JPH07113174A - Production of thin film - Google Patents
Production of thin filmInfo
- Publication number
- JPH07113174A JPH07113174A JP25538993A JP25538993A JPH07113174A JP H07113174 A JPH07113174 A JP H07113174A JP 25538993 A JP25538993 A JP 25538993A JP 25538993 A JP25538993 A JP 25538993A JP H07113174 A JPH07113174 A JP H07113174A
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- JP
- Japan
- Prior art keywords
- thin film
- substrate
- substance
- height
- ratio
- 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
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、薄膜の製造方法に関
し、さらに詳しくは、光，電子，磁気応用分野で使用さ
れる強誘電体，超伝導体，半導体，合金などの薄膜の製
造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a thin film, and more particularly to a method for producing a thin film such as a ferroelectric, a superconductor, a semiconductor or an alloy used in the fields of optical, electronic and magnetic applications. .
【０００２】[0002]
【従来の技術】従来、２種以上の物質の薄膜を基体上に
成膜し、熱処理して、薄膜を製造する方法が知られてい
る。この従来の薄膜の製造方法を、ＬｉＮｂＯ3 薄膜の
製造を例にとって説明する。まず、図５に示すように、
Ｌｉ3ＮｂＯ4（ニオブ酸リチウム）とＮｂ2Ｏ5（五酸化
ニオブ）のターゲットを用い、同時スパッタにより、常
温のＬｉＴａＯ3 基体１上に、薄膜５２’を成膜する。
このとき、Ｌｉ／Ｎｂ比が１．２になるように保つ。な
お、図５で、Ｌｉ／Ｎｂ比を、薄膜５２’中の横線の長
さにより表す。2. Description of the Related Art Conventionally, there is known a method of manufacturing a thin film by forming a thin film of two or more kinds of substances on a substrate and heat-treating it. This conventional method for producing a thin film will be described by taking the production of a LiNbO 3 thin film as an example. First, as shown in FIG.
Using a target of Li 3 NbO 4 (lithium niobate) and Nb 2 O 5 (niobium pentoxide), a thin film 52 ′ is formed on the LiTaO 3 substrate 1 at room temperature by co-sputtering.
At this time, the Li / Nb ratio is maintained at 1.2. In FIG. 5, the Li / Nb ratio is represented by the length of the horizontal line in the thin film 52 ′.
【０００３】次に、図６に示すように、１気圧の酸素気
流中で、６００℃，３時間の熱処理を施し、薄膜５２’
の結晶化を行い、ＬｉＮｂＯ3 薄膜５２を製造する。図
７に、製造されたＬｉＮｂＯ3 薄膜５２の深さ方向のＬ
ｉ／Ｎｂ比を、ＳＩＭＳ（２次イオン質量分析）で測定
した結果を示す。基体１からの高さが１．３μｍまで
は、Ｌｉ／Ｎｂ比が約１．０であり、ＬｉＮｂＯ3 薄膜
が得られていることが判る。Next, as shown in FIG. 6, a heat treatment is carried out at 600 ° C. for 3 hours in an oxygen stream of 1 atm to form a thin film 52 '.
Is crystallized to produce a LiNbO 3 thin film 52. FIG. 7 shows the L in the depth direction of the manufactured LiNbO 3 thin film 52.
The result of having measured i / Nb ratio by SIMS (secondary ion mass spectrometry) is shown. When the height from the substrate 1 is 1.3 μm, the Li / Nb ratio is about 1.0, and it can be seen that a LiNbO 3 thin film is obtained.
【０００４】[0004]
【発明が解決しようとする課題】図７を詳細に見ると、
薄膜５２の表面近く（基体１からの高さが１．３μｍ以
上）ではＬｉ／Ｎｂ比が急激に小さくなっており、Ｌｉ
が欠乏していることが判る。これは、熱処理温度６００
℃でのＬｉの蒸発圧がＮｂの蒸発圧に比べて著しく高い
ことから、熱処理時に、表面近くのＬｉがＮｂよりも多
量に蒸発してしまったためと考えられる。すなわち、従
来の薄膜の製造方法では、熱処理時に、表面近くの易蒸
発性の物質（例えば、Ｌｉ，Ａｓ，Ｎａ，Ｋなどの融点
の低い金属元素）が他の物質よりも多量に蒸発してしま
うため、表面近くでは、易蒸発性の物質と他の物質の濃
度比が所望の値にならない問題点がある。そこで、この
発明の目的は、易蒸発性の物質と他の物質の濃度比を薄
膜全体にわたり（すなわち、表面近くでも，内部でも）
所望の値にすることが出来る薄膜の製造方法を提供する
ことにある。DISCLOSURE OF THE INVENTION Looking at FIG. 7 in detail,
In the vicinity of the surface of the thin film 52 (the height from the substrate 1 is 1.3 μm or more), the Li / Nb ratio is rapidly reduced.
It turns out that is lacking. This is the heat treatment temperature 600
Since the vaporization pressure of Li at 0 ° C. is significantly higher than the vaporization pressure of Nb, it is considered that Li near the surface was vaporized in a larger amount than Nb during the heat treatment. That is, in the conventional method of manufacturing a thin film, a substance that is easily vaporized near the surface (for example, a metal element having a low melting point such as Li, As, Na, or K) evaporates in a larger amount than other substances during the heat treatment. Therefore, there is a problem that the concentration ratio between the easily evaporative substance and another substance does not reach a desired value near the surface. Therefore, an object of the present invention is to make the concentration ratio of the easily evaporative substance and the other substance throughout the thin film (that is, near the surface or inside).
It is an object of the present invention to provide a method for producing a thin film that can achieve a desired value.
【０００５】[0005]
【課題を解決するための手段】この発明の薄膜の製造方
法は、易蒸発性の物質を含む２種以上の物質の薄膜を基
体上に成膜し、熱処理して、薄膜を製造する薄膜の製造
方法において、熱処理による前記易蒸発性の物質の蒸発
により熱処理後に所望の濃度比となるように、基体から
の高さに応じて易蒸発性の物質と他の物質の濃度比を変
えて薄膜を成膜することを構成上の特徴とするものであ
る。なお、基体からの高さに応じて易蒸発性の物質と他
の物質の濃度比を階段状に変えてもよいし、連続的に変
えてもよい。また、成膜方法は、ＰＶＤ，ＣＶＤ，めっ
き，真空蒸着などのいずれの成膜方法でもよい。The method for producing a thin film according to the present invention is a thin film for producing a thin film by forming a thin film of two or more kinds of substances containing an easily evaporative substance on a substrate and heat-treating the thin film. In the manufacturing method, the concentration ratio of the easily-evaporable substance and the other substance is changed according to the height from the substrate so that the desired concentration ratio after the heat treatment is obtained by the evaporation of the easily-evaporable substance by the heat treatment. Is a structural feature. The concentration ratio of the easily evaporative substance and the other substance may be changed stepwise or continuously depending on the height from the substrate. Further, the film forming method may be any film forming method such as PVD, CVD, plating, or vacuum deposition.
【０００６】この発明の薄膜の製造方法により製造され
る薄膜としては、例えば、光磁気記録に用いられるＹＩ
Ｇ（Ｙ3Ｆｅ5Ｏ12）や，固体レーザ発振材料として用い
られるＹＡＧ（Ｙ3Ａｌ5Ｏ12）や，光導波路型の光学素
子に用いられる ＬｉＮｂＯ3や，高温超伝導体として用
いられるＹＢＣＯ系化合物などの金属元素複合酸化物の
薄膜が挙げられる。また、光学部品などに用いられるＧ
ａＡｓ，ＧａＡｌＡｓなどの化合物半導体の薄膜が挙げ
られる。さらに、磁性膜に用いられるＣｏ−Ｎｉ系，Ｃ
ｏ−Ｃｒ系などの合金の薄膜が挙げられる。The thin film manufactured by the thin film manufacturing method of the present invention is, for example, YI used for magneto-optical recording.
G (Y 3 Fe 5 O 12 ), YAG (Y 3 Al 5 O 12 ) used as a solid-state laser oscillation material, LiNbO 3 used for optical waveguide type optical elements, and YBCO used as a high temperature superconductor. Examples thereof include thin films of metal element composite oxides such as system compounds. G used for optical parts
Examples thereof include thin films of compound semiconductors such as aAs and GaAlAs. Further, Co-Ni system, C used for the magnetic film
A thin film of an alloy such as an o-Cr system may be used.
【０００７】[0007]
【作用】この発明の薄膜の製造方法では、熱処理による
易蒸発性の物質の蒸発により熱処理後に所望の濃度比と
なるように、基体からの高さに応じて易蒸発性の物質と
他の物質の濃度比を変えて薄膜を成膜する。具体的に
は、基体からの高さに応じて異なる易蒸発性の物質の蒸
発量を求め、その蒸発量の分だけ当該基体からの高さで
の所望の濃度比より易蒸発性の物質の割合が余分になる
ように濃度比を変えて薄膜を成膜する。熱処理により基
体からの高さに応じた前記蒸発量だけ易蒸発性の物質が
蒸発すると、余分に加えた易蒸発性の物質がなくなるた
め、易蒸発性の物質と他の物質の濃度比が所望の値にな
る。According to the method of manufacturing a thin film of the present invention, the easily evaporative substance and other substances are adjusted according to the height from the substrate so that the desired concentration ratio is obtained after the heat treatment by evaporating the easily evaporative substance by the heat treatment. A thin film is formed by changing the concentration ratio of. Specifically, the evaporation amount of an easily evaporative substance that differs depending on the height from the substrate is obtained, and the amount of the easily evaporative substance is higher than the desired concentration ratio at the height from the substrate by the amount of the evaporation amount. A thin film is formed by changing the concentration ratio so that the ratio becomes excessive. When the heat-evaporable substance evaporates by the heat treatment in an amount corresponding to the height from the substrate, the additional easily-evaporable substance disappears. Therefore, the concentration ratio of the easily-evaporable substance to another substance is desired. Becomes the value of.
【０００８】例えば、基体からの高さに応じた易蒸発性
の物質の蒸発量の分だけ一定の濃度比より易蒸発性の物
質の割合が余分になるように、基体からの高さに応じて
易蒸発性の物質と他の物質の濃度比を変えて成膜すれ
ば、易蒸発性の物質と他の物質の濃度比が基体からの高
さにかかわらず均一な薄膜を製造できる。For example, depending on the height from the substrate, the ratio of the easily-evaporable substance may become excessive by a certain concentration ratio by the amount of evaporation of the easily-evaporable substance depending on the height from the substrate. By forming the film by changing the concentration ratio of the easily-evaporable substance and the other substance, a thin film having a uniform concentration ratio of the easily-evaporable substance and the other substance regardless of the height from the substrate can be manufactured.
【０００９】[0009]
【実施例】以下、この発明の薄膜の製造方法の一実施例
であるＬｉＮｂＯ3 薄膜の製造方法を説明する。なお、
これによりこの発明が限定されるものではない。まず、
図１に示すように、Ｌｉ3ＮｂＯ4（ニオブ酸リチウム）
とＮｂ2Ｏ5（五酸化ニオブ）のターゲットを用い、同時
スパッタにより、常温のＬｉＴａＯ3 基体１上に、薄膜
２’を成膜する。このとき、基体１からの高さ１．０μ
ｍまではＬｉ／Ｎｂ比を１．０にし、基体１からの高さ
１．０μｍ〜１．３μｍの間はＬｉ／Ｎｂ比を１．２に
し、基体１からの高さ１．３μｍ〜１．５μｍ（薄膜表
面）まではＬｉ／Ｎｂ比を１．５にする。なお、図１
で、Ｌｉ／Ｎｂ比を、薄膜２’中の横線の長さにより表
す。EXAMPLES A method for producing a LiNbO 3 thin film, which is an example of the method for producing a thin film of the present invention, will be described below. In addition,
This does not limit the present invention. First,
As shown in FIG. 1, Li 3 NbO 4 (lithium niobate)
And a target of Nb 2 O 5 (niobium pentoxide) are used to form a thin film 2 ′ on the LiTaO 3 substrate 1 at room temperature by co-sputtering. At this time, the height from the base 1 is 1.0 μ
up to m, the Li / Nb ratio is 1.0, the height from the substrate 1 is 1.0 μm to 1.3 μm, the Li / Nb ratio is 1.2, and the height from the substrate 1 is 1.3 μm to 1. The Li / Nb ratio is set to 1.5 up to 0.5 μm (thin film surface). Note that FIG.
The Li / Nb ratio is represented by the length of the horizontal line in the thin film 2 ′.
【００１０】次に、図２に示すように、１気圧の酸素気
流中で、６００℃，３時間の熱処理を施し、薄膜２’の
結晶化を行い、ＬｉＮｂＯ3 薄膜２を製造する。図３
に、製造されたＬｉＮｂＯ3 薄膜２の深さ方向のＬｉ／
Ｎｂ比を、ＳＩＭＳ（２次イオン質量分析）で測定した
結果を示す。薄膜２の表面までＬｉ／Ｎｂ比が約１．０
であり、表面近くでもＬｉＮｂＯ3薄膜が得られている
ことが判る。Next, as shown in FIG. 2, heat treatment is performed at 600 ° C. for 3 hours in an oxygen stream of 1 atm to crystallize the thin film 2 ′ to produce a LiNbO 3 thin film 2. Figure 3
In the depth direction of the manufactured LiNbO 3 thin film 2,
The result of having measured Nb ratio by SIMS (secondary ion mass spectrometry) is shown. Li / Nb ratio up to the surface of thin film 2 is about 1.0
It can be seen that the LiNbO 3 thin film is obtained even near the surface.
【００１１】図４に、製造されたＬｉＮｂＯ3 薄膜２の
Ｘ線回折結果を示す。ＬｉＮｂＯ3 薄膜２の＜００６＞
面とＬｉＴａＯ3 基板１の＜００６＞面のピークのみが
現れており、ＬｉＮｂＯ3 薄膜２が単結晶膜であること
が判る。FIG. 4 shows the X-ray diffraction result of the manufactured LiNbO 3 thin film 2. <006> of LiNbO 3 thin film 2
Surface and the peak of the <006> plane of the LiTaO 3 substrate 1 appear, which shows that the LiNbO 3 thin film 2 is a single crystal film.
【００１２】[0012]
【発明の効果】この発明の薄膜の製造方法によれば、易
蒸発性の物質と他の物質の濃度比を薄膜全体にわたり所
望の値にすることが出来る。According to the method of manufacturing a thin film of the present invention, the concentration ratio of the easily evaporative substance to another substance can be set to a desired value over the entire thin film.
【図１】この発明の一実施例のＬｉＮｂＯ3 薄膜の製造
方法における成膜工程の説明図である。FIG. 1 is an explanatory diagram of a film forming step in a method for manufacturing a LiNbO 3 thin film according to an embodiment of the present invention.
【図２】この発明の一実施例のＬｉＮｂＯ3 薄膜の製造
方法により製造されたＬｉＮｂＯ3 薄膜の模式的断面図
である。FIG. 2 is a schematic cross-sectional view of a LiNbO 3 thin film manufactured by the method for manufacturing a LiNbO 3 thin film according to an embodiment of the present invention.
【図３】この発明の一実施例のＬｉＮｂＯ3 薄膜の製造
方法により製造されたＬｉＮｂＯ3 薄膜の深さ方向のＬ
ｉ／Ｎｂ比を２次イオン質量分析で測定した結果のグラ
フである。FIG. 3 is an L in the depth direction of a LiNbO 3 thin film manufactured by the method for manufacturing a LiNbO 3 thin film according to an embodiment of the present invention.
It is a graph of the result which measured the i / Nb ratio by the secondary ion mass spectrometry.
【図４】この発明の一実施例のＬｉＮｂＯ3 薄膜の製造
方法により製造されたＬｉＮｂＯ3 薄膜のＸ線回折結果
を示すグラフである。FIG. 4 is a graph showing an X-ray diffraction result of a LiNbO 3 thin film manufactured by the method for manufacturing a LiNbO 3 thin film according to an example of the present invention.
【図５】従来のＬｉＮｂＯ3 薄膜の製造方法における成
膜工程の説明図である。FIG. 5 is an explanatory diagram of a film forming step in a conventional method for manufacturing a LiNbO 3 thin film.
【図６】従来のＬｉＮｂＯ3 薄膜の製造方法により製造
されたＬｉＮｂＯ3 薄膜の模式的断面図である。6 is a schematic cross-sectional view of a LiNbO 3 thin film manufactured by the conventional method of manufacturing a LiNbO 3 thin film.
【図７】従来のＬｉＮｂＯ3 薄膜の製造方法により製造
されたＬｉＮｂＯ3 薄膜の深さ方向のＬｉ／Ｎｂ比を２
次イオン質量分析で測定した結果のグラフである。[7] the depth direction of the Li / Nb ratio of LiNbO 3 thin film manufactured by the conventional method of manufacturing a LiNbO 3 thin film 2
It is a graph of the result measured by secondary ion mass spectrometry.
１ ＬｉＴａＯ3 基体 ２ ＬｉＮｂＯ3 薄膜 ２’ 薄膜1 LiTaO 3 substrate 2 LiNbO 3 thin film 2'thin film
フロントページの続き (72)発明者 佐野 一也 千葉県四街道市鷹の台一丁目３番 株式会 社日本製鋼所内 (72)発明者 山口 毅 千葉県四街道市鷹の台一丁目３番 株式会 社日本製鋼所内Front Page Continuation (72) Inventor Kazuya Sano, 1-3 Takanodai, Yotsukaido, Chiba Prefecture, Japan Steel Works (72) Inventor, Takeshi Yamaguchi, 1-3, Takanodai, Yotsukaido, Chiba Prefecture, Japan Steel Works
Claims (2)
薄膜を基体上に成膜し、熱処理して、薄膜を製造する薄
膜の製造方法において、 熱処理による前記易蒸発性の物質の蒸発により熱処理後
に所望の濃度比となるように、基体からの高さに応じて
易蒸発性の物質と他の物質の濃度比を変えて薄膜を成膜
することを特徴とする薄膜の製造方法。1. A method for producing a thin film, comprising forming a thin film of two or more kinds of substances containing an easily evaporative substance on a substrate and heat-treating the thin film. A method for producing a thin film, characterized in that the concentration ratio of an easily-evaporable substance and another substance is changed according to the height from the substrate so that the desired concentration ratio is obtained after evaporation by heat treatment. .
て、基体からの高さに応じた易蒸発性の物質の蒸発量の
分だけ一定の濃度比より易蒸発性の物質の割合が余分に
なるように、基体からの高さに応じて易蒸発性の物質と
他の物質の濃度比を変えて薄膜を成膜することを特徴と
する薄膜の製造方法。2. The method for producing a thin film according to claim 1, wherein the ratio of the easily-evaporable substance exceeds a certain concentration ratio by the amount of evaporation of the easily-evaporable substance according to the height from the substrate. The method of manufacturing a thin film, wherein the thin film is formed by changing the concentration ratio of the easily-evaporable substance and the other substance according to the height from the substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25538993A JPH07113174A (en) | 1993-10-13 | 1993-10-13 | Production of thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25538993A JPH07113174A (en) | 1993-10-13 | 1993-10-13 | Production of thin film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH07113174A true JPH07113174A (en) | 1995-05-02 |
Family
ID=17278086
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25538993A Pending JPH07113174A (en) | 1993-10-13 | 1993-10-13 | Production of thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07113174A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8971410B2 (en) | 2010-06-18 | 2015-03-03 | Samsung Electronics Co., Ltd. | Method, apparatus and computer-readable medium processing frames obtained by multiple exposures |
-
1993
- 1993-10-13 JP JP25538993A patent/JPH07113174A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8971410B2 (en) | 2010-06-18 | 2015-03-03 | Samsung Electronics Co., Ltd. | Method, apparatus and computer-readable medium processing frames obtained by multiple exposures |
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