JP2012250874A - Iridium crucible, and method for producing lithium tantalate single crystal using the same - Google Patents

Iridium crucible, and method for producing lithium tantalate single crystal using the same Download PDF

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JP2012250874A
JP2012250874A JP2011124156A JP2011124156A JP2012250874A JP 2012250874 A JP2012250874 A JP 2012250874A JP 2011124156 A JP2011124156 A JP 2011124156A JP 2011124156 A JP2011124156 A JP 2011124156A JP 2012250874 A JP2012250874 A JP 2012250874A
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lithium tantalate
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Atsushi Abe
淳 阿部
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Shin Etsu Chemical Co Ltd
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Abstract

PROBLEM TO BE SOLVED: To provide a crucible suited for producing a lithium tantalate single crystal without any defect such as a void at a low cost.SOLUTION: In the iridium crucible used for growing an oxide single crystal from a melt with a Czochralski method, it is desirable that, when plate thickness of a side face and that of a bottom face are respectively represented by t and t', t>t' is satisfied, the t' value satisfies 0.5t≤t'≤0.95t, and the t value is 1.5 mm-10.0 mm, and furthermore the shape of the bottom face of the iridium crucible is rounded.

Description

本発明はイリジウムルツボに関し、特に、チョクラルスキー法(Cz法)を用いたタンタル酸リチウム単結晶の製造に使用されるイリジウムルツボに関する。   The present invention relates to an iridium crucible, and more particularly to an iridium crucible used for producing a lithium tantalate single crystal using the Czochralski method (Cz method).

表面弾性波素子等に好適に用いられるタンタル酸リチウム単結晶は、一般にチョクラルスキー法によって製造されている。チョクラルスキー法によってタンタル酸リチウム単結晶を製造する場合には、(1)炉の中で、イリジウム製のルツボのまわりを耐火物で囲み、該ルツボ又は耐火物の上に、ルツボ上部の温度勾配を適切に保つための熱反射の機能を持たせたアフターヒーター、及び、アフターヒーター蓋を有する貴金属製の構造物を設置し、(2)原料となるタンタル酸リチウム結晶塊をルツボの中で加熱溶融し、(3)得られた融液に種結晶を浸漬した後に、(4)所定の回転数で、種結晶及びルツボを回転させながら該種結晶を静かに引き上げ、(5)種結晶の下にタンタル酸リチウムの単結晶を成長させるのが一般的である。   A lithium tantalate single crystal suitably used for a surface acoustic wave device or the like is generally manufactured by the Czochralski method. When producing a lithium tantalate single crystal by the Czochralski method, (1) Surrounding the iridium crucible with a refractory in a furnace, the temperature at the top of the crucible is placed on the crucible or the refractory. An after-heater with a function of heat reflection to keep the gradient appropriate, and a precious metal structure with an after-heater lid were installed, and (2) the lithium tantalate crystal mass as a raw material was placed in the crucible (3) After the seed crystal is immersed in the obtained melt, (4) the seed crystal is gently pulled up while rotating the seed crystal and the crucible at a predetermined rotational speed, and (5) the seed crystal. It is common to grow a single crystal of lithium tantalate underneath.

図4は、36度回転Y軸タンタル酸リチウムの単結晶、若しくは38度回転Y軸タンタル酸リチウムの単結晶の製造に用いられている、従来の、タンタル酸リチウム単結晶製造装置の縦概略断面図である。   FIG. 4 is a schematic vertical sectional view of a conventional lithium tantalate single crystal manufacturing apparatus used for manufacturing a single crystal of 36 ° rotated Y-axis lithium tantalate or a single crystal of 38 ° rotated Y-axis lithium tantalate. FIG.

図4に示されるように、従来のタンタル酸リチウムの単結晶製造装置は、耐火性ルツボ台23と、ルツボ台23の底部に設けられたアルミナ台22と、アルミナ台22上に設けられたルツボ21と、ルツボ21を囲む断熱材24と、断熱材24の上部に設けられた耐火性アルミナ25を備え、更に、ルツボ21の上方に設けられたアフターヒーターと称される円筒状の熱反射板27と、アフターヒーター27の蓋であるアフターヒーター蓋28を備えている。必要に応じて、ルツボ21の上部には、リフレクターと称されるドーナツ型で円板状の熱反射板26を設けることもできる。   As shown in FIG. 4, the conventional apparatus for producing a single crystal of lithium tantalate includes a refractory crucible base 23, an alumina base 22 provided at the bottom of the crucible base 23, and a crucible provided on the alumina base 22. 21, a heat insulating material 24 surrounding the crucible 21, and a refractory alumina 25 provided above the heat insulating material 24, and a cylindrical heat reflector called an after heater provided above the crucible 21. 27 and an after heater lid 28 that is a lid of the after heater 27. If necessary, a donut-shaped and disk-shaped heat reflecting plate 26 called a reflector may be provided on the upper portion of the crucible 21.

図4に示されるように、耐火性ルツボ台23の周囲には、加熱コイル29が設けられ、ルツボ21を誘導加熱し、ルツボ21内の原料を融解して、融液30を調製し、シードホルダー31に取り付けた種結晶32を融液30に浸漬た後、種結晶32を引き上げる。これによって、円錐状の肩部35aと円柱状の胴部35bよりなる、タンタル酸リチウム単結晶35が生成される。 As shown in FIG. 4, a heating coil 29 is provided around the refractory crucible base 23 to heat the crucible 21, melt the raw material in the crucible 21, prepare a melt 30, and seed after the seed crystal 32 attached to the holder 31 is immersed in the melt 30, pulling the seed crystal 32. As a result, a lithium tantalate single crystal 35 composed of a conical shoulder portion 35a and a cylindrical body portion 35b is generated.

近年、上記のような単結晶を製造するコストを低減するために、ルツボの使用回数をできる限り増やして長期間使用する試みがなされている。しかしながら、ルツボの使用回数を増加させるにつれてルツボの変形が進み、その変形の仕方によっては、歩留まりが低下したりボイド等が単結晶中に含まれたりするという問題があった。   In recent years, attempts have been made to increase the number of times the crucible is used as much as possible in order to reduce the cost of manufacturing the single crystal as described above. However, as the number of times the crucible is used increases, deformation of the crucible progresses, and depending on how the crucible is deformed, there is a problem in that the yield decreases and voids are included in the single crystal.

そこで、従来からルツボの改良について研究がなされ(例えば、特許文献1及び2)ているが、何れも融液の温度勾配を制御し、自然対流を強くすることに主眼がおかれており、ルツボ自身の構造を改良するものではない。したがってこれらの従来技術においては、ランガサイト単結晶について言及されているものの、異方性の強いタンタル酸リチウム結晶については全く言及されていない。   Therefore, research on the improvement of the crucible has been made conventionally (for example, Patent Documents 1 and 2). However, both of them focus on controlling the temperature gradient of the melt and strengthening the natural convection. It does not improve its structure. Therefore, in these prior arts, although mention is made of a langasite single crystal, there is no mention of a highly anisotropic lithium tantalate crystal.

特開2004-284853号公報JP 2004-284853 A 特開2004-284854号公報JP 2004-284854 A

しかしながら、タンタル酸リチウム結晶の様に異方性が強い場合には、タンタル酸リチウム融液が冷却される際、あるいは固体が加熱されて融液になる際に、前記異方性が原因となってルツボを変形させるという特有の問題がある。したがって、前記従来技術によって、タンタル酸リチウム単結晶の製造に使用するルツボの使用回数を増大させることは不可能であった。   However, when the anisotropy is strong like the lithium tantalate crystal, the anisotropy is caused when the lithium tantalate melt is cooled or when the solid is heated to become a melt. There is a unique problem of deforming the crucible. Therefore, it has been impossible to increase the number of times the crucible used for manufacturing the lithium tantalate single crystal is used by the conventional technique.

したがって本発明の第1の目的は、チョクラルスキー法を用いた、異方性の強い単結晶の製造に好適なイリジウムルツボを提供することにある。
本発明の第2の目的は、低コストで、ボイドのような欠陥のないタンタル酸リチウム単結晶を製造する方法を提供することにある。
Accordingly, a first object of the present invention is to provide an iridium crucible suitable for producing a highly anisotropic single crystal using the Czochralski method.
A second object of the present invention is to provide a method for producing a lithium tantalate single crystal that is low in cost and free from defects such as voids.

本発明者は、上記の諸目的を達成するために鋭意検討を重ねた結果、ルツボが横方向に変形しやすいことに着目し、ルツボ底面側の板厚を側面方向の板厚よりも薄くして、底面側に変形を逃がすようなルツボ構造とし、ルツボが横方向に変形することを防いだところ、これによって、歩留まりを低下させることなく使用回数を増大させることができるだけでなく、底面に滞留するような融液がなくなり、自然対流によってルツボ内の融液が均一になるので、ボイド等の欠陥が発生しなくなることを見出し、本発明に到達した。   As a result of intensive studies to achieve the above-mentioned objects, the present inventor has paid attention to the fact that the crucible is easily deformed in the lateral direction, and has made the plate thickness on the bottom side of the crucible thinner than the plate thickness in the side direction. The crucible structure that allows deformation to escape on the bottom side prevents the crucible from deforming in the lateral direction, which not only increases the number of uses without reducing the yield, but also stays on the bottom surface. Thus, the present inventors have found that defects such as voids do not occur because the melt in the crucible becomes uniform due to natural convection, and no defects such as voids occur.

即ち本発明は、チョクラルスキー法によって融液から単結晶を育成させるために使用するイリジウムルツボであって、側面のイリジウム金属の厚みと底面のイリジウム金属の厚みをそれぞれt、t’としたとき、t>t’であることを特徴とするイリジウムルツボ、及び、該ルツボを使用してタンタル酸リチウムの単結晶を育成することを特徴とするタンタル酸リチウム単結晶の製造方法である。
本発明においては、t’は0.5t≦t’≦0.95tの関係を満たすことが好ましく、tは1.5mm以上10.0mm以下であることが好ましい。また、底面の形状は、丸味を帯びていることが好ましい。
That is, the present invention is an iridium crucible used for growing a single crystal from a melt by the Czochralski method, wherein the thickness of the iridium metal on the side surface and the thickness of the iridium metal on the bottom surface are t and t ′, respectively. T> t ′, and a method for producing a lithium tantalate single crystal characterized by growing a lithium tantalate single crystal using the crucible and the crucible.
In the present invention, t ′ preferably satisfies the relationship of 0.5 t ≦ t ′ ≦ 0.95 t, and t is preferably 1.5 mm or greater and 10.0 mm or less. Moreover, it is preferable that the shape of a bottom face is roundish.

本発明によれば、低コストで、ボイドのような欠陥のないタンタル酸リチウム単結晶を製造することが可能になる。   According to the present invention, it becomes possible to produce a lithium tantalate single crystal free from defects such as voids at low cost.

図1は、本発明のイリジウムルツボの、断面図の一例である。FIG. 1 is an example of a cross-sectional view of an iridium crucible of the present invention. 図2は、本発明のイリジウムルツボの、他の断面図の例である。FIG. 2 is an example of another cross-sectional view of the iridium crucible of the present invention. 図3は、従来のイリジウムルツボの断面図である。FIG. 3 is a cross-sectional view of a conventional iridium crucible. 図4は、36度回転Y軸タンタル酸リチウム単結晶の製造方法、又は、38度回転Y軸タンタル酸リチウム単結晶の製造方法に好適に用いることができる、タンタル酸リチウム単結晶の製造装置の縦断面概略図である。FIG. 4 shows an apparatus for producing a lithium tantalate single crystal that can be suitably used in a method for producing a 36-degree rotated Y-axis lithium tantalate single crystal or a method for producing a 38-degree rotated Y-axis lithium tantalate single crystal. It is a longitudinal cross-sectional schematic diagram. 実施例1で200回使用した後の、本発明のルツボの形状である。It is the shape of the crucible of this invention after using 200 times in Example 1. FIG. 実施例2で200回使用した後の、本発明のルツボの形状である。It is the shape of the crucible of this invention after using 200 times in Example 2. FIG. 実施例3で200回使用した後の、本発明のルツボの形状である。It is the shape of the crucible of this invention after using 200 times in Example 3. FIG. 比較例1で200回使用した後の、従来のルツボの形状である。It is the shape of the conventional crucible after using 200 times in the comparative example 1. FIG.

以下、添付図面に基づいて、本発明の好ましい実施態様につき、詳細に説明する。   Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

図1及び図2は、側面の肉厚より底面の肉厚の方が薄い、本発明のイリジウムルツボである。本発明においては、単にルツボ底面の肉厚が側面の肉厚より薄ければ良く、それ以外の形状は特に限定されない。例えば、図1は底面が平坦である場合であり、図2の場合には底面が丸くなっている。図3は従来のルツボであり、側面の肉厚と底面の肉厚は同じである。   1 and 2 show the iridium crucible of the present invention in which the bottom wall thickness is thinner than the side wall thickness. In the present invention, it is only necessary that the thickness of the bottom surface of the crucible is thinner than the thickness of the side surface, and other shapes are not particularly limited. For example, FIG. 1 shows a case where the bottom surface is flat, and in FIG. 2, the bottom surface is rounded. FIG. 3 shows a conventional crucible, in which the side wall thickness and the bottom wall thickness are the same.

一般に、タンタル酸リチウムのような単結晶製造装置は、図4に示されるように、セラミックス製の耐火性ルツボ台23と、該耐火性ルツボ台23の底部に設けられたアルミナ台22と、該アルミナ台22上に設けられたルツボ21と、該ルツボ21を囲む断熱材24と、ドーナツ型で円板状の熱反射板であるリフレクター26と、該リフレクター26の上方に設けられた円筒状の熱反射板であるアフターヒーター27と、該アフターヒーター27の蓋であるアフターヒーター蓋28と、ルツボ台23の周囲に設けられた加熱コイル29を備えている。   In general, a single crystal manufacturing apparatus such as lithium tantalate, as shown in FIG. 4, includes a ceramic fireproof crucible base 23, an alumina base 22 provided at the bottom of the fireproof crucible base 23, A crucible 21 provided on an alumina table 22, a heat insulating material 24 surrounding the crucible 21, a reflector 26 which is a donut-shaped and disk-like heat reflecting plate, and a cylindrical shape provided above the reflector 26 An after heater 27 that is a heat reflecting plate, an after heater cover 28 that is a lid of the after heater 27, and a heating coil 29 provided around the crucible base 23 are provided.

本発明にかかるイリジウムルツボは、図4中のルツボ21に相当する。タンタル酸リチウムの単結晶を製造する場合には、ルツボ21を誘導加熱し、ルツボ1内の原料を融解して融液30とし、シードホルダー31に取り付けた種結晶32であるタンタル酸リチウム単結晶を融液30に浸漬して、シードホルダー31を回転させながら、種結晶32を引き上げる。これによって、円錐状の肩部35aと円柱状の胴部35bよりなるタンタル酸リチウム単結晶35が生成される。   The iridium crucible according to the present invention corresponds to the crucible 21 in FIG. In the case of producing a lithium tantalate single crystal, the crucible 21 is induction-heated, the raw material in the crucible 1 is melted to form a melt 30, and the lithium tantalate single crystal that is the seed crystal 32 attached to the seed holder 31. Is immersed in the melt 30 and the seed crystal 32 is pulled up while rotating the seed holder 31. As a result, a lithium tantalate single crystal 35 composed of a conical shoulder portion 35a and a cylindrical body portion 35b is generated.

本発明のイリジウムルツボは、ルツボ底面側の板厚を側面方向よりも薄くして板厚の薄い底面側に変形を逃がすようなルツボ構造となっているので、ルツボが横方向に変形し難い。これによって、歩留まりを低下させることなく使用回数を増大させることができる。また、底面に滞留するような融液がなくなり、自然対流によってルツボ内の融液が均一になるので、ボイド等の欠陥が発生しなくなる
以下、本発明を実施例に基づいて更に説明するが、本発明はこれによって何ら限定されるものではない。
The iridium crucible of the present invention has a crucible structure in which the plate thickness on the bottom surface side of the crucible is made thinner than the side surface direction and the deformation is released to the bottom surface side where the plate thickness is thin. As a result, the number of times of use can be increased without reducing the yield. Further, there is no melt that stays on the bottom surface, and the melt in the crucible becomes uniform by natural convection, so that defects such as voids do not occur.Hereinafter, the present invention will be further described based on examples. This invention is not limited at all by this.

図1に示された形状のイリジウムルツボであって、円筒部の板厚が2mm、底部の板厚1.5mm、内径150mm、高さ150mmのイリジウム製ルツボを、図4に示された38度回転Y軸タンタル酸リチウム単結晶の製造装置にセットし、38度回転Y軸タンタル酸リチウム単結晶を製造した。使用したリフレクターのサイズは、外径160mm、内径105mm、厚さ2mmであり、アフターヒーターとしては直径150mm、高さ180mmのイリジウム製アフターヒーターを使用した。   1. An iridium crucible having the shape shown in FIG. 1 and an iridium crucible having a cylindrical portion thickness of 2 mm, a bottom portion thickness of 1.5 mm, an inner diameter of 150 mm, and a height of 150 mm is shown in FIG. It set to the manufacturing apparatus of the rotation Y-axis lithium tantalate single crystal, and produced the 38 degree rotation Y-axis lithium tantalate single crystal. The size of the reflector used was an outer diameter of 160 mm, an inner diameter of 105 mm, and a thickness of 2 mm. As the after heater, an iridium after heater having a diameter of 150 mm and a height of 180 mm was used.

具体的には、ルツボ内に、組成比がLi/Ta=0.943(モル比)のY軸タンタル酸リチウムの焼成原料4500gと結晶塊5500gの合計10000gを入れてルツボを加熱し、溶融した。溶融後、シードホルダーに取り付けた38度回転Y軸タンタル酸リチウムの種結晶を融液中に浸漬し、シードホルダーを7rpmの回転数で回転させながら種結晶をゆっくり引き上げて、直径が100mmで、円柱状の胴部の長さが約110mmのタンタル酸リチウム単結晶のサンプルを製造した。   Specifically, a crucible was heated and melted by putting a total of 10,000 g of 4500 g of Y-axis lithium tantalate firing material having a composition ratio of Li / Ta = 0.944 (molar ratio) and a crystal mass of 5500 g into the crucible. . After melting, the 38 ° rotated Y-axis lithium tantalate seed crystal attached to the seed holder was immersed in the melt, and the seed crystal was slowly pulled up while rotating the seed holder at a rotation speed of 7 rpm. A sample of lithium tantalate single crystal having a columnar body length of about 110 mm was manufactured.

上記タンタル酸リチウム結晶の製造を、繰返し200回実施した。その時の歩留まりは80%で、得られた全てのタンタル酸リチウム単結晶サンプル中には、ボイドなどの欠陥(インクルージョンの発生)は認められなかった。また、200回使用した後のルツボの形状は図5に示した通りであり、横方向へのルツボの広がりが少ないことが確認された。   The production of the lithium tantalate crystal was repeated 200 times. The yield at that time was 80%, and defects such as voids (occurrence of inclusion) were not observed in all the obtained lithium tantalate single crystal samples. Further, the shape of the crucible after being used 200 times is as shown in FIG. 5, and it was confirmed that there was little spread of the crucible in the lateral direction.

実施例1で使用されたイリジウムルツボを、円筒部の板厚が2mm、底部の板厚が1.9mmのルツボに替えた他は実施例1と同様にしてサンプルを製造した。その時の歩留まりは82%で、得られた全てのタンタル酸リチウム単結晶サンプル中には、ボイドなどの欠陥(インクルージョンの発生)は認められなかった。また、200回使用した後のルツボの形状は図6に示した通りであり、横方向へのルツボの広がりが少ないことが確認された。   Samples were produced in the same manner as in Example 1 except that the iridium crucible used in Example 1 was replaced with a crucible having a cylindrical thickness of 2 mm and a bottom thickness of 1.9 mm. The yield at that time was 82%, and no defects such as voids (occurrence of inclusion) were observed in all the obtained lithium tantalate single crystal samples. Moreover, the shape of the crucible after being used 200 times is as shown in FIG. 6, and it was confirmed that the crucible did not spread in the horizontal direction.

図2に示された形状で、寸法及び板厚が実施例1で用いたイリジウムルツボと同じイリジウムルツボを用いた他は、実施例1と同様にしてサンプルを200回製造した。その時の歩留まりは86%で、得られた全てのタンタル酸リチウムの単結晶サンプル中には、ボイドなどの欠陥(インクルージョンの発生)は認められなかった。また、200回使用した後のルツボの形状は図7に示した通りであり、横方向へのルツボの広がりが少ないことが確認された。   A sample was manufactured 200 times in the same manner as in Example 1 except that the same iridium crucible as that used in Example 1 was used in the shape shown in FIG. The yield at that time was 86%, and no defects such as voids (occurrence of inclusion) were observed in all the obtained single crystal samples of lithium tantalate. Moreover, the shape of the crucible after being used 200 times is as shown in FIG. 7, and it was confirmed that there is little spread of the crucible in the lateral direction.

実施例1で使用されたイリジウムルツボを、円筒部の板厚が3mm、底部の板厚が2.25mmのルツボに替えた他は実施例1と同様にして200回サンプルを製造した。その時の歩留まりは81%で、得られた全てのタンタル酸リチウム単結晶サンプル中には、ボイドなどの欠陥(インクルージョンの発生)は認められなかった。また、200回使用した後のルツボの形状は図6に示した通りであり、横方向へのルツボの広がりが少ないことが確認された。   Samples were produced 200 times in the same manner as in Example 1, except that the iridium crucible used in Example 1 was replaced with a crucible having a cylindrical thickness of 3 mm and a bottom thickness of 2.25 mm. The yield at that time was 81%, and no defects such as voids (occurrence of inclusion) were observed in all the obtained lithium tantalate single crystal samples. Moreover, the shape of the crucible after being used 200 times is as shown in FIG. 6, and it was confirmed that the crucible did not spread in the horizontal direction.

比較例1
円筒部及び底部の板厚が共に2mmである点だけが実施例1で用いたルツボと異なるルツボを使用した他は、実施例1と同様にして200回サンプルを製造した。この時の歩留まりは70%で、ルツボの使用回数が150回以降となったときに得られた全てのタンタル酸リチウム単結晶のサンプル中には、ボイドなどの欠陥(インクルージョンの発生)が認められた。また、200回使用した後のルツボの形状は図8に示した通りであり、横方向へのルツボの広がりが大きいことが確認された。
Comparative Example 1
Samples were manufactured 200 times in the same manner as in Example 1 except that a crucible different from the crucible used in Example 1 was used only in that the thickness of both the cylindrical part and the bottom part was 2 mm. At this time, the yield was 70%, and all the lithium tantalate single crystal samples obtained when the crucible was used after 150 times showed defects such as voids (occurrence of inclusion). It was. Moreover, the shape of the crucible after being used 200 times is as shown in FIG. 8, and it was confirmed that the crucible spreads in the horizontal direction.

比較例2
円筒部の板厚が2mmで底部の板厚が1mmの、図1に示した形状のイリジウムルツボを使用した他は実施例1と同様にして、200回サンプルを製造することを試みた。この時の歩留まりは82%であり、得られた全てのタンタル酸リチウム単結晶サンプル中に、ボイドなどの欠陥(インクルージョンの発生)は認められなかったが、160回使用後には湯漏れが発生した(使用後のルツボ形状は図5と同様の形状であった)ので、それ以上同じルツボを使用して製造することはできなかった。
Comparative Example 2
An attempt was made to manufacture a sample 200 times in the same manner as in Example 1 except that an iridium crucible having the shape shown in FIG. 1 having a cylindrical thickness of 2 mm and a bottom thickness of 1 mm was used. The yield at this time was 82%, and no defects such as voids (occurrence of inclusion) were observed in all the obtained lithium tantalate single crystal samples, but after 160 times of use, hot water leaked. (The crucible shape after use was the same as that shown in FIG. 5), so it could not be produced using the same crucible.

比較例3
円筒部の板厚が1mmで底部の板厚が0.75mmの、図1に示した形状のイリジウムルツボを使用した他は実施例1と同様にして、200回サンプルを製造することを試みた。しかしながら、ルツボの板厚が薄いため結晶が溶融又は固化する際の応力に耐えられず、板厚2mm又は3mmの時と比べるとルツボが加速的に変形し、30回使用時には湯漏れが発生した。
Comparative Example 3
An attempt was made to manufacture samples 200 times in the same manner as in Example 1 except that an iridium crucible having the shape shown in FIG. 1 having a cylindrical thickness of 1 mm and a bottom thickness of 0.75 mm was used. . However, because the crucible plate is thin, it cannot withstand the stress when the crystal melts or solidifies, and the crucible deforms at an accelerated rate compared to when the plate thickness is 2 mm or 3 mm. .

実施例1、2及び比較例1、2の結果から、側面のイリジウムの厚みと底面のイリジウムの厚みをそれぞれt、t’とした場合、t’は0.5t≦t’≦0.95tであることが好ましい。
又、比較例3の結果から、側面のイリジウムの厚みが1mmよりも小さいとルツボの変形が加速的に進み、湯漏れにつながることが判明した。又、実施例3で使用したルツボの底部の板厚が1.5mmの場合も鑑みると、ルツボ側面の板厚tはt≧1.5mmであることが好ましい。
一方、実施例3、4の比較から、ルツボ側面の板厚を厚くすればルツボの変形を低減する効果はあるものの、ルツボ側面の板厚を1.5mm以上としても歩留り等に大きな差は見られないことが判明した。これらの事実から、t≧1.5mmであれば良いことが分かるが、ルツボの材質が非常に高価なイリジウムであるため、10.0mmを越えると、価格競争力において不利となる。
From the results of Examples 1 and 2 and Comparative Examples 1 and 2, assuming that the thickness of the iridium on the side surface and the thickness of the iridium on the bottom surface are t and t ′, respectively, t ′ is 0.5t ≦ t ′ ≦ 0.95t. Is preferred.
Further, from the result of Comparative Example 3, it was found that when the thickness of the iridium on the side surface is smaller than 1 mm, the crucible deforms at an accelerated rate and leads to hot water leakage. In view of the case where the thickness of the bottom portion of the crucible used in Example 3 is 1.5 mm, the thickness t of the side surface of the crucible is preferably t ≧ 1.5 mm.
On the other hand, from the comparison of Examples 3 and 4, although increasing the thickness of the crucible side surface has the effect of reducing the deformation of the crucible, there is no significant difference in yield even when the thickness of the crucible side surface is 1.5 mm or more. It turned out not to be. From these facts, it can be understood that t ≧ 1.5 mm, but since the material of the crucible is very expensive iridium, if it exceeds 10.0 mm, it is disadvantageous in price competitiveness.

本発明によれば、異方性のあるタンタル酸リチウムの単結晶を、低コストでボイドのような欠陥なしに製造することが可能であるので、本発明は産業上極めて有意義である。   According to the present invention, since an anisotropic lithium tantalate single crystal can be produced at low cost and without defects such as voids, the present invention is extremely significant in industry.

21 ルツボ
22 アルミナ台
23 ルツボ台
24 断熱材
25 耐火性アルミナ
26 リフレクター
27 アフターヒーター
28 アフターヒーター蓋
29 加熱コイル
30 融液
31 シードホルダー
32 種結晶
35 タンタル酸リチウム単結晶
35a タンタル酸リチウム単結晶の円錐状の肩部
35b タンタル酸リチウム単結晶の円柱状の胴部
21 crucible 22 alumina base 23 crucible base 24 heat insulating material 25 refractory alumina 26 reflector 27 after heater 28 after heater lid 29 heating coil 30 melt 31 seed holder 32 seed crystal 35 lithium tantalate single crystal 35a cone of lithium tantalate single crystal Shoulder 35b cylindrical body of lithium tantalate single crystal

Claims (5)

チョクラルスキー法で融液から酸化物単結晶を育成するのに使用するイリジウムルツボであって、側面の板厚と底面の板厚をそれぞれt及びt’とした場合、t>t’であることを特徴とするイリジウムルツボ。 An iridium crucible used for growing an oxide single crystal from a melt by the Czochralski method, where t> t ′ where t and t ′ are the thicknesses of the side and bottom surfaces, respectively. Iridium crucible characterized by that. 前記t’値が0.5t≦t’≦0.95tである、請求項1に記載されたイリジウムルツボ。 The iridium crucible according to claim 1, wherein the t ′ value is 0.5 t ≦ t ′ ≦ 0.95 t. 前記t値が1.5mm〜10.0mmである、請求項1又は2に記載されたイリジウムルツボ。 The iridium crucible according to claim 1 or 2, wherein the t value is 1.5 mm to 10.0 mm. 底面の形状が丸味を帯びている、請求項1〜3の何れかに記載されたイリジウムルツボ。 The iridium crucible according to any one of claims 1 to 3, wherein the shape of the bottom surface is rounded. 請求項1〜4の何れかに記載されたイリジウムルツボを用い、チョクラルスキー法によって、タンタル酸リチウムの融液からタンタル酸リチウムの単結晶を育成することを特徴とする、タンタル酸リチウム単結晶の製造方法。 A lithium tantalate single crystal is grown from a lithium tantalate melt by the Czochralski method using the iridium crucible according to any one of claims 1 to 4. Manufacturing method.
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