JPH05306460A - Method for producing insulating material coated with alumina film - Google Patents
Method for producing insulating material coated with alumina filmInfo
- Publication number
- JPH05306460A JPH05306460A JP13759792A JP13759792A JPH05306460A JP H05306460 A JPH05306460 A JP H05306460A JP 13759792 A JP13759792 A JP 13759792A JP 13759792 A JP13759792 A JP 13759792A JP H05306460 A JPH05306460 A JP H05306460A
- Authority
- JP
- Japan
- Prior art keywords
- film
- alumina film
- substrate
- insulating material
- material coated
- 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- Withdrawn
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- Physical Vapour Deposition (AREA)
Abstract
(57)【要約】
【目的】 本発明はステンレス鋼板を基板としてアルミ
ナ膜をコーティングした材料において、絶縁性を向上さ
せる方法を提供する。
【構成】 ステンレス基板上にスパッタリング等により
アルミナ膜をドライコーティングし、引き続いて酸化雰
囲気中で５００℃以上の温度で熱処理する。
(57) [Summary] [Object] The present invention provides a method for improving the insulating property in a material coated with an alumina film using a stainless steel plate as a substrate. [Structure] An alumina film is dry-coated on a stainless steel substrate by sputtering or the like, and subsequently heat-treated at a temperature of 500 ° C. or higher in an oxidizing atmosphere.
Description
【０００１】[0001]
【産業上の利用分野】本発明は金属基板上にドライコー
ティング法によりアルミナ膜を形成した電気絶縁材料の
製造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 producing an electrically insulating material in which an alumina film is formed on a metal substrate by a dry coating method.
【０００２】[0002]
【従来の技術】電気絶縁性板状材料は、ＩＣ基板、セン
サー基板、太陽電池基板、電極基板等に使用され電子・
電気産業に欠かせない材料になっている。2. Description of the Related Art Electrically insulating plate-shaped materials are used in electronic substrates such as IC substrates, sensor substrates, solar cell substrates, and electrode substrates.
It has become an indispensable material for the electric industry.
【０００３】この絶縁材料には、従来セラミックス材
料、ガラス材料、有機系材料等が用いられているが、セ
ラミックス・ガラス材料は強度および加工性が劣るとい
う欠点、有機系材料はガス放出性および耐熱性が劣ると
いう欠点を持っている。Ceramic materials, glass materials, organic materials, etc. have been conventionally used for this insulating material. However, ceramic / glass materials have the drawback of poor strength and workability, and organic materials have gas releasing and heat resistance properties. It has the drawback of being inferior in sex.
【０００４】絶縁材料としては、ドライコーティング法
を用いて金属基板上にセラミック薄膜をコーティングす
ることによって、電気絶縁性を付与した金属材料があ
る。As the insulating material, there is a metal material which is provided with an electric insulating property by coating a ceramic thin film on a metal substrate using a dry coating method.
【０００５】この金属基板としては、耐薬品性、強度等
の面からステンレス鋼板が用いられている。As the metal substrate, a stainless steel plate is used in terms of chemical resistance and strength.
【０００６】Ａｌ2Ｏ3の様な金属酸化物を基板上にドラ
イコーティングすると酸素が欠損して、化学量論組成か
らずれて、例えばＡｌ2Ｏ3の場合にはＡｌ2Ｏ3-xの組成
となることが知られている。[0006] The metal oxides such as Al 2 O 3 deficient oxygen when dry coating on a substrate, deviate from the stoichiometric composition, for example in the case of Al 2 O 3 is of Al 2 O 3-x It is known to have a composition.
【０００７】このため、酸素を放電ガスの中に適当な割
合で混合した雰囲気中でドライコーティングすることに
よって、欠損する酸素を補い、前記の化学量論組成から
のずれ（ｘの値）を小さくする方法がある。Therefore, dry coating is performed in an atmosphere in which oxygen is mixed in a discharge gas at an appropriate ratio to compensate for the deficient oxygen and reduce the deviation (value of x) from the stoichiometric composition. There is a way to do it.
【０００８】しかし、放電ガス中への過度の酸素の混合
は、絶縁膜にピンホール等の絶縁欠陥を生じ易く、かえ
って絶縁性を低下させたり、成膜速度が小さくなり生産
性を悪くする等の欠点を有している。However, excessive mixing of oxygen into the discharge gas is liable to cause insulation defects such as pinholes in the insulating film, rather lowering the insulating property or reducing the film forming rate to deteriorate productivity. Has the drawback of.
【０００９】尚、本発明におけるドライコーティング法
とは、プラズマを媒体として、真空中で薄膜を形成する
方法の総称であり、イオンプレーティング、スパッタリ
ング、プラズマ―ＣＶＤ等である。The dry coating method in the present invention is a general term for a method of forming a thin film in a vacuum using plasma as a medium, such as ion plating, sputtering and plasma-CVD.
【００１０】[0010]
【発明が解決しようとする課題】ドライコーティング中
のガス雰囲気の調整によって欠損する酸素を補うという
従来方法においては、絶縁膜にピンホール等の絶縁欠陥
を生じ易いため、良好な絶縁性を得ることは困難であっ
た。In the conventional method of compensating for deficient oxygen by adjusting the gas atmosphere during dry coating, it is easy to cause insulation defects such as pinholes in the insulation film, and therefore good insulation is obtained. Was difficult.
【００１１】すなわち、本発明はステンレス鋼板を基板
とするアルミナ膜をコーティングした材料の製造におい
て、皮膜組成をピンホール等の絶縁欠陥を生じることな
く化学量論組成からのずれを小さくすることによって、
絶縁欠陥の少ない絶縁膜を生成し、絶縁材料の絶縁性を
向上させることを目的とするものである。That is, according to the present invention, in the production of a material coated with an alumina film using a stainless steel plate as a substrate, the deviation of the film composition from the stoichiometric composition can be reduced without causing insulation defects such as pinholes.
The purpose of the present invention is to form an insulating film with few insulating defects and improve the insulating property of the insulating material.
【００１２】[0012]
【課題を解決するための手段】本発明の方法は、ステン
レス基板上にアルミナ膜をドライコーティングし、引き
続いて酸化雰囲気中で５００℃以上の温度で熱処理す
る。According to the method of the present invention, an alumina film is dry-coated on a stainless steel substrate and subsequently heat-treated at a temperature of 500 ° C. or higher in an oxidizing atmosphere.
【００１３】[0013]
【作用】本発明の基板はステンレス鋼を用いる。前記基
板の表面性状としては膜の絶縁性をより確実に確保する
ために、酸洗による粒界腐食や研削目などの凹凸の少な
い状態にしておくことが望ましい。The substrate of the present invention uses stainless steel. As for the surface properties of the substrate, in order to ensure the insulating property of the film more reliably, it is desirable that there be little unevenness such as intergranular corrosion due to pickling and grinding marks.
【００１４】該基板に、例えばＡｌ2Ｏ3をターゲットに
してＡｒでスパッタリングすることによって成膜処理す
ると、前述のように酸素が欠損したＡｌ2Ｏ3-xの組成の
コーティング膜が生成される。この組成の膜はＡｌ2Ｏ3
膜に比較して絶縁性が劣る。When a film is formed on the substrate by sputtering Al with a target of Al 2 O 3 , for example, a coating film of oxygen-deficient Al 2 O 3-x composition is formed as described above. .. The film of this composition is Al 2 O 3
Insulation is inferior to the film.
【００１５】本発明者等は絶縁性の向上対策について検
討した結果、酸素を含むガス雰囲気中で５００℃以上の
温度で熱処理することによって膜組成がＡｌ2Ｏ3に近く
なり絶縁性が向上することを見出した。The inventors of the present invention have examined measures for improving the insulating property, and as a result, heat treatment at a temperature of 500 ° C. or higher in a gas atmosphere containing oxygen makes the film composition close to that of Al 2 O 3 and improves the insulating property. I found that.
【００１６】適正熱処理条件を求めるために、以下の実
験を行った。The following experiments were carried out in order to determine the proper heat treatment conditions.
【００１７】基板としてＳＵＳ４３０ＢＡを用い、これ
にスパッタリングにより同一条件でアルミナ膜を形成し
た。膜厚は全て０．９μｍである。SUS430BA was used as a substrate, and an alumina film was formed on this by sputtering under the same conditions. All film thicknesses are 0.9 μm.
【００１８】アルミナ膜を観察して、ピンホール等の欠
陥があるもの〔Ａ〕と、ないもの〔Ｂ〕に層別した。こ
れらの絶縁材料を大気中で熱処理した。The alumina film was observed and layered into those having defects such as pinholes [A] and those having no defects [B]. These insulating materials were heat-treated in the atmosphere.
【００１９】絶縁材料の抵抗値は、表面にアルミ（１０
ｍｍ角×０．２μｍ）を電極として蒸着した後、電極上
にテスターの測定子を置き、１８ヵ所の電気抵抗値を測
定した。The resistance value of the insulating material is that aluminum (10
(mm square × 0.2 μm) was vapor-deposited as an electrode, and a probe of a tester was placed on the electrode to measure the electric resistance value at 18 places.
【００２０】測定した内で１ＭΩ以上の電気抵抗値を示
す割合を合格率（％）とした。熱処理条件と合格率の関
係を図１に示す。The rate of showing an electric resistance value of 1 MΩ or more in the measurement was defined as the pass rate (%). The relationship between the heat treatment conditions and the pass rate is shown in FIG.
【００２１】５００℃以上の熱処理で合格率が上昇し、
６００〜７００℃では８０％程度の合格率が得られた。
ピンホール等の欠陥があるもの〔Ａ〕は７５０℃以上の
熱処理温度で減少した。The heat treatment at 500 ° C. or higher increases the acceptance rate,
A pass rate of about 80% was obtained at 600 to 700 ° C.
Those having defects such as pinholes [A] decreased at the heat treatment temperature of 750 ° C. or higher.
【００２２】７５０℃以上の熱処理では、アルミナ膜の
ピンホール部の基板が酸化して、合格率が減少したもの
であり、ピンホールがない場合〔Ｂ〕は７５０℃以上で
も高い合格率を維持した。In the heat treatment at 750 ° C. or higher, the substrate in the pinhole portion of the alumina film was oxidized and the pass rate was reduced. In the case of no pinhole [B], the high pass rate was maintained even at 750 ° C. or higher. did.
【００２３】また、オージェ電子分光法によりＡｌ2Ｏ
3-x膜の組成分析をした。Ｏ／Ａｌ組成比を図２に示
す。Al 2 O by Auger electron spectroscopy
The composition of the 3-x film was analyzed. The O / Al composition ratio is shown in FIG.
【００２４】非熱処理材や４００℃以下の熱処理材は、
Ｏ／Ａｌの値が１．２〜１．３であるが、５００℃以上
からＯ／Ａｌの値は上昇し、６００℃×２４ｈｒ熱処理
した材料においては、表面近傍でのＯ／Ａｌの値が化学
量論組成（１．５）に近い１．４５まで上昇しており、
酸素の付加によって絶縁性が向上していることが分か
る。Non-heat-treated materials and heat-treated materials below 400 ° C.
The value of O / Al is 1.2 to 1.3, but the value of O / Al increases from 500 ° C. or higher, and in the material heat-treated at 600 ° C. for 24 hours, the value of O / Al near the surface is It has risen to 1.45, which is close to the stoichiometric composition (1.5),
It can be seen that the insulating property is improved by the addition of oxygen.
【００２５】以上の結果より、熱処理雰囲気は酸素を含
んでいれば良く、大気中でも良い。熱処理温度は５００
℃以上であれば良いが、アルミナ膜にピンホール等の欠
陥がある〔Ａ〕場合は７００℃以下が望ましい。ピンホ
ール等の欠陥がない〔Ｂ〕場合には７００℃以上でも良
い。From the above results, the heat treatment atmosphere should just contain oxygen, and may be in the air. Heat treatment temperature is 500
The temperature may be at least ℃, but if the alumina film has defects such as pinholes [A], it is preferably at 700 ℃ or less. If there are no defects such as pinholes [B], the temperature may be 700 ° C. or higher.
【００２６】[0026]
【実施例】基板とし、表面の平滑なＳＵＳ４３０ＢＡと
ＳＵＳ３０４ＢＡを用いた。[Example] As the substrate, SUS430BA and SUS304BA having smooth surfaces were used.
【００２７】これにＲＦマグネトロンスパッタリング装
置を用い、Ａｌ2Ｏ3をターゲットとして、同一条件でＡ
ｌ2Ｏ3-x絶縁膜を形成した。An RF magnetron sputtering apparatus was used for this, and Al 2 O 3 was used as a target under the same conditions.
An l 2 O 3 -x insulating film was formed.
【００２８】尚、コーティング条件は第１表に示す通り
で、膜厚は全て０．９μｍである。この電気絶縁性材料
を酸化雰囲気中で３００〜８００℃の温度で熱処理を行
った。The coating conditions are as shown in Table 1, and the film thicknesses are all 0.9 μm. This electrically insulating material was heat-treated at a temperature of 300 to 800 ° C. in an oxidizing atmosphere.
【００２９】第２表はこの材料の熱処理後の電気抵抗値
であり、ピンホールのない〔Ｂ〕ＳＵＳ４３０ＢＡ基板
では５００〜８００℃の熱処理温度で絶縁性が向上して
いる。Table 2 shows the electric resistance value of this material after heat treatment. In the [B] SUS430BA substrate having no pinhole, the insulating property is improved at the heat treatment temperature of 500 to 800 ° C.
【００３０】ピンホール等の欠陥があるもの〔Ａ〕は７
５０℃以上の温度では、ステンレス基板の酸化により絶
縁性が低下している。[A] having a defect such as a pinhole is 7
At a temperature of 50 ° C. or higher, the insulating property is lowered due to the oxidation of the stainless steel substrate.
【００３１】[0031]
【表１】 [Table 1]
【００３２】[0032]
【表２】 [Table 2]
【００３３】[0033]
【表３】 [Table 3]
【００３４】[0034]
【表４】 [Table 4]
【００３５】[0035]
【発明の効果】本発明によれば、成膜処理を行った後に
酸化雰囲気中で５００℃以上の熱処理を行うことによ
り、電気絶縁性に優れる板状材料を提供することができ
る。According to the present invention, it is possible to provide a plate-shaped material having excellent electrical insulation properties by performing heat treatment at 500 ° C. or higher in an oxidizing atmosphere after performing a film forming process.
【図１】熱処理条件と合格率の関係を示す図。FIG. 1 is a diagram showing a relationship between heat treatment conditions and a pass rate.
【図２】非熱処理材および各熱処理温度で熱処理後のＡ
ｌ2Ｏ3-x膜の深さ方向のＯ／Ａｌ組成比分布を示す図。[Fig. 2] Non-heat treated material and A after heat treatment at each heat treatment temperature
l 2 O 3-x shows the O / Al composition ratio distribution in the depth direction of the film.
Claims (1)
コーティングし、引き続いて酸化雰囲気中で５００℃以
上の温度で熱処理することを特徴とするアルミナ膜をコ
ーティングした絶縁材料の製造方法。1. A method for producing an insulating material coated with an alumina film, which comprises dry-coating an alumina film on a stainless steel substrate and subsequently heat-treating at a temperature of 500 ° C. or higher in an oxidizing atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13759792A JPH05306460A (en) | 1992-05-01 | 1992-05-01 | Method for producing insulating material coated with alumina film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13759792A JPH05306460A (en) | 1992-05-01 | 1992-05-01 | Method for producing insulating material coated with alumina film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05306460A true JPH05306460A (en) | 1993-11-19 |
Family
ID=15202423
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13759792A Withdrawn JPH05306460A (en) | 1992-05-01 | 1992-05-01 | Method for producing insulating material coated with alumina film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05306460A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006196483A (en) * | 2005-01-11 | 2006-07-27 | Dainippon Printing Co Ltd | Wiring board and manufacturing method thereof |
| JP2008280578A (en) * | 2007-05-10 | 2008-11-20 | Ulvac Japan Ltd | Method for forming metal oxide film |
| WO2012077827A1 (en) | 2010-12-10 | 2012-06-14 | Ｊｆｅスチール株式会社 | Steel foil for solar cell substrate, solar cell substrate, solar cell, and methods for manufacturing the steel foil and the solar cell |
| WO2013175643A1 (en) | 2012-05-23 | 2013-11-28 | Ｊｆｅスチール株式会社 | Stainless steel foil solar cell substrate material and method for manufacturing same |
| JP2015105387A (en) * | 2013-11-28 | 2015-06-08 | 中外炉工業株式会社 | Film deposition method, production method of insulating substrate, and module |
-
1992
- 1992-05-01 JP JP13759792A patent/JPH05306460A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006196483A (en) * | 2005-01-11 | 2006-07-27 | Dainippon Printing Co Ltd | Wiring board and manufacturing method thereof |
| JP2008280578A (en) * | 2007-05-10 | 2008-11-20 | Ulvac Japan Ltd | Method for forming metal oxide film |
| WO2012077827A1 (en) | 2010-12-10 | 2012-06-14 | Ｊｆｅスチール株式会社 | Steel foil for solar cell substrate, solar cell substrate, solar cell, and methods for manufacturing the steel foil and the solar cell |
| KR20140074248A (en) | 2010-12-10 | 2014-06-17 | 제이에프이 스틸 가부시키가이샤 | Steel foil for solar cell substrate, solar cell substrate, solar cell, and methods for manufacturing the steel foil and the solar cell |
| WO2013175643A1 (en) | 2012-05-23 | 2013-11-28 | Ｊｆｅスチール株式会社 | Stainless steel foil solar cell substrate material and method for manufacturing same |
| US10312385B2 (en) | 2012-05-23 | 2019-06-04 | Jfe Steel Corporation | Solar cell substrate made of stainless steel foil and method for manufacturing the same |
| JP2015105387A (en) * | 2013-11-28 | 2015-06-08 | 中外炉工業株式会社 | Film deposition method, production method of insulating substrate, and module |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 19990706 |