[go: up one dir, main page]

WO2015064505A1 - Crucible and single crystal sapphire production method using same - Google Patents

Crucible and single crystal sapphire production method using same Download PDF

Info

Publication number
WO2015064505A1
WO2015064505A1 PCT/JP2014/078375 JP2014078375W WO2015064505A1 WO 2015064505 A1 WO2015064505 A1 WO 2015064505A1 JP 2014078375 W JP2014078375 W JP 2014078375W WO 2015064505 A1 WO2015064505 A1 WO 2015064505A1
Authority
WO
WIPO (PCT)
Prior art keywords
crucible
molybdenum
alloy
opening
plate
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2014/078375
Other languages
French (fr)
Japanese (ja)
Inventor
芳竹 深谷
加藤　昌宏
慎 渡辺
謙一 岡本
亮 後藤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ALMT Corp
Original Assignee
ALMT Corp
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 ALMT Corp filed Critical ALMT Corp
Priority to JP2015544973A priority Critical patent/JPWO2015064505A1/en
Priority to CN201480059447.4A priority patent/CN105683425A/en
Publication of WO2015064505A1 publication Critical patent/WO2015064505A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Images

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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/20—Aluminium oxides
    • 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
    • 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
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C30B35/002—Crucibles or containers
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D5/00—Supports, screens or the like for the charge within the furnace
    • F27D5/0068—Containers
    • F27D2005/0075—Pots, e.g. slag pots, ladles

Definitions

  • the present invention relates to a crucible and a method for manufacturing a single crystal sapphire using the crucible, and more particularly to a crucible made of molybdenum or an alloy thereof and a method for manufacturing a single crystal sapphire using the crucible.
  • Patent Document 1 discloses a quartz crucible for a silicon single crystal pulling apparatus.
  • Patent Document 2 discloses a crucible and a method for growing polycrystalline silicon using the crucible.
  • Molybdenum crucible is used for sapphire single crystal growth. Even if the raw material alumina is filled up to the crucible internal volume limit, the volume of the sapphire ingot after melting and solidification is reduced to about 50% of the internal volume of the crucible. In order to manufacture a single crystal sapphire wafer from an ingot with a high yield, it is desired to manufacture an ingot having a large volume.
  • the alumina raw material used for single crystal growth is granular having a diameter of about several millimeters or a lump of several millimeters to several tens of millimeters, and a large void is created in the crucible when filled. It is obvious that this void hinders effective use of the crucible internal volume, and each crystal maker has devised to increase the crucible internal volume.
  • Patent Documents 1 and 2 of the prior art are both related to silicon crystals (single crystals and polycrystals), and devised for effective use of crucible internal volume, and disclosed auxiliary tools such as a cover ring or an upper crucible. .
  • Patent Document 1 discloses a raw material filling auxiliary tool made of ceramics (carbon, silicon carbide, quartz, etc.) serving as a cover.
  • a flange structure is provided at the lower part of the cover ring, and a flange is also provided at the upper edge of the lower crucible, which is the crucible body.
  • Such a flange structure is formed by cutting a thick member or part with a cutting tool and is not suitable for a thin material. Further, since sapphire melting is performed at an extremely high temperature exceeding 2050 ° C., ceramics are uneasy about durability performance.
  • Patent Document 2 discloses a raw material holding crucible made of graphite.
  • An example of the connection structure according to the present invention is a simple system in which the lower end outer peripheral portion of the raw material holding crucible is hanged into a skirt shape on the inner peripheral side of the lower crucible upper edge which is the crucible body.
  • a raw material holding crucible is placed on a lower crucible which is a crucible body, which is also a simple method.
  • a ⁇ -shaped groove is carved in the lower end of the raw material holding crucible, and it is devised to fit in the upper edge of the lower crucible.
  • the method of fitting the lower end of the raw material holding crucible into the inner peripheral side of the lower crucible may cause sticking or cracking due to thermal expansion during high-temperature heating, and there is concern about the stability of the posture.
  • the process of carving a ⁇ -shaped groove in the lower end of the raw material holding crucible requires cutting with a cutting tool, and is not suitable for a thin crucible with a thickness of about several millimeters.
  • the present invention has been made to solve the above-described problems, and an object thereof is to provide a crucible made of molybdenum or an alloy thereof capable of efficiently producing a large single crystal sapphire. It is.
  • a crucible according to the present invention is a crucible made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible provided with an opening and an upper crucible fitted into the opening, and the upper crucible is made of molybdenum or It is formed by bending the alloy plate and joining both ends of the plate.
  • a crucible according to the present invention is a crucible made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible provided with an opening and an upper crucible fitted into the opening, and the upper crucible is made of molybdenum or The alloy plate material is formed by continuous in the circumferential direction without a seam.
  • a crucible capable of stably producing a large single crystal sapphire ingot and a method for producing a single crystal sapphire using the crucible can be provided.
  • FIG. 2 is a plan view of a crucible according to Embodiment 1.
  • FIG. FIG. 2 is a cross-sectional view taken along line II-II in FIG. 3 is a perspective view of a crucible according to Embodiment 1.
  • FIG. 6 is a plan view of a crucible according to a second embodiment.
  • FIG. FIG. 5 is a sectional view taken along line VV in FIG. 4.
  • FIG. 6 is a sectional view taken along line VI-VI in FIG. 5.
  • 6 is a perspective view of a crucible according to a second embodiment.
  • FIG. 10 is a plan view of a crucible according to Embodiment 3.
  • FIG. FIG. 9 is a cross-sectional view taken along line IX-IX in FIG.
  • FIG. 10 is a perspective view of a crucible according to Embodiment 3.
  • FIG. FIG. 6 is a plan view of a crucible according to a fourth embodiment.
  • FIG. 12 is a sectional view taken along line XII-XII in FIG.
  • FIG. 13 is a cross-sectional view taken along line XIII-XIII in FIG. 10 is a perspective view of a crucible according to a fourth embodiment.
  • FIG. FIG. 10 is a plan view of a crucible according to a fifth embodiment.
  • FIG. 16 is a cross-sectional view taken along line XVI-XVI in FIG. 15.
  • FIG. 10 is a perspective view of a crucible according to a fifth embodiment.
  • FIG. 10 is a plan view of a crucible according to a sixth embodiment.
  • FIG. 19 is a cross-sectional view taken along line XIX-XIX in FIG.
  • FIG. 20 is a cross-sectional view taken along line XX-XX in FIG.
  • FIG. 10 is a perspective view of a crucible according to a sixth embodiment.
  • FIG. 10 is a plan view of a crucible according to a seventh embodiment.
  • FIG. 23 is a cross-sectional view taken along line XXIII-XXIII in FIG.
  • FIG. 10 is a perspective view of a crucible according to a seventh embodiment.
  • FIG. 10 is a plan view of a crucible according to an eighth embodiment.
  • FIG. 19 is a cross-sectional view taken along line XIX-XIX in FIG.
  • FIG. 20 is a cross-sectional view taken along line XX-XX in FIG.
  • FIG. 10 is a perspective view of
  • FIG. 26 is a sectional view taken along line XXVI-XXVI in FIG. 25.
  • FIG. 27 is a cross-sectional view along the line XXVII-XXVII in FIG. 26.
  • FIG. 10 is a perspective view of a crucible according to an eighth embodiment.
  • FIG. 10 is a plan view of a crucible according to a ninth embodiment.
  • FIG. 30 is a cross-sectional view taken along line XXX-XXX in FIG. 29.
  • FIG. 10 is a perspective view of a crucible according to a ninth embodiment.
  • FIG. 10 is a plan view of a crucible according to a tenth embodiment.
  • FIG. 33 is a cross-sectional view taken along line XXXIII-XXXIII in FIG.
  • FIG. 34 is a cross-sectional view taken along line XXXIV-XXXIV in FIG. 33.
  • FIG. 10 is a perspective view of a crucible according to a tenth embodiment.
  • FIG. 22 is a plan view of a crucible according to an eleventh embodiment.
  • FIG. 37 is a cross-sectional view taken along line XXXVII-XXXVII in FIG. 36.
  • FIG. 20 is a perspective view of a crucible according to an eleventh embodiment.
  • FIG. 38 is a plan view of a crucible according to a twelfth embodiment.
  • FIG. 40 is a cross-sectional view taken along line XL-XL in FIG. 39.
  • FIG. 41 is a cross-sectional view taken along line XLI-XLI in FIG. 40.
  • FIG. 20 is a perspective view of a crucible according to a twelfth embodiment.
  • FIG. 38 is a plan view of a crucible according to a thirteenth embodiment.
  • FIG. 44 is a cross-sectional view taken along line XLIV-XLIV in FIG. 43.
  • FIG. 23 is a perspective view of a crucible according to a thirteenth embodiment.
  • FIG. 25 is a plan view of a crucible according to a fourteenth embodiment.
  • FIG. 47 is a cross-sectional view taken along the line XLVII-XLVII in FIG. 46.
  • FIG. 48 is a cross-sectional view taken along line XLVIII-XLVIII in FIG. 47.
  • FIG. 25 is a perspective view of a crucible according to a fourteenth embodiment.
  • FIG. 20 is a plan view of a crucible according to a fifteenth embodiment.
  • FIG. 51 is a cross-sectional view taken along line LI-LI in FIG. 50.
  • FIG. 17 is a perspective view of a crucible according to a fifteenth embodiment.
  • FIG. 20 is a plan view of a crucible according to a sixteenth embodiment.
  • FIG. 54 is a cross-sectional view taken along the line LIV-LIV in FIG. 53.
  • 20 is a perspective view of a crucible according to a sixteenth embodiment.
  • FIG. 20 is a plan view of a crucible according to a seventeenth embodiment.
  • FIG. 57 is a cross-sectional view taken along line LVII-LVII in FIG. 56.
  • FIG. 18 is a perspective view of a crucible according to a seventeenth embodiment.
  • FIG. 23 is a plan view of a crucible according to an eighteenth embodiment.
  • FIG. 60 is a cross-sectional view taken along line LX-LX in FIG. 59.
  • FIG. 20 is a perspective view of a crucible according to an eighteenth embodiment.
  • FIG. 38 is a plan view of a crucible according to a nineteenth embodiment.
  • FIG. 63 is a cross-sectional view taken along line LXIII-LXIII in FIG. 62.
  • FIG. 23 is a perspective view of a crucible according to a nineteenth embodiment.
  • FIG. 38 is a plan view of a crucible according to a twentieth embodiment.
  • FIG. 66 is a cross-sectional view taken along line LXVI-LXVI in FIG. 65.
  • FIG. 32 is a perspective view of a crucible according to a twentieth embodiment. It is a photograph of the upper crucible side flange portion used in the crucible according to the twenty-first embodiment.
  • the crucible is a crucible made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible provided with an opening and an upper crucible fitted into the opening, and the upper crucible is a plate made of molybdenum or an alloy thereof. It is formed by bending both ends of the plate material.
  • the lower crucible is formed by drawing a plate made of molybdenum or an alloy thereof, and the opening is provided with a lower crucible side flange portion extending in the outer circumferential direction of the cylinder and continuing in the circumferential direction. Yes.
  • the upper crucible has an engaging portion that is fitted to the inner peripheral side of the opening and engages with the lower crucible, and the upper crucible is detachably provided to the lower crucible.
  • an upper crucible side flange portion extending in the radial direction of the cylinder is provided at the lower portion of the upper crucible.
  • the crucible is a crucible made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible provided with an opening and an upper crucible fitted into the opening, and the upper crucible is a plate made of molybdenum or an alloy thereof. Is formed by continuous in the circumferential direction without seams.
  • the lower crucible is formed by drawing a plate made of molybdenum or an alloy thereof, and the opening is provided with a lower crucible side flange portion extending in the outer circumferential direction of the cylinder and continuing in the circumferential direction. Yes.
  • the upper crucible has a small diameter portion on the side close to the lower crucible and a large diameter portion on the side far from the lower crucible, and the small diameter portion fits inside the lower crucible.
  • a tapered surface that is inclined downward toward the inner peripheral side is provided between the large-diameter portion and the small-diameter portion.
  • the single crystal sapphire manufacturing method includes the steps of filling the lower crucible and upper crucible of the molybdenum or the alloy crucible described in any of the above, and melting the raw material and then solidifying it into the lower crucible. Producing a single crystal sapphire.
  • crucible 1 according to Embodiment 1 is made of molybdenum or an alloy thereof, and fits into opening 11 with bottomed cylindrical lower crucible 10 provided with opening 11.
  • the upper crucible 20 includes an upper crucible 20, and the upper crucible 20 is formed by bending a plate 23 made of molybdenum or its alloy and joining both ends of the plate.
  • the lower crucible 10 is formed by drawing a plate 13 made of molybdenum or an alloy thereof, and the opening 11 is provided with a lower crucible side flange portion 12 extending in the circumferential direction and extending in the circumferential direction. ing.
  • the upper crucible 20 has an engaging portion 28 that is fitted to the inner peripheral side of the opening 11 and engages with the lower crucible 10, and the upper crucible 20 is provided detachably with respect to the lower crucible 10.
  • An upper crucible side flange 30 extending in the radial direction of the cylinder is provided at the lower portion of the upper crucible 20.
  • Both end portions of the plate material 23 are welded to the contact plate 40.
  • the angle ⁇ 1 formed by the side wall of the lower crucible 10 with respect to the vertical direction is about 10 °, and the side wall of the upper crucible 20 is arranged substantially parallel to the vertical direction.
  • the upper crucible 20 has no bottom, and the upper crucible 20 and the lower crucible 10 communicate with each other.
  • the angle ⁇ 2 formed by the side wall of the upper crucible 20 with respect to the vertical direction is approximately 10 °, and according to the first embodiment. Different from the crucible 1.
  • the angle ⁇ ⁇ b> 1 formed by the side wall of the lower crucible 10 with respect to the vertical direction is approximately 2 °, according to the first embodiment.
  • the lower crucible 10 is different from the crucible 1 according to the first embodiment in that no flange is provided.
  • the angle ⁇ ⁇ b> 2 formed by the side wall of the upper crucible 20 with respect to the vertical direction is approximately 2 °, according to the second embodiment.
  • the lower crucible 10 is different from the crucible 1 according to the second embodiment in that no flange is provided.
  • the crucible 1 according to the first embodiment is that the end of the upper crucible 20 is joined to the caulking plate 40 by a rivet 50. And different.
  • the rivets 50 are arranged in parallel in two rows, and eight rivets 50 are provided in the vertical direction.
  • the angle ⁇ 2 formed by the side wall of the upper crucible 20 with respect to the vertical direction is approximately 10 °, according to the fifth embodiment. Different from the crucible 1.
  • rivets 50 are arranged in a staggered manner in two rows in pad plate 40, and four rivets 50 are provided in the vertical direction. Thus, it differs from the crucible 1 according to the fifth embodiment.
  • the angle ⁇ 2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 10 °. Different from the crucible 1.
  • rivets 50 are arranged in two rows in parallel in pad plate 40, and four rivets 50 are provided in the vertical direction. , Different from crucible 1 according to the fifth embodiment.
  • the angle ⁇ 2 formed by the side wall of upper crucible 20 with respect to the vertical direction is approximately 10 °, according to the ninth embodiment. Different from the crucible 1.
  • the angle ⁇ 2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 10 °. Different from the crucible 1.
  • the angle ⁇ 2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 10 °. Different from the crucible 1.
  • crucible 1 Referring to FIGS. 50 to 52, crucible 1 according to the fifteenth embodiment is a crucible 1 made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible 10 provided with an opening 11 and an opening 11. And the upper crucible 20 is formed by continuously connecting the plate material 23 made of molybdenum or its alloy seamlessly in the circumferential direction.
  • the lower crucible 10 is formed by drawing a plate 13 made of molybdenum or an alloy thereof, and the opening 11 is provided with a lower crucible side flange portion 12 extending in the circumferential direction and extending in the circumferential direction. ing.
  • the upper crucible 20 has a small diameter portion 25 on the side close to the lower crucible 10 and a large diameter portion 27 on the side far from the lower crucible 10, and the small diameter portion 25 fits inside the lower crucible 10.
  • a tapered surface 26 is provided between the large-diameter portion 27 and the small-diameter portion 25 and is inclined downward toward the inner peripheral side.
  • a reduced diameter portion 24 extending inward is provided at the lower end of the small diameter portion 25.
  • the angle ⁇ 1 made by the side wall of the lower crucible 10 with respect to the vertical direction is about 10 °
  • the angle ⁇ 2 made by the side wall of the upper crucible 20 with respect to the vertical direction is about 10 °.
  • the upper crucible 20 has no bottom, and the upper crucible 20 and the lower crucible 10 communicate with each other.
  • crucible 1 according to the sixteenth embodiment is different from crucible 1 according to the fifteenth embodiment in that reduced diameter portion 24 is not provided in upper crucible 20.
  • the angle ⁇ 2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 2 °. Different from the crucible 1.
  • crucible 1 according to the nineteenth embodiment differs from crucible 1 according to the eighteenth embodiment in that reduced diameter portion 24 is not provided in upper crucible 20.
  • the angle ⁇ 2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 2 °. Different from the crucible 1.
  • the upper crucible 20 capable of increasing the raw material filling amount is added so that the inner volume of the lower crucible 10 main body can be effectively used and a large single crystal sapphire ingot can be manufactured.
  • the material of the crucible 1 is a metal molybdenum and its alloy having a melting point of over 2600 ° C. and excellent in high temperature resistance, and is resistant to high temperature deformation and has a characteristic of withstanding melting of raw material alumina with a thickness of about several mm.
  • upper crucible side flange portion 30 includes a plurality of claws 310, 320, 330, 340 and a barrel to which these claws 310.30.30.340 are connected. Part 300.
  • a plurality of claw portions 310, 320, 330, and 340 are provided, and a gap is provided between each claw portion 310, 320, 330, and 340. Therefore, it is possible to easily manufacture the upper crucible side flange portion 30 as compared with a structure in which the claw portion is formed of a single plate material.
  • claw portions 310, 320, 330, and 340 are disclosed, but more or fewer claw portions may be provided.
  • the upper crucible side flange portion 30 according to the twenty-first embodiment may be applied to other embodiments.
  • the barrel 300 is fixed to the plate member 23 by rivets 50.
  • the body part 300 may be fixed to the plate member 23 other than rivets, such as welding or brazing material.
  • Single crystal sapphire can be manufactured using the crucible 1 made of molybdenum and its alloy shown in Embodiments 1 to 20.
  • a molybdenum plate or molybdenum alloy plate having a thickness of about several millimeters is rounded and formed by sheet metal processing and joined with a rivet 50 (Embodiments 5 to 14) or welded (Embodiments 1 to 4) to form a cylinder or a hollow cone Make a stand.
  • the upper crucible 20 is made by drawing (Embodiments 15 to 20), and the bottom of the upper crucible 20 is removed by cutting to form a cylinder or a hollow truncated cone.
  • the upper crucible side flange 30 is retrofitted by rivet joining or welding to several places on the outer periphery (in the case of sheet metal processing), or a flange (tapered surface 26) is formed on the entire outer periphery ( In the case of drawing), the upper crucible 20 is placed on the upper edge of the lower crucible 10 through these flanges.
  • Step A1 Each plate material for crucible and backing plate A molybdenum plate material having a surface roughness Ra of about 5 ⁇ m, or a molybdenum alloy plate material such as a lanthanum oxide-added alloy or a TZM alloy is prepared.
  • the cold-rolled plate size for the crucible is 3 mm thick x 250 mm wide x 1100 mm long. This rolled sheet is cut into a fan-shaped rounding material based on the material development using a discharge wire cutting machine or the like.
  • a drill through hole for rivet joining (diameter 3 mm, both for contact plate joining and flange joining) is opened in the rounding material using a drilling machine based on the development.
  • the rolled plate material for the contact plate is the same material as the plate material for the crucible, and is dimensioned and cut with a discharge wire cutter or a shear cutter to a thickness of 3 mm x width 80 mm x length 150 mm. Based on the developed view, a through hole for a rivet is provided in advance as described above.
  • Step A2 Flange and rivet plate / bar material The same quality as the crucible material and the same surface roughness (thickness 3 mm x width 50 mm x length is optionally about 200 mm to 1000 mm) and bar (diameter 3 mm x length) About 1000 mm).
  • ⁇ Four parts for the flange are cut to a length of 200mm.
  • the rivet rod used for the flange attachment is also prepared with the same material as the flange plate, cut to a length of 12 mm with a grinding wheel cutting or a discharge wire cutter, and then the cutting burr is removed with a grinding stone or the like.
  • Step A3 Sheet metal processing such as rounding and L-shaped bending The materials or parts prepared in Step A1 and Step A2 will be sequentially described.
  • the rounding material prepared in step A1 is rounded into a truncated cone shape with a commercially available roller bender, and it is confirmed that it is abutted securely.
  • the patch plate was rounded with a brake press (PAS5020 manufactured by KOMAT’SU) according to the curvature of the outer surface of the crucible.
  • a patch plate was placed on the outside of the abutting part, and the minute deformation correction of the rivet hole and the mutual position were confirmed. The minute deformation of the hole is corrected manually with a diamond file.
  • the 50 mm width plate material prepared in step A2 was bent by a brake press in an L shape along the length direction so as to have a width of 2: 3.
  • This L-shaped part was obtained by cutting four 50 mm long L-shaped flanges.
  • Four rivet through-holes are opened on the wide side of the L-shape, using a drilling machine in a straight line. Thereafter, using a brake press, the holed side is bent in accordance with the crucible outer surface curvature. A hole that has been deformed by bending is corrected with a file.
  • Step A4 Assembly Processing
  • the upper crucible body is completed by assembling the manufactured parts by rivet bonding.
  • the upper crucible body is assembled. Temporarily assemble the crucible using auxiliary jigs, pass the bar through the holes arranged in a straight line or zigzag pattern with the base plate as a reference to the upper edge of the crucible, and protrude 3 mm inward with a small diameter burner Heat and crush with a small hammer. After filling all the holes, the rod protruding 3 mm outward is crushed with a small hammer to complete the rivet joint.
  • the flange assembly is completed by performing the work in the manner of assembling the stopper metal on the four-equal outer peripheral surface outside the lower end of the stopper plate.
  • Process B1 Crucible plate material A plate material having the same material, standard and quality as A1 is used. A molybdenum plate material having a surface roughness Ra of about 5 ⁇ m, or a molybdenum alloy plate material such as a lanthanum oxide-added alloy or a TZM alloy is prepared.
  • the cold-rolled plate size for the crucible is 3 mm thick x 250 mm wide x 1100 mm long. This rolled sheet is cut into a fan-shaped rounding material based on the material development using a discharge wire cutting machine or the like. Based on the developed view, a drill through hole (3 mm diameter, for flange connection) for rivet bonding is opened in the rounding material using a drilling machine. When all the joining is performed by the welding method, the through hole processing is unnecessary.
  • Step B2 Flange Plate Material A plate material having the same quality as the crucible material and the same surface roughness (thickness 3 mm ⁇ width 50 mm ⁇ length is optionally about 200 mm to 1000 mm) is used. Four flange parts are cut to a length of 200 mm. Bar material (diameter 3 mm x length 1000 mm) is used. The rivet bar used for flange mounting is also prepared with the same material as the flange plate, cut to a length of 12 mm with a grinding wheel cutting or a discharge wire cutter, and then the cutting burr is removed with a grinding stone. In addition, when attaching a flange to a crucible main body with a welding method, a bar is unnecessary.
  • Step B3 Sheet metal processing such as rounding and L-shaped bending
  • the rounding of the crucible body part and the L-shaped bending of the flange part are performed in the same manner as in the case of manufacturing by rivet joining.
  • Step B4 Assembly processing In order to prevent oxidation embrittlement during welding, TIG welding is performed in a chamber replaced with an inert gas. First, the crucible body temporarily assembled with auxiliary jigs is welded. After the rounded butt portion is welded at 3 to 4 points, the entire butt portion is welded to complete the main body crucible.
  • the outer periphery of the flange is welded to the outer periphery of the crucible (4 to 6 points may be fixed).
  • the method is the same as that in step A4.
  • Process C1 Crucible plate material A plate material having the same material, standard and quality as described above is used. A molybdenum plate material having a surface roughness Ra of about 5 ⁇ m, or a molybdenum alloy plate material such as a lanthanum oxide-added alloy or a TZM alloy is prepared. The cold-rolled plate size for the crucible is 3 mm ⁇ ⁇ 620 mm in thickness. Using this rolled sheet material, a drawing blank material having a thickness of 3 mm and a diameter of 600 mm is cut out using a discharge wire cutting machine or a lathe.
  • Step C2 Flange plate material A plate material having the same quality as the crucible material and the same surface roughness (thickness 3 mm ⁇ width 50 mm ⁇ length is optionally about 200 mm to 1000 mm) is used. Four flange parts are cut to a length of 200 mm. Bar material (diameter 3 mm x length 1000 mm) is used.
  • the rod material for rivets used for flange mounting is also prepared with the same material as the flange plate material, cut to a length of 12 mm with a grinding wheel cutting or a discharge wire cutting machine, and then the cutting burr is removed with a grinding stone.
  • a bar is unnecessary.
  • Step C3 Drawing and processing the crucible body using a drawing and L-shaped spinning machine.
  • the spinning machine mainly includes an apparatus main body, a mold as a core, a pressing rod, and a roller. This is a processing method in which a blank material, which is a material to be molded, is molded by pressing it against the outer surface of a mold with a roller.
  • a mold is attached to a horizontal rotation shaft, a blank material with a diameter of 600 mm, a pressing rod are arranged in series, and the blank material rotating at 100 to 300 rpm is heated red by a propane burner etc. It is shaped like a crucible. If the material to be molded is a shape that can be removed from the mold, the crucible side wall can be molded not only in a straight line but also in a step shape. In order to manufacture a cylindrical crucible, it is necessary to finish the bottom to the designed shape. Finishing can be scraped off with a cutting tool using a horizontal lathe to obtain a bottomless (hollow) crucible of any shape.
  • a small-diameter hole can be provided in advance in the blank material at the portion corresponding to the bottom of the crucible.
  • providing a large-diameter hole in advance is not preferable because it may cause cracks during drawing.
  • a hollow frustoconical crucible having a thickness of 3 mm ⁇ an upper end outer diameter of 330 mm ⁇ a lower end outer diameter of 300 mm ⁇ a height of 200 mm is obtained.
  • the flange parts are the same as in step A2, so they are shown again.
  • the 50 mm width plate material prepared in step A2 was bent into a L shape along the length direction by a brake press so as to have a width of 2: 3.
  • This L-shaped part was obtained by cutting four 50 mm long L-shaped flanges. Five rivet through-holes are opened on the wide L-shaped side, and a staggered drilling machine is used. Thereafter, using a brake press, the holed side is bent in accordance with the crucible outer surface curvature. A hole that has been deformed by bending is corrected with a file.
  • Process C4 assembly process
  • the flange can be attached by joining with a rivet or by a welding method.
  • the method and work procedure are as described above.
  • the flange itself is unnecessary.
  • the lower crucible is a crucible made of molybdenum having a thickness of 5 mm, an opening diameter of 310 mm, and a depth of 400 mm.
  • the approximate size of the ingot is an outer diameter of 300 mm ⁇ height of 200 mm and a weight of about 60 kg. It is 50% utilization of the lower crucible internal volume.
  • the overall configuration when the flanged upper crucible is placed on the lower crucible is a total height of 550 mm.
  • the approximate size of the ingot obtained by melting and solidifying was an outer diameter of 300 mm ⁇ height of 280 mm, and a weight of about 84 kg. It is a utilization rate of 70% of the inner volume of the lower crucible.
  • the upper crucible of all the constituent crucibles taken out of the growth furnace could be separated from the lower crucible simply by lifting it upward with both hands, and no damage occurred. Moreover, the state which can be used repeatedly was maintained, without the trace which the sapphire melt adhered.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

In order to provide a crucible of molybdenum or an alloy thereof, said crucible being capable of efficiently producing large single crystal sapphires, the present invention is equipped with a lower crucible (10) that is provided with an opening (11) and has a bottomed cylindrical shape, and an upper crucible (20) that is fitted to the opening (11). The upper crucible (20) is formed by a plate (23) of molybdenum, or an alloy thereof, being bent, and both ends of the plate being joined. The lower crucible (10) is formed by a plate (13) of molybdenum, or an alloy thereof, being drawn, and a lower-crucible side flange (12), which extends in the outer circumferential direction of the cylinder and is continuous in the circumferential direction, is provided to the opening (11).

Description

坩堝およびそれを用いた単結晶サファイヤの製造方法Crucible and method for producing single crystal sapphire using the same

　この発明は、坩堝およびそれを用いた単結晶サファイヤの製造方法に関し、より特定的には、モリブデンまたはその合金製の坩堝およびそれを用いた単結晶サファイヤの製造方法に関する。 The present invention relates to a crucible and a method for manufacturing a single crystal sapphire using the crucible, and more particularly to a crucible made of molybdenum or an alloy thereof and a method for manufacturing a single crystal sapphire using the crucible.

　従来、坩堝に関しては、特開昭６４―４２３８８号公報（特許文献１）では、シリコン単結晶引き上げ装置用石英坩堝が開示されている。 Conventionally, regarding a crucible, Japanese Patent Laid-Open No. 64-42388 (Patent Document 1) discloses a quartz crucible for a silicon single crystal pulling apparatus.

　また、特開２００２―１７０７８０号公報（特許文献２）では、ルツボおよびそれを使用した多結晶シリコンの成長方法が開示されている。 Also, Japanese Patent Laid-Open No. 2002-170780 (Patent Document 2) discloses a crucible and a method for growing polycrystalline silicon using the crucible.

特開昭６４―４２３８８号公報JP-A 64-42388 特開２００２―１７０７８０号公報JP 2002-170780 A

　サファイア単結晶育成にモリブデン坩堝が使用されている。坩堝内容積限度まで原料アルミナを充填しても、溶解・凝固後のサファイアインゴット体積は坩堝の内容積の５０％程度に減少してしまう。単結晶サファイアウエファーをインゴットから高い数量歩留まりで製造するために、体積の大きなインゴットの製造が望まれている。 Molybdenum crucible is used for sapphire single crystal growth. Even if the raw material alumina is filled up to the crucible internal volume limit, the volume of the sapphire ingot after melting and solidification is reduced to about 50% of the internal volume of the crucible. In order to manufacture a single crystal sapphire wafer from an ingot with a high yield, it is desired to manufacture an ingot having a large volume.

　単結晶育成に使用するアルミナ原料は、直径数ｍｍ程度の粒状或いは数ｍｍから十数ｍｍの大きさの塊状であり、坩堝内に充填時に大きな空隙が生まれてしまう。この空隙が坩堝内容積の有効利用を阻害することは自明であり、坩堝内容積を増大させる工夫を各結晶メーカーが行っている。先行技術の特許文献１および２は共にシリコン結晶（単結晶並びに多結晶）に関しての考案であり、坩堝内容積の有効活用について鋭意工夫し、カバーリング或いは上部坩堝などの補助具を開示している。 The alumina raw material used for single crystal growth is granular having a diameter of about several millimeters or a lump of several millimeters to several tens of millimeters, and a large void is created in the crucible when filled. It is obvious that this void hinders effective use of the crucible internal volume, and each crystal maker has devised to increase the crucible internal volume. Patent Documents 1 and 2 of the prior art are both related to silicon crystals (single crystals and polycrystals), and devised for effective use of crucible internal volume, and disclosed auxiliary tools such as a cover ring or an upper crucible. .

　特許文献１ではカバーリングなるセラミックス製(炭素、炭化ケイ素、石英など）の原料充填補助具を開示している。カバーリング下部にフランジ構造を設けるとともに、坩堝本体である下部坩堝の上縁部にもフランジを設け、両者をバヨネット方式で着脱自在ならしめている。 Patent Document 1 discloses a raw material filling auxiliary tool made of ceramics (carbon, silicon carbide, quartz, etc.) serving as a cover. A flange structure is provided at the lower part of the cover ring, and a flange is also provided at the upper edge of the lower crucible, which is the crucible body.

　このようなフランジ構造は、厚手の部材や部品を刃具による切削加工によって形成され、薄手の材料には不向きである。また、サファイア溶融は２０５０℃を越える超高温下で行われるので、セラミックスは耐久性能に不安がある。 Such a flange structure is formed by cutting a thick member or part with a cutting tool and is not suitable for a thin material. Further, since sapphire melting is performed at an extremely high temperature exceeding 2050 ° C., ceramics are uneasy about durability performance.

　特許文献２には、黒鉛製の原料保持坩堝が開示されている。この考案による接続構造の一例は、原料保持坩堝の下端外周部を坩堝本体である下部坩堝上縁部内周側にスカート状に垂れさげて嵌めこむ簡便な方式である。 Patent Document 2 discloses a raw material holding crucible made of graphite. An example of the connection structure according to the present invention is a simple system in which the lower end outer peripheral portion of the raw material holding crucible is hanged into a skirt shape on the inner peripheral side of the lower crucible upper edge which is the crucible body.

　他の一例として、原料保持坩堝を坩堝本体である下部坩堝上に載せ置く、これも簡便なる方式である。原料保持坩堝の下端部にП字状の溝を彫りこみ、下部坩堝上縁部に嵌めこめるよう工夫されている。 As another example, a raw material holding crucible is placed on a lower crucible which is a crucible body, which is also a simple method. A П-shaped groove is carved in the lower end of the raw material holding crucible, and it is devised to fit in the upper edge of the lower crucible.

　原料保持坩堝下端部を下部坩堝内周側に嵌めこむ方式は、高温加熱時の熱膨張によって固着したり割れが生じる恐れがあり、姿勢の安定性にも不安がある。 The method of fitting the lower end of the raw material holding crucible into the inner peripheral side of the lower crucible may cause sticking or cracking due to thermal expansion during high-temperature heating, and there is concern about the stability of the posture.

　原料保持坩堝の下端部にП字状の溝を彫りこむ加工は刃具による切削加工が必要であり、厚さ数ｍｍ程度の薄い坩堝には不向きである。 The process of carving a П-shaped groove in the lower end of the raw material holding crucible requires cutting with a cutting tool, and is not suitable for a thin crucible with a thickness of about several millimeters.

　そこで、この発明は上述のような課題を解決するためになされたものであり、効率よく大きな単結晶サファイヤを製造することが可能なモリブデンまたはその合金製の坩堝を提供することを目的とするものである。 Accordingly, the present invention has been made to solve the above-described problems, and an object thereof is to provide a crucible made of molybdenum or an alloy thereof capable of efficiently producing a large single crystal sapphire. It is.

　この発明に従った坩堝は、モリブデンまたはその合金製の坩堝であって、開口が設けられた有底円筒形状の下部坩堝と、開口に嵌まり合う上部坩堝とを備え、上部坩堝は、モリブデンまたはその合金製の板材を曲げて板材の両端部を接合することで形成される。 A crucible according to the present invention is a crucible made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible provided with an opening and an upper crucible fitted into the opening, and the upper crucible is made of molybdenum or It is formed by bending the alloy plate and joining both ends of the plate.

　この発明に従った坩堝は、モリブデンまたはその合金製の坩堝であって、開口が設けられた有底円筒形状の下部坩堝と、開口に嵌まり合う上部坩堝とを備え、上部坩堝は、モリブデンまたはその合金製の板材が継ぎ目なく周方向に連続することで形成される。 A crucible according to the present invention is a crucible made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible provided with an opening and an upper crucible fitted into the opening, and the upper crucible is made of molybdenum or The alloy plate material is formed by continuous in the circumferential direction without a seam.

　この発明に従えば、大きな単結晶サファイヤインゴットを安定して作成することができる坩堝およびそれを用いた単結晶サファイヤの製造方法を提供することができる。 According to the present invention, a crucible capable of stably producing a large single crystal sapphire ingot and a method for producing a single crystal sapphire using the crucible can be provided.

実施の形態１に従った坩堝の平面図である。2 is a plan view of a crucible according to Embodiment 1. FIG. 図１中のＩＩ－ＩＩ線に沿った断面図である。FIG. 2 is a cross-sectional view taken along line II-II in FIG. 実施の形態１に従った坩堝の斜視図である。3 is a perspective view of a crucible according to Embodiment 1. FIG. 実施の形態２に従った坩堝の平面図である。6 is a plan view of a crucible according to a second embodiment. FIG. 図４中のＶ－Ｖ線に沿った断面図である。FIG. 5 is a sectional view taken along line VV in FIG. 4. 図５中のＶＩ－ＶＩ線に沿った断面図である。FIG. 6 is a sectional view taken along line VI-VI in FIG. 5. 実施の形態２に従った坩堝の斜視図である。6 is a perspective view of a crucible according to a second embodiment. FIG. 実施の形態３に従った坩堝の平面図である。10 is a plan view of a crucible according to Embodiment 3. FIG. 図８中のＩＸ－ＩＸ線に沿った断面図である。FIG. 9 is a cross-sectional view taken along line IX-IX in FIG. 実施の形態３に従った坩堝の斜視図である。10 is a perspective view of a crucible according to Embodiment 3. FIG. 実施の形態４に従った坩堝の平面図である。FIG. 6 is a plan view of a crucible according to a fourth embodiment. 図１１中のＸＩＩ－ＸＩＩ線に沿った断面図である。FIG. 12 is a sectional view taken along line XII-XII in FIG. 図１２中のＸＩＩＩ－ＸＩＩＩ線に沿った断面図である。FIG. 13 is a cross-sectional view taken along line XIII-XIII in FIG. 実施の形態４に従った坩堝の斜視図である。10 is a perspective view of a crucible according to a fourth embodiment. FIG. 実施の形態５に従った坩堝の平面図である。FIG. 10 is a plan view of a crucible according to a fifth embodiment. 図１５中のＸＶＩ－ＸＶＩ線に沿った断面図である。FIG. 16 is a cross-sectional view taken along line XVI-XVI in FIG. 15. 実施の形態５に従った坩堝の斜視図である。FIG. 10 is a perspective view of a crucible according to a fifth embodiment. 実施の形態６に従った坩堝の平面図である。FIG. 10 is a plan view of a crucible according to a sixth embodiment. 図１８中のＸＩＸ－ＸＩＸ線に沿った断面図である。FIG. 19 is a cross-sectional view taken along line XIX-XIX in FIG. 図１９中のＸＸ－ＸＸ線に沿った断面図である。FIG. 20 is a cross-sectional view taken along line XX-XX in FIG. 実施の形態６に従った坩堝の斜視図である。FIG. 10 is a perspective view of a crucible according to a sixth embodiment. 実施の形態７に従った坩堝の平面図である。FIG. 10 is a plan view of a crucible according to a seventh embodiment. 図２２中のＸＸＩＩＩ－ＸＸＩＩＩ線に沿った断面図である。FIG. 23 is a cross-sectional view taken along line XXIII-XXIII in FIG. 実施の形態７に従った坩堝の斜視図である。FIG. 10 is a perspective view of a crucible according to a seventh embodiment. 実施の形態８に従った坩堝の平面図である。FIG. 10 is a plan view of a crucible according to an eighth embodiment. 図２５中のＸＸＶＩ－ＸＸＶＩ線に沿った断面図である。FIG. 26 is a sectional view taken along line XXVI-XXVI in FIG. 25. 図２６中のＸＸＶＩＩ－ＸＸＶＩＩ線に沿った断面図である。FIG. 27 is a cross-sectional view along the line XXVII-XXVII in FIG. 26. 実施の形態８に従った坩堝の斜視図である。FIG. 10 is a perspective view of a crucible according to an eighth embodiment. 実施の形態９に従った坩堝の平面図である。FIG. 10 is a plan view of a crucible according to a ninth embodiment. 図２９中のＸＸＸ－ＸＸＸ線に沿った断面図である。FIG. 30 is a cross-sectional view taken along line XXX-XXX in FIG. 29. 実施の形態９に従った坩堝の斜視図である。FIG. 10 is a perspective view of a crucible according to a ninth embodiment. 実施の形態１０に従った坩堝の平面図である。FIG. 10 is a plan view of a crucible according to a tenth embodiment. 図３２中のＸＸＸＩＩＩ－ＸＸＸＩＩＩ線に沿った断面図である。FIG. 33 is a cross-sectional view taken along line XXXIII-XXXIII in FIG. 32. 図３３中のＸＸＸＩＶ－ＸＸＸＩＶ線に沿った断面図である。FIG. 34 is a cross-sectional view taken along line XXXIV-XXXIV in FIG. 33. 実施の形態１０に従った坩堝の斜視図である。FIG. 10 is a perspective view of a crucible according to a tenth embodiment. 実施の形態１１に従った坩堝の平面図である。FIG. 22 is a plan view of a crucible according to an eleventh embodiment. 図３６中のＸＸＸＶＩＩ－ＸＸＸＶＩＩ線に沿った断面図である。FIG. 37 is a cross-sectional view taken along line XXXVII-XXXVII in FIG. 36. 実施の形態１１に従った坩堝の斜視図である。FIG. 20 is a perspective view of a crucible according to an eleventh embodiment. 実施の形態１２に従った坩堝の平面図である。FIG. 38 is a plan view of a crucible according to a twelfth embodiment. 図３９中のＸＬ－ＸＬ線に沿った断面図である。FIG. 40 is a cross-sectional view taken along line XL-XL in FIG. 39. 図４０中のＸＬＩ－ＸＬＩ線に沿った断面図である。FIG. 41 is a cross-sectional view taken along line XLI-XLI in FIG. 40. 実施の形態１２に従った坩堝の斜視図である。FIG. 20 is a perspective view of a crucible according to a twelfth embodiment. 実施の形態１３に従った坩堝の平面図である。FIG. 38 is a plan view of a crucible according to a thirteenth embodiment. 図４３中のＸＬＩＶ－ＸＬＩＶ線に沿った断面図である。FIG. 44 is a cross-sectional view taken along line XLIV-XLIV in FIG. 43. 実施の形態１３に従った坩堝の斜視図である。FIG. 23 is a perspective view of a crucible according to a thirteenth embodiment. 実施の形態１４に従った坩堝の平面図である。FIG. 25 is a plan view of a crucible according to a fourteenth embodiment. 図４６中のＸＬＶＩＩ－ＸＬＶＩＩ線に沿った断面図である。FIG. 47 is a cross-sectional view taken along the line XLVII-XLVII in FIG. 46. 図４７中のＸＬＶＩＩＩ－ＸＬＶＩＩＩ線に沿った断面図である。FIG. 48 is a cross-sectional view taken along line XLVIII-XLVIII in FIG. 47. 実施の形態１４に従った坩堝の斜視図である。FIG. 25 is a perspective view of a crucible according to a fourteenth embodiment. 実施の形態１５に従った坩堝の平面図である。FIG. 20 is a plan view of a crucible according to a fifteenth embodiment. 図５０中のＬＩ－ＬＩ線に沿った断面図である。FIG. 51 is a cross-sectional view taken along line LI-LI in FIG. 50. 実施の形態１５に従った坩堝の斜視図である。FIG. 17 is a perspective view of a crucible according to a fifteenth embodiment. 実施の形態１６に従った坩堝の平面図である。FIG. 20 is a plan view of a crucible according to a sixteenth embodiment. 図５３中のＬＩＶ－ＬＩＶ線に沿った断面図である。FIG. 54 is a cross-sectional view taken along the line LIV-LIV in FIG. 53. 実施の形態１６に従った坩堝の斜視図である。20 is a perspective view of a crucible according to a sixteenth embodiment. FIG. 実施の形態１７に従った坩堝の平面図である。FIG. 20 is a plan view of a crucible according to a seventeenth embodiment. 図５６中のＬＶＩＩ－ＬＶＩＩ線に沿った断面図である。FIG. 57 is a cross-sectional view taken along line LVII-LVII in FIG. 56. 実施の形態１７に従った坩堝の斜視図である。FIG. 18 is a perspective view of a crucible according to a seventeenth embodiment. 実施の形態１８に従った坩堝の平面図である。FIG. 23 is a plan view of a crucible according to an eighteenth embodiment. 図５９中のＬＸ－ＬＸ線に沿った断面図である。FIG. 60 is a cross-sectional view taken along line LX-LX in FIG. 59. 実施の形態１８に従った坩堝の斜視図である。FIG. 20 is a perspective view of a crucible according to an eighteenth embodiment. 実施の形態１９に従った坩堝の平面図である。FIG. 38 is a plan view of a crucible according to a nineteenth embodiment. 図６２中のＬＸＩＩＩ－ＬＸＩＩＩ線に沿った断面図である。FIG. 63 is a cross-sectional view taken along line LXIII-LXIII in FIG. 62. 実施の形態１９に従った坩堝の斜視図である。FIG. 23 is a perspective view of a crucible according to a nineteenth embodiment. 実施の形態２０に従った坩堝の平面図である。FIG. 38 is a plan view of a crucible according to a twentieth embodiment. 図６５中のＬＸＶＩ－ＬＸＶＩ線に沿った断面図である。FIG. 66 is a cross-sectional view taken along line LXVI-LXVI in FIG. 65. 実施の形態２０に従った坩堝の斜視図である。FIG. 32 is a perspective view of a crucible according to a twentieth embodiment. 実施の形態２１に従った坩堝で用いられる上部坩堝側フランジ部の写真である。It is a photograph of the upper crucible side flange portion used in the crucible according to the twenty-first embodiment.

　[本願発明の実施形態の説明]
　坩堝は、モリブデンまたはその合金製の坩堝であって、開口が設けられた有底円筒形状の下部坩堝と、開口に嵌まり合う上部坩堝とを備え、上部坩堝は、モリブデンまたはその合金製の板材を曲げて板材の両端部を接合することで形成される。 [Description of Embodiment of Present Invention]
The crucible is a crucible made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible provided with an opening and an upper crucible fitted into the opening, and the upper crucible is a plate made of molybdenum or an alloy thereof. It is formed by bending both ends of the plate material.

　好ましくは、下部坩堝は、モリブデンまたはその合金製の板材を絞り加工することで形成され、開口には円筒の外周方向に延在する、円周方向に連続する下部坩堝側フランジ部が設けられている。 Preferably, the lower crucible is formed by drawing a plate made of molybdenum or an alloy thereof, and the opening is provided with a lower crucible side flange portion extending in the outer circumferential direction of the cylinder and continuing in the circumferential direction. Yes.

　好ましくは、上部坩堝は、開口の内周側に嵌め合わせられて下部坩堝に係合する係合部を有し、上部坩堝は下部坩堝に対して着脱自在に設けられる。 Preferably, the upper crucible has an engaging portion that is fitted to the inner peripheral side of the opening and engages with the lower crucible, and the upper crucible is detachably provided to the lower crucible.

　好ましくは、上部坩堝の下部には、円筒の半径方向に延在する上部坩堝側フランジ部が設けられている。 Preferably, an upper crucible side flange portion extending in the radial direction of the cylinder is provided at the lower portion of the upper crucible.

　坩堝は、モリブデンまたはその合金製の坩堝であって、開口が設けられた有底円筒形状の下部坩堝と、開口に嵌まり合う上部坩堝とを備え、上部坩堝は、モリブデンまたはその合金製の板材が継ぎ目なく周方向に連続することで形成される。 The crucible is a crucible made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible provided with an opening and an upper crucible fitted into the opening, and the upper crucible is a plate made of molybdenum or an alloy thereof. Is formed by continuous in the circumferential direction without seams.

　好ましくは、下部坩堝は、モリブデンまたはその合金製の板材を絞り加工することで形成され、開口には円筒の外周方向に延在する、円周方向に連続する下部坩堝側フランジ部が設けられている。 Preferably, the lower crucible is formed by drawing a plate made of molybdenum or an alloy thereof, and the opening is provided with a lower crucible side flange portion extending in the outer circumferential direction of the cylinder and continuing in the circumferential direction. Yes.

　好ましくは、上部坩堝は、下部坩堝に近い側の小径部と、下部坩堝から遠い側の大径部とを有し、小径部が下部坩堝の内側に嵌まり合う。 Preferably, the upper crucible has a small diameter portion on the side close to the lower crucible and a large diameter portion on the side far from the lower crucible, and the small diameter portion fits inside the lower crucible.

　好ましくは、大径部と小径部との間には内周側に向かって下方向に傾斜するテーパー面が設けられている。 Preferably, a tapered surface that is inclined downward toward the inner peripheral side is provided between the large-diameter portion and the small-diameter portion.

　好ましくは、小径部の下端に内側へ延在する縮径部が設けられている。
　単結晶サファイヤの製造方法は、上記のいずれかに記載のモリブデンまたはその合金製の坩堝の下部坩堝および上部坩堝に原料を充填する工程と、原料を溶融させたのち凝固させることで下部坩堝内に単結晶サファイヤを生成する工程とを備える。 Preferably, a reduced diameter portion extending inward is provided at the lower end of the small diameter portion.
The single crystal sapphire manufacturing method includes the steps of filling the lower crucible and upper crucible of the molybdenum or the alloy crucible described in any of the above, and melting the raw material and then solidifying it into the lower crucible. Producing a single crystal sapphire.

　[本願発明の実施形態の詳細]
　以下、本発明の実施形態の詳細について、図面を参照して説明する。 [Details of the embodiment of the present invention]
Hereinafter, details of embodiments of the present invention will be described with reference to the drawings.

　（実施の形態１）
　図１から３を参照して、実施の形態１に従った坩堝１は、モリブデンまたはその合金製であり、開口１１が設けられた有底円筒形状の下部坩堝１０と、開口１１に嵌まり合う上部坩堝２０とを備え、上部坩堝２０は、モリブデンまたはその合金製の板材２３を曲げて板材の両端部を接合することで形成される。下部坩堝１０は、モリブデンまたはその合金製の板材１３を絞り加工することで形成され、開口１１には円筒の外周方向に延在する、円周方向に連続する下部坩堝側フランジ部１２が設けられている。上部坩堝２０は、開口１１の内周側に嵌め合わせられて下部坩堝１０に係合する係合部２８を有し、上部坩堝２０は下部坩堝１０に対して着脱自在に設けられる。上部坩堝２０の下部には、円筒の半径方向に延在する上部坩堝側フランジ部３０が設けられている。 (Embodiment 1)
Referring to FIGS. 1 to 3, crucible 1 according to Embodiment 1 is made of molybdenum or an alloy thereof, and fits into opening 11 with bottomed cylindrical lower crucible 10 provided with opening 11. The upper crucible 20 includes an upper crucible 20, and the upper crucible 20 is formed by bending a plate 23 made of molybdenum or its alloy and joining both ends of the plate. The lower crucible 10 is formed by drawing a plate 13 made of molybdenum or an alloy thereof, and the opening 11 is provided with a lower crucible side flange portion 12 extending in the circumferential direction and extending in the circumferential direction. ing. The upper crucible 20 has an engaging portion 28 that is fitted to the inner peripheral side of the opening 11 and engages with the lower crucible 10, and the upper crucible 20 is provided detachably with respect to the lower crucible 10. An upper crucible side flange 30 extending in the radial direction of the cylinder is provided at the lower portion of the upper crucible 20.

　板材２３の両端部が当て板４０に溶接されている。下部坩堝１０の側壁が鉛直方向に対してなす角度θ１は、約１０°であり、上部坩堝２０の側壁は鉛直方向とほぼ平行に配置される。上部坩堝２０に底は無く、上部坩堝２０と下部坩堝１０とが連通している。 Both end portions of the plate material 23 are welded to the contact plate 40. The angle θ1 formed by the side wall of the lower crucible 10 with respect to the vertical direction is about 10 °, and the side wall of the upper crucible 20 is arranged substantially parallel to the vertical direction. The upper crucible 20 has no bottom, and the upper crucible 20 and the lower crucible 10 communicate with each other.

　（実施の形態２）
　図４から７を参照して、実施の形態２に従った坩堝１では、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２が約１０°である点で、実施の形態１に従った坩堝１と異なる。 (Embodiment 2)
4 to 7, according to the crucible 1 according to the second embodiment, the angle θ2 formed by the side wall of the upper crucible 20 with respect to the vertical direction is approximately 10 °, and according to the first embodiment. Different from the crucible 1.

　（実施の形態３）
　図８から１０を参照して、実施の形態３に従った坩堝１では、下部坩堝１０の側壁が鉛直方向に対してなす角度θ１が約２°である点で、実施の形態１に従った坩堝１と異なる。さらに、下部坩堝１０にフランジが設けられていない点で、実施の形態１に従った坩堝１と異なる。 (Embodiment 3)
With reference to FIGS. 8 to 10, according to the crucible 1 according to the third embodiment, the angle θ <b> 1 formed by the side wall of the lower crucible 10 with respect to the vertical direction is approximately 2 °, according to the first embodiment. Different from the crucible 1. Furthermore, the lower crucible 10 is different from the crucible 1 according to the first embodiment in that no flange is provided.

　（実施の形態４）
　図１１から１４を参照して、実施の形態４に従った坩堝１では、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２が約２°である点で、実施の形態２に従った坩堝１と異なる。さらに、下部坩堝１０にフランジが設けられていない点で、実施の形態２に従った坩堝１と異なる。 (Embodiment 4)
Referring to FIGS. 11 to 14, according to the crucible 1 according to the fourth embodiment, the angle θ <b> 2 formed by the side wall of the upper crucible 20 with respect to the vertical direction is approximately 2 °, according to the second embodiment. Different from the crucible 1. Furthermore, the lower crucible 10 is different from the crucible 1 according to the second embodiment in that no flange is provided.

　（実施の形態５）
　図１５から１７を参照して、実施の形態５に従った坩堝１では、上部坩堝２０の端部がリベット５０により当て板４０に接合されている点で、実施の形態１に従った坩堝１と異なる。リベット５０は２列に並列に配置され、縦方向に８つのリベット５０が設けられている。 (Embodiment 5)
With reference to FIGS. 15 to 17, in the crucible 1 according to the fifth embodiment, the crucible 1 according to the first embodiment is that the end of the upper crucible 20 is joined to the caulking plate 40 by a rivet 50. And different. The rivets 50 are arranged in parallel in two rows, and eight rivets 50 are provided in the vertical direction.

　（実施の形態６）
　図１８から２１を参照して、実施の形態６に従った坩堝１では、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２が約１０°である点で、実施の形態５に従った坩堝１と異なる。 (Embodiment 6)
18 to 21, according to the crucible 1 according to the sixth embodiment, the angle θ2 formed by the side wall of the upper crucible 20 with respect to the vertical direction is approximately 10 °, according to the fifth embodiment. Different from the crucible 1.

　（実施の形態７）
　図２２から２４を参照して、実施の形態７に従った坩堝１では、当て板４０において、リベット５０は２列に千鳥状に配置され、縦方向に４つのリベット５０が設けられている点で、実施の形態５に従った坩堝１と異なる。 (Embodiment 7)
With reference to FIGS. 22 to 24, in crucible 1 according to the seventh embodiment, rivets 50 are arranged in a staggered manner in two rows in pad plate 40, and four rivets 50 are provided in the vertical direction. Thus, it differs from the crucible 1 according to the fifth embodiment.

　（実施の形態８）
　図２５から２８を参照して、実施の形態８に従った坩堝１では、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２が約１０°である点で、実施の形態７に従った坩堝１と異なる。 (Embodiment 8)
Referring to FIGS. 25 to 28, in crucible 1 according to the eighth embodiment, according to the seventh embodiment, the angle θ2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 10 °. Different from the crucible 1.

　（実施の形態９）
　図２９から３１を参照して、実施の形態９に従った坩堝１では、当て板４０において、リベット５０は２列に並列に配置され、縦方向に４つのリベット５０が設けられている点で、実施の形態５に従った坩堝１と異なる。 (Embodiment 9)
With reference to FIGS. 29 to 31, in crucible 1 according to the ninth embodiment, rivets 50 are arranged in two rows in parallel in pad plate 40, and four rivets 50 are provided in the vertical direction. , Different from crucible 1 according to the fifth embodiment.

　（実施の形態１０）
　図３２から３５を参照して、実施の形態１０に従った坩堝１では、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２が約１０°である点で、実施の形態９に従った坩堝１と異なる。 (Embodiment 10)
Referring to FIGS. 32 to 35, in crucible 1 according to the tenth embodiment, the angle θ2 formed by the side wall of upper crucible 20 with respect to the vertical direction is approximately 10 °, according to the ninth embodiment. Different from the crucible 1.

　（実施の形態１１）
　図３６から３８を参照して、実施の形態１１に従った坩堝１では、当て板４０において、リベット５０は２列に並列に配置され、縦方向に１２個のリベット５０が設けられている点で、実施の形態５に従った坩堝１と異なる。 (Embodiment 11)
36 to 38, in crucible 1 according to the eleventh embodiment, rivets 50 are arranged in two rows in parallel in pad plate 40, and twelve rivets 50 are provided in the vertical direction. Thus, it differs from the crucible 1 according to the fifth embodiment.

　（実施の形態１２）
　図３９から４２を参照して、実施の形態１２に従った坩堝１では、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２が約１０°である点で、実施の形態１１に従った坩堝１と異なる。 (Embodiment 12)
Referring to FIGS. 39 to 42, in crucible 1 according to the twelfth embodiment, according to the eleventh embodiment, the angle θ2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 10 °. Different from the crucible 1.

　（実施の形態１３）
　図４３から４５を参照して、実施の形態１３に従った坩堝１では、当て板４０において、リベット５０は２列に千鳥状に配置され、縦方向に６つのリベット５０が設けられている点で、実施の形態５に従った坩堝１と異なる。 (Embodiment 13)
43 to 45, in crucible 1 according to the thirteenth embodiment, in rivet plate 40, rivets 50 are arranged in a staggered pattern in two rows, and six rivets 50 are provided in the vertical direction. Thus, it differs from the crucible 1 according to the fifth embodiment.

　（実施の形態１４）
　図４６から４９を参照して、実施の形態１４に従った坩堝１では、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２が約１０°である点で、実施の形態１３に従った坩堝１と異なる。 (Embodiment 14)
46 to 49, in crucible 1 according to the fourteenth embodiment, according to the thirteenth embodiment, the angle θ2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 10 °. Different from the crucible 1.

　（実施の形態１５）
　図５０から５２を参照して、実施の形態１５に従った坩堝１は、モリブデンまたはその合金製の坩堝１であって、開口１１が設けられた有底円筒形状の下部坩堝１０と、開口１１に嵌まり合う上部坩堝２０とを備え、上部坩堝２０は、モリブデンまたはその合金製の板材２３が継ぎ目なく周方向に連続することで形成される。 (Embodiment 15)
Referring to FIGS. 50 to 52, crucible 1 according to the fifteenth embodiment is a crucible 1 made of molybdenum or an alloy thereof, and includes a bottomed cylindrical lower crucible 10 provided with an opening 11 and an opening 11. And the upper crucible 20 is formed by continuously connecting the plate material 23 made of molybdenum or its alloy seamlessly in the circumferential direction.

　下部坩堝１０は、モリブデンまたはその合金製の板材１３を絞り加工することで形成され、開口１１には円筒の外周方向に延在する、円周方向に連続する下部坩堝側フランジ部１２が設けられている。上部坩堝２０は、下部坩堝１０に近い側の小径部２５と、下部坩堝１０から遠い側の大径部２７とを有し、小径部２５が下部坩堝１０の内側に嵌まり合う。大径部２７と小径部２５との間には内周側に向かって下方向に傾斜するテーパー面２６が設けられている。小径部２５の下端に内側へ延在する縮径部２４が設けられている。 The lower crucible 10 is formed by drawing a plate 13 made of molybdenum or an alloy thereof, and the opening 11 is provided with a lower crucible side flange portion 12 extending in the circumferential direction and extending in the circumferential direction. ing. The upper crucible 20 has a small diameter portion 25 on the side close to the lower crucible 10 and a large diameter portion 27 on the side far from the lower crucible 10, and the small diameter portion 25 fits inside the lower crucible 10. A tapered surface 26 is provided between the large-diameter portion 27 and the small-diameter portion 25 and is inclined downward toward the inner peripheral side. A reduced diameter portion 24 extending inward is provided at the lower end of the small diameter portion 25.

　下部坩堝１０の側壁が鉛直方向に対してなす角度θ１は、約１０°であり、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２は約１０°である。上部坩堝２０に底は無く、上部坩堝２０と下部坩堝１０とが連通している。 The angle θ1 made by the side wall of the lower crucible 10 with respect to the vertical direction is about 10 °, and the angle θ2 made by the side wall of the upper crucible 20 with respect to the vertical direction is about 10 °. The upper crucible 20 has no bottom, and the upper crucible 20 and the lower crucible 10 communicate with each other.

　（実施の形態１６）
　図５３から５５を参照して、実施の形態１６に従った坩堝１では、上部坩堝２０に縮径部２４が設けられていない点で、実施の形態１５に従った坩堝１と異なる。 (Embodiment 16)
Referring to FIGS. 53 to 55, crucible 1 according to the sixteenth embodiment is different from crucible 1 according to the fifteenth embodiment in that reduced diameter portion 24 is not provided in upper crucible 20.

　（実施の形態１７）
　図５６から５８を参照して、実施の形態１７に従った坩堝１では、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２が約２°である点で、実施の形態１６に従った坩堝１と異なる。 (Embodiment 17)
56 to 58, in crucible 1 according to the seventeenth embodiment, according to the sixteenth embodiment, the angle θ2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 2 °. Different from the crucible 1.

　（実施の形態１８）
　図５９から６１を参照して、実施の形態１８に従った坩堝１では、下部坩堝１０の側壁が鉛直方向に対してなす角度θ１が２°であり、下部坩堝側フランジが存在しない点で、実施の形態１５に従った坩堝１と異なる。 (Embodiment 18)
59 to 61, in crucible 1 according to the eighteenth embodiment, angle θ1 formed by the side wall of lower crucible 10 with respect to the vertical direction is 2 °, and there is no lower crucible side flange. Different from crucible 1 according to the fifteenth embodiment.

　（実施の形態１９）
　図６２から６４を参照して、実施の形態１９に従った坩堝１では、上部坩堝２０に縮径部２４が設けられていない点で、実施の形態１８に従った坩堝１と異なる。 (Embodiment 19)
62 to 64, crucible 1 according to the nineteenth embodiment differs from crucible 1 according to the eighteenth embodiment in that reduced diameter portion 24 is not provided in upper crucible 20.

　（実施の形態２０）
　図６５から６７を参照して、実施の形態２０に従った坩堝１では、上部坩堝２０の側壁が鉛直方向に対してなす角度θ２が約２°である点で、実施の形態１６に従った坩堝１と異なる。 (Embodiment 20)
65 to 67, in crucible 1 according to the twentieth embodiment, according to the sixteenth embodiment, the angle θ2 formed by the side wall of upper crucible 20 with respect to the vertical direction is about 2 °. Different from the crucible 1.

　上記の実施の形態１から２０では、下部坩堝１０本体の内容積を有効に利用し、大きな単結晶サファイアインゴットを製作できるように、原料充填量を増加させ得る上部坩堝２０を追加している。坩堝１の材質は融点２６００℃超の耐高温性能に優れる金属モリブデン及びその合金であり、高温変形に強く、数ｍｍ程度の厚さで原料アルミナの溶解に耐え得る特性を有している。 In the above-described first to twentieth embodiments, the upper crucible 20 capable of increasing the raw material filling amount is added so that the inner volume of the lower crucible 10 main body can be effectively used and a large single crystal sapphire ingot can be manufactured. The material of the crucible 1 is a metal molybdenum and its alloy having a melting point of over 2600 ° C. and excellent in high temperature resistance, and is resistant to high temperature deformation and has a characteristic of withstanding melting of raw material alumina with a thickness of about several mm.

　（実施の形態２１）
　図６８を参照して、実施の形態２１では、上部坩堝側フランジ部３０は、複数の爪部３１０，３２０，３３０，３４０と、それらの爪部３１０．３２０．３３０．３４０が接続される胴部３００とを有する。複数の爪部３１０，３２０，３３０，３４０を設け、各々の爪部３１０，３２０，３３０，３４０の間に隙間が設けられている。そのため、爪部が一枚の板材により構成されている構造と比較して、上部坩堝側フランジ部３０を容易に製造することができる。 (Embodiment 21)
Referring to FIG. 68, in the twenty-first embodiment, upper crucible side flange portion 30 includes a plurality of claws 310, 320, 330, 340 and a barrel to which these claws 310.30.30.340 are connected. Part 300. A plurality of claw portions 310, 320, 330, and 340 are provided, and a gap is provided between each claw portion 310, 320, 330, and 340. Therefore, it is possible to easily manufacture the upper crucible side flange portion 30 as compared with a structure in which the claw portion is formed of a single plate material.

　この実施の形態２１では４つの爪部３１０，３２０，３３０，３４０が開示されているが、さらに多い爪部または少ない爪部が設けられていてもよい。実施の形態２１に従った上部坩堝側フランジ部３０を、他の実施の形態にも適用してよい。 In the twenty-first embodiment, four claw portions 310, 320, 330, and 340 are disclosed, but more or fewer claw portions may be provided. The upper crucible side flange portion 30 according to the twenty-first embodiment may be applied to other embodiments.

　胴部３００はリベット５０により板材２３に固定されている。胴部３００が溶接、ロウ材など、リベット以外で板材２３に固定されていてもよい。 The barrel 300 is fixed to the plate member 23 by rivets 50. The body part 300 may be fixed to the plate member 23 other than rivets, such as welding or brazing material.

　（坩堝の構造）
　実施の形態１から２０で示す、モリブデン製及びその合金製の坩堝１を用いて単結晶サファイアを製造することができる。厚さ数ｍｍ程度のモリブデン板材或いはモリブデン合金板材を板金加工によって丸め成形後リベット５０で接合し（実施の形態５から１４）、或いは溶接して（実施の形態１から４）、円筒或いは中空円錐台を作る。また、或いは絞り成型して（実施の形態１５から２０）上部坩堝２０を作り、当該上部坩堝２０の底部を切削加工によって除去し、円筒或いは中空円錐台となす。これらを本体として、外周部の数か所にリベット接合又は溶接によって上部坩堝側フランジ部３０を後付けし（板金加工の場合）、或いは外周部の全周にフランジ（テーパー面２６）を形成し（絞り成型の場合）、これらのフランジを介して下部坩堝１０上縁部に上部坩堝２０が載せ置かれる。 (Crucible structure)
Single crystal sapphire can be manufactured using the crucible 1 made of molybdenum and its alloy shown in Embodiments 1 to 20. A molybdenum plate or molybdenum alloy plate having a thickness of about several millimeters is rounded and formed by sheet metal processing and joined with a rivet 50 (Embodiments 5 to 14) or welded (Embodiments 1 to 4) to form a cylinder or a hollow cone Make a stand. Alternatively, the upper crucible 20 is made by drawing (Embodiments 15 to 20), and the bottom of the upper crucible 20 is removed by cutting to form a cylinder or a hollow truncated cone. With these as the main body, the upper crucible side flange 30 is retrofitted by rivet joining or welding to several places on the outer periphery (in the case of sheet metal processing), or a flange (tapered surface 26) is formed on the entire outer periphery ( In the case of drawing), the upper crucible 20 is placed on the upper edge of the lower crucible 10 through these flanges.

　（坩堝の製造方法）
　上部坩堝の製造方法を、Ａ；リベット接合、Ｂ；溶接、Ｃ；絞り成型の３種類に分けて記述する。 (Crucible manufacturing method)
The manufacturing method of the upper crucible will be described by dividing it into three types: A; rivet joining, B: welding, C;

　Ａ；リベット接合による、厚さ３ｍｍｘ上端外径３３０ｍｍｘ下端外径３００ｍｍｘ高さ２００ｍｍの中空円錐台状坩堝（突き出し幅２０ｍｍで長さ５０ｍｍの４等配フランジ付き）の製造方法。 A: A manufacturing method of a hollow frustoconical crucible having a thickness of 3 mm, an upper end outer diameter of 330 mm, a lower end outer diameter of 300 mm and a height of 200 mm by rivet joining (with a four-equal flange with a protruding width of 20 mm and a length of 50 mm).

　工程Ａ１；坩堝用および当て板用の各板材
　冷間圧延仕上げされた表面粗さＲａ５μｍ程度のモリブデン板材、或いは酸化ランタン添加合金、ＴＺＭ合金などのモリブデン合金板材を準備する。坩堝用の冷間圧延板材サイズは、厚さ３ｍｍｘ幅２５０ｍｍｘ長さ１１００ｍｍである。この圧延板材を放電ワイヤーカット機などを用いて、扇状の丸め加工用素材に素材展開図に基づいて切り出す。この丸め加工用素材には展開図に基づき、リベット接合用のドリル貫通穴（直径３ｍｍ、当て板接合用、フランジ接合用ともに）をボール盤を用いて開けておく。 Step A1: Each plate material for crucible and backing plate A molybdenum plate material having a surface roughness Ra of about 5 μm, or a molybdenum alloy plate material such as a lanthanum oxide-added alloy or a TZM alloy is prepared. The cold-rolled plate size for the crucible is 3 mm thick x 250 mm wide x 1100 mm long. This rolled sheet is cut into a fan-shaped rounding material based on the material development using a discharge wire cutting machine or the like. A drill through hole for rivet joining (diameter 3 mm, both for contact plate joining and flange joining) is opened in the rounding material using a drilling machine based on the development.

　当て板用の圧延板材は坩堝用板材と同材質で、厚さ３ｍｍｘ幅８０ｍｍｘ長さ１５０ｍｍに放電ワイヤーカット機或いはシェアカッターなどで寸法だし切断する。展開図に基づきリベット用の貫通穴を、上述のとおり事前に設けておく。 The rolled plate material for the contact plate is the same material as the plate material for the crucible, and is dimensioned and cut with a discharge wire cutter or a shear cutter to a thickness of 3 mm x width 80 mm x length 150 mm. Based on the developed view, a through hole for a rivet is provided in advance as described above.

　工程Ａ２；フランジ用およびリベット用の板・棒材
　坩堝素材と同質で、同様の表面粗度の板材（厚さ３ｍｍｘ幅５０ｍｍｘ長さは任意で２００ｍｍ～１０００ｍｍ程度）および棒材（直径３ｍｍｘ長さ１０００ｍｍ程度）を用いる。 Step A2: Flange and rivet plate / bar material The same quality as the crucible material and the same surface roughness (thickness 3 mm x width 50 mm x length is optionally about 200 mm to 1000 mm) and bar (diameter 3 mm x length) About 1000 mm).

　フランジ用部品は、４個分を長さ２００ｍｍで切断しておく。フランジ取り付けに用いるリベット用の棒材もフランジ用板材と同材質で準備し、砥石刃切断或いは放電ワイヤカット機などで長さ１２ｍｍに切断した後、切断バリを砥石などで除去しておく。 ¡Four parts for the flange are cut to a length of 200mm. The rivet rod used for the flange attachment is also prepared with the same material as the flange plate, cut to a length of 12 mm with a grinding wheel cutting or a discharge wire cutter, and then the cutting burr is removed with a grinding stone or the like.

　工程Ａ３；丸め、Ｌ字曲げなどの板金加工
　工程Ａ１および工程Ａ２で準備した素材或いは部品の成型加工について、順次記載する。 Step A3: Sheet metal processing such as rounding and L-shaped bending The materials or parts prepared in Step A1 and Step A2 will be sequentially described.

　工程Ａ１で準備した丸め加工用素材を、市販のローラーベンダーで円錐台形状に丸め加工を施し、確実に突き合うことを確認する。 The rounding material prepared in step A1 is rounded into a truncated cone shape with a commercially available roller bender, and it is confirmed that it is abutted securely.

　当て板についてはブレーキプレス（KOMAT’SU製PAS5020）で、坩堝外面の曲率に合わせて丸め加工を施した。突き合せ部の外側に当て板をあてがい、リベット穴の微小変形修正、相互位置などを確認した。穴の微小変形はダイヤモンドやすりなどで手修正する。 The patch plate was rounded with a brake press (PAS5020 manufactured by KOMAT’SU) according to the curvature of the outer surface of the crucible. A patch plate was placed on the outside of the abutting part, and the minute deformation correction of the rivet hole and the mutual position were confirmed. The minute deformation of the hole is corrected manually with a diamond file.

　工程Ａ２で準備した５０ｍｍ幅板材を２：３の幅になるように、長さ方向に沿ってＬ字状にブレーキプレスによって曲げ加工を実施した。このＬ字状部品から、４個の長さ５０ｍｍＬ型フランジを切断して得た。Ｌ字の幅が広い側にリベット用貫通穴を４穴、直線状にボール盤を用いて開ける。その後、ブレーキプレスを用いて、穴付き側を坩堝外面曲率に合わせて曲げ加工する。曲げ加工によって微小変形した穴は、やすりなどで修正しておく。 The 50 mm width plate material prepared in step A2 was bent by a brake press in an L shape along the length direction so as to have a width of 2: 3. This L-shaped part was obtained by cutting four 50 mm long L-shaped flanges. Four rivet through-holes are opened on the wide side of the L-shape, using a drilling machine in a straight line. Thereafter, using a brake press, the holed side is bent in accordance with the crucible outer surface curvature. A hole that has been deformed by bending is corrected with a file.

　工程Ａ４；組み立て加工
　上部坩堝本体は、製作した各部品をリベット接合によって組み付けることで完成する。先ず上部坩堝本体を組み上げる。補助治具類を用いて坩堝を仮組みしておき、当て板を坩堝上縁部基準にして、直線または千鳥状に配列された穴に棒材を通し、内側に３ｍｍ突き出させて小径バーナーで加熱して小ハンマーで叩いて潰す。全ての穴を埋めた後、外側に３ｍｍ突き出した棒を小ハンマーで叩いて潰し、リベット接合を完成させる。 Step A4: Assembly Processing The upper crucible body is completed by assembling the manufactured parts by rivet bonding. First, the upper crucible body is assembled. Temporarily assemble the crucible using auxiliary jigs, pass the bar through the holes arranged in a straight line or zigzag pattern with the base plate as a reference to the upper edge of the crucible, and protrude 3 mm inward with a small diameter burner Heat and crush with a small hammer. After filling all the holes, the rod protruding 3 mm outward is crushed with a small hammer to complete the rivet joint.

　次に、４個のフランジを組み付ける。当て板の下端部外の４等配外周面に、当て金を組み付ける要領で作業を行い、フランジの組みつけを完成させる。 Next, assemble four flanges. The flange assembly is completed by performing the work in the manner of assembling the stopper metal on the four-equal outer peripheral surface outside the lower end of the stopper plate.

　この際、潰した部分のバリは、小型リューター或いはマイクロ研磨機を用いて除去する。こうして、リベット接合による４等配フランジ付き上部坩堝が完成する。 At this time, the crushed burrs are removed by using a small luter or a micro polishing machine. Thus, an upper crucible with four equally spaced flanges by rivet joining is completed.

　Ｂ；溶接による、厚さ３ｍｍｘ上端外径３３０ｍｍｘ下端外径３００ｍｍｘ高さ２００ｍｍの中空円錐台状坩堝（突き出し幅２０ｍｍで長さ５０ｍｍの４等配フランジ付き）の製造方法。 B: Manufacturing method of a hollow frustoconical crucible having a thickness of 3 mm, an upper end outer diameter of 330 mm, a lower end outer diameter of 300 mm and a height of 200 mm by welding (with a four-part flange having a protruding width of 20 mm and a length of 50 mm).

　工程Ｂ１；坩堝用板材
　上記Ａ１と同じ材質・規格・品質の板材を用いる。冷間圧延仕上げされた表面粗さＲａ５μｍ程度のモリブデン板材、或いは酸化ランタン添加合金、ＴＺＭ合金などのモリブデン合金板材を準備する。坩堝用の冷間圧延板材サイズは、厚さ３ｍｍｘ幅２５０ｍｍｘ長さ１１００ｍｍである。この圧延板材を放電ワイヤーカット機などを用いて、扇状の丸め加工用素材に素材展開図に基づいて切り出す。この丸め加工用素材には展開図に基づき、リベット接合用のドリル貫通穴（直径３ｍｍ、フランジ接合用）をボール盤を用いて開けておく。全ての接合を溶接工法で行う場合は、貫通穴加工は不要である。 Process B1: Crucible plate material A plate material having the same material, standard and quality as A1 is used. A molybdenum plate material having a surface roughness Ra of about 5 μm, or a molybdenum alloy plate material such as a lanthanum oxide-added alloy or a TZM alloy is prepared. The cold-rolled plate size for the crucible is 3 mm thick x 250 mm wide x 1100 mm long. This rolled sheet is cut into a fan-shaped rounding material based on the material development using a discharge wire cutting machine or the like. Based on the developed view, a drill through hole (3 mm diameter, for flange connection) for rivet bonding is opened in the rounding material using a drilling machine. When all the joining is performed by the welding method, the through hole processing is unnecessary.

　工程Ｂ２；フランジ用板材
　坩堝素材と同質で、同様の表面粗度の板材（厚さ３ｍｍｘ幅５０ｍｍｘ長さは任意で２００ｍｍ～１０００ｍｍ程度）を用いる。フランジ用部品は、４個分を長さ２００ｍｍで切断しておく。棒材（直径３ｍｍｘ長さ１０００ｍｍ程度）を用いる。
フランジ取り付けに用いるリベット用の棒材も、フランジ用板材と同材質で準備し、砥石刃切断或いは放電ワイヤカット機などで長さ１２ｍｍに切断した後、切断バリを砥石などで除去しておく。なお、フランジを坩堝本体に溶接工法で取り付ける場合は棒材は不要である。 Step B2: Flange Plate Material A plate material having the same quality as the crucible material and the same surface roughness (thickness 3 mm × width 50 mm × length is optionally about 200 mm to 1000 mm) is used. Four flange parts are cut to a length of 200 mm. Bar material (diameter 3 mm x length 1000 mm) is used.
The rivet bar used for flange mounting is also prepared with the same material as the flange plate, cut to a length of 12 mm with a grinding wheel cutting or a discharge wire cutter, and then the cutting burr is removed with a grinding stone. In addition, when attaching a flange to a crucible main body with a welding method, a bar is unnecessary.

　工程Ｂ３；丸め、Ｌ字曲げなどの板金加工
　リベット接合によって製作する場合と同様工程Ａ３の手順で、坩堝本体用部品の丸め加工およびフランジ用部品のＬ字曲げ加工を実施する。 Step B3: Sheet metal processing such as rounding and L-shaped bending The rounding of the crucible body part and the L-shaped bending of the flange part are performed in the same manner as in the case of manufacturing by rivet joining.

　工程Ｂ４；組み立て加工
　溶接中の酸化脆化を防止するために、不活性ガスで置換したチャンバー内でＴＩＧ溶接を実施する。補助治具類で仮組みした坩堝本体を、先ず溶接する。丸め加工した突合せ部を３～４箇所点止め溶接した後、突合せ部全域を溶接して本体坩堝を完成させる。 Step B4: Assembly processing In order to prevent oxidation embrittlement during welding, TIG welding is performed in a chamber replaced with an inert gas. First, the crucible body temporarily assembled with auxiliary jigs is welded. After the rounded butt portion is welded at 3 to 4 points, the entire butt portion is welded to complete the main body crucible.

　フランジを坩堝本体に溶接する場合も、治具類で仮固定した後、フランジ部外周を坩堝外周部に溶接する（４～６箇所の点止めでも良い）。リベット接合する場合は工程Ａ４の方法と同じである。 Also when the flange is welded to the crucible body, after temporarily fixing with a jig, the outer periphery of the flange is welded to the outer periphery of the crucible (4 to 6 points may be fixed). In the case of riveting, the method is the same as that in step A4.

　こうして、溶接による（或いは一部リベット接合による）４等配フランジ付き上部坩堝が完成する。 In this way, an upper crucible with four equally spaced flanges is completed by welding (or by partial rivet joining).

　Ｃ；絞り加工による、厚さ３ｍｍｘ上端外径３３０ｍｍｘ下端外径３００ｍｍｘ高さ２００ｍｍの中空円錐台状坩堝（突き出し幅２０ｍｍで長さ５０ｍｍの４等配フランジ付き）の製造方法。 C: A manufacturing method of a hollow frustoconical crucible having a thickness of 3 mm, an upper end outer diameter of 330 mm, a lower end outer diameter of 300 mm and a height of 200 mm by a drawing process (with a four-equal flange with a protruding width of 20 mm and a length of 50 mm).

　工程Ｃ１；坩堝用板材
　上記と同じ材質・規格・品質の板材を用いる。冷間圧延仕上げされた表面粗さＲａ５μｍ程度のモリブデン板材、或いは酸化ランタン添加合金、ＴＺＭ合金などのモリブデン合金板材を準備する。坩堝用の冷間圧延板材サイズは、厚さ３ｍｍｘ□６２０ｍｍである。この圧延板材を放電ワイヤーカット機や旋盤などを用いて、厚さ３ｍｍｘ直径６００ｍｍの絞り成型用ブランク材を切り出す。 Process C1: Crucible plate material A plate material having the same material, standard and quality as described above is used. A molybdenum plate material having a surface roughness Ra of about 5 μm, or a molybdenum alloy plate material such as a lanthanum oxide-added alloy or a TZM alloy is prepared. The cold-rolled plate size for the crucible is 3 mm × □ 620 mm in thickness. Using this rolled sheet material, a drawing blank material having a thickness of 3 mm and a diameter of 600 mm is cut out using a discharge wire cutting machine or a lathe.

　工程Ｃ２；　フランジ用板材
　坩堝素材と同質で、同様の表面粗度の板材（厚さ３ｍｍｘ幅５０ｍｍｘ長さは任意で２００ｍｍ～１０００ｍｍ程度）を用いる。フランジ用部品は、４個分を長さ２００ｍｍで切断しておく。棒材（直径３ｍｍｘ長さ１０００ｍｍ程度）を用いる。 Step C2: Flange plate material A plate material having the same quality as the crucible material and the same surface roughness (thickness 3 mm × width 50 mm × length is optionally about 200 mm to 1000 mm) is used. Four flange parts are cut to a length of 200 mm. Bar material (diameter 3 mm x length 1000 mm) is used.

　フランジ取り付けに用いるリベット用の棒材も、フランジ用板材と同材質で準備し、砥石刃切断或いは放電ワイヤーカット機などで長さ１２ｍｍに切断した後、切断バリを砥石などで除去しておく。なお、フランジを坩堝本体に溶接工法で取り付ける場合は棒材は不要である。 The rod material for rivets used for flange mounting is also prepared with the same material as the flange plate material, cut to a length of 12 mm with a grinding wheel cutting or a discharge wire cutting machine, and then the cutting burr is removed with a grinding stone. In addition, when attaching a flange to a crucible main body with a welding method, a bar is unnecessary.

　工程Ｃ３；絞り成型加工およびＬ字曲げ加工
スピニングマシンを用いて、坩堝本体の絞り成型加工を行う。スピニングマシンは装置本体、中子となる金型、押し当て棒、およびローラーで主構成されている。被成型加工材であるブランク材を、ローラーによって金型外面に押しつけるようにして成型する加工方法である。 Step C3: Drawing and processing the crucible body using a drawing and L-shaped spinning machine. The spinning machine mainly includes an apparatus main body, a mold as a core, a pressing rod, and a roller. This is a processing method in which a blank material, which is a material to be molded, is molded by pressing it against the outer surface of a mold with a roller.

　横型回転軸に金型が取り付けられ、直径６００ｍｍブランク材、押し当て棒が直列に並び、１００～３００ｒｐｍで回転するブランク材をプロパンバーナーなどで赤熱しながら、側方から繰り出されるローラーによって、金型になぞらえて坩堝形状に成型する。被成型材が金型から外れる形状であれば、坩堝側壁が直線状のみならず階段状であっても成型可能である。円筒坩堝を製作するには、底部を設計した形状に仕上げる必要がある。仕上げは横型旋盤などを利用してバイトによって削り落し、任意の形状の底なし（中空）坩堝を得ることができる。 A mold is attached to a horizontal rotation shaft, a blank material with a diameter of 600 mm, a pressing rod are arranged in series, and the blank material rotating at 100 to 300 rpm is heated red by a propane burner etc. It is shaped like a crucible. If the material to be molded is a shape that can be removed from the mold, the crucible side wall can be molded not only in a straight line but also in a step shape. In order to manufacture a cylindrical crucible, it is necessary to finish the bottom to the designed shape. Finishing can be scraped off with a cutting tool using a horizontal lathe to obtain a bottomless (hollow) crucible of any shape.

　なお、坩堝底部にあたる部分に小径の穴をブランク材に事前に設けておくことができる。しかしながら、大径の穴を事前に設けておくと、絞り加工に際して亀裂発生の原因となるおそれがあり好ましくない。 It should be noted that a small-diameter hole can be provided in advance in the blank material at the portion corresponding to the bottom of the crucible. However, providing a large-diameter hole in advance is not preferable because it may cause cracks during drawing.

　このようにして、厚さ３ｍｍｘ上端外径３３０ｍｍｘ下端外径３００ｍｍｘ高さ２００ｍｍの中空円錐台状坩堝を得る。 Thus, a hollow frustoconical crucible having a thickness of 3 mm × an upper end outer diameter of 330 mm × a lower end outer diameter of 300 mm × a height of 200 mm is obtained.

　フランジ用部品については、工程Ａ２と同様であるので再掲した。工程Ａ２で準備した５０ｍｍ幅板材を２：３の幅になるように、長さ方向に沿ってＬ字状にブレーキプレスによって曲げ加工を実施した。このＬ字状部品から、４個の長さ５０ｍｍＬ型フランジを切断して得た。Ｌ字の幅が広い側にリベット用貫通穴を５穴、千鳥状にボール盤を用いて開ける。その後、ブレーキプレスを用いて、穴付き側を坩堝外面曲率に合わせて曲げ加工する。曲げ加工によって微小変形した穴は、やすりなどで修正しておく。 The flange parts are the same as in step A2, so they are shown again. The 50 mm width plate material prepared in step A2 was bent into a L shape along the length direction by a brake press so as to have a width of 2: 3. This L-shaped part was obtained by cutting four 50 mm long L-shaped flanges. Five rivet through-holes are opened on the wide L-shaped side, and a staggered drilling machine is used. Thereafter, using a brake press, the holed side is bent in accordance with the crucible outer surface curvature. A hole that has been deformed by bending is corrected with a file.

　工程Ｃ４；組み立て加工
　フランジはリベットによる接合、或いは溶接工法によっても取り付けができる。その方法・作業手順は上述のとおりである。坩堝本体外周に階段状のフランジ部分が形成されている坩堝においては、フランジ自体が不要である。 Process C4; assembly process The flange can be attached by joining with a rivet or by a welding method. The method and work procedure are as described above. In a crucible in which a stepped flange portion is formed on the outer periphery of the crucible body, the flange itself is unnecessary.

　このようにして、溶接による（或いは一部リベット接合による）４等配フランジ付き上部坩堝が完成する。 In this way, an upper crucible with four equally spaced flanges is completed by welding (or by partial rivet joining).

　（効果の確認）
　製作した４等配フランジ付き上部坩堝（厚さ３ｍｍｘ上端外径３３０ｍｍｘ下端外径３００ｍｍｘ高さ２００ｍｍの中空円錐台状坩堝）を利用して、サファイア原料充填量増加の確認を行った。 (Confirmation of effect)
An increase in the sapphire material filling amount was confirmed using the produced upper crucible with four equally spaced flanges (a hollow frustoconical crucible having a thickness of 3 mm × upper outer diameter 330 mm × lower outer diameter 300 mm × height 200 mm).

　下部坩堝はモリブデン製の厚さ５ｍｍｘ開口径３１０ｍｍｘ深さ４００ｍｍの坩堝である。従来通り下部坩堝のみでサファイア結晶を育成した場合、インゴットの大略サイズは外径３００ｍｍｘ高さ２００ｍｍ、重量約６０ｋｇである。下部坩堝内容積の５０％利用率である。 The lower crucible is a crucible made of molybdenum having a thickness of 5 mm, an opening diameter of 310 mm, and a depth of 400 mm. When a sapphire crystal is grown only with a lower crucible as usual, the approximate size of the ingot is an outer diameter of 300 mm × height of 200 mm and a weight of about 60 kg. It is 50% utilization of the lower crucible internal volume.

　下部坩堝にフランジ付き上部坩堝を載せ置きした場合の全体構成は、総高さ５５０ｍｍである。 The overall configuration when the flanged upper crucible is placed on the lower crucible is a total height of 550 mm.

　サファイア原料を上部坩堝上縁部下６５ｍｍ位置まで充填した後、融解・固化して得たインゴットの大略サイズは外径３００ｍｍｘ高さ２８０ｍｍ、重量約８４ｋｇであった。下部坩堝内容積の７０％利用率である。 After filling the sapphire raw material up to 65 mm below the upper edge of the upper crucible, the approximate size of the ingot obtained by melting and solidifying was an outer diameter of 300 mm × height of 280 mm, and a weight of about 84 kg. It is a utilization rate of 70% of the inner volume of the lower crucible.

　育成炉外へ取り出した全構成坩堝の上部坩堝は、両手で上方に持ち上げるだけで下部坩堝から分離でき、損傷も発生しなかった。また、サファイア融液が付着した痕跡もなく、繰り返し使用できる状態を保っていた。 The upper crucible of all the constituent crucibles taken out of the growth furnace could be separated from the lower crucible simply by lifting it upward with both hands, and no damage occurred. Moreover, the state which can be used repeatedly was maintained, without the trace which the sapphire melt adhered.

　今回開示された実施の形態はすべての点で例示であって制限的なものではないと考えられるべきである。本発明の範囲は上記した説明ではなくて請求の範囲によって示され、請求の範囲と均等の意味および範囲内でのすべての変更が含まれることが意図される。 The embodiment disclosed this time should be considered as illustrative in all points and not restrictive. The scope of the present invention is defined by the terms of the claims, rather than the description above, and is intended to include any modifications within the scope and meaning equivalent to the terms of the claims.

　１　坩堝、１０　下部坩堝、１１　開口、１２　下部坩堝側フランジ部、１３，２３　板材、２０　上部坩堝、２４　縮径部、２５　小径部、２６　テーパー面、２７　大径部、２８　係合部、３０　上部坩堝側フランジ部、４０　当て板、５０　リベット。 1 crucible, 10 lower crucible, 11 opening, 12 lower crucible side flange part, 13, 23 plate material, 20 upper crucible, 24 reduced diameter part, 25 small diameter part, 26 tapered surface, 27 large diameter part, 28 engaging part, 30 Upper crucible side flange, 40 batting plate, 50 rivets.

Claims (10)

　モリブデンまたはその合金製の坩堝であって、
　開口が設けられた有底円筒形状の下部坩堝と、前記開口に嵌まり合う上部坩堝とを備え、
　前記上部坩堝は、モリブデンまたはその合金製の板材を曲げて板材の両端部を接合することで形成される、坩堝。 A crucible made of molybdenum or an alloy thereof,
A bottomed cylindrical lower crucible provided with an opening, and an upper crucible that fits into the opening,
The upper crucible is formed by bending a plate made of molybdenum or an alloy thereof and joining both ends of the plate. 　前記下部坩堝は、モリブデンまたはその合金製の板材を絞り加工することで形成され、前記開口には円筒の外周方向に延在する、円周方向に連続する下部坩堝側フランジ部が設けられている、請求項１に記載の坩堝。 The lower crucible is formed by drawing a plate made of molybdenum or its alloy, and the opening is provided with a lower crucible side flange portion extending in the outer circumferential direction of the cylinder and continuing in the circumferential direction. The crucible according to claim 1. 　前記上部坩堝は、前記開口の内周側に嵌め合わせられて前記下部坩堝に係合する係合部を有し、前記上部坩堝は前記下部坩堝に対して着脱自在に設けられる、請求項１または請求項２に記載の坩堝。 The upper crucible has an engaging portion that is fitted to the inner peripheral side of the opening and engages with the lower crucible, and the upper crucible is provided detachably with respect to the lower crucible. The crucible according to claim 2. 　前記上部坩堝の下部には、円筒の半径方向に延在する上部坩堝側フランジ部が設けられている、請求項１から請求項３のいずれか１項に記載の坩堝。 The crucible according to any one of claims 1 to 3, wherein an upper crucible side flange portion extending in a radial direction of a cylinder is provided at a lower portion of the upper crucible. 　モリブデンまたはその合金製の坩堝であって、
　開口が設けられた有底円筒形状の下部坩堝と、前記開口に嵌まり合う上部坩堝とを備え、
　前記上部坩堝は、モリブデンまたはその合金製の板材が継ぎ目なく周方向に連続することで形成される、坩堝。 A crucible made of molybdenum or an alloy thereof,
A bottomed cylindrical lower crucible provided with an opening, and an upper crucible that fits into the opening,
The upper crucible is a crucible formed by continuously connecting a plate made of molybdenum or an alloy thereof in the circumferential direction. 　前記下部坩堝は、モリブデンまたはその合金製の板材を絞り加工することで形成され、前記開口には円筒の外周方向に延在する、円周方向に連続する下部坩堝側フランジ部が設けられている、請求項５に記載の坩堝。 The lower crucible is formed by drawing a plate made of molybdenum or its alloy, and the opening is provided with a lower crucible side flange portion extending in the outer circumferential direction of the cylinder and continuing in the circumferential direction. The crucible according to claim 5. 　前記上部坩堝は、前記下部坩堝に近い側の小径部と、前記下部坩堝から遠い側の大径部とを有し、前記小径部が前記下部坩堝の内側に嵌まり合う、請求項５または請求項６に記載の坩堝。 The said upper crucible has a small diameter part near the said lower crucible and a large diameter part far from the lower crucible, and the small diameter part fits inside the lower crucible. Item 7. The crucible according to Item 6. 　前記大径部と前記小径部との間には内周側に向かって下方向に傾斜するテーパー面が設けられている、請求項７に記載の坩堝。 The crucible according to claim 7, wherein a tapered surface inclined downward toward the inner peripheral side is provided between the large diameter portion and the small diameter portion. 　前記小径部の下端に内側へ延在する縮径部が設けられている、請求項７または請求項８に記載の坩堝。 The crucible according to claim 7 or 8, wherein a reduced diameter portion extending inward is provided at a lower end of the small diameter portion. 　単結晶サファイヤの製造方法であって、
　請求項１から請求項９のいずれかに記載の坩堝の前記下部坩堝および前記上部坩堝に原料を充填する工程と、
　前記原料を溶融させたのち凝固させることで前記下部坩堝内に単結晶サファイヤを生成する工程とを備えた、単結晶サファイヤの製造方法。 A method for producing single crystal sapphire,
Filling the raw material into the lower crucible and the upper crucible of the crucible according to any one of claims 1 to 9,
A step of producing a single crystal sapphire in the lower crucible by melting the raw material and then solidifying the raw material.
PCT/JP2014/078375 2013-10-30 2014-10-24 Crucible and single crystal sapphire production method using same Ceased WO2015064505A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2015544973A JPWO2015064505A1 (en) 2013-10-30 2014-10-24 crucible
CN201480059447.4A CN105683425A (en) 2013-10-30 2014-10-24 Crucible and single crystal sapphire production method using same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2013-225571 2013-10-30
JP2013225571 2013-10-30

Publications (1)

Publication Number Publication Date
WO2015064505A1 true WO2015064505A1 (en) 2015-05-07

Family

ID=53004111

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2014/078375 Ceased WO2015064505A1 (en) 2013-10-30 2014-10-24 Crucible and single crystal sapphire production method using same

Country Status (3)

Country Link
JP (3) JPWO2015064505A1 (en)
CN (1) CN105683425A (en)
WO (1) WO2015064505A1 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017214229A (en) * 2016-05-30 2017-12-07 京セラ株式会社 crucible
US10142086B2 (en) 2015-06-11 2018-11-27 At&T Intellectual Property I, L.P. Repeater and methods for use therewith
CN109537059A (en) * 2018-12-25 2019-03-29 内蒙古晶环电子材料有限公司 A kind of crucible structure for sapphire crystal growth

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111778557A (en) * 2020-06-19 2020-10-16 山东新升光电科技有限责任公司 Crucible for preparing sapphire single crystal
JP7422819B1 (en) 2022-07-25 2024-01-26 北海道電力株式会社 Reinforcing plate, tubular member reinforcement structure, and method of constructing reinforcing plate

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61123433A (en) * 1984-11-01 1986-06-11 Tohoku Metal Ind Ltd Production of metal crucible
JPH06247719A (en) * 1993-02-19 1994-09-06 Tanaka Kikinzoku Kogyo Kk Method for manufacturing crucible for melting glass
JPH06273060A (en) * 1993-03-18 1994-09-30 Asahi Chem Ind Co Ltd Refining crucible for metal disliking mixture of cr
JP2005206416A (en) * 2004-01-22 2005-08-04 Japan Science & Technology Agency Single crystal growth vessel
JP2007240037A (en) * 2006-03-07 2007-09-20 Ulvac Materials Inc Metallic crucible
JP2011042560A (en) * 2009-07-22 2011-03-03 Shinshu Univ Method and equipment for producing sapphire single crystal
JP2012254916A (en) * 2011-05-18 2012-12-27 Covalent Materials Corp Carbon fiber-reinforced carbon composite cylindrical member, method of manufacturing carbon fiber-reinforced carbon composite cylindrical member, carbon fiber-reinforced carbon composite material crucible, and method of manufacturing carbon fiber-reinforced carbon composite material crucible
CN203049098U (en) * 2013-01-18 2013-07-10 奕雪春 Volume adjusting structure of tungsten-molybdenum tube for quartz crucible
JP2013230970A (en) * 2012-04-28 2013-11-14 Luoyang Hi-Tech Metals Co Ltd Non-monolithic crucible

Family Cites Families (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4366571A (en) * 1981-03-16 1982-12-28 Corning Glass Works Electric furnace construction
JPS59103767U (en) * 1982-12-28 1984-07-12 富士通株式会社 carbon crucible
JPS6228880U (en) * 1985-08-02 1987-02-21
JP2559235B2 (en) * 1987-08-07 1996-12-04 東芝セラミックス株式会社 Quartz crucible for silicon single crystal pulling equipment
JPH0512488A (en) * 1991-03-15 1993-01-22 Omron Corp Graphic data reader
JPH07242978A (en) * 1994-03-09 1995-09-19 Tokyo Tungsten Co Ltd Alloy material for welding
JP2000290739A (en) * 1999-04-06 2000-10-17 Tanaka Kikinzoku Kogyo Kk Cr alloy crucible
JP2001048693A (en) * 1999-08-06 2001-02-20 Hitachi Chem Co Ltd Glassy carbon crucible having inner face being polygonal form
JP2002060296A (en) * 2000-08-21 2002-02-26 Crystal System:Kk Crucible for single crystal production, single crystal production apparatus and single crystal production method using the same
JP2002170780A (en) * 2000-12-01 2002-06-14 Sharp Corp Crucible and method for growing polycrystalline silicon using the same
JP2003112998A (en) * 2001-09-28 2003-04-18 Furuya Kinzoku:Kk Single crystal production crucible
JP5433300B2 (en) * 2009-05-19 2014-03-05 株式会社東芝 Molybdenum crucible and manufacturing method thereof, and manufacturing method of sapphire single crystal
JP2011105575A (en) * 2009-11-20 2011-06-02 Showa Denko Kk Single crystal pulling apparatus
JP2012236733A (en) * 2011-05-11 2012-12-06 Shinshu Univ Crucible for growing crystal, and method for growing crystal
DE112012003129B4 (en) * 2011-07-26 2018-12-20 Nikon Corporation Method for producing a connection crystal by means of a crucible
CN102304751A (en) * 2011-09-15 2012-01-04 江苏华盛天龙光电设备股份有限公司 Composite crucible for growth of sapphire crystals
US20130087094A1 (en) * 2011-10-05 2013-04-11 Siemens Medical Solutions Usa, Inc. Composite Crucible For Crystal Growth
JP5709776B2 (en) * 2012-01-30 2015-04-30 三菱重工業株式会社 Welded pipe shape measuring device
CN202530199U (en) * 2012-02-28 2012-11-14 浙江上城科技有限公司 Assembly type high-temperature resistant crucible
CN202530198U (en) * 2012-02-28 2012-11-14 浙江上城科技有限公司 Combined type high-temperature resistant crucible
CN202993825U (en) * 2012-12-13 2013-06-12 西安西工大超晶科技发展有限责任公司 Large-size wall thickness-reducing molybdenum crucible
CN203034137U (en) * 2013-01-11 2013-07-03 英利集团有限公司 Novel heat shielding assembly and novel heat shielding device thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61123433A (en) * 1984-11-01 1986-06-11 Tohoku Metal Ind Ltd Production of metal crucible
JPH06247719A (en) * 1993-02-19 1994-09-06 Tanaka Kikinzoku Kogyo Kk Method for manufacturing crucible for melting glass
JPH06273060A (en) * 1993-03-18 1994-09-30 Asahi Chem Ind Co Ltd Refining crucible for metal disliking mixture of cr
JP2005206416A (en) * 2004-01-22 2005-08-04 Japan Science & Technology Agency Single crystal growth vessel
JP2007240037A (en) * 2006-03-07 2007-09-20 Ulvac Materials Inc Metallic crucible
JP2011042560A (en) * 2009-07-22 2011-03-03 Shinshu Univ Method and equipment for producing sapphire single crystal
JP2012254916A (en) * 2011-05-18 2012-12-27 Covalent Materials Corp Carbon fiber-reinforced carbon composite cylindrical member, method of manufacturing carbon fiber-reinforced carbon composite cylindrical member, carbon fiber-reinforced carbon composite material crucible, and method of manufacturing carbon fiber-reinforced carbon composite material crucible
JP2013230970A (en) * 2012-04-28 2013-11-14 Luoyang Hi-Tech Metals Co Ltd Non-monolithic crucible
CN203049098U (en) * 2013-01-18 2013-07-10 奕雪春 Volume adjusting structure of tungsten-molybdenum tube for quartz crucible

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10142086B2 (en) 2015-06-11 2018-11-27 At&T Intellectual Property I, L.P. Repeater and methods for use therewith
JP2017214229A (en) * 2016-05-30 2017-12-07 京セラ株式会社 crucible
WO2017209144A1 (en) * 2016-05-30 2017-12-07 京セラ株式会社 Crucible
CN109537059A (en) * 2018-12-25 2019-03-29 内蒙古晶环电子材料有限公司 A kind of crucible structure for sapphire crystal growth
CN109537059B (en) * 2018-12-25 2023-11-24 内蒙古晶环电子材料有限公司 Crucible structure for sapphire crystal growth

Also Published As

Publication number Publication date
CN105683425A (en) 2016-06-15
JP2016108240A (en) 2016-06-20
JP2016108241A (en) 2016-06-20
JPWO2015064505A1 (en) 2017-03-09
JP6085046B2 (en) 2017-02-22

Similar Documents

Publication Publication Date Title
JP6085046B2 (en) crucible
US7454825B2 (en) Method of manufacturing thin-walled structures
US8061408B2 (en) Casting method for matrix drill bits and reamers
CN106011370B (en) The online replacing options of fire door flange of converter
TWI523979B (en) Non-monolithic crucible
CN110449844A (en) A kind of titanium pot manufacture craft
EP2501504B1 (en) Compensation grooves to absorb dilatation during infiltration of a matrix drill bit
CN104588647B (en) The processing method of ring type diamond composite wear-resistant belt and mould
US10989345B2 (en) Process for brazing an accessory on a tube, and corresponding assembly
US20130087094A1 (en) Composite Crucible For Crystal Growth
CN109312490A (en) crucible
CN100528411C (en) Method of manufacturing a hollow blade comprising a squealer tip and method of repairing such a blade
CN114559567B (en) Processing method of large-size quartz ring product
JP6394124B2 (en) Method for producing crucible and single crystal
CN116988140A (en) Straight arm thickening split type air guide cylinder and processing method thereof
JP6354399B2 (en) Method for producing crucible and single crystal
JP3206952U (en) Polycrystalline silicon connection
JP3206951U (en) Connection structure of polycrystalline silicon
JP6347410B2 (en) Hot forging method for disc-shaped materials
CN204276903U (en) The processing mold of ring type diamond composite wear-resistant belt
CN202482485U (en) Cutting mould for recycling single-lobe block body of graphite crucible
CN111482591B (en) A scoop for slag removal, purification and impurity removal of cast aluminum alloy solution
JP6248832B2 (en) Method for producing crucible and single crystal
RU154599U1 (en) REPLACE RING DRILL MODULE
CN119352153A (en) Seed crystal for drawing columnar polycrystalline silicon rod and processing method of seed crystal head thereof

Legal Events

Date Code Title Description
ENP Entry into the national phase

Ref document number: 2015544973

Country of ref document: JP

Kind code of ref document: A

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 14858581

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 14858581

Country of ref document: EP

Kind code of ref document: A1