JP2502608B2 - Method for producing single-domain lithium tantalate single crystal - Google Patents

Method for producing single-domain lithium tantalate single crystal

Info

Publication number
JP2502608B2
JP2502608B2 JP62180836A JP18083687A JP2502608B2 JP 2502608 B2 JP2502608 B2 JP 2502608B2 JP 62180836 A JP62180836 A JP 62180836A JP 18083687 A JP18083687 A JP 18083687A JP 2502608 B2 JP2502608 B2 JP 2502608B2
Authority
JP
Japan
Prior art keywords
single crystal
lithium tantalate
domain
crystal
electrode plate
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 - Lifetime
Application number
JP62180836A
Other languages
Japanese (ja)
Other versions
JPS6424096A (en
Inventor
正美 寺島
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.)
Shin Etsu Chemical Co Ltd
Original Assignee
Shin Etsu Chemical 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 Shin Etsu Chemical Co Ltd filed Critical Shin Etsu Chemical Co Ltd
Priority to JP62180836A priority Critical patent/JP2502608B2/en
Publication of JPS6424096A publication Critical patent/JPS6424096A/en
Application granted granted Critical
Publication of JP2502608B2 publication Critical patent/JP2502608B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は単一分域化されたタンタル酸リチウム単結晶
の製造方法、特には単結晶側面に電極板を対向配置し、
通電によりタンタル酸リチウム単結晶を単一分域化する
方法の改良に関するものである。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing a single-domainized lithium tantalate single crystal, in particular, an electrode plate is arranged opposite to a side surface of the single crystal.
The present invention relates to an improvement in a method for dividing a lithium tantalate single crystal into a single domain by energization.

(従来の技術) 従来、チョクラルスキー法によるX軸方向に引き上げ
たタンタル酸リチウム単結晶を単一分域化する方法とし
ては、引き上げ単結晶の側面すなわちZ軸方向の面にた
とえば帯状の形状をした正負電極を単結晶を挟むように
して対向配置し、キューリー温度以上一般には610℃以
上の温度に加熱しながら両電極間に電圧を印加すること
により単一分域化する方法が知られている。
(Prior Art) Conventionally, as a method for domain-dividing a lithium tantalate single crystal pulled in the X-axis direction by the Czochralski method, a side surface of the pulled single crystal, that is, a surface in the Z-axis direction, for example, has a strip shape. A method is known in which positive and negative electrodes are placed opposite to each other so as to sandwich a single crystal, and a voltage is applied between both electrodes while heating to a temperature not lower than the Curie temperature, generally 610 ° C. or higher, thereby forming a single domain. .

しかして、この方法においてはこの電極板として通常
白金が使用されているが、これには単結晶への白金電極
のくみ込みがあるために単結晶が白金によって汚染され
るおそれがあるし、この場合には単結晶全体に均一に電
界をかけることが難しく、得られる単結晶が結晶欠陥を
もつものになるという不利があることから、この単結晶
と白金電界板との間にこの結晶と同種の粉末を充填して
通電するという方法が提案されており(特公昭59-51156
号公報参照)、これによれば単結晶の白金による汚染が
防止されるし、単結晶全体に均一に電界をかけることが
できるので結晶欠陥の少ない単一分域化結晶を得ること
ができるとされているけれども、これには単結晶と白金
電極板の間に充填するものが単結晶と同種の粉末とされ
るので極めて高価なものになるという経済的な不利があ
るほか、この粉末には組成変動があるし、この粉末は単
結晶、白金電極板との密着性がわるいので白金電極板に
印加された電圧が単結晶に均一に伝導されず、単一分域
化が必ずしも良好に行われず、得られる単結晶の単一分
域化にバラツキが発生するという問題点がある。
In this method, however, platinum is usually used as the electrode plate, but there is a risk that the single crystal may be contaminated by platinum because of the inclusion of the platinum electrode in the single crystal. In this case, it is difficult to apply an electric field uniformly to the entire single crystal, and the resulting single crystal has the disadvantage of having crystal defects. A method has been proposed in which the powder of the above is filled and electricity is applied (Japanese Patent Publication No. 59-51156).
According to this, it is possible to prevent contamination of the single crystal with platinum and to apply a uniform electric field to the entire single crystal, and thus to obtain a single-domain crystal with few crystal defects. However, this has the economical disadvantage that it becomes extremely expensive because the material filled between the single crystal and the platinum electrode plate is the same kind of powder as the single crystal, and this powder also has a compositional variation. However, since this powder is a single crystal, the adhesion to the platinum electrode plate is poor, so the voltage applied to the platinum electrode plate is not uniformly conducted to the single crystal, and single domainization is not always performed well, There is a problem in that the obtained single crystal has variations in forming a single domain.

(発明の構成) 本発明はこのような不利を解決した単一分域化タンタ
ル酸リチウム単結晶の製造方法に関するものであり、こ
れはチョクラルスキー法で引き上げ成長させたタンタル
酸リチウム単結晶の側面に正負電極を対向設置し、単結
晶体と電極体との間に炭素からなる繊維状、フェルト
状、不織布状またはクロス状に成形された導電性材料を
充填し、両電極間に電圧を印加して単一分域化すること
を特徴とするものである。
(Structure of the Invention) The present invention relates to a method for producing a single-domain domain lithium tantalate single crystal in which such disadvantages are solved, and it relates to a lithium tantalate single crystal pulled up and grown by the Czochralski method. Positive and negative electrodes are installed opposite to each other on the side surface, and a conductive material formed of carbon in a fibrous, felt, non-woven or cross shape is filled between the single crystal body and the electrode body, and a voltage is applied between both electrodes. It is characterized in that it is applied to form a single domain.

すなわち、本発明者らは従来公知のタンタル酸リチウ
ム単結晶の単一分域化方法における不利を解決する方法
について種々検討した結果、単結晶と白金電極板との間
に充填される充填材を炭素からなる導電性材料を繊維
状、フェルト状、不織布状またはクロス状に成形したも
のとすると、このものはタンタル酸リチウムとは反応し
ない化学的な安定なものであるし、柔軟性をもつ成形材
料で単結晶および白金電極とよく密着するので単結晶に
対する電圧の印加が均一となり、したがって得られる単
結晶の単一分域化はバラツキのない均一なものになると
いうことを見出し、これによれば充填材が成形された炭
素と入手し易い安価なものであることから充填材として
タンタル酸単結晶の粉末を使用する公知の方法にくらべ
て著しい経済的な有利性が得られること、また、この成
形された充填材は柔軟性をもっているので密着性がよ
く、凹凸のある単結晶にもよく密着するので良質な単一
分域化されたタンタル酸リチウム単結晶を与えることを
確認し、ここに使用する充填材の種類、形状、構造につ
いての研究を進めて本発明を完成させた。
That is, as a result of various studies on the method of solving the disadvantage in the conventionally known single domainization method of lithium tantalate single crystal, the present inventors have found that the filler to be filled between the single crystal and the platinum electrode plate is When a conductive material made of carbon is molded into a fiber shape, felt shape, non-woven shape or cloth shape, this is a chemically stable material that does not react with lithium tantalate and has a flexible shape. It was found that the material is in good contact with the single crystal and the platinum electrode, so that the voltage application to the single crystal is uniform, and thus the obtained single crystal has a uniform domain with no variation. If the filler is formed carbon and it is easily available and inexpensive, it is significantly economically advantageous as compared with the known method using the powder of tantalic acid single crystal as the filler. In addition, since this molded filler has flexibility, it has good adhesiveness and also adheres well to uneven single crystals, so that a good single-domain lithium tantalate single crystal can be obtained. After confirming that it was given, the present invention was completed by conducting research on the type, shape, and structure of the filler used here.

本発明の方法で用いられるタンタル酸リチウム単結晶
はタンタル酸リチウム融液からチョクラルスキー法で引
き上げ成長させて得たものとすればよい。
The lithium tantalate single crystal used in the method of the present invention may be obtained by pulling and growing from a lithium tantalate melt by the Czochralski method.

また、このタンタル酸リチウム単結晶の単一分域化は
この単結晶の側面に正負の電極板を対向配置し、この電
極板に電圧を印加することによって行われるが、この電
極板は白金製、金製または銅に金メッキを施したもので
作ればよく、この形状は単結晶に密着させるために断面
円弧状のものとすればよい。
The single domainization of the lithium tantalate single crystal is performed by arranging positive and negative electrode plates facing each other on the side faces of the single crystal and applying a voltage to the electrode plate. It may be made of gold or copper plated with gold, and its shape may be arcuate in cross section so as to adhere to the single crystal.

本発明の方法はこのタンタル酸リチウム単結晶と電極
板との間に成形された導電性材料を充填するのである
が、この導電性材料は炭素とすればよく、その形状は電
極板の形状に合わせたものとすればよいが、このものは
繊維状、フェルト状、不織布状あるいはクロス状に成形
することがよく、このようにすれば柔軟性に富んだもの
となるので、単結晶、電極板との密着性がより高くなる
という有利性が与えられる。
The method of the present invention is to fill the conductive material formed between the lithium tantalate single crystal and the electrode plate, the conductive material may be carbon, the shape of which is the shape of the electrode plate. Although it may be combined, it is preferable to form this into a fibrous, felt-like, non-woven fabric-like or cloth-like form, which makes it highly flexible, so single crystal, electrode plate The advantage is that the adhesiveness with is higher.

つぎに本発明の方法を添付の図面にもとづいて説明す
る。第1図は本発明の方法によるタンタル酸リチウム単
結晶の単一分域化を示す縦断面図、第2図はこの横断面
図を示したものであり、この方法ではタンタル酸リチウ
ム単結晶1はアルミナなどで製られた支持台2に載置さ
れており、この単結晶の両側には断面が円弧状である白
金電極3、3′が取り付けられ、これはバンド5でおさ
えられていて、この単結晶1と白金電極3、3′との間
にはフェルト状またはクロス状に成形された炭素製の充
填材層4が設けられている。タンタル酸リチウム単結晶
の単一分域化(ポーリング)はこれらを加熱炉中に装入
に、所定温度、例えばキューリー温度である610℃以上
に加熱してからこの電極間に5〜25V/cmの電圧を印加す
ることによって行われるが、これによれば単結晶と電極
間とが柔軟性のある成形された導電性の充填材層を介し
て接続されているので単結晶に凹凸があっても充填材層
は単結晶に密着し、電極に印加された電圧は単結晶に均
一に印加されるので単結晶の単一分域化が均等に行われ
結晶欠陥が生じることもないし、この充填材層は数10回
にも繰返し使用することができるので、経済的効果も大
きいという有利性が与えられる。
Next, the method of the present invention will be described with reference to the accompanying drawings. FIG. 1 is a vertical sectional view showing a single domainization of a lithium tantalate single crystal according to the method of the present invention, and FIG. 2 is a transverse sectional view thereof. In this method, a lithium tantalate single crystal 1 Is placed on a support base 2 made of alumina or the like, and platinum electrodes 3, 3'having an arc-shaped cross section are attached to both sides of this single crystal, which are held by a band 5, Between the single crystal 1 and the platinum electrodes 3 and 3 ', a felt-like or cross-like carbon filler layer 4 is provided. Single domainization (poling) of lithium tantalate single crystal is carried out by charging them into a heating furnace and heating at a predetermined temperature, for example, Curie temperature of 610 ° C or higher, and then 5 to 25 V / cm between the electrodes. This is done by applying a voltage of 1. According to this, since the single crystal and the electrodes are connected through the flexible and formed conductive filler layer, the single crystal has irregularities. Also, since the filler layer adheres to the single crystal and the voltage applied to the electrode is uniformly applied to the single crystal, the single crystal is evenly divided into single domains and crystal defects do not occur. Since the material layer can be repeatedly used several tens of times, it is advantageous in that it has a large economic effect.

つぎに本発明の実施例をあげる。 Next, examples of the present invention will be described.

実施例1、比較例 チョクラルスキー法でX軸引上げを行ない成長させた
直径82mm、長さ135mmのタンタル酸リチウム単結晶体の
両端をカットして研磨加工を施し、この両側面のZ軸方
向に断面円弧状の白金電極板(円弧長さ50mm、高さ150m
m、厚さ0.5mm)を取り付けると共に、この単結晶体と白
金電極との間に炭素よりなる、厚さ7mmで標準重量が810
g/m2のフェルト状の成形体を充填して単結晶と白金電極
とをこの充填材層を介して密着させたのち、これを電気
炉中に装入して炉内を窒素ガス置換した後640℃に加熱
しながらこの電極体に110Vの電圧を印加して単結晶体の
単一分域化を行い、得られた単一分域化タンタル酸リチ
ウム単結晶の分域化均一性を結晶歪偏光検査器を用いて
しらべたところ、これには特性上問題となる不均一部の
存在しないことが確認された。
Example 1, Comparative Example A lithium tantalate single crystal body having a diameter of 82 mm and a length of 135 mm, which was grown by pulling up the X axis by the Czochralski method, was cut at both ends and subjected to polishing, and the Z axis direction on both side surfaces thereof. Platinum electrode plate with an arc cross section (arc length 50 mm, height 150 m
m, thickness 0.5mm), and made of carbon between this single crystal and the platinum electrode, thickness 7mm and standard weight 810
After filling a g / m 2 felt-like compact and closely contacting the single crystal and the platinum electrode via this filler layer, this was charged into an electric furnace and the inside of the furnace was replaced with nitrogen gas. After that, a voltage of 110 V was applied to this electrode body while heating at 640 ° C. to perform single domainization of the single crystal body, and to obtain domainization uniformity of the obtained single domainized lithium tantalate single crystal. When a crystal strain polarization tester was used, it was confirmed that there was no non-uniform portion, which is a problem in terms of characteristics.

しかし、比較のために上記における充填材としてタン
タル酸リチウム単結晶粉25gを用いることとしたが、こ
の場合には粉体であるために単結晶体と電極板との間に
良好に密着させることが困難なので、これをメチルセル
ロース系のバインダー(信越化学工業(株)製メトセル
SM50商品名)を使用してペースト状とし、これを厚さ約
3cmで電極板に密着させ、これについて上記と同様に処
理してタンタル酸リチウム単結晶体の単一分域化を行な
ったところ、この場合には上記ペーストの密着不良部分
に分域化均一性の不均一部の存在することが確認され、
これは単結晶体の断面積のおよそ10%程度存在するもの
であった。
However, for comparison, it was decided to use 25 g of lithium tantalate single crystal powder as the filler in the above, but in this case, since it is a powder, it is necessary to make good adhesion between the single crystal body and the electrode plate. Since this is difficult, use this as a methylcellulose-based binder (Metcel manufactured by Shin-Etsu Chemical Co., Ltd.).
(SM50 product name) made into a paste, and this is about the thickness
It was adhered to the electrode plate at 3 cm, and the same treatment as above was carried out to make a single domain of the lithium tantalate single crystal. It was confirmed that there was a non-uniform
This was about 10% of the cross-sectional area of the single crystal.

なお、このペースト状物を用いて電極板を密着させる
作業は約25分の時間を要したが、実施例におけるフェル
ト状成形物の取り付けは5分間で終了した。
The work of bringing the electrode plate into close contact with the paste-like product took about 25 minutes, but the felt-like molded product was attached in 5 minutes in the examples.

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

第1図は本発明の方法によるタンタル酸リチウム単結晶
の単一分域化方法を示す縦断面図、第2図はこの横断面
図を示したものである。 1、……タンタル酸リチウム単結晶、2、……支持台、
3、3′……白金電極、4、……充填材層、5、……バ
ンド。
FIG. 1 is a vertical sectional view showing a method for single domainization of a lithium tantalate single crystal according to the method of the present invention, and FIG. 2 is a transverse sectional view thereof. 1, ... Lithium tantalate single crystal, 2, ... Support base,
3, 3 '... Platinum electrode, 4, Filler layer, 5, Band.

Claims (1)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】チョクラルスキー法で引き上げ成長させた
タンタル酸リチウム単結晶の側面に正負電極を対向設置
し、単結晶体と電極体との間に炭素からなる繊維状、フ
ェルト状、不織布状またはクロス状に成形された導電性
材料を充填し、両電極間に電圧を印加して単一分域化す
ることを特徴とする単一分域化タンタル酸リチウム単結
晶の製造方法。
1. A positive electrode and a negative electrode are installed opposite to each other on the side surfaces of a lithium tantalate single crystal grown by pulling and growing by the Czochralski method, and a fibrous, felt-like, or non-woven fabric made of carbon is formed between the single crystal and the electrode body. Alternatively, a method for producing a single-domain domain lithium tantalate single crystal, which comprises filling a cross-shaped conductive material and applying a voltage between both electrodes to achieve a single domain domain.
JP62180836A 1987-07-20 1987-07-20 Method for producing single-domain lithium tantalate single crystal Expired - Lifetime JP2502608B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62180836A JP2502608B2 (en) 1987-07-20 1987-07-20 Method for producing single-domain lithium tantalate single crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62180836A JP2502608B2 (en) 1987-07-20 1987-07-20 Method for producing single-domain lithium tantalate single crystal

Publications (2)

Publication Number Publication Date
JPS6424096A JPS6424096A (en) 1989-01-26
JP2502608B2 true JP2502608B2 (en) 1996-05-29

Family

ID=16090207

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62180836A Expired - Lifetime JP2502608B2 (en) 1987-07-20 1987-07-20 Method for producing single-domain lithium tantalate single crystal

Country Status (1)

Country Link
JP (1) JP2502608B2 (en)

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61146796A (en) * 1984-12-14 1986-07-04 Shin Etsu Chem Co Ltd Method for making lithium tantalate single crystal into single domain
JPS61155300A (en) * 1984-12-26 1986-07-14 Shin Etsu Chem Co Ltd Transformation of lithium tantalate single crystal to single zone
JPS61155299A (en) * 1984-12-28 1986-07-14 Shin Etsu Chem Co Ltd Transformation of lithium tantalate single crystal to single zone
JPS61155298A (en) * 1984-12-28 1986-07-14 Shin Etsu Chem Co Ltd Transformation of lithium tantalate single crystal to single zone

Also Published As

Publication number Publication date
JPS6424096A (en) 1989-01-26

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