JP4429702B2 - Manufacturing method of flat bottom quartz crucible - Google Patents
Manufacturing method of flat bottom quartz crucible Download PDFInfo
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- JP4429702B2 JP4429702B2 JP2003399508A JP2003399508A JP4429702B2 JP 4429702 B2 JP4429702 B2 JP 4429702B2 JP 2003399508 A JP2003399508 A JP 2003399508A JP 2003399508 A JP2003399508 A JP 2003399508A JP 4429702 B2 JP4429702 B2 JP 4429702B2
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- crucible
- mold
- quartz
- flat bottom
- flat
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 88
- 239000010453 quartz Substances 0.000 title claims description 82
- 238000004519 manufacturing process Methods 0.000 title claims description 44
- 230000002093 peripheral effect Effects 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005304 joining Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
- C03B11/06—Construction of plunger or mould
- C03B11/07—Suction moulds
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/0026—Re-forming shaped glass by gravity, e.g. sagging
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/0073—Re-forming shaped glass by blowing
- C03B23/008—Vacuum-blowing
Description
本発明は柱状晶シリコン等の製造に用いる平底石英ルツボの製造方法に関する。 The present invention relates to a method for producing a flat bottom quartz crucible used for producing columnar crystal silicon or the like.
従来、シリコンインゴットの鋳造や、一方向凝固による柱状晶シリコンの製造には、底面の平坦な石英ルツボが使用されてきた（例えば特許文献１）。この底面が平坦な石英ルツボを製造する方法として、中空の石英円筒体に石英円板を溶接する方法（例えば特許文献２）が知られている。あるいは、平底のモールドを用い、このモールド内に石英粉を装入し、回転することによってモールドの内周面に石英粉を押し付けながら加熱溶融することによって、モールド側壁に沿った側壁部を先ず形成し、次いでモールドを減圧し、底部に石英粉を吸引した状態で加熱溶融することによって平底の底部を形成する製造方法も知られている（例えば特許文献３）。 Conventionally, a quartz crucible with a flat bottom surface has been used for casting silicon ingots and producing columnar crystal silicon by unidirectional solidification (for example, Patent Document 1). As a method of manufacturing a quartz crucible having a flat bottom surface, a method of welding a quartz disk to a hollow quartz cylinder (for example, Patent Document 2) is known. Alternatively, a flat-bottom mold is used, and quartz powder is charged into the mold and rotated to heat and melt while pressing the quartz powder against the inner peripheral surface of the mold, thereby first forming a side wall portion along the mold side wall. Then, there is also known a manufacturing method in which the bottom of the flat bottom is formed by decompressing the mold and heating and melting the quartz powder while sucking the quartz powder at the bottom (for example, Patent Document 3).
しかし、前者の中空の石英円筒体に石英円板を溶接する方法は、モールドにこれらを設置する場合、底部円板をモールドに入れて位置決めした後に、その上に円筒体を突き合わせて設置しなければならず、円筒体と円板の設置が面倒であり、位置ずれを生じやすい。また、あらかじめ石英円筒体と石英円板とを個別に製造しておく必要があり、しかも円筒体の口径に一致した円板を製造しなければならず、また加熱溶融時に円筒体や円板が歪みを生じ易いため接合精度が低いなどの問題がある。 However, in the former method of welding quartz disks to a hollow quartz cylinder, when these are installed in a mold, the bottom disk must be placed in the mold and positioned, and then the cylinder should be placed against it. In addition, the installation of the cylindrical body and the disk is troublesome, and a positional shift is likely to occur. In addition, it is necessary to manufacture the quartz cylinder and the quartz disk separately in advance, and a disk corresponding to the diameter of the cylinder must be manufactured. There is a problem that the joining accuracy is low because distortion tends to occur.
一方、後者の回転モールド法による製造方法は、モールドの回転数を制御して、最初は石英粉を遠心力によってモールド側壁に沿って上昇させ、加熱溶融して側壁部を形成し、その後は減圧に切り替えて石英粉を底部に吸引しながら加熱溶融すると云う微妙な操作を行わなければならず、回転数や減圧状態が僅かに外れると成形体が崩れると云う問題があり、また製造状態が途中で切り替わるので肉厚の均一なルツボを製造するのが難しいと云う問題がある。
本発明は、従来の製造方法における上記問題を解決したものであり、丸底石英ルツボを利用して平底ルツボを製造することによって、肉厚が均一で成形精度に優れた平底ルツボを容易に製造することができる製造方法を提供する。 The present invention solves the above-mentioned problems in the conventional manufacturing method. By manufacturing a flat bottom crucible using a round bottom quartz crucible, a flat bottom crucible with uniform thickness and excellent molding accuracy can be easily manufactured. Provided is a manufacturing method that can.
本発明によれば以下示す平底石英ルツボの製造方法が提供される。
（１）丸底石英ガラスルツボを、底部に減圧吸引手段を有する回転平底モールドに挿入し、加熱して軟化させると共に、回転しているモールド底部を減圧吸引してルツボ底部を平底モールドの底部に密着させることによって、ルツボ底部を丸底から平底にすることを特徴とする平底石英ルツボの製造方法。
（２）丸底モールドに石英粉を装入し、該モールドを回転して石英粉をモールド内周面全体に張り付けた状態で加熱溶融することによって丸底石英ルツボを製造し、次いで、底部に減圧吸引手段を有する回転平底モールドを用い、上記丸底石英ルツボを平底モールドに装入し加熱して軟化させる共に、回転しているモールド底部を減圧吸引してルツボ底部を平底モールドの底部に密着させることによって、ルツボ底部を丸底から平底にする上記(1)の平底石英ルツボの製造方法。
（３）周壁および底部が角型であって底部と共に周壁に減圧吸引手段を有する平底モールドを用い、円筒丸底の石英ルツボを該平底モールドに装入し、加熱して軟化させる共に、モールドの周壁および底部を減圧吸引してルツボの周壁および底部を平底モールドに密着させることによって、ルツボの形状を円筒丸底から角型平底にする上記(1)または(2)に記載する平底石英ルツボの製造方法。
（４）コーナ部の曲率が９０〜２００mmの丸底石英ルツボを該曲率が２０〜６０mmの平底石英ルツボに成形する上記(1)、(2)または(3)に記載する製造方法。
（５）石英粉の加熱手段としてアーク加熱を行う上記(1)〜(4)の何れかに記載する製造方法。
（６）上記(1)〜(5)の何れかの方法によって製造された平底石英ルツボ。
According to the present invention, the following method for producing a flat bottom quartz crucible is provided.
(1) A round bottom quartz glass crucible is inserted into a rotating flat bottom mold having a vacuum suction means at the bottom, heated and softened, and the rotating mold bottom is vacuum suctioned so that the crucible bottom becomes the bottom of the flat bottom mold. A method for producing a flat-bottomed quartz crucible, characterized in that the bottom of the crucible is changed from a round bottom to a flat bottom by bringing them into close contact.
(2) Quartz powder is charged into a round bottom mold, and the mold is rotated to heat and melt the quartz powder stuck to the entire inner peripheral surface of the mold to produce a round bottom quartz crucible. Using a rotating flat bottom mold with vacuum suction means, the above round bottom quartz crucible is placed in the flat bottom mold and heated to soften it, and the rotating mold bottom is sucked under reduced pressure to bring the crucible bottom into close contact with the bottom of the flat bottom mold. The method for producing a flat-bottomed quartz crucible according to the above (1), wherein the crucible bottom is changed from a round bottom to a flat bottom.
(3) A flat bottom mold having a square wall and a bottom portion and a vacuum suction means on the peripheral wall together with the bottom portion is inserted into a cylindrical round bottom quartz crucible and heated to soften the mold. The flat walled quartz crucible described in (1) or (2) above, wherein the shape of the crucible is changed from a cylindrical round bottom to a square flat bottom by sucking the peripheral wall and the bottom under reduced pressure to bring the crucible into close contact with the flat bottom mold. Production method.
(4) The manufacturing method according to the above (1), (2) or (3), wherein a round bottom quartz crucible having a corner portion curvature of 90 to 200 mm is formed into a flat bottom quartz crucible having a curvature of 20 to 60 mm.
(5) The manufacturing method according to any one of (1) to (4), wherein arc heating is performed as a heating means for the quartz powder.
(6) A flat bottom quartz crucible manufactured by any one of the above methods (1) to (5).
〔発明の具体的な説明〕
本発明の製造方法は、丸底石英ガラスルツボを、底部に減圧吸引手段を有する回転平底モールドに挿入し、加熱して軟化させると共に、回転しているモールド底部を減圧吸引してルツボ底部を平底モールドの底部に密着させることによって、ルツボ底部を丸底から平底にすることを特徴とする平底石英ルツボの製造方法である。
[Detailed Description of the Invention]
In the production method of the present invention, a round bottom quartz glass crucible is inserted into a rotating flat bottom mold having a vacuum suction means at the bottom and heated and softened, and the rotating mold bottom is sucked under reduced pressure to flatten the crucible bottom. A method for producing a flat-bottomed quartz crucible, wherein the bottom of the crucible is changed from a round bottom to a flat bottom by closely contacting the bottom of the mold.
平底モールドに挿入する丸底石英ルツボの製造方法は限定されない。なお、丸底石英ルツボは例えば回転モールド法によって製造することができる。本発明の製造方法は、最初に回転モールド法によって丸底石英ルツボを製造し、次いでこの丸底石英ルツボを平底石英ルツボに成形する方法を含む。すなわち、本発明は、丸底モールドに石英粉を装入し、該モールドを回転して石英粉をモールド内周面全体に張り付けた状態で加熱溶融することによって丸底石英ルツボを製造し、次いで、底部に減圧吸引手段を有する回転平底モールドを用い、上記丸底石英ルツボを平底モールドに装入し加熱して軟化させる共に、回転しているモールド底部を減圧吸引してルツボ底部を平底モールドの底部に密着させることによって、ルツボ底部を丸底から平底にする平底石英ルツボの製造方法を含む。 The manufacturing method of the round bottom quartz crucible inserted into the flat bottom mold is not limited. The round bottom quartz crucible can be manufactured by, for example, a rotational mold method. The production method of the present invention includes a method in which a round bottom quartz crucible is first produced by a rotary mold method, and then this round bottom quartz crucible is formed into a flat bottom quartz crucible. That is, the present invention produces a round-bottom quartz crucible by charging the round-bottom mold with quartz powder and rotating the mold to heat and melt the quartz powder attached to the entire inner peripheral surface of the mold. Using a rotating flat bottom mold having a vacuum suction means at the bottom, the round bottom quartz crucible is charged into a flat bottom mold and heated and softened, and the rotating mold bottom is vacuumed to remove the crucible bottom from the flat bottom mold. It includes a method for producing a flat bottom quartz crucible that makes the crucible bottom from a round bottom to a flat bottom by closely contacting the bottom.
回転モールド法によって丸底石英ルツボを製造し、次いでこの丸底石英ルツボを平底石英ルツボに成形する方法について、その概略を図１に示す。図示するように、上記製造方法は丸底ルツボを製造する工程と、製造した丸底ルツボを平底ルツボに加工する工程とを有する。丸底ルツボの製造工程は一般的な回転モールド法による製造工程であり、底部が丸く凹んだ円形凹部を有する丸底モールド１１を用いる。この丸底モールド１１は減圧吸引手段を有するものが好ましい。丸底モールド１１に石英粉１２を入れてモールド１１を回転しながら加熱溶融する。石英粉１２は遠心力によってモールド内周面に堆積した状態になり、内周面に沿った石英粉層が形成され、この石英粉層が溶融して石英ガラス層になる。加熱手段１３はアーク加熱が好ましい。アーク棒をモールド１１の内側に挿入し、石英の融点以上に加熱して石英粉層を溶融してガラス化する。 FIG. 1 shows an outline of a method for producing a round bottom quartz crucible by a rotary mold method and then forming the round bottom quartz crucible into a flat bottom quartz crucible. As shown in the drawing, the manufacturing method includes a step of manufacturing a round bottom crucible and a step of processing the manufactured round bottom crucible into a flat bottom crucible. The manufacturing process of the round bottom crucible is a manufacturing process by a general rotary mold method, and a round bottom mold 11 having a circular concave portion with a round bottom is used. The round bottom mold 11 preferably has a vacuum suction means. Quartz powder 12 is put in the round bottom mold 11 and the mold 11 is heated and melted while rotating. The quartz powder 12 is deposited on the inner peripheral surface of the mold by centrifugal force, a quartz powder layer is formed along the inner peripheral surface, and the quartz powder layer melts to become a quartz glass layer. The heating means 13 is preferably arc heating. An arc bar is inserted inside the mold 11 and heated above the melting point of quartz to melt the quartz powder layer and vitrify it.
このアーク加熱と共にモールド内部に設けた通気孔１４を通じてモールド内周面を減圧する。通気孔１４はモールド内周面に開口しており、吸引することによって、表面がガラス化した石英粉層の内部が減圧され、石英粉層内部の気泡が通気孔１４を通じて外部に吸引除去される。この減圧吸引によって内表面部分が透明な石英ガラス層が形成される。 Along with this arc heating, the inner peripheral surface of the mold is decompressed through the vent hole 14 provided in the mold. The air holes 14 are opened on the inner peripheral surface of the mold, and by sucking, the inside of the quartz powder layer whose surface is vitrified is reduced in pressure, and bubbles inside the quartz powder layer are sucked and removed to the outside through the air holes 14. . By this vacuum suction, a quartz glass layer having a transparent inner surface portion is formed.
上記丸底モールドを用いた回転モールド法では、石英粉層が丸底モールドの内周面から底面まで、すなわち内表面全体に一体に形成されているので、一回の加熱によって丸い底部を有する石英ルツボが形成される。冷却後、製造した丸底ルツボ１５をモールド１１から取り出す。 In the rotary mold method using the round bottom mold, the quartz powder layer is integrally formed from the inner peripheral surface to the bottom surface of the round bottom mold, that is, the entire inner surface. A crucible is formed. After cooling, the manufactured round bottom crucible 15 is taken out from the mold 11.
次いで、底部に減圧吸引手段を有する回転平底モールド１６を用い、丸底ルツボ１５を回転平底モールド１６に装入し、石英の軟化点をやや上回る温度に加熱して丸底ルツボ１５を軟化させる。加熱手段１３は先の場合と同様にアーク加熱が好ましい。平底ルツボ１６の底部に設けた減圧吸引手段としては、例えば、平底モールドの底部の材質として嵩比重１.４〜１.８g/cm3のカーボンまたはカーボン繊維の網目構造を有する部材を用いることによって通気性を有する底部とし、この底部に減圧吸引手段を接続した構造にしたものなどを用いると良い。 Next, using a rotary flat bottom mold 16 having a vacuum suction means at the bottom, the round bottom crucible 15 is inserted into the rotary flat bottom mold 16 and heated to a temperature slightly above the softening point of quartz to soften the round bottom crucible 15. The heating means 13 is preferably arc heating as in the previous case. As the vacuum suction means provided at the bottom of the flat bottom crucible 16, for example, a member having a carbon or carbon fiber network structure with a bulk specific gravity of 1.4 to 1.8 g / cm 3 is used as the material of the bottom of the flat bottom mold. A bottom portion having air permeability and a structure in which a vacuum suction means is connected to the bottom portion may be used.
丸底ルツボ１５の加熱軟化と共に通気孔１７を通じてモールド底部を減圧吸引し、ルツボ底部を平底モールド１６の底部に密着させることによって丸底ルツボ１５の底部を丸底から平底に加工する。減圧吸引操作は吸引圧が定圧化した段階で終了すればよい。以上の工程によって平底ルツボ１８が製造される。冷却後、製造した平底ルツボ１５をモールド１６から取り出す。 The bottom of the round bottom crucible 15 is processed from the round bottom to the flat bottom by sucking the bottom of the mold through the vent hole 17 and softening the round bottom crucible 15 under reduced pressure and bringing the bottom of the crucible into close contact with the bottom of the flat bottom mold 16. The vacuum suction operation may be completed when the suction pressure is constant. The flat bottom crucible 18 is manufactured by the above process. After cooling, the produced flat bottom crucible 15 is removed from the mold 16.
上記製造方法によれば、コーナ部の曲率が９０〜２００mmの丸底石英ルツボを、例えばコーナ部の曲率が２０〜６０mmの平底石英ルツボに成形することができる。 According to the above manufacturing method, a round bottom quartz crucible with a corner portion having a curvature of 90 to 200 mm can be formed into a flat bottom quartz crucible with a corner portion having a curvature of 20 to 60 mm, for example.
本発明の上記製造方法においては、あらかじめ製造した丸底石英ルツボを、底部に減圧吸引手段を有する平底モールドに装入し、加熱して軟化させる共に、モールド底部を減圧吸引してルツボ底部を平底モールドの底部に密着させることによって丸底から平底に加工しても良い。あらかじめ製造した丸底石英ルツボを用いることによって、例えば、使用済み丸底ルツボを平底ルツボに加工し直すことができる。 In the production method of the present invention, a round-bottomed quartz crucible manufactured in advance is placed in a flat bottom mold having a vacuum suction means at the bottom and heated and softened, and the bottom of the crucible is vacuum suctioned to flatten the bottom of the crucible. You may process from a round bottom to a flat bottom by making it contact | adhere to the bottom part of a mold. By using a round bottom quartz crucible manufactured in advance, for example, a used round bottom crucible can be processed again into a flat bottom crucible.
さらに、本発明の上記製造方法は角型平底ルツボの製造に適用することができる。すなわち、周壁および底部が角型であって底部と共に周壁に減圧吸引手段を有する平底モールドを用い、円筒丸底の石英ルツボを該平底モールドに装入し、加熱して軟化させる共に、モールドの周壁および底部を減圧吸引してルツボの周壁および底部を平底モールドに密着させて、ルツボの形状を円筒丸底から角型平底に加工することによって角型平底ルツボを製造することができる。 Furthermore, the production method of the present invention can be applied to the production of a square flat bottom crucible. That is, a flat bottom mold having a square peripheral wall and a bottom part and having a vacuum suction means on the peripheral wall together with the bottom part, a quartz crucible having a cylindrical round bottom is inserted into the flat bottom mold, heated and softened, and the peripheral wall of the mold A square flat bottom crucible can be manufactured by suctioning the bottom part under reduced pressure to bring the peripheral wall and bottom part of the crucible into close contact with the flat bottom mold and processing the shape of the crucible from a cylindrical round bottom to a square flat bottom.
図１の製造工程において、平底モールド１６として、周壁および底部が角型であって底部と共に周壁に減圧吸引手段を有するものを用い、この平底モールド１６に丸底ルツボ１５を設置し、石英の軟化点をやや上回る温度に加熱し、丸底ルツボ１５を軟化させる。この加熱軟化と共に角型のモールド周壁および底部の通気孔１７を通じて吸引減圧し、ルツボの周壁および底部を平底モールドの角型周壁および平底に密着させて、ルツボの形状を円筒丸底から角型平底に加工する。 In the manufacturing process of FIG. 1, a flat bottom mold 16 having a square peripheral wall and bottom and having a vacuum suction means on the peripheral wall together with the bottom is provided with a round bottom crucible 15 installed on the flat bottom mold 16 to soften the quartz. Heat to a temperature slightly above the point to soften the round bottom crucible 15. With this heat softening, the pressure is reduced by suction through the square mold peripheral wall and the bottom vent hole 17, the peripheral wall and bottom of the crucible are brought into close contact with the square peripheral wall and the flat bottom of the flat bottom mold, and the shape of the crucible is changed from the cylindrical round bottom to the square flat bottom. To process.
本発明の製造方法によれば、均一な肉厚を得やすい丸底石英ルツボを用い、しかも平底化工程ではアーク加熱温度を石英ガラスの軟化温度をやや上回る程度にすればよいので、遠心力によるコーナー部へのガラスの移動が抑制され、肉厚が均一な平底ルツボを得ることができる。また、本発明の製造方法はルツボの側壁部と底部とを接合する方法ではないので、位置合わせや接合を行う必要がなく、製造工程が簡略であり、容易に高品質の平底石英ルツボを安定に製造することができる。 According to the production method of the present invention, a round bottom quartz crucible that is easy to obtain a uniform thickness is used, and in the flat bottoming process, the arc heating temperature may be set slightly higher than the softening temperature of quartz glass. The movement of the glass to the corner portion is suppressed, and a flat bottom crucible having a uniform thickness can be obtained. In addition, since the manufacturing method of the present invention is not a method of joining the side wall portion and the bottom portion of the crucible, there is no need for alignment and joining, the manufacturing process is simple, and a high-quality flat-bottomed quartz crucible can be easily stabilized. Can be manufactured.
さらに、アーク加熱を行えば、酸水素バーナーを用いた場合のＯＨ基濃度の増加や高温使用時の変形を生じることがなく、また、酸水素バーナー使用時のアニール等の後処理工程を行う必要が無く、生産効率が向上する。 Furthermore, if arc heating is performed, there will be no increase in OH group concentration or deformation during high temperature use when an oxyhydrogen burner is used, and post-treatment steps such as annealing when using an oxyhydrogen burner are required. Production efficiency is improved.
本発明を実施例および比較例によって具体的に示す。
丸底石英ルツボ（口径18inch、平均肉厚９mm）を用い、これのルツボを、周壁および底部が角型であって底部と共に周壁に減圧吸引手段を有する平底モールド（底部460mm角、高さ200mm）に設置し、表１に示す製造条件下で平底石英ルツボを製造した。この結果を表１に示した。
The present invention is specifically illustrated by examples and comparative examples.
A round bottom quartz crucible (caliber: 18 inch, average wall thickness: 9 mm). This crucible is a flat bottom mold (bottom 460 mm square, height 200 mm) with a peripheral wall and bottom having a square shape and a vacuum suction means on the peripheral wall along with the bottom. The flat bottom quartz crucible was manufactured under the manufacturing conditions shown in Table 1. The results are shown in Table 1.
表１に示すように、本発明の方法によって製造した平底石英ルツボ（No.１〜No.５）は何れもコーナ部の曲率が小さく、また側壁部の軟化やコーナ部の亀裂などが発生せず、高品質の平底石英ルツボが得られる。一方、本発明の好適な製造条件から外れる比較例（No.６〜No.９）のルツボはコーナ部の曲率が大きく、従って平底化が不十分であり、また比較例の一部は側壁部が軟化し、あるいはコーナ部に亀裂が生じている。 As shown in Table 1, all of the flat bottom quartz crucibles (No. 1 to No. 5) manufactured by the method of the present invention have a small curvature at the corners, and softening of the side walls and cracks at the corners. Therefore, a high-quality flat bottom quartz crucible can be obtained. On the other hand, the crucibles of the comparative examples (No. 6 to No. 9) that deviate from the preferred production conditions of the present invention have a large curvature at the corners, and therefore are insufficiently flattened, and some of the comparative examples are side wall parts. Has softened or cracks have occurred in the corners.
１１−丸底モールド、１２−石英粉(層)、１３−アーク加熱手段、１４−通気孔、１５−丸底石英ルツボ、１６−平底モールド、１７−通気孔、１８−平底石英ルツボ。 11-round bottom mold, 12-quartz powder (layer), 13-arc heating means, 14-vent hole, 15-round bottom quartz crucible, 16-flat bottom mold, 17-vent hole, 18-flat bottom quartz crucible.
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