WO2012153465A1 - シリコン芯線ホルダおよび多結晶シリコンの製造方法 - Google Patents
シリコン芯線ホルダおよび多結晶シリコンの製造方法 Download PDFInfo
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- WO2012153465A1 WO2012153465A1 PCT/JP2012/002623 JP2012002623W WO2012153465A1 WO 2012153465 A1 WO2012153465 A1 WO 2012153465A1 JP 2012002623 W JP2012002623 W JP 2012002623W WO 2012153465 A1 WO2012153465 A1 WO 2012153465A1
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- core wire
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
Definitions
- Siemens method is known as a method for producing polycrystalline silicon which is a raw material of single crystal silicon for semiconductor production or silicon for solar cell production.
- the Siemens method is a method in which a source gas containing chlorosilane is brought into contact with a heated silicon core wire, and polycrystalline silicon is vapor-phase grown on the surface of the silicon core wire by using a CVD (Chemical Vapor Deposition) method.
- CVD Chemical Vapor Deposition
- a source gas for example, a mixed gas of trichlorosilane and hydrogen is supplied from the gas nozzle into the reactor.
- Silicon contained in the source gas is deposited (vapor phase growth) as polycrystalline silicon on the silicon core wire, and a polycrystalline silicon rod having a desired diameter is formed in an inverted U shape.
- FIG. 1 is a schematic cross-sectional view for explaining a state in which a silicon core wire is held by a core wire holder in a conventional manner.
- the cross section of the silicon core wire 5 is generally rectangular, and in this case, the cross section of the hole 21 formed in the core wire holder 20 is also square.
- the end portion of the silicon core wire is inserted into the hole having the rectangular cross section, and is pressed and fixed to two adjacent surfaces among the four surfaces of the inner surface of the hole 21 by a rod-like fastening member 40 or the like.
- the current supplied from the metal electrode to the lower end side of the core wire holder 20 flows into the silicon core wire 5 from the two surfaces that are in close contact with the end of the silicon core wire. Since the current that has flowed into the silicon core wire 5 flows to the upper side of the silicon core wire 5 with the shortest distance, the silicon core wire 5 on the second surface side that is in close contact with the silicon core wire 5 among the four surfaces of the inner surface of the hole 21 of the core wire holder 20. Heat generation at the part is promoted as compared with the part of the silicon core wire 5 on the non-contact two-surface side.
- FIG. 2 is a schematic cross-sectional view for explaining a state in which the silicon core wire is held by the core wire holder in another conventional mode, but the silicon core wire 5 has a circular cross section and is formed in the core wire holder 20. Even when the cross section of 21 is circular, a non-contact portion with the silicon core wire 5 is formed on the inner surface of the hole 21, and the same problem as described above occurs.
- Patent Document 3 discloses a holding portion in which a portion for holding a silicon core wire is divided into three or more symmetrically in order to suppress damage due to initial heating.
- Patent Document 4 in order to obtain a good contact between the silicon core wire and the core wire holder, silicon to be held by a cap mechanism having a gap provided in a part of the core wire holder and having a taper. A method of tightening the lower end portion of the core wire has been proposed.
- the silicon core wire holder is a holder for holding a silicon core wire used when manufacturing polycrystalline silicon by the Siemens method
- the main body of the holder Includes a hole extending from the upper surface toward the lower surface, a core wire insertion hole for inserting the silicon core wire, and a slit-shaped gap portion positioned on a virtual plane including the central axis of the core wire insertion hole, or the virtual space
- a slit-like gap portion located on a plane parallel to the plane, the gap portion extending from the core wire insertion hole to the outer surface of the holder body is provided, and tightened so that the gap portion is narrowed.
- a fixing member for fixing the silicon core wire inserted in the core wire insertion hole is provided.
- a silicon core wire holder is a holder for holding a silicon core wire used in the production of polycrystalline silicon by the Siemens method, and the main body of the holder has a hole from the upper surface toward the lower surface side.
- the silicon core wire holder of the present invention If the silicon core wire holder of the present invention is used, the silicon core wire can be fixed substantially symmetrically and evenly from both ends of the core wire insertion hole. For this reason, the thermal environment such as heat conduction and heat radiation becomes uniform from the beginning of the precipitation reaction, and as a result, the shape of the deposited polycrystalline silicon becomes symmetrical with respect to the axis.
- 3A to 3C are views for explaining a configuration example of the silicon core wire holder according to the first aspect of the present invention, and are a side view, a front view, and a top view, respectively.
- a portion that can obtain the same action is formed on the upper portion of the main body of the holder 20 without using the plate-like member 31 c as shown in FIG. 3C. May be. And you may make it use the fixing member 31 of the structure which passes a bolt-shaped member (fixed shaft) through the hole (fixed member insertion hole) provided in the said site
- a convex portion 31 a that is one of the fixing members 31 is formed in the holder body 20 in a male screw shape, and the convex portion 31 a and the other of the fixing member 31 are formed.
- the silicon core wire 5 may be fixed by tightening so that the gap 60 is narrowed by a combination of certain nut-like members 31b.
- FIG. 7A and 7B are views for explaining a configuration example of the silicon core wire holder according to the second aspect of the present invention, and are a sectional view and a top view, respectively.
- the insertion hole 30 of the fixing member 31 penetrating the core wire holder is provided on the truncated cone-shaped slope near the opening 22.
- the silicon core wire 5 inserted into the core wire insertion hole 21 is provided with a through hole 32 at the same height as the insertion hole 30 provided in the holder body 20.
- FIG. 12 is a schematic explanatory diagram showing an example of a vapor phase growth apparatus 100 in which the present invention is used.
- the vapor phase growth apparatus 100 is an apparatus for vapor growth of polycrystalline silicon 6 on the surface of the silicon core wire 5 by the Siemens method, and is roughly constituted by the base plate 1 and the reaction furnace 10.
- the core wire holder 20 is a carbon electrode made of graphite.
- the reason why the heat conduction is 145 W / m ⁇ K or less depends on the results of the study by the present inventors. However, the lower the thermal conductivity of the core wire holder 20 itself, the lower the amount of heat that escapes to the metal electrode 2, thereby This is because the effect works and the temperature of the upper part of the core wire holder 20 can be kept high. If the temperature of the upper part of the core wire holder 20 can be kept high, the temperature of the lower part of the silicon core wire at the time of energization can be kept high, so that the applied voltage can be lowered and damage at the time of energization can be suppressed. Also, the deposition rate of polycrystalline silicon at the initial stage of the reaction at this portion can be increased.
- the through hole 32 is opened so that the bolt 31 a which is a common fixed shaft passes through the through hole 32 of the core wire holder and the insertion hole 30 of the silicon core wire 5.
- a silicon core wire 5 was used.
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
Description
上端側が円錐台状で、芯線挿入孔21の開口部22から10mm離れた円錐台の斜面位置に、芯線挿入孔21に向かって4mmネジの挿入孔30が形成され、開口部22には縦方向にスリット60の入ったグラファイト製芯線ホルダ20を用いた。
実施例1と同じタイプのグラファイト製芯線ホルダ20を用い、該芯線ホルダ20に保持されたシリコン芯線5を1050℃に加熱しながら、水素ガスとともにトリクロロシランガスを原料ガスとして供給した。気相成長開始後12時間の成長速度抑制期間で、芯線ホルダ20の第一端側は多結晶シリコン6の析出により均等に被覆された。その際、多結晶シリコン6の直径は13mm、電流値は195Aであった。この時点から供給ガス量アップを始め、その後、多結晶シリコン棒の径の成長に伴い電流値を上げ、62時間で119mm径の多結晶を得ることができた。
実施例1と同じ材料からなるグラファイト製の芯線ホルダ20であって、図1に示す構造の従来タイプの芯線ホルダ20を用いた。この芯線ホルダ20に保持されたシリコン芯線5を1055℃に加熱しながら、水素ガスとともにトリクロロシランガスを原料ガスとして供給した。気相成長開始後16時間の成長速度抑制期間で、多結晶シリコン6の直径は18mm、電流値は240Aであった。実施例1および2と同様に、供給ガス量アップを開始した後に電流値を上げ始めたが、この時点で既に、芯線ホルダ20の上端側での多結晶シリコン6の析出形状は図10に示したように不均一なものとなっていた。その後も電流値を514Aとして成長を継続したところ、多結晶シリコン6の直径が36mmとなったところで多結晶シリコン棒は倒れてしまい、反応継続ができなかった。
比較例1と同様に反応初期条件を制御して多結晶シリコンの析出を行った。33時間で多結晶シリコン6の直径が35mmとなったところで芯線ホルダ20の上端側での多結晶シリコン6の析出が均一となった。その後、供給ガス量アップを開始して電流値を上げ始めた。87時間の析出で121mm径の多結晶シリコン棒を得ることができた。
2 金属電極
3 ガスノズル
4 排気口
5 シリコン芯線
6 多結晶シリコン
7 絶縁物
10 反応炉
20 芯線ホルダ
21 芯線挿入孔
22 開口部
30 固定部材の挿入孔
31 固定部材
32 貫通孔
40 棒状の締付部材
60 スリット状の間隙部
61 導電性シート
100 気相成長装置
Claims (7)
- シーメンス法による多結晶シリコン製造時に用いられるシリコン芯線を保持するためのホルダであって、
前記ホルダの本体には、上面から下面側に向かう孔部であって前記シリコン芯線を挿入するための芯線挿入孔と、前記芯線挿入孔の中心軸を含む仮想平面上に位置するスリット状の間隙部もしくは該仮想平面と平行な面上に位置するスリット状の間隙部であって前記芯線挿入孔から前記ホルダ本体の外側面にまで至る間隙部が設けられており、
前記間隙部の間隔が狭まるように締め付けて前記芯線挿入孔内に挿入された前記シリコン芯線の固定を行う固定部材を備えている、シリコン芯線ホルダ。 - シーメンス法による多結晶シリコン製造時に用いられるシリコン芯線を保持するためのホルダであって、
前記ホルダの本体には、上面から下面側に向かう孔部であって前記シリコン芯線を挿入するための芯線挿入孔と、前記芯線挿入孔の中心軸を含む仮想平面上に位置するスリット状の間隙部もしくは該仮想平面と平行な面上に位置するスリット状の間隙部であって前記芯線挿入孔から前記ホルダ本体の外側面にまで至る間隙部と、前記芯線挿入孔の中心軸を通り且つ前記仮想平面に垂直な方向に固定部材挿入孔が設けられており、
前記固定部材挿入孔から前記シリコン芯線の下端側に設けられた貫通孔を通るように挿入され、前記間隙部の間隔が狭まるように締め付けて前記芯線挿入孔内に挿入された前記シリコン芯線の固定を行う固定部材を備えている、シリコン芯線ホルダ。 - 前記間隙部は、前記芯線挿入孔の中心軸に対してn回対称(nは2以上の整数)の関係にある前記ホルダ本体の外側面にまで至るn個のスリット状の間隙部として設けられている、請求項1又は2に記載のシリコン芯線ホルダ。
- 前記スリット状の間隙部の下端は、前記ホルダ本体の底面より高い位置にあり、前記ホルダ本体の底面が分割されていない、請求項1又は2に記載のシリコン芯線ホルダ。
- 前記スリット状の間隙部の下端は、前記ホルダ本体の底面にまで達しており、前記ホルダ本体の底面が分割されている、請求項1又は2に記載のシリコン芯線ホルダ。
- 前記ホルダ本体は、曲げ強さが10MPa以上でショア硬さが20以上の強度を有する材料からなる、請求項1又は2に記載のシリコン芯線ホルダ。
- 請求項1又は2に記載のシリコン芯線ホルダを用い、前記シリコン芯線を前記芯線挿入孔内に挿入するに際して、前記ホルダ本体と前記シリコン芯線との接触面に抵抗率が1500μΩ-cm以下の導電性シートを挟み込み、前記シリコン芯線に通電した際の前記ホルダ本体と前記シリコン芯線との接触面における接触抵抗を下げる、ことを特徴とする多結晶シリコンの製造方法。
Priority Applications (4)
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EP12782705.3A EP2708508B1 (en) | 2011-05-09 | 2012-04-16 | Silicon core wire holder and method for manufacturing polycrystalline silicon |
KR1020137032515A KR20140033095A (ko) | 2011-05-09 | 2012-04-16 | 실리콘 심선 홀더 및 다결정 실리콘의 제조 방법 |
US14/110,959 US20140030440A1 (en) | 2011-05-09 | 2012-04-16 | Silicon core wire holder and polycrystalline silicon manufacturing method |
CN201280022814.4A CN103517873B (zh) | 2011-05-09 | 2012-04-16 | 硅芯线支架及多晶硅的制造方法 |
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JP2011104183A JP5666983B2 (ja) | 2011-05-09 | 2011-05-09 | シリコン芯線ホルダおよび多結晶シリコンの製造方法 |
JP2011-104183 | 2011-05-09 |
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JP2012232879A (ja) * | 2011-05-09 | 2012-11-29 | Shin-Etsu Chemical Co Ltd | シリコン芯線ホルダおよび多結晶シリコンの製造方法 |
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KR102270479B1 (ko) * | 2014-10-15 | 2021-06-29 | 삼성전자주식회사 | 디스플레이 장치, 서버, 및 디스플레이 장치의 제어방법 |
JP2018065710A (ja) | 2016-10-18 | 2018-04-26 | 信越化学工業株式会社 | 多結晶シリコン塊、多結晶シリコン棒、および単結晶シリコンの製造方法 |
CN112424121A (zh) * | 2018-07-23 | 2021-02-26 | 株式会社德山 | 芯线支架、硅制造装置及硅制造方法 |
JP7345441B2 (ja) * | 2020-07-02 | 2023-09-15 | 信越化学工業株式会社 | 多結晶シリコン製造装置 |
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2012
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- 2012-04-16 KR KR1020137032515A patent/KR20140033095A/ko not_active Application Discontinuation
- 2012-04-16 EP EP12782705.3A patent/EP2708508B1/en active Active
- 2012-04-16 US US14/110,959 patent/US20140030440A1/en not_active Abandoned
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EP2708508B1 (en) | 2015-11-25 |
CN103517873A (zh) | 2014-01-15 |
JP2012232878A (ja) | 2012-11-29 |
EP2708508A1 (en) | 2014-03-19 |
KR20140033095A (ko) | 2014-03-17 |
JP5666983B2 (ja) | 2015-02-12 |
US20140030440A1 (en) | 2014-01-30 |
EP2708508A4 (en) | 2014-12-31 |
CN103517873B (zh) | 2016-04-13 |
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