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JPS6234719B2 - - Google Patents
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JPS6234719B2 - - Google Patents

Info

Publication number
JPS6234719B2
JPS6234719B2 JP56195609A JP19560981A JPS6234719B2 JP S6234719 B2 JPS6234719 B2 JP S6234719B2 JP 56195609 A JP56195609 A JP 56195609A JP 19560981 A JP19560981 A JP 19560981A JP S6234719 B2 JPS6234719 B2 JP S6234719B2
Authority
JP
Japan
Prior art keywords
single crystal
temperature
electric field
litao
predetermined
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
JP56195609A
Other languages
Japanese (ja)
Other versions
JPS5899200A (en
Inventor
Kenji Enokida
Yoshinori Okada
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 JP56195609A priority Critical patent/JPS5899200A/en
Publication of JPS5899200A publication Critical patent/JPS5899200A/en
Publication of JPS6234719B2 publication Critical patent/JPS6234719B2/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)
  • Inorganic Insulating Materials (AREA)

Description

【発明の詳細な説明】 発明の技術分野 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。
[Detailed Description of the Invention] Technical Field of the Invention The present invention relates to lithium tantalate (hereinafter referred to as LiTaO 3
) relates to a single domain method for single crystals.

発明の技術的背景と問題点 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)。
Technical Background and Problems of the Invention It is known to single-domain a LiTaO 3 single crystal. (Special Publication No. 47-8450, Japanese Patent Publication No. 15196-1974, etc.).

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t2
までの保持温度はキユリー点TCより高い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から温度を降下させ、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。
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 to t 2
The holding temperature is up to 650℃, which is higher than the Curie point TC.
The temperature drop is 200°C/hour. A voltage is applied at t 1 20 minutes after the time t 0 when the temperature is maintained at a constant temperature, the temperature is lowered from t 2 after another 20 minutes, and the voltage is turned off at t 3 one hour after t 1 . With the above operations
Single domainization of LiTaO 3 single crystal is completed.

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がある。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。
Now, the single polarization obtained in this way
In LiTaO 3 single crystal, cracks in the single crystal may be 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 about 5%.

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。
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.

発明の目的 本発明は上記欠点をなくすためになされたもの
でクラツクの少ないLiTaO3単結晶の単一分域化
方法を提供することを目的とする。
OBJECTS OF THE INVENTION The present invention was made in order to eliminate the above-mentioned drawbacks, and an object thereof is to provide a method for forming a LiTaO 3 single crystal into a single domain with fewer cracks.

発明の概要 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。
Summary of the Invention The inventors conducted experimental research on various factors in the polarization method in order to reduce cracks after polarization, and discovered that the voltage application conditions of the single crystal were also a cause of the cracks. Completed the invention.

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
加は前記単結晶の温度が500℃以下のときに開始
することを特徴とするLiTaO3単結晶の単一分極
化方法である。
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. A method for single-domaining a LiTaO 3 single crystal, characterized in that application of the predetermined electric field starts when the temperature of the single crystal is below 500°C. .

数多くの実験の結果、所定の電界印加を開始す
るときの単結晶の温度はクラツク発生率に関係し
ていることを見出した。第3図に実験により求め
た電界印加が開始するときの単結晶の温度とクラ
ツク発生率との関係を示す。
As a result of numerous experiments, it has been found that the temperature of the single crystal at the start of application of a predetermined electric field is related to the crack generation rate. FIG. 3 shows the relationship between the temperature of the single crystal at the start of electric field application and the crack occurrence rate, which was determined through experiments.

図から明らかなように所定電界の印加は単結晶
の温度が500℃以下のときクラツク発生率が減少
し、400℃以下では著しく減少することがわか
る。
As is clear from the figure, when a predetermined electric field is applied, the crack occurrence rate decreases when the temperature of the single crystal is below 500°C, and decreases significantly when the temperature of the single crystal is below 400°C.

発明の実施例 以下実施例により本発明を説明する。Examples of the invention The present invention will be explained below with reference to Examples.

第1図に示すように直径2インチのLiTaO3
結晶3のZ軸の両端に電極4、電気炉2内に挿入
し、スイツチ7を投入してリード線5から電圧を
60V印加する。次に電気炉2のヒータ1に通電
し、徐々に熱して炉温を高める。単結晶温度が
650℃になつたら20分間維持すると単結晶はほゞ
単一分域化される。その後炉温を徐々に下降させ
単結晶温度が150℃になつたら電界の印加をやめ
60℃になつてから単結晶を取り出すことにより単
一分域化処理は終了する。
As shown in Fig. 1, electrodes 4 are placed on both ends of the Z axis of a LiTaO 3 single crystal 3 with a diameter of 2 inches, and the electrodes 4 are inserted into the electric furnace 2, and the switch 7 is turned on to apply voltage from the lead wire 5.
Apply 60V. Next, the heater 1 of the electric furnace 2 is energized and gradually heated to raise the furnace temperature. single crystal temperature
Once the temperature reaches 650°C, maintain it for 20 minutes, and the single crystal will become almost a single domain. After that, gradually lower the furnace temperature and stop applying the electric field when the single crystal temperature reaches 150℃.
The single-domaining process is completed by taking out the single crystal after the temperature reaches 60°C.

この方法により得られた単結晶のクラツク発生
率は約2%であつた。
The crack occurrence rate of the single crystal obtained by this method was about 2%.

以上の実施例では電気炉の昇温開始前に単結晶
への電界の印加を開始したが、電気炉の昇温途中
であつても500℃以下のときに開始すればクラツ
ク発生率は減少する。
In the above example, the electric field was started to be applied to the single crystal before the temperature of the electric furnace started to rise, but even if the electric field is in the middle of heating up the electric furnace, if it starts when the temperature is below 500℃, the crack occurrence rate will be reduced. .

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

第1図はLiTaO3単結晶の単一分域化を行う装
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図は電界
印加を開始するときの単結晶の温度とクラツク発
生率との関係を示す図である。
Figure 1 is a schematic diagram of the device for single-domaining LiTaO 3 single crystal, Figure 2 is a diagram showing the heating curve and voltage application characteristics of conventional LiTaO 3 single crystal, and Figure 3 is when electric field application starts. FIG. 3 is a diagram showing the relationship between the temperature of a single crystal and the crack occurrence rate when

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
印加は前記単結晶の温度が500℃以下のときに開
始す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. A method for single-segmenting a lithium tantalate single crystal, characterized in that application of the predetermined electric field starts when the temperature of the single crystal is 500° C. or lower.
JP56195609A 1981-12-07 1981-12-07 Forming method for single crystal of lithium tantalate into single domain Granted JPS5899200A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP56195609A JPS5899200A (en) 1981-12-07 1981-12-07 Forming method for single crystal of lithium tantalate into single domain

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP56195609A JPS5899200A (en) 1981-12-07 1981-12-07 Forming method for single crystal of lithium tantalate into single domain

Publications (2)

Publication Number Publication Date
JPS5899200A JPS5899200A (en) 1983-06-13
JPS6234719B2 true JPS6234719B2 (en) 1987-07-28

Family

ID=16344001

Family Applications (1)

Application Number Title Priority Date Filing Date
JP56195609A Granted JPS5899200A (en) 1981-12-07 1981-12-07 Forming method for single crystal of lithium tantalate into single domain

Country Status (1)

Country Link
JP (1) JPS5899200A (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11236298A (en) * 1997-12-05 1999-08-31 Crystal Technol Inc Crystal for use in photolithographic process and preconditioning method of the same, for enhancing capability of absorbing electromagnetic radiation

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

Also Published As

Publication number Publication date
JPS5899200A (en) 1983-06-13

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