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JPS6234718B2 - - Google Patents
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JPS6234718B2 - - Google Patents

Info

Publication number
JPS6234718B2
JPS6234718B2 JP56147012A JP14701281A JPS6234718B2 JP S6234718 B2 JPS6234718 B2 JP S6234718B2 JP 56147012 A JP56147012 A JP 56147012A JP 14701281 A JP14701281 A JP 14701281A JP S6234718 B2 JPS6234718 B2 JP S6234718B2
Authority
JP
Japan
Prior art keywords
single crystal
litao
voltage
applying
electric field
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
Application number
JP56147012A
Other languages
Japanese (ja)
Other versions
JPS5849696A (en
Inventor
Kenji Enokida
Masao Tsunoda
Mitsunobu Ootani
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.)
Toshiba Corp
Original Assignee
Tokyo Shibaura Electric 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 Tokyo Shibaura Electric Co Ltd filed Critical Tokyo Shibaura Electric Co Ltd
Priority to JP56147012A priority Critical patent/JPS5849696A/en
Publication of JPS5849696A publication Critical patent/JPS5849696A/en
Publication of JPS6234718B2 publication Critical patent/JPS6234718B2/ja
Granted legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides
    • C30B29/30Niobates; Vanadates; Tantalates

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Description

【発明の詳細な説明】[Detailed description of the invention]

本発明はリチウムタンタレート(以下LiTaO3
と記す)単結晶の単一分域の方法に関する。 LiTaO3単結晶を単一分域化することは公知で
ある。(特公昭47−8450号、特開昭54−15196号
等)。 例えばX軸引上げLiTaO3単結晶を単一分域化
する為には第1図に示すようにヒータ1で加熱で
きるようにした電気炉2内に引上げた単結晶3を
Z面に電極4を設け、スイツチ7を投入してリー
ド線5から電圧6を加えられるようにしておく。
このときのLiTaO3単結晶の加熱曲線(実線)お
よび電圧印加特性(破線)を第2図に示す。多く
の場合単結晶の温度上昇は200℃/時間、t0から
h2までの保持温度は650℃、温度降下は200℃/時
間である。一定温度に保持し始める時間t0から20
分後t1において電圧を印加し、さらに20分後t2
ら温度を降下させ、t1から1時間後t3で電圧を切
る。以上の操作によりLiTaO3単結晶の単一分域
化は終了する。 さてこのようにして得られる単一分極化した
LiTaO3単結晶は、分極化終了時点で単結晶のク
ラツクが観察されることである。このクラツクの
大きさは種々様々で大きいものはX軸方向に長さ
10cm外周面での幅1mm程度から小さいものは肉眼
でやつと見つかる程度のものまである。又クラツ
クの方向もX軸方向とは限らない。数多くの実験
中に発生したクラツク発生率は約5%であつた。 単結晶に発生するクラツクは生産コスト面だけ
でなく単結晶の品質特性面からみても好ましい現
象ではなく極力減少しなければならない。 発明者等は分極化後のクラツクを減少させるべ
く分極化の方法における種々の要因について実験
研究を行う中で単結晶の電圧印加条件もクラツク
の一原因になつていることを見出しこの発明を完
成した。 すなわち本発明はLiTaO3単結晶のZ軸の両端
に電界印加のための電極を設け、この単結晶を所
定の温度に加熱し、この所定温度において前記単
結晶に所定の電界を印加する工程を有する単結晶
の単一分域化方法において、前記所定の電界の印
加は緩やかに行うことを特徴とするLiTaO3の単
一分極化方法である。 数多くの実験によれば第3図の破線(実線は単
結晶の温度)に示す様に電圧を印加するに当り、
時間に対して傾斜を与えるように緩やかに印加す
ることによりクラツクが防止され、第2図の破線
に示すような急峻な電圧印加ではクラツクが多
い。こゝで電圧印加の緩やかさとクラツク発生率
との関係を第1表に示す。
The present invention uses lithium tantalate (hereinafter referred to as LiTaO 3
) relates to a single domain method for single crystals. It is known to single-sectorize LiTaO 3 single crystals. (Special Publication No. 47-8450, JP-A-54-15196, etc.). For example, in order to make an X-axis pulled LiTaO 3 single crystal into a single domain, as shown in Fig. 1, the pulled single crystal 3 is placed in an electric furnace 2 that can be heated with a heater 1, and an electrode 4 is placed on the Z plane. The switch 7 is turned on so that a voltage 6 can be applied from the lead wire 5.
The heating curve (solid line) and voltage application characteristics (broken line) of the LiTaO 3 single crystal at this time are shown in FIG. In most cases, the temperature rise of single crystals is 200°C/hour, from t 0
The holding temperature up to h 2 is 650 °C, and the temperature drop is 200 °C/hour. Time to start holding at constant temperature t 0 to 20
After a minute, a voltage is applied at t1 , and after another 20 minutes, the temperature is lowered from t2 , and one hour after t1 , the voltage is turned off at t3 . The above operations complete the single domain formation of the LiTaO 3 single crystal. Now, the single polarization obtained in this way
In LiTaO 3 single crystal, cracks in the single crystal are observed at the end of polarization. The size of this crack varies, and the largest one has a length in the X-axis direction.
They range in size from about 1mm wide on the outer surface of 10cm to those that can be easily seen with the naked eye. Also, the direction of the crack is not limited to the X-axis direction. The crack incidence during many experiments was approximately 5%. Cracks occurring in single crystals are not a desirable phenomenon not only in terms of production costs but also in terms of quality characteristics of single crystals and must be reduced as much as possible. In order to reduce cracks after polarization, the inventors conducted experimental research on various factors in the polarization method, and discovered that voltage application conditions for single crystals were also a cause of cracks, and completed this invention. did. That is, the present invention includes the steps of providing electrodes for applying an electric field to both ends of the Z axis of a LiTaO 3 single crystal, heating this single crystal to a predetermined temperature, and applying a predetermined electric field to the single crystal at this predetermined temperature. In the method for single - domaining a single crystal, the method is characterized in that the application of the predetermined electric field is performed slowly. According to numerous experiments, when applying a voltage, as shown by the broken line in Figure 3 (the solid line is the temperature of the single crystal),
Cracks can be prevented by applying the voltage gradually so as to give a slope with respect to time, and if the voltage is applied steeply as shown by the broken line in FIG. 2, many cracks occur. Table 1 shows the relationship between the gradualness of voltage application and the crack occurrence rate.

【表】 この表に示す通り電圧の印加が緩やかであれば
クラツク発生率が小さく電圧印加条件が15V/分
を越えるとクラツクが多発し、10V/分以下では
非常にクラツクが少ない。 以下実施例により本発明を説明する。 実施例 1 第1図に示すように直径2インチのLiTaO3
結晶のZ軸の両端に電極4を設け、電気炉2内に
挿入し、650℃まで加熱する。その後、スイツチ
7を入れ、電圧6を10V/分の割合で徐々に昇圧
し、60Vになるまで昇圧を続ける。650℃60Vの条
件で20分間の処理を行つた後200℃/時間で降温
させる。このようにしてn=800個の単一分極化
処理を行つたところ4個がクラツクしていた。 実施例 2 実施例1と同様に2インチのLiTaO2単結晶の
Z軸の両端に電極4を設け、電気炉2内に挿入し
700℃まで加熱する。その後スイツチ7を入れ電
圧6を15V/分の割合で昇上し、60Vになるまで
昇圧を続ける。700℃60Vの条件で20分間の処理
を行つた後200℃/時間で降温させる。このよう
にしてn=600個の単一分極化処理を行つたとこ
ろ3個がクラツクしていた。 以上説明した通り、本発明はLiTaO3単結晶の
単一分極化方法において単極結晶に印加する電界
を緩やかに行うことに特徴を有するもので、本発
明によれば分極化処理における単結晶のクラツク
が大幅に減少する。
[Table] As shown in this table, if the voltage application is gentle, the crack occurrence rate is small; if the voltage application condition exceeds 15V/min, cracks occur frequently, and if the voltage application condition is 10V/min or less, there are very few cracks. The present invention will be explained below with reference to Examples. Example 1 As shown in FIG. 1, electrodes 4 were provided at both ends of the Z axis of a LiTaO 3 single crystal with a diameter of 2 inches, and the crystal was inserted into an electric furnace 2 and heated to 650°C. After that, switch 7 is turned on and voltage 6 is gradually increased at a rate of 10V/minute, and the voltage continues to increase until it reaches 60V. After processing for 20 minutes at 650°C and 60V, the temperature is lowered at 200°C/hour. When n=800 pieces were subjected to single polarization processing in this way, 4 pieces were cracked. Example 2 As in Example 1, electrodes 4 were provided at both ends of the Z axis of a 2-inch LiTaO 2 single crystal, and the material was inserted into an electric furnace 2.
Heat to 700℃. After that, switch 7 is turned on and voltage 6 is increased at a rate of 15V/minute, and continues to increase until it reaches 60V. After processing for 20 minutes at 700°C and 60V, the temperature is lowered at 200°C/hour. When n=600 single polarization processes were performed in this way, three cracks were found. As explained above, the present invention is characterized in that the electric field applied to the monopolar crystal is applied slowly in the single polarization method of LiTaO 3 single crystal. Cracks are significantly reduced.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図はLiTaO3単結晶の単一分極処理を行う
装置の概略図、第2図は従来のLiTaO3単結晶の
加熱曲線及び電圧印加特性を示す図、第3図は本
発明に係るLiTaO3単結晶の電圧印加特性を説明
する図である。
Figure 1 is a schematic diagram of an apparatus for single polarization treatment of LiTaO 3 single crystal, Figure 2 is a diagram showing the heating curve and voltage application characteristics of a conventional LiTaO 3 single crystal, and Figure 3 is a diagram showing the LiTaO according to the present invention. FIG . 3 is a diagram illustrating voltage application characteristics of a single crystal.

Claims (1)

【特許請求の範囲】[Claims] 1 リチウムタンタレート(LiTaO3)単結晶の両
端に電界印加のための電極を設け、前記単結晶を
所定の温度に加熱し、この所定温度において前記
単結晶に所定の電界を印加する工程を有する単結
晶の単一分域化方法において、前記所定の電界の
印加のために電圧を上昇するときの割合は1分間
に15V以下の割合であることを特徴とするリチウ
ムタンタレート単結晶の単一分域化方法。
1. Providing electrodes for applying an electric field at both ends of a lithium tantalate (LiTaO 3 ) single crystal, heating the single crystal to a predetermined temperature, and applying a predetermined electric field to the single crystal at this predetermined temperature. In the method for single-segmenting a single crystal, the voltage is increased at a rate of 15 V or less per minute for applying the predetermined electric field. Regionalization method.
JP56147012A 1981-09-19 1981-09-19 Single domain formation of lithium tantalate single crystal Granted JPS5849696A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP56147012A JPS5849696A (en) 1981-09-19 1981-09-19 Single domain formation of lithium tantalate single crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP56147012A JPS5849696A (en) 1981-09-19 1981-09-19 Single domain formation of lithium tantalate single crystal

Publications (2)

Publication Number Publication Date
JPS5849696A JPS5849696A (en) 1983-03-23
JPS6234718B2 true JPS6234718B2 (en) 1987-07-28

Family

ID=15420548

Family Applications (1)

Application Number Title Priority Date Filing Date
JP56147012A Granted JPS5849696A (en) 1981-09-19 1981-09-19 Single domain formation of lithium tantalate single crystal

Country Status (1)

Country Link
JP (1) JPS5849696A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0168628U (en) * 1987-10-27 1989-05-02

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5932438B2 (en) * 1976-11-22 1984-08-08 株式会社東芝 Single crystal single domainization method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0168628U (en) * 1987-10-27 1989-05-02

Also Published As

Publication number Publication date
JPS5849696A (en) 1983-03-23

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