JPH0920596A - Device for producing lithium tetraborate single crystal - Google Patents

Device for producing lithium tetraborate single crystal

Info

Publication number
JPH0920596A
JPH0920596A JP16973995A JP16973995A JPH0920596A JP H0920596 A JPH0920596 A JP H0920596A JP 16973995 A JP16973995 A JP 16973995A JP 16973995 A JP16973995 A JP 16973995A JP H0920596 A JPH0920596 A JP H0920596A
Authority
JP
Japan
Prior art keywords
crucible
lithium tetraborate
single crystal
platinum crucible
outside container
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
Application number
JP16973995A
Other languages
Japanese (ja)
Other versions
JP2868204B2 (en
Inventor
Tsunekazu Yamazaki
常和 山崎
Ikuo Machida
郁夫 町田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chichibu Fuji Co Ltd
Original Assignee
Chichibu Fuji Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Chichibu Fuji Co Ltd filed Critical Chichibu Fuji Co Ltd
Priority to JP16973995A priority Critical patent/JP2868204B2/en
Publication of JPH0920596A publication Critical patent/JPH0920596A/en
Application granted granted Critical
Publication of JP2868204B2 publication Critical patent/JP2868204B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Landscapes

  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain the non-porous high quality product reduced in the change of crystal growth speed due to the fluctuation of temperature by covering a platinum crucible with an outside container comprising a heat-resistant material selected from alumina, cordierite, mullite, quartz glass, boron nitride and graphite. SOLUTION: An outside container 4 supported on a support 3 and produced from either one of alumina, cordierite, mullite, quartz glass, boron nitride and graphite is received in an electric oven 1 having a heater 2 disposed therein. A depression 4a formed in the outside container 4 receives a platinum crucible 5 in a fit and detachable state. The upper opening 4b of the depression 4a is openably closed with a lid made from the same material as that of the outside container 4. The operation of a vertically moving mechanism 6 disposed at the lower end of the support 3 enables to integrally and vertically move the support 3, the outside container 4 and the crucible 5. Single crystals (a) and a seed crystal (b) are charged into the trunk 5a and the seed tube 5b of the crucible, respectively. The single crystals are melted so as not to melt the seed crystal (b), and subsequently cooled at a prescribed temperature gradient and at a cruciblelowering speed to raise the objective single crystal.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は、四ほう酸リチウム
の製造装置、特に表面弾性波デバイス用基板材料として
有用である四ほう酸リチウムの製造装置に関するもので
ある。
TECHNICAL FIELD The present invention relates to an apparatus for producing lithium tetraborate, and particularly to an apparatus for producing lithium tetraborate which is useful as a substrate material for surface acoustic wave devices.

【0002】[0002]

【従来の技術】従来、表面弾性波デバイス用基板材料と
して、ニオブ酸リチウム、タンタル酸リチウム、水晶、
四ほう酸リチウムなどが実用化されている。これらの単
結晶の中で、四ほう酸リチウムは、電気機械結合係数が
比較的大きく、且つ室温で非常に小さい遅延時間の温度
係数を有していることから移動体通信機器のフィルター
として有用な材料とされている。
Conventionally, as a substrate material for surface acoustic wave devices, lithium niobate, lithium tantalate, quartz,
Lithium tetraborate and the like have been put to practical use. Among these single crystals, lithium tetraborate is a material useful as a filter for mobile communication devices because it has a relatively large electromechanical coupling coefficient and a very small temperature coefficient of delay time at room temperature. It is said that.

【0003】四ほう酸リチウム単結晶の育成方法として
は、チョコラルスキー法もしくは垂直ブリッジマン法に
より融液から成長させる方法が従来から知られている。
このうちチョコラルスキー法は、原料をルツボに入れ、
加熱融解させ、その融液に種結晶を接触させて、これを
回転させながら徐々に引き上げることにより結晶成長を
行うもので、垂直ブリッジマン法に比べて成長速度を早
くできるという利点はあるが、急激な温度勾配により結
晶内に熱歪みが生じたり、炉内のガス対流による温度の
ゆらぎが原因となって育成中にクラックが発生し易く、
結晶の歩留りが低いという欠点があった。
As a method of growing a lithium tetraborate single crystal, a method of growing from a melt by the Czochralski method or the vertical Bridgman method has been conventionally known.
Among them, the Czochralski method puts raw materials in crucibles,
It is heated and melted, the seed crystal is brought into contact with the melt, and the crystal is grown by gradually pulling it while rotating it, which has the advantage that the growth rate can be made faster than the vertical Bridgman method. Thermal strain occurs in the crystal due to a sharp temperature gradient, cracks are likely to occur during growth due to temperature fluctuations due to gas convection in the furnace,
There was a defect that the yield of crystals was low.

【0004】これに対し垂直ブリッジマン法は、温度勾
配をもった炉内で融液を入れたルツボを移動し、種結晶
を挿入したルツボ先端より四ほう酸リチウム融液を凝固
させるもので、温度勾配が比較的緩やかで、且つ温度の
ゆらぎが小さいため、チョコラルスキー法に比べ良質の
単結晶が得られるという特徴を持っている。また垂直ブ
リッジマン法に使われるルツボは、耐熱性、耐熱衝撃
性、耐食性、安定性等の観点から、白金製のものが一般
に用いられている(特開平6−247796号等)。
On the other hand, in the vertical Bridgman method, a crucible containing a melt is moved in a furnace having a temperature gradient so that the lithium tetraborate melt is solidified from the tip of the crucible containing a seed crystal. Since the gradient is relatively gentle and the temperature fluctuation is small, it is characterized in that a single crystal of good quality can be obtained as compared with the Czochralski method. The crucible used in the vertical Bridgman method is generally made of platinum from the viewpoint of heat resistance, thermal shock resistance, corrosion resistance, stability, etc. (Japanese Patent Laid-Open No. 6-247796).

【0005】[0005]

【発明が解決しようとする課題】しかし乍ら、白金製ル
ツボを用いた従来のブリッジマン法による四ほう酸リチ
ウム単結晶の育成についてさらに詳細に検討すると、以
下のような問題点がないとは云えなかった。すなわち白
金製ルツボを使用した場合、温度のゆらぎの影響により
単結晶の成長速度が変化し、気泡介在物が混入して格子
欠陥が生じ易くなる。さらに、白金は四ほう酸リチウム
と濡れ性がよく、冷却時に白金製ルツボが収縮した際、
熱膨張差により結晶に歪みが発生するという問題があ
り、高品質の結晶を歩留り良く製造することが困難であ
った。また、垂直ブリッジマン法においては融液を高温
で長時間保持しなければならないことから、ルツボは最
低でも0.3〜0.35mmの肉厚が必要であり、ルツ
ボ再生時の精製コストが高いという欠点があった。
However, when the more detailed examination of the growth of a lithium tetraborate single crystal by the conventional Bridgman method using a platinum crucible, it can be said that the following problems do not exist. There wasn't. That is, when a platinum crucible is used, the growth rate of the single crystal changes due to the influence of temperature fluctuations, and bubble inclusions are easily mixed into the crucible to easily generate lattice defects. Furthermore, platinum has good wettability with lithium tetraborate, and when the platinum crucible contracts during cooling,
There is a problem that the crystal is distorted due to the difference in thermal expansion, and it is difficult to manufacture a high quality crystal with a high yield. Further, in the vertical Bridgman method, since the melt must be kept at a high temperature for a long time, the crucible needs to have a wall thickness of at least 0.3 to 0.35 mm, and the refining cost at the time of regenerating the crucible is high. There was a drawback.

【0006】上記したような白金製ルツボの問題点を解
消するべく、特開平5−262596号では黒鉛製ルツ
ボを使用することが提案されている。この場合、温度の
ゆらぎが直接融液に影響しにくくなって気泡介在物の混
入がなくなるものの、ルツボからの不純物の混入及び濃
縮により部分的に四ほう酸リチウム単結晶が黒鉛に融着
し、冷却時の熱膨張差により四ほう酸リチウムに引張り
応力が働き、部分的にクラックが発生するという問題点
があった。
In order to solve the above-mentioned problems of the platinum crucible, JP-A-5-262596 proposes to use a graphite crucible. In this case, the fluctuation of temperature is less likely to directly affect the melt and the inclusion of bubble inclusions is eliminated, but due to the inclusion and concentration of impurities from the crucible, the lithium tetraborate single crystal is partially fused to graphite and cooled. There is a problem that tensile stress acts on lithium tetraborate due to the difference in thermal expansion, and cracks are partially generated.

【0007】本発明は上述したような従来事情に鑑みて
なされたもので、その目的とするところは、高品質の四
ほう酸リチウム単結晶を、再現よく、高い歩留りで育成
できる製造装置を提供するものである。
The present invention has been made in view of the above-mentioned conventional circumstances, and an object of the present invention is to provide a manufacturing apparatus capable of growing a high quality lithium tetraborate single crystal with good reproducibility and high yield. It is a thing.

【0008】[0008]

【課題を解決するための手段】本発明者等は、温度のゆ
らぎがルツボ内の融液に直接影響しないようにすること
が気泡介在物の無い結晶を得るために不可欠の要因であ
り、さらに、高温時における白金製ルツボの変形を抑え
ることがクラックの無い結晶を得るために不可欠の要因
であり、この点を改良するべく鋭意研究を重ねた結果、
白金製ルツボの外側を所定の耐熱材料で覆うこと、白金
製ルツボの肉厚を従来より薄くすることが有用であるこ
とを見出し、本発明を完成するに至った。すなわち、本
願第1発明は、垂直ブリッジマン法もしくは垂直温度勾
配凝固法により、融液から四ほう酸リチウム単結晶を製
造するための装置であって、アルミナ、コーディエライ
ト、ムライト、石英ガラス、窒化ホウ素、黒鉛の中から
選ばれた何れか一つを主成分とする耐熱材料からなる外
側容器と、該外側容器内に入れる白金製ルツボとを備え
てなることを特徴とする四ほう酸リチウム単結晶の製造
装置である。また本願第2発明は、上記第1発明におい
て白金製ルツボの肉厚を0.05〜0.25mmとした
ことを特徴とする四ほう酸リチウム単結晶の製造装置で
ある。
The inventors of the present invention have found that preventing temperature fluctuations from directly affecting the melt in the crucible is an essential factor for obtaining crystals free of bubble inclusions. , It is an indispensable factor to obtain a crack-free crystal to suppress the deformation of the platinum crucible at high temperature, and as a result of repeated studies to improve this point,
The inventors have found that it is useful to cover the outside of the platinum crucible with a predetermined heat-resistant material and to make the thickness of the platinum crucible thinner than before, and have completed the present invention. That is, the first invention of the present application is an apparatus for producing a lithium tetraborate single crystal from a melt by a vertical Bridgman method or a vertical temperature gradient solidification method, which comprises alumina, cordierite, mullite, quartz glass, nitride A lithium tetraborate single crystal characterized by comprising an outer container made of a heat-resistant material containing at least one selected from boron and graphite as a main component, and a platinum crucible placed in the outer container. Manufacturing equipment. The second invention of the present application is the apparatus for producing a lithium tetraborate single crystal, wherein the platinum crucible has a thickness of 0.05 to 0.25 mm in the first invention.

【0009】以上の構成によれば、白金製ルツボの外側
を耐熱材料からなる外側容器で覆う二重ルツボ構造によ
り、温度のゆらぎによる単結晶の成長速度への影響が小
さくなり、気泡介在物の無い高品質の四ほう酸リチウム
単結晶を得ることができる。
According to the above structure, the double crucible structure in which the outer side of the platinum crucible is covered with the outer container made of the heat-resistant material reduces the influence of the temperature fluctuation on the growth rate of the single crystal, and the inclusion of the air bubbles. It is possible to obtain a high quality lithium tetraborate single crystal that does not exist.

【0010】さらに、外側容器で白金製ルツボを覆う二
重構造としたので、白金製ルツボの肉厚を従来より薄く
でき、二重ルツボ構造により高温時に白金製ルツボの変
形を抑えることができると共に従来より薄い白金製ルツ
ボを使用するので結晶に加わる熱歪みの応力を低減で
き、気泡介在物が無くクラックの発生も無い極めて高品
質の四ほう酸リチウム単結晶を得ることができる。ま
た、白金製ルツボを作製するための白金量が従来より少
くてすむので、白金製ルツボを再生する際の精製コスト
が安くなる。
Further, since the outer container has a double structure for covering the platinum crucible, the thickness of the platinum crucible can be made thinner than before, and the double crucible structure can suppress deformation of the platinum crucible at high temperature. Since a crucible made of platinum, which is thinner than before, is used, the stress of thermal strain applied to the crystal can be reduced, and an extremely high quality lithium tetraborate single crystal having no bubble inclusions and no cracks can be obtained. Further, since the amount of platinum for producing the platinum crucible is smaller than in the conventional case, the refining cost for regenerating the platinum crucible becomes low.

【0011】[0011]

【発明の実施の形態】以下、本発明に係る製造装置の実
施の形態を、垂直ブリッジマン法により四ほう酸リチウ
ム単結晶を製造する場合を例にとって、図面を参照して
説明する。図中1はヒータ2が配設された電気炉で、こ
の電気炉1の中には支持台3で支持された外側容器4が
収容される。外側容器4は、アルミナ、コーディエライ
ト、ムライト、石英ガラス、窒化ホウ素、黒鉛の中から
選ばれた何れか一つを主成分とする耐熱材料からなり、
支持台3の上面に設置される。外側容器4の内部には、
後述する白金製ルツボ5が嵌合状且つ取出し自在に収容
される凹部4aが形成される。またその凹部4aの上部
開口4bは、外側容器4と同一の材料で形成された蓋体
4cで開閉される。
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, an embodiment of a manufacturing apparatus according to the present invention will be described with reference to the drawings, taking a case where a lithium tetraborate single crystal is manufactured by a vertical Bridgman method as an example. In the figure, reference numeral 1 denotes an electric furnace in which a heater 2 is arranged, and an outer container 4 supported by a support 3 is accommodated in the electric furnace 1. The outer container 4 is made of a heat-resistant material whose main component is any one selected from alumina, cordierite, mullite, quartz glass, boron nitride, and graphite.
It is installed on the upper surface of the support base 3. Inside the outer container 4,
A recess 4a is formed in which a platinum crucible 5 to be described later is fitted and can be taken out. Further, the upper opening 4b of the recess 4a is opened and closed by a lid 4c made of the same material as the outer container 4.

【0012】白金製ルツボ5は、この種製法において用
いられるものと同様に、大径状の胴体部5aと、この胴
体部5aの下方に設けられる小径状の種管5bとを備え
た形状もので、前記凹部4a内に収容されてその周囲を
外側容器4で覆われる。
The platinum crucible 5 has a shape having a large-diameter body portion 5a and a small-diameter seed tube 5b provided below the body portion 5a, like the one used in this kind of manufacturing method. Then, the outer container 4 is housed in the recess 4 a and the periphery thereof is covered with the outer container 4.

【0013】支持台3の下端には上下機構6が設けら
れ、この上下機構6の作動により、支持台3と一体に外
側容器4及び白金製ルツボ5が上下動するように構成す
る。
An up-and-down mechanism 6 is provided at the lower end of the support base 3, and the operation of the up-and-down mechanism 6 causes the outer container 4 and the platinum crucible 5 to move up and down integrally with the support base 3.

【0014】[0014]

【実施例】次に、本発明の装置を用いた四ほう酸リチウ
ム単結晶の製造、及びこれにより得られた四ほう酸リチ
ウムの評価試験について説明する。まず大気中もしくは
不活性雰囲気において所定のモル比で調合された純度4
N(99.99wt%)の四ほう酸リチウム単結晶原料
aを、直径80mm,長さ300mmに作製した白金製
ルツボの胴体部5aに入れ、直径5mm,長さ100m
mの<110>方位に加工した四ほう酸リチウムの種結
晶bを種管5bに挿入し、さらにその白金製ルツボ5を
外側容器4内に入れ、種結晶bを溶かさないように92
0℃以上で融解した。次いで、育成点における温度勾配
を20℃とし、ルツボ降下速度を0.3mm/時とし
て、白金製ルツボ5を200mm移動させ、単結晶を成
長させたのち、室温まで冷却した。さらに白金製ルツボ
5を破いて四ほう酸リチウムを取り出し、このものにお
ける気泡介在物の混入、及びクラックの有無を調べた。
外側容器4の材質、白金製ルツボ5の厚さと気泡介在
物、クラック発生の関係を、比較例と共に表1に示す。
また、本発明の装置により3インチの四ほう酸リチウム
基板を製造した場合の歩留りの一例を、比較例と共に表
2に示す。比較例は、外側容器を備えず白金製ルツボの
みからなる従来の装置を用いて垂直ブリッジマン法で製
造した四ほう酸リチウムである。
EXAMPLES Next, the production of a lithium tetraborate single crystal using the apparatus of the present invention and the evaluation test of the lithium tetraborate thus obtained will be described. First, a purity of 4 at a prescribed molar ratio in the air or an inert atmosphere.
N (99.99 wt%) lithium tetraborate single crystal raw material a was put into the body portion 5a of a platinum crucible having a diameter of 80 mm and a length of 300 mm, and the diameter was 5 mm and the length was 100 m.
A seed crystal b of lithium tetraborate processed in the <110> direction of m was inserted into the seed tube 5b, and the platinum crucible 5 was placed in the outer container 4 so as not to melt the seed crystal b.
It melted above 0 ° C. Then, the temperature gradient at the growth point was set to 20 ° C., the crucible lowering speed was set to 0.3 mm / hour, the platinum crucible 5 was moved 200 mm to grow a single crystal, and then cooled to room temperature. Further, the platinum crucible 5 was broken to take out lithium tetraborate, and the inclusion of bubble inclusions and the presence of cracks in this product were examined.
Table 1 shows the relationship between the material of the outer container 4, the thickness of the platinum crucible 5 and the inclusion of bubbles, and the occurrence of cracks.
Table 2 shows an example of the yield when a 3-inch lithium tetraborate substrate was manufactured by the apparatus of the present invention, together with a comparative example. The comparative example is lithium tetraborate produced by the vertical Bridgman method using a conventional apparatus having only an platinum crucible without an outer container.

【0015】[0015]

【表1】 [Table 1]

【0016】[0016]

【表2】 [Table 2]

【0017】以上の結果から、アルミナ、コーディエラ
イト、ムライト、石英ガラス、窒化ホウ素、黒鉛の中か
ら選ばれた何れか一つを主成分とする耐熱材料からなる
外側容器と、該外側容器内に入れる白金製ルツボとを備
えてなる本発明の製造装置を用いて垂直ブリッジマン法
により製造した四ほう酸リチウムは、気泡介在物の無い
高品質のものであり、再現よく高い歩留りで製造可能で
あることが確認できた。またその中でも、白金製ルツボ
の肉厚を0.05〜0.25mmとした場合は、部分的
クラックも無い極めて高品質なものであり、且つ極めて
高い歩留りが得られることが確認できた。
From the above results, an outer container made of a heat-resistant material whose main component is any one selected from alumina, cordierite, mullite, quartz glass, boron nitride, and graphite, and the inside of the outer container Lithium tetraborate produced by the vertical Bridgman method using the production apparatus of the present invention comprising a platinum crucible placed in is a high quality product without bubble inclusions, and can be produced with good reproducibility and high yield. It was confirmed that there is. Further, among them, it was confirmed that when the thickness of the platinum crucible was set to 0.05 to 0.25 mm, the quality was extremely high with no partial cracks and an extremely high yield was obtained.

【0018】これに対し、外側容器を備えず白金製ルツ
ボのみからなる従来の装置を用いて垂直ブリッジマン法
で製造した比較例の四ほう酸リチウムは、気泡介在物及
びクラックが存在することが確認できた。
On the other hand, the lithium tetraborate of the comparative example manufactured by the vertical Bridgman method using the conventional apparatus having only the platinum crucible without the outer container was confirmed to have bubble inclusions and cracks. did it.

【0019】尚、本実施例では垂直ブリッジマン法によ
り四ほう酸リチウム単結晶を製造する場合の一例につい
て説明したが、白金製ルツボの寸法や種結晶の方位、融
解温度、育成点における温度勾配、ルツボ降下速度やル
ツボ移動量等の各種条件は上記のものに限定されず、且
つ外側容器4及び白金製ルツボ5は固定し、電気炉1を
上下機構で支持するように構成する等、周知の範囲内で
の変更は任意である。また本発明は垂直ブリッジマン法
に用いるものに限定されず、上下機構6を用いず、ヒー
タ2の温度を電気炉1の上下方向に対して適宜に制御す
る(上側のヒータを高温、下側のヒータを低温とする)
ことが可能なよう構成すれば、垂直温度勾配凝固法によ
り四ほう酸リチウム単結晶を製造する場合にも適用可能
であることは云うまでもない。
In this embodiment, an example of producing a lithium tetraborate single crystal by the vertical Bridgman method has been described, but the dimensions of the platinum crucible, the orientation of the seed crystal, the melting temperature, the temperature gradient at the growing point, Various conditions such as the crucible lowering speed and the crucible movement amount are not limited to the above, and the outer container 4 and the platinum crucible 5 are fixed, and the electric furnace 1 is configured to be supported by an up-and-down mechanism. Changes within the range are arbitrary. Further, the present invention is not limited to the one used in the vertical Bridgman method, and the temperature of the heater 2 is appropriately controlled in the vertical direction of the electric furnace 1 without using the vertical mechanism 6 (the upper heater has a high temperature, the lower heater has a high temperature). Of the heater of low temperature)
Needless to say, if it is configured so that it can be applied to the case of producing a lithium tetraborate single crystal by the vertical temperature gradient solidification method.

【0020】[0020]

【発明の効果】本発明の四ほう酸リチウム単結晶の製造
装置は以上説明したように、アルミナ、コーディエライ
ト、ムライト、石英ガラス、窒化ホウ素、黒鉛の中から
選ばれた何れか一つを主成分とする耐熱材料からなる外
側容器によって白金製ルツボを覆う新規な構成としたこ
とから、温度のゆらぎによる成長速度の変化を低くし、
気泡介在物の無い高品質な四ほう酸リチウム単結晶が得
られる。
As described above, the apparatus for producing a lithium tetraborate single crystal of the present invention mainly comprises any one selected from alumina, cordierite, mullite, quartz glass, boron nitride and graphite. With a new configuration that covers the platinum crucible with an outer container made of a heat-resistant material, the change in growth rate due to temperature fluctuations is reduced,
A high-quality lithium tetraborate single crystal free of bubble inclusions can be obtained.

【0021】さらに、前記した外側容器と白金製ルツボ
とを備えた二重ルツボ構造としたことから、白金製ルツ
ボの肉厚を従来より薄くでき、これにより結晶に加わる
歪みがより小さくなってクラックの発生を抑えることが
でき、気泡介在物の混入が無く、且つ部分的クラックの
発生もない極めて高品質な四ほう酸リチウム単結晶を、
再現よく高い歩留りで育成することが可能になり、前述
の効果をより実効あるものとすることができる。さらに
加えて、白金製ルツボを再生する際の精製コストを従来
に比して大幅に低減し得、従来よりも低コストで前記効
果が得られる等、多くの利点を奏する。
Further, since the double crucible structure including the outer container and the platinum crucible described above is used, the thickness of the platinum crucible can be made thinner than before, so that the strain applied to the crystal is further reduced and cracks are generated. The formation of extremely high quality lithium tetraborate single crystal that can suppress the occurrence of bubbles, is free from inclusion of bubble inclusions, and is free from partial cracks.
It is possible to grow with good reproducibility and high yield, and the above-mentioned effects can be made more effective. In addition, the refining cost when regenerating the platinum crucible can be greatly reduced as compared with the conventional method, and the above-mentioned effect can be obtained at a lower cost than the conventional method.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明に係る四ほう酸リチウム単結晶の製造装
置の一実施例を示す縦断正面図。
FIG. 1 is a vertical sectional front view showing an embodiment of an apparatus for producing a lithium tetraborate single crystal according to the present invention.

【符号の説明】[Explanation of symbols]

1:電気炉 2:ヒータ 3:支持台 4:外側容器 5:白金製ルツボ 5a:胴体部 5b:種管 a:四ほう酸リチウム単結晶原料 b:種結晶 1: Electric furnace 2: Heater 3: Support stand 4: Outer container 5: Platinum crucible 5a: Body part 5b: Seed tube a: Lithium tetraborate single crystal raw material b: Seed crystal

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 垂直ブリッジマン法もしくは垂直温度勾
配凝固法により、融液から四ほう酸リチウム単結晶を製
造する装置であって、アルミナ、コーディエライト、ム
ライト、石英ガラス、窒化ホウ素、黒鉛の中から選ばれ
た何れか一つを主成分とする耐熱材料からなる外側容器
と、該外側容器内に入れる白金製ルツボとを備えてなる
ことを特徴とする四ほう酸リチウム単結晶の製造装置。
1. An apparatus for producing a lithium tetraborate single crystal from a melt by a vertical Bridgman method or a vertical temperature gradient solidification method, which comprises alumina, cordierite, mullite, quartz glass, boron nitride and graphite. An apparatus for producing a lithium tetraborate single crystal, comprising: an outer container made of a heat-resistant material containing any one of the above as a main component, and a platinum crucible placed in the outer container.
【請求項2】 上記白金製ルツボの肉厚を0.05〜
0.25mmとしたことを特徴とする請求項1記載の四
ほう酸リチウム単結晶の製造装置。
2. The platinum crucible has a wall thickness of 0.05 to
The apparatus for producing a lithium tetraborate single crystal according to claim 1, wherein the apparatus has a length of 0.25 mm.
JP16973995A 1995-07-05 1995-07-05 Equipment for producing lithium tetraborate single crystal Expired - Lifetime JP2868204B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP16973995A JP2868204B2 (en) 1995-07-05 1995-07-05 Equipment for producing lithium tetraborate single crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP16973995A JP2868204B2 (en) 1995-07-05 1995-07-05 Equipment for producing lithium tetraborate single crystal

Publications (2)

Publication Number Publication Date
JPH0920596A true JPH0920596A (en) 1997-01-21
JP2868204B2 JP2868204B2 (en) 1999-03-10

Family

ID=15891955

Family Applications (1)

Application Number Title Priority Date Filing Date
JP16973995A Expired - Lifetime JP2868204B2 (en) 1995-07-05 1995-07-05 Equipment for producing lithium tetraborate single crystal

Country Status (1)

Country Link
JP (1) JP2868204B2 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1074641A1 (en) * 1999-08-02 2001-02-07 Sumitomo Electric Industries, Ltd. Crystal growth vessel and crystal growth method
WO2010047429A1 (en) * 2008-10-22 2010-04-29 Myungjoo Kwon Double layered crucible for crystal growth
JP2011126719A (en) * 2009-12-15 2011-06-30 Fuji Electric Co Ltd Apparatus for growing single crystal
CN102906314A (en) * 2010-05-21 2013-01-30 住友电气工业株式会社 Pyrolytic boron nitride vessel for crystal growth, and growth method for semiconductor crystal using same

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1074641A1 (en) * 1999-08-02 2001-02-07 Sumitomo Electric Industries, Ltd. Crystal growth vessel and crystal growth method
EP1460153A3 (en) * 1999-08-02 2005-04-20 Sumitomo Electric Industries, Ltd. Crystal growth vessel and crystal growth method
WO2010047429A1 (en) * 2008-10-22 2010-04-29 Myungjoo Kwon Double layered crucible for crystal growth
JP2011126719A (en) * 2009-12-15 2011-06-30 Fuji Electric Co Ltd Apparatus for growing single crystal
CN102906314A (en) * 2010-05-21 2013-01-30 住友电气工业株式会社 Pyrolytic boron nitride vessel for crystal growth, and growth method for semiconductor crystal using same

Also Published As

Publication number Publication date
JP2868204B2 (en) 1999-03-10

Similar Documents

Publication Publication Date Title
US20150221511A1 (en) Method for producing sic single crystal
JP4803784B2 (en) Method for producing quartz glass crucible for pulling silicon single crystal
JP2937115B2 (en) Single crystal pulling method
JP2868204B2 (en) Equipment for producing lithium tetraborate single crystal
US4251315A (en) Method of growing metal halide and chalcogenide crystals for use as infrared windows
JPS59213697A (en) Pulling device for single crystal semiconductor
JP2020125242A (en) Polycrystalline silicon ingot, polycrystalline silicon rod, and method for producing monocrystalline silicon
JP2636929B2 (en) Method for producing bismuth germanate single crystal
JP3887444B2 (en) Method for producing lithium tetraborate single crystal
JPH1179892A (en) Production of lithium tetraborate single crystal
JP2543449B2 (en) Crystal growth method and apparatus
JP2733898B2 (en) Method for manufacturing compound semiconductor single crystal
JPH0825835B2 (en) Single crystal pulling device
JPS62138385A (en) Device for pulling semiconductor single crystal
JPH08319195A (en) Production of lithium borate single crystal
JP2012036015A (en) Crystal growth method
JPH0411513B2 (en)
JPH05339094A (en) Apparatus for producing oxide single crystal
JP2535773B2 (en) Method and apparatus for producing oxide single crystal
JPH07138095A (en) Method of growing single crystal of lithium borate
JPS6126519B2 (en)
JPS58181798A (en) Manufacture of single crystal silicon
JPH09278582A (en) Production of single crystal and apparatus therefor
JPS6012318B2 (en) Single crystal pulling method and device
JPH0558772A (en) Production of compound semiconductor single crystal

Legal Events

Date Code Title Description
R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20081225

Year of fee payment: 10

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20091225

Year of fee payment: 11

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20101225

Year of fee payment: 12

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20111225

Year of fee payment: 13

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20111225

Year of fee payment: 13

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20121225

Year of fee payment: 14

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20121225

Year of fee payment: 14

FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20131225

Year of fee payment: 15

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

EXPY Cancellation because of completion of term