JPH01100100A - Single domain of oxide single crystal - Google Patents
Single domain of oxide single crystalInfo
- Publication number
- JPH01100100A JPH01100100A JP25854087A JP25854087A JPH01100100A JP H01100100 A JPH01100100 A JP H01100100A JP 25854087 A JP25854087 A JP 25854087A JP 25854087 A JP25854087 A JP 25854087A JP H01100100 A JPH01100100 A JP H01100100A
- Authority
- JP
- Japan
- Prior art keywords
- ingot
- single crystal
- domain
- heater
- powder
- 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
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 18
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 11
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920002678 cellulose Polymers 0.000 claims abstract description 6
- 239000001913 cellulose Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 abstract description 8
- 229910012463 LiTaO3 Inorganic materials 0.000 abstract description 3
- 239000004020 conductor Substances 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 2
- 229910003327 LiNbO3 Inorganic materials 0.000 abstract 1
- 230000005611 electricity Effects 0.000 abstract 1
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
Description
【発明の詳細な説明】
〔概要〕
特にニオブ酸リチウム（ＬｉＮｂ０３）単結晶のインゴ
ットまたはタンタル酸リチウム（ＬｉＴａＯｓ）単結晶
のインゴットを単一分域化させる処理方法の改良に関し
、
従来より長い柱状単結晶の分域処理を可能にすると共に
、分域処理用ヒータを長寿命化にすることを目的とし、
単一分域処理する酸化物単結晶のインゴットとほぼ同じ
成分の粉末と、メチルエチルケトンと、ジブチルフタレ
ートと、セルロースとを混合した導体ペーストを介して
一対の電極で該インゴット挟み、
該単結晶のキューリ点を越える温度雰囲気中で該電極に
単一分域電圧を印加することを特徴とし構成する。[Detailed Description of the Invention] [Summary] In particular, the present invention relates to an improvement in a processing method for converting a lithium niobate (LiNb03) single crystal ingot or a lithium tantalate (LiTaOs) single crystal ingot into a single domain. In order to enable domain treatment of crystals and to extend the life of the heater for domain treatment, we used powder with almost the same composition as the oxide single crystal ingot to be subjected to single domain treatment, methyl ethyl ketone, The ingot is sandwiched between a pair of electrodes via a conductive paste containing a mixture of dibutyl phthalate and cellulose, and a single domain voltage is applied to the electrodes in an atmosphere at a temperature exceeding the Curie point of the single crystal. do.
本発明は酸化物単結晶、特にニオブ酸リチウム（ＬｉＮ
ｂＯｓ）単結晶のインゴットまたはタンタル酸リチウム
（ＬｉＴａＯｓ）単結晶のインゴットを単一分域化させ
る処理方法の改良に関する。The present invention is directed to oxide single crystals, especially lithium niobate (LiN).
The present invention relates to an improvement in a processing method for converting a single crystal ingot (bOs) or a single crystal ingot of lithium tantalate (LiTaOs) into a single domain.
ＬｉＮｂ０．単結晶およびＬｉＴａＯ３単結晶を育成し
たインゴットは、圧電振動子や弾性表面波フィルタ等の
素子基板とするため、薄く切断しウェーハを作成するに
先立って、育成中に生じた内部ひずみをアニールに依っ
て除去し、さらに分域を整える単一分域処理（ポーリン
グ）が行われる。LiNb0. The ingots grown with single crystals and LiTaO3 single crystals are used as substrates for devices such as piezoelectric vibrators and surface acoustic wave filters, so before they are cut into thin pieces and made into wafers, the internal strain generated during growth is removed by annealing. A single domain process (polling) is performed to remove and further cleanse the domain.
第２図は従来方法による分域処理を説明するための模式
側面図（イ）とその模式平面図（Ｕ）である。FIG. 2 is a schematic side view (A) and a schematic plan view (U) for explaining the domain processing according to the conventional method.
第２図において、ＬｉＮｂ０．またはＬｉＴａＯ５辱に
てなる酸化物単結晶°のインゴット１は、分域を単一化
する処理に先立ってほぼ円柱状に形状を整え、その−側
を全長に渡り除去した平面１ａを形成する。In FIG. 2, LiNb0. Alternatively, an oxide single crystal ingot 1 made of LiTaO5 is shaped into a substantially cylindrical shape prior to the treatment to unify the domain, and its negative side is removed over its entire length to form a plane 1a.
分域処理装置の台８に搭載し白金（Ｐ ｔ）にてなる箱
形電極２には、インゴット１と同じＬｉＮｂＯ５または
ＬｉＴａＯ３単結晶の粉末を半焼成したセラミック板３
を収容し、インゴット１と同じＬｉＮｂＯ５またはＬｉ
ＴａＯ３単結晶の粉末４を入れ、その粉末４の上に平面
１ａが上向きとなるようにインゴット１を寝かせた状態
に搭載する。A box-shaped electrode 2 made of platinum (Pt) mounted on the stand 8 of the zone treatment device is equipped with a ceramic plate 3 made of semi-sintered LiNbO5 or LiTaO3 single crystal powder, which is the same as the ingot 1.
The same LiNbO5 or Li as ingot 1
TaO3 single crystal powder 4 is put therein, and the ingot 1 is placed in a lying state on top of the powder 4 so that the plane 1a faces upward.
次いで、平面１ａには粉末４を介してセラミック板３を
搭載し、その上にｐｔ電極５を搭載し、一対の対向電極
２と５を電源６に接続する。Next, a ceramic plate 3 is mounted on the flat surface 1a via a powder 4, a PT electrode 5 is mounted thereon, and a pair of opposing electrodes 2 and 5 are connected to a power source 6.
このようなインゴット１は、ヒータ７に通電しインゴッ
トｌのキューリ点を少し越える温度で適宜の時間だけ、
例えばインゴットｌがＬｉＮｂ０１にてなり直径が１５
０ｎｕｓ程度のときは１２００’Ｃで４時間程度加熱す
ると、図中に矢印で示すようにインゴットｌの長さ方向
（結晶の２軸方向）に単一分域Ｐｓが形成される。Such an ingot 1 is heated at a temperature slightly exceeding the Curie point of the ingot 1 for an appropriate period of time by energizing the heater 7.
For example, ingot l is made of LiNb01 and has a diameter of 15
When the temperature is about 0 nus, heating at 1200'C for about 4 hours forms a single domain Ps in the length direction of the ingot 1 (in the direction of the two axes of the crystal) as shown by the arrow in the figure.
以上説明したように、円柱状インゴットの２軸方向に単
一分域Ｐｓを形成させようとすると、Ｚ軸に直交する方
向、即ちインゴットの円柱面を挟むように一対の分域電
極を接続する必要があり、かつ、インゴットと該電極と
の間にインゴットと同じ酸化物のセラミック板および粉
末を介在させる必要がある。As explained above, when trying to form a single domain Ps in two axial directions of a cylindrical ingot, a pair of domain electrodes are connected in a direction perpendicular to the Z-axis, that is, so as to sandwich the cylindrical surface of the ingot. It is necessary to interpose a ceramic plate and powder of the same oxide as the ingot between the ingot and the electrode.
そこで、設置スペースが狭くて済むためヒータが縦型で
ある従来の装置は、一対の電極が上下方向にインゴット
を挟む方式であり、かかる装置は細心の注意のもとに段
取りし操作するも、酸化物の粉末が散ってヒータの寿命
を損なうと共に、ヒータの直径をｄとしたとき、インゴ
ットの長さり、は直径ｄの２／３程度が限度となり、単
結晶の育成長さが単一分域処理によって制約されるとい
う問題点があった。Therefore, conventional equipment with vertical heaters, which require less space for installation, uses a method in which a pair of electrodes sandwich the ingot in the vertical direction. Although such equipment must be set up and operated with great care, The oxide powder scatters, impairing the life of the heater, and when the diameter of the heater is d, the length of the ingot is limited to about 2/3 of the diameter d, and the growth of a single crystal is limited to a single fraction. The problem was that it was restricted by area processing.
上記問題点の除去を目的とした本発明方法は、第１図の
実施例によれば、単一分域処理する酸化物単結晶のイン
ボッＨ１とほぼ同じ成分の粉末と、メチルエチルケトン
と、ジブチルフタレートと、セルロースとを混合した導
体ペースト１２を介して一対の電極１５でインゴット１
１を挟み、該単結晶のキエーり点を越える温度雰囲気中
で電極１５に単一分域電圧を印加することを特徴とする
酸化物単結晶の単一分域方法である。According to the embodiment shown in FIG. 1, the method of the present invention, which aims to eliminate the above-mentioned problems, uses a powder having almost the same components as the in-bore H1 of an oxide single crystal to be treated in a single domain, methyl ethyl ketone, and dibutyl phthalate. The ingot 1 is connected to a pair of electrodes 15 via a conductive paste 12 containing a mixture of cellulose and cellulose.
This is a single-domain method for oxide single crystals, which is characterized by applying a single-domain voltage to electrodes 15 in an atmosphere at a temperature exceeding the key point of the single crystal.
上記手段によれば、分域処理するインゴットとほぼ同じ
線分の粉末を含む導体ペーストを使用し、柱状インゴッ
トを直立姿態で分域処理可能としたことにより、インゴ
ットはその一側を削除して平面を形成する必要がなくな
り、縦型分域処理用ヒータの直径に制限されず長いイン
ゴットの分域処理が可能となり、インゴットと同じ粉末
の飛び散りがなくなってヒータの長寿命化が可能になっ
た。According to the above means, a conductive paste containing powder of almost the same line as the ingot to be subjected to area processing is used, and the columnar ingot can be subjected to area processing in an upright position, so that one side of the ingot can be removed. It is no longer necessary to form a flat surface, and long ingots can be processed in sections without being limited by the diameter of the vertical section processing heater, and the same powder as the ingot is no longer scattered, making it possible to extend the life of the heater. .
以下に、図面を用いて本発明方法の実施例を説明する。 Examples of the method of the present invention will be described below with reference to the drawings.
第１図は本発明方法の実施例による分域処理を説明する
ための模式側面図（イ）とその模式平面図（ＥＴ）であ
る。FIG. 1 is a schematic side view (A) and a schematic plan view (ET) for explaining domain processing according to an embodiment of the method of the present invention.
第１図において、ＬｉＮｂＯ５またはＬｉＴａ０＋にて
なる単結晶のインゴット１１は、分域処理に先立ってほ
ぼ円柱状にその形状を整え、インゴット１１と同じＬｉ
ＮｂＯ３またはＬｉＴａＯ５（酸化物単結晶）の粉末、
メチルエチルケトン、ジブチルフタレートセルロースを
混合した導体ペースト１２を、インゴット１１の円柱面
の対向する２ケ所に塗付する。 ′一方、分域処
理装置の台８にインゴット１１と同じ成分の単結晶の粉
末を半焼成したセラミック板１４を搭載し、セラミック
板１４の上にインゴット１１を搭載し、一対の導体ペー
スト１２には、ｐｔにてなり分域処理電源６に接続する
一対の電極１５を接合させる。In FIG. 1, a single-crystal ingot 11 made of LiNbO5 or LiTa0+ is shaped into a substantially cylindrical shape prior to domain treatment, and the same LiNbO5 or LiTa0+ ingot 11 is
NbO3 or LiTaO5 (oxide single crystal) powder,
A conductor paste 12 containing a mixture of methyl ethyl ketone and dibutyl phthalate cellulose is applied to two opposing locations on the cylindrical surface of the ingot 11. 'Meanwhile, a ceramic plate 14 made by semi-sintering single crystal powder having the same composition as the ingot 11 is mounted on the stage 8 of the zone processing device, the ingot 11 is mounted on the ceramic plate 14, and a pair of conductive pastes 12 are placed on the ingot 11. A pair of electrodes 15 connected to the domain processing power source 6 are connected using PT.
このようなインゴット１１は、ヒータ７に通電しインボ
ッ）１１のキューリ点を少し越える温度で適宜の時間だ
け加熱すると、図中に矢印で示すようにインゴットｌｌ
の長さ方向（結晶の２軸方向）の単一分域ｐｓが形成さ
れる。そして、インゴット１１の長さし！は、ヒータ７
の長さにより拘束されるがヒータ７の直径に拘束されず
、従って従来と同じヒータ７を使用するまたは、ヒータ
７と同じ直径で適当に長いヒータと交換するだけで、従
来のインゴット１より長いインゴット１１の分域処理が
可能になる。When such an ingot 11 is heated for an appropriate time at a temperature slightly exceeding the Curie point of the ingot 11 by energizing the heater 7, the ingot 11 is heated as shown by the arrow in the figure.
A single domain ps in the length direction (directions of the two axes of the crystal) is formed. And the length of the ingot is 11! is heater 7
It is restricted by the length, but not by the diameter of the heater 7. Therefore, by using the same heater 7 as the conventional one, or by simply replacing it with an appropriately long heater with the same diameter as the heater 7, the ingot 1 can be made longer than the conventional ingot 1. Domain processing of the ingot 11 becomes possible.
以上説明したように本発明方法によれば、分域処理する
円柱状インゴットは、その長さ方向をヒータの長さ方向
と同一の直立姿態に支持して分域処理するため、従来よ
りも長いものが分域処理できるようになり、生産性が著
しく向上されると共に、インゴットと電極との間には該
インゴットと同成分の粉末をペースト状にして介在させ
ることにより、該粉末がヒータの寿命を損なうという従
来の欠点をなくし得た効果がある。As explained above, according to the method of the present invention, the cylindrical ingot to be subjected to zone treatment is longer than the conventional method because it is supported in an upright position with its length direction being the same as the length direction of the heater. Productivity can be significantly improved by making it possible to process products in separate areas, and by interposing powder with the same composition as the ingot in the form of a paste between the ingot and the electrode, the powder can extend the life of the heater. This has the effect of eliminating the conventional drawback of damaging the
第１図は本発明方法の実施例による分域処理を説明する
ための図、
第２図は従来方法による分域処理を説明するための図、
である。
図中において、
６は分域処理電源、 ７はヒータ、
１１はインゴット、
１２はインゴットと同じ単結晶の粉末を含む導体ペース
ト、
１４はセラミック板、 １５は電極、Ｐｓは分極方向
、
を示す。
代理人 弁理士 井 桁 貞 −、パｊ＼
イ
１″：２
第２図FIG. 1 is a diagram for explaining domain processing according to an embodiment of the method of the present invention, and FIG. 2 is a diagram for explaining domain processing according to a conventional method. In the figure, 6 is a domain processing power supply, 7 is a heater, 11 is an ingot, 12 is a conductive paste containing the same single crystal powder as the ingot, 14 is a ceramic plate, 15 is an electrode, and Ps is a polarization direction. Agent Patent Attorney Sada Iji -, Paj＼ I1″:2 Figure 2
Claims (1)
とほぼ同じ成分の粉末と、メチルエチルケトンと、ジブ
チルフタレートと、セルロースとを混合した導体ペース
ト（１２）を介して一対の電極（１５）で該インゴット
（１１）を挟み、 該単結晶のキューリ点を越える温度雰囲気中で該電極（
１５）に単一分域電圧を印加することを特徴とする酸化
物単結晶の単一分域方法。[Claims] Oxide single crystal ingot subjected to single domain treatment (11)
The ingot (11) is sandwiched between a pair of electrodes (15) via a conductive paste (12) made of a mixture of powder having almost the same composition as , methyl ethyl ketone, dibutyl phthalate, and cellulose, and the Curie point of the single crystal is The electrode (
15) A single domain method for an oxide single crystal, characterized in that a single domain voltage is applied to the oxide single crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25854087A JPH01100100A (en) | 1987-10-14 | 1987-10-14 | Single domain of oxide single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25854087A JPH01100100A (en) | 1987-10-14 | 1987-10-14 | Single domain of oxide single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01100100A true JPH01100100A (en) | 1989-04-18 |
Family
ID=17321646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25854087A Pending JPH01100100A (en) | 1987-10-14 | 1987-10-14 | Single domain of oxide single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01100100A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103266354A (en) * | 2013-06-08 | 2013-08-28 | 西安交通大学 | Polarization method for obtaining single-domain relaxor-based ferroelectric crystal |
-
1987
- 1987-10-14 JP JP25854087A patent/JPH01100100A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103266354A (en) * | 2013-06-08 | 2013-08-28 | 西安交通大学 | Polarization method for obtaining single-domain relaxor-based ferroelectric crystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH01100100A (en) | Single domain of oxide single crystal | |
| JP2015098410A (en) | Method of producing lithium tantalate single crystal substrate for elastic surface wave element and lithium tantalate single crystal substrate for elastic surface wave element | |
| JPS5933559B2 (en) | Single crystal manufacturing method | |
| CN1332078C (en) | Polarization method for lithium niobate | |
| KR950008736A (en) | Method for preparing single crystal of potassium niobate | |
| JPH0367999B2 (en) | ||
| JPH01172299A (en) | Polling method for lithium tantalate single crystal | |
| JPH01196878A (en) | Poling of lithium tantalate single crystal | |
| JP2508334B2 (en) | Piezoelectric substrate polarization method | |
| JPS57613A (en) | Liquid crystal display element | |
| JPS6148299A (en) | Manufacture of ultrasonic probe | |
| JP2910095B2 (en) | Piezoelectric element and method of manufacturing piezoelectric element | |
| JPS57140400A (en) | Formation of single domain in single crystal of ferroelectric substance | |
| JP2615019B2 (en) | Method for producing LiNbO single crystal piezoelectric substrate having domain-inverted region | |
| JPS6134279B2 (en) | ||
| JPH06191983A (en) | Production of oxide single crystal and apparatus therefor | |
| JPS63218599A (en) | Method for subjecting lithium tantalate single crystal to single domain | |
| JPS55166320A (en) | Frequency response adjusting method for piezo-electric ceramic filter element | |
| JPH04285025A (en) | Method for rendering single domain to piezoelectric single crystal | |
| JP2502608B2 (en) | Method for producing single-domain lithium tantalate single crystal | |
| JPS6335498A (en) | Method for making single domain lithium niobate single crystal | |
| JPS62154406A (en) | Single isolation of ferroelectric single crystal | |
| JPS63311808A (en) | Manufacture of vibration element | |
| JPH0265185A (en) | Manufacture of circular piezoelectric vibrator | |
| JPS61155300A (en) | Transformation of lithium tantalate single crystal to single zone |