熱した芯材からの放熱に対して保護するために、電極の内部には冷却水が流れる構造が形成されており、電極および絶縁材が水冷されている（特許文献２）。
特許第２８６７３０６号公報 特表２００２−５０８２９４号公報 As described above, since a large amount of current flows through the silicon core material through the electrode and the holder, it is necessary to ensure insulation of the electrode provided on the furnace bottom with respect to the reaction furnace main body. Therefore, an insulating material is provided between the electrode and the reaction furnace. Furthermore, in order to protect the electrode against heat radiation from the red-hot core material, a structure in which cooling water flows is formed inside the electrode, and the electrode and the insulating material are water-cooled (Patent Document 2).
Japanese Patent No. 2867306 Special Table 2002-508294

炉内でトリクロロシランなどのクロロシラン類の原料ガスが反応してシリコン心材表面に多結晶シリコンを析出させる際に、シリコン析出時の副生物であるクロロシランポリマーが凝縮し、流れ落ちて電極や絶縁材に付着する場合がある。このポリマーはシリコン心材からの放射熱を受けて多結晶シリコンに転化して電極や絶縁材およびその周囲に付着し、この付着したシリコンによって電極とその周囲の炉本体との間で短絡が生じ、電源接地のトラブルを招くことがある。 When the source gas of chlorosilanes such as trichlorosilane reacts in the furnace to deposit polycrystalline silicon on the surface of the silicon core, the by-product chlorosilane polymer at the time of silicon deposition condenses and flows down to the electrodes and insulation. May adhere. This polymer receives radiant heat from the silicon core material and is converted into polycrystalline silicon and adheres to the electrode and the insulating material and its surroundings. This deposited silicon causes a short circuit between the electrode and the surrounding furnace body, May cause power grounding problems.

本発明は、多結晶シリコン製造における従来の上記問題を解決したものであり、反応炉に設置した電極の短絡を防止する方法と手段を提供する。本発明の短絡防止方法ないし手段は既存の反応炉の構造を変更せずに容易に実施することができ、確実な短絡防止効果を得ることができるので、安定操業の確保、および生産性の向上に有用である。 The present invention solves the above-mentioned conventional problems in the production of polycrystalline silicon, and provides a method and means for preventing a short circuit of an electrode installed in a reaction furnace. The short-circuit prevention method or means of the present invention can be easily implemented without changing the structure of the existing reactor, and a reliable short-circuit prevention effect can be obtained, ensuring stable operation and improving productivity. Useful for.

本発明は、以下の構成を有する電極短絡防止方法と短絡防止手段に関する。
（１）多結晶シリコンの製造反応炉に設置された電極に板材を装着し、該板材が電極まわりに張り出すように設けることによって、電極まわりの液滴の流下を阻止し、液滴の析出と堆積による短絡を防止することを特徴とする電極の短絡防止方法。
（２）側方に開口する凹部を有する板材によって形成した短絡防止板を少なくとも二枚用い、これら短絡防止板の開口凹部の向きが重ならないように、該短絡防止板を上下に重ねて電極に装着し、該短絡防止材が電極まわりに張り出すように設けることによって、電極まわりの液滴の流下を阻止する上記(１)に記載する電極の短絡防止方法。
（３）電極と反応炉との間に介設されている絶縁材の上側に短絡防止板を設けて、電極まわりの液滴の流下を阻止する上記(１)または(２)に記載する電極の短絡防止方法。
（４）多結晶シリコンの製造反応炉に設置された電極に装着される短絡防止板であって、側方に開口する凹部を有する板材によって形成されており、該凹部が電極の軸まわりに装入されることによって該板材が電極まわりに張り出して装着され、電極まわりの液滴の流下を阻止することを特徴とする電極の短絡防止板。
（５）カーボン製の板材によって形成された上記(４)に記載する電極の短絡防止板。 The present invention relates to an electrode short-circuit prevention method and a short-circuit prevention means having the following configurations.
(1) Production of polycrystalline silicon A plate is attached to an electrode installed in a reaction furnace, and the plate is provided so as to protrude around the electrode, thereby preventing the liquid droplet from flowing around the electrode and depositing the droplet. And a method of preventing a short circuit due to deposition.
(2) Use at least two short-circuit prevention plates formed of a plate material having recesses that open to the side, and stack the short-circuit prevention plates on top and bottom so that the orientation of the opening recesses of these short-circuit prevention plates does not overlap. The electrode short-circuit prevention method according to the above (1), wherein the electrode is installed and the short-circuit prevention material is provided so as to protrude around the electrode, thereby preventing the liquid droplet from flowing down around the electrode.
(3) The electrode described in (1) or (2) above, wherein a short-circuit prevention plate is provided on the upper side of the insulating material interposed between the electrode and the reactor to prevent the liquid droplet from flowing around the electrode. How to prevent short circuit.
(4) Production of polycrystalline silicon A short-circuit prevention plate to be attached to an electrode installed in a reaction furnace, which is formed of a plate material having a concave portion that opens to the side, and the concave portion is mounted around the axis of the electrode. An electrode short-circuit prevention plate, wherein the plate material is mounted so as to protrude around the electrode by being inserted, and the flow of liquid droplets around the electrode is prevented.
(5) The electrode short-circuit prevention plate according to (4), which is formed of a carbon plate material.

本発明は、反応炉の電極に短絡防止材を装着し、好ましくは絶縁材よりも上側に装着し、該短絡防止板が電極まわりに張り出すように設けるので、原料ガスの反応によって副生するクロロシランポリマーの液滴の流下が短絡防止板によって阻止され、電極および絶縁材と炉底との間に流れ込まないので、この部分に析出するシリコン量が大幅に低減され、従って、電極と炉底との間の短絡を確実に防止することができる。 In the present invention, the short-circuit prevention material is attached to the electrode of the reaction furnace, preferably on the upper side of the insulating material, and the short-circuit prevention plate is provided so as to protrude around the electrode. Since the flow of chlorosilane polymer droplets is prevented by the short-circuit prevention plate and does not flow between the electrode and the insulating material and the bottom of the furnace, the amount of silicon deposited in this part is greatly reduced. Can be reliably prevented.

短絡防止板を電極まわりに張り出すように設けるので、短絡防止板より下側の部分には原料ガスが触れ難くなり、またシリコン心材から受ける放射熱も減少するので、絶縁材に析出するシリコン量が大幅に減少する。 Since the short-circuit prevention plate is provided so as to protrude around the electrode, it is difficult for the source gas to touch the part below the short-circuit prevention plate, and the radiant heat received from the silicon core material is reduced, so the amount of silicon deposited on the insulating material Is greatly reduced.

本発明の短絡防止方法ないし防止手段は、短絡防止板を電極に装着するだけであり、反応炉の構造を変更する必要がないので、容易に実施することができる。また、短絡防止板は側方に開口する凹部を設けた板材であるので、容易に製造することができ、しかも確実な短絡防止効果を得ることができる。さらに、この短絡防止板は着脱自在であり、この上側に多結晶シリコンが析出して堆積量が多くなったときには容易に交換することができる。 The short-circuit prevention method or prevention means of the present invention can be easily implemented because only the short-circuit prevention plate is attached to the electrode and there is no need to change the structure of the reactor. Further, since the short-circuit prevention plate is a plate material provided with a concave portion that opens to the side, it can be easily manufactured and a reliable short-circuit prevention effect can be obtained. Further, the short-circuit prevention plate is detachable, and can be easily replaced when polycrystalline silicon is deposited on the upper side and the deposition amount increases.

以下、本発明の短絡防止方法と手段について、図面を参照して具体的に説明する。
本発明の短絡防止方法は、多結晶シリコンの製造反応炉に設置された電極に板材を装着し、該板材が電極まわりに張り出すように設けることによって、電極まわりの液滴の流下を阻止し、液滴の析出と堆積による短絡を防止することを特徴とする電極の短絡防止方法である。 The short-circuit prevention method and means of the present invention will be specifically described below with reference to the drawings.
The short-circuit prevention method of the present invention prevents the flow of liquid droplets around the electrode by attaching a plate material to an electrode installed in a polycrystalline silicon production reactor and providing the plate material so as to protrude around the electrode. An electrode short-circuit prevention method characterized by preventing a short-circuit due to deposition and deposition of droplets.

本発明の短絡防止板は、上記短絡防止方法に用いるものであって、側方に開口する凹部を有する板材によって形成されており、該凹部が電極の軸まわりに装入されることによって該板材が電極まわりに張り出して装着され、電極まわりの液滴の流下を阻止することを特徴とする電極の短絡防止板である。 The short-circuit prevention plate of the present invention is used for the above-mentioned short-circuit prevention method, and is formed of a plate material having a concave portion that opens to the side. The plate material is formed by inserting the concave portion around the axis of the electrode. Is a short-circuit prevention plate for an electrode, which is mounted so as to protrude around the electrode and prevents the flow of droplets around the electrode.

本発明の短絡防止板とその装着状態を図１および図２に示す。図示するように、反応炉１０の炉底２０を貫通して電極６０が設けられており、電極６０と炉底２０との間には絶縁材４０が介設されている。電極６０の先端にはホルダー６１が形成されており、該ホルダー６１にはシリコン心材５０が差し込まれている。該シリコン心材５０は、図３に示すように、炉内に逆Ｕ字型に設置されており、その両端部は上記ホルダー６１によって電極６０に支持されている。 The short-circuit prevention plate of the present invention and its mounting state are shown in FIGS. As shown in the drawing, an electrode 60 is provided through the furnace bottom 20 of the reaction furnace 10, and an insulating material 40 is interposed between the electrode 60 and the furnace bottom 20. A holder 61 is formed at the tip of the electrode 60, and the silicon core material 50 is inserted into the holder 61. As shown in FIG. 3, the silicon core material 50 is installed in an inverted U shape in the furnace, and both ends thereof are supported by the electrode 60 by the holder 61.

絶縁材４０の上側の電極まわりに本発明の短絡防止板８０が装着されている。短絡防止板８０は、図２に示すように、側方に開口する凹部８１を有する板材によって形成されている。開口凹部８１の大きさは電極６０の外径に対応しており、該開口凹部８１に電極６０を嵌合することによって短絡防止板８０を電極の軸まわりに張り出して装着させる。 A short-circuit prevention plate 80 of the present invention is mounted around the upper electrode of the insulating material 40. As shown in FIG. 2, the short-circuit prevention plate 80 is formed of a plate material having a concave portion 81 that opens to the side. The size of the opening recess 81 corresponds to the outer diameter of the electrode 60. By fitting the electrode 60 into the opening recess 81, the short-circuit prevention plate 80 is projected and attached around the electrode axis.

短絡防止板８０は電極３０の軸まわりに十分に張り出した状態を形成すればよいので、その外周部の形状は限定されず、丸形、角形、または多角形の何れででもよい。短絡防止板８０は反応炉１０の炉内に設置されるので、炉内の汚染を生じないように、その材質は電極６０やホルダー６１と同様にカーボン等が好ましい。また、短絡防止板８０の板厚は任意であり十分な強度が得られる板厚であれば良い。なお、電極６０に嵌合した短絡防止板８０を安定に装着させるには、電極６０の側面に突起（図示省略）を設け、この突起で短絡防止板８０を支持させると良い。 The short-circuit prevention plate 80 only needs to be formed so as to protrude sufficiently around the axis of the electrode 30, and therefore the shape of the outer peripheral portion thereof is not limited, and may be round, square, or polygonal. Since the short-circuit prevention plate 80 is installed in the furnace of the reaction furnace 10, the material is preferably carbon or the like as in the case of the electrode 60 and the holder 61 so as not to cause contamination in the furnace. Moreover, the plate | board thickness of the short circuit prevention board 80 is arbitrary, and should just be a board thickness from which sufficient intensity | strength is obtained. In order to stably mount the short-circuit prevention plate 80 fitted to the electrode 60, it is preferable to provide a protrusion (not shown) on the side surface of the electrode 60 and to support the short-circuit prevention plate 80 by this protrusion.

短絡防止板８０には開口凹部８１が設けられているので、電極６０に装着したときに、この部分を通じて液滴が流下しないように、短絡防止板８０を少なくとも二枚用い、これら短絡防止板８０の開口凹部８１の向きが重ならないように、該短絡防止板８０を上下に重ねて電極６０に装着させると良い。図１は二枚の短絡防止板８０を用いた例である。 Since the opening recess 81 is provided in the short-circuit prevention plate 80, at least two short-circuit prevention plates 80 are used so that the liquid droplets do not flow through this portion when the electrode 60 is attached to the short-circuit prevention plate 80. The short-circuit prevention plate 80 may be attached to the electrode 60 so as to overlap each other so that the direction of the opening recess 81 does not overlap. FIG. 1 shows an example in which two short-circuit prevention plates 80 are used.

また、短絡防止板８０を電極６０に装着させる際、電極６０と反応炉１０との間に介設されている絶縁材４０よりも上側の部分に短絡防止板８０を設けるのが好ましい。図１に示す例では、絶縁材４０の上端に接して短絡防止板８０が装着されている。絶縁材４０よりも上側に短絡防止板８０を設けることによって、副生ポリマーの液滴が絶縁材４０に接触しないように、該液滴の流下を確実に防止することができる。 Further, when the short-circuit prevention plate 80 is attached to the electrode 60, it is preferable to provide the short-circuit prevention plate 80 in a portion above the insulating material 40 interposed between the electrode 60 and the reaction furnace 10. In the example shown in FIG. 1, a short-circuit prevention plate 80 is attached in contact with the upper end of the insulating material 40. By providing the short-circuit prevention plate 80 above the insulating material 40, it is possible to reliably prevent the droplets from flowing down so that the by-product polymer droplets do not contact the insulating material 40.

さらに、この短絡防止板は凹部８１の部分に電極６０を嵌合して装着するので、着脱自在であり、短絡防止板の上側に多結晶シリコンが析出して堆積量が多くなったときには容易に交換することができる。 Further, since the electrode 60 is fitted and attached to the concave portion 81, the short-circuit prevention plate is detachable, and it is easy to deposit when polycrystalline silicon is deposited on the upper side of the short-circuit prevention plate. Can be exchanged.

原料ガスの反応によって副生したクロロシランポリマーの液滴は、短絡防止板によって流下が阻止され、一部は蒸発する。さらに短絡防止板よりも下側の部分は短絡防止板によって覆われた状態になるので、短絡防止板より下側の部分には原料ガスが触れ難くなり、さらに、シリコン芯材から受ける放射熱が少なくなるので、この部分では原料ガスが多結晶シリコンに転化し難くくなる。従って、多結晶シリコンが殆ど析出しないので電極の短絡が確実に防止される。 The chlorosilane polymer droplets by-produced by the reaction of the raw material gas are prevented from flowing by the short-circuit prevention plate, and partly evaporate. Furthermore, since the part below the short-circuit prevention plate is covered with the short-circuit prevention plate, it becomes difficult for the raw material gas to touch the part below the short-circuit prevention plate, and the radiant heat received from the silicon core material is further reduced. Therefore, in this portion, the source gas is difficult to convert to polycrystalline silicon. Therefore, since the polycrystalline silicon hardly precipitates, the short circuit of the electrode is surely prevented.

短絡防止板を電極まわりに張り出して設けた反応炉を用いて多結晶シリコンを製造した。一枚の短絡防止板を用いた場合（実施例１）、二枚の短絡防止板を開口凹部が重ならないように上下に設けた場合（実施例２）について、短絡発生率を表１に示した。また、短絡防止板を用いない場合を比較例として示した。実施例１では短絡発生率が比較例の概ね１／４以下であり、実施例２では短絡が発生せず、いずれも確実に短絡が防止されている。 Polycrystalline silicon was produced using a reactor provided with a short-circuit prevention plate extending around the electrode. Table 1 shows the short-circuit occurrence rate when one short-circuit prevention plate is used (Example 1) and two short-circuit prevention plates are provided vertically so that the opening recesses do not overlap (Example 2). It was. Moreover, the case where a short circuit prevention board is not used was shown as a comparative example. In Example 1, the short-circuit occurrence rate is approximately ¼ or less of that of the comparative example, and in Example 2, no short-circuit occurs, and both are reliably prevented from being short-circuited.

Figure 2007107030
Figure 2007107030

本発明の短絡防止板の装着状態を示す説明図Explanatory drawing which shows the mounting state of the short-circuit prevention board of this invention 本発明の短絡防止板の平面図Plan view of the short-circuit prevention plate of the present invention 多結晶シリコン製造装置の概略模式図Schematic diagram of polycrystalline silicon manufacturing equipment

符号の説明Explanation of symbols

１０−反応炉、３０−ベルジャ、５０−シリコン芯材、４０−絶縁材、６０−電極、６１−ホルダー、７０−原料ガス供給ノズル、８０−短絡防止板、８１−開口凹部、９０−原料ガス供給管路、９２−流量調整弁、９３−排出口、９４−排出管路。 10-reactor, 30-belger, 50-silicon core material, 40-insulating material, 60-electrode, 61-holder, 70-source gas supply nozzle, 80-short-circuit prevention plate, 81-opening recess, 90-source gas Supply line, 92-flow regulating valve, 93-discharge port, 94-discharge line.

Claims (5)

多結晶シリコンの製造反応炉に設置された電極に板材を装着し、該板材が電極まわりに張り出すように設けることによって、電極まわりの液滴の流下を阻止し、液滴の析出と堆積による短絡を防止することを特徴とする電極の短絡防止方法。
Polycrystalline silicon production A plate is attached to the electrode installed in the reactor, and the plate is provided so that it protrudes around the electrode, thereby preventing the flow of droplets around the electrode, and by depositing and depositing droplets. An electrode short-circuit prevention method characterized by preventing a short circuit.
側方に開口する凹部を有する板材によって形成した短絡防止板を少なくとも二枚用い、これら短絡防止板の開口凹部の向きが重ならないように、該短絡防止板を上下に重ねて電極に装着し、該短絡防止材が電極まわりに張り出すように設けることによって、電極まわりの液滴の流下を阻止する請求項１に記載する電極の短絡防止方法。
Using at least two short-circuit prevention plates formed by a plate material having a concave portion that opens to the side, the short-circuit prevention plates are stacked on top and bottom so that the orientation of the opening concave portions of these short-circuit prevention plates does not overlap, 2. The method for preventing an electrode from being short-circuited according to claim 1, wherein the short-circuit preventing material is provided so as to project around the electrode, thereby preventing the liquid droplet from flowing around the electrode.
電極と反応炉との間に介設されている絶縁材の上側に短絡防止板を設けて、電極まわりの液滴の流下を阻止する請求項１または２に記載する電極の短絡防止方法。
The method for preventing an electrode from being short-circuited according to claim 1 or 2, wherein a short-circuit prevention plate is provided on an upper side of an insulating material interposed between the electrode and the reaction furnace to prevent a liquid droplet from flowing around the electrode.
多結晶シリコンの製造反応炉に設置された電極に装着される短絡防止板であって、側方に開口する凹部を有する板材によって形成されており、該凹部が電極の軸まわりに装入されることによって該板材が電極まわりに張り出して装着され、電極まわりの液滴の流下を阻止することを特徴とする電極の短絡防止板。
A short-circuit prevention plate attached to an electrode installed in a reactor for producing polycrystalline silicon, which is formed of a plate material having a concave portion that opens to the side, and the concave portion is inserted around the axis of the electrode. An electrode short-circuit prevention plate, wherein the plate material is mounted so as to protrude around the electrode and prevents the liquid droplet from flowing around the electrode.
カーボン製の板材によって形成された請求項４に記載する電極の短絡防止板。


The electrode short-circuit prevention plate according to claim 4, which is formed of a carbon plate material.


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