JPH0578200A - Synthesis of piezoelectric thin film - Google Patents

Synthesis of piezoelectric thin film

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Publication number
JPH0578200A
JPH0578200A JP3243209A JP24320991A JPH0578200A JP H0578200 A JPH0578200 A JP H0578200A JP 3243209 A JP3243209 A JP 3243209A JP 24320991 A JP24320991 A JP 24320991A JP H0578200 A JPH0578200 A JP H0578200A
Authority
JP
Japan
Prior art keywords
film
thin film
target
substrate
synthesis
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.)
Withdrawn
Application number
JP3243209A
Other languages
Japanese (ja)
Inventor
Yoshihiko Shibata
佳彦 柴田
Tatsuyoshi Kaya
樹佳 嘉屋
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.)
Asahi Chemical Industry Co Ltd
Original Assignee
Asahi Chemical Industry 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 Asahi Chemical Industry Co Ltd filed Critical Asahi Chemical Industry Co Ltd
Priority to JP3243209A priority Critical patent/JPH0578200A/en
Publication of JPH0578200A publication Critical patent/JPH0578200A/en
Withdrawn legal-status Critical Current

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  • Physical Or Chemical Processes And Apparatus (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)

Abstract

PURPOSE:To obtain a film composed of Li(NbxTa1-x)O3 single phase and capable of providing a material for SAW devices and optics by the laser ablation method. CONSTITUTION:Laser ablation synthesis of a piezoelectric thin film, characterized by the ratio between target-constituting elements adjusted to 1.5<=Li/(NbxTa1-x)<=3.5 when synthesizing an Li(NbxTa1-x)O3 thin film (0<=x<=1).

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は光関連デバイス及び弾性
表面波(SurfaceAcousticWave、以
下SAWと呼ぶ)デバイスとして好適なLi(Nbx
1-x )O 3 薄膜の製造方法に関するものである。
FIELD OF THE INVENTION The present invention relates to an optical device and elasticity.
Surface wave (Surface Acoustic Wave,
Li (Nb) suitable as a lower SAW devicexT
a1-x) O 3The present invention relates to a method for manufacturing a thin film.

【0002】[0002]

【従来の技術】LiNbO3 単結晶あるいはLiTaO
3 単結晶は高いキューリー温度を有する強誘電体であ
り、その大きな電気機械結合定数、電気光学効果、非線
形光学効果などにおいて非常に優れた性質を有してお
り、SAWデバイス用材料として実用化される一方、光
学素子として有望視されている材料である。
2. Description of the Related Art LiNbO 3 single crystal or LiTaO
3 Single crystal is a ferroelectric substance with a high Curie temperature, and has extremely excellent properties in terms of its large electromechanical coupling constant, electro-optical effect, nonlinear optical effect, etc., and is put to practical use as a material for SAW devices. On the other hand, it is a promising material for optical elements.

【0003】近年の半導体技術の進歩による電子部品の
集積化及び小型化に伴い、強誘電体素子、圧電体素子も
小型化、薄膜化が進みつつあり、LiNbO3 単結晶あ
るいはLiTaO3 単結晶に関しても薄膜化に対する需
要は強く数多くの研究がなされてきている。従来、Li
NbO3 薄膜あるいはLiTaO3 薄膜の製造方法とし
ては液相エピタキシャル法、CVD法、真空蒸着法、ゾ
ルゲル法、スパッタリング法等が報告されているが、レ
ーザーアブレーション法による報告はほとんど無い。
With the recent progress in semiconductor technology and the increasing integration and miniaturization of electronic components, ferroelectric elements and piezoelectric elements are also becoming smaller and thinner, and LiNbO 3 single crystal or LiTaO 3 single crystal is being used. The demand for thin films is strong, and many studies have been conducted. Conventionally, Li
As a method for producing the NbO 3 thin film or the LiTaO 3 thin film, a liquid phase epitaxial method, a CVD method, a vacuum vapor deposition method, a sol-gel method, a sputtering method and the like have been reported, but there is almost no report by the laser ablation method.

【0004】レーザーアブレーション法は最近注目を浴
びている新たな成膜手段であり、スパッタリング法に比
べ、ターゲット組成と得られる膜の組成がほぼ等しい
事、不純物の混入が極めて少ない事、成膜速度を自由に
調節できる事などの有利な点を有していると一般に言わ
れている。レーザーアブレーション法によるLi(Nb
x Ta1-x )O3 薄膜(0≦x≦1)の合成において、
ターゲットの組成がLi/ (Nbx Ta1-x )=1では
いかなる基板温度、圧力でもLi(NbxTa1-x )O
3 単相から成る膜は得られないという問題があった。
The laser ablation method is a new film-forming means that has recently been receiving attention. Compared with the sputtering method, the target composition and the composition of the obtained film are almost the same, the mixing of impurities is extremely small, and the film-forming rate. It is generally said that it has the advantage that it can be adjusted freely. Li (Nb by laser ablation method
x Ta 1-x ) O 3 thin film (0 ≦ x ≦ 1)
When the composition of the target is Li / (Nb x Ta 1-x ) = 1, Li (Nb x Ta 1-x ) O is obtained at any substrate temperature and pressure.
There is a problem that a film consisting of three single phases cannot be obtained.

【0005】[0005]

【発明が解決しようとする課題】レーザーアブレーショ
ン法で、Li(Nbx Ta1-x )O3 薄膜を作るには、
先ず、Li(Nbx Ta1-x )O3 単相から成る膜が得
られる条件を見いだす必要がある。
In order to prepare a Li (Nb x Ta 1-x ) O 3 thin film by the laser ablation method,
First, it is necessary to find out the conditions under which a film composed of a Li (Nb x Ta 1-x ) O 3 single phase can be obtained.

【0006】[0006]

【課題を解決するための手段】本発明は、Li(Nbx
Ta1-x )O3 薄膜(0≦x≦1)を合成する際に、タ
ーゲットを構成する元素の比が1.5≦Li/(Nbx
Ta1-x )≦3.5であることを特徴とし、特に該薄膜
を合成する基板がサファイア基板である事を特徴とし、
特に該サファイア基板がサファイア基板C面である事を
特徴とするレーザーアブレーション法による圧電体薄膜
の合成方法に関する物である。
According to the present invention, Li (Nb x
When synthesizing a Ta 1-x ) O 3 thin film (0 ≦ x ≦ 1), the ratio of elements constituting the target is 1.5 ≦ Li / (Nb x
Ta 1-x ) ≦ 3.5, in particular, the substrate for synthesizing the thin film is a sapphire substrate,
In particular, the present invention relates to a method for synthesizing a piezoelectric thin film by a laser ablation method, wherein the sapphire substrate is the C surface of the sapphire substrate.

【0007】レーザーアブレーション法では、スパッタ
リング法に比べ、ターゲット組成と得られる膜の組成が
ほぼ等しいという特徴を持つためにターゲットのLi/
(Nbx Ta1-x )は1程度で十分と予測されていたが
1.5>Li/(Nbx Ta 1-x )ではいかなる基板温
度、圧力に依らずLi(Nbx Ta1-x)O3 単相膜は
得られなかった。
In the laser ablation method, spatter is used.
Compared to the ring method, the target composition and the composition of the obtained film are
The target Li /
(NbxTa1-x) Was predicted to be about 1, but
1.5> Li / (NbxTa 1-x) At any substrate temperature
Li (NbxTa1-x) O3Single-phase membrane
I couldn't get it.

【0008】発明者らが鋭意検討を進めた結果、予想外
にターゲット中のLiを大過剰にする事によって初めて
Li(Nbx Ta1-x )O3 単相膜が得られる事を発見
した。すなわち、ターゲット組成が1.5≦Li/(N
x Ta1-x )≦3.5でのみLi(Nbx Ta1-x
3単相から成る膜が得られる事がわかった。ターゲッ
ト組成は、1.5≦Li/(Nbx Ta1-x )≦3.5
である事が必要で、さらに好ましくは、1.75≦Li
/(Nbx Ta1-x )≦2.5である。1.5≦Li/
(Nbx Ta1-x )≦3.5以外の条件では、Li(N
x Ta1-x 3 8 やLi3 (Nbx Ta1-x )O4
と思われるものが共存した膜となった。
As a result of the inventors' earnest studies, it was unexpected.
First by making Li in the target too large
Li (NbxTa1-x) O3Discovered that a single phase film can be obtained
did. That is, the target composition is 1.5 ≦ Li / (N
bxTa1-x) ≦ 3.5 only for Li (NbxTa1-x)
O3It was found that a film composed of a single phase was obtained. Target
Composition is 1.5 ≦ Li / (NbxTa1-x) ≤ 3.5
And more preferably 1.75 ≦ Li
/ (NbxTa1-x) ≦ 2.5. 1.5 ≦ Li /
(NbxTa1-x) ≦ 3.5, Li (N
bxTa1-x) 3O8And Li3(NbxTa1-x) OFour
It became a film with what seemed to coexist.

【0009】ここで用いるレーザー装置は特に限定され
る物ではないが以下のような装置を用い、以下のような
条件で合成を行った。レーザーはエキシマレーザー(A
rF193nm)を用い、レーザー周波数は1から10
0Hz、レーザー出力は80から800mJとした。タ
ーゲットは合金製、セラミックス製どちらも用いること
が可能であるがLi2 CO3 及び、Nb2 5 、Ta2
5 を原料とする焼結体(サイズ15mmΦ×1〜5m
t )は製造しやすく本発明を実施する手段として好的
である。圧力は酸化性ガスで、0.0001〜0.05
torrの範囲であり、さらに好ましくは0.001〜
0.05torrの範囲が用いられる。圧力範囲0.0
001〜0.003torrにおいて雰囲気ガスが酸素
の場合には膜が着色する傾向を示すが、この圧力範囲に
おいてオゾンやN2 O、NO2 などのより強い酸化力を
持つ雰囲気ガスを用いれば無色の膜が得られる。これら
は本発明の実施にあたって好ましい態様である。基板温
度は500〜850℃の範囲であり10分から450分
間の範囲で成膜を行った。ただし、基板温度や反応時間
は本発明の実施にあたって制限を加えるものでは無い。
反応中のターゲットと基板間距離は1〜5cmの範囲が
好ましいが、特に制限されるものでは無い。基板として
は、特に限定はされないが単結晶基板(サファイア、S
iなど)及び非晶質基板(石英など)などが用いられ
る。いずれの基板を用いる場合にも成膜に供する基板表
面は鏡面研磨されていることが好ましい。
The laser apparatus used here is not particularly limited, but the following apparatus was used to synthesize under the following conditions. The laser is an excimer laser (A
rF193nm) and laser frequency is 1 to 10
The laser output was 0 Hz and the laser output was 80 to 800 mJ. Both targets made of alloy and ceramics can be used as the target, but Li 2 CO 3 , Nb 2 O 5 and Ta 2 are used.
Sintered body using O 5 as a raw material (size 15 mmΦ × 1-5 m
m t ) is easy to manufacture and is a preferred means of practicing the invention. Pressure is oxidizing gas, 0.0001-0.05
torr, more preferably 0.001 to
A range of 0.05 torr is used. Pressure range 0.0
When the atmosphere gas is oxygen at 001 to 0.003 torr, the film tends to be colored, but if an atmosphere gas having a stronger oxidizing power such as ozone, N 2 O, or NO 2 is used in this pressure range, a colorless film is obtained. A film is obtained. These are preferred embodiments for carrying out the present invention. The substrate temperature was in the range of 500 to 850 ° C., and the film formation was performed in the range of 10 minutes to 450 minutes. However, the substrate temperature and the reaction time do not limit the implementation of the present invention.
The distance between the target and the substrate during the reaction is preferably in the range of 1 to 5 cm, but is not particularly limited. The substrate is not particularly limited, but a single crystal substrate (sapphire, S
i) and an amorphous substrate (such as quartz). Whatever substrate is used, it is preferable that the substrate surface used for film formation is mirror-polished.

【0010】以下に例としてサファイア基板を用いた実
施例を示す。尚、この実施例は本発明を制限するもので
はない。
An example using a sapphire substrate will be shown below as an example. It should be noted that this embodiment does not limit the present invention.

【0011】[0011]

【実施例】図1にこの発明を実施するにあたって用いた
装置の概要を示す。焼結体ターゲットにレーザー光を照
射し酸化性ガス( 酸素及びオゾン)雰囲気で基板に成膜
させた。以下合成にあたって使用した条件を列記する。 合成条件 ターゲット Li、(Nbx Ta1-x )、Oから構 成される焼結体 単結晶基板 サファイアC面 基板温度(T) 500〜850℃ 導入ガス 酸素、オゾン 反応圧力(P) 0.0005〜0.05torr レーザー出力 150mJ レーザー周波数 15Hz 反応時間 50分 以上の条件を用い、Li(Nbx Ta1-x )O3 薄膜の
合成を行った。合成した膜の相は、X線回折法に依って
調べた。結果を表1に示す。図2にX線回折の1例を示
す。ターゲット組成1.5≦Li/(Nbx Ta1-x
≦3.5ではいずれにおいてもLi(Nbx Ta1-x
3 単相膜であった。
DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 shows an outline of an apparatus used for carrying out the present invention. The sintered target was irradiated with laser light to form a film on the substrate in an oxidizing gas (oxygen and ozone) atmosphere. The conditions used in the synthesis are listed below. Synthesis conditions Target Sintered body composed of Li, (Nb x Ta 1-x ), O Single crystal substrate Sapphire C surface Substrate temperature (T) 500 to 850 ° C Introduced gas Oxygen, ozone Reaction pressure (P) 0. A Li (Nb x Ta 1-x ) O 3 thin film was synthesized under the conditions of 0005 to 0.05 torr laser output 150 mJ laser frequency 15 Hz reaction time 50 minutes or more. The phase of the synthesized film was examined by X-ray diffractometry. The results are shown in Table 1. FIG. 2 shows an example of X-ray diffraction. Target composition 1.5 ≦ Li / (Nb x Ta 1-x )
Li (Nb x Ta 1-x ) in all cases where ≦ 3.5
It was an O 3 single-phase film.

【0012】[0012]

【比較例】比較例として、ターゲット組成Li/ (Nb
x Ta1-x )<1.5, Li/ (Nbx Ta1-x )>
3.5での合成実験を行った。合成した膜の相を表2に
示す。X線回折の例をそれぞれ図3、図4に示す。Li
/ (Nbx Ta1-x )<1.5ではLi(Nbx Ta
1-x 3 8 、Li/ (Nbx Ta1-x )>3.5 では
Li3 (Nbx Ta1-x )O4 の相が見られLi(Nb
x Ta1-x )O3 単相が得られない事がわかる。
Comparative Example As a comparative example, the target composition Li / (Nb
x Ta 1-x ) <1.5, Li / (Nb x Ta 1-x )>
A synthetic experiment at 3.5 was performed. The phases of the synthesized membrane are shown in Table 2. Examples of X-ray diffraction are shown in FIGS. 3 and 4, respectively. Li
/ (Nb x Ta 1-x ) <1.5, Li (Nb x Ta
1-x ) 3 O 8 and Li / (Nb x Ta 1-x )> 3.5, a phase of Li 3 (Nb x Ta 1-x ) O 4 was observed and Li (Nb
It can be seen that x Ta 1-x ) O 3 single phase cannot be obtained.

【0013】[0013]

【表1】 [Table 1]

【0014】[0014]

【表2】 [Table 2]

【0015】[0015]

【発明の効果】本発明に依れば、レーザーアブレーショ
ン法により、Li(Nbx Ta1-x )O3 単相から成る
膜が得られ、SAWデバイス用材料、光学素子用材料の
供給が可能となる。
According to the present invention, a film composed of a Li (Nb x Ta 1-x ) O 3 single phase can be obtained by the laser ablation method, and it is possible to supply materials for SAW devices and materials for optical elements. Becomes

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

【図1】本発明に用いる合成装置の概略図である。FIG. 1 is a schematic view of a synthesizer used in the present invention.

【図2】ターゲット組成Li/ Nb=2.0で合成した
膜のX線回折
FIG. 2 X-ray diffraction of a film synthesized with a target composition Li / Nb = 2.0

【図3】ターゲット組成Li/ Nb=1.4で合成した
膜のX線回折
FIG. 3 X-ray diffraction of a film synthesized with a target composition Li / Nb = 1.4

【図4 】ターゲット組成Li/ Nb=4.0で合成した
膜のX線回折
FIG. 4 X-ray diffraction of a film synthesized with a target composition Li / Nb = 4.0.

【符号の説明】[Explanation of symbols]

1 ArFエキシマレーザー 2 レンズ 3 ウインドウ 4 ターゲット 5 基板 6 膜厚測定装置 7 ガス導入口 1 ArF excimer laser 2 lens 3 window 4 target 5 substrate 6 film thickness measuring device 7 gas inlet

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 FI 技術表示箇所 H01L 41/18 ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Internal reference number FI Technical indication H01L 41/18

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 Li(Nbx Ta1-x )O3 薄膜(0≦
x≦1)を合成する際に、ターゲットを構成する元素の
比が1.5≦Li/(Nbx Ta1-x )≦3.5である
ことを特徴とするレーザーアブレーション法による圧電
体薄膜の合成方法。
1. A Li (Nb x Ta 1-x ) O 3 thin film (0 ≦
When synthesizing x ≦ 1), the ratio of the elements constituting the target is 1.5 ≦ Li / (Nb x Ta 1-x ) ≦ 3.5, and the piezoelectric thin film by the laser ablation method is characterized. Method of synthesis.
JP3243209A 1991-09-24 1991-09-24 Synthesis of piezoelectric thin film Withdrawn JPH0578200A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3243209A JPH0578200A (en) 1991-09-24 1991-09-24 Synthesis of piezoelectric thin film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3243209A JPH0578200A (en) 1991-09-24 1991-09-24 Synthesis of piezoelectric thin film

Publications (1)

Publication Number Publication Date
JPH0578200A true JPH0578200A (en) 1993-03-30

Family

ID=17100455

Family Applications (1)

Application Number Title Priority Date Filing Date
JP3243209A Withdrawn JPH0578200A (en) 1991-09-24 1991-09-24 Synthesis of piezoelectric thin film

Country Status (1)

Country Link
JP (1) JPH0578200A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002042527A1 (en) * 2000-11-22 2002-05-30 Sumitomo Electric Industries, Ltd. Diamond substrate having piezoelectric thin film, and method for manufacturing it

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002042527A1 (en) * 2000-11-22 2002-05-30 Sumitomo Electric Industries, Ltd. Diamond substrate having piezoelectric thin film, and method for manufacturing it
US6794683B2 (en) 2000-11-22 2004-09-21 Sumitomo Electric Industries, Ltd. Diamond substrate having piezoelectric thin film, and method for manufacturing it

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