WO2014073163A1 - Single-crystal manufacturing device - Google Patents
Single-crystal manufacturing device Download PDFInfo
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- WO2014073163A1 WO2014073163A1 PCT/JP2013/006043 JP2013006043W WO2014073163A1 WO 2014073163 A1 WO2014073163 A1 WO 2014073163A1 JP 2013006043 W JP2013006043 W JP 2013006043W WO 2014073163 A1 WO2014073163 A1 WO 2014073163A1
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- crucible
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
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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
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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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
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
Definitions
- the present invention relates to a single crystal manufacturing apparatus used when an oxide single crystal such as a sapphire single crystal is manufactured by a CZ method.
- Various growth methods such as the EFG method, the Bridgman method, and the Kyropoulos method are used to manufacture a sapphire single crystal that is in great demand as an LED substrate.
- a sapphire single crystal is grown using a crucible of a refractory metal (tungsten, molybdenum, etc.), but a c-axis crystal necessary for an LED substrate cannot be obtained.
- a process of obtaining a c-axis crystal by piercing the crystal from a right angle direction is necessary, and productivity and yield are extremely inferior.
- the Czochralski method has recently attracted attention because it allows c-axis crystal growth, and various crystal growth methods have been attempted using high-frequency induction heating or resistance heating methods.
- a growth furnace is configured with an iridium crucible and a zirconia heat insulating material, and iridium is very expensive. ing. Therefore, it is expected that the crucible is made of a refractory metal (tungsten, molybdenum, etc.) that is cheaper and versatile than iridium, and the cost is reduced by repeated use.
- Patent Document 1 discloses a method of supporting a molybdenum or tungsten crucible with an iridium crucible through a molybdenum or tungsten spacer.
- an expensive iridium crucible is used, there is a limit to cost reduction.
- Tungsten absorbs and carbides carbon at 850 ° C. to 1600 ° C., and molybdenum carbonizes at 1100 ° C. or higher. For this reason, even at a temperature lower than the melting point 2050 ° C. of aluminum oxide as a raw material, embrittlement and deformation due to carbonization are inevitable.
- the refractory metal crucible is made of a brittle material, but at high temperatures, the contact portion with the graphite material is accelerated due to carbonization, and deterioration such as cracks becomes remarkable. Therefore, the number of times the crucible is used has been remarkably reduced, and the production cost has been remarkably deteriorated.
- the present invention has been made in view of the above problems, and an object of the present invention is to provide an apparatus capable of improving the life of a crucible even when a graphite crucible holder is used in a single crystal manufacturing apparatus.
- the present invention is an apparatus for producing an oxide single crystal from a melt obtained by heating and melting a raw material in a crucible by the CZ method, and heating the raw material in the crucible And a main chamber in which the crucible is disposed, and the crucible is held by a refractory metal sacrificial material by a graphite holder. To do.
- the crucible will not directly contact the graphite holder, so cracks due to carbonization of the crucible etc. Deterioration can be suppressed, and the life of the crucible can be improved. Furthermore, the cost can be reduced by using a graphite holder. Therefore, it becomes an apparatus which can achieve the life improvement of a crucible simultaneously with cost reduction.
- the material of the crucible is mainly composed of at least one of tungsten, molybdenum, and tantalum. If it is such a crucible, since it is an inexpensive material, it becomes an apparatus which can reduce cost more.
- the heater is preferably a resistance heater.
- a resistance heater can be used in the apparatus of the present invention.
- the sacrificial material of the refractory metal is preferably composed mainly of at least one of tungsten, molybdenum, and tantalum. With such a sacrificial material, the device does not melt even at a high temperature and does not have a risk of contamination of the melt.
- the oxide single crystal is preferably a sapphire single crystal.
- the apparatus of the present invention can be an apparatus for the production of a sapphire single crystal.
- the sacrificial material of the refractory metal preferably has a thickness of 2 mm or more. If it is such thickness, it will become a device which can prevent carburization to a crucible certainly and can control degradation of a crucible more effectively.
- FIG. 1 is a schematic view of a single crystal production apparatus of the present invention.
- the single crystal production apparatus 10 of the present invention shown in FIG. 1 is an apparatus for producing an oxide single crystal 17 such as a sapphire single crystal from a melt 15 obtained by heating and melting a raw material in a crucible 14 by a CZ method. It is.
- the single crystal manufacturing apparatus 10 includes a heater 22 that heats the raw material in the crucible 14, a main chamber 11 in which the crucible 14 is disposed, and a pull chamber 13 that is connected to the main chamber 11 so as to be partitioned by a gate valve 12. It is provided.
- the apparatus 10 includes a gas introduction pipe 25 and a gas discharge pipe 26.
- a gas introduction pipe 25 For example, during normal times such as when a single crystal is grown, inert gas or the like is introduced into the furnace from above the pull chamber 13. The introduced gas can be discharged to the outside of the furnace from the gas discharge pipe 26 at the bottom of the main chamber 11 by a vacuum pump 27 or the like.
- the gate valve 12 is closed and the raw material charging or the like is performed in the pull chamber 13.
- the pull chamber 13 includes a gas exhaust pipe 28 and a gas introduction pipe 25 for the pull chamber. Can be used to perform gas replacement.
- the apparatus 10 supports a heat insulating material 16 such as a graphite-based felt material surrounding the crucible 14 and the heater 22, a pulling shaft 20 used for pulling up the single crystal 17, a seed holder 21 that holds a seed crystal, and the crucible 14.
- a graphite holder 18 and a crucible support shaft 19 that supports the crucible 14 via the graphite holder 18 are provided.
- the crucible 14 is held by a graphite holder 18 through a refractory metal sacrificial material 23.
- the sacrificial material 23 is inserted and set between the bottom of the crucible 14 and the upper surface of the graphite holder 18.
- the crucible 14 is held in a non-contact state by the graphite holder 18, and the crucible 14 Deterioration such as cracking due to carbonization can be prevented, and the life of the crucible 14 can be effectively improved.
- the thermal conductivity is good and the cost can be reduced. Accordingly, the life of the crucible 14 can be improved while reducing the cost.
- the graphite holder 18 is held so as to surround the side surface of the crucible 14, not only the bottom surface of the crucible 14 but also the side surface thereof is not in direct contact with the graphite holder 18 by the sacrificial material 23. Hold on.
- Fig. 2 shows an image of the state of crucible deterioration when it comes into contact with a graphite holder at a high temperature.
- FIG. 2 (a) when the crucible was directly held by the graphite holder, cracks occurred on the bottom of the crucible, making it difficult to use repeatedly.
- FIG. 2B when the graphite holder was in contact with the side surface of the crucible, it reacted, expanded and deformed. In the present invention, such crucible deterioration can be effectively prevented.
- the heater 22 is a resistance heater
- the material of the crucible 14 is a metal crucible containing at least one of tungsten, molybdenum, and tantalum as a main component.
- a high-frequency heater can be used as the heater 22 of the apparatus 10 of the present invention, and an iridium crucible can be used as the crucible 14, but in the present invention, an inexpensive crucible mainly composed of tungsten, molybdenum, or tantalum is used. Is preferred.
- the carbon heat insulating material 16 is used. Since carbon is a good conductor, the high-frequency heating method has poor thermal efficiency, and a resistance heater may be used. preferable. Thereby, cost can be further reduced.
- the refractory metal sacrificial material 23 is preferably composed mainly of at least one of tungsten, molybdenum, and tantalum. Such a sacrificial material 23 does not melt even at high temperatures, and there is no fear of contamination of the melt 15. At this time, the sacrificial material 23 is preferably made of a material different from the material of the crucible 14. If the same material is used, the sacrificial material 23 may be fused (diffusion welding) to the bottom of the crucible due to the diffusion welding phenomenon, so that different materials can further improve the life of the crucible 14, and the sacrificial material 23 is also used. It can be used repeatedly.
- the refractory metal sacrificial material 23 can be, for example, a disc-shaped material, and preferably has a thickness of 2 mm or more, particularly 3 mm or more. If it is such thickness, the carburizing to the crucible 14 can be prevented reliably and deterioration of the crucible 14 can be suppressed more effectively.
- the upper limit of the thickness of the sacrificial material 23 is not particularly limited. However, since the sacrificial material 23 needs to be replaced by observing the state of deterioration, for example, by setting the thickness to 20 mm or less, it is easy to handle. The increase in cost due to can be kept low.
- the crucible By producing an oxide single crystal such as a sapphire single crystal using the single crystal production apparatus of the present invention as described above, the crucible can be used repeatedly, so that the apparatus cost can be reduced and the production cost of the oxide single crystal can be reduced.
- Example and comparative examples Sapphire single crystals were produced using the single crystal production apparatus of the present invention shown in FIG.
- a tungsten and molybdenum disc (thickness 2 mm) was inserted between the bottom of a tungsten crucible and a graphite holder, and a molybdenum and tungsten disc (thickness). 2 mm) was inserted between the bottom of the molybdenum crucible and the graphite holder, and the crucible was confirmed for deterioration.
- the size of the crucible was 250 mm in outer diameter
- the diameter of the crucible bottom flat portion was 170 mm
- the height was 200 mm
- the size of the sacrificial disc was 160 mm in outer diameter and 2 mm in thickness. Further, the disc was inserted between the crucible bottom and the graphite holder in consideration of concentricity.
- Table 1 shows the results of confirming the deterioration status of the crucible bottom for each combination of the crucible material and the disc (sacrificial material) in the examples, and the results of confirming the degradation status of the crucible bottom in the comparative example.
- 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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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention provides a single-crystal manufacturing device that uses the Czochralski technique to manufacture a single oxide crystal from a molten liquid obtained by heating and melting a feedstock inside a crucible. Said single-crystal manufacturing device is provided with the following: a heater that heats the feedstock inside the crucible; and a main chamber in which the crucible is placed. This single-crystal manufacturing device is characterized in that the crucible is held by a graphite holding tool via a sacrificial material consisting of a metal having a high melting point. A single-crystal manufacturing device for manufacturing single oxide crystals in which the usable life of the crucible can be extended even with the use of a graphite holding tool is thus provided.
Description
本発明は、サファイア単結晶等の酸化物単結晶をCZ法により製造する際に用いる単結晶製造装置に関する。
The present invention relates to a single crystal manufacturing apparatus used when an oxide single crystal such as a sapphire single crystal is manufactured by a CZ method.
LED基板として需要が旺盛なサファイア単結晶の製造には、EFG法、ブリッジマン法、Kyropoulos法など様々な成長方法が使用されている。
最近主流となっているKyropoulos法では、高融点金属(タングステン、モリブデン等)のルツボを使用してサファイア単結晶を成長させているが、LED基板に必要なc軸結晶を得ることができず、この方法でa軸結晶を作製した後、直角方向から結晶を刳り貫いてc軸結晶を得る工程が必要で、生産性と歩留まりが著しく劣ることが課題となっている。 Various growth methods such as the EFG method, the Bridgman method, and the Kyropoulos method are used to manufacture a sapphire single crystal that is in great demand as an LED substrate.
In the Kyropoulos method which has become the mainstream recently, a sapphire single crystal is grown using a crucible of a refractory metal (tungsten, molybdenum, etc.), but a c-axis crystal necessary for an LED substrate cannot be obtained. After producing an a-axis crystal by this method, a process of obtaining a c-axis crystal by piercing the crystal from a right angle direction is necessary, and productivity and yield are extremely inferior.
最近主流となっているKyropoulos法では、高融点金属(タングステン、モリブデン等)のルツボを使用してサファイア単結晶を成長させているが、LED基板に必要なc軸結晶を得ることができず、この方法でa軸結晶を作製した後、直角方向から結晶を刳り貫いてc軸結晶を得る工程が必要で、生産性と歩留まりが著しく劣ることが課題となっている。 Various growth methods such as the EFG method, the Bridgman method, and the Kyropoulos method are used to manufacture a sapphire single crystal that is in great demand as an LED substrate.
In the Kyropoulos method which has become the mainstream recently, a sapphire single crystal is grown using a crucible of a refractory metal (tungsten, molybdenum, etc.), but a c-axis crystal necessary for an LED substrate cannot be obtained. After producing an a-axis crystal by this method, a process of obtaining a c-axis crystal by piercing the crystal from a right angle direction is necessary, and productivity and yield are extremely inferior.
そこで、チョクラルスキー法(CZ法)はc軸結晶成長が可能なため最近注目され、高周波誘導加熱や抵抗加熱方式を使い、種々の結晶成長方法が試みられている。高周波誘導加熱法を用いたCZ法では、イリジウムルツボと、ジルコニア製断熱材で成長炉を構成して結晶成長が行われているが、イリジウムが非常に高価なため結晶コスト低減の阻害要因となっている。そこで、イリジウムより安価で汎用性のある高融点金属(タングステン、モリブデン等)でルツボを製作し、繰り返し使用によるコスト低減が期待されている。
Therefore, the Czochralski method (CZ method) has recently attracted attention because it allows c-axis crystal growth, and various crystal growth methods have been attempted using high-frequency induction heating or resistance heating methods. In the CZ method using the high-frequency induction heating method, a growth furnace is configured with an iridium crucible and a zirconia heat insulating material, and iridium is very expensive. ing. Therefore, it is expected that the crucible is made of a refractory metal (tungsten, molybdenum, etc.) that is cheaper and versatile than iridium, and the cost is reduced by repeated use.
特許文献1には、モリブデン又はタングステンのスペーサーを介して、イリジウム製のルツボによりモリブデン製又はタングステン製のルツボを支持する方法が開示されている。しかし、高価なイリジウム製ルツボを使用するため、コスト低減には限界があった。
Patent Document 1 discloses a method of supporting a molybdenum or tungsten crucible with an iridium crucible through a molybdenum or tungsten spacer. However, since an expensive iridium crucible is used, there is a limit to cost reduction.
このため、単結晶製造装置において、炉内構成部品に黒鉛材を使用し、特に高融点金属ルツボを黒鉛材料で保持することがコスト低減や熱伝導性の点で有利である。
しかし、このような装置では、高融点金属材料はアルミナ等の原料の融点以下で炭化(浸炭)が進むため、ルツボに著しい劣化や変形が起こり、ライフが低下してしまうという問題を、本発明者らが見出した。 For this reason, in a single crystal manufacturing apparatus, it is advantageous in terms of cost reduction and thermal conductivity to use a graphite material for the in-furnace component, and particularly to hold a refractory metal crucible with a graphite material.
However, in such an apparatus, since the refractory metal material is carbonized (carburized) below the melting point of the raw material such as alumina, the crucible is significantly deteriorated and deformed, and the life is reduced. Found them.
しかし、このような装置では、高融点金属材料はアルミナ等の原料の融点以下で炭化(浸炭)が進むため、ルツボに著しい劣化や変形が起こり、ライフが低下してしまうという問題を、本発明者らが見出した。 For this reason, in a single crystal manufacturing apparatus, it is advantageous in terms of cost reduction and thermal conductivity to use a graphite material for the in-furnace component, and particularly to hold a refractory metal crucible with a graphite material.
However, in such an apparatus, since the refractory metal material is carbonized (carburized) below the melting point of the raw material such as alumina, the crucible is significantly deteriorated and deformed, and the life is reduced. Found them.
タングステンは、850℃~1600℃で、炭素を吸収、カーバイド化し、モリブデンは、1100℃以上で炭化してしまう。このため、原料である酸化アルミニウムの融点2050℃より低い温度でも、炭化による脆化や変形は避けられない。
Tungsten absorbs and carbides carbon at 850 ° C. to 1600 ° C., and molybdenum carbonizes at 1100 ° C. or higher. For this reason, even at a temperature lower than the melting point 2050 ° C. of aluminum oxide as a raw material, embrittlement and deformation due to carbonization are inevitable.
高融点金属ルツボは脆性材料で製作されるが、高温下では黒鉛材との接触部は炭化により脆化が加速され、ひび割れ等の劣化が顕著となる。従って、ルツボの使用回数は著しく低下し、生産コストを著しく悪化させていた。
The refractory metal crucible is made of a brittle material, but at high temperatures, the contact portion with the graphite material is accelerated due to carbonization, and deterioration such as cracks becomes remarkable. Therefore, the number of times the crucible is used has been remarkably reduced, and the production cost has been remarkably deteriorated.
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いて黒鉛製のルツボ保持具を用いても、ルツボのライフを向上できる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 an object of the present invention is to provide an apparatus capable of improving the life of a crucible even when a graphite crucible holder is used in a single crystal manufacturing apparatus.
上記目的を達成するために、本発明は、CZ法により、ルツボ内で原料を加熱溶融して得られた融液から酸化物単結晶を製造する装置であって、前記ルツボ内の原料を加熱するヒータと、前記ルツボを配置するメインチャンバーとを備え、前記ルツボは、黒鉛製保持具により高融点金属の犠牲材を介して保持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 is an apparatus for producing an oxide single crystal from a melt obtained by heating and melting a raw material in a crucible by the CZ method, and heating the raw material in the crucible And a main chamber in which the crucible is disposed, and the crucible is held by a refractory metal sacrificial material by a graphite holder. To do.
このように、ルツボが黒鉛製保持具により高融点金属の犠牲材を介して保持されたものであれば、ルツボが黒鉛製保持具に直接接触することがないため、ルツボの炭化によるひび割れ等の劣化を抑制することができ、ルツボのライフを向上できる。さらに、黒鉛製保持具を用いることで、コストを低減できる。従って、コスト低減と同時にルツボのライフ向上を達成できる装置となる。
In this way, if the crucible is held by a graphite holder through a refractory metal sacrificial material, the crucible will not directly contact the graphite holder, so cracks due to carbonization of the crucible etc. Deterioration can be suppressed, and the life of the crucible can be improved. Furthermore, the cost can be reduced by using a graphite holder. Therefore, it becomes an apparatus which can achieve the life improvement of a crucible simultaneously with cost reduction.
このとき、前記ルツボの材質は、タングステン、モリブデン、タンタルの少なくとも1つを主成分とするものであることが好ましい。
このようなルツボであれば、安価な材質であるため、コストをより低減できる装置となる。 At this time, it is preferable that the material of the crucible is mainly composed of at least one of tungsten, molybdenum, and tantalum.
If it is such a crucible, since it is an inexpensive material, it becomes an apparatus which can reduce cost more.
このようなルツボであれば、安価な材質であるため、コストをより低減できる装置となる。 At this time, it is preferable that the material of the crucible is mainly composed of at least one of tungsten, molybdenum, and tantalum.
If it is such a crucible, since it is an inexpensive material, it becomes an apparatus which can reduce cost more.
このとき、前記ヒータは、抵抗加熱ヒータであることが好ましい。
本発明の装置には、このような抵抗加熱ヒータを用いることができる。 At this time, the heater is preferably a resistance heater.
Such a resistance heater can be used in the apparatus of the present invention.
本発明の装置には、このような抵抗加熱ヒータを用いることができる。 At this time, the heater is preferably a resistance heater.
Such a resistance heater can be used in the apparatus of the present invention.
このとき、前記高融点金属の犠牲材は、タングステン、モリブデン、タンタルの少なくとも1つを主成分とするものであることが好ましい。
このような犠牲材であれば、高温においても溶けたりすることがなく、また、融液への汚染の恐れがない装置となる。 At this time, the sacrificial material of the refractory metal is preferably composed mainly of at least one of tungsten, molybdenum, and tantalum.
With such a sacrificial material, the device does not melt even at a high temperature and does not have a risk of contamination of the melt.
このような犠牲材であれば、高温においても溶けたりすることがなく、また、融液への汚染の恐れがない装置となる。 At this time, the sacrificial material of the refractory metal is preferably composed mainly of at least one of tungsten, molybdenum, and tantalum.
With such a sacrificial material, the device does not melt even at a high temperature and does not have a risk of contamination of the melt.
このとき、前記酸化物単結晶は、サファイア単結晶であることが好ましい。
本発明の装置は、サファイア単結晶の製造のための装置とすることができる。 At this time, the oxide single crystal is preferably a sapphire single crystal.
The apparatus of the present invention can be an apparatus for the production of a sapphire single crystal.
本発明の装置は、サファイア単結晶の製造のための装置とすることができる。 At this time, the oxide single crystal is preferably a sapphire single crystal.
The apparatus of the present invention can be an apparatus for the production of a sapphire single crystal.
このとき、前記高融点金属の犠牲材は、厚さが2mm以上であることが好ましい。
このような厚さであれば、ルツボへの浸炭を確実に防止して、ルツボの劣化をより効果的に抑制することができる装置となる。 At this time, the sacrificial material of the refractory metal preferably has a thickness of 2 mm or more.
If it is such thickness, it will become a device which can prevent carburization to a crucible certainly and can control degradation of a crucible more effectively.
このような厚さであれば、ルツボへの浸炭を確実に防止して、ルツボの劣化をより効果的に抑制することができる装置となる。 At this time, the sacrificial material of the refractory metal preferably has a thickness of 2 mm or more.
If it is such thickness, it will become a device which can prevent carburization to a crucible certainly and can control degradation of a crucible more effectively.
以上のように、本発明によれば、ルツボのライフ向上と装置のコスト低減を同時に達成できる。
As described above, according to the present invention, it is possible to simultaneously improve the crucible life and reduce the cost of the apparatus.
以下、本発明について、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概略図である。 Hereinafter, the present invention will be described in detail as an example of an embodiment with reference to the drawings, but the present invention is not limited thereto.
FIG. 1 is a schematic view of a single crystal production apparatus of the present invention.
図1は、本発明の単結晶製造装置の概略図である。 Hereinafter, the present invention will be described in detail as an example of an embodiment with reference to the drawings, but the present invention is not limited thereto.
FIG. 1 is a schematic view of a single crystal production apparatus of the present invention.
図1の本発明の単結晶製造装置10は、CZ法により、ルツボ14内で原料を加熱溶融して得られた融液15からサファイア単結晶等の酸化物単結晶17を引上げて製造する装置である。
単結晶製造装置10は、ルツボ14内の原料を加熱するヒータ22と、ルツボ14を配置するメインチャンバー11と、該メインチャンバー11上にゲートバルブ12で仕切り可能に接続されたプルチャンバー13とを備えたものである。 The singlecrystal production apparatus 10 of the present invention shown in FIG. 1 is an apparatus for producing an oxide single crystal 17 such as a sapphire single crystal from a melt 15 obtained by heating and melting a raw material in a crucible 14 by a CZ method. It is.
The singlecrystal manufacturing apparatus 10 includes a heater 22 that heats the raw material in the crucible 14, a main chamber 11 in which the crucible 14 is disposed, and a pull chamber 13 that is connected to the main chamber 11 so as to be partitioned by a gate valve 12. It is provided.
単結晶製造装置10は、ルツボ14内の原料を加熱するヒータ22と、ルツボ14を配置するメインチャンバー11と、該メインチャンバー11上にゲートバルブ12で仕切り可能に接続されたプルチャンバー13とを備えたものである。 The single
The single
また、図1に示すように、装置10は、ガス導入管25とガス排出管26を有し、例えば、単結晶成長時等の通常時はプルチャンバー13の上方から不活性ガス等を炉内にガス導入管25を介して導入し、この導入したガスを、メインチャンバー11の底部のガス排出管26から真空ポンプ27等により炉外へ排出することができる。一方、原料チャージ等の際には、ゲートバルブ12を閉めてプルチャンバー13内で原料チャージ等の作業を行い、その後、プルチャンバー13内をプルチャンバー用のガス排出管28とガス導入管25を用いてガス置換を実施できる。
Further, as shown in FIG. 1, the apparatus 10 includes a gas introduction pipe 25 and a gas discharge pipe 26. For example, during normal times such as when a single crystal is grown, inert gas or the like is introduced into the furnace from above the pull chamber 13. The introduced gas can be discharged to the outside of the furnace from the gas discharge pipe 26 at the bottom of the main chamber 11 by a vacuum pump 27 or the like. On the other hand, when charging the raw material or the like, the gate valve 12 is closed and the raw material charging or the like is performed in the pull chamber 13. Thereafter, the pull chamber 13 includes a gas exhaust pipe 28 and a gas introduction pipe 25 for the pull chamber. Can be used to perform gas replacement.
また、装置10は、ルツボ14やヒータ22を囲む黒鉛系フェルト材等の断熱材16と、単結晶17の引上げに用いる引上げ軸20と、種結晶を保持する種ホルダー21と、ルツボ14を支える黒鉛製保持具18と、ルツボ14を黒鉛製保持具18を介して支持するルツボ支持軸19とを備える。
In addition, the apparatus 10 supports a heat insulating material 16 such as a graphite-based felt material surrounding the crucible 14 and the heater 22, a pulling shaft 20 used for pulling up the single crystal 17, a seed holder 21 that holds a seed crystal, and the crucible 14. A graphite holder 18 and a crucible support shaft 19 that supports the crucible 14 via the graphite holder 18 are provided.
本発明の装置10において、ルツボ14は、黒鉛製保持具18により高融点金属の犠牲材23を介して保持されたものである。例えば、ルツボ14の底部と黒鉛製保持具18の上面との間に犠牲材23を挿入してセットする。
このように、ルツボ14が黒鉛製保持具18により高融点金属の犠牲材23を介して保持されたものであれば、ルツボ14が黒鉛製保持具18に非接触状態で保持され、ルツボ14の炭化によるひび割れ等の劣化を防止することができ、ルツボ14のライフを効果的に向上できる。さらに、ルツボ14を保持する保持具18を、黒鉛材やカーボンコンポジット材等を用いた黒鉛製とすることで、熱伝導性が良く、さらにはコストを低減できる。従って、コスト低減と同時にルツボ14のライフ向上を達成できる。ここで、黒鉛製保持具18がルツボ14の側面まで囲うように保持するものである場合は、犠牲材23によって、ルツボ14の底面のみならず、側面も黒鉛製保持具18と直接接触しないように保持する。 In theapparatus 10 of the present invention, the crucible 14 is held by a graphite holder 18 through a refractory metal sacrificial material 23. For example, the sacrificial material 23 is inserted and set between the bottom of the crucible 14 and the upper surface of the graphite holder 18.
Thus, if thecrucible 14 is held by the graphite holder 18 via the refractory metal sacrificial material 23, the crucible 14 is held in a non-contact state by the graphite holder 18, and the crucible 14 Deterioration such as cracking due to carbonization can be prevented, and the life of the crucible 14 can be effectively improved. Furthermore, by making the holder 18 that holds the crucible 14 made of graphite using a graphite material, a carbon composite material, or the like, the thermal conductivity is good and the cost can be reduced. Accordingly, the life of the crucible 14 can be improved while reducing the cost. Here, in the case where the graphite holder 18 is held so as to surround the side surface of the crucible 14, not only the bottom surface of the crucible 14 but also the side surface thereof is not in direct contact with the graphite holder 18 by the sacrificial material 23. Hold on.
このように、ルツボ14が黒鉛製保持具18により高融点金属の犠牲材23を介して保持されたものであれば、ルツボ14が黒鉛製保持具18に非接触状態で保持され、ルツボ14の炭化によるひび割れ等の劣化を防止することができ、ルツボ14のライフを効果的に向上できる。さらに、ルツボ14を保持する保持具18を、黒鉛材やカーボンコンポジット材等を用いた黒鉛製とすることで、熱伝導性が良く、さらにはコストを低減できる。従って、コスト低減と同時にルツボ14のライフ向上を達成できる。ここで、黒鉛製保持具18がルツボ14の側面まで囲うように保持するものである場合は、犠牲材23によって、ルツボ14の底面のみならず、側面も黒鉛製保持具18と直接接触しないように保持する。 In the
Thus, if the
図2に、高温下で黒鉛製保持具と接触した場合のルツボの劣化状況の画像を示す。図2(a)に示すように、ルツボを黒鉛製保持具に直接保持させた場合には、ルツボ底面にひび割れが生じて繰り返し使用が困難であった。また、図2(b)に示すように、ルツボの側面に黒鉛製保持具が接触した場合は、反応し、膨張して変形した。本発明では、このようなルツボの劣化を効果的に防止できる。
Fig. 2 shows an image of the state of crucible deterioration when it comes into contact with a graphite holder at a high temperature. As shown in FIG. 2 (a), when the crucible was directly held by the graphite holder, cracks occurred on the bottom of the crucible, making it difficult to use repeatedly. Further, as shown in FIG. 2B, when the graphite holder was in contact with the side surface of the crucible, it reacted, expanded and deformed. In the present invention, such crucible deterioration can be effectively prevented.
また、ヒータ22を抵抗加熱ヒータとし、ルツボ14の材質は、タングステン、モリブデン、タンタルの少なくとも1つを主成分とする金属ルツボであることが好ましい。
本発明の装置10のヒータ22としては、高周波加熱ヒータを用い、ルツボ14として、イリジウムルツボを用いることもできるが、本発明では、安価なタングステン、モリブデン、タンタルを主成分とするルツボを用いることが好ましい。この場合、イリジウムに比べて耐酸化性が低いため、カーボン製の断熱材16を使用することになり、カーボンは良導体であるため、高周波加熱方式では熱効率が悪く、抵抗加熱ヒータを使用することが好ましい。これにより、コストを更に低減することができる。 Moreover, it is preferable that theheater 22 is a resistance heater, and the material of the crucible 14 is a metal crucible containing at least one of tungsten, molybdenum, and tantalum as a main component.
A high-frequency heater can be used as theheater 22 of the apparatus 10 of the present invention, and an iridium crucible can be used as the crucible 14, but in the present invention, an inexpensive crucible mainly composed of tungsten, molybdenum, or tantalum is used. Is preferred. In this case, since the oxidation resistance is lower than that of iridium, the carbon heat insulating material 16 is used. Since carbon is a good conductor, the high-frequency heating method has poor thermal efficiency, and a resistance heater may be used. preferable. Thereby, cost can be further reduced.
本発明の装置10のヒータ22としては、高周波加熱ヒータを用い、ルツボ14として、イリジウムルツボを用いることもできるが、本発明では、安価なタングステン、モリブデン、タンタルを主成分とするルツボを用いることが好ましい。この場合、イリジウムに比べて耐酸化性が低いため、カーボン製の断熱材16を使用することになり、カーボンは良導体であるため、高周波加熱方式では熱効率が悪く、抵抗加熱ヒータを使用することが好ましい。これにより、コストを更に低減することができる。 Moreover, it is preferable that the
A high-frequency heater can be used as the
高融点金属の犠牲材23は、タングステン、モリブデン、タンタルの少なくとも1つを主成分とするものであることが好ましい。
このような犠牲材23であれば、高温においても溶けたりすることがなく、また、融液15への汚染の恐れがない。この際、ルツボ14の材質と異なる材質の犠牲材23とすることがより好ましい。同じ材質であると、拡散溶接現象にて犠牲材23がルツボ底に融着(拡散溶接)することがあるため、異なる材質同士の方がルツボ14のライフをより向上できるとともに、犠牲材23も繰り返し使用可能となる。 The refractory metalsacrificial material 23 is preferably composed mainly of at least one of tungsten, molybdenum, and tantalum.
Such asacrificial material 23 does not melt even at high temperatures, and there is no fear of contamination of the melt 15. At this time, the sacrificial material 23 is preferably made of a material different from the material of the crucible 14. If the same material is used, the sacrificial material 23 may be fused (diffusion welding) to the bottom of the crucible due to the diffusion welding phenomenon, so that different materials can further improve the life of the crucible 14, and the sacrificial material 23 is also used. It can be used repeatedly.
このような犠牲材23であれば、高温においても溶けたりすることがなく、また、融液15への汚染の恐れがない。この際、ルツボ14の材質と異なる材質の犠牲材23とすることがより好ましい。同じ材質であると、拡散溶接現象にて犠牲材23がルツボ底に融着(拡散溶接)することがあるため、異なる材質同士の方がルツボ14のライフをより向上できるとともに、犠牲材23も繰り返し使用可能となる。 The refractory metal
Such a
高融点金属の犠牲材23は、例えば円板状のものとすることができ、また、厚さが2mm以上、特には3mm以上であることが好ましい。
このような厚さであれば、ルツボ14への浸炭を確実に防止して、ルツボ14の劣化をより効果的に抑制することができる。このとき、犠牲材23の厚さの上限は特に限定されないが、犠牲材23は劣化の様子を観察して交換する必要があるので、例えば厚さを20mm以下とすることで、取り扱い易く、交換によるコストの上昇も低く抑えることができる。 The refractory metalsacrificial material 23 can be, for example, a disc-shaped material, and preferably has a thickness of 2 mm or more, particularly 3 mm or more.
If it is such thickness, the carburizing to thecrucible 14 can be prevented reliably and deterioration of the crucible 14 can be suppressed more effectively. At this time, the upper limit of the thickness of the sacrificial material 23 is not particularly limited. However, since the sacrificial material 23 needs to be replaced by observing the state of deterioration, for example, by setting the thickness to 20 mm or less, it is easy to handle. The increase in cost due to can be kept low.
このような厚さであれば、ルツボ14への浸炭を確実に防止して、ルツボ14の劣化をより効果的に抑制することができる。このとき、犠牲材23の厚さの上限は特に限定されないが、犠牲材23は劣化の様子を観察して交換する必要があるので、例えば厚さを20mm以下とすることで、取り扱い易く、交換によるコストの上昇も低く抑えることができる。 The refractory metal
If it is such thickness, the carburizing to the
以上のような本発明の単結晶製造装置を用いてサファイア単結晶等の酸化物単結晶を製造することで、ルツボを繰り返し使用できるため、装置コストを低減でき、酸化物単結晶の製造コスト低減に資する。
By producing an oxide single crystal such as a sapphire single crystal using the single crystal production apparatus of the present invention as described above, the crucible can be used repeatedly, so that the apparatus cost can be reduced and the production cost of the oxide single crystal can be reduced. Contribute to
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)
図1に示す本発明の単結晶製造装置を用いてサファイア単結晶製造を行った。
実施例として、タングステン製及びモリブデン製円板(厚さ2mm)を、タングステン製ルツボの底部と黒鉛製保持具との間に挿入してセットした場合と、モリブデン製及びタングステン製円板(厚さ2mm)を、モリブデン製ルツボの底部と黒鉛製保持具との間に挿入してセットした場合の、ルツボの劣化を確認した。 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)
Sapphire single crystals were produced using the single crystal production apparatus of the present invention shown in FIG.
As an example, a tungsten and molybdenum disc (thickness 2 mm) was inserted between the bottom of a tungsten crucible and a graphite holder, and a molybdenum and tungsten disc (thickness). 2 mm) was inserted between the bottom of the molybdenum crucible and the graphite holder, and the crucible was confirmed for deterioration.
(実施例、比較例)
図1に示す本発明の単結晶製造装置を用いてサファイア単結晶製造を行った。
実施例として、タングステン製及びモリブデン製円板(厚さ2mm)を、タングステン製ルツボの底部と黒鉛製保持具との間に挿入してセットした場合と、モリブデン製及びタングステン製円板(厚さ2mm)を、モリブデン製ルツボの底部と黒鉛製保持具との間に挿入してセットした場合の、ルツボの劣化を確認した。 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)
Sapphire single crystals were produced using the single crystal production apparatus of the present invention shown in FIG.
As an example, a tungsten and molybdenum disc (thickness 2 mm) was inserted between the bottom of a tungsten crucible and a graphite holder, and a molybdenum and tungsten disc (thickness). 2 mm) was inserted between the bottom of the molybdenum crucible and the graphite holder, and the crucible was confirmed for deterioration.
また、比較例として、タングステン製及びモリブデン製ルツボを、黒鉛製保持具で直接保持した以外は実施例と同様に、単結晶製造を行い、ルツボの劣化を確認した。
As a comparative example, single crystal production was performed in the same manner as in Example except that tungsten and molybdenum crucibles were directly held by a graphite holder, and deterioration of the crucible was confirmed.
このとき、ルツボのサイズは、外径250mm、ルツボ底平面部直径170mm、高さ200mmとし、犠牲材である円板のサイズは、外径160mm、厚さ2mmとした。また、円板を、ルツボ底と黒鉛製保持具との間に同心性に配慮して挿入した。
At this time, the size of the crucible was 250 mm in outer diameter, the diameter of the crucible bottom flat portion was 170 mm, and the height was 200 mm, and the size of the sacrificial disc was 160 mm in outer diameter and 2 mm in thickness. Further, the disc was inserted between the crucible bottom and the graphite holder in consideration of concentricity.
表1は、実施例において、ルツボの材質と円板(犠牲材)の材質の組み合わせ毎のルツボ底の劣化状況を確認した結果と、比較例においてルツボ底の劣化状況を確認した結果である。
Table 1 shows the results of confirming the deterioration status of the crucible bottom for each combination of the crucible material and the disc (sacrificial material) in the examples, and the results of confirming the degradation status of the crucible bottom in the comparative example.
円板を介して保持した実施例の場合、引上げ終了後のルツボ底の状態を観察すると、ルツボ底の劣化は見られなかった。
円板を敷いていない比較例の場合、1バッチでもルツボ底面の変化が大きく、ひび割れ、変形等の劣化が見られた。 In the case of the example held through the disc, when the state of the crucible bottom after the completion of the pulling was observed, no deterioration of the crucible bottom was observed.
In the case of the comparative example in which no disc was laid, the change in the bottom of the crucible was large even in one batch, and deterioration such as cracks and deformation was observed.
円板を敷いていない比較例の場合、1バッチでもルツボ底面の変化が大きく、ひび割れ、変形等の劣化が見られた。 In the case of the example held through the disc, when the state of the crucible bottom after the completion of the pulling was observed, no deterioration of the crucible bottom was observed.
In the case of the comparative example in which no disc was laid, the change in the bottom of the crucible was large even in one batch, and deterioration such as cracks and deformation was observed.
また、モリブデンルツボにモリブデン製の円板を挿入した場合、ルツボの劣化は見られなかったが拡散溶接現象にて円板がルツボ底に融着した場合もあった。従って、ルツボと円板(犠牲材)の材質が異なる方が、安定的に使えることがわかる。
Also, when a molybdenum disc was inserted into the molybdenum crucible, the crucible was not deteriorated, but the disc was sometimes fused to the bottom of the crucible due to the diffusion welding phenomenon. Therefore, it can be seen that the crucible and the disc (sacrificial material) of different materials can be used stably.
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 (7)
- CZ法により、ルツボ内で原料を加熱溶融して得られた融液から酸化物単結晶を製造する装置であって、
前記ルツボ内の原料を加熱するヒータと、前記ルツボを配置するメインチャンバーとを備え、
前記ルツボは、黒鉛製保持具により高融点金属の犠牲材を介して保持されたものであることを特徴とする単結晶製造装置。 An apparatus for producing an oxide single crystal from a melt obtained by heating and melting a raw material in a crucible by a CZ method,
A heater for heating the raw material in the crucible, and a main chamber in which the crucible is arranged,
The crucible is held by a refractory metal sacrificial material by a graphite holder, and the single crystal manufacturing apparatus according to claim 1. - 前記ルツボの材質は、タングステン、モリブデン、タンタルの少なくとも1つを主成分とする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。 The single crystal manufacturing apparatus according to claim 1, wherein the material of the crucible is mainly composed of at least one of tungsten, molybdenum, and tantalum.
- 前記ヒータは、抵抗加熱ヒータ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。 The single crystal manufacturing apparatus according to claim 1 or 2, wherein the heater is a resistance heater.
- 前記高融点金属の犠牲材は、タングステン、モリブデン、タンタルの少なくとも1つを主成分とするもの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。 The single crystal manufacturing apparatus according to any one of claims 1 to 3, wherein the sacrificial material of the refractory metal contains at least one of tungsten, molybdenum, and tantalum as a main component. .
- 前記高融点金属の犠牲材の材質は、前記ルツボの材質と異なるものであることを特徴とする請求項1乃至請求項4のいずれか一項に記載の単結晶製造装置。 The single crystal manufacturing apparatus according to any one of claims 1 to 4, wherein a material of the sacrificial material of the refractory metal is different from a material of the crucible.
- 前記酸化物単結晶は、サファイア単結晶であることを特徴とする請求項1乃至請求項5のいずれか一項に記載の単結晶製造装置。 The single crystal manufacturing apparatus according to any one of claims 1 to 5, wherein the oxide single crystal is a sapphire single crystal.
- 前記高融点金属の犠牲材は、厚さが2mm以上であることを特徴とする請求項1乃至請求項6のいずれか一項に記載の単結晶製造装置。 The single crystal manufacturing apparatus according to any one of claims 1 to 6, wherein the refractory metal sacrificial material has a thickness of 2 mm or more.
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WO (1) | WO2014073163A1 (en) |
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AT15378U1 (en) * | 2016-02-05 | 2017-07-15 | Plansee Se | crucible |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61247683A (en) * | 1985-04-23 | 1986-11-04 | Seiko Epson Corp | Pulling device for single crystal sapphire |
JP2005001934A (en) * | 2003-06-11 | 2005-01-06 | Daiichi Kiden:Kk | Apparatus for pulling and growing sapphire single crystal |
WO2011062092A1 (en) * | 2009-11-20 | 2011-05-26 | 昭和電工株式会社 | Single crystal pulling apparatus |
WO2011074533A1 (en) * | 2009-12-17 | 2011-06-23 | 昭和電工株式会社 | Single crystal pulling apparatus and single crystal pulling method |
JP2011195423A (en) * | 2010-03-24 | 2011-10-06 | Sumitomo Metal Mining Co Ltd | Method of manufacturing sapphire single crystal |
-
2012
- 2012-11-06 JP JP2012244780A patent/JP2014091670A/en active Pending
-
2013
- 2013-10-10 WO PCT/JP2013/006043 patent/WO2014073163A1/en active Application Filing
- 2013-10-23 TW TW102138293A patent/TW201422858A/en unknown
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61247683A (en) * | 1985-04-23 | 1986-11-04 | Seiko Epson Corp | Pulling device for single crystal sapphire |
JP2005001934A (en) * | 2003-06-11 | 2005-01-06 | Daiichi Kiden:Kk | Apparatus for pulling and growing sapphire single crystal |
WO2011062092A1 (en) * | 2009-11-20 | 2011-05-26 | 昭和電工株式会社 | Single crystal pulling apparatus |
WO2011074533A1 (en) * | 2009-12-17 | 2011-06-23 | 昭和電工株式会社 | Single crystal pulling apparatus and single crystal pulling method |
JP2011195423A (en) * | 2010-03-24 | 2011-10-06 | Sumitomo Metal Mining Co Ltd | Method of manufacturing sapphire single crystal |
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JP2014091670A (en) | 2014-05-19 |
TW201422858A (en) | 2014-06-16 |
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