WO2010089816A1 - Apparatus for manufacturing single crystal - Google Patents

Apparatus for manufacturing single crystal Download PDF

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Publication number
WO2010089816A1
WO2010089816A1 PCT/JP2009/005552 JP2009005552W WO2010089816A1 WO 2010089816 A1 WO2010089816 A1 WO 2010089816A1 JP 2009005552 W JP2009005552 W JP 2009005552W WO 2010089816 A1 WO2010089816 A1 WO 2010089816A1
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Prior art keywords
wire
seed
single crystal
tip
pulling
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PCT/JP2009/005552
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French (fr)
Japanese (ja)
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森隆
岩崎淳
井上七夫
石橋政範
石本弘幸
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信越半導体株式会社
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Publication of WO2010089816A1 publication Critical patent/WO2010089816A1/en

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/32Seed holders, e.g. chucks

Definitions

  • the present invention relates to a single crystal manufacturing apparatus for manufacturing a single crystal by pulling a seed crystal from a polycrystalline melt with a seed wire by the Czochralski method.
  • This CZ method is a method of manufacturing a single crystal by melting a polycrystalline raw material, fusing a seed crystal into a polycrystalline melt, and then pulling it up, and using a shaft as a means for pulling up the single crystal And a method using a seed wire.
  • a method of pulling with a seed wire uses a tungsten wire, stainless steel wire, molybdenum wire or the like that has excellent heat resistance and high strength.
  • the diameter of a CZ method silicon single crystal has increased, the weight of the single crystal has increased, and in the case of a seed wire, a thicker one is usually used according to the increase in the weight of the single crystal.
  • Patent Document 1 describes that thermal degradation is reduced by covering a region exposed to a high temperature of the seed wire with a collar. However, even with this method, local degradation of the seed wire occurs, which is insufficient to extend the replacement cycle.
  • the present invention has been made in view of the above problems, and by extending the replacement cycle of the seed wire for pulling up the single crystal in the single crystal manufacturing apparatus, the cost is reduced, the quality loss is small and the weight is high.
  • An object of the present invention is to provide an apparatus for producing a single crystal capable of producing a single crystal with high yield.
  • the present invention provides a single crystal manufacturing apparatus that pulls a seed crystal held by a seed chuck with a seed wire when pulling the single crystal by the Czochralski method.
  • An upper end of a tip wire is connected to the lower end, and the seed chuck is coupled to the lower end of the tip wire.
  • the tip wire By connecting the tip wire between the seed wire and the seed chuck, it is lowered to the vicinity of the high-temperature melt at the initial stage of pulling the single crystal.
  • the tip wire will be located. For this reason, the local thermal deterioration of the seed wire is suppressed, and the seed wire replacement cycle can be effectively extended.
  • replacement of the tip wire does not require disassembly of the wire winding part, and the length of the tip wire to be replaced is shorter than that of the seed wire, so the cost is greatly reduced, and the tip wire is short. Therefore, the initial elongation after replacement is small, and there is almost no quality loss due to tip wire replacement.
  • the single crystal manufacturing apparatus of the present invention it is possible to manufacture a single crystal having a high yield with reduced cost, low quality loss, and high yield.
  • the seed wire is connected so as to be positioned in a region of 700 ° C. or lower when the single crystal is pulled.
  • the tip wire By connecting the tip wire to the region where the temperature becomes higher than 700 ° C. and oxidation proceeds rapidly in this way, the seed wire is positioned in a region where the seed wire is 700 ° C. or lower when the single crystal is pulled.
  • the local thermal deterioration of the seed wire can be more reliably suppressed, and the replacement cycle can be further extended.
  • hook metal fittings are provided at both ends of the tip wire and the lower end of the seed wire, and the upper end of the tip wire is connected to the lower end of the seed wire via a wire joint.
  • the material of the seed wire and the material of the tip wire can be one selected from tungsten, stainless steel, and molybdenum.
  • these metals and alloys can be used as appropriate.
  • the single crystal manufacturing apparatus of the present invention since the replacement cycle of the seed wire is extended, the cost can be reduced, the quality loss can be reduced, and a heavy single crystal can be manufactured with a high yield.
  • Patent Document 1 discloses a method of covering a seed wire with a collar.
  • the heat conduction from the joint portion with the seed chuck leads to local thermal deterioration of the joint portion which is particularly apt to break due to concentration of stress, thereby extending the seed wire replacement cycle.
  • FIG. 3 shows a connecting portion between a conventional seed wire and a seed chuck.
  • the seed chuck 32 on which the seed crystal 34 is held and the seed wire 31 are coupled by a hook fitting 33.
  • the vicinity of the tip of the seed wire 31 close to the melt is exposed to a particularly high temperature and the thermal deterioration progresses. Further, stress concentrates at the joint portion with the seed chuck 32. It has been found that it is easy to break.
  • the tip wire can be easily exchanged between the seed chuck and the seed wire, so that local thermal deterioration of the seed wire can be suppressed, so that the replacement cycle can be extended.
  • the present invention has been completed by finding that the replacement cost can be reduced and that quality loss hardly occurs.
  • FIG. 1 is a schematic view showing an example of an embodiment of the single crystal production apparatus of the present invention.
  • 2A is a partially enlarged view showing an example of an embodiment of the single crystal production apparatus of the present invention
  • FIG. 2B is a plan view and a side view of a wire joint.
  • a single crystal pulling apparatus 12 shown in FIG. 1 includes, for example, a crucible 17 that stores a silicon melt, and rotates a seed chuck 14 that holds a seed crystal 15, a seed wire 13 that pulls up the seed chuck 14, and a seed wire 13. Or it is comprised from the wire winding part 11 to wind up.
  • a heater 10 for heating the melt in the crucible 17 is disposed around the crucible 17 so that the single crystal 16 is pulled up.
  • the silicon polycrystal is heated by the heater 10 to a melting point or higher in the crucible 17 to be melted, and the seed wire 13. And the tip of the seed crystal 15 is brought into contact with or immersed in the center of the melt.
  • the crucible 17 is rotated in an appropriate direction, the seed wire 13 is wound while being wound, and the seed crystal 15 held by the seed chuck 14 is pulled up to start growing the single crystal 16. Thereafter, a substantially cylindrical growth single crystal can be obtained by appropriately controlling the pulling rate and temperature.
  • the upper end of the tip wire 19 is connected to the lower end of the seed wire 13, and the seed chuck 14 is coupled to the lower end of the tip wire 19.
  • the tip wire is lowered to near the high-temperature melt at the initial stage of pulling the single crystal, and further due to heat conduction from the seed chuck,
  • the tip wire is located in a region where the heat deterioration proceeds. For this reason, the local thermal deterioration of the seed wire positioned on the tip wire is suppressed, and the seed wire replacement cycle can be effectively extended.
  • the tip wire is subject to thermal degradation, the cost of the tip wire itself is significantly lower than that of the seed wire because the cost of the tip wire itself is reduced because it does not require disassembly of the wire winding part. Can be reduced. Furthermore, since the tip wire is short, the initial elongation after replacement is small and the pulling speed deviation can be negligibly small, so there is almost no quality loss due to tip wire replacement.
  • the seed wire 13 is connected so as to be positioned in a region of 700 ° C. or lower when the single crystal is pulled.
  • the tip wire By connecting the tip wire in a region where the temperature is higher than 700 ° C. and the oxidation proceeds rapidly in this way, the seed wire becomes 700 ° C. or less, so that local thermal deterioration is more effectively suppressed.
  • the seed wire exchange cycle can be further extended.
  • a certain distance from the melt surface becomes a high-temperature region. Therefore, in order to connect the tip wire so that the seed wire is located in a region where the seed wire is 700 ° C. or less even in the initial stage of pulling, Is required.
  • the length of the tip wire 19 is not particularly limited, but it is preferable that there is almost no loss of quality of the single crystal due to initial elongation and that the wire joint can be attached and detached.
  • the thickness is preferably 30 mm or more and less than 200 mm.
  • the length of the seed wire is 5000 mm or more, if the tip wire has a length in the above range, the elongation is very small compared to the time of replacement of the entire seed wire, and it is short, so it is inexpensive. Even if it is exchanged, the cost will not increase that much.
  • the tip wire has such a length, the seed wire can be kept at a temperature of 700 ° C. or lower because the seed wire is sufficiently separated from the melt even at the initial stage of pulling.
  • hook metal fittings 20 and 21 are provided at both ends of the tip wire 19 and the lower end of the seed wire 13, and the upper end of the tip wire 19 is connected to the lower end of the seed wire 13 via the wire joint 18. It is preferred that The hooks 20 and 21 are inserted into the wire joint 18 through a wire on the side surface of the wire joint 18 as shown in FIG. .
  • the single crystal manufacturing apparatus of the present invention can be easily configured without using a special apparatus. This can be easily performed without disassembling the winding part.
  • the material of the seed wire 13 and the material of the tip wire 19 are not particularly limited.
  • one type selected from tungsten, stainless steel, and molybdenum can be used.
  • these metals and alloys can be used as appropriate. That is, according to the present invention, since a wire material conventionally used can be applied, it is possible to avoid an increase in cost in this respect as well.
  • the tip wire material since the tip wire is separate from the seed wire, the tip wire material is different from the seed wire material, or the tip wire is thicker than the seed wire. It is possible to lower the replacement frequency of the tip wire itself by using a material having higher heat resistance and strength.
  • the single crystal manufacturing apparatus of the present invention it is possible to manufacture a high-weight single crystal with a low yield, a low quality loss, and a high yield.
  • Example and comparative examples The tip wire was connected to the seed wire via a wire joint to prepare a single crystal manufacturing apparatus as shown in FIGS.
  • a seed wire as shown in FIG. 3 was directly connected to the seed chuck by a hook and a single crystal manufacturing apparatus similar to the example was prepared (comparative example).
  • Tungsten with the same diameter of 2.5 mm was used as the material of the seed wire and the tip wire of these single crystal manufacturing apparatuses.
  • both seed wires were 5000 mm in length, and the length of the tip wire was 100 mm. In this case, the tip wire when the seed crystal is brought into contact with the silicon melt is positioned in the temperature range of 700 to 800 ° C.
  • the breaking strength was the tensile strength at the time of breaking in the tensile test as shown in FIG.
  • the tip of the seed wire (about 250 mm) is used as a test piece, the upper side of the test piece is chucked and the lower end of the test piece (hanging metal fitting) is pulled downward at a speed of 10 mm / min.
  • the tensile strength was measured when it was pulled and broken. The measurement results are shown in FIG.
  • the operation time to reach the breaking strength as a guide for replacement was about 6000 hours in the comparative example and about 12000 hours in the example.
  • the exchange cycle can be extended to about twice that of the conventional one, and the quality loss of the single crystal due to the initial elongation of the seed wire that occurs at each exchange can be reduced to about one half. Can do.
  • the present invention is not limited to the above embodiment.
  • the above-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.

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

Abstract

Provided is an apparatus for manufacturing single crystals, wherein a seed crystal held by a seed chuck is pulled using a seed wire at the time of pulling a single crystal by the Czochralski method.  The upper end of a leading end wire is connected to the lower end of the seed wire, and the seed chuck is connected to the lower end of the leading end wire.  Thus, by extending the replacement cycle of the seed wire which pulls the single crystal in the apparatus for manufacturing single crystals, cost is reduced, and the single crystals having a small quality loss and high weight can be manufactured with a high yield.

Description

単結晶製造装置Single crystal manufacturing equipment
 本発明は、チョクラルスキー法によってシードワイヤーで種結晶を多結晶の融液から引上げることにより単結晶を製造する単結晶製造装置に関する。
 
The present invention relates to a single crystal manufacturing apparatus for manufacturing a single crystal by pulling a seed crystal from a polycrystalline melt with a seed wire by the Czochralski method.
 従来、半導体シリコン単結晶等の単結晶材料はチョクラルスキー法(以下、CZ法という。)によって、棒状単結晶として得る方法が広く用いられている。
 このCZ法は、多結晶原料を融解し、種結晶を多結晶の融液に融着した後引上げることにより単結晶を製造する方法であり、単結晶を引上げる手段として、シャフトを用いる方法とシードワイヤーを用いる方法とがある。
Conventionally, a method of obtaining a single crystal material such as a semiconductor silicon single crystal as a rod-shaped single crystal by the Czochralski method (hereinafter referred to as CZ method) has been widely used.
This CZ method is a method of manufacturing a single crystal by melting a polycrystalline raw material, fusing a seed crystal into a polycrystalline melt, and then pulling it up, and using a shaft as a means for pulling up the single crystal And a method using a seed wire.
 CZ法による単結晶製造において、シードワイヤーで引上げる方法では、耐熱性に優れ、高強度のタングステンワイヤーやステンレススチールワイヤーあるいはモリブデンワイヤー等が使用されている。近年、CZ法シリコン単結晶の大口径化と共に、単結晶の高重量化が進んでおり、シードワイヤーの場合、単結晶の高重量化に応じて太いものを使用するのが通常である。 In single crystal production by the CZ method, a method of pulling with a seed wire uses a tungsten wire, stainless steel wire, molybdenum wire or the like that has excellent heat resistance and high strength. In recent years, as the diameter of a CZ method silicon single crystal has increased, the weight of the single crystal has increased, and in the case of a seed wire, a thicker one is usually used according to the increase in the weight of the single crystal.
 また、このような単結晶を引き上げるシードワイヤーは、操業中に高温にさらされており、操業時間の経過に伴い熱劣化するため、交換サイクルを設定して定期的にシードワイヤーの交換を行う。このシードワイヤーの交換は種結晶を保持するシードチャックを取外した後、ワイヤー巻き取り部を分解して実施される。
 しかし、シードワイヤーは高価であり、その交換もワイヤー巻取り部の分解を要するため、コストのかかるものである。また、シードワイヤーは交換初期の段階で伸びが生じるため、実際の引き上げ速度とワイヤー巻き取り速度とにずれが生じ、交換の度に単結晶の品質ロスが発生する。このため、これらのような問題を軽減するためにシードワイヤーの交換サイクルを延ばすことが望まれていた。また、引き上げる単結晶の高重量化に伴い、シードワイヤーが融液近くで高温になっている時にもある程度の荷重がシードワイヤーにかかって破断の可能性もあるため、さらに交換サイクルが短くなっていた。
In addition, such a seed wire for pulling up a single crystal is exposed to a high temperature during operation and thermally deteriorates as the operation time elapses. Therefore, an exchange cycle is set to periodically replace the seed wire. The replacement of the seed wire is performed by removing the seed chuck holding the seed crystal and then disassembling the wire winding portion.
However, since the seed wire is expensive and its replacement requires the disassembly of the wire winding portion, it is expensive. In addition, since the seed wire is elongated at the initial stage of exchange, a deviation occurs between the actual pulling speed and the wire winding speed, and the quality of the single crystal is lost at each exchange. For this reason, in order to reduce such problems, it has been desired to extend the replacement cycle of the seed wire. In addition, as the weight of the single crystal to be pulled increases, even when the seed wire is near the melt and is hot, a certain amount of load is applied to the seed wire and it may break, so the replacement cycle is further shortened. It was.
 このような問題に対して、特許文献1にはシードワイヤーの高温にさらされる領域をカラーで覆うことにより、熱劣化を低減することが記載されている。
 しかし、このような方法でもシードワイヤーの局所的な劣化は発生してしまい、交換サイクルを延ばすには不十分であった。
 
In order to solve such a problem, Patent Document 1 describes that thermal degradation is reduced by covering a region exposed to a high temperature of the seed wire with a collar.
However, even with this method, local degradation of the seed wire occurs, which is insufficient to extend the replacement cycle.
特開2005-119891号公報JP 2005-119891 A
 本発明は、上記問題点に鑑みてなされたものであって、単結晶製造装置における単結晶の引き上げを行うシードワイヤーの交換サイクルを延ばすことにより、コストが低減されて、品質ロスが少なく高重量の単結晶を歩留まり良く製造することができる単結晶製造装置を提供することを目的とする。 The present invention has been made in view of the above problems, and by extending the replacement cycle of the seed wire for pulling up the single crystal in the single crystal manufacturing apparatus, the cost is reduced, the quality loss is small and the weight is high. An object of the present invention is to provide an apparatus for producing a single crystal capable of producing a single crystal with high yield.
 上記目的を達成するために、本発明は、少なくとも、チョクラルスキー法により単結晶を引き上げる際にシードチャックで保持された種結晶をシードワイヤーで引き上げる単結晶製造装置であって、前記シードワイヤーの下端に先端ワイヤーの上端が連結され、前記先端ワイヤーの下端に前記シードチャックが結合されたものであることを特徴とする単結晶製造装置を提供する。 In order to achieve the above object, the present invention provides a single crystal manufacturing apparatus that pulls a seed crystal held by a seed chuck with a seed wire when pulling the single crystal by the Czochralski method. An upper end of a tip wire is connected to the lower end, and the seed chuck is coupled to the lower end of the tip wire.
 シードワイヤーとシードチャックの間に先端ワイヤーを連結することにより、単結晶引き上げ初期には高温の融液近くまで下がり、さらにはシードチャックからの熱伝導によって、特に高温になり熱劣化が進む領域に先端ワイヤーが位置することになる。このためシードワイヤーは局所的な熱劣化が抑制され、シードワイヤーの交換サイクルを効果的に延ばすことができる。また、先端ワイヤーの交換にはワイヤー巻き取り部の分解等が不要であり、交換される先端ワイヤーの長さは、シードワイヤーに比べて短いので大幅にコストが低減され、さらには先端ワイヤーは短いので交換後の初期伸びも小さく先端ワイヤー交換による品質ロスはほとんど無い。
 以上より、本発明の単結晶製造装置によれば、コストが低減され、品質ロスが少なく、高重量の単結晶を歩留まり良く製造することができる。
By connecting the tip wire between the seed wire and the seed chuck, it is lowered to the vicinity of the high-temperature melt at the initial stage of pulling the single crystal. The tip wire will be located. For this reason, the local thermal deterioration of the seed wire is suppressed, and the seed wire replacement cycle can be effectively extended. Also, replacement of the tip wire does not require disassembly of the wire winding part, and the length of the tip wire to be replaced is shorter than that of the seed wire, so the cost is greatly reduced, and the tip wire is short. Therefore, the initial elongation after replacement is small, and there is almost no quality loss due to tip wire replacement.
As described above, according to the single crystal manufacturing apparatus of the present invention, it is possible to manufacture a single crystal having a high yield with reduced cost, low quality loss, and high yield.
 このとき、前記シードワイヤーが、前記単結晶引き上げの際に700℃以下となる領域に位置するように連結されたものであることが好ましい。
 このように温度が700℃より高くなり、急激に酸化が進む領域に先端ワイヤーが位置するように連結することで、シードワイヤーが単結晶引き上げの際に700℃以下となる領域に位置するようになり、シードワイヤーの局所的熱劣化をより確実に抑制することができ、その交換サイクルもより延ばすことができる。
At this time, it is preferable that the seed wire is connected so as to be positioned in a region of 700 ° C. or lower when the single crystal is pulled.
By connecting the tip wire to the region where the temperature becomes higher than 700 ° C. and oxidation proceeds rapidly in this way, the seed wire is positioned in a region where the seed wire is 700 ° C. or lower when the single crystal is pulled. Thus, the local thermal deterioration of the seed wire can be more reliably suppressed, and the replacement cycle can be further extended.
 このとき、前記先端ワイヤーの両端と前記シードワイヤーの下端に引っ掛け金具を有し、前記シードワイヤーの下端に前記先端ワイヤーの上端がワイヤージョイントを介して連結されたものであることが好ましい。
 このように、ワイヤージョイントを介して、引っ掛け金具により連結することで、特別な装置を用いなくても簡単に本発明の単結晶製造装置を構成することができ、さらには先端ワイヤーの交換を簡便に行うことができる。
At this time, it is preferable that hook metal fittings are provided at both ends of the tip wire and the lower end of the seed wire, and the upper end of the tip wire is connected to the lower end of the seed wire via a wire joint.
Thus, by connecting with a hook metal fitting through a wire joint, the single crystal manufacturing apparatus of the present invention can be easily configured without using a special apparatus, and the tip wire can be easily replaced. Can be done.
 このとき、前記シードワイヤーの材質、及び、前記先端ワイヤーの材質を、タングステン、ステンレススチール、モリブデンの内から選択される1種とすることができる。
 本発明のシードワイヤー、先端ワイヤーの材質としては、これらの金属、合金を適宜用いることができる。
At this time, the material of the seed wire and the material of the tip wire can be one selected from tungsten, stainless steel, and molybdenum.
As materials for the seed wire and the tip wire of the present invention, these metals and alloys can be used as appropriate.
 以上のように、本発明の単結晶製造装置によれば、シードワイヤーの交換サイクルが延びるため、コストが低減され、また品質ロスが少なく、高重量の単結晶を歩留まり良く製造することができる。
 
As described above, according to the single crystal manufacturing apparatus of the present invention, since the replacement cycle of the seed wire is extended, the cost can be reduced, the quality loss can be reduced, and a heavy single crystal can be manufactured with a high yield.
本発明の単結晶製造装置の実施態様の一例を示す概略図である。It is the schematic which shows an example of the embodiment of the single crystal manufacturing apparatus of this invention. (A)本発明の単結晶製造装置の部分拡大図及び、(B)ワイヤージョイントの平面図と側面図である。(A) The elements on larger scale of the single-crystal manufacturing apparatus of this invention, (B) The top view and side view of a wire joint. 従来の単結晶製造装置のシードワイヤーとシードチャックの結合部分を説明するための説明図である。It is explanatory drawing for demonstrating the coupling | bond part of the seed wire and seed chuck | zipper of the conventional single crystal manufacturing apparatus. シードワイヤーの破断強度の操業時間での推移を示すグラフである。It is a graph which shows transition in the operation time of breaking strength of a seed wire. 引っ張り試験を説明するための説明図である。It is explanatory drawing for demonstrating a tension test.
 単結晶製造装置のシードワイヤーの交換を行う際にシードワイヤー交換に伴うコストや品質ロスが生じてしまうため、これらの問題を低減するために、シードワイヤーの交換サイクルを延ばす方法が求められていた。
 これに対して、特許文献1では、シードワイヤーをカラーで覆う方法が開示されている。しかし、このような方法でも、シードチャックとの結合部分からの熱伝導により、特に応力が集中して破断し易い結合部分の局所的な熱劣化が進んでしまい、シードワイヤーの交換サイクルを延ばすには不十分であった。
Costs and quality loss associated with seed wire replacement occur when replacing the seed wire of a single crystal manufacturing apparatus, and in order to reduce these problems, a method of extending the seed wire replacement cycle was required. .
On the other hand, Patent Document 1 discloses a method of covering a seed wire with a collar. However, even in such a method, the heat conduction from the joint portion with the seed chuck leads to local thermal deterioration of the joint portion which is particularly apt to break due to concentration of stress, thereby extending the seed wire replacement cycle. Was insufficient.
 これに対して、本発明者らは鋭意検討して、以下のことを見出した。
 図3に従来のシードワイヤーとシードチャックの結合部分を示す。図3に示すように、種結晶34が保持されたシードチャック32とシードワイヤー31とは、引っ掛け金具33で結合される。このような場合に、融液に近くなるシードワイヤー31の先端付近が特に高温にさらされて熱劣化が進み、さらに、シードチャック32との結合部分では応力が集中するため、結合部分の付近が破断し易くなることを見出した。
On the other hand, the present inventors diligently studied and found the following.
FIG. 3 shows a connecting portion between a conventional seed wire and a seed chuck. As shown in FIG. 3, the seed chuck 32 on which the seed crystal 34 is held and the seed wire 31 are coupled by a hook fitting 33. In such a case, the vicinity of the tip of the seed wire 31 close to the melt is exposed to a particularly high temperature and the thermal deterioration progresses. Further, stress concentrates at the joint portion with the seed chuck 32. It has been found that it is easy to break.
 これに対して、シードチャックとシードワイヤーの間に先端ワイヤーを交換容易に連結することにより、シードワイヤーの局所的な熱劣化を抑制することができるため交換サイクルを延ばすことができ、また先端ワイヤーの交換であれば、交換時のコストを低減できるとともに、品質ロスもほとんど生じないことを見出して、本発明を完成させた。 In contrast, the tip wire can be easily exchanged between the seed chuck and the seed wire, so that local thermal deterioration of the seed wire can be suppressed, so that the replacement cycle can be extended. Thus, the present invention has been completed by finding that the replacement cost can be reduced and that quality loss hardly occurs.
 以下、本発明の単結晶製造装置について、実施態様の一例として、図を参照しながら詳細に説明するが、本発明はこれに限定されるものではない。
 図1は、本発明の単結晶製造装置の実施態様の一例を示す概略図である。図2は、(A)本発明の単結晶製造装置の実施態様の一例を示す部分拡大図と(B)ワイヤージョイントの平面図と側面図である。
Hereinafter, the single crystal production apparatus of the present invention will be described in detail as an example of an embodiment with reference to the drawings. However, the present invention is not limited to this.
FIG. 1 is a schematic view showing an example of an embodiment of the single crystal production apparatus of the present invention. 2A is a partially enlarged view showing an example of an embodiment of the single crystal production apparatus of the present invention, and FIG. 2B is a plan view and a side view of a wire joint.
 図1に示す単結晶引上げ装置12は、例えばシリコン融液を収容するルツボ17を配置し、種結晶15を保持するシードチャック14と、シードチャック14を引き上げるシードワイヤー13と、シードワイヤー13を回転または巻き取るワイヤー巻取り部11とから構成されている。また、ルツボ17の周囲にはルツボ17内の融液を加熱するためのヒータ10を配置して単結晶16を引上げる構造になっている。 A single crystal pulling apparatus 12 shown in FIG. 1 includes, for example, a crucible 17 that stores a silicon melt, and rotates a seed chuck 14 that holds a seed crystal 15, a seed wire 13 that pulls up the seed chuck 14, and a seed wire 13. Or it is comprised from the wire winding part 11 to wind up. In addition, a heater 10 for heating the melt in the crucible 17 is disposed around the crucible 17 so that the single crystal 16 is pulled up.
 このような単結晶引上げ装置12によりチョクラルスキー法を用いて例えばシリコン単結晶を製造するには、ルツボ17内でシリコンの多結晶を融点以上にヒータ10により加熱して融解し、シードワイヤー13を巻き出して種結晶15の先端を融液の中心に接触又は浸漬させる。次いで、ルツボ17を適宜の方向に回転させると共に、シードワイヤー13を回転させながら巻取り、シードチャック14で保持された種結晶15を引き上げることにより単結晶16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を得ることができる。 In order to manufacture, for example, a silicon single crystal using the Czochralski method by such a single crystal pulling apparatus 12, the silicon polycrystal is heated by the heater 10 to a melting point or higher in the crucible 17 to be melted, and the seed wire 13. And the tip of the seed crystal 15 is brought into contact with or immersed in the center of the melt. Next, the crucible 17 is rotated in an appropriate direction, the seed wire 13 is wound while being wound, and the seed crystal 15 held by the seed chuck 14 is pulled up to start growing the single crystal 16. Thereafter, a substantially cylindrical growth single crystal can be obtained by appropriately controlling the pulling rate and temperature.
 そして、本発明の単結晶製造装置12は、シードワイヤー13の下端に先端ワイヤー19の上端が連結され、先端ワイヤー19の下端にシードチャック14が結合されたものである。
 このように、シードワイヤーとシードチャックの間に先端ワイヤーを連結することにより、先端ワイヤーは単結晶引き上げ初期には高温の融液近くまで下げられ、さらにはシードチャックからの熱伝導によって、特に高温になり熱劣化が進む領域に先端ワイヤーが位置することになる。このため先端ワイヤーの上に位置するシードワイヤーは局所的な熱劣化が抑制され、シードワイヤーの交換サイクルを効果的に延ばすことができる。また、先端ワイヤーは熱劣化することになるが、その交換にはワイヤー巻き取り部の分解等が不要であるためコストが低減され、また短いので、先端ワイヤー自体の価格もシードワイヤーに比べ大幅に低減できる。さらには先端ワイヤーは短いので、交換後の初期伸びも小さく引き上げ速度のずれも無視できるほど小さくできるので先端ワイヤー交換による品質ロスはほとんど無い。
In the single crystal manufacturing apparatus 12 of the present invention, the upper end of the tip wire 19 is connected to the lower end of the seed wire 13, and the seed chuck 14 is coupled to the lower end of the tip wire 19.
In this way, by connecting the tip wire between the seed wire and the seed chuck, the tip wire is lowered to near the high-temperature melt at the initial stage of pulling the single crystal, and further due to heat conduction from the seed chuck, The tip wire is located in a region where the heat deterioration proceeds. For this reason, the local thermal deterioration of the seed wire positioned on the tip wire is suppressed, and the seed wire replacement cycle can be effectively extended. In addition, although the tip wire is subject to thermal degradation, the cost of the tip wire itself is significantly lower than that of the seed wire because the cost of the tip wire itself is reduced because it does not require disassembly of the wire winding part. Can be reduced. Furthermore, since the tip wire is short, the initial elongation after replacement is small and the pulling speed deviation can be negligibly small, so there is almost no quality loss due to tip wire replacement.
 このとき、シードワイヤー13が、単結晶引き上げの際に700℃以下となる領域に位置するように連結されたものであることが好ましい。
 このように温度が700℃より高くなり、急激に酸化が進む領域に先端ワイヤーが位置するように連結することで、シードワイヤーが700℃以下となるため、局所的熱劣化をより効果的に抑制することができ、シードワイヤーの交換サイクルをより延ばすことができる。単結晶引き上げ時には融液面から一定距離は高温の領域になるため、引き上げ初期にもシードワイヤーが700℃以下となる領域に位置するように先端ワイヤーが連結されるためには、先端ワイヤーがある程度の長さが必要である。
At this time, it is preferable that the seed wire 13 is connected so as to be positioned in a region of 700 ° C. or lower when the single crystal is pulled.
By connecting the tip wire in a region where the temperature is higher than 700 ° C. and the oxidation proceeds rapidly in this way, the seed wire becomes 700 ° C. or less, so that local thermal deterioration is more effectively suppressed. The seed wire exchange cycle can be further extended. When the single crystal is pulled, a certain distance from the melt surface becomes a high-temperature region. Therefore, in order to connect the tip wire so that the seed wire is located in a region where the seed wire is 700 ° C. or less even in the initial stage of pulling, Is required.
 この先端ワイヤー19の長さとしては、特に限定されないが、初期伸びによる単結晶の品質ロスがほとんど無く、かつ、ワイヤージョイントとの着脱が可能な範囲とすることが好ましく、そのような範囲の長さとして30mm以上200mm未満が好ましい。通常、シードワイヤーの長さが5000mm以上であるため、上記範囲の長さの先端ワイヤーであれば、シードワイヤー全体の交換時に比べて伸びは非常に小さく、また短いので安価であり、定期的に交換しても、コストはそれ程上昇しない。また先端ワイヤーがこのような範囲の長さであれば、引き上げ初期でもシードワイヤーが融液と十分に離れた位置になるためシードワイヤーを700℃以下とすることができる。 The length of the tip wire 19 is not particularly limited, but it is preferable that there is almost no loss of quality of the single crystal due to initial elongation and that the wire joint can be attached and detached. The thickness is preferably 30 mm or more and less than 200 mm. Usually, since the length of the seed wire is 5000 mm or more, if the tip wire has a length in the above range, the elongation is very small compared to the time of replacement of the entire seed wire, and it is short, so it is inexpensive. Even if it is exchanged, the cost will not increase that much. If the tip wire has such a length, the seed wire can be kept at a temperature of 700 ° C. or lower because the seed wire is sufficiently separated from the melt even at the initial stage of pulling.
 このとき、図2に示すような、先端ワイヤー19の両端とシードワイヤー13の下端に引っ掛け金具20、21を有し、シードワイヤー13の下端に先端ワイヤー19の上端がワイヤージョイント18を介して連結されたものであることが好ましい。
 図2(B)に示すようなワイヤージョイント18の側面の溝にワイヤーを通して、引っ掛け金具20、21をワイヤージョイント18内に入れることで、図2(A)のような状態で簡便に連結される。
 このようなワイヤージョイントを介して、引っ掛け金具により連結することで、特別な装置を用いなくても本発明の単結晶製造装置を簡単に構成することができ、さらには先端ワイヤーの交換を、ワイヤー巻き取り部の解体等をすることなく簡便に行うことができる。
At this time, as shown in FIG. 2, hook metal fittings 20 and 21 are provided at both ends of the tip wire 19 and the lower end of the seed wire 13, and the upper end of the tip wire 19 is connected to the lower end of the seed wire 13 via the wire joint 18. It is preferred that
The hooks 20 and 21 are inserted into the wire joint 18 through a wire on the side surface of the wire joint 18 as shown in FIG. .
By connecting with a hook metal fitting through such a wire joint, the single crystal manufacturing apparatus of the present invention can be easily configured without using a special apparatus. This can be easily performed without disassembling the winding part.
 また、シードワイヤー13の材質、及び、先端ワイヤー19の材質としては、特に限定されないが、例えば、タングステン、ステンレススチール、モリブデンの内から選択される1種を用いることできる。
 本発明のシードワイヤー、先端ワイヤーの材質としては、これらの金属、合金を適宜用いることができる。すなわち、本発明は、ワイヤー材質として従来より用いられているものを適用することができるので、この点においても、コスト高となることを回避できる。そして、本発明では、先端ワイヤーはシードワイヤーとは別体であるため、先端ワイヤーの材質を、シードワイヤーの材質とは異なるものを用いたり、あるいは先端ワイヤーの方がシードワイヤーより径が太いものを用いることとして、より耐熱性や強度の高いものを用い、先端ワイヤー自体の交換頻度を下げることが可能である。
Further, the material of the seed wire 13 and the material of the tip wire 19 are not particularly limited. For example, one type selected from tungsten, stainless steel, and molybdenum can be used.
As materials for the seed wire and the tip wire of the present invention, these metals and alloys can be used as appropriate. That is, according to the present invention, since a wire material conventionally used can be applied, it is possible to avoid an increase in cost in this respect as well. In the present invention, since the tip wire is separate from the seed wire, the tip wire material is different from the seed wire material, or the tip wire is thicker than the seed wire. It is possible to lower the replacement frequency of the tip wire itself by using a material having higher heat resistance and strength.
 以上より、本発明の単結晶製造装置によればコストが低減されて、品質ロスが少なく、高重量の単結晶を歩留まり良く製造することができる。
 
As described above, according to the single crystal manufacturing apparatus of the present invention, it is possible to manufacture a high-weight single crystal with a low yield, a low quality loss, and a high yield.
 以下、実施例及び比較例を示して本発明をより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。
(実施例、比較例)
 シードワイヤーにワイヤージョイントを介して先端ワイヤーを連結して、図1、2に示すような単結晶製造装置を用意した(実施例)。
 また、従来のように、図3に示すようなシードワイヤーをシードチャックに引っ掛け金具で直接結合させ、その他は実施例と同じ単結晶製造装置を用意した(比較例)。
 これらの単結晶製造装置のシードワイヤー、先端ワイヤーの材質としては同じ径の直径2.5mmのタングステンを用いた。また、どちらのシードワイヤーも長さ5000mmで、先端ワイヤーの長さは100mmとした。この場合、種結晶をシリコン融液に接触させた時の先端ワイヤーは700~800℃の温度領域に位置するようになる。
EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated more concretely, this invention is not limited to these.
(Examples and comparative examples)
The tip wire was connected to the seed wire via a wire joint to prepare a single crystal manufacturing apparatus as shown in FIGS.
In addition, as in the prior art, a seed wire as shown in FIG. 3 was directly connected to the seed chuck by a hook and a single crystal manufacturing apparatus similar to the example was prepared (comparative example).
Tungsten with the same diameter of 2.5 mm was used as the material of the seed wire and the tip wire of these single crystal manufacturing apparatuses. Moreover, both seed wires were 5000 mm in length, and the length of the tip wire was 100 mm. In this case, the tip wire when the seed crystal is brought into contact with the silicon melt is positioned in the temperature range of 700 to 800 ° C.
 二つの単結晶製造装置を用いて、直径200mm、重量140kgの単結晶引き上げを行い、シードワイヤーの破断強度と操業時間の関係を調べた。
 破断強度は、図5に示すような引っ張り試験において破断した時の引っ張り強度とした。測定方法としては、図5に示すように、シードワイヤーの先端部(約250mm)を試験片として、試験片上側をチャッキング固定し、試験片下端(引っ掛け金具)を下方に引っ張り速度10mm/minで引っ張り、破断した時の引っ張り強度を測定した。測定結果を図4に示す。
Using two single crystal manufacturing apparatuses, a single crystal having a diameter of 200 mm and a weight of 140 kg was pulled, and the relationship between the breaking strength of the seed wire and the operation time was examined.
The breaking strength was the tensile strength at the time of breaking in the tensile test as shown in FIG. As a measuring method, as shown in FIG. 5, the tip of the seed wire (about 250 mm) is used as a test piece, the upper side of the test piece is chucked and the lower end of the test piece (hanging metal fitting) is pulled downward at a speed of 10 mm / min. The tensile strength was measured when it was pulled and broken. The measurement results are shown in FIG.
 図4からわかるように、交換目安とした破断強度に達するまでの操業時間が、比較例は約6000時間であり、実施例は約12000時間であった。このため、本発明によれば、交換サイクルを従来の約2倍に延ばすことができ、交換の度に発生するシードワイヤーの初期伸びによる単結晶の品質ロスを約2分の1に低減することができる。 As can be seen from FIG. 4, the operation time to reach the breaking strength as a guide for replacement was about 6000 hours in the comparative example and about 12000 hours in the example. For this reason, according to the present invention, the exchange cycle can be extended to about twice that of the conventional one, and the quality loss of the single crystal due to the initial elongation of the seed wire that occurs at each exchange can be reduced to about one half. Can do.
 なお、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-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.

Claims (4)

  1.  少なくとも、チョクラルスキー法により単結晶を引き上げる際にシードチャックで保持された種結晶をシードワイヤーで引き上げる単結晶製造装置であって、前記シードワイヤーの下端に先端ワイヤーの上端が連結され、前記先端ワイヤーの下端に前記シードチャックが結合されたものであることを特徴とする単結晶製造装置。
     
    At least a single crystal manufacturing apparatus for pulling up a seed crystal held by a seed chuck with a seed wire when pulling up the single crystal by the Czochralski method, wherein an upper end of a tip wire is connected to a lower end of the seed wire, and the tip A single crystal manufacturing apparatus, wherein the seed chuck is coupled to a lower end of a wire.
  2.  前記シードワイヤーが、前記単結晶引き上げの際に700℃以下となる領域に位置するように連結されたものであることを特徴とする請求項1に記載の単結晶製造装置。
     
    2. The single crystal manufacturing apparatus according to claim 1, wherein the seed wire is connected so as to be positioned in a region of 700 ° C. or lower when the single crystal is pulled.
  3.  前記先端ワイヤーの両端と前記シードワイヤーの下端に引っ掛け金具を有し、前記シードワイヤーの下端に前記先端ワイヤーの上端がワイヤージョイントを介して連結されたものであることを特徴とする請求項1又は請求項2に記載の単結晶製造装置。
     
    2. A hook fitting is provided at both ends of the tip wire and the lower end of the seed wire, and the upper end of the tip wire is connected to the lower end of the seed wire via a wire joint. The single crystal manufacturing apparatus according to claim 2.
  4.  前記シードワイヤーの材質、及び、前記先端ワイヤーの材質が、タングステン、ステンレススチール、モリブデンの内から選択される1種であることを特徴とする請求項1乃至請求項3のいずれか一項に記載の単結晶製造装置。 4. The material according to claim 1, wherein a material of the seed wire and a material of the tip wire are one selected from tungsten, stainless steel, and molybdenum. 5. Single crystal manufacturing equipment.
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