JPH05117096A - Method for growing thin film of lithium niobate single crystal - Google Patents
Method for growing thin film of lithium niobate single crystalInfo
- Publication number
- JPH05117096A JPH05117096A JP28456391A JP28456391A JPH05117096A JP H05117096 A JPH05117096 A JP H05117096A JP 28456391 A JP28456391 A JP 28456391A JP 28456391 A JP28456391 A JP 28456391A JP H05117096 A JPH05117096 A JP H05117096A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- thin film
- composition
- crystal
- lithium niobate
- 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
Landscapes
- Optical Integrated Circuits (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ニオブ酸リチウム単結
晶の薄膜の育成方法に関し、特に、液相エピタキシャル
法によってニオブ酸リチウム単結晶の薄膜を育成する方
法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for growing a lithium niobate single crystal thin film, and more particularly to a method for growing a lithium niobate single crystal thin film by a liquid phase epitaxial method.
【０００２】[0002]
【従来の技術】近年、ニオブ酸リチウム（ＬｉＮｂ
Ｏ3 ）単結晶は導波路型光スイッチ用基板材料としてそ
の応用が期待されている。この単結晶の製造方法として
はチョクラルスキー法が一般的である。ところで、従
来、この方法で得られるニオブ酸リチウム結晶の組成は
コングルエント（調和溶融）組成で、Ｌｉ／Ｎｂ＝０．
９４となり、リチウムが不足している。これによって、
導波路型光スイッチにおけるＤＣドリフト（駆動電圧の
変動）、光高調波発生時の光損傷閾値低下の原因になる
と考えられる。従って、Ｌｉ／Ｎｂ＝１．０のストイキ
オメトリー（化学量論）組成の結晶を用いた特性改善が
求められている。2. Description of the Related Art In recent years, lithium niobate (LiNb
O 3 ) single crystal is expected to be applied as a substrate material for a waveguide type optical switch. The Czochralski method is generally used as a method for producing this single crystal. By the way, conventionally, the composition of the lithium niobate crystal obtained by this method is a congruent (harmonic melting) composition, and Li / Nb = 0.
94, and there is a shortage of lithium. by this,
This is considered to be a cause of DC drift (fluctuation of drive voltage) in the waveguide type optical switch and reduction of the optical damage threshold value when optical harmonics are generated. Therefore, it is required to improve the characteristics by using a crystal having a stoichiometry (stoichiometry) composition of Li / Nb = 1.0.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、チョク
ラルスキー法でストイキオメトリー組成の結晶の育成を
行うためには、育成中に原料のチャージを行う必要があ
り、結晶の組成の制御が困難である。However, in order to grow a crystal having a stoichiometric composition by the Czochralski method, it is necessary to charge the raw materials during the growth, and it is difficult to control the composition of the crystal. is there.
【０００４】そこで、本発明の技術的課題は、上記問題
点を解決し、Ｌｉ／Ｎｂ＝１．０のストイキオメトリー
組成の結晶の薄膜を育成するため、所望の組成近傍にお
ける組成制御が容易な単結晶の薄膜の育成方法を得るこ
とである。Therefore, the technical problem of the present invention is to solve the above problems and to grow a thin film of a crystal having a stoichiometric composition of Li / Nb = 1.0, so that composition control in the vicinity of a desired composition is easy. To obtain a simple single crystal thin film growing method.
【０００５】[0005]
【課題を解決するための手段】本発明によれば、液相エ
ピタキシャル法によるニオブ酸リチウム単結晶の薄膜の
育成方法であって、融液の組成がＬｉ2 Ｏ：Ｎｂ2 Ｏ5
＝ｘ：（１−ｘ），０．４７≦ｘ≦０．６１とすること
を特徴とするニオブ酸リチウム単結晶の薄膜の育成方法
が得られる。According to the present invention, there is provided a method for growing a thin film of a lithium niobate single crystal by a liquid phase epitaxial method, wherein the composition of the melt is Li 2 O: Nb 2 O 5
= X: (1-x), 0.47 ≦ x ≦ 0.61 is obtained, and a method for growing a thin film of a lithium niobate single crystal is obtained.
【０００６】[0006]
【作用】融液組成をＬｉ2 Ｏ：Ｎｂ2 Ｏ5 ＝ｘ：（１−
ｘ），０．４７≦ｘ≦０．６１とし、モル比を可変する
ことによって、単結晶の薄膜のＬｉ2 Ｏ組成を４８％か
ら５１％の間で任意に制御する。The melt composition is changed to Li 2 O: Nb 2 O 5 = x: (1-
x), 0.47 ≤ x ≤ 0.61, and by varying the molar ratio, the Li 2 O composition of the single crystal thin film is arbitrarily controlled between 48% and 51%.
【０００７】[0007]
【実施例】以下に本発明の一実施例によるニオブ酸リチ
ウム単結晶の薄膜の育成方法を図面を用いて説明する。EXAMPLE A method for growing a thin film of lithium niobate single crystal according to an example of the present invention will be described below with reference to the drawings.
【０００８】単結晶の薄膜の製造方法である液相エピタ
キシャル法は、半導体結晶や磁性ガーネット結晶等の製
造に用いられ、図１は液相エピタキシャル法による単結
晶の薄膜の育成炉内の断面図である。図１に示すように
白金るつぼ１に保持された酸化リチウムと五酸化ニオブ
との融液７にニオブ酸リチウム結晶基板２を浸漬して所
望組成のニオブ酸リチウム単結晶の薄膜を育成する。The liquid phase epitaxial method, which is a method for manufacturing a single crystal thin film, is used for manufacturing semiconductor crystals, magnetic garnet crystals, etc., and FIG. 1 is a cross-sectional view of a single crystal thin film grown in a liquid phase epitaxial growth furnace. Is. As shown in FIG. 1, a lithium niobate crystal substrate 2 is immersed in a melt 7 of lithium oxide and niobium pentoxide held in a platinum crucible 1 to grow a thin film of lithium niobate single crystal having a desired composition.
【０００９】図１に示すように、白金るつぼ１、ニオブ
酸リチウム単結晶基板２、結晶ホルダー３、結晶ホルダ
ー支持棒４、抵抗加熱装置５、結晶回転機構６からなる
単結晶育成炉において、白金るつぼ１に炭酸リチウムお
よび五酸化ニオブをそれぞれｘモル、対（１−ｘ）モル
の比で装入する。これを抵抗加熱装置５で１０５０℃以
上に保持し、炭酸リチウム中の炭酸ガスを分離して酸化
リチウムとする。その後、所定温度の酸化リチウムと五
酸化ニオブとの融液７に結晶基板２を毎分１０回転させ
ながら６０分間浸漬して、厚さ約４００μｍのニオブ酸
リチウム単結晶の薄膜を結晶基板２のｃ面上に育成し
た。一方、モル比はｘ＝０．４７，０．４８６，０．５
０，０．５８，０．６１の４つの場合で行ったが、育成
温度（℃）、単結晶膜のｃ軸格子定数（ ）およびＬｉ
2 Ｏ組成（％）の関係を表１に示す。As shown in FIG. 1, in a single crystal growth furnace comprising a platinum crucible 1, a lithium niobate single crystal substrate 2, a crystal holder 3, a crystal holder support rod 4, a resistance heating device 5 and a crystal rotation mechanism 6, platinum is used. Crucible 1 is charged with lithium carbonate and niobium pentoxide at a ratio of x moles to (1-x) moles, respectively. This is held at 1050 ° C. or higher by the resistance heating device 5 to separate carbon dioxide gas in lithium carbonate to form lithium oxide. Then, the crystal substrate 2 is immersed in a melt 7 of lithium oxide and niobium pentoxide at a predetermined temperature for 60 minutes while rotating at 10 revolutions per minute to form a thin film of a lithium niobate single crystal having a thickness of about 400 μm on the crystal substrate 2. Raised on the c-plane. On the other hand, the molar ratio is x = 0.47, 0.486, 0.5
The growth temperature (° C.), the c-axis lattice constant () of the single crystal film, and Li were measured in four cases of 0, 0.58, and 0.61.
Table 1 shows the relationship of the 2 O composition (%).
【００１０】[0010]
【表１】 [Table 1]
【００１１】本発明は、モル比が４つの場合を示した本
実施例のみならず、液相エピタキシャル法を用いてニオ
ブ酸リチウム単結晶の薄膜の育成の際に、Ｌｉ2 Ｏ：Ｎ
ｂ2 Ｏ5 ＝ｘ：（１−ｘ），０．４７≦ｘ≦０．６１な
る組成を有する融液を用いて行えば良く、これにより結
晶組成の制御を行うことを特徴とするニオブ酸リチウム
単結晶の薄膜の製造方法全般に適用されるものであるこ
とはいうまでもない。The present invention is not limited to this embodiment showing the case where the molar ratio is four, but also when growing a thin film of a lithium niobate single crystal using a liquid phase epitaxial method, Li 2 O: N is used.
b 2 O 5 = x: (1-x), 0.47 ≦ x ≦ 0.61 may be used for the melt, and the crystal composition is controlled by this. It goes without saying that the present invention is applied to all methods of manufacturing a thin film of a lithium single crystal.
【００１２】[0012]
【発明の効果】以上説明した如く、本発明を用いること
により液相エピタキシャル法で所望の組成を有するニオ
ブ酸リチウム単結晶の薄膜の育成を行う際の結晶組成制
御が容易となるため、工業的利用価値は大である。As described above, the use of the present invention makes it easy to control the crystal composition when growing a thin film of a lithium niobate single crystal having a desired composition by the liquid phase epitaxial method. The utility value is great.
【図１】本発明の一実施例によるニオブ酸リチウム単結
晶の薄膜の育成の方法を示す図で、育成炉内に白金るつ
ぼに保持された融液及び基板結晶を挿入した断面図であ
る。FIG. 1 is a diagram showing a method for growing a thin film of a lithium niobate single crystal according to an embodiment of the present invention, and is a cross-sectional view in which a melt held in a platinum crucible and a substrate crystal are inserted into a growth furnace.
１ 白金るつぼ ２ 結晶基板 ３ 結晶ホルダー ４ 結晶ホルダー支持棒 ５ 抵抗加熱装置 ６ 結晶回転機構 ７ 結晶原料 1 Platinum crucible 2 Crystal substrate 3 Crystal holder 4 Crystal holder support rod 5 Resistance heating device 6 Crystal rotation mechanism 7 Crystal raw material
Claims (2)
チウム単結晶の薄膜の育成方法であって、融液の組成が
Ｌｉ2 Ｏ：Ｎｂ2 Ｏ5＝ｘ：（１−ｘ），０．４７≦ｘ
≦０．６１とすることを特徴とするニオブ酸リチウム単
結晶の薄膜の育成方法。1. A method for growing a thin film of a lithium niobate single crystal by a liquid phase epitaxial method, wherein the composition of the melt is Li 2 O: Nb 2 O 5 = x: (1-x), 0.47 ≦ x
A method of growing a thin film of a lithium niobate single crystal, wherein ≦ 0.61.
晶の薄膜の育成方法によって得られ、組成がＬｉ／Ｎｂ
＝１である薄膜を有することを特徴とするニオブ酸リチ
ウム単結晶。2. A method of growing a thin film of a lithium niobate single crystal according to claim 1, wherein the composition is Li / Nb.
Lithium niobate single crystal having a thin film of = 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28456391A JPH05117096A (en) | 1991-10-30 | 1991-10-30 | Method for growing thin film of lithium niobate single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28456391A JPH05117096A (en) | 1991-10-30 | 1991-10-30 | Method for growing thin film of lithium niobate single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05117096A true JPH05117096A (en) | 1993-05-14 |
Family
ID=17680083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28456391A Pending JPH05117096A (en) | 1991-10-30 | 1991-10-30 | Method for growing thin film of lithium niobate single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05117096A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0676491A1 (en) * | 1994-03-25 | 1995-10-11 | Ngk Insulators, Ltd. | A process for producing optoelectronic articles |
| EP0676490A1 (en) * | 1994-03-25 | 1995-10-11 | Ngk Insulators, Ltd. | Optoelectric articles and a process for producing the same |
| US5603762A (en) * | 1994-05-31 | 1997-02-18 | Ngk Insulators, Ltd. | Process and apparatus for the production of films of oxide type single crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6278197A (en) * | 1985-09-27 | 1987-04-10 | アメリカン テレフォン アンド テレグラフ カムパニー | Manufacture of homogeneous lithium niobate |
| JPH01320294A (en) * | 1988-06-22 | 1989-12-26 | Natl Inst For Res In Inorg Mater | Production of lithium niobate single crystal |
-
1991
- 1991-10-30 JP JP28456391A patent/JPH05117096A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6278197A (en) * | 1985-09-27 | 1987-04-10 | アメリカン テレフォン アンド テレグラフ カムパニー | Manufacture of homogeneous lithium niobate |
| JPH01320294A (en) * | 1988-06-22 | 1989-12-26 | Natl Inst For Res In Inorg Mater | Production of lithium niobate single crystal |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0676491A1 (en) * | 1994-03-25 | 1995-10-11 | Ngk Insulators, Ltd. | A process for producing optoelectronic articles |
| EP0676490A1 (en) * | 1994-03-25 | 1995-10-11 | Ngk Insulators, Ltd. | Optoelectric articles and a process for producing the same |
| US5643688A (en) * | 1994-03-25 | 1997-07-01 | Ngk Insulators, Ltd. | Optoelectric articles and a process for producing the same |
| US5985022A (en) * | 1994-03-25 | 1999-11-16 | Ngk Insulators, Ltd. | Optoelectric articles and a process for producing the same |
| US5603762A (en) * | 1994-05-31 | 1997-02-18 | Ngk Insulators, Ltd. | Process and apparatus for the production of films of oxide type single crystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Furukawa et al. | The correlation of MgO-doped near-stoichiometric LiNbO3 composition to the defect structure | |
| Lukasiewicz et al. | Strontium–barium niobate single crystals, growth and ferroelectric properties | |
| Hofmeister et al. | Growth and characterization of the perovskite K1-yLiyTa1-xNbxO3: Cu | |
| WO1992009917A1 (en) | Thin film of lithium niobate single crystal | |
| US3446603A (en) | Growth of lithium niobate crystals | |
| JPH05117096A (en) | Method for growing thin film of lithium niobate single crystal | |
| Fujino et al. | Electrooptic and ferroelectric properties of lithium tantalate single crystals as a function of melt composition | |
| JP2001287999A (en) | Lithium tantalate single crystal, optical element thereof and method for producing the same | |
| JP2915787B2 (en) | Method and apparatus for producing oxide single crystal film | |
| JP3013206B2 (en) | Method for producing lithium niobate single crystal | |
| JP2507910B2 (en) | Method for producing oxide single crystal | |
| JPH07267792A (en) | Production of electro-optical product | |
| Zydzik | The growth of LiNbO3 crystals using an automated puller | |
| JPS63195198A (en) | Production of lithium niobate single crystal thin film | |
| JP2636481B2 (en) | Growing nonlinear optical materials | |
| CA1302848C (en) | Process for making homogeneous lithium niobate | |
| JPH07311370A (en) | Electro-optical part and its production | |
| JPH05270992A (en) | Lithium niobate single crystal free from optical damage | |
| CN114645315B (en) | KTP crystal for quasi-phase matching device PPKTP and preparation method thereof | |
| JP3289904B2 (en) | Method for producing single crystal of MTiOAsO4, composition comprising single-domain crystal of MTIOAsO4 and crystalline MTiOAsO4 | |
| CN1048569A (en) | Monocrystal lithium uniformly doped with magnesium niobic acid and preparation method thereof | |
| JPH05310499A (en) | Lithium niobate single crystal, its production and optics | |
| JP2881737B2 (en) | Manufacturing method of optical single crystal | |
| JPH0793212B2 (en) | Oxide garnet single crystal | |
| KR950007601B1 (en) | Method for preparing crystallized linbo3 powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 19951212 |