JPH08175896A - Method and device for producing single crystal - Google Patents
Method and device for producing single crystalInfo
- Publication number
- JPH08175896A JPH08175896A JP33544794A JP33544794A JPH08175896A JP H08175896 A JPH08175896 A JP H08175896A JP 33544794 A JP33544794 A JP 33544794A JP 33544794 A JP33544794 A JP 33544794A JP H08175896 A JPH08175896 A JP H08175896A
- Authority
- JP
- Japan
- Prior art keywords
- crystal
- crucible
- heat reflector
- radiant heat
- single crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 4
- 239000000956 alloy Substances 0.000 claims abstract description 4
- 239000000155 melt Substances 0.000 claims description 28
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 230000006698 induction Effects 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 2
- 230000001939 inductive effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 5
- -1 platinum group metals Chemical group 0.000 description 5
- 239000011810 insulating material Substances 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 4
- 229910001260 Pt alloy Chemical group 0.000 description 3
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 3
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910018967 Pt—Rh Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000012943 hotmelt Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は単結晶、特に酸化物単結
晶の製造に適した方法及び装置に関する。FIELD OF THE INVENTION The present invention relates to a method and apparatus suitable for producing single crystals, especially oxide single crystals.
【０００２】[0002]
【従来の技術】従来、高周波加熱方式の単結晶引き上げ
法により、ＬｉＮｂＯ3 やＬｉＴａＯ3 といった割れ易
い単結晶を育成する場合、特公昭５６−２７４７６号、
特公昭５７−５０７５６号等に示されているようなドー
ム状の放射熱反射体を使用していた。また結晶の長尺化
に関しては特公昭６１−５４４０号、特公昭６１−２６
５１９号、特公昭５８−２５０７８号等に示されている
ように、ルツボとコイルの相対位置を育成の進行に応じ
て変えて育成を行っていた。これらの技術は次に述べる
ように結晶育成に必要な温度勾配を適正に保つための技
術である。2. Description of the Related Art Conventionally, when a fragile single crystal such as LiNbO 3 or LiTaO 3 is grown by a high frequency heating single crystal pulling method, Japanese Patent Publication No. 56-27476,
A dome-shaped radiant heat reflector as disclosed in Japanese Examined Patent Publication No. S57-50756 was used. Regarding the lengthening of the crystal, Japanese Examined Patent Publication No. 61-5440 and Japanese Examined Patent Publication No.
As shown in No. 519 and Japanese Patent Publication No. 58-25078, the relative positions of the crucible and the coil were changed according to the progress of the growing. These techniques are techniques for properly maintaining the temperature gradient required for crystal growth as described below.
【０００３】[0003]
【発明が解決しようとする課題】特公昭５６−２７４７
６号等のようにドーム状の放射熱反射体を用いた場合、
結晶平行長（結晶引き上げ軸の方向の長さ）が１．０ｄ
〜２．０ｄ（ｄは単結晶直径）以上に成長させると結晶
外形の変形が発生し、それ以上に長い結晶育成が不可能
であった。この欠点を補うために、特公昭６１−５４４
０号等のようにルツボに対するコイルの相対位置を育成
に応じて変える方法を用いた場合、育成条件が非常に複
雑になり、条件設定のための労力が過大となる上、コイ
ルに低速駆動系を設ける必要があった。したがって、本
発明の目的は、これらの欠点を解決して、ＬｉＮｂＯ
3 、ＬｉＴａＯ3 などのクラックや曲がりの生じ易い酸
化物系等の結晶の充分に長い単結晶を製造する方法及び
装置を提供することにある。[Problems to be Solved by the Invention] Japanese Patent Publication No. 56-2747
When using a dome-shaped radiant heat reflector like No. 6,
Crystal parallel length (length in the direction of the crystal pulling axis) is 1.0d
When the crystal was grown to a diameter of ˜2.0 d (d is the diameter of a single crystal) or more, the outer shape of the crystal was deformed, and it was impossible to grow a crystal longer than that. In order to make up for this drawback, Japanese Patent Publication No. 61-544
When the method of changing the relative position of the coil to the crucible according to the growth such as No. 0 is used, the growing condition becomes very complicated, the labor for setting the condition becomes excessive, and the coil has a low speed drive system. Had to be provided. Therefore, an object of the present invention is to solve these drawbacks and to provide LiNbO
It is an object of the present invention to provide a method and an apparatus for producing a sufficiently long single crystal of an oxide-based crystal or the like in which cracks or bending easily occur such as 3 , LiTaO 3 .
【０００４】[0004]
【課題を解決するための手段】本発明者は、上記問題点
を解決するために鋭意研究した結果、ドーム状の放射熱
反射体の代わりに、放射熱反射体の位置を融液の残存量
に依存して修正することを試みた結果、上記した方法で
は得られない長い単結晶が得られることを見い出して本
発明を完成するに至った。すなわち、本発明の単結晶成
長方法は、融液を収容するルツボと、該融液を加熱する
加熱手段と、前記ルツボ内の融液に種子結晶を接触さ
せ、その種子結晶を引き上げて単結晶を製造する方法に
おいて、ルツボの上方に設置した放射熱反射体を結晶引
き上げに伴い上昇させることを特徴とする。本発明はま
たこのような方法を実施するために使用する単結晶成長
装置を提供するもので、ルツボの上方に設けた放射熱反
射体と、単結晶の引き上げにつれてこれを上昇する手段
とを設けたことを特徴とする。以下に説明するように、
本発明によると結晶引き上げ部の放射熱勾配が適正に保
持できるので、変形やクラックの発生がない長い単結晶
が生成できる。As a result of intensive studies to solve the above-mentioned problems, the present inventor has found that instead of the dome-shaped radiant heat reflector, the position of the radiant heat reflector is used to determine the residual amount of the melt. As a result of attempting to modify depending on the above, it was found that a long single crystal which could not be obtained by the above method was obtained, and the present invention was completed. That is, the single crystal growth method of the present invention, a crucible for containing a melt, heating means for heating the melt, a seed crystal is brought into contact with the melt in the crucible, and the seed crystal is pulled up to a single crystal. In the method for manufacturing the above, the radiant heat reflector installed above the crucible is raised as the crystal is pulled up. The present invention also provides a single crystal growth apparatus used for carrying out such a method, which comprises a radiant heat reflector provided above the crucible and means for raising the radiant heat reflector as the single crystal is pulled up. It is characterized by that. As explained below,
According to the present invention, the radiant heat gradient of the crystal pulling portion can be appropriately maintained, so that a long single crystal free from deformation and cracks can be produced.
【０００５】[0005]
【作用】従来、結晶径の２倍以上の平行長を有する単結
晶の成育が困難であった主な原因は、育成初期と後期の
温度勾配が変化することであった。この点を図４を参照
して説明すると、従来例１の曲線に示すように、育成初
期において適正な育成条件に設定してある場合には、結
晶の成長につれて融液の量が減少するに従い、融液直上
の温度勾配は小さくなる。これは、融液の高さが低くな
り、露出したルツボ周囲壁が反射板として作用して融液
直上の温度勾配を小さくすることが原因である。特に加
熱手段が誘導加熱の場合には融液の高さが低くなると、
露出したルツボ周壁がアフターヒータとしても作用し融
液直上の温度勾配を小さくすることが原因である。つま
り、育成初期を適当な温度勾配に保つと結晶化が進むに
従って温度勾配が小さくなり、育成後期には結晶化の際
の凝固放射熱を充分に放散することができなくなり、結
晶の曲がりとなって現れる。また図４の従来例２の曲線
のように、育成後期に結晶が曲がらない条件で育成する
と、育成初期の温度勾配が大きくなり過ぎ、結晶にクラ
ックが発生し、育成に適さなくなる。In the past, the main cause of difficulty in growing a single crystal having a parallel length twice or more the crystal diameter was that the temperature gradient in the early and late stages of growth changed. This point will be described with reference to FIG. 4. As shown in the curve of Conventional Example 1, when the proper growth conditions are set in the initial stage of growth, the amount of melt decreases as the crystal grows. , The temperature gradient directly above the melt becomes smaller. This is because the height of the melt becomes low and the exposed peripheral wall of the crucible acts as a reflector to reduce the temperature gradient directly above the melt. Especially when the heating means is induction heating and the height of the melt becomes low,
The reason is that the exposed peripheral wall of the crucible also acts as an after-heater and reduces the temperature gradient directly above the melt. In other words, if the initial growth is kept at an appropriate temperature gradient, the temperature gradient becomes smaller as the crystallization progresses, and the solidification radiant heat during crystallization cannot be sufficiently dissipated in the latter half of the growth, resulting in the bending of the crystal. Appears. Further, when the crystal is grown under the condition that the crystal is not bent in the latter stage of the growth as shown by the curve of Conventional Example 2 in FIG. 4, the temperature gradient in the initial stage of the growth becomes too large, and the crystal is cracked and becomes unsuitable for the growth.
【０００６】そこで、本発明はこの問題を解決するため
に、ルツボの上方に放射熱反射体を配置し、これを結晶
引き上げに伴い上昇させ、育成初期と後期の温度勾配差
を小さくすることにより、図４の実施例の曲線のよう
に、結晶育成の進行により融液の残量が減少しても、温
度勾配が余り変化せず適正な成長条件を長時間保持で
き、その結果長尺結晶を育成できるようにしたものであ
る。すなわち、 １）育成初期には放射熱反射体が融液に非常に近い位置
にあるため、放射熱反射体によって融液へ反射される放
射熱放射が大きくなり、温度勾配を小さくする。 ２）育成が進むと放射熱反射体は融液表面から離れ、融
液付近の温度勾配には影響を与えない。 ３）放射熱反射体が高温の融液側とホットゾーン上部と
の間を遮蔽するため、放射熱反射体より上部の放射熱の
放散が良くなり、引き上げ軸を通しての放射熱伝導量が
増大する。 このうち、上記１）の効果により、放射熱反射体がない
場合では温度勾配が大き過ぎて育成に不適当なコイルと
ルツボの相対位置でも、放射熱反射体が融液上の温度勾
配を育成に適当な範囲に保ち、また育成が進行し放射熱
反射体が融液から遠のくに従って放射熱反射体の効果は
小さくなり、育成に伴い温度勾配が小さくなる効果を相
殺する。この結果融液量の変化に対して図４の実施例の
曲線が示すような温度勾配を取ることになり、平行長の
長い結晶を育成することが可能となる。なお、育成初期
の条件は、装置の形状、寸法、電力等の初期設定により
図４のように結晶割れが生じない部分に設定できる。Therefore, in order to solve this problem, the present invention arranges a radiant heat reflector above the crucible and raises the radiant heat reflector as the crystal is pulled up to reduce the temperature gradient difference between the early and late stages of growth. As shown by the curve in the example of FIG. 4, even if the remaining amount of the melt decreases due to the progress of crystal growth, the temperature gradient does not change so much and proper growth conditions can be maintained for a long time. It was made possible to train. That is, 1) Since the radiant heat reflector is located very close to the melt in the initial stage of growth, the radiant heat radiation reflected by the radiant heat reflector to the melt becomes large and the temperature gradient is made small. 2) As the growth proceeds, the radiant heat reflector separates from the surface of the melt and does not affect the temperature gradient near the melt. 3) Since the radiant heat reflector shields between the hot melt side and the upper part of the hot zone, the radiant heat above the radiant heat reflector is better dissipated and the amount of radiant heat conduction through the pulling shaft increases. . Of these, due to the effect of 1) above, in the case where there is no radiant heat reflector, the temperature gradient is too large and the radiant heat reflector grows a temperature gradient on the melt even at the relative position of the coil and the crucible which is inappropriate for growth. The effect of the radiant heat reflector becomes smaller as the radiant heat reflector becomes farther from the melt as the growth progresses, and the effect of the temperature gradient becomes smaller as it grows. As a result, a temperature gradient as shown by the curve of the embodiment of FIG. 4 is taken with respect to the change of the melt amount, and it becomes possible to grow a crystal having a long parallel length. The initial conditions of the growth can be set to a portion where crystal crack does not occur as shown in FIG. 4 by the initial setting of the shape, dimensions, electric power and the like of the apparatus.
【０００７】放射熱反射体は結晶引き上げ軸とは別個の
駆動系を設けてその引き上げ速度を制御しても良いが、
結晶引き上げ軸に固定すると、結晶引き上げに伴い充分
に大きい平行長の結晶が製造できる条件内で放射熱反射
体を種子結晶と同じ速度で上昇させることができ、装置
の機構を単純にすることができる。また、ルツボを加熱
する手段としては、高周波誘導加熱が一般的であるが、
抵抗加熱によっても良い。放射熱反射体は好ましくは円
盤形または円錐台形に構成した放射熱反射性の材料から
製作する。この形状は対称性が高いので均等な加熱効果
が得られる。また円錐台形の傾斜角を調整することによ
り適正な放射熱反射を設定することができる。放射熱反
射体の熱反射率は熱放射率が小さい材料ほど大きいの
で、育成温度での熱放射率が充分に小さく、化学的・物
理的に安定な物質から選択することが望ましく、特にＰ
ｔ、Ｒｈ、Ｉｒ、Ｏｓ等の耐熱性の白金族金属および白
金族金属の合金が望ましい。例えば、ＬｉＮｂＯ3 結晶
の育成には白金族金属の単体または１ｗｔ％以下のジル
コニア微粒子を含むＰｔ−ＺｒＯ2 合金が使用できる。
より高温度での育成が必要なＬｉＴａＯ3 の場合にはＩ
ｒまたはＰｔ−Ｒｈ系合金が使用できる。ここでいう白
金族金属の合金とは、白金族金属同志の合金と、白金族
金属と白金族以外の金属又は化合物からなる合金の両方
が含まれる。ルツボの加熱が高周波誘導加熱コイルを使
用して行われる場合には、放射熱反射体が金属の場合に
は円盤部分に外周部から中心に向かって適当な長さのス
リットを設けて発熱量を制御し、融液上の温度勾配を制
御することが可能である。The radiant heat reflector may be provided with a drive system separate from the crystal pulling shaft to control the pulling speed.
When fixed to the crystal pulling shaft, the radiant heat reflector can be raised at the same speed as the seed crystal within the condition that a sufficiently long parallel length crystal can be produced with the crystal pulling, and the mechanism of the device can be simplified. it can. In addition, as a means for heating the crucible, high frequency induction heating is generally used.
It may be done by resistance heating. The radiant heat reflector is preferably made of a radiant heat reflective material configured in the shape of a disc or a truncated cone. Since this shape has high symmetry, a uniform heating effect can be obtained. Further, by adjusting the inclination angle of the truncated cone, an appropriate radiant heat reflection can be set. Since the material having a smaller thermal emissivity has a larger thermal emissivity of the radiant heat reflector, it is desirable to select a substance having a sufficiently small thermal emissivity at a growing temperature and being chemically and physically stable.
Heat-resistant platinum group metals and alloys of platinum group metals such as t, Rh, Ir and Os are desirable. For example, for growing a LiNbO 3 crystal, a platinum group metal simple substance or a Pt—ZrO 2 alloy containing 1 wt% or less of zirconia fine particles can be used.
In the case of LiTaO 3 which needs to be grown at a higher temperature, I
r or Pt-Rh based alloys can be used. The platinum group metal alloy as used herein includes both alloys of platinum group metals and alloys of platinum group metals and metals or compounds other than platinum group metals. When the crucible is heated using a high-frequency induction heating coil, when the radiant heat reflector is metal, a slit with an appropriate length is provided on the disk part from the outer periphery to the center to reduce the amount of heat generation. It is possible to control and control the temperature gradient over the melt.
【０００８】[0008]
【実施例】次に本発明の実施例を詳しく説明する。図３
は本発明による単結晶の製造装置の一例を示す。図にお
いて、ルツボ２はその周りに充填された断熱材６により
絶縁されており、ルツボ２の上部には上記の熱反射性金
属等から構成される円筒形熱反射板１０で裏打ちしたカ
ップ状の耐火物円筒１１が配置され、その頂部壁１３に
は中心開口が設けてあり、下端に種子結晶５を取りつけ
た結晶引き上げ軸７が図示しない動力源から垂直に延び
てこの開口を貫通している。引き上げ軸７には熱反射体
９が水平に固定されている。断熱材６および耐火物円筒
１１の周りには、頂部壁１４に結晶引き上げ軸７が貫通
する開口を有する耐火物ハウジング８が配置されてい
る。耐火物ハウジング８の周壁には高周波誘導コイル１
が巻かれており、高周波電流を流した時にルツボ内に収
容されている結晶原料の融液を加熱して所定温度に維持
する。EXAMPLES Next, examples of the present invention will be described in detail. FIG.
Shows an example of an apparatus for producing a single crystal according to the present invention. In the figure, the crucible 2 is insulated by a heat insulating material 6 which is filled around the crucible 2. The upper part of the crucible 2 has a cup-like shape which is lined with a cylindrical heat reflection plate 10 made of the above heat-reflecting metal or the like. A refractory cylinder 11 is arranged, a central opening is provided in a top wall 13 thereof, and a crystal pulling shaft 7 having a seed crystal 5 attached to a lower end thereof extends vertically from a power source (not shown) and penetrates this opening. . A heat reflector 9 is horizontally fixed to the lifting shaft 7. Around the heat insulating material 6 and the refractory cylinder 11, a refractory housing 8 having an opening through which the crystal pulling shaft 7 penetrates is arranged in the top wall 14. The high frequency induction coil 1 is provided on the peripheral wall of the refractory housing 8.
Is wound, and when a high-frequency current is applied, the melt of the crystal raw material contained in the crucible is heated and maintained at a predetermined temperature.
【０００９】図５は本発明による単結晶の製造装置の他
の一例を示す。図において、ルツボ２２はその側壁およ
び底壁を円筒状の耐火物壁３０および耐火物支柱３１に
より支持絶縁されており、ルツボ２２の周りには円筒状
の発熱体２１が配置されている。発熱体の周囲には更に
断熱材２６を充填した絶縁ハウジング２８が配置され、
その底部は耐火物支持体により支持されている。また絶
縁ハウジング２８の頂部壁中央には開口３３が形成さ
れ、下端に種子結晶を取りつけた結晶引き上げ軸２７が
図示しない動力源から延びてこの開口を貫通している。
引き上げ軸２７には熱反射体２９が固定されている。FIG. 5 shows another example of the apparatus for producing a single crystal according to the present invention. In the figure, the side wall and bottom wall of the crucible 22 are supported and insulated by a cylindrical refractory wall 30 and a refractory support column 31, and a cylindrical heating element 21 is arranged around the crucible 22. An insulating housing 28 filled with a heat insulating material 26 is arranged around the heating element,
Its bottom is supported by a refractory support. An opening 33 is formed in the center of the top wall of the insulating housing 28, and a crystal pulling shaft 27 having a seed crystal attached to the lower end thereof extends from a power source (not shown) and penetrates the opening.
A heat reflector 29 is fixed to the pull-up shaft 27.
【００１０】次に、図１〜２を参照して本発明で使用す
る熱反射体９、２９について説明する。図１は図３また
は図５に示した実施例に使用できる円盤形の熱反射体を
例示する。上述の金属から形成した円盤４０はカラー４
３に固定されており、カラー４３は引き上げ軸７または
２７に嵌合する内孔を有し、固定ピン４１により引き上
げ軸の適正な位置に固定できるようになっている。熱源
が図３のような誘導加熱型の場合には、適当な長さおよ
び数のスリット４４を切り込むことにより、発熱量を調
整または抑制することができる。Next, the heat reflectors 9 and 29 used in the present invention will be described with reference to FIGS. FIG. 1 illustrates a disk-shaped heat reflector that can be used in the embodiment shown in FIG. 3 or 5. The disc 40 formed of the above-mentioned metal has a collar 4
The collar 43 has an inner hole that fits into the pull-up shaft 7 or 27, and can be fixed to an appropriate position of the pull-up shaft by a fixing pin 41. When the heat source is an induction heating type as shown in FIG. 3, the calorific value can be adjusted or suppressed by cutting slits 44 having an appropriate length and number.
【００１１】図２は図３または図５に示した実施例に使
用できる円錐台形の熱反射体を例示する。上述の金属か
ら形成した円錐板４５はカラー４３に固定されており、
カラー４３は引き上げ軸７または２７に嵌合する内孔を
有し、固定ピン４１により引き上げ軸の適正な位置に固
定できるようになっている。熱源が図３のような誘導加
熱型の場合には、適当な長さおよび数のスリット４４を
切り込むことにより、発熱量を調整または抑制すること
ができる。また、円錐板４５の開き角度を適宜に調整す
ることにより熱反射量を制御して、結晶成長に必要な温
度勾配を適正な値に制御することができる。例えば、融
液の表面中央部を高温にしたい場合には図示のように下
方に開いたものを、また逆に融液の表面中央部を低温に
したい場合には上に開いた円錐板を使用し、且つ円錐角
を適当に調整しておく。FIG. 2 illustrates a frustoconical heat reflector that can be used in the embodiment shown in FIG. 3 or 5. The conical plate 45 formed of the above-mentioned metal is fixed to the collar 43,
The collar 43 has an inner hole that fits into the pull-up shaft 7 or 27, and can be fixed to an appropriate position of the pull-up shaft by a fixing pin 41. When the heat source is an induction heating type as shown in FIG. 3, the calorific value can be adjusted or suppressed by cutting slits 44 having an appropriate length and number. Further, the amount of heat reflection can be controlled by appropriately adjusting the opening angle of the conical plate 45, and the temperature gradient necessary for crystal growth can be controlled to an appropriate value. For example, if you want to raise the temperature of the center of the melt surface, use the one that opens downward as shown in the figure, and conversely, if you want to lower the temperature of the center of the surface of the melt, use the cone plate that opens upward. And adjust the cone angle appropriately.
【００１２】次に、本発明を具体例によって説明する。 実施例１ 高周波発振器として周波数４０ｋＨｚのものを用いた。
図３において、直径１００ｍｍ、高さ１００ｍｍおよび
厚さ１．５ｍｍの白金製ルツボ２にニオブ酸リチウム約
２３００ｇを装入した。熱反射体９として白金製で直径
６０ｍｍ、厚さ０．５ｍｍ、該周部から中心までのスリ
ットが１本入ったものを使用した。種子結晶５としてＺ
方向（垂直方向）ニオブ酸リチウム単結晶を用いて４ｍ
ｍ／ｈｒの速度で引き上げたところ直径５０ｍｍ、長さ
１５０ｍｍのニオブ酸リチウム単結晶が得られた。比較
のため、熱反射体９を使用しない他は上記と同じ条件で
結晶育成を行ったところ、結晶の長さが１００ｍｍ以上
になると曲がってしまい、長くすることはできなかっ
た。Next, the present invention will be described with reference to specific examples. Example 1 A high frequency oscillator having a frequency of 40 kHz was used.
In FIG. 3, about 2300 g of lithium niobate was charged into a platinum crucible 2 having a diameter of 100 mm, a height of 100 mm and a thickness of 1.5 mm. The heat reflector 9 was made of platinum and had a diameter of 60 mm, a thickness of 0.5 mm, and one slit from the peripheral portion to the center. Z as seed crystal 5
Direction (vertical direction) 4m using lithium niobate single crystal
When pulled up at a speed of m / hr, a lithium niobate single crystal having a diameter of 50 mm and a length of 150 mm was obtained. For comparison, when the crystal was grown under the same conditions as above except that the heat reflector 9 was not used, when the crystal length was 100 mm or more, the crystal was bent and could not be lengthened.
【００１３】[0013]
【発明の効果】以上のように、本発明によると、結晶の
引き上げに伴い、結晶の上部に設置した放射熱反射体を
上昇させることにより、従来育成が困難であった長尺結
晶の育成が可能となり、生産性の向上とコストの削減が
可能となった。As described above, according to the present invention, as the crystal is pulled up, the radiant heat reflector installed on the upper part of the crystal is raised to grow a long crystal which has been difficult to grow conventionally. This has made it possible to improve productivity and reduce costs.
【図面の簡単な説明】[Brief description of drawings]
【図１】本発明の単結晶製造方法に使用する熱反射体の
実施例であり、図（ａ）は平面図、（ｂ）は正面図であ
る。FIG. 1 is an example of a heat reflector used in the method for producing a single crystal of the present invention, FIG. 1 (a) is a plan view and FIG. 1 (b) is a front view.
【図２】本発明の単結晶製造方法に使用する熱反射体の
他の実施例の正面図である。FIG. 2 is a front view of another embodiment of the heat reflector used in the method for producing a single crystal of the present invention.
【図３】本発明の単結晶製造装置の一例を示す正面断面
図である。FIG. 3 is a front sectional view showing an example of a single crystal production apparatus of the present invention.
【図４】本発明と従来の単結晶製造方法の作用を対比説
明する図である。FIG. 4 is a diagram for explaining the effects of the present invention and a conventional method for producing a single crystal for comparison.
【図５】本発明の単結晶製造装置の他の例を示す正面断
面図である。FIG. 5 is a front sectional view showing another example of the single crystal manufacturing apparatus of the present invention.
１ 高周波誘導コイル ２、２２ ルツボ ５ 種子結晶 ６、２６ 断熱材 ７、２７ 引き上げ軸 ８ 耐火物ハウジング ９、２９ 熱反射体 １０ 円筒形熱反射板 １１ 耐火物円筒 １３、１４ 頂部壁 ２１ 発熱体 ２８ 絶縁ハウジング ３０ 耐火物壁 ３１ 耐火物支柱 ３３ 開口 ４０ 円盤 ４３ カラー ４１ 固定ピン ４４ スリット ４５ 円錐板 DESCRIPTION OF SYMBOLS 1 High-frequency induction coil 2,22 Crucible 5 Seed crystal 6,26 Insulating material 7,27 Pulling shaft 8 Refractory housing 9,29 Heat reflector 10 Cylindrical heat reflector 11 Refractory cylinder 13,14 Top wall 21 Heating element 28 Insulation housing 30 Refractory wall 31 Refractory post 33 Opening 40 Disc 43 Color 41 Fixing pin 44 Slit 45 Conical plate
Claims (8)
する加熱手段と、前記ルツボ内の融液に種子結晶を接触
させ、その種子結晶を引き上げて単結晶を製造する方法
において、ルツボの上方に設置した放射熱反射体を結晶
引き上げに伴い上昇させることを特徴とする製造方法。1. A crucible for containing a melt, a heating means for heating the melt, and a method for producing a single crystal by bringing seed crystals into contact with the melt in the crucible and pulling the seed crystals. A manufacturing method characterized in that a radiant heat reflector installed above a crucible is raised along with crystal pulling.
法。2. The method according to claim 1, wherein the single crystal is an oxide.
ることにより、結晶引き上げに伴い前記放射熱反射体を
種子結晶と同じ速度で上昇させることを特徴とする請求
項１または２の製造方法。3. The method according to claim 1, wherein the radiant heat reflector is fixed to a crystal pulling shaft to raise the radiant heat reflector at the same speed as the seed crystal as the crystal is pulled up. .
する加熱手段と、前記ルツボ内の融液に種子結晶を接触
させその種子結晶を引き上げる手段とを備えた単結晶の
製造装置において、結晶引き上げに伴い上昇させる手段
を有する放射熱反射体をルツボの上方に設けたことを特
徴とする単結晶の製造装置。4. An apparatus for producing a single crystal, comprising a crucible containing a melt, heating means for heating the melt, and means for bringing the seed crystal into contact with the melt in the crucible and pulling up the seed crystal. In the apparatus for producing a single crystal, a radiant heat reflector having means for raising the crystal as the crystal is pulled is provided above the crucible.
ることにより、結晶引き上げに伴い前記放射熱反射体を
種子結晶と同じ速度で上昇させることを特徴とする請求
項４の製造装置。5. The manufacturing apparatus according to claim 4, wherein the radiant heat reflector is fixed to a crystal pulling shaft to raise the radiant heat reflector at the same speed as the seed crystal as the crystal is pulled up.
していることを特徴とする請求項４または５の製造装
置。6. The manufacturing apparatus according to claim 4, wherein the radiant heat reflector has a disk shape or a truncated cone shape.
びその合金から選択されている請求項４ないし６のいず
れかに記載の製造装置。7. The manufacturing apparatus according to claim 4, wherein the radiant heat reflector is selected from a heat-resistant platinum group metal simple substance and an alloy thereof.
段であり、放射熱反射体が１つまたは複数の切込を設け
たことを特徴とする請求項４ないし７のいずれかに記載
の製造装置。8. The heating means for heating the melt is an induction heating means, and the radiant heat reflector is provided with one or a plurality of cuts. Manufacturing equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33544794A JP3662962B2 (en) | 1994-12-22 | 1994-12-22 | Single crystal manufacturing method and apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33544794A JP3662962B2 (en) | 1994-12-22 | 1994-12-22 | Single crystal manufacturing method and apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08175896A true JPH08175896A (en) | 1996-07-09 |
| JP3662962B2 JP3662962B2 (en) | 2005-06-22 |
Family
ID=18288668
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33544794A Expired - Fee Related JP3662962B2 (en) | 1994-12-22 | 1994-12-22 | Single crystal manufacturing method and apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3662962B2 (en) |
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| JP2009179524A (en) * | 2008-01-31 | 2009-08-13 | Shin Etsu Handotai Co Ltd | Single crystal manufacturing apparatus and manufacturing method |
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| WO2013108567A1 (en) * | 2012-01-20 | 2013-07-25 | トヨタ自動車株式会社 | Seed crystal isolating spindle for single crystal production device and method for producing single crystals |
| JP2013147397A (en) * | 2012-01-20 | 2013-08-01 | Toyota Motor Corp | Seed crystal isolating spindle used in single crystal production device, and method for producing single crystal |
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| JPWO2013161999A1 (en) * | 2012-04-26 | 2015-12-24 | 京セラ株式会社 | Holder, crystal growth method and crystal growth apparatus |
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