WO2011096821A1 - Creuset segmenté - Google Patents

Creuset segmenté Download PDF

Info

Publication number
WO2011096821A1
WO2011096821A1 PCT/NO2011/000043 NO2011000043W WO2011096821A1 WO 2011096821 A1 WO2011096821 A1 WO 2011096821A1 NO 2011000043 W NO2011000043 W NO 2011000043W WO 2011096821 A1 WO2011096821 A1 WO 2011096821A1
Authority
WO
WIPO (PCT)
Prior art keywords
crucible
crucible part
incision
silicon
sectioned
Prior art date
Application number
PCT/NO2011/000043
Other languages
English (en)
Inventor
Oddvar SKÅRDAL
Original Assignee
Nordic Ceramics As
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nordic Ceramics As filed Critical Nordic Ceramics As
Publication of WO2011096821A1 publication Critical patent/WO2011096821A1/fr

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Classifications

    • 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
    • C30B11/002—Crucibles or containers for supporting the melt

Definitions

  • the invention regards a crucible for casing silicon, particularly a sectioned crucible with a lower and an upper crucible part, respectively.
  • Polycrystalline silicon in the form of slices is used in large volume in the solar cell or PV-industry (Photo Voltaic). These wafers are manufactured from casted ingots having been manufactured by melting silicon in crucible and then let the silicon solidify in the crucible at a controlled speed. It is an object to manufacture silicon crystals in a cost-effective manner without the silicon being contaminated by impurities from the crucible and without formation of cracks in the crucible. _
  • the quartz crucible can only be used once because it cracks and is destroyed during the process of melting and solidification of the silicon. —
  • the quartz crucible is not stable in terms of shape and high temperatures.
  • the size of the crucibles is limited for technical reasons, for instance since during use large thermal stresses, thermal shock and mechanical loads arise that can easily lead to uncontrolled breakage and cracks in the crucibles.
  • the expansion coefficient for the crucible material and the solidified product must be adapted to the process since different expansion/contraction will lead to large stresses in the crucible material and thus crack formations in the crucibles during temperature changes.
  • the most important reason for the cracking of quartz crucibles during the first time use is frequently different expansion coefficients.
  • the quartz material during the cooling down undergoes a transformation of the binder phase from an amorphous glass phase to a crystalline phase, and this transition leads to crack formations in the quartz material.
  • the raw material is in form of bits, pellets or smaller particles.
  • the object of the invention is to provide a two part crucible that can be reused.
  • a sectioned crucible With a sectioned crucible the inner stresses that form in the wall of the crucible due to temperature gradients arising during cooling down of crucible and melt will be significantly lower than for a corresponding whole crucible.
  • Secondary a sectioned crucible will be more economical in that the upper part of the crucible can be reused several times; it can in principle be used until significant cracks are formed.
  • Other advantages of a sectioned crucible will be that it is easier to handle during production and that the lower crucible part will be better adapted to the finished ingot which makes it easier to sectioned ingot from crucible.
  • This invention provides thus a sectioned crucible for use during manufacturing of polycrystalline silicon, where the crucible is characterized in that it comprises a lower crucible part and an upper crucible part where the ratio between the height of the lower crucible part and the height of the upper crucible part is approximately 3: 1.
  • Fig. 1 shows schematically a crucible with a track around the entire circumference of the crucible.
  • Fig. 2 shows schematically a crucible with nearly quadratic cross sections and with a penetrating incision in each corner.
  • Fig. 3 shows schematically a sectioned crucible with a loose upper crucible part where the upper crucible parts lower edge can reside within the lower crucible part.
  • Fig. 4 shows schematically a sectioned crucible with a loose upper crucible part where the upper crucible part is facing the lower crucible part with coinciding contact faces.
  • the silicon raw material When processing polycrystalline silicon the silicon raw material is brought to melting and to solidify in crucibles that are typically made from a quartz material. As a raw material high grade purity silicon metal is normally used in form of bits, pellets, granulates or powder with different dimensions. During melting the highest temperatures can be more than 1.550 °C. The liquid silicon material is then allowed to solidify in which way the polycrystalline material is formed. At the beginning of the crystal formation the crucible will be subjected to a very rapid cooling (thermal shock). Thermal shock is one of the main causes of crack formations in ceramics, and this is proportional to the dimensions of the ceramics.
  • the crucible When the crucible is prepared for melting, the crucible is filled with so much raw material that it extends into the upper crucible part, yet when the material has liquefied the top surface of the melt will be below the lower edge of the upper crucible part. Therefore, no liquid will leak out in an eventual opening between the crucible parts.
  • a two part crucible will lead to the side wall area of the crucible being reduced significantly, which again leads to stresses due to thermal shock and temperature gradients will be more tolerated by the ceramic material. It appears that the crack formation in the crucibles is reduced and that the crucible can be reused several times ⁇ .
  • the height of the upper and lower crucible part can vary, however in practical experiments it is shown that a beneficial relationship between height of the lower crucible part and the height of the upper crucible part is approximately 3: 1 and in practical use it is necessary to make sure that the upper crucible part is above the top point of the liquid.
  • Figure 1 shows a melt crucible 1 1 comprising a lower crucible part 12 and an upper crucible part 13. Between lower crucible part 12 and upper crucible part 13 there is an external track 14.
  • the track is typically executed as an incision in the crucible wall from the outside of the crucible.
  • the depths of the incision will typically be 10% to 80%> of the wall thickness, preferably 40-80% of the wall thickness and more preferred approximately 60% of the wall thickness.
  • the width of the track will typically be in the area 1 : 12 mm, preferably 2-10 mm and more preferable approximately 5 mm.
  • Figure 2 shows a crucible 2 comprising a lower crucible part 22 and upper crucible part 23.
  • This crucible will typically have a square cross section.
  • a penetrating incision 24 is provided in each corner of the crucible.
  • the length of each incision comprises typically from 5 - 45% of the width of the crucible wall, preferably 20 - 45% of the crucible wall, more preferably approximately 40% of the crucible's width.
  • the incision penetrates the entire wall and forms an opening in the crucible wall.
  • the height of the incision is typically in the area 1 - 12 mm, preferably 3 - 7 mm and more preferable approximately 5 mm.
  • the incisions can be executed perpendicular to the wall or form an angle with respect to the wall of up to approximately 45°, preferably 20 - 45°, more preferably approximately 30°.
  • Figure 3 shows a crucible with loose upper crucible part.
  • the melt crucible 3 comprises a lower crucible part 32 and an upper crucible part 33.
  • the upper crucible part is placed on top of the lower crucible part 34.
  • the upper crucible part is smaller than the lower crucible in such a way that the lower edge of the upper crucible part is within the side walls of the lower crucible.
  • the corners of the upper crucible part are formed with extensions in such a way that the upper part rests on its corners on the lower crucible parts upper corners.
  • it can be formed by providing the side surfaces of the upper crucible part with stops resting on the top of the lower crucible part.
  • the side walls of the upper crucible part overlap with the side walls of the lower crucible, the overlap is typically in the area 1 - 20 mm, preferably 3 - 15 mm, more preferably 5 - 10 mm and most preferred an overlap of approximately 5 mm.
  • the clearance between the side walls of the upper crucible part and the side walls of the lower crucible part is not critical, but should be made as small as practically possible.
  • Figure 4 shows a crucible with loose upper crucible part.
  • the melt crucible 4 comprises a lower crucible part 42 and an upper crucible part 43.
  • the upper crucible part is placed on top of the lower crucible part, and the lower and the upper crucible part are completely adapted to each other and have the same size in the meeting point 44.
  • the upper crucible part rests directly on top of lower crucible part and the common surface from the dividing point between lower and upper crucible part can be performed perpendicular to the wall or form an angle with respect to the wall of up to approximately 45°, preferably 20-45°, and most preferably approximately 30°.
  • a sectioned crucible with loose upper crucible part is a preferred embodiment of the invention.
  • An advantage with such a solution is that the crucible itself, lower crucible part 32 or 42 and upper crucible part 33 or 43 can be processed separately and the crucible 32 or 42 will be smaller than the corresponding melt crucible 1 and 2, shown on figures 1 and 2, respectively.
  • Upper crucible part is preferably manufactured from the same material as the crucible. Upper crucible part can however also be manufactured from a different and cheaper material because the upper crucible part will not be in contact with the melt and therefore will not contribute with contamination to the ingot material
  • Crucibles for casting silicon for use in the solar cell industry can have different sizes. Normal crucibles of the type G5 are used with dimensions approximately 700x700x420 mm, and the largest in the market are now of type G6 with dimensions approximately 900x900x500 mm. Typically the crucibles have a square cross section, however for a reusable crucible there should be a small draft angle provided on all side surfaces with a typical angle of 1-3°.
  • the crucibles are manufactured as known in the art from pure raw materials such as a pure, reaction bound silicon nitride (RBSN) or with a portion filler from pure silicon nitride powder (SI 3 N 4 ) and/or silicon carbide powder (SiC).
  • RBSN reaction bound silicon nitride
  • SI 3 N 4 pure silicon nitride powder
  • SiC silicon carbide powder
  • the crucible is manufactured with a lower crucible part having height of approximately 300 mm and a loose upper crucible part of height approximately 120 mm.
  • the upper crucible part dimensions are such that the lower edge of the frame extends approximately 5-10 mm into the lower crucible part.
  • the crucible is filled with silicon in such an amount that when the silicon has melted the top of the melt is below the lower edge of upper crucible part. The silicon melt will therefore not be in contact with the upper crucible part. This leads to the frame being subjected to lesser thermal stresses than in a corresponding whole crucible, and the frame can be reused several times.
  • a plate with dimension 750x750x10 mm was made from a homogenous RBSN-material.
  • the bending stress of the plate was measured using 3 or 4 points bending test at room temperature and up to more than 1.500 °C as being more than 100 MPa.
  • This plate dimension was tested several times, brought into crystallization furnace detached without external stresses. All tests failed with cracks in the plate as a result. Then the corresponding plate was sectioned into two equal parts and corresponding test were performed in crystallization furnace. Inspections of the sectioned plates after testing in the crystallization furnace showed no cracks.
  • the object according to the invention is a part of a melt crucible that is used industrially by the manufacturing of ceramic materials that must be sintered at high temperature. It is particularly well suited for the manufacturing of polycrystalline silicon for use in the solar cell industry.

Landscapes

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

Abstract

L'invention porte sur un creuset segmenté qui est destiné à être utilisé lors de la fabrication de silicium poly-cristallin, le creuset comportant une partie inférieure de creuset et une partie supérieure de creuset, le rapport entre la hauteur de la partie inférieure de creuset et la hauteur de la partie supérieure de creuset étant d'environ 3:1.
PCT/NO2011/000043 2010-02-08 2011-02-03 Creuset segmenté WO2011096821A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
NO20100197 2010-02-08
NO20100197 2010-02-08

Publications (1)

Publication Number Publication Date
WO2011096821A1 true WO2011096821A1 (fr) 2011-08-11

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/NO2011/000043 WO2011096821A1 (fr) 2010-02-08 2011-02-03 Creuset segmenté

Country Status (1)

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WO (1) WO2011096821A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2657372A1 (fr) * 2012-04-28 2013-10-30 Luoyang Hi-Tech Metals Co., Ltd. Creuset non monolithique
CN106468649A (zh) * 2015-08-19 2017-03-01 华北电力大学 用于模拟生物质高温腐蚀的瓷皿及方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60137893A (ja) * 1983-12-26 1985-07-22 Toshiba Ceramics Co Ltd 半導体単結晶引上用黒鉛ルツボ
JP2000169285A (ja) * 1998-12-10 2000-06-20 Sumitomo Metal Ind Ltd 融液収容ルツボ
US20020083886A1 (en) * 2000-12-01 2002-07-04 Nobuyuki Katoh Cruicible and growth method for polycrystal silicon using same
JP2009249218A (ja) * 2008-04-04 2009-10-29 Sumco Corp 単結晶引き上げ用黒鉛ルツボ

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60137893A (ja) * 1983-12-26 1985-07-22 Toshiba Ceramics Co Ltd 半導体単結晶引上用黒鉛ルツボ
JP2000169285A (ja) * 1998-12-10 2000-06-20 Sumitomo Metal Ind Ltd 融液収容ルツボ
US20020083886A1 (en) * 2000-12-01 2002-07-04 Nobuyuki Katoh Cruicible and growth method for polycrystal silicon using same
JP2009249218A (ja) * 2008-04-04 2009-10-29 Sumco Corp 単結晶引き上げ用黒鉛ルツボ

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2657372A1 (fr) * 2012-04-28 2013-10-30 Luoyang Hi-Tech Metals Co., Ltd. Creuset non monolithique
CN106468649A (zh) * 2015-08-19 2017-03-01 华北电力大学 用于模拟生物质高温腐蚀的瓷皿及方法

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