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WO2013035498A1 - Procédé de fabrication d'un lingot de silicium polycristallin - Google Patents

Procédé de fabrication d'un lingot de silicium polycristallin Download PDF

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Publication number
WO2013035498A1
WO2013035498A1 PCT/JP2012/070605 JP2012070605W WO2013035498A1 WO 2013035498 A1 WO2013035498 A1 WO 2013035498A1 JP 2012070605 W JP2012070605 W JP 2012070605W WO 2013035498 A1 WO2013035498 A1 WO 2013035498A1
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WO
WIPO (PCT)
Prior art keywords
crucible
polycrystalline silicon
silicon ingot
silicon
resistance heater
Prior art date
Application number
PCT/JP2012/070605
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English (en)
Japanese (ja)
Inventor
直行 塩塚
大石　隆一
和也 上野
梶本　公彦
Original Assignee
シャープ株式会社
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Filing date
Publication date
Application filed by シャープ株式会社 filed Critical シャープ株式会社
Publication of WO2013035498A1 publication Critical patent/WO2013035498A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003—Heating or cooling of the melt or the crystallised material
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/007—Mechanisms for moving either the charge or the heater
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon

Definitions

  • the present invention relates to a method for producing a polycrystalline silicon ingot.
  • the casting method is a method for producing a silicon ingot by solidifying molten silicon in a crucible serving as a mold.
  • a method for solidifying molten silicon in a crucible a solid silicon raw material is charged into a crucible and melted into molten silicon, and then a molten silicon is solidified in the same crucible.
  • a silicon raw material is charged into a crucible and melted to form molten silicon, then the molten silicon is transferred into another crucible, and the molten silicon is solidified in the crucible.
  • the molten silicon is solidified while applying a temperature gradient in one direction from the bottom of the crucible, so that metal impurities (Fe, Al, Ti, etc.) with a small segregation coefficient are siliconized.
  • metal impurities Fe, Al, Ti, etc.
  • One-way solidification is widely performed by agglomerating at the upper end of the ingot and reducing the metal impurity concentration in a portion other than the upper end to about several ppm.
  • a wafer having a low impurity concentration can be obtained by manufacturing a wafer from a silicon ingot from which the upper end portion having a high metal impurity concentration is removed.
  • foreign matter including impurities such as nitrides and carbides precipitated in the silicon ingot may be generated. Large ones of these foreign substances can be identified visually or with a camera, but it is difficult to remove the foreign substances contained in the silicon ingot.
  • the small foreign material is about 10 ⁇ m in size, as described in, for example, 22nd European Photovoltaic Solar Energy Conference, 3-7 September 2007, Milan, Italy, p.994-997 (Non-patent Document 1). It is very small. Therefore, it is very difficult to identify foreign substances contained in the silicon ingot before putting the silicon ingot into the solar cell production line.
  • the wire saw wire When a silicon ingot containing foreign material is put into a solar cell production line, the wire saw wire may be cut when the wafer is cut out.
  • a device such as a solar cell is manufactured using a wafer including a foreign substance, a leakage current is generated by the foreign substance and the solar cell becomes defective, which causes a decrease in yield.
  • compositional supercooling occurs at the solid-liquid interface when solidifying molten silicon, resulting in instability of the solid-liquid interface and dendrite growth and cell growth.
  • the quality of the polycrystalline silicon is deteriorated due to the occurrence of a large disturbance in the crystalline state.
  • Patent Document 1 Japanese Patent Laid-Open Nos. 5-254817 (Patent Document 1) and 10-182135 (Patent Documents). 2) and JP-A-10-25190 (Patent Document 3).
  • JP-A-5-254817 Japanese Patent Laid-Open No. 10-182135 Japanese Patent Laid-Open No. 10-25190
  • the molten silicon is agitated by an induction heating method in which a magnetic field is applied using a coil to discharge impurities, but the apparatus is very expensive, There is a need to use a conductive material such as a graphite member as a material, and there is no freedom in selecting a material for the crucible.
  • the molten silicon is stirred by blowing an inert gas into the molten silicon above the solidification interface, but the gas pipe for blowing the inert gas is provided in the molten silicon. Therefore, the molten silicon is contaminated, and the degree of freedom in selecting the material of the gas pipe is low in terms of heat resistance.
  • Patent Document 3 when preparing a melt to be fed into a crystal growth crucible of a single crystal pulling furnace, a solid material is supplied to a melting vessel held in an Ar atmosphere, Three-phase alternating current is supplied to 3n (n is a natural number) resistance heaters arranged at equal intervals around the solid material, and the solid material is heated and dissolved while a rotating magnetic field generated by the three-phase alternating current is applied.
  • 3n is a natural number
  • the present invention has been made in view of the above problems, and an object of the present invention is to provide a method for producing a polycrystalline silicon ingot capable of producing a high-quality polycrystalline silicon ingot.
  • the method for producing a polycrystalline silicon ingot according to the present invention supplies a three-phase alternating current to 3n (n is a natural number) resistance heaters arranged around a crucible, and acts on a rotating magnetic field generated by the three-phase alternating current.
  • the frequency of the three-phase alternating current is 50 Hz or more and 1000 Hz or less.
  • a high-quality polycrystalline silicon ingot can be produced.
  • FIG. 5 It is a partial cross section figure which shows the structure of the manufacturing apparatus for enforcing the manufacturing method of the polycrystalline silicon ingot which concerns on one Embodiment of this invention. It is the figure seen from the II-II line arrow direction of FIG. 5 is a graph showing changes in wire disconnection rate, foreign matter contamination rate, and leakage current failure rate with three-phase AC frequency in the method for producing a polycrystalline silicon ingot according to the embodiment.
  • FIG. 1 is a partial cross-sectional view showing a configuration of a manufacturing apparatus for carrying out a method for manufacturing a polycrystalline silicon ingot according to an embodiment of the present invention.
  • FIG. 2 is a view as seen from the direction of arrows II-II in FIG.
  • a manufacturing apparatus 1 for carrying out a method for manufacturing a polycrystalline silicon ingot according to an embodiment of the present invention includes a substantially rectangular parallelepiped casing 10 made of stainless steel.
  • An opening 11 for introducing one end of a gas supply pipe 13 to be described later into the interior of the housing 10 is provided in the upper portion of the housing 10.
  • An exhaust port 12 for exhausting the inside of the housing 10 is provided in the lower portion of the housing 10.
  • a crucible 20 is arranged inside the housing 10.
  • the crucible 20 is mounted on the mounting table 40.
  • the crucible 20 is made of silica.
  • the material of the crucible 20 is not limited to silica but may be graphite.
  • Silicon nitride powder is applied to the inner surface of the crucible 20 in order to prevent reaction with molten silicon. The silicon nitride powder is dried and then sintered.
  • the mounting table 40 is mounted on the support table 50.
  • the mounting table 40 and the support table 50 are formed of a material having high thermal conductivity and heat resistance.
  • the support base 50 is connected to the support part 71 at the lower part.
  • the support portion 71 is connected to a drive portion 70 disposed outside the housing 10 so as to be movable up and down as indicated by an arrow 72.
  • the drive unit 70 has a motor.
  • the driving unit 70 is connected to a cooling unit 90 disposed outside the housing 10.
  • the cooling unit 90 cools the drive unit 70 and the support unit 71 by circulating a cooling medium inside the drive unit 70 and the support unit 71.
  • the cooling unit 90 includes a pump and a heat exchanger. By cooling the support part 71 by the cooling part 90, the bottom part of the crucible 20 can be cooled via the support table 50 and the mounting table 40.
  • a resistance heater 30 is disposed around the crucible 20.
  • the resistance heater 30 includes a first resistance heater 31, a second resistance heater 32, and a third resistance heater 33 arranged so as to surround the crucible 20 with a space therebetween.
  • each of the first resistance heater 31 and the second resistance heater 32 has a bent shape and the third resistance heater 33 has a linear shape in plan view.
  • the shapes of the first resistance heater 31, the second resistance heater 32, and the third resistance heater 33 are not limited to the above, and may be curved in plan view.
  • Each of the first resistance heater 31, the second resistance heater 32, and the third resistance heater 33 is connected to a three-phase AC power supply 34 disposed outside the housing 10.
  • the three-phase AC power supply 34 has three systems u, v, and w. Three systems of the three-phase AC power supply 34 and the resistance heater 30 are connected to each other.
  • the u system of the three-phase AC power supply 34 and the first resistance heater 31 are connected.
  • the v system of the three-phase AC power supply 34 and the second resistance heater 32 are connected.
  • the w system of the three-phase AC power supply 34 and the third resistance heater 33 are connected.
  • An inner lid 60 made of a heat insulating material is disposed above the support base 50.
  • the inner lid 60 has a side wall that surrounds the resistance heater 30 and a ceiling that faces the support base 50.
  • the ceiling is provided with a hole for introducing one end of the gas supply pipe 13 into the inner lid 60.
  • the inner side of the inner lid 60 surrounded by the side wall portion and the ceiling portion is a heating region 61.
  • thermocouple (not shown) is arranged in the heating area 61.
  • the thermocouple is connected to a three-phase AC power source 34.
  • the voltage applied to the resistance heater 30 is controlled by feeding back the temperature measured by the thermocouple to the three-phase AC power supply 34.
  • the gas supply pipe 13 One end of the gas supply pipe 13 is positioned above the crucible 20 in the heating region 61, and the other end is connected to a gas supply unit (not shown) disposed outside the housing 10.
  • An inert gas such as Ar sent from the gas supply unit passes through the inside of the gas supply pipe 13 and is supplied into the heating region 61.
  • the gas supply unit includes a plurality of gas cylinders storing various gases and a mass flow controller.
  • the exhaust port 12 is connected to an exhaust unit (not shown) disposed outside the housing 10.
  • the exhaust part includes various vacuum pumps.
  • the inert gas supplied into the heating region 61 passes through the exhaust port 12 and is discharged to the outside of the housing 10.
  • the three-phase AC power supply 34 is turned on and a voltage is applied to the resistance heater 30.
  • a voltage is applied to the resistance heater 30
  • the temperature in the heating region 61 rises.
  • the temperature in the heating region 61 is raised to 1550 ° C. and held for 2 hours. Silicon having a melting point of 1410 ° C. is completely melted in the crucible 20.
  • molten silicon previously melted may be put into the crucible 20, and similarly, decompression, Ar gas supply, and exhaust amount adjustment may be performed.
  • the three-phase AC power supply 34 is turned on and a voltage is applied to the resistance heater 30 so that the molten silicon placed in the crucible 20 does not solidify. Good.
  • a rotating magnetic field in the direction indicated by an arrow 81 acts on the molten silicon 80 by three-phase alternating current supplied to the resistance heater 30. Specifically, the voltages of the three systems u, v, and w whose phases are shifted by 120 degrees are applied to the first resistance heater 31, the second resistance heater 32, and the third resistance heater 33, respectively. The rotational force in the same direction as the rotational direction of the rotating magnetic field acts on the molten silicon 80. As a result, the molten silicon 80 is stirred in the circumferential direction. In the vertical direction, the molten silicon 80 is stirred by thermal convection.
  • the voltage applied to the resistance heater 30 is lowered so that the temperature of the molten silicon 80 is close to the melting point.
  • the voltage applied to the resistance heater 30 is further lowered while operating the drive unit 70 to move the support unit 71 downward.
  • the bottom of the crucible 20 is positioned outside the heating region 61. Therefore, the bottom of the crucible 20 is cooled by operating the cooling unit 90. As a result, the crucible 20 is cooled from the bottom toward the top. In this way, the molten silicon 80 is gradually cooled at a cooling rate of about 1 ° C./hour while a rotating magnetic field is applied to the molten silicon 80 located in the heating region 61.
  • the molten silicon 80 is solidified in order from the bottom, and stirring of the unsolidified molten silicon 80 by the rotating magnetic field is maintained.
  • the generation of foreign substances including impurities such as carbides and nitrides precipitated in the polycrystalline silicon ingot is effectively suppressed. it can. It is also possible to suppress destabilization of the solid-liquid interface due to the occurrence of compositional supercooling.
  • the concentration of impurities contained in solid-phase silicon follows the following Scheil equation using a distribution (segregation) coefficient at the solid-liquid interface.
  • C s k ⁇ C 0 (1-f s ) k-1
  • C s Concentration of impurities contained in silicon in solid phase
  • C 0 Initial concentration of impurities contained in molten silicon before solidification
  • k Distribution (segregation) coefficient
  • fs Ratio of solid phase Distribution coefficient k is type of impurity element It varies depending on factors such as the solidification speed of molten silicon and the stirring speed of molten silicon.
  • the distribution coefficient k is reduced by stirring the molten silicon with a rotating magnetic field. Therefore, the concentration of impurities contained in the solid phase silicon is reduced, and precipitation of impurities such as silicon nitride and silicon carbide can be suppressed.
  • the gas sent from the gas supply unit is changed from Ar to He. Thereafter, the polycrystalline silicon ingot is cooled to room temperature.
  • ⁇ Remove the ends containing many impurities and crystal defects from the polycrystalline silicon ingot, cut into a predetermined size, and form blocks. Further, a plurality of wafers can be obtained by cutting the block-shaped polycrystalline silicon ingot to a predetermined thickness with a wire saw. Since this wafer is made of high-quality polycrystalline silicon in which the precipitation of impurities such as carbides and nitrides is suppressed, it contributes to improving the characteristics of the solar cell when used as a substrate.
  • a solar cell was manufactured using a wafer manufactured by the method for manufacturing a polycrystalline silicon ingot according to this embodiment.
  • the inventor focused on the frequency of the three-phase alternating current supplied to the resistance heater 30 and experimented with the relationship between the frequency and various characteristics of the polycrystalline silicon ingot. Details of the experiment will be described below.
  • the wire disconnection rate of the wire saw that was disconnected when the block-shaped polycrystalline silicon ingot was cut to a predetermined thickness was calculated.
  • the wire breakage rate is the ratio of the number of wire saw breaks to the number of wire saw cuts. The reason why the wire saw is disconnected is that the cutting resistance is rapidly changed by the foreign matter contained in the polycrystalline silicon ingot.
  • the contamination rate of foreign matter contained in the wafer was calculated by visual inspection or image analysis.
  • the foreign matter mixing rate is the ratio of the number of wafers in which foreign matter has been confirmed to the number of manufactured wafers.
  • the leakage current defect rate under the reverse voltage of the fabricated solar cell was calculated.
  • the leakage current defect rate is the ratio of the number of solar cells in which a current of 2.5 A or more flows when a voltage of ⁇ 12 V is applied to the number of manufactured solar cells.
  • the wire disconnection rate, the foreign matter contamination rate, and the leakage current failure rate in the polycrystalline silicon ingot manufacturing method according to this embodiment were calculated.
  • the frequency of the three-phase alternating current was varied in the range of 1 Hz to 2000 Hz, and the wire breakage rate, foreign matter contamination rate, and leakage current failure rate calculated in the comparative example were normalized to 1 respectively.
  • FIG. 3 is a graph showing changes in the wire disconnection rate, foreign matter contamination rate, and leakage current failure rate due to the three-phase AC frequency in the method of manufacturing a polycrystalline silicon ingot according to the present embodiment.
  • the vertical axis shows the wire disconnection rate, foreign matter contamination rate and leakage current failure rate of the example normalized with the calculation result of the comparative example as 1, and the horizontal axis shows the frequency of the three-phase alternating current.
  • the frequency of the three-phase alternating current is 50 Hz or more
  • the wire disconnection rate, the foreign matter contamination rate, and the leakage current failure rate were significantly reduced.
  • the frequency of the three-phase alternating current is in the range of 50 Hz to 1000 Hz
  • the wire disconnection rate, the foreign matter contamination rate, and the leakage current failure rate gradually decreased as the frequency of the three-phase alternating current increased.
  • a high-quality polycrystalline silicon ingot can be manufactured by setting the frequency of the three-phase alternating current to 50 Hz or more and 1000 Hz or less.
  • three resistance heaters are arranged around the crucible 20, but the number of resistance heaters is not limited to this, and may be a natural number multiple of 3 (3n). For example, six resistance heaters may be provided, and two resistance heaters may be connected to each of u, v, and w systems.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne un procédé de fabrication d'un lingot de silicium polycristallin qui comporte : une étape de chauffage dans laquelle un courant alternatif triphasé est fourni à 3n dispositifs de chauffage résistif (n est un nombre naturel) disposés sur la circonférence d'un creuset (20), et un silicium fondu à l'intérieur du creuset (20) est chauffé, tout en faisant agir un champ magnétique tournant, ledit champ magnétique tournant ayant été généré en raison du courant alternatif triphasé ; et une étape de refroidissement dans laquelle le silicium est solidifié par refroidissement du silicium à partir d'une partie inférieure du creuset (20) vers une partie supérieure, tout en faisant agir le champ magnétique en rotation.
PCT/JP2012/070605 2011-09-09 2012-08-13 Procédé de fabrication d'un lingot de silicium polycristallin WO2013035498A1 (fr)

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JP2011197040A JP2013056812A (ja) 2011-09-09 2011-09-09 多結晶シリコンインゴットの製造方法
JP2011-197040 2011-09-09

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6236097A (ja) * 1985-08-07 1987-02-17 Kawasaki Steel Corp 単結晶の製造方法およびその装置
JPH03177392A (ja) * 1989-12-06 1991-08-01 Nippon Steel Corp 単結晶引上げ方法および装置
JPH05254817A (ja) * 1992-03-12 1993-10-05 Kawasaki Steel Corp 多結晶シリコン鋳塊の製造方法
JPH1025190A (ja) * 1996-07-11 1998-01-27 Super Silicon Kenkyusho:Kk 三相交流加熱による結晶原料の溶解方法及び溶解装置
JPH10182135A (ja) * 1996-12-20 1998-07-07 Kawasaki Steel Corp シリコンの凝固精製方法
JP2002201017A (ja) * 2000-12-28 2002-07-16 Sharp Corp シリコン溶湯の精製方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61141612A (ja) * 1984-12-11 1986-06-28 Osaka Titanium Seizo Kk シリコン多結晶の造塊方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6236097A (ja) * 1985-08-07 1987-02-17 Kawasaki Steel Corp 単結晶の製造方法およびその装置
JPH03177392A (ja) * 1989-12-06 1991-08-01 Nippon Steel Corp 単結晶引上げ方法および装置
JPH05254817A (ja) * 1992-03-12 1993-10-05 Kawasaki Steel Corp 多結晶シリコン鋳塊の製造方法
JPH1025190A (ja) * 1996-07-11 1998-01-27 Super Silicon Kenkyusho:Kk 三相交流加熱による結晶原料の溶解方法及び溶解装置
JPH10182135A (ja) * 1996-12-20 1998-07-07 Kawasaki Steel Corp シリコンの凝固精製方法
JP2002201017A (ja) * 2000-12-28 2002-07-16 Sharp Corp シリコン溶湯の精製方法

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