WO2003106742A1 - Seed crystal holding jig and process for producing single crystal - Google Patents
Seed crystal holding jig and process for producing single crystal Download PDFInfo
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- WO2003106742A1 WO2003106742A1 PCT/JP2003/007319 JP0307319W WO03106742A1 WO 2003106742 A1 WO2003106742 A1 WO 2003106742A1 JP 0307319 W JP0307319 W JP 0307319W WO 03106742 A1 WO03106742 A1 WO 03106742A1
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- seed crystal
- holding jig
- holding
- crystal
- jig
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Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/32—Seed holders, e.g. chucks
Definitions
- the present invention relates to a jig for holding a seed crystal used for pulling a silicon single crystal or a compound semiconductor single crystal or the like by a Chiral Clarke method (CZ method), and a method for manufacturing a single crystal.
- CZ method Chiral Clarke method
- a silicon seed crystal is immersed in a molten material obtained by melting polycrystalline silicon, and then the silicon seed crystal is pulled up while being rotated to convert the silicon single crystal.
- CZ method Chiyolarski method
- FIG. 7 shows an example of a single crystal pulling apparatus used for the CZ method.
- the single crystal pulling apparatus 20 includes a crucible 3 for accommodating a silicon melt 2 in a chamber 10, a crucible support shaft 4 for rotating the crucible 3, and a rotating mechanism (not shown); It comprises a seed crystal holding jig 6 for holding the seed crystal 5, a wire 7 for lifting the seed crystal holding jig 6, and a winding mechanism (not shown) for rotating or winding the wire 7.
- a heater 8 is arranged around the crucible 3, and a heat insulating material 9 is arranged around the heater 8 to pull up the single crystal.
- a silicon polycrystal is heated in a crucible 3 to a temperature higher than the melting point and melted, and a wire 7 is unwound to melt.
- the tip of seed crystal 5 is contacted or immersed in the center of 2.
- the crucible 3 is rotated in an appropriate direction, the wire 7 is wound while being rotated, and the seed crystal 5 is pulled up to start growing a single crystal. After that, by appropriately controlling the pulling rate and temperature, the growth of almost cylindrical growth Crystal 1 can be obtained.
- FIG. 1 There is a lock type holding jig.
- a reverse-tapered fitting 24 is inserted from the side of the main body of the holding jig 6 a into the tapered holding surface 18 of the seed crystal 5, and A ring-shaped outer cover 26 is put on the main body so as to prevent the insertion fitting 24 from falling out.
- the holding surface 18 of the seed crystal 5 is pressed against the end surface 15 of the fitting 24 so that the seed crystal 5 is held.
- FIG. 9 shows another holding jig 6b of the key lock type. ⁇ ⁇ Insert the key 25 into the fitting 24 and lock it so that the end face 15 of the insertion fitting 24 is formed. Is pressed against the holding surface 18 of the seed crystal 5 to hold the seed crystal 5.
- the holding jig 6 c is for locking the seed crystal by inserting a cylindrical pin 27 into a circular hole provided between the jig body and the seed crystal 5.
- the point between pin 27 and the seed crystal 5 is smaller than that of the key lock type, which holds the seed crystal by pressing the tapered surface into contact. Since the seed crystal 5 is liable to be damaged due to contact, and high processing accuracy is required, a tapered key-mouth type holding jig is preferably used.
- the weight of a conventional silicon single crystal having a diameter of less than 200 mm was at most about 120 kg , but in recent years it has become mainstream.
- Such large silicon single crystals can exceed 170 kg.
- the load applied to the holding jig becomes extremely large.
- isotropic sintered carbon has been generally used as a material for a seed crystal holding jig.
- a holding jig of such a material does not cause metal contamination of single crystal and can withstand a load of about 160 kgf, so that the diameter is less than 20 Omm. It can be used to grow single crystals. However, it is difficult to obtain a load bearing capacity of more than 170 kgf, which is required for growing silicon single crystals with a diameter of 300 mm.
- Japanese Patent Application Laid-Open No. 11-197882 discloses a heat-resistant cushion such as a carbon fiber or metal fiber flute between a seed crystal and a contact surface of a seed crystal holding jig.
- a holding jig and a seed crystal holding jig that prevent breakage of a seed crystal by one point concentration of load stress by interposing a material are disclosed.
- this holding jig is not strong enough to pull a heavy single crystal of 170 kg or more, and when the cushion material is pressed, the fine powder is removed from the cushion material. May be scattered and mixed into the molten raw material, thereby lowering the purity of the single crystal.
- Japanese Patent Application Laid-Open No. 9-123541 discloses that at least two surfaces of a seed crystal having a rectangular cross section are pressed against a seed crystal of a holding jig toward an inner surface of an insertion hole.
- a crystal holding jig is disclosed. By using this holding jig, the seed crystal can be accurately positioned and held without tilting, and the holding force is increased.
- the strength is not sufficient to pull a heavier single crystal in the future, and the seed crystal or the holding jig may be broken during the pulling.
- the present invention can safely and reliably pull a high-purity single crystal without breaking the seed crystal or holding jig even when growing a high-weight single crystal of 170 kg or more. It is intended to provide a seed crystal holding jig and a method for producing a single crystal.
- an end face of a reverse fitting with a reverse taper is attached to a holding surface of a tapered seed crystal.
- a holding jig for holding the seed crystal by pressing comprising two or more of the above-mentioned fittings, wherein these inserting fittings are at the same height as the main body of the holding jig and around the center axis.
- a seed crystal holding jig characterized by being provided at equal intervals is provided.
- the fitting preferably has a tensile strength of 200 kgf / cm 2 or more and an elastic modulus of 200 O kgf Zm ni 2 or less, and is made of carbon fiber reinforced carbon. It is preferably made of a composite material or isotropic sintered carbon.
- the seed crystal may break when subjected to a high load by pressing against it, but the tensile modulus is more than 200 kgf / cm2 and the elastic modulus is 200 if kgf / rn m 2 following ⁇ tool, Ru can and child to prevent this Yo I Do Yabu ⁇ effectively.
- the material of the insert is carbon fiber reinforced carbon composite material or isotropic sintered carbon, the strength of the insert is sufficient, and since the insert has flexibility, it can be broken. In addition, seed crystal destruction can be effectively prevented, and metal contamination of the grown single crystal can be prevented.
- the holding jig body preferably has a tensile strength of at least 20 O kgf Z cm 2 and an elastic modulus of at least 800 kgf / mm 2 , and particularly, the material is carbon fiber.
- it is a reinforced carbon composite, reinforced isotropic sintered carbon, molybdenum or at least one of them. If the holding jig body has a tensile strength of 200 kgf / cm 2 or more and an elastic modulus of 800 kgf Z mm 2 or more, the strength of the holding jig body can be sufficiently increased.
- materials such as carbon fiber reinforced carbon composite material, reinforced isotropic sintered carbon, and molybdenum have extremely high heat resistance, so that sufficient strength can be maintained even in a high-temperature chamber. .
- the seed crystal is held by pressing the end face of a fitting having a reverse taper of the seed crystal holding jig against the tapered holding surface of the seed crystal by holding the seed crystal.
- a method for producing a single crystal by the Kralski method as a seed crystal, two or more tapered holding surfaces are provided at the same height and at equal intervals around a central axis.
- the seed crystal is held using a holding jig provided with an insertion fitting for pressing all the holding surfaces of the seed crystal as the seed crystal holding jig.
- a method for producing a single crystal characterized by pulling up the single crystal is provided.
- the load of the grown single crystal can be evenly dispersed, so that even a heavy single crystal can be reliably pulled up and manufactured with a diameter of 30%.
- the productivity of a single crystal having a large diameter of 0 mm or more can be improved, and the material of the holding jig can be prevented from being scattered and the single crystal can be prevented from being contaminated.
- the holding jig of the present invention since two or more fittings are provided at the same height of the main body of the holding jig and at equal intervals around the central axis, the holding jig is used for seeding.
- the load that increases as the crystals grow can be evenly dispersed, and the load bearing capacity of the seed crystal and the seed crystal holding jig can be greatly improved.
- even large silicon single crystals with a diameter of, for example, 30 O mm or more and a mass of 170 kg or more can be safely pulled up with high purity, improving the yield of single crystal production. Cost reductions can also be achieved.
- FIG. 1 is a schematic sectional view showing an example of a seed crystal holding jig of the present invention. (a) Longitudinal section
- Figure 2 is a schematic diagram of the seed crystal that is retained.
- FIG. 3 is a view showing another example of a seed crystal holding jig according to the present invention and a seed crystal held.
- FIG. 4 is a schematic sectional view of still another example of the main body of the seed crystal holding jig according to the present invention.
- FIG. 5 is a diagram showing a test seed crystal used in the tensile test.
- Figure 6 is a diagram illustrating the outline of the tensile test.
- FIG. 7 shows an example of a single crystal pulling apparatus using the Chiyo-Kralski method.
- FIG. 8 is a schematic diagram showing an example of a conventional key-lock type seed crystal holding jig.
- FIG. 9 is a schematic diagram showing another example of a conventional keylock type seed crystal holding jig.
- FIG. 10 is a schematic diagram showing an example of a pin-lock type seed crystal holding jig. BEST MODE FOR CARRYING OUT THE INVENTION
- FIG. 1 shows an example of a seed crystal holding jig of the present invention
- FIG. 2 shows a seed crystal to be held
- Seed crystal 5 is a quadrangular prism
- two tapered holding surfaces 18 are provided at the same height and opposed around central axis 19 ′.
- the holding jig 11 is formed at the same height as the main body 12 and with two through holes 13 for inserting the insertion fitting 14 around the center axis 19 facing each other.
- a fitting 14 having a taper opposite to the taper of the holding surface 18 of the seed crystal 5 is inserted so as to face the through hole 13.
- the end surface 15 of such a fitting 14 and the holding surface 18 of the seed crystal 5 are provided at corresponding positions, and furthermore, the angle of the taper of the holding surface 18, The angle of the taper at the end of the tool 14 is formed at the same angle. Then, the jig body 12 is covered with a ring-shaped mantle 16 so as to prevent the fitting tool 14 from coming off, so that the jig body 12 is locked. Are pressed equally to hold the seed crystal 5.
- FIG. 3 shows a cross section of another main body of the seed crystal holding jig according to the present invention and a seed crystal held by the main body.
- a cylindrical seed crystal insertion hole 17 is formed at the center of the holding jig main body 12 shown in FIG. 3 (a). Also, three through holes 13 are formed at the same height of the jig body 12 and around the center axis 19 at equal intervals, and these through holes 13 are respectively formed. The insertion fitting can be inserted.
- the retained seed crystal 5 ' has a columnar shape as a whole, and has three tapers with the same angle as the taper of the end face of the fitting.
- the holding surface 18 is provided at the same height and opposed around the center axis 19.
- the seed crystal 5 ′ is held by pressing all three holding surfaces 18 with ⁇ fittings.
- FIG. 4 shows a cross section of the holding jig main body 12 having four insertion fittings.
- the four through holes 13 are at the same height as the holding jig main body 12, and the center axis is It is provided at equal intervals around 19.
- the material of the holding jig of the present invention it is necessary to use a material having a compressive strength and a tensile strength sufficiently strong to safely pull up a heavy crystal having a high weight.
- a hard material such as molybdenum, stainless steel, or an alloy thereof with an elastic modulus of more than 1000 kg Zinm 2
- a seed crystal consisting of a single crystal, which is a brittle material, is pressed. At times, the seed crystal may be damaged to lower the load-bearing capacity, or the seed crystal may be broken. Therefore, the insert has a tensile strength of S200 to 700 kgf / to prevent the breakage of the insert itself and to prevent damage and destruction of the seed crystal and the jig body.
- cm 2 and a conductivity coefficient of 500 to 200 kgf Zmm 2 is preferable.
- the insert itself may be broken, so it includes the commonly used CIP (Cold Isostatic Pressing) material (CIP — A) also because the material, 2 0 O kgf / cm 2 or more is preferred rather, good Ri favored properly the CIP material molded high strength - those materials containing (CIP B), 3 0 0 kgf Z cm 2 or more It is.
- CIP Cold Isostatic Pressing
- the tensile strength of the material of the insert exceeds 700 kgf / cm 2 , the seed crystal or the jig body may be damaged or broken.
- the elastic modulus of the inserted instrument is less than 5 0 0 k g f / mm 2, carry the risk that the strength reduction due to deformation easily stress concentration occurs, whereas, the 2 0 0 0 kgi / mm 2 If it exceeds, the seed crystal and the jig body may be damaged or destroyed.
- a carbon fiber reinforced carbon composite material (C / C material) or isotropic sintered carbon can be used. Made of these materials. With a fitting, the seed crystal is not broken, and the end face is appropriately crushed when the seed crystal is pressed, so that surface contact can be obtained. Even if the fine powder is mixed into the raw material melt, it is simply There is no metal contamination of the crystal. However, for example, when an isotropic sintered carbon material having a tensile strength of less than 200 kgf no c in 2 is used, the strength becomes insufficient and there is a risk of compressive fracture.
- the insert is made of an isotropic sintered carbon material having a tensile strength of at least 0 kgf / cm 2, more preferably at least 30 O kgi Z cm 2 (the range of general carbon materials)
- both the insert and the seed crystal are less likely to be crushed, which is preferable.
- the body of the holding jig can be molybdenum, carbon fiber reinforced carbon composite, reinforced isotropic sintered carbon, or at least one of them.
- the holding jig body is made of a metal with a high melting point such as molybdenum, the strength of the jig body will be extremely high, and the strength will be sufficiently high even in a chamber that becomes hot during pulling of a single crystal. Can be maintained.
- the fine metal powder may be mixed into the raw material melt during the growth of the single crystal and cause metal contamination.Therefore, cover the metal surface of the body with a carbon material. To prevent metal contamination.
- the holding jig body, tensile strength force S 2 0 0 ⁇ 2 0 0 0 0 kgf / cm 2 der is, the elastic coefficient is the well 8 0 0 ⁇ 3 0 0 0 0 kgf / mm 2 for this Is preferred. If the tensile strength of the holding jig body is less than 200 kg ⁇ / cm 2 , the jig body will be easily ruptured, while if it exceeds 2000 kgf / cm 2 , the seed crystal will be damaged. Or there is a risk of being destroyed.
- the above-mentioned isotropic sintered carbon can be used as a material of each member other than the insertion fitting, and all the members of the holding jig may be made of isotropic sintered carbon.
- the holding jig body is made of isotropic sintered carbon
- the cross-sectional area of that part may decrease and the strength may be insufficient.
- two ⁇ fittings 14 as shown in Fig. 1 are opposed to each other. It is preferable to adopt a structure in which they are arranged in a position.
- a seed crystal 5 as shown in FIG. 2 having a tapered holding surface 18 corresponding to the end surface 15 of the insertion fitting 14 is prepared.
- the seed crystal 5 is inserted into the seed crystal insertion hole 13 of the jig 11, and the insertion fitting 14 is inserted into each through hole 13 of the holding jig body 12, and Put a ring-shaped jacket 16 on the body 12 and lock it so that 14 does not come off.
- the end face of the fitting 14 can hold the seed crystal 5 by pressing the holding surface 18 of the seed crystal 5 against the holding face 18.
- the tip of the seed crystal 5 held by the holding jig 11 of the present invention is immersed in the molten silicon material accommodated in the rutupo of the single crystal pulling apparatus as shown in FIG.
- the seed crystal holding jig 11 is rotated, and the single crystal 1 is grown following the seed crystal 5 by pulling the jig directly upward by an upper pulling means (wire winding mechanism).
- an upper pulling means wire winding mechanism
- the load applied to the seed crystal 5 can be evenly distributed to each of the inserts 14, and the dispersed load is applied to the center of the holding jig 11. Since it is distributed evenly as viewed from the shaft 19, there is no uneven load. Therefore, in the holding jig 11 of the present invention, the load-bearing strength of the holding jig main body is improved as compared with the conventional holding jig having one insertion fitting.
- the seed crystals are arranged at equal angular intervals around the central axis. Since it is held in a suspended state by a plurality of fittings, it is pressed against the inner wall surface of the center hole of the holding jig, or rubs against the inner wall surface and scratches the seed crystal surface. There is no such thing. Therefore, when the holding jig of the present invention is used, the load bearing strength of the seed crystal itself is also improved.
- a high crystal having a diameter of 30 O mm or more and a weight of 170 kg or more, particularly more than 250 kg. Even heavy silicon single crystals can be pulled up reliably without breaking the holding jig and seed crystal.
- a tensile test was conducted to measure the strength of the seed crystal and the seed crystal holding jig.
- both ends of the test seed crystal 5a (5b) are held by holding jigs 12a and 12b, respectively, and one holding jig 12b is fixed to the fixed end, and the other end is fixed to the other end.
- the holding jig 12a was fixed to a shaft to which a tensile load could be applied via a flexible joint.
- Pull A load cell is provided at the end of the shaft to which a load can be applied, so that the tensile load when the seed crystal or the seed crystal holding jig is broken can be measured.
- the holding jig 12a was pulled at a constant speed of 0.1 mm / min, and the seed crystal 5a (5b) or the seed crystal holding jigs 12a and 12b were pulled until they were broken.
- the load at the time of failure was measured continuously.
- Table 1 shows the holding jigs used for the test and the measurement results. Table 1>
- CIP A Bow I Tensile strength 250kgf / cm 2 , Modulus of elasticity 1000kgf / mm 2
- CIP B Bow I Tensile strength 700 kgf / cm 2 , Modulus of elasticity 1300 kgf / mm 2
- Moripden pure moripden Tensile strength 7000 18200 kgf / cm 2 , Modulus of elasticity 28000 kgf / mm 2
- a safety factor of 3 is preferably used for growing a single crystal up to a weight of 1 to 3 of the crushing load obtained in the tensile test, and this was set as the load bearing capacity. For example, it was evaluated that a jig broken by a tensile load of 300 kgf in a tensile test can be safely used for growing a single crystal of 100 kg or less.
- the withstand load became 170 kgf or more in each case.
- the material of the holding jig of Example 1 was the same as that of Comparative Example 1, but the load capacity was improved by about 87% compared with that of Comparative Example 1, and the single crystal of up to 187 kg It turned out that we could cope with training.
- Example 2 In the holding jig of Example 2, the load resistance was 250 kg, and in Example 3 in which the material of the holding jig body and the jacket was made of molybdenum, the breaking load was 160,000. kgf, which indicates that single crystals can be grown up to 533 kg.
- the present invention is not limited to the above embodiment.
- the above embodiment is an exemplification, and has substantially the same configuration as the technical idea described in the claims of the present invention, and any device having the same function and effect can be obtained. It is included in the technical scope of the present invention.
- the locking type using the ring-shaped outer jacket has been described, but the locking method is not limited, and the key is inserted into the insertion fitting as shown in FIG. 9. It may be of a type that can be sucked at.
- the overall shape of the seed crystal to be held is not particularly limited. In addition to holding a cylindrical seed crystal in the holding jig shown in Fig. 1, it can also hold a hexagonal or octagonal seed crystal. Alternatively, a material whose tip is machined into a shape such as a conical shape may be used.
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Abstract
Seed crystal holding jig (11) capable of, at the time of drawing up a single crystal in accordance with the Cyochralski method, holding a seed crystal by bringing tapered end face (15) of insert fit member (14) into pressed contact with tapered hold face (18) of seed crystal (5), the taper of the end face (15) in reverse relationship to that of the hold face (18), characterized in that the holding jig (11) is furnished with two or more insert fit members, these insert fit members having a height equal to that of main body (12) of the holding jig and provided at equal intervals round center axis (19) of the holding jig. Preferably, the insert fit members are constituted of a carbon fiber reinforced carbon composite material or an isotropic sintered carbon, while the main body of holding jig comprises eiher a carbon fiber reinforced carbon composite material or a reinforced isotropic sintered carbon or molybdenum. Thus, there are provided a seed crystal holding jig and a process for producing a single crystal, which enable securely drawing up a single crystal of high purity without breakage of seed crystal or holding jig even when a single crystal of large weight, such as 170 kg or more, is grown.
Description
明 細 書 種結晶保持治具及び単結晶の製造方法 技術分野 Description Seed crystal holding jig and manufacturing method of single crystal
本発明は、 チヨ ク ラルス キー法 ( C Z法) によ り シ リ コ ン単結晶や化 合物半導体単結晶等を引き上げる際に用いられる種結晶保持治具及び単結 晶の製造方法に関する。 背景技術 The present invention relates to a jig for holding a seed crystal used for pulling a silicon single crystal or a compound semiconductor single crystal or the like by a Chiral Clarke method (CZ method), and a method for manufacturing a single crystal. Background art
従来、 例えばシ リ コ ン単結晶を製造する場合、 多結晶シ リ コ ンを溶融し た溶融原料にシリ コン種結晶を浸した後、 これを回転させながら引き上げ てシ リ コ ン単結晶を成長させるチヨ ク ラルス キー法 ( C Z法) と呼ばれる 製造方法が知られている。 Conventionally, for example, when manufacturing a silicon single crystal, a silicon seed crystal is immersed in a molten material obtained by melting polycrystalline silicon, and then the silicon seed crystal is pulled up while being rotated to convert the silicon single crystal. There is known a manufacturing method called the Chiyolarski method (CZ method) for growing.
図 7 は、 C Z法に用いられる単結晶引上げ装置の一例を示している。 こ の単結晶引上げ装置 2 0 は、 チャンバ一 1 0 内にシリ コン融液 2 を収容す るルツボ 3 を配置し、 ルツボ 3 を回転させるルツボ支持軸 4及び回転機構 (図示せず) と、 種結晶 5 を保持する種結晶保持治具 6 と、 種結晶保持治 具 6 を引き上げるワイ ヤー 7 と、 ワイヤー 7 を回転または卷き取る卷取り 機構 (図示せず) とから構成されている。 また、 ルツボ 3 の周囲にはヒー タ 8 を配置し、 ヒータ 8 の外周には断熱材 9 を配置して単結晶を引上げる 構造になっている。 FIG. 7 shows an example of a single crystal pulling apparatus used for the CZ method. The single crystal pulling apparatus 20 includes a crucible 3 for accommodating a silicon melt 2 in a chamber 10, a crucible support shaft 4 for rotating the crucible 3, and a rotating mechanism (not shown); It comprises a seed crystal holding jig 6 for holding the seed crystal 5, a wire 7 for lifting the seed crystal holding jig 6, and a winding mechanism (not shown) for rotating or winding the wire 7. In addition, a heater 8 is arranged around the crucible 3, and a heat insulating material 9 is arranged around the heater 8 to pull up the single crystal.
上記単結晶引上げ装置 2 0 によ り シリ コン単結晶を製造するには、 ルツ ボ 3 内でシリ コ ンの多結晶を融点以上に加熱して融解し、 ワイヤー 7 を卷 き出して融液 2の中心に種結晶 5の先端を接触又は浸漬させる。 次いで、 ルツボ 3 を適宜の方向に回転させる と共に、 ワイヤー 7 を回転させながら 卷取り 、 種結晶 5 を引き上げるこ とによ り 単結晶の育成が開始される。 そ の後、 引上げ速度と温度を適切に制御するこ とによ り ほぼ円柱状の成長単
結晶 1 を得るこ とができ る。 In order to produce a silicon single crystal using the single crystal pulling apparatus 20, a silicon polycrystal is heated in a crucible 3 to a temperature higher than the melting point and melted, and a wire 7 is unwound to melt. The tip of seed crystal 5 is contacted or immersed in the center of 2. Next, the crucible 3 is rotated in an appropriate direction, the wire 7 is wound while being rotated, and the seed crystal 5 is pulled up to start growing a single crystal. After that, by appropriately controlling the pulling rate and temperature, the growth of almost cylindrical growth Crystal 1 can be obtained.
上記の種結晶 5 を保持する種結晶保持治具 6 は、 従来、 様々な構造のも のが提案されてお り 、 一般的に使用されているものと して図 8 に示したキ 一ロ ック型の保持治具がある。 この保持治具 6 a は、 種結晶 5のテーパが 付いた保持面 1 8 に対して保持治具 6 a の本体の横から逆のテーパが付い た揷嵌具 2 4 を差込み、 さ らにリ ング状の外套 2 6 を本体に被せて挿嵌具 2 4が抜けないよ う に口 ック されている。 これによ り種結晶 5の保持面 1 8が揷嵌具 2 4 の端面 1 5 で圧接されて種結晶 5が保持される。 As the seed crystal holding jig 6 for holding the seed crystal 5 described above, various types of structures have been proposed in the past, and as shown in FIG. There is a lock type holding jig. In this holding jig 6 a, a reverse-tapered fitting 24 is inserted from the side of the main body of the holding jig 6 a into the tapered holding surface 18 of the seed crystal 5, and A ring-shaped outer cover 26 is put on the main body so as to prevent the insertion fitting 24 from falling out. As a result, the holding surface 18 of the seed crystal 5 is pressed against the end surface 15 of the fitting 24 so that the seed crystal 5 is held.
図 9 は、 キーロ ック型の他の保持治具 6 b を示しており、 揷嵌具 2 4 に キー 2 5 を嵌め込んで口 ックするこ とで挿嵌具 2 4の端面 1 5 を種結晶 5 の保持面 1 8 に圧接し、 種結晶 5 を保持している。 FIG. 9 shows another holding jig 6b of the key lock type. キ ー Insert the key 25 into the fitting 24 and lock it so that the end face 15 of the insertion fitting 24 is formed. Is pressed against the holding surface 18 of the seed crystal 5 to hold the seed crystal 5.
また、 他の保持治具と して例えば図 1 0 に示したよ う なピンロ ック型の ものがある。 この保持治具 6 c は、 治具本体と種結晶 5 との間に設けた円 形の孔に円柱状のピン 2 7 を挿入して種結晶を係止するものであるが、 ピ ンロ ック型の保持治具 6 c の場合、 キーロ ック型のよ う にテーパの付いた 面を圧接させて種結晶を保持するのものに比べ、 ピン 2 7 と種結晶 5 との 間に点接触が生じて種結晶 5 を破損し易いほか、 高い加工精度が要求され るなどの問題があるため、 テーパの付いたキー口 ック型の保持治具が好ん で使用されている。 As another holding jig, there is, for example, a pin lock type as shown in FIG. The holding jig 6 c is for locking the seed crystal by inserting a cylindrical pin 27 into a circular hole provided between the jig body and the seed crystal 5. In the case of the holding jig 6c, the point between pin 27 and the seed crystal 5 is smaller than that of the key lock type, which holds the seed crystal by pressing the tapered surface into contact. Since the seed crystal 5 is liable to be damaged due to contact, and high processing accuracy is required, a tapered key-mouth type holding jig is preferably used.
キー口 ック型の種結晶保持治具で種結晶を保持して単結晶を製造する際、 保持治具や種結晶には、 種結晶に続いて育成した単結晶の全重量がかかる。 もし保持治具または種結晶が強度不足で破壊する と、 極めて高温の溶融原 料に単結晶が落下し、 育成した単結晶や装置を破損させるこ とになる。 そ のため、 育成する単結晶を確実に保持するこ とができ る保持治具を使用す る必要がある。 When a single crystal is manufactured by holding a seed crystal with a key-open type seed crystal holding jig, the total weight of the single crystal grown after the seed crystal is applied to the holding jig and the seed crystal. If the holding jig or the seed crystal breaks due to insufficient strength, the single crystal falls on the extremely high-temperature molten raw material and damages the grown single crystal or equipment. Therefore, it is necessary to use a holding jig that can securely hold the single crystal to be grown.
例えば、 従来一般的に製造されている直径 2 0 O m m以下のシリ コ ン単 結晶の重量は最大でも 1 2 0 k g程度だったが、 近年主流にな りつつある 直径 3 0 O m mのよ う な大型化したシリ コン単結晶は 1 7 0 k g以上にも
な り 、 保持治具に加わる荷重が極めて大き く なる。 特に、 直径 3 0 0 m m の単結晶の育成では、 望ましく は 2 5 0 k g を超える長尺の結晶を安全に かつ確実に引き上げるこ とが切望されている。 For example, the weight of a conventional silicon single crystal having a diameter of less than 200 mm was at most about 120 kg , but in recent years it has become mainstream. Such large silicon single crystals can exceed 170 kg. As a result, the load applied to the holding jig becomes extremely large. In particular, in growing a single crystal having a diameter of 300 mm, it is desired to safely and surely pull a long crystal desirably exceeding 250 kg.
従来、 種結晶保持治具の材質と しては、 一般的には等方性焼結カーボン が用いられてきた。 このよ う な材質の保持治具であれば、 単結晶の金属汚 染を引き起こすこ とがなく、 また、 1 6 0 k g f 程度の耐荷重を得るこ と ができるため、 直径 2 0 O m m以下の単結晶を育成するのに使用するこ と ができ る。 しかし、 直径 3 0 0 m mのシ リ コ ン単結晶の育成で求め られる 1 7 0 k g f 以上の耐荷重を得るこ とは難しく なる。 Conventionally, isotropic sintered carbon has been generally used as a material for a seed crystal holding jig. A holding jig of such a material does not cause metal contamination of single crystal and can withstand a load of about 160 kgf, so that the diameter is less than 20 Omm. It can be used to grow single crystals. However, it is difficult to obtain a load bearing capacity of more than 170 kgf, which is required for growing silicon single crystals with a diameter of 300 mm.
従来、 保持治具あるいは種結晶の破損を防ぐために様々な工夫がなされ てきた。 例えば、 特開平 1 1一 7 9 8 8 2号公報には、 種結晶と種結晶保 持治具の当接面の間に、 炭素繊維製あるいは金属繊維製フュル トなどの耐 熱性ク ッショ ン材を介在させるこ とによ り、 荷重応力の一点集中による保 持治具や種結晶の破損を防止する種結晶保持治具が開示されている。 Conventionally, various measures have been taken to prevent the holding jig or the seed crystal from being damaged. For example, Japanese Patent Application Laid-Open No. 11-197882 discloses a heat-resistant cushion such as a carbon fiber or metal fiber flute between a seed crystal and a contact surface of a seed crystal holding jig. A holding jig and a seed crystal holding jig that prevent breakage of a seed crystal by one point concentration of load stress by interposing a material are disclosed.
しかしながらこの保持治具では、 1 7 0 k g以上の高重量の単結晶を引 き上げるには強度的に十分でなく 、 また、 ク ッショ ン材が押圧されたと き にク ッショ ン材から微粉末が飛散して溶融原料に混入し、 単結晶の純度を 低下させるおそれがある。 However, this holding jig is not strong enough to pull a heavy single crystal of 170 kg or more, and when the cushion material is pressed, the fine powder is removed from the cushion material. May be scattered and mixed into the molten raw material, thereby lowering the purity of the single crystal.
また、 特開平 9 一 2 3 5 1 8 4号公報には、 断面が角形の種結晶の少な く と も 2面を、 保持治具の種結晶揷入孔の内側面に向けて圧接する種結晶 保持治具が開示されている。 こ の保持治具を用いれば、 種結晶を傾けずに 正確に位置決め して保持するこ とができ、 また、 保持力が高まるこ とにな る。 Also, Japanese Patent Application Laid-Open No. 9-123541 discloses that at least two surfaces of a seed crystal having a rectangular cross section are pressed against a seed crystal of a holding jig toward an inner surface of an insertion hole. A crystal holding jig is disclosed. By using this holding jig, the seed crystal can be accurately positioned and held without tilting, and the holding force is increased.
しかしながら、 このよ うな保持治具でも今後のよ り高重量の単結晶を引 き上げるには強度が十分でなく 、 引上げ中に種結晶あるいは保持治具が破 壊されてしま うおそれがある。 However, even with such a holding jig, the strength is not sufficient to pull a heavier single crystal in the future, and the seed crystal or the holding jig may be broken during the pulling.
このよ う にたと えキー口 ック型の種結晶保持治具を使用したと しても、 今後一層高重量の単結晶を育成しょ う とする と、 保持治具の一部が破損し
て汚染物質が飛散し、 これが高純度な原料融液に不純物が混入するこ とで 単結晶の純度品質が低下したり 、 種結晶あるいは保持治具が破損して育成 中の単結晶が落下する可能性がある という問題があった。 Even if a key-lock type seed crystal holding jig is used in this way, if a higher weight single crystal is to be grown in the future, a part of the holding jig will be damaged. The contaminants are scattered, and the impurities are mixed into the high-purity raw material melt, thereby deteriorating the purity quality of the single crystal, or the seed crystal or the holding jig is damaged and the growing single crystal falls. There was a problem that there was a possibility.
発明の開示 Disclosure of the invention
そこで本発明は、 1 7 0 k g以上の高重量の単結晶を育成する場合でも、 種結晶や保持治具が破壊せず、 高純度の単結晶を安全かつ確実に引き上げ るこ とができ る種結晶保持治具及び単結晶の製造方法を提供するこ と を目 的とする。 Therefore, the present invention can safely and reliably pull a high-purity single crystal without breaking the seed crystal or holding jig even when growing a high-weight single crystal of 170 kg or more. It is intended to provide a seed crystal holding jig and a method for producing a single crystal.
上記目的を達成するため、 本発明によれば、 チヨ ク ラルスキー法によ り 単結晶を引き上げる際、 テーパーが付いた種結晶の保持面に、 逆のテーパ 一が付いた揷嵌具の端面を圧接させて前記種結晶を保持する保持治具であ つて、 前記揷嵌具を 2つ以上具備し、 これらの挿嵌具が、 保持治具の本体 の同じ高さに、 かつ中心軸の周 り に等間隔で設けられているこ と を特徴と する種結晶保持治具が提供される。 In order to achieve the above object, according to the present invention, when pulling a single crystal by the Chiyo-Kralski method, an end face of a reverse fitting with a reverse taper is attached to a holding surface of a tapered seed crystal. A holding jig for holding the seed crystal by pressing, comprising two or more of the above-mentioned fittings, wherein these inserting fittings are at the same height as the main body of the holding jig and around the center axis. In addition, a seed crystal holding jig characterized by being provided at equal intervals is provided.
こ の よ う な種結晶保持治具を用いれば、 同じ高さの周囲に等間隔で設け られている複数の挿嵌具で種結晶の保持面を圧接して種結晶を保持する こ とができ、 育成中の単結晶による荷重が均等に分散される。 従って、 種結 晶ゃ保持治具の耐荷重が向上し、 高重量の単結晶でも高純度で確実に引き 上げるこ とができ る。 By using such a seed crystal holding jig, it is possible to hold the seed crystal by pressing the holding surface of the seed crystal with a plurality of inserts provided at equal intervals around the same height. The load from the growing single crystal is evenly distributed. Therefore, the load resistance of the seed crystal / holding jig is improved, and even a heavy single crystal can be reliably pulled with high purity.
揷嵌具は、 引張り強度が 2 0 0 k g f / c m 2以上で弾性係数が 2 0 0 O k g f Z m ni 2以下のものであるこ とが好ま しく 、 その材質と しては、 炭素繊維強化炭素複合材又は等方性焼結カーボンからなるものである こ と が好ま しい。 揷 The fitting preferably has a tensile strength of 200 kgf / cm 2 or more and an elastic modulus of 200 O kgf Zm ni 2 or less, and is made of carbon fiber reinforced carbon. It is preferably made of a composite material or isotropic sintered carbon.
揷嵌具が硬すぎると、 種結晶を圧接して高荷重を負荷したときに破壊し てしま うおそれがあるが、 引張り強度が 2 0 0 k g f / c m 2以上で弾性 係数が 2 0 0 0 k g f / rn m 2以下の揷嵌具であれば、 このよ う な破壌を 効果的に防ぐこ とができ る。
また、 挿嵌具の材質を炭素繊維強化炭素複合材又は等方性焼結カーボン とすれば、 挿嵌具の強度と しても十分である し、 かつ柔軟性を有するので 破壊するこ と もなく 、 種結晶の破壊も効果的に防ぐこ とができ る上、 育成 する単結晶の金属汚染を防ぐこ と もでき る。 揷 If the fitting is too hard, the seed crystal may break when subjected to a high load by pressing against it, but the tensile modulus is more than 200 kgf / cm2 and the elastic modulus is 200 if kgf / rn m 2 following揷嵌tool, Ru can and child to prevent this Yo I Do Yabu壌effectively. Also, if the material of the insert is carbon fiber reinforced carbon composite material or isotropic sintered carbon, the strength of the insert is sufficient, and since the insert has flexibility, it can be broken. In addition, seed crystal destruction can be effectively prevented, and metal contamination of the grown single crystal can be prevented.
また、 保持治具の本体は、 引張り 強度が 2 0 O k g f Z c m 2以上で弾 性係数が 8 0 0 k g f / m m 2以上のものであるこ とが好ま しく 、 特にそ の材質は、 炭素繊維強化炭素複合材、 強化等方性焼結カーボン、 モリ ブデ ン又は少なく と もそれらのいずれかを含むものであるこ とが好ま しい。 保持治具の本体を引張り強度が 2 0 0 k g f / c m 2以上で弾性係数が 8 0 0 k g f Z m m 2以上のものとすれば、 保持治具本体の強度を十分高 くするこ とができ、 特に炭素繊維強化炭素複合材、 強化等方性焼結カーボ ン、 又はモリ プデンなどの材質のものは耐熱性が極めて高いため、 高温と なるチャ ンバ内でも強度を十分保つこ とができ る。 The holding jig body preferably has a tensile strength of at least 20 O kgf Z cm 2 and an elastic modulus of at least 800 kgf / mm 2 , and particularly, the material is carbon fiber. Preferably, it is a reinforced carbon composite, reinforced isotropic sintered carbon, molybdenum or at least one of them. If the holding jig body has a tensile strength of 200 kgf / cm 2 or more and an elastic modulus of 800 kgf Z mm 2 or more, the strength of the holding jig body can be sufficiently increased. Particularly, materials such as carbon fiber reinforced carbon composite material, reinforced isotropic sintered carbon, and molybdenum have extremely high heat resistance, so that sufficient strength can be maintained even in a high-temperature chamber. .
また、 本発明によれば、 種結晶のテーパーが付いた保持面に、 種結晶保 持治具の逆のテーパーが付いた揷嵌具の端面を圧接させて前記種結晶を保 持し、 チヨ クラルスキー法によ り 単結晶を製造する方法において、 種結晶 と して、 前記テーパーが付いた 2つ以上の保持面が、 同じ高さに、 かつ中 心軸の周 り に等間隔で設けられている種結晶を用いる と と もに、 種結晶保 持治具と して、 前記種結晶の全ての保持面を圧接する挿嵌具を具備する保 持治具を用いて種結晶を保持し、 単結晶を引き上げるこ と を特徴とする単 結晶の製造方法も提供される。 According to the present invention, the seed crystal is held by pressing the end face of a fitting having a reverse taper of the seed crystal holding jig against the tapered holding surface of the seed crystal by holding the seed crystal. In a method for producing a single crystal by the Kralski method, as a seed crystal, two or more tapered holding surfaces are provided at the same height and at equal intervals around a central axis. The seed crystal is held using a holding jig provided with an insertion fitting for pressing all the holding surfaces of the seed crystal as the seed crystal holding jig. Also, a method for producing a single crystal characterized by pulling up the single crystal is provided.
こ の よ う に種結晶を保持すれば、 育成単結晶による荷重を均一に分散さ せるこ とができ るので、 高重量の単結晶でも確実に引き上げて製造する こ とができ、 直径 3 0 0 m m以上といった大口径単結晶の生産性を向上させ るこ とができる と と もに、 保持治具の材質が飛散して単結晶が汚染する こ と も防ぐこ とができ る。 By holding the seed crystal in this way, the load of the grown single crystal can be evenly dispersed, so that even a heavy single crystal can be reliably pulled up and manufactured with a diameter of 30%. The productivity of a single crystal having a large diameter of 0 mm or more can be improved, and the material of the holding jig can be prevented from being scattered and the single crystal can be prevented from being contaminated.
本発明の保持治具は、 2つ以上の揷嵌具が、 保持治具の本体の同じ高さ に、 かつ中心軸の周 り に等間隔で設けられているので、 これを用いて種結
晶を保持すれば、 結晶の育成につれて増加する荷重を均等に分散させるこ とができ、 種結晶と種結晶保持治具の耐荷重を大幅に向上させるこ とがで き る。 その結果、 例えば直径 3 0 O m m以上の大口径で、 1 7 0 k g以上 の大型のシリ コン単結晶でも高純度で安全に引き上げるこ とができ、 単結 晶製造の歩留ま り 向上と コス ト低減を達成するこ と もでき る。 図面の簡単な説明 In the holding jig of the present invention, since two or more fittings are provided at the same height of the main body of the holding jig and at equal intervals around the central axis, the holding jig is used for seeding. By holding the crystals, the load that increases as the crystals grow can be evenly dispersed, and the load bearing capacity of the seed crystal and the seed crystal holding jig can be greatly improved. As a result, even large silicon single crystals with a diameter of, for example, 30 O mm or more and a mass of 170 kg or more can be safely pulled up with high purity, improving the yield of single crystal production. Cost reductions can also be achieved. BRIEF DESCRIPTION OF THE FIGURES
図 1 は、 本発明の種結晶保持治具の一例を示す概略断面図である。 ( a ) 縦断面 FIG. 1 is a schematic sectional view showing an example of a seed crystal holding jig of the present invention. (a) Longitudinal section
( b ) 本体部分の横断面 (b) Cross section of main body
図 2 は、 保持される種結晶の概略図である。 Figure 2 is a schematic diagram of the seed crystal that is retained.
図 3 は、 本発明に係る種結晶保持治具の他の例と保持される種結晶を示 す図である。 FIG. 3 is a view showing another example of a seed crystal holding jig according to the present invention and a seed crystal held.
( a ) 保持治具本体の概略断面図 (a) Schematic sectional view of the holding jig body
( b ) 保持される種結晶の斜視図 (b) Perspective view of retained seed crystal
図 4 は、 本発明に係る種結晶保持治具のさ らに別の例の本体の概略断面 図である。 FIG. 4 is a schematic sectional view of still another example of the main body of the seed crystal holding jig according to the present invention.
図 5 は、 引っ張り試験で用いた試験用種結晶を示す図である。 FIG. 5 is a diagram showing a test seed crystal used in the tensile test.
( a ) 実施例 (a) Example
( b ) 比較例 (b) Comparative example
図 6 は、 引っ張り試験の概要を説明する図である。 Figure 6 is a diagram illustrating the outline of the tensile test.
図 7 は、 チヨ クラルスキー法による単結晶引き上げ装置の一例である。 図 8 は、 従来のキー口 ック型の種結晶保持治具の一例を示す概略図であ る。 Figure 7 shows an example of a single crystal pulling apparatus using the Chiyo-Kralski method. FIG. 8 is a schematic diagram showing an example of a conventional key-lock type seed crystal holding jig.
図 9 は、 従来のキーロ ック型の種結晶保持治具の他の例を示す概略図で ある。 FIG. 9 is a schematic diagram showing another example of a conventional keylock type seed crystal holding jig.
図 1 0 は、 ピンロ ック型の種結晶保持治具の一例を示す概略図である。
発明を実施するための最良の形態 FIG. 10 is a schematic diagram showing an example of a pin-lock type seed crystal holding jig. BEST MODE FOR CARRYING OUT THE INVENTION
以下、 本発明の実施の形態について具体的に説明するが、 本発明はこれ らに限定されるも のではない。 Hereinafter, embodiments of the present invention will be specifically described, but the present invention is not limited thereto.
図 1 は、 本発明の種結晶保持治具の一例を示し、 図 2 は、 保持される種 結晶を示している。 種結晶 5 は四角柱のものであり 、 テーパーが付いた 2 つの保持面 1 8 が、 同じ高さに、 かつ中心軸 1 9 ' の周 り に対向して設け られている。 一方、 保持治具 1 1 は、 本体 1 2の同じ高さに、 かつ中心軸 1 9の周 り に挿嵌具 1 4 を挿入するための 2つの貫通孔 1 3が対向して形 成されており 、 これらの貫通孔 1 3 には種結晶 5の保持面 1 8 のテーパー とは逆のテーパーが付いている揷嵌具 1 4が対向して挿入されている。 このよ う な揷嵌具 1 4 の端面 1 5 と種結晶 5の保持面 1 8 は対応する位 置に設けられてお り 、 さ らに、 保持面 1 8 のテーパーの角度と、 揷嵌具 1 4の端部のテーパーの角度は同じ角度に形成されている。 そして、 揷嵌具 1 4が抜けないよ う にリ ング状の外套 1 6 を治具本体 1 2に被せるこ とで ロ ック され、 これによ り種結晶 5の 2つの保持面 1 8 を均等に圧接して種 結晶 5 を保持している。 FIG. 1 shows an example of a seed crystal holding jig of the present invention, and FIG. 2 shows a seed crystal to be held. Seed crystal 5 is a quadrangular prism, and two tapered holding surfaces 18 are provided at the same height and opposed around central axis 19 ′. On the other hand, the holding jig 11 is formed at the same height as the main body 12 and with two through holes 13 for inserting the insertion fitting 14 around the center axis 19 facing each other. In these through holes 13, a fitting 14 having a taper opposite to the taper of the holding surface 18 of the seed crystal 5 is inserted so as to face the through hole 13. The end surface 15 of such a fitting 14 and the holding surface 18 of the seed crystal 5 are provided at corresponding positions, and furthermore, the angle of the taper of the holding surface 18, The angle of the taper at the end of the tool 14 is formed at the same angle. Then, the jig body 12 is covered with a ring-shaped mantle 16 so as to prevent the fitting tool 14 from coming off, so that the jig body 12 is locked. Are pressed equally to hold the seed crystal 5.
図 3 は、 本発明に係る種結晶保持治具の他の本体の断面と これに保持さ れる種結晶を示したものである。 FIG. 3 shows a cross section of another main body of the seed crystal holding jig according to the present invention and a seed crystal held by the main body.
図 3 ( a ) に示されている保持治具本体 1 2の中央には円筒形の種結晶 挿入孔 1 7 が形成されている。 また、 治具本体 1 2 の同じ高さに、 かつ 中心軸 1 9 の周 り には、 3つの貫通孔 1 3 が等間隔で形成されてお り 、 こ れらの貫通孔 1 3 にそれぞれ挿嵌具を挿入するこ とができるよ う になつて いる。 A cylindrical seed crystal insertion hole 17 is formed at the center of the holding jig main body 12 shown in FIG. 3 (a). Also, three through holes 13 are formed at the same height of the jig body 12 and around the center axis 19 at equal intervals, and these through holes 13 are respectively formed. The insertion fitting can be inserted.
一方、 保持される種結晶 5 ' は、 図 3 ( b ) に示されているよ う に全体 が円柱形状をしており 、 揷嵌具の端面のテーパーと同じ角度のテーパーが 付いた 3つの保持面 1 8 が、 同じ高さに、 かつ中心軸 1 9 の周 り に対向 して設けられている。 種結晶は 5 'は、 3 つの保持面 1 8全てがそれぞれ 揷嵌具で圧接されて保持される。
さ らに図 4 は、 4つの挿嵌具を具備する保持治具本体 1 2の断面を示し ており 、 4つの貫通孔 1 3が保持治具本体 1 2 の同じ高さに、 かつ中心軸 1 9の周 り に等間隔で設けられている。 このよ うな保持治具で種結晶を保 持する場合は、 挿嵌具に対応する 4つの保持面を有する種結晶を用い、 こ れら全ての保持面を揷嵌具の端面で圧接して保持するよ う にする。 On the other hand, as shown in Fig. 3 (b), the retained seed crystal 5 'has a columnar shape as a whole, and has three tapers with the same angle as the taper of the end face of the fitting. The holding surface 18 is provided at the same height and opposed around the center axis 19. The seed crystal 5 ′ is held by pressing all three holding surfaces 18 with 揷 fittings. FIG. 4 shows a cross section of the holding jig main body 12 having four insertion fittings. The four through holes 13 are at the same height as the holding jig main body 12, and the center axis is It is provided at equal intervals around 19. When a seed crystal is held by such a holding jig, a seed crystal having four holding surfaces corresponding to the insertion fitting is used, and all these holding surfaces are pressed against the end face of the fitting. Try to keep it.
本発明の保持治具の材質に関しては、 高重量の単結晶を安全に引き上げ るのに十分強い圧縮強度及び引っ張り強度を有するものを使用する必要が あるが、 挿嵌具の材質と して非常に硬い材質、 例えば弾性係数が 1 0 0 0 0 k g Zinm 2を超えるモリ ブデンやステ ン レス、 あるいはそれらの合金 といった金属材料を用いると、 脆性材料である単結晶からなる種結晶を圧 接したときに種結晶を傷 όけて耐荷重を低下させたり 、 さ らには種結晶を 折損してしま うおそれがある。 従って、 挿嵌具は、 挿嵌具自体の破壊が防 がれる と と もに、 種結晶や治具本体の損傷 · 破壊を防ぐため、 引張り強度 力 S 2 0 0 〜 7 0 0 0 k g f / c m 2であ り 、 かつ弹性係数が 5 0 0 〜 2 0 0 0 k g f Zmm 2 となるものが好ま しい。 As for the material of the holding jig of the present invention, it is necessary to use a material having a compressive strength and a tensile strength sufficiently strong to safely pull up a heavy crystal having a high weight. When a hard material such as molybdenum, stainless steel, or an alloy thereof with an elastic modulus of more than 1000 kg Zinm 2 is used, a seed crystal consisting of a single crystal, which is a brittle material, is pressed. At times, the seed crystal may be damaged to lower the load-bearing capacity, or the seed crystal may be broken. Therefore, the insert has a tensile strength of S200 to 700 kgf / to prevent the breakage of the insert itself and to prevent damage and destruction of the seed crystal and the jig body. cm 2 and a conductivity coefficient of 500 to 200 kgf Zmm 2 is preferable.
挿嵌具の引張り 強度が 2 0 0 k g f / c m 2未満である と揷嵌具自体が 破壊するおそれがあるので、 通常使用される C I P (冷間静水圧成形) 材 ( C I P — A ) を含む材料のも ので、 2 0 O k g f / c m 2以上が好ま し く 、 よ り好ま しく は高強度に成形した C I P材 ( C I P — B ) を含む材料 のもので、 3 0 0 k g f Z c m 2以上である。 一方、 挿嵌具の材質の引張 り強度が 7 0 0 0 k g f / c m 2を超える と、 種結晶や治具本体を損傷し たり破壊するおそれがある。 If the tensile strength of the insert is less than 200 kgf / cm2, the insert itself may be broken, so it includes the commonly used CIP (Cold Isostatic Pressing) material (CIP — A) also because the material, 2 0 O kgf / cm 2 or more is preferred rather, good Ri favored properly the CIP material molded high strength - those materials containing (CIP B), 3 0 0 kgf Z cm 2 or more It is. On the other hand, if the tensile strength of the material of the insert exceeds 700 kgf / cm 2 , the seed crystal or the jig body may be damaged or broken.
また、 挿嵌具の弾性係数が 5 0 0 k g f / m m 2未満である と、 変形し やすく応力集中による強度低下が発生するおそれがあ り、 一方、 2 0 0 0 k g i /mm 2を超える と種結晶や治具本体を損傷したり破壊するおそれ があ る。 Further, when the elastic modulus of the inserted instrument is less than 5 0 0 k g f / mm 2, carry the risk that the strength reduction due to deformation easily stress concentration occurs, whereas, the 2 0 0 0 kgi / mm 2 If it exceeds, the seed crystal and the jig body may be damaged or destroyed.
挿嵌具の好ましい材質と しては、 炭素繊維強化炭素複合材 ( Cノ C材) 又は等方性焼結カーボンを用いるこ とができ る。 これらの材質からなる揷
嵌具であれば、 種結晶を破壊せず、 種結晶を圧接する ときに端面が適度に 潰れて面接触を得るこ とができ、 仮にその微粉末が原料融液中に混入して も単結晶を金属汚染するこ とがない。 ただし、 例えば引張り強度が 2 0 0 k g f ノ c in 2未満の等方性焼結カーボン材を用いた場合には強度が不十 分とな り圧縮破壊されるおそれが.あるので、 好ましく は 2 0 0 k g f / c m 2以上、 よ り 好ま しく は 3 0 O k g i Z c m 2以上 (一般的なカーボン 材の範囲) の引張り強度を有する等方性焼結カーボン材からなる挿嵌具と すれば、 挿嵌具も種結晶も破壌され難く な り、 好適である。 As a preferable material of the insertion fitting, a carbon fiber reinforced carbon composite material (C / C material) or isotropic sintered carbon can be used. Made of these materials. With a fitting, the seed crystal is not broken, and the end face is appropriately crushed when the seed crystal is pressed, so that surface contact can be obtained. Even if the fine powder is mixed into the raw material melt, it is simply There is no metal contamination of the crystal. However, for example, when an isotropic sintered carbon material having a tensile strength of less than 200 kgf no c in 2 is used, the strength becomes insufficient and there is a risk of compressive fracture. When the insert is made of an isotropic sintered carbon material having a tensile strength of at least 0 kgf / cm 2, more preferably at least 30 O kgi Z cm 2 (the range of general carbon materials) However, both the insert and the seed crystal are less likely to be crushed, which is preferable.
一方、 揷嵌具以外の各部材の材質と しては、 金属を好適に用いるこ とが でき る。 例えば保持治具の本体は、 モリ ブデン、 炭素繊維強化炭素複合材、 強化等方性焼結カーボン又は少なく と もそれらのいずれかを含むものとす るこ とができ る。 例えばモリ ブデンのよ う な高融点の金属で保持治具本体 を構成すれば、 治具本体の強度が極めて高く な り、 単結晶の引上げ中に高 温になるチャ ンバ一内でも十分高い強度を保つこ とができ る。 なお、 保持 治具本体に金属材料を用いた場合、 その金属微粉が単結晶の育成中に原料 融液に混入して金属汚染を引き起こすおそれもあるので、 本体の金属表面 をカーボン材で被覆して金属汚染を防ぐよ う にしても良い。 On the other hand, metal can be suitably used as a material of each member other than the fitting. For example, the body of the holding jig can be molybdenum, carbon fiber reinforced carbon composite, reinforced isotropic sintered carbon, or at least one of them. For example, if the holding jig body is made of a metal with a high melting point such as molybdenum, the strength of the jig body will be extremely high, and the strength will be sufficiently high even in a chamber that becomes hot during pulling of a single crystal. Can be maintained. If a metal material is used for the holding jig body, the fine metal powder may be mixed into the raw material melt during the growth of the single crystal and cause metal contamination.Therefore, cover the metal surface of the body with a carbon material. To prevent metal contamination.
なお、 保持治具本体は、 引張り強度力 S 2 0 0〜 2 0 0 0 0 k g f / c m 2であ り 、 弾性係数が 8 0 0〜 3 0 0 0 0 k g f /mm 2の も のである こ とが好ま しい。 保持治具本体の引張り 強度が 2 0 0 k g ί / c m 2未満で ある と治具本体が破壌し易く な り、 一方、 2 0 0 0 0 k g f / c m 2を超 える と種結晶を損傷あるいは破壊するおそれがある。 The holding jig body, tensile strength force S 2 0 0~ 2 0 0 0 0 kgf / cm 2 der is, the elastic coefficient is the well 8 0 0~ 3 0 0 0 0 kgf / mm 2 for this Is preferred. If the tensile strength of the holding jig body is less than 200 kgί / cm 2 , the jig body will be easily ruptured, while if it exceeds 2000 kgf / cm 2 , the seed crystal will be damaged. Or there is a risk of being destroyed.
また、 保持治具本体の弹性係数が 8 0 0 k g ί / m m 2未満である と変 形しやすく応力集中による強度低下を招く おそれがあり 、 一方、 3 0 0 0 0 k g i /mm 2を超える と種結晶を損傷あるいは破壊するおそれがある。 また、 挿嵌具以外の各部材の材質と して前記等方性焼結カーボンを使用 するこ と もでき、 保持治具の全ての部材を等方性焼結カーボンで構成して もよい。 ただし、 保持治具本体を等方性焼結カーボンで構成した場合、 挿
嵌具を嵌め込む貫通孔の数が増えるとその部分の断面積が減少して強度が 不十分となるおそれがあるので、 図 1 に示されるよ う な揷嵌具 1 4 を 2つ 対向させて配置する構造とするのが好ま しい。 Further, there is a possibility that弹性coefficient holding jig body incurs 8 0 0 kg strength reduction due to deformation easily stress concentration and ί is less than / mm 2, whereas, more than 3 0 0 0 0 kgi / mm 2 And the seed crystal may be damaged or destroyed. Further, the above-mentioned isotropic sintered carbon can be used as a material of each member other than the insertion fitting, and all the members of the holding jig may be made of isotropic sintered carbon. However, if the holding jig body is made of isotropic sintered carbon, If the number of through holes into which the fittings are fitted increases, the cross-sectional area of that part may decrease and the strength may be insufficient.Therefore, two 揷 fittings 14 as shown in Fig. 1 are opposed to each other. It is preferable to adopt a structure in which they are arranged in a position.
次に、 図 1 に示される種結晶保持治具 1 1 を用いて C Z法によ り シリ コ ン単結晶を製造する場合を説明する。 Next, a case where a silicon single crystal is manufactured by the CZ method using the seed crystal holding jig 11 shown in FIG. 1 will be described.
まず、 挿嵌具 1 4 の端面 1 5 に対応するテーパーが付いた保持面 1 8 を 有する、 図 2 に示されるよ う な種結晶 5 を用意する。 この種結晶 5 を治具 1 1 の種結晶挿入孔 1 3 に挿入する と と もに、 保持治具本体 1 2 の各貫通 孔 1 3 に挿嵌具 1 4 を揷入し、 揷嵌具 1 4が抜けないよ う にリ ング状の外 套 1 6 を本体 1 2に被せてロ ックする。 これによ り 、 揷嵌具 1 4 の端面が 種結晶 5 の保持面 1 8 を圧接して種結晶 5 を保持するこ とができ る。 First, a seed crystal 5 as shown in FIG. 2 having a tapered holding surface 18 corresponding to the end surface 15 of the insertion fitting 14 is prepared. The seed crystal 5 is inserted into the seed crystal insertion hole 13 of the jig 11, and the insertion fitting 14 is inserted into each through hole 13 of the holding jig body 12, and Put a ring-shaped jacket 16 on the body 12 and lock it so that 14 does not come off. Thus, the end face of the fitting 14 can hold the seed crystal 5 by pressing the holding surface 18 of the seed crystal 5 against the holding face 18.
こ の よ う に本発明の保持治具 1 1 に保持された種結晶 5の先端を、 図 7 に示したよ う な単結晶引き上げ装置のルツポ内に収容されたシリ コン溶融 原料に浸漬した後、 種結晶保持治具 1 1 を回転させる と と もに上方の引き 上げ手段 (ワイ ヤ卷取り機構) によって真上に引き上げるこ とで、 種結晶 5 に続けて単結晶 1 を育成するこ とができる。 Thus, the tip of the seed crystal 5 held by the holding jig 11 of the present invention is immersed in the molten silicon material accommodated in the rutupo of the single crystal pulling apparatus as shown in FIG. The seed crystal holding jig 11 is rotated, and the single crystal 1 is grown following the seed crystal 5 by pulling the jig directly upward by an upper pulling means (wire winding mechanism). Can be.
単結晶 1 が育成するにつれて種結晶 5 には下方に引っ張る荷重が掛かり、 こ の荷重は、 種結晶 5 の保持面 1 8 を圧接する端面 1 5 を介して揷嵌具 1 4 に伝わる。 さ らに揷嵌具 1 4 の下面から治具本体 1 2 に荷重が伝わ り 、 揷嵌具 1 4 の下面に接する本体の A— A '面で本体を引き裂く よ う な引つ 張り応力が生じる。 As the single crystal 1 grows, a downward pulling load is applied to the seed crystal 5, and this load is transmitted to the fitting 14 via the end surface 15 that presses the holding surface 18 of the seed crystal 5. In addition, a load is transmitted from the lower surface of the fitting 14 to the jig main body 12, and a tensile stress that tears the main body at the A--A 'face of the body in contact with the lower surface of the fitting 14 is applied. Occurs.
こ の と き、 本発明の保持治具 1 1 では、 種結晶 5 に掛かる荷重を各挿嵌 具 1 4に均等に分散させるこ と ができ、 分散された荷重は保持治具 1 1 の 中心軸 1 9からみて均等な位置に分散されるため、 偏荷重も生じない。 従 つて、 本発明の保持治具 1 1 では、 挿嵌具が一つの従来の保持治具よ り も 保持治具本体の耐荷重強度が向上するこ とになる。 At this time, with the holding jig 11 of the present invention, the load applied to the seed crystal 5 can be evenly distributed to each of the inserts 14, and the dispersed load is applied to the center of the holding jig 11. Since it is distributed evenly as viewed from the shaft 19, there is no uneven load. Therefore, in the holding jig 11 of the present invention, the load-bearing strength of the holding jig main body is improved as compared with the conventional holding jig having one insertion fitting.
なお、 図 8及ぴ図 9に示した揷嵌具が一つの従来の構造では、 種結晶保 持治具 6 a , 6 b の中心軸から偏芯した位置に全ての荷重が集中して揷嵌
具 2 4が栓抜きのよ う に働き、 高重量の単結晶を育成する と治具本体を引 き裂く よ う に破壊してしま う可能性が高い。 これは、 揷嵌具を複数と して も、 中心軸の周 り に等間隔で設けなかつた場合には保持治具本体の断面積 が小さ く なるのでよ り顕著になる。 In the conventional structure having one fitting shown in FIGS. 8 and 9, all loads are concentrated at positions eccentric from the central axes of the seed crystal holding jigs 6a and 6b. Fitting The tool 24 acts like a bottle opener, and growing a heavy single crystal is likely to tear the jig body apart. This becomes more remarkable even when a plurality of fittings are provided, unless the fittings are provided at equal intervals around the center axis, because the cross-sectional area of the holding jig body is reduced.
また、 種結晶は表面にキズが付く と劈開しやすく なり著しく耐荷重が低 下するが、 本発明の保持治具では、 種結晶は中心軸の周 り に均等な角度間 隔で配置された複数の揷嵌具によつて宙づり にされた状態で保持されるこ とになるので、 保持治具の中心孔の内壁面に圧接されたり 、 内壁面と擦れ 合って種結晶表面にキズが付く よ う なこ とがない。 従って、 本発明の保持 治具を用いれば、 種結晶自体の耐荷重強度も向上するこ とになる。 Also, if the surface of the seed crystal is scratched, it is easily cleaved and the load capacity is significantly reduced.However, in the holding jig of the present invention, the seed crystals are arranged at equal angular intervals around the central axis. Since it is held in a suspended state by a plurality of fittings, it is pressed against the inner wall surface of the center hole of the holding jig, or rubs against the inner wall surface and scratches the seed crystal surface. There is no such thing. Therefore, when the holding jig of the present invention is used, the load bearing strength of the seed crystal itself is also improved.
このよ う に本発明に係る種結晶保持治具を用いて単結晶を育成すれば、 直径 3 0 O m m以上で、 重量が 1 7 0 k g以上、 特に 2 5 0 k g を超える よ う な高重量のシリ コン単結晶でも、 保持治具や種結晶を破壌するこ とな く確実に引き上げるこ とができ る。 As described above, when a single crystal is grown using the seed crystal holding jig according to the present invention, a high crystal having a diameter of 30 O mm or more and a weight of 170 kg or more, particularly more than 250 kg. Even heavy silicon single crystals can be pulled up reliably without breaking the holding jig and seed crystal.
以下、 本発明の実施例および比較例を説明する。 Hereinafter, Examples and Comparative Examples of the present invention will be described.
(引っ張り試験) (Tensile test)
種結晶と種結晶保持治具の強度測定をするために、 引っ張り試験を行つ た。 A tensile test was conducted to measure the strength of the seed crystal and the seed crystal holding jig.
引っ張り試験には、 保持治具と して、 挿嵌具が 2つのもの (本発明のタ ィプ) と、 1つのもの (従来のタイプ) を用い、 それぞれ図 5 ( a ) 又は ( b ) に示したよ う な両端に切 り 欠き (保持面) を付けた試験用種結晶 ( 1 5 m m X l 5 m m X l 2 5 m m ) を保持した。 なお、 保持治具の材質 と しては、 2種類の等方性焼結カーボン材と、 純モリ プデンを用いた。 試験は、 図 6 に示すよ う に行った。 具体的には、 試験用種結晶 5 a ( 5 b ) の両端をそれぞれ保持治具 1 2 a, 1 2 b で保持した上、 一方の保持 治具 1 2 b を固定端に固定し、 他方の保持治具 1 2 a はフ レキシブルジョ イ ン トを介して引っ張り荷重を掛けられるシャ フ トに固定した。 引っ張り
荷重を掛けられるシャフ トの端部には、 ロー ドセルが装備されており 、 種 結晶または種結晶保持治具が破壊された時の引っ張り荷重を計測でき る よ う になつている。 試験では、 0 . 1 m m / m i nの一定速度で保持治具 1 2 a を引っ張り 、 種結晶 5 a ( 5 b ) または種結晶保持治具 1 2 a , 1 2 b が破壊されるまで引っ張り を継続し、 破壊時の荷重を計測した。 試験に 用いた保持治具と計測結果を表 1 に示した。 く表 1 > In the tensile test, two holding jigs (type of the present invention) and one holding jig (conventional type) were used as the holding jigs, respectively, as shown in Fig. 5 (a) or (b) A test seed crystal (15 mm X 15 mm X 125 mm) with notches (holding surfaces) at both ends as shown in Fig. 7 was held. As the material of the holding jig, two types of isotropic sintered carbon materials and pure molybdenum were used. The test was performed as shown in Figure 6. Specifically, both ends of the test seed crystal 5a (5b) are held by holding jigs 12a and 12b, respectively, and one holding jig 12b is fixed to the fixed end, and the other end is fixed to the other end. The holding jig 12a was fixed to a shaft to which a tensile load could be applied via a flexible joint. Pull A load cell is provided at the end of the shaft to which a load can be applied, so that the tensile load when the seed crystal or the seed crystal holding jig is broken can be measured. In the test, the holding jig 12a was pulled at a constant speed of 0.1 mm / min, and the seed crystal 5a (5b) or the seed crystal holding jigs 12a and 12b were pulled until they were broken. The load at the time of failure was measured continuously. Table 1 shows the holding jigs used for the test and the measurement results. Table 1>
CIP A : 弓 I張強度 250kgf/cm2、 弾性係数 1000kgf/mm2 CIP A: Bow I Tensile strength 250kgf / cm 2 , Modulus of elasticity 1000kgf / mm 2
CIP B : 弓 I張強度 700kgf/cm2、 弾性係数 1300kgf/mm2 CIP B: Bow I Tensile strength 700 kgf / cm 2 , Modulus of elasticity 1300 kgf / mm 2
モ リ プデ ン : 純モ リ プデ ン 引張強度 7000 18200kgf /cm2、 弾性係数 28000kgf/mm2 種結晶または種結晶保持治具が破壊する荷重に相当する重さの単結晶を 育成するとなる と、 育成した単結晶が落下する危険が大きい。 そこで、 実 用的には安全率 3 と して、 引っ張り試験で得られた破壌荷重の 1 ノ 3 の重 さまでの単結晶の育成に用いるこ とが好ま しく 、 これを耐荷重と した。 例 えば引っ張り試験で 3 0 0 k g f の引っ張り荷重で破壊した治具は、 1 0 0 k g以下の単結晶の育成に安全に用いるこ とができ る と評価した。 Moripden: pure moripden Tensile strength 7000 18200 kgf / cm 2 , Modulus of elasticity 28000 kgf / mm 2 When a seed crystal or a single crystal with a weight corresponding to the load to break the seed crystal holding jig is grown, There is a great risk that the grown single crystal will fall. Therefore, in practice, a safety factor of 3 is preferably used for growing a single crystal up to a weight of 1 to 3 of the crushing load obtained in the tensile test, and this was set as the load bearing capacity. For example, it was evaluated that a jig broken by a tensile load of 300 kgf in a tensile test can be safely used for growing a single crystal of 100 kg or less.
表 1 に示した結果から明らかなよ う に、 揷嵌具を 1 つだけ具備する比較 例 1 〜 3 の種結晶保持治具を用いた場合には、 目標と した 1 7 0 k g以上 の耐荷重には達せず、 3 0 O mm径の高重量シ リ コン単結晶を育成するに
は強度が十分でないこ とがわかる。 特に、 保持治具全体を高強度のモリ ブ デンで構成した比較例 3 では、 保持治具自体は破壊されなかったが、 最も 弱い破壊荷重で種結晶が折れてしまった。 これは、 揷嵌具が 1つであり 、 良好な面接触が得られておらず、 種結晶の接触点に荷重が集中したためと 考えられる。 As is evident from the results shown in Table 1, 揷 When the seed crystal holding jigs of Comparative Examples 1 to 3 having only one fitting were used, the target resistance of 170 kg or more was achieved. To grow a heavy silicon single crystal with a diameter of 30 O mm without reaching the load Shows that the strength is not enough. In particular, in Comparative Example 3 in which the entire holding jig was made of high-strength molybdenum, the holding jig itself was not broken, but the seed crystal broke under the weakest breaking load. This is considered to be due to the fact that since there was only one fitting and good surface contact was not obtained, the load concentrated on the contact point of the seed crystal.
一方、 2 つの揷嵌具を具備する実施例 1 ないし 3 の種結晶保持治具を用 いた場合には、 いずれも耐荷重が 1 7 0 k g f 以上となった。 特に、 実施 例 1 の保持治具の材質は比較例 1 のものと同じであつたが、 比較例 1 のも のよ り耐荷重が約 8 7 %向上し、 1 8 7 k gまでの単結晶育成に対応でき るこ とがわかった。 On the other hand, when the seed crystal holding jigs of Examples 1 to 3 provided with the two fittings were used, the withstand load became 170 kgf or more in each case. In particular, the material of the holding jig of Example 1 was the same as that of Comparative Example 1, but the load capacity was improved by about 87% compared with that of Comparative Example 1, and the single crystal of up to 187 kg It turned out that we could cope with training.
また、 実施例 2 の保持治具では、 耐荷重が 2 5 0 k g となり 、 さ らに、 保持治具本体と外套の材質をモリ プデンと した実施例 3では、 破壌荷重は 1 6 0 0 k g f に達し、 5 3 3 k gまでの単結晶育成に対応でき るこ とが わかった。 In the holding jig of Example 2, the load resistance was 250 kg, and in Example 3 in which the material of the holding jig body and the jacket was made of molybdenum, the breaking load was 160,000. kgf, which indicates that single crystals can be grown up to 533 kg.
尚、 本発明は、 上記実施形態に限定されるものではない。 上記実施形態 は、 例示であ り 、 本発明の特許請求の範囲に記載された技術的思想と実質 的に同一な構成を有し、 同様な作用効果を奏するものは、 いかなるも ので あっても本発明の技術的範囲に包含される。 Note that the present invention is not limited to the above embodiment. The above embodiment is an exemplification, and has substantially the same configuration as the technical idea described in the claims of the present invention, and any device having the same function and effect can be obtained. It is included in the technical scope of the present invention.
例えば、 上記実施形態においては、 リ ング状の外套を用いてロ ックする タイプについて説明 したが、 ロ ッ ク の仕方は限定されず、 図 9 に示したよ うな挿嵌具にキーを嵌め込んで口 ックするタイプのものと しても よい。 また、 保持する種結晶の全体形状は特に限定されず、 図 1 の保持治具に 円柱状の種結晶を保持するこ とができ るほか、 六角柱や八角柱の種結晶も 保持でき、 また、 先端が円錐状等に尖った形状に加工されているも のを用 いても良い。
For example, in the above-described embodiment, the locking type using the ring-shaped outer jacket has been described, but the locking method is not limited, and the key is inserted into the insertion fitting as shown in FIG. 9. It may be of a type that can be sucked at. The overall shape of the seed crystal to be held is not particularly limited. In addition to holding a cylindrical seed crystal in the holding jig shown in Fig. 1, it can also hold a hexagonal or octagonal seed crystal. Alternatively, a material whose tip is machined into a shape such as a conical shape may be used.
Claims
1 . チヨ ク ラルス キー法によ り 単結晶を引き上げる際、 テーパーが付 いた種結晶の保持面に、 逆のテーパーが付いた挿嵌具の端面を圧接させて 前記種結晶を保持する保持治具であって、 前記揷嵌具を 2つ以上具備し、 これらの揷嵌具が、 保持治具の本体の同じ高さに、 かつ中心軸の周 り に等 間隔で設けられているこ とを特徴とする種結晶保持治具。 1. When the single crystal is pulled up by the Chiral Clarke method, the holding surface for holding the seed crystal by pressing the end face of the reverse-tapered insertion fitting against the holding surface of the tapered seed crystal. A jig, wherein two or more of the jigs are provided, and these jigs are provided at the same height of the main body of the holding jig and at equal intervals around the center axis. A jig for holding a seed crystal.
2 . 前記揷嵌具が、 引張り強度が 2 0 0 k g ί / c m 2以上で弾性係数 カ 2 0 0 0 k g f Z m m 2以下のものであるこ と を特徴とする請求項 1 に 記載の種結晶保持治具。 2. The seed crystal according to claim 1, wherein the fitting has a tensile strength of not less than 200 kgί / cm 2 and an elastic modulus of not more than 200 kgf Z mm 2. Holding jig.
3 . 前記揷嵌具が、 炭素繊維強化炭素複合材又は等方性焼結カーボンか らなるものであるこ とを特徴とする請求項 1又は請求項 2 に記載の種結晶 保持治具。 3. The seed crystal holding jig according to claim 1, wherein the metal fitting is made of carbon fiber reinforced carbon composite material or isotropic sintered carbon.
4 . 前記保持治具の本体が、 引張り 強度が 2 0 0 k g f / c m 2以上で 弹性係数が 8 0 0 k g f / m m 2以上のものであるこ とを特徴とする請求 項 1 ないし請求項 3 のいずれか一項に記載の種結晶保持治具。 4. The holding jig body according to claim 1, wherein the holding jig has a tensile strength of 200 kgf / cm 2 or more and a elasticity coefficient of 800 kgf / mm 2 or more. A seed crystal holding jig according to any one of the preceding claims.
5 . 前記保持治具の本体が、 炭素繊維強化炭素複合材、 強化等方性焼結 カーボン、 モリ ブデン又は少なく と もそれらのいずれかを含むものである こ と を特徴とする請求項 4に記載の種結晶保持治具。 5. The method according to claim 4, wherein the main body of the holding jig is made of carbon fiber reinforced carbon composite material, reinforced isotropic sintered carbon, molybdenum, or at least any one of them. Seed crystal holding jig.
6 . 種結晶のテーパーが付いた保持面に、 種結晶保持治具の逆のテーパ 一が付いた揷嵌具の端面を圧接させて前記種結晶を保持し、 チヨ クラルス キー法によ り 単結晶を製造する方法において、 種結晶と して、 前記テーパ 一が付いた 2つ以上の保持面が、 同じ高さに、 かつ中心軸の周 り に等間隔
で設けられている種結晶を用いる と と もに、 種結晶保持治具と して、 前記 種結晶の全ての保持面を圧接する挿嵌具を具備する保持治具を用いて種結 晶を保持し、 単結晶を引き上げるこ と を特徴とする単結晶の製造方法。
6. Hold the seed crystal by pressing the end face of the fitting with the reverse taper of the seed crystal holding jig against the tapered holding surface of the seed crystal, hold the seed crystal, and use the Chiyo Klarski method. In the method for producing a crystal, as a seed crystal, the two or more tapered holding surfaces are at the same height and are equally spaced around a central axis. In addition to using the seed crystal provided in the above, as a seed crystal holding jig, the seed crystal is formed by using a holding jig having an insertion fitting for pressing all the holding surfaces of the seed crystal. A method for producing a single crystal, comprising holding and pulling the single crystal.
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JP2002171071A JP4135405B2 (en) | 2002-06-12 | 2002-06-12 | Seed crystal holding jig and method for producing single crystal |
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JP2010173893A (en) * | 2009-01-29 | 2010-08-12 | Shin Etsu Handotai Co Ltd | Seed chuck of single crystal pulling device and method for producing single crystal |
JP5071406B2 (en) * | 2009-02-13 | 2012-11-14 | トヨタ自動車株式会社 | Composite bonding method of seed crystal for SiC single crystal growth by solution method |
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JPS4981950U (en) * | 1972-10-30 | 1974-07-16 | ||
JPS5560098A (en) * | 1978-10-26 | 1980-05-06 | Ricoh Co Ltd | Seed crystal holder |
JPS5637294A (en) * | 1979-09-05 | 1981-04-10 | Ricoh Co Ltd | Crystal seed supporting device |
JPS5924769U (en) * | 1982-08-05 | 1984-02-16 | 東北金属工業株式会社 | Seed crystal holding chuck |
JPH03174391A (en) * | 1989-12-01 | 1991-07-29 | Japan Steel Works Ltd:The | Seed crystal fitting structural body for growing single crystal and production thereof |
JPH0489558U (en) * | 1990-11-20 | 1992-08-05 | ||
JPH07144994A (en) * | 1993-11-24 | 1995-06-06 | Sanyo Electric Co Ltd | Production of single crystal |
EP0783047A1 (en) * | 1995-12-25 | 1997-07-09 | Shin-Etsu Handotai Company Limited | Crystal Pulling Apparatus |
EP0900862A1 (en) * | 1997-09-02 | 1999-03-10 | Shin-Etsu Handotai Company Limited | Seed crystal holder |
-
2002
- 2002-06-12 JP JP2002171071A patent/JP4135405B2/en not_active Expired - Fee Related
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2003
- 2003-06-10 WO PCT/JP2003/007319 patent/WO2003106742A1/en active Application Filing
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Publication number | Priority date | Publication date | Assignee | Title |
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JPS4981950U (en) * | 1972-10-30 | 1974-07-16 | ||
JPS5560098A (en) * | 1978-10-26 | 1980-05-06 | Ricoh Co Ltd | Seed crystal holder |
JPS5637294A (en) * | 1979-09-05 | 1981-04-10 | Ricoh Co Ltd | Crystal seed supporting device |
JPS5924769U (en) * | 1982-08-05 | 1984-02-16 | 東北金属工業株式会社 | Seed crystal holding chuck |
JPH03174391A (en) * | 1989-12-01 | 1991-07-29 | Japan Steel Works Ltd:The | Seed crystal fitting structural body for growing single crystal and production thereof |
JPH0489558U (en) * | 1990-11-20 | 1992-08-05 | ||
JPH07144994A (en) * | 1993-11-24 | 1995-06-06 | Sanyo Electric Co Ltd | Production of single crystal |
EP0783047A1 (en) * | 1995-12-25 | 1997-07-09 | Shin-Etsu Handotai Company Limited | Crystal Pulling Apparatus |
EP0900862A1 (en) * | 1997-09-02 | 1999-03-10 | Shin-Etsu Handotai Company Limited | Seed crystal holder |
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