JPS5814398B2 - Method for producing lithium tantalate single crystal - Google Patents
Method for producing lithium tantalate single crystalInfo
- Publication number
- JPS5814398B2 JPS5814398B2 JP13806178A JP13806178A JPS5814398B2 JP S5814398 B2 JPS5814398 B2 JP S5814398B2 JP 13806178 A JP13806178 A JP 13806178A JP 13806178 A JP13806178 A JP 13806178A JP S5814398 B2 JPS5814398 B2 JP S5814398B2
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- lithium tantalate
- tantalate single
- producing lithium
- 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.)
- Expired
Links
- 239000013078 crystal Substances 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 title claims description 10
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 239000010937 tungsten Substances 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 230000007547 defect Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 229910052741 iridium Inorganic materials 0.000 description 3
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 229910012463 LiTaO3 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002503 iridium Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
本発明はタンタル酸リチウム(LsTaOa)単結晶の
製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing lithium tantalate (LsTaOa) single crystal.
従来LiTaOs単結晶は応用光学結晶として用いられ
る為に格子欠陥や不純物に依る光の吸収熔がなく光学的
に透明である必要があった。Conventionally, since LiTaOs single crystals are used as applied optical crystals, they have been required to be optically transparent without absorbing light due to lattice defects or impurities.
通常このLiTa03単結晶の製造はチョコラフスキ(
CZ)法と呼ばれる引上げ法に依って行なわれていた。Normally, this LiTa03 single crystal is manufactured by Czokolawski (
This was done using a pulling method called the CZ) method.
この引上げにはLITa03単結晶の融点である165
0℃より遥かに高融点の材料から成る坩啼を用いなけれ
ば該坩堝の組成が一部溶融して不純物としてLiTaO
s単結晶に溶け込み着色する恐れがある。For this pulling, the melting point of LITa03 single crystal is 165
Unless a crucible made of a material with a melting point much higher than 0°C is used, the composition of the crucible will partially melt and contain LiTaO as impurities.
s There is a risk that it will dissolve into the single crystal and cause coloration.
この為に従来に於いては融点、2454℃のイリジウム
から成る坩堝を用いていたが、このイリジウムは高価で
あり数回の引上げに対して行なう補修の費用が高くつく
と云う欠点があった。For this purpose, a crucible made of iridium, which has a melting point of 2454° C., has conventionally been used, but this iridium has the disadvantage that it is expensive and the cost of repairs after several pullings is high.
一方、高純度の原料からLiTa03単結晶を引上げ成
長せしめると数回の引上げに対して1回程度の割合で結
晶中にクラツクが発生し、再引上げをしなければならな
い為に歩留りを低下させ結果的にコストアップの要因と
なっていた。On the other hand, when LiTa03 single crystal is pulled and grown from a high-purity raw material, cracks occur in the crystal at a rate of about once for every few times the crystal is pulled, and as it has to be pulled again, the yield decreases. This caused an increase in costs.
然し、このLiTa03単結晶を最近脚光を浴び始めた
表面波応用デバイスや圧電応用デバイスとして利用する
場合必ずしも透明である必要はなく多少の不純物を含ん
でいて着色状態にあっても特性的にあまり大きな影響を
受けない事が知られている。However, when this LiTa03 single crystal is used in surface wave application devices or piezoelectric application devices, which have recently begun to attract attention, it is not necessarily transparent, and it may contain some impurities, and even if it is in a colored state, its characteristics may not be large enough. known to be unaffected.
本発明製造方法は上述の諸問題に鑑みて為されたもので
あって特に表面波応用デバイスや圧電応用デバイスとし
て用いて有用なLiTa03単結晶を提供するものであ
る。The manufacturing method of the present invention has been devised in view of the above-mentioned problems, and provides a LiTa03 single crystal that is particularly useful for use as a surface wave application device or a piezoelectric application device.
一般に単結晶に於いては或る程度の格子欠陥を含む方が
安定であるとされている。It is generally believed that single crystals are more stable if they contain a certain amount of lattice defects.
そこで本発明製造方法に於いてはLiTaOsの溶液に
三酸化タングステンW03の形で低濃度のタングステン
Wを添加して結晶を成長せしめ、結晶中のタンタルTa
が配置すべき位置にWを位置せしめると、5価のTaに
対してWは6価であるのでチャージ補償の為に次式に示
すようなリチウムLi格子欠陥を形成する。Therefore, in the manufacturing method of the present invention, a low concentration of tungsten W in the form of tungsten trioxide W03 is added to a LiTaOs solution to grow a crystal, and tantalum Ta in the crystal is grown.
When W is placed at the position where W should be placed, since W is hexavalent compared to Ta, which is pentavalent, lithium Li lattice defects are formed as shown in the following equation for charge compensation.
ただし、ψはLi格子欠陥を示す。However, ψ indicates a Li lattice defect.
この様にLtTa03の溶液に少量のWを添加してLi
TaOa単結晶を成長せしめると結晶中にLi格子欠陥
をもたらす。In this way, by adding a small amount of W to the LtTa03 solution, Li
When a TaOa single crystal is grown, Li lattice defects are produced in the crystal.
このLi格子欠陥の発生に依つて結晶引上げの際発生す
るクラツクの発生回かが減少した。Due to the occurrence of Li lattice defects, the number of cracks that occur during crystal pulling is reduced.
図はその実験結果を示し、横軸にはLiTa03に対す
るWの含有量(モルチ)が縦軸には10回の引上げに対
するクラツクの発生回数が夫々採られている。The figure shows the experimental results, with the horizontal axis plotting the W content (molch) relative to LiTa03, and the vertical axis plotting the number of cracks per 10 pullings.
同図に於いて、Wの含有量を零、即ち従来通り引き上げ
た場合平均的に3回のクラツクが発生したものが0.1
〜0.2モル係になると1回となり2.0モル係に於い
ても2.5回の発生となり従来の3回に比べクラツクの
発生回数を抑える事が出来る。In the same figure, when the W content is zero, that is, when raised as usual, the average number of cracks that occur is 0.1.
At ~0.2 molar ratio, the crack occurs once, and even at 2.0 molar ratio, the crack occurs 2.5 times, making it possible to suppress the number of cracks that occur compared to the conventional three times.
具体的実施例を以下に記述する。Specific examples will be described below.
直径120mmφ高さ120trの白金・ロジウムから
成る合金坩堝にLiTaOa焼結体を入れ高周波加熱炉
で該LiTa03を融解し融解後LtTaOsのチップ
結晶を低速回転せしめて直径6011φ高さ100mm
のLiTa03単結晶を引上げ成長せしめた場合、W等
の不純物を含有しないものに於いては10回の引上げに
対して平均的に3回のクラツクが発生したが、0,1モ
ル係のWを含有せしめたものはクラツクの発生を10回
に対し1回に抑える事が出来た。A LiTaOa sintered body was placed in an alloy crucible made of platinum and rhodium with a diameter of 120 mmφ and a height of 120 tr, and the LiTaO3 was melted in a high-frequency heating furnace. After melting, a chip crystal of LtTaOs was rotated at low speed to form a crucible with a diameter of 6011 mm and a height of 100 mm.
When pulling and growing a LiTa03 single crystal of The product that contained it was able to suppress the occurrence of cracks to 1 out of 10.
即ち、0.1モル係のWを含有せしめる事に依ってクラ
ツクの発生率を1/3に低下させる事が出来る。That is, by containing 0.1 mole of W, the crack occurrence rate can be reduced to 1/3.
この製造方法に依って引上げられたLsTaO3単結晶
は坩堝のロジウムとWとに依って赤褐色に着色するが表
面波応用テバイス等に利用する場合何ら影響を与えない
程度であった。Although the LsTaO3 single crystal pulled by this production method was colored reddish brown due to the rhodium and W in the crucible, it did not have any effect when used in surface wave application devices.
尚、以上の説明に於いてはチョコラフスキ(CZ)法に
依る引上げ成長について述べたが同じ引上げ成長のEF
G法や引下げ法、キプロス法等製造方法に於いても本発
明は有用である。In the above explanation, we have talked about upward growth using the Czokolawski (CZ) method, but the EF of the same upward growth
The present invention is also useful in manufacturing methods such as the G method, the pull-down method, and the Cyprus method.
本発明は以上の説明から明らかな如く、タンタル酸リチ
ウム溶液中にタングステンを含有せしめて成長せしめた
ので、タングステン等の不純物を含まず成長したものに
比べクラツクの発生率を低下させる事が出来る。As is clear from the above description, in the present invention, since tungsten is grown in a lithium tantalate solution, the incidence of cracks can be lowered compared to products grown without impurities such as tungsten.
従って歩留りが向上するので製造コストの低減化が図れ
る。Therefore, since the yield is improved, manufacturing costs can be reduced.
また、表面波応用デバイスや圧電応用デバイス等の光学
的透明度を必要としないものについては白金ロジウム坩
堝の使用が可能となるので、高価なイリジウム坩堝を使
用しなくて済みより一層のコストダウンが図れる等本発
明製造方法の得るところは大きい。In addition, platinum-rhodium crucibles can be used for devices that do not require optical transparency, such as surface wave application devices and piezoelectric application devices, so there is no need to use expensive iridium crucibles, resulting in further cost reductions. The advantages of the production method of the present invention are significant.
図はタンタル酸リチウム中のタングステンの含有量とク
ラツクの発生回数との関係を示す曲線図である・The figure is a curve diagram showing the relationship between the tungsten content in lithium tantalate and the number of cracks.
Claims (1)
ンタル酸リチウム溶液中にタングステンを含む化合物を
含有せしめて成長せしめた事を特部とするタンタル酸リ
チウム単結晶の製造方法。 2 上記タングステンの含有量を0.01〜2モル係と
した事を特徴とする特許請求の範囲第1項記載のタンタ
ル酸リチウム単結晶の製造方法。 3 上記タンタル酸リチウム単結晶の成長は白金ロジウ
ムから成る合金坩堝内にて行なわれる事を特徴とした特
許請求の範囲第1項又は第2項記載のタンタル酸リチウ
ム単結晶の製造方法。[Claims] 1. A method for producing a lithium tantalate single crystal, which is characterized in that the lithium tantalate single crystal is grown, stored, and grown by containing a compound containing tungsten in the lithium tantalate solution. . 2. The method for producing a lithium tantalate single crystal according to claim 1, characterized in that the content of the tungsten is 0.01 to 2 mol. 3. The method for producing a lithium tantalate single crystal according to claim 1 or 2, wherein the growth of the lithium tantalate single crystal is carried out in an alloy crucible made of platinum rhodium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13806178A JPS5814398B2 (en) | 1978-11-06 | 1978-11-06 | Method for producing lithium tantalate single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13806178A JPS5814398B2 (en) | 1978-11-06 | 1978-11-06 | Method for producing lithium tantalate single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5562898A JPS5562898A (en) | 1980-05-12 |
| JPS5814398B2 true JPS5814398B2 (en) | 1983-03-18 |
Family
ID=15213056
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13806178A Expired JPS5814398B2 (en) | 1978-11-06 | 1978-11-06 | Method for producing lithium tantalate single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5814398B2 (en) |
-
1978
- 1978-11-06 JP JP13806178A patent/JPS5814398B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5562898A (en) | 1980-05-12 |
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