WO2011104796A1 - Silicium polycristallin pour cellule solaire - Google Patents

Silicium polycristallin pour cellule solaire Download PDF

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Publication number
WO2011104796A1
WO2011104796A1 PCT/JP2010/006735 JP2010006735W WO2011104796A1 WO 2011104796 A1 WO2011104796 A1 WO 2011104796A1 JP 2010006735 W JP2010006735 W JP 2010006735W WO 2011104796 A1 WO2011104796 A1 WO 2011104796A1
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Prior art keywords
polycrystalline silicon
lifetime
silicon
crucible
temperature
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PCT/JP2010/006735
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English (en)
Japanese (ja)
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宣正 内藤
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株式会社Sumco
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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
    • 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
    • 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
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/08—Downward pulling
    • 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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/10—Production of homogeneous polycrystalline material with defined structure from liquids by pulling from a melt
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic Table
    • H01L31/182—Special manufacturing methods for polycrystalline Si, e.g. Si ribbon, poly Si ingots, thin films of polycrystalline Si
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/546—Polycrystalline silicon PV cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/547—Monocrystalline silicon PV cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention relates to polycrystalline silicon used as a substrate material for solar cells.
  • Silicon crystals include single crystals and polycrystals.
  • conversion efficiency ratio of energy that can be converted into electrical energy and extracted with respect to incident light energy
  • High solar cells can be manufactured.
  • This silicon single crystal is manufactured by the Czochralski method of pulling and growing a single crystal directly from molten silicon because it requires high-quality, low-defect, dislocation-free crystals equivalent to those used for semiconductor integrated circuit substrate materials. Is done. For this reason, manufacturing cost rises and the manufacturing cost of a solar cell becomes high.
  • polycrystalline silicon is manufactured by a casting method in which high-purity silicon as a raw material is heated and melted in a quartz crucible and solidified in a crucible as it is, or poured into a mold and solidified. Since the substrate material can be manufactured at a lower cost than the Czochralski method, various studies have been conducted for the purpose of increasing the conversion efficiency of the obtained solar cell as much as possible by using this low-cost polycrystalline silicon for the substrate. Has been done.
  • Patent Document 1 discloses polycrystalline silicon to which Ga (gallium) is added as a dopant.
  • This casting method is, for example, a method as disclosed in Patent Document 2, in which electrical conductivity is electrically insulated from each other in the circumferential direction inside the high-frequency induction coil and the interior is water-cooled. And a device with a structure in which strips of objects with good thermal conductivity (usually copper) are arranged.
  • the cross-sectional shape of the coil and the shape of the portion surrounded by the strip-shaped object that becomes the melting container (cooling crucible) may be cylindrical or rectangular.
  • a support base that can move downward is provided at the lower part thereof.
  • the molten silicon hardly comes into contact with the crucible wall, and impurity contamination can be prevented. Since there is no contamination from the crucible, there is an advantage that it is not necessary to use a high-purity material as the material of the crucible. Moreover, since it can cast continuously, manufacturing cost can be significantly reduced.
  • the present invention relates to polycrystalline silicon manufactured by applying a continuous casting method by electromagnetic induction using a cooling crucible, having good crystallinity, a long lifetime, and suitable as a substrate material for solar cells.
  • the purpose is to provide silicon.
  • thermal conditions solidification rate, temperature gradient, etc.
  • the present inventor is in the solidification process in producing a polycrystalline silicon ingot by a continuous casting method using electromagnetic induction using a cylindrical cooling crucible (hereinafter also simply referred to as “electromagnetic induction continuous casting method”).
  • electromagagnetic induction continuous casting method By changing the temperature of the silicon ingot (specifically, the high temperature ingot close to the solidification interface), the lifetime of the silicon ingot obtained under these temperature conditions (resistivity is 1 to 2 ⁇ ⁇ cm The lifetime when a p-type semiconductor was used was measured.
  • the change in the temperature of the silicon ingot in the solidification process was performed by controlling the temperature of a plurality of stages of heat retaining devices (heaters) provided below the cooling crucible (see FIG. 2 described later).
  • the lifetime of the obtained silicon ingot was measured because the lifetime is considered as one of the indicators for electrically evaluating the crystallinity (crystal integrity) of the silicon substrate. This is because the conversion efficiency when a solar cell is configured using a substrate can be evaluated to some extent.
  • the higher the lifetime of the carrier generated by light the higher the conversion efficiency. If there are lattice defects or metal impurities in the substrate, these become trap levels, and carriers disappear due to recombination (that is, the carrier lifetime is short), and conversion efficiency decreases.
  • the lifetime is defined as the time when the carrier concentration decreases to 1 / e due to recombination, and the short time corresponds to the short carrier life. Therefore, by measuring the lifetime of the substrate, it is possible to evaluate the conversion efficiency of the solar cell using the substrate to some extent.
  • the lifetime measurement if the average temperature of the first heat insulating device below the cooling crucible is 1275 ° C. or higher, the lifetime is reduced when the ingot is a p-type semiconductor having a resistivity of 1 to 2 ⁇ ⁇ cm. It was found to be 80 ⁇ sec or more. If the lifetime is within this range, it can be said that there are relatively few crystal defects and the crystallinity is generally good.
  • This invention is made
  • the “region from the solidification interface to 300 mm” means a region from each position of the solidification interface to 300 mm downward (that is, into the solidification phase).
  • the solidification interface is shallow in the vicinity of the periphery of the crucible due to the large heat removal to the outside, and becomes deeper as it approaches the center of the crucible and has a convex shape downward. Therefore, the region from the solidification interface to 300 mm has a shape that is deeply curved at the center of the crucible when viewed in its longitudinal section (see FIG. 2).
  • the region from the solidification interface to 300 mm is 1275 ° C. or higher” is, precisely, the first stage (immediately below the cooling crucible) of the plural stages of heat retaining devices (heaters) provided below the cooling crucible. It means that the average temperature of the heater is 1275 ° C. or higher. It is considered that the temperature of the silicon ingot in the region changes in accordance with the change in the heater temperature. The temperature of the heater was measured by inserting a thermocouple near the middle between the heater and the side of the ingot.
  • the “lifetime after phosphorus diffusion” is the lifetime measured after gettering treatment with phosphorus in order to eliminate the influence of metal impurities that become noise during lifetime measurement.
  • lifetime simply referred to as “lifetime”.
  • the lifetime mentioned here is a lifetime when a p-type semiconductor having a resistivity of 1 to 2 ⁇ ⁇ cm is used.
  • the holding temperature in the region from the solidification interface to 300 mm is 1280 ° C. or more and the lifetime is 100 ⁇ sec or more can be adopted.
  • This polycrystalline silicon can be expected to have higher conversion efficiency when a solar cell is constructed using the polycrystalline silicon as a substrate.
  • the polycrystalline silicon for solar cells of the present invention has good crystallinity and a long lifetime, and is suitable as a substrate material for solar cells.
  • FIG. 1 is a diagram schematically showing a configuration example of an electromagnetic induction continuous casting apparatus suitable for producing polycrystalline silicon for solar cells of the present invention.
  • FIG. 2 is a diagram schematically showing a solidification process at the time of producing an ingot of polycrystalline silicon for solar cells of the present invention.
  • FIG. 3 is a diagram showing the relationship between the average temperature of the first stage heat retaining device of the electromagnetic induction continuous casting device and the lifetime of the obtained polycrystalline silicon as a result of the example.
  • the polycrystalline silicon for solar cells of the present invention is manufactured by an electromagnetic induction continuous casting method using a cooling crucible.
  • FIG. 1 is a diagram schematically showing a configuration example of an electromagnetic induction continuous casting apparatus suitable for producing polycrystalline silicon according to the present invention.
  • a longitudinally long copper plate 3 that can be cooled with water is parallel to the winding axis direction of the induction coil 2 and within the induction coil 2.
  • the support base 4 which can move below is installed in the lower end position of the induction coil 2 for heating.
  • a space surrounded by the support 4 at the bottom and the plate-like piece 3 constitutes a crucible (a cooling crucible in which the interior is water-cooled).
  • the ingot 8 can be drawn downward by the transporting device 6.
  • a heat retention device (heater) 5 for retaining the solidified ingot 8 is installed below the heating induction coil 2. This is because the ingot 8 is rapidly cooled by moving downward from the induction coil 2 for heating, and excessive thermal stress is generated due to the difference in shrinkage due to the temperature difference, and the ingot 8 may be cracked. .
  • a raw material charging machine 9 capable of charging the raw material into the crucible during melting is installed. Further, in this example, a heating element 10 for heating the raw material silicon is attached above the crucible.
  • molten silicon and high-temperature crystals do not come into direct contact with the atmosphere, and the inside of the container 1 is vacuum, inert gas, or reduced pressure. It is configured so that continuous casting can be performed by substituting in an active gas atmosphere.
  • the raw material In the production of polycrystalline silicon, when a silicon raw material is filled in a space corresponding to a crucible and a high frequency induction current is passed through the heating induction coil 2, the raw material generates heat and melts. At this time, the heating element 10 can be used in combination.
  • the molten silicon 7 in the crucible repels the plate-like piece 3 due to the induced current and does not contact the side wall of the crucible. After the molten silicon 7 has become sufficiently uniform, if the support 4 is moved downward little by little, cooling starts by moving away from the induction coil 2, and unidirectional solidification toward the molten silicon 7 in the crucible occurs. proceed.
  • the amount of the molten silicon 7 decreases corresponding to the downward movement of the support 4, the amount of raw silicon is supplied from the raw material feeder 9 so that the upper surface of the molten liquid is always at the same position.
  • the polycrystalline silicon of the present invention is polycrystalline silicon produced by the electromagnetic induction continuous casting method using a cooling crucible as described above, and the region from the solidification interface to 300 mm is maintained at 1275 ° C.
  • the polycrystalline silicon is characterized in that the time is 80 ⁇ sec or more.
  • FIG. 2 is a diagram schematically showing a solidification process during the production of an ingot of polycrystalline silicon for solar cells of the present invention, and shows a longitudinal section including the central axis of the ingot.
  • the molten silicon 7 in the space (crucible) surrounded by the plate-like piece 3 and the support base (not shown) is separated from the induction coil 2 by the downward movement of the support base.
  • the molten silicon 7 begins to cool, but since it is heated by the heat retaining devices (heaters) 5-1, 5-2, there is no sudden temperature drop, and unidirectional solidification toward the molten silicon 7 in the crucible occurs. proceed.
  • the solidification interface is a boundary surface between the molten silicon 7 and the ingot 8 (indicated as S1 in FIG. 2), and is shallow in the vicinity of the crucible because it has a large heat removal outward, and approaches the center of the crucible.
  • Become deeper with. 2 is a vertical cross section of a curved surface of 300 mm from the solidification interface (a cross section including the central axis of the ingot) indicated by a broken line S2 in the ingot 8 in FIG.
  • a region from the solidification interface to 300 mm refers to a region above the curved surface (including the curved surface) indicated by the broken line S2.
  • the region held at the predetermined temperature is the region from the solidification interface to 300 mm, because the temperature of this region up to 300 mm is appropriately controlled, the crystallinity is good, the life This is because polycrystalline silicon having a long time can be obtained.
  • the temperature control of the region up to 300 mm can be performed by controlling the average temperature of the first stage heat retaining device (the heat retaining device 5-1 in FIG. 2) below the cooling crucible.
  • the holding temperature in the region from the solidification interface to 300 mm is set to 1275 ° C. or higher, as shown in the examples described later, by keeping the holding temperature at 1275 ° C. or higher. This is because silicon is obtained.
  • the lifetime is 80 ⁇ sec or more because the retention temperature in the region from the solidification interface to 300 mm is set to 1275 ° C. This is because it can be set to 80 ⁇ sec or more. If the lifetime is within this range, the crystal defects are relatively few and the crystallinity is generally good. If a solar cell is formed using this polycrystalline silicon as a substrate, stable and high conversion efficiency can be expected.
  • the holding temperature in the region from the solidification interface to 300 mm is 1280 ° C. or more and the lifetime is 100 ⁇ sec or more. Since this polycrystalline silicon has a longer lifetime, a higher conversion efficiency can be expected in a solar cell using it as a substrate.
  • the lifetime of the silicon ingot obtained by changing the temperature of the (silicon ingot in the region from the solidification interface to 300 mm) (p-type semiconductor with a resistivity of 1 to 2 ⁇ ⁇ cm) Measured lifetime).
  • a doping material was added to form a p-type semiconductor, and the resistivity was adjusted to 1 to 2 ⁇ ⁇ cm.
  • the change of the temperature of the silicon ingot in the region from the solidification interface to 300 mm was performed by changing the temperature of the heat retaining devices (heaters) 5-1 and 5-2 provided below the cooling crucible.
  • the temperature of the heater was measured by inserting a thermocouple 11 near the middle between the heater and the side of the ingot as illustrated in FIG.
  • the lifetime was measured by the ⁇ -PCD method in which the reflection microwave was used to measure by optical transmission attenuation.
  • FIG. 3 shows lifetime measurement results obtained with the average temperature of the first stage heat retaining device of the electromagnetic induction continuous casting device (in other words, the temperature of the silicon ingot in the region from the solidification interface to 300 mm) and the conditions thereof. It is the figure which showed the relationship with the lifetime of other polycrystalline silicon. Regardless of the electromagnetic induction continuous casting apparatus (furnace) used, a certain correlation is observed between the temperature of the silicon ingot and the lifetime of the polycrystalline silicon.
  • the lifetime becomes longer, and the retention temperature of the region from the solidification interface to 300 mm is set to 1275 ° C. or more, thereby reducing the lifetime of the polycrystalline silicon. It can be seen that it can be maintained at 80 ⁇ sec or more. If the holding temperature is 1280 ° C. or higher, the lifetime can be 100 ⁇ sec or higher.
  • the polycrystalline silicon for solar cells of the present invention has good crystallinity and a long lifetime, and is suitable as a substrate material for solar cells. Therefore, it can be used effectively in the manufacturing field of solar cells, and can greatly contribute to the progress of natural energy utilization technology.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Electromagnetism (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Silicon Compounds (AREA)
  • Photovoltaic Devices (AREA)

Abstract

La présente invention concerne un silicium polycristallin pour cellules solaires qui est fabriqué selon un procédé de moulage continu par induction électromagnétique utilisant un creuset de refroidissement. Le silicium polycristallin, qui présente une excellente cristallinité et une grande longévité et qui convient comme matériau de substrat pour cellules solaires, est produit en maintenant une région à moins de 300 mm de l'interface de solidification à 1275 °C ou plus et en ayant une durée de vie de 80 μsec ou plus après la diffusion du phosphore. La température de la région à moins de 300 mm de l'interface de solidification est de préférence maintenue à 1280 °C ou plus car à cette température, on peut s'attendre à une meilleure efficacité de conversion lorsqu'une cellule solaire est configurée en utilisant comme substrat le silicium polycristallin.
PCT/JP2010/006735 2010-02-25 2010-11-17 Silicium polycristallin pour cellule solaire WO2011104796A1 (fr)

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JP2010-039876 2010-02-25
JP2010039876A JP2011176180A (ja) 2010-02-25 2010-02-25 太陽電池用多結晶シリコン

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110685010A (zh) * 2019-10-30 2020-01-14 晶科能源有限公司 一种高效多晶硅铸锭方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04342496A (ja) * 1991-05-16 1992-11-27 Osaka Titanium Co Ltd 太陽電池用多結晶シリコン鋳塊の製造方法
WO1993012272A1 (fr) * 1991-12-18 1993-06-24 Nobuyuki Mori Procede et appareil de coulee d'un lingot de silicium cristallin par fusion par bombardement electronique
JPH08293619A (ja) * 1995-04-25 1996-11-05 Sanyo Electric Co Ltd 多結晶シリコン半導体，光起電力装置及び多結晶シリコン半導体の形成方法
JP2005200279A (ja) * 2004-01-16 2005-07-28 Sharp Corp シリコンインゴットの製造方法、太陽電池

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04342496A (ja) * 1991-05-16 1992-11-27 Osaka Titanium Co Ltd 太陽電池用多結晶シリコン鋳塊の製造方法
WO1993012272A1 (fr) * 1991-12-18 1993-06-24 Nobuyuki Mori Procede et appareil de coulee d'un lingot de silicium cristallin par fusion par bombardement electronique
JPH08293619A (ja) * 1995-04-25 1996-11-05 Sanyo Electric Co Ltd 多結晶シリコン半導体，光起電力装置及び多結晶シリコン半導体の形成方法
JP2005200279A (ja) * 2004-01-16 2005-07-28 Sharp Corp シリコンインゴットの製造方法、太陽電池

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110685010A (zh) * 2019-10-30 2020-01-14 晶科能源有限公司 一种高效多晶硅铸锭方法

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JP2011176180A (ja) 2011-09-08

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