JPS58217497A - Method for converting oxide single crystal to single domain crystal - Google Patents

Method for converting oxide single crystal to single domain crystal

Info

Publication number
JPS58217497A
JPS58217497A JP57098274A JP9827482A JPS58217497A JP S58217497 A JPS58217497 A JP S58217497A JP 57098274 A JP57098274 A JP 57098274A JP 9827482 A JP9827482 A JP 9827482A JP S58217497 A JPS58217497 A JP S58217497A
Authority
JP
Japan
Prior art keywords
crystal
single crystal
powder
domain
electrodes
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.)
Pending
Application number
JP57098274A
Other languages
Japanese (ja)
Inventor
Yasuo Nojo
野条 靖雄
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.)
Proterial Ltd
Original Assignee
Hitachi Metals 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 Hitachi Metals Ltd filed Critical Hitachi Metals Ltd
Priority to JP57098274A priority Critical patent/JPS58217497A/en
Publication of JPS58217497A publication Critical patent/JPS58217497A/en
Pending legal-status Critical Current

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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

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  • 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)

Abstract

PURPOSE:To decrease the deterioration layer in the surface of a crystal in the stage of converting the multi-domain single crystal of an oxide ferrodielectric and to improve yield by sticking electrodes to said crystal by means of powder or a sintered body of the same material as the material of the single crystal and having two kinds of grain sizes and viscosities. CONSTITUTION:Arc-shaped platinum electrodes 2, 2' are provided on both side surfaces corresponding to the Z face of a crystal grown in an X-axis direction in the stage of applying a specified voltage in the Z-axis direction and converting said crystal to a single domain crystal. A mixture of powder of lithium tantalate which is the same material as the material of a single crystal of, for example, LiTaO3 which is a single crystal of ferrodielectric oxide and starch is prepd. into a paste with water and such paste is used as an electrode material in said stage. An electrode material 4 of a low viscosity kneaded with the powder of lithium tantalate and the powder of starch having fine grains is coated on both side surfaces of the single crystal 1 and the contact surfaces of the electrodes 2, 2' and an electrode material 5 of a high viscosity using lithium tantalate having coarse grain sizes is coated between the electrode materials 4 and 4. The entire part is thus formed to a uniform thickness so that an electric field is applied uniformly thereon.

Description

【発明の詳細な説明】 本発明は強誘電体酸化物11i結晶の単分域化方法に関
するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for forming a ferroelectric oxide 11i crystal into a single domain.

強誘電体単結晶を単分域化J−るいわゆるポーリングは
よく知られている。単分域化yj法としくは種々の報告
がなされているが、結晶と電極の固着プ〕法として、適
当なブロックに切断加工したものに電極をつける場合と
、育成した結晶に加]−を流さずイのまま電極づけづる
場合とに大別される。
So-called poling, in which a ferroelectric single crystal is made into a single domain, is well known. Various reports have been made regarding the single-domain yj method, but as a method for fixing crystals and electrodes, there are cases in which electrodes are attached to blocks cut into appropriate blocks, and methods in which electrodes are attached to blocks that have been cut into suitable blocks, and cases in which electrodes are attached to a grown crystal. There are two main types: cases in which the electrodes are attached without flowing water, and cases in which the electrodes are attached as they are.

前者の場合には、結晶部分か多く(さ歩+、1’(It
(1・の原因とイrす、後者の場合に1.!、たとえば
白金電444の表面にA(J−PCIベース1〜舌を塗
イIIシ(電界をか(ノるど結晶表面に変質層か多数で
きるたvノーどの部分を切りどる必要があり、これが歩
留低下の原因と/【−1た。
In the former case, the crystalline part is large (Saho+, 1'(It
(If the cause is 1., in the latter case 1.!, for example, apply A (J-PCI base 1 to tongue) to the surface of platinum electrode 444. Many deteriorated layers were formed and it was necessary to cut off which part, which caused a decrease in yield.

上記の欠点を改良する方法として上記ベースl−を用い
ることなく、単分域化する結晶と同じ+J ’LQの粉
末を曲の物質(たどえばFlね)とよUだ電極剤と結晶
の間にいれC単分域化りる方法がある。
As a method to improve the above-mentioned drawbacks, without using the base l-, the powder of +J'LQ, which is the same as the crystal to be made into a single domain, is used as a material (for example, Fl) and the electrode material and the crystal. There is a way to make it into a single C domain.

この場合には結晶表面の変質は少なくなるが、−されで
もなJ5、結晶表面とこの粉末との間の畜り性が悪く、
したがって結晶表向に均一な電界がかからず部分的に変
質層が出来たり、またはクラックが発生する等の欠点が
あった。
In this case, the alteration of the crystal surface is reduced, but the stability between the crystal surface and this powder is poor.
Therefore, a uniform electric field is not applied to the surface of the crystal, resulting in the formation of a partially degraded layer or the occurrence of cracks.

本発明は1記従来技術の欠点を改良し、単分域化の際の
結晶表面の変質層を少なくし、歩留を向上−Cさる酸化
物単結晶の単分域化方法をJIB供することを目的とす
るしのて゛ある。
The present invention improves the drawbacks of the prior art described in 1 above, reduces the altered layer on the crystal surface during single domain formation, and improves the yield. There is a purpose for this purpose.

すなわら、本発明は多分域化単結晶と電極どの間に単結
晶と同じltA KAで 2種類の粒1旦をもらか2 つ(れそれが異−)た粘度をもつ状態で・固盾しく単分
域化処理を1′」うことを1;’r 倣どりるしのであ
る。
In other words, in the present invention, two types of grains with the same ltA KA as the single crystal are placed between the multi-area single crystal and the electrode, and then the grains are solidified in a state with different viscosities. In order to protect the single-domain processing, it is possible to imitate it.

たとえば、表向弾性波材わ1どしく近年性1]されCい
るL 1−1−aQ  単結晶について以−トに説明−
リ−る。
For example, the L 1-1-aQ single crystal, which is a surface acoustic wave material that has recently been developed, will be explained below.
Lee.

第1図はX軸方向に育成し1JfIIJ品を7軸1ノ向
に一定電圧をか−り単分域化りる場合の説明図(ある。
FIG. 1 is an explanatory diagram of the case where a 1JfIIJ product grown in the X-axis direction is made into a single domain by applying a constant voltage in 7 axes and 1 direction.

電界をか【)る方向はZ方向である1、結晶の/而にあ
Iこる両側面に円弧状の白金電極2.2′をa5J <
jる。この際、白金電極2,2−ど結晶1どの間にタン
タル酸すチュウムのわ)未く粒子イ0.1・〜50μm
 )とivl粉とを混合し、水Cのり状にしたしの4電
極剤としてtUいる。この場合、粒径が人きりぎたり、
水の焔が多ケ♂′でな1性が小8づざるど、結晶の表面
の凹凸ど上記電極剤の厚みが小さくなって、第2図に示
づ様な変質層3が(さる3、シかるに、この電極剤の富
者をよりシシかも電極と結晶どのスペースを一定に保つ
ために、第3図に示すように3層のタンタル酸すヂュウ
ムの粉により形成された電極剤4.5をスベーリーーに
しく配置りる際、5の電極剤として、(り平均粒径30
fノロ1以」−の粒度をもつタンタル酸すヂュウムの粉
末’a H粉ど)1シ合し水でのり上にしたもの、また
は(多上記3071m以上の粉末を所定の形状にプレス
し1,4oo ′c以上のkQ 瓜”C仮焼したものを
用い、これらと電14! 2 。
The direction in which the electric field is applied is the Z direction.Arc-shaped platinum electrodes 2.2' are placed on both sides of the crystal.
jru. At this time, between the platinum electrodes 2, 2 and the crystal 1, particles of tantalate (0.1 to 50 μm) are present.
) and ivl powder are mixed and made into a paste-like form as a 4-electrode agent. In this case, the particle size may be too large or
Although the water flame is large and the 1 property is small, the thickness of the electrode material becomes small due to the irregularities on the surface of the crystal, and the altered layer 3 as shown in Fig. 2 is formed. However, in order to keep the space between the electrode and the crystal constant, the electrode material 4 is made of three layers of tantalate powder as shown in Figure 3. When arranging .5 in a smooth manner, as an electrode material of 5, (average particle size of 30
Sodium tantalate powder with a particle size of 1"-1" or more (such as powder 3071m or more) combined with water, or (1 powder of 3071m or more above) pressed into a specified shape. , using calcined melons with a kQ of 4oo'c or more, and heat them with 14!2.

2−とが接触りる部分は0.1  μm1以上のタンタ
ル酎リチウムの粉末を澱粉と十分)昆合し、水で少くと
も上記■よりも粘度を小さくした、のり状のスヘーリー
−1,、4−を電極2.2−に固着さけたものを用いる
。このJ、うにして、本発明ににれば単結晶と白金電極
板との間のタンタル配lノチウム粉末の電極剤がり−き
まなく充填されlζ状態どなり、しかも、全体に均一な
所定の厚さを形成4るノζめ結晶全体に電界が均一にが
がり、表面変質層が少なくかつクラックの生じない単分
域化が可能となった。
The part that contacts 2- is a paste-like shale-1, which is made by mixing tantalum lithium powder of 0.1 μm or more with starch and reducing the viscosity at least lower than the above ① with water. 4- is fixed to the electrode 2.2- is used. In this way, according to the present invention, the electrode material of the tantalum alloy powder between the single crystal and the platinum electrode plate is filled evenly and in a lζ state, and moreover, the predetermined thickness is uniform throughout the entire surface. The electric field spreads uniformly over the entire crystal, making it possible to form a single domain with fewer surface-altered layers and no cracks.

次に実施例により本発明を説明り−る。Next, the present invention will be explained by examples.

X軸方向に育成した大きざ5層mmφX 4 C)mm
lのLiTa0.単結晶を、あらがじめ分極方向がある
Z iql+ /J向をX線により決定りる31次に第
1図に承り如く、+−1−+−a o、  単結晶1の
/軸方向の両側Ffjに、粒度の細い(粒度0.1 以
1・)タンタル酸すチュウム粉末と澱わ)わ)木とを’
 ifa合し水とね・ノた粘性の低い電極剤を塗4+り
る。、白金電極2゜2−についても同様な方法で粒度の
細いタンタル酸リブニウム粉末を用い(’1 イ1+ 
?j’る。。
Size: 5 layers grown in the X-axis direction mmφX 4 C) mm
l of LiTa0. The Z iql+ /J direction of the single crystal, which already has a polarization direction, is determined by X-rays.31 Next, as shown in Figure 1, +-1-+-a o, the /axis direction of the single crystal 1. On both sides of Ffj, add tantalate powder with fine grain size (grain size 0.1 to 1) and wood.
Ifa, mix it with water and apply a low viscosity electrode agent. For the platinum electrode 2゜2-, fine-grained rhibium tantalate powder was used in the same manner ('1 I1+).
? j'ru. .

次に粒度の粗い(粒径30μn1以−1−)タンタル酸
リブニウム粉末を上記澱粉粉末とを)1へ合し、1−記
細い粉末の際より粘度の高いのり状のもの、もしくは所
定の形状にプレスし1.4(10℃以」、の81品C仮
焼して成型したもの5を」−記単結晶と電極どの間に3
層になる様に形成りる。′εの後、両電極間に一定の圧
力を加え室温で一定時間放置りる。
Next, a coarse-grained (particle size of 30 μn or more) livium tantalate powder is combined with the above starch powder into 1), and a glue-like material with a higher viscosity than the fine powder described in 1-1 or a predetermined shape is prepared. 81 items of 1.4 (10°C or higher) are calcined and molded.
Form into layers. After 'ε, a certain pressure is applied between both electrodes and the electrodes are left at room temperature for a certain period of time.

これを第3図の状態で電気炉に入れ、7 (10−・・
800℃まで昇温する。その後電極2,2′に接続した
リード線を通じて10・〜1!+V/amの直流ミル4
かけたまま、室)扁まて 30・〜40℃/′11の冷
k]速度で降下さU単分域化LiTa0ヨ 単結晶を得
l、−6一方、これに対し上記実施例と同様なX軸方位
に育成したl i l’a Q、単結晶を用い−c、l
 ’l’ill /’J向の両・側面に、上記実施例と
同様に2種類のゎ)末を用いることなく、1種類の粒度
の粉末−C且っ一層となる様に形成した電極っけの状態
C1上記実施例ど同条1′1.トC′加熱し自流電圧を
か(プC中分域化せしめたLiTaQ3単結晶を得た。
This was placed in an electric furnace in the state shown in Figure 3, and 7 (10-...
Raise the temperature to 800°C. After that, 10.~1! is passed through the lead wires connected to the electrodes 2 and 2'. +V/am DC mill 4
While still hanging, it was lowered at a cooling rate of 30-40°C/'11 to obtain a single crystal of LiTa0, -6, while the same as in the above example was obtained. Using l i l'a Q, single crystal grown in the X-axis direction, -c, l
On both sides in the 'l'ill/'J direction, electrodes were formed in a single layer using powder-C of one type of particle size instead of using two types of powder as in the above embodiment. Condition C1 The same article 1'1 in the above embodiment. A single crystal of LiTaQ3 was obtained by heating at C' and applying a self-current voltage to form a medium-domain region.

 ゛上記2つの実施例で7また単分域化単結晶の表面変
質層を調べた結果、第2図に承り様に後者の実施例°C
は、結晶の場所により 1・〜2111111の変質層
3があり多数の転位が12寮された。また白金電極には
霜色した反応生成物がf」着した。どころが本発明によ
る前者の実施例の方法では、単結晶ど電4−14の表面
どか電極剤により一1分に畜者しているため、表面の変
質層も少なく不均一ざをなくりことが出来lζ。
゛In addition, as a result of investigating the surface altered layer of the single domain single crystal in the above two examples, as shown in Figure 2, the latter example °C
Depending on the location of the crystal, there was an altered layer 3 of 1.~2111111, and a large number of dislocations were formed in 12 dormitory. In addition, a frost-colored reaction product was deposited on the platinum electrode. However, in the method of the former embodiment of the present invention, since the surface of the single crystal electrode 4-14 is removed in 11 minutes using an electrode agent, there is less altered layer on the surface and unevenness can be eliminated. is completed lζ.

以上説明した如く本発明方法によれば、単分域化による
結晶表面の変質層を少くすることが出来よた単分域化処
理によるクラックの発生もなく、歩留向上の効果が得ら
れる。
As explained above, according to the method of the present invention, it is possible to reduce the number of altered layers on the crystal surface due to the single-domain treatment, and there is no occurrence of cracks due to the single-domain treatment, resulting in the effect of improving the yield.

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

第1図は本発明の一実施例を承り説明図、第2図は他の
実施例による結晶表11の2買層−の生成状態を承り図
、第3図は本発明の実施′例にA; +、:Jる炉仲人
状態の3(明図である。 ’l : !i1結晶、2.2−:電(1′Iス、S)
;表面変質N。 4;細い粒度の電極剤、!J:、1li1いネ1γ反の
電極剤シ・Jl、゛二゛? 手続補正書(方式)57.12゜ 酸化物単結晶の単分域化方法 補11°をする者 事f1との閉11    才i’  j’l   出 
喚1 八    −fl   所  東上;(都千代I
l1区丸の胚河j“l」l音2壮名 相  +5081
 1.11°I傘属株式会社代   ノシ   古  
 jlll    与11゛       典   大
成   理   人 二
FIG. 1 is an explanatory diagram of one embodiment of the present invention, FIG. 2 is an explanatory diagram of the generation state of the second layer in crystal table 11 according to another embodiment, and FIG. 3 is an explanatory diagram of an embodiment of the present invention. A; +, :Juru furnace matchmaker state 3 (clear diagram. 'l: !i1 crystal, 2.2-: electricity (1'Isu, S)
;Surface alteration N. 4; Electrode agent with fine particle size! J:、1li1ine 1γantielectrode material shi・Jl、゛2゛? Procedural amendment (method) 57.12゜Method for converting oxide single crystal into single domain
Kan 1 8 -fl Tokoro Higashijo; (Miyakochiyo I
l1 Ku Maru's embryo river j "l" l sound 2 Some phase +5081
1.11°I Umbrella Co., Ltd. Noshi Furu
jllll Yo11゛ Nori Taisei Ritoji

Claims (1)

【特許請求の範囲】 1、酸化物強誘電イホ多分域単結晶に電極を同名しC単
分域化り−るのに筋1し、前記電極剤としく単結晶ど同
4A賀Cかつ2種類の粒度ど粘度を6つ粉末または焼結
体で同義づることを特徴どする強、、f、電体酸化物単
結晶の単分域化力1人。 2、上記酸化物は二Aブ酸リブニウムまた(まタンタル
酸すヂコウム−Cある時r[請求の範囲第1項記載の強
誘電体酸化物単結晶の単分域化り法。
[Claims] 1. It is reasonable to use the same name for the electrode in the oxide ferroelectric Iho multi-domain single crystal to make it into a C single-domain, and the electrode material is the same as the single crystal 4A, C and 2. 6 types of particle size and viscosity are synonymous with powder or sintered body, which is characterized by strong, f, single domain power of electric oxide single crystal. 2. The above-mentioned oxide may be livium dibutyrate or (studicium tantalate).
JP57098274A 1982-06-08 1982-06-08 Method for converting oxide single crystal to single domain crystal Pending JPS58217497A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP57098274A JPS58217497A (en) 1982-06-08 1982-06-08 Method for converting oxide single crystal to single domain crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57098274A JPS58217497A (en) 1982-06-08 1982-06-08 Method for converting oxide single crystal to single domain crystal

Publications (1)

Publication Number Publication Date
JPS58217497A true JPS58217497A (en) 1983-12-17

Family

ID=14215356

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57098274A Pending JPS58217497A (en) 1982-06-08 1982-06-08 Method for converting oxide single crystal to single domain crystal

Country Status (1)

Country Link
JP (1) JPS58217497A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62154406A (en) * 1985-12-26 1987-07-09 株式会社東芝 Single isolation of ferroelectric single crystal

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62154406A (en) * 1985-12-26 1987-07-09 株式会社東芝 Single isolation of ferroelectric single crystal

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