JPH0442856A - Preparation of lead titanate thin film - Google Patents
Preparation of lead titanate thin filmInfo
- Publication number
- JPH0442856A JPH0442856A JP2147249A JP14724990A JPH0442856A JP H0442856 A JPH0442856 A JP H0442856A JP 2147249 A JP2147249 A JP 2147249A JP 14724990 A JP14724990 A JP 14724990A JP H0442856 A JPH0442856 A JP H0442856A
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- lead titanate
- lead
- alkoxide
- titanate thin
- 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.)
- Granted
Links
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- Photometry And Measurement Of Optical Pulse Characteristics (AREA)
- Radiation Pyrometers (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、赤外線検出材料であるチタン酸鉛薄膜の製造
方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for manufacturing a lead titanate thin film, which is an infrared detection material.
（従来の技術）
一般に赤外線検出材料として代表的なものにはＣｄＨｇ
Ｔｅ、 ＩｎＳｂ及びＳｉ等の半導体とチタン酸鉛、ゲ
ルマン酸鉛、Ｔ（：Ｓ、 ＰＶＦ、等の焦電体とがある
。前者は液体窒素で冷却して用いる必要があり、後者は
冷却する必要がない、従って、焦電体を用いた非冷却型
の赤外線検出器は冷却型に比べて性能面ではやや劣るも
のの、低価格、小型軽量及び扱い易い等の特徴があるた
め、人体検知器や火災幹知器等に利用されており、今後
ますます利用範囲が広がる傾向にある。チタン酸鉛は、
数多くある焦電材料のなかで、薄膜化が容易であり、感
度の良い赤外線検出材料として有望なものである。(Prior art) In general, CdHg is a typical infrared detection material.
There are semiconductors such as Te, InSb, and Si, and pyroelectric materials such as lead titanate, lead germanate, T(:S, PVF, etc.).The former must be cooled with liquid nitrogen, and the latter must be cooled. Therefore, although uncooled infrared detectors using pyroelectric materials are slightly inferior in performance to cooled infrared detectors, they are low cost, small and lightweight, and easy to handle, so they are suitable for human body detectors. Lead titanate is used in fire alarms, fire alarms, etc., and its range of use is likely to expand in the future.Lead titanate is
Among the many pyroelectric materials, it is easy to make into thin films and is promising as a highly sensitive infrared detection material.
従来、チタン酸鉛薄膜はチタン及び鉛の各酸化物を混合
・焼結し、得られた素材を研磨することにより作られて
きた。しかし、一般にセラミックスはもろく、この方法
ではほぼ３０μ−程度が厚さの限界であると共に加工工
程でのひび割れも多く、大きな面積の薄膜を得るのが困
難である。また、チタン酸鉛薄膜を得る他の方法として
、スパッタ法が用いられている。この方法は良質の薄膜
を作る技術として多くの電子材料に応用されているが、
焦電体薄膜の形成では成膜速度が１０〜２０人／ｗｉｎ
と非常に遅く、所定の厚さの膜を得るのに長時間を要す
る。さらに、チタン酸鉛の薄膜を得る他の方法として化
学気相成長（ＣＶＤ）法が近年用いられてきたが、この
方法は成膜速度がスパッタ法に比べて１０〜２０倍と比
較的速く、かつ膜組成の制御も容易であるが、スパッタ
法同様、大掛かりな装置を必要とする点が問題である。Conventionally, lead titanate thin films have been made by mixing and sintering titanium and lead oxides, and polishing the resulting material. However, ceramics are generally brittle, and this method has a thickness limit of approximately 30 μm, and there are many cracks during the processing process, making it difficult to obtain a thin film with a large area. Additionally, sputtering is used as another method for obtaining a lead titanate thin film. This method is applied to many electronic materials as a technology for creating high-quality thin films, but
In the formation of pyroelectric thin films, the deposition rate is 10 to 20 people/win.
It is very slow and takes a long time to obtain a film of a given thickness. Furthermore, chemical vapor deposition (CVD) has recently been used as another method for producing thin films of lead titanate; Although it is easy to control the film composition, the problem is that, like the sputtering method, it requires large-scale equipment.
（発明が解決しようとする課題）
従来のチタン酸鉛薄膜の製造方法は、スパッタ装置又は
ＣＶＤ装置など大掛かりな装置を必要とするうえ、成膜
に膨大な時間を要する等の欠点があった。(Problems to be Solved by the Invention) Conventional methods for producing lead titanate thin films have drawbacks such as requiring large-scale equipment such as sputtering equipment or CVD equipment, and requiring a huge amount of time for film formation.
本発明は、上記のような問題点を解消するためになされ
たもので、簡単な装置を用い、短時間で、チタン酸鉛の
薄膜を得ることが可能なチタン酸鉛薄膜の製造方法を提
供することを目的とする。The present invention has been made in order to solve the above-mentioned problems, and provides a method for producing a lead titanate thin film that can obtain a lead titanate thin film in a short time using a simple device. The purpose is to
（課題を解決するための手段）
本発明では、原料に鉛のアルコキシドとチタンのアルコ
キシドとを用い、スプレーパイロリシス法によりチタン
酸鉛薄膜を製造する。(Means for Solving the Problems) In the present invention, a lead titanate thin film is manufactured by a spray pyrolysis method using lead alkoxide and titanium alkoxide as raw materials.
本発明におけるスプレーパイロリシス法によるチタン酸
鉛薄膜の製造手順は次のようになる。まず、出発原料と
して鉛のアルコキシド及びチタンのアルコキシドを用い
、各成分の金属アルコキシドを所定の成分比に混合する
９次に、混合した原料溶液を加熱した基板上に吹き付は
非晶質焦電体薄膜を形成する。その後、電気炉等を用い
て熱処理を加えて焦電体薄膜を得る。The procedure for producing a lead titanate thin film by the spray pyrolysis method in the present invention is as follows. First, lead alkoxide and titanium alkoxide are used as starting materials, and the metal alkoxides of each component are mixed to a predetermined component ratio.Next, the mixed raw material solution is sprayed onto a heated substrate to form an amorphous pyroelectric Forms a thin body membrane. Thereafter, heat treatment is applied using an electric furnace or the like to obtain a pyroelectric thin film.
（作用）
上述のように、本発明では、原料として溶液を使用する
なめ、（１）各成分が原子レベルで混合し均一な膜が得
られる。（２）膜組成が仕込みの成分比を調整するだけ
で簡単に制御できる。（３）平板状の基板のみならず、
多様な形状の基板を用いることにより、自由なパターン
形成が可能である。(Function) As described above, in the present invention, since a solution is used as a raw material, (1) each component is mixed at the atomic level and a uniform film can be obtained. (2) The film composition can be easily controlled by simply adjusting the ingredient ratio of the ingredients. (3) Not only flat substrates, but also
Free pattern formation is possible by using substrates of various shapes.
（４）膜厚は吹き付けの回数と原料溶液の濃度を調整す
ることによって任意に設定することができる等の利点が
ある。(4) There is an advantage that the film thickness can be arbitrarily set by adjusting the number of times of spraying and the concentration of the raw material solution.
また、工業的には吹き付は装置と電気炉などの簡単な装
置により短時間の焼成で焦電特性をもつチタン酸鉛薄膜
の成膜が可能となり、極めて経済性の高い薄膜作成技術
である。In addition, from an industrial perspective, spraying is an extremely economical thin film production technology that allows the formation of lead titanate thin films with pyroelectric properties in a short firing time using simple equipment such as equipment and electric furnaces. .
さらに、スプレーパイロリシス法における出発原料とし
ては無機酸、有機酸、無機金属塩及び有機金属塩などが
あるが、これらの中で有機金属塩に含まれる金属アルコ
キシドは、高純度のものが得やすく、原子レベルで混合
できるので低温での成膜が可能であるなど他の金属塩に
比べて優れた点が多い。Furthermore, the starting materials for the spray pyrolysis method include inorganic acids, organic acids, inorganic metal salts, and organic metal salts, but among these, the metal alkoxides contained in the organic metal salts are easily obtainable with high purity. It has many advantages over other metal salts, such as being able to be mixed at the atomic level and forming films at low temperatures.
（発明の実施例）
第１図に本発明の実施例におけるチタン酸鉛薄膜の製造
工程のフローチャートを示す、以下順を追って本発明の
詳細な説明する。(Embodiments of the Invention) FIG. 1 shows a flowchart of the manufacturing process of a lead titanate thin film in an embodiment of the present invention, and the present invention will be described in detail below in order.
まず、混合工程１において各成分の金属アルコキシドを
所定の成分比に混合する。具体的には、金属アルコキシ
ドとして、ジ−イソ−プロポキシ船（Ｐｂ（０−ｉ−Ｃ
Ｊ、）ｚ）とテトラ−イソ−プロポキシチタン（Ｔｉ（
０−ｉ−ＣＪ−）４）を用いる。なお、ジ−イソ−プロ
ポキシ船は室温では固体のため、エタノールを溶媒とし
たジ−イソ−プロポキシ鉛のエタノール溶液を用いる。First, in a mixing step 1, the metal alkoxides of each component are mixed at a predetermined component ratio. Specifically, as the metal alkoxide, di-iso-propoxy carrier (Pb(0-i-C
J,)z) and tetra-iso-propoxytitanium (Ti(
0-i-CJ-)4) is used. Note that since the di-iso-propoxy ship is solid at room temperature, an ethanol solution of di-iso-propoxy lead using ethanol as a solvent is used.
これらの溶液をｐｂとＴｉのモル比が１＝１の化学量論
的組成比になるように秤量し混合する。These solutions are weighed and mixed so that the molar ratio of pb and Ti becomes a stoichiometric composition ratio of 1=1.
次に、スプレー工程２において混合溶液を基板に吹き付
は塗布する。吹き付けにはハンドスプレーを用い、５０
℃に加熱したアルミナ基板上に大気中で１回当たり０．
５μ−程度堆積させ、乾燥工程３にて乾燥させる。これ
らの工程２．３は所定の膜厚になるまで繰り返す６次に
、焼成工程４において、この塗布した基板を電気炉を用
いて大気中で約６００〜１２００℃の範囲内の特定温度
で１０分間若しくはそれ以上加熱・焼成する。この結果
、結晶のＣ軸（基板面に垂直）に強く配向した焦電特性
をもつペロブスカイト構造のチタン酸鉛薄膜を得ること
ができる。Next, in a spraying step 2, the mixed solution is sprayed onto the substrate. Use a hand sprayer for spraying, 50
0.0°C per time in air on an alumina substrate heated to .
It is deposited on the order of 5 μm and dried in the drying step 3. These steps 2.3 are repeated until a predetermined film thickness is achieved.6 Next, in the baking step 4, the coated substrate is heated in the air at a specific temperature within the range of about 600 to 1200°C for 10 minutes using an electric furnace. Heat and bake for a minute or more. As a result, a lead titanate thin film having a perovskite structure having pyroelectric properties strongly oriented along the C axis of the crystal (perpendicular to the substrate surface) can be obtained.
なお、焼成温度が約６００℃よりも低い場合には基板上
に堆積した非晶質薄膜を充分結晶化させることができず
、また約１２００℃より高いとチタン酸鉛が溶融状態と
なってしまうので好ましくない。Note that if the firing temperature is lower than about 600°C, the amorphous thin film deposited on the substrate cannot be sufficiently crystallized, and if it is higher than about 1200°C, the lead titanate becomes molten. So I don't like it.
また、基板はアルミナ以外の耐熱材を採用することもで
きる。Furthermore, the substrate can also be made of a heat-resistant material other than alumina.
（発明の効果）
以上のように、本発明のチタン酸鉛薄膜の製造方法によ
れば、出発材料に各成分の金属アルコキシトを用い、か
つスプレーパイロリシス法を採用したので、製造装置が
簡単であり、かつ短時間でチタン酸鉛薄膜が得られる効
果がある。(Effects of the Invention) As described above, according to the method for producing a lead titanate thin film of the present invention, metal alkoxides of each component are used as starting materials and the spray pyrolysis method is adopted, so the production equipment is simple. This method has the effect that a lead titanate thin film can be obtained in a short time.
第１図は本発明の一実施例に係るチタン酸鉛薄膜の作製
フローチャートである。
１・・・混合工程、２・・・スプレー工程、３・・・乾
燥工程、４・・・焼成工程。FIG. 1 is a flowchart for producing a lead titanate thin film according to an embodiment of the present invention. 1... Mixing process, 2... Spraying process, 3... Drying process, 4... Baking process.
Claims (1)
シドとを用い、スプレーパイロリシス法によりチタン酸
鉛薄膜を作成することを特徴とするチタン酸鉛薄膜の製
造方法。(1) A method for producing a lead titanate thin film, which comprises creating a lead titanate thin film by a spray pyrolysis method using lead alkoxide and titanium alkoxide as raw materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2147249A JPH0637329B2 (en) | 1990-06-07 | 1990-06-07 | Method for producing lead titanate thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2147249A JPH0637329B2 (en) | 1990-06-07 | 1990-06-07 | Method for producing lead titanate thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0442856A true JPH0442856A (en) | 1992-02-13 |
| JPH0637329B2 JPH0637329B2 (en) | 1994-05-18 |
Family
ID=15425961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2147249A Expired - Lifetime JPH0637329B2 (en) | 1990-06-07 | 1990-06-07 | Method for producing lead titanate thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0637329B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019225696A1 (en) * | 2018-05-25 | 2019-11-28 | コニカミノルタ株式会社 | Molecular transformation member, layered body, and method for modifying substrate |
-
1990
- 1990-06-07 JP JP2147249A patent/JPH0637329B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019225696A1 (en) * | 2018-05-25 | 2019-11-28 | コニカミノルタ株式会社 | Molecular transformation member, layered body, and method for modifying substrate |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0637329B2 (en) | 1994-05-18 |
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