JPH0551285A - Formation of composite of alumina and aluminum nitride - Google Patents
Formation of composite of alumina and aluminum nitrideInfo
- Publication number
- JPH0551285A JPH0551285A JP3209577A JP20957791A JPH0551285A JP H0551285 A JPH0551285 A JP H0551285A JP 3209577 A JP3209577 A JP 3209577A JP 20957791 A JP20957791 A JP 20957791A JP H0551285 A JPH0551285 A JP H0551285A
- Authority
- JP
- Japan
- Prior art keywords
- alumina
- aluminum nitride
- film
- powder
- composite
- 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
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0306—Inorganic insulating substrates, e.g. ceramic, glass
Landscapes
- Other Surface Treatments For Metallic Materials (AREA)
- Ceramic Products (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、アルミナ・窒化アル
ミニウム複合体からなる板状体を得たり、基材表面にア
ルミナ・窒化アルミニウム複合体からなる皮膜を有する
基板を得たりする方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for obtaining a plate-like body made of an alumina / aluminum nitride composite or a substrate having a coating film made of an alumina / aluminum nitride composite on the surface of a base material.
【０００２】[0002]
【従来の技術】アルミナ・窒化アルミニウム複合体から
なる板状体、または、基材表面にアルミナ・窒化アルミ
ニウム複合体からなる皮膜を有する基板は、電子回路基
板や耐高温腐食用表面処理等の用途において電気的性能
や耐腐食性能などに優れているため、大いに必要とされ
ている。2. Description of the Related Art Plates made of an alumina / aluminum nitride composite or substrates having a film made of an alumina / aluminum nitride composite on the surface of a substrate are used for electronic circuit boards and surface treatments for high temperature corrosion resistance. It is highly required for its excellent electrical performance and corrosion resistance.
【０００３】このようなアルミナ・窒化アルミニウム複
合体を得るためには、従来、アルミニウムを窒化処理し
て窒化アルミニウム粉体を得るか、アルミナから還元処
理して窒化アルミニウム粉体を得るかしたのち、この窒
化アルミニウム粉体にアルミナ粉体を混合し焼結してア
ルミナ・窒化アルミニウム複合体からなる板状体を製造
するようにしていた。また、皮膜付き基板については、
このアルミナ・窒化アルミニウム複合体からなる板状体
を基材上に貼りつけると言う方法によって製造してい
た。In order to obtain such an alumina / aluminum nitride composite, conventionally, aluminum is subjected to a nitriding treatment to obtain an aluminum nitride powder or a reduction treatment from alumina to obtain an aluminum nitride powder. Alumina powder was mixed with this aluminum nitride powder and sintered to produce a plate-like body made of an alumina / aluminum nitride composite. For coated substrates,
It was manufactured by a method of sticking a plate-shaped body made of this alumina-aluminum nitride composite on a substrate.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、アルミ
ナ・窒化アルミニウム複合体からなる板状体を製造する
前記従来の方法は、工程数が多いと言う問題点があっ
た。また、皮膜付き基板を製造する前記従来の方法は、
貼付け工程があって工程数が多くなるほか、貼付けが不
足し、かつ貼付け面全面で均一な接合力が得にくいと言
う問題もあった。さらに、前記アルミナ・窒化アルミニ
ウム複合体からなる板状体は厚みがあるため、本当の意
味での「皮膜」状ではないと言う問題もあった。However, the above-mentioned conventional method for producing a plate-like body made of an alumina / aluminum nitride composite has a problem that it requires a large number of steps. Further, the conventional method for producing a film-coated substrate is
There is a problem that the number of steps is increased due to the attaching step, the attaching is insufficient, and it is difficult to obtain a uniform joining force over the entire attaching surface. Furthermore, since the plate-shaped body made of the alumina-aluminum nitride composite has a thickness, there is a problem that it is not a "film" in the true sense.
【０００５】そこで、この発明は、製造工程数が少な
く、しかも皮膜付き基板を得る場合においては接合力が
強くかつ均一で薄い皮膜が得られるアルミナ・窒化アル
ミニウム複合体の製造方法を提供することを課題とす
る。Therefore, the present invention provides a method of manufacturing an alumina-aluminum nitride composite body which has a small number of manufacturing steps and has a strong bonding force and a uniform and thin film can be obtained when a substrate with a film is obtained. It is an issue.
【０００６】[0006]
【課題を解決するための手段】このような課題を解決す
るため、この発明にかかるアルミナと窒化アルミニウム
の複合体形成方法は、第１に、アルミナ粉体とアルミニ
ウム粉体との混合物を基材上に溶射することにより前記
基材表面に溶射皮膜を形成したのち、窒素雰囲気中で熱
処理して前記溶射皮膜中のアルミニウム成分を窒化アル
ミニウムに変化させることによりアルミナ・窒化アルミ
ニウム複合体からなる皮膜を得るようにする。この場
合、熱処理温度が６００〜１３００°Ｃであることが好
ましい。この温度が６００°Ｃ未満であると窒化反応が
十分には進行しにくく、１３００°Ｃを超えると反応が
急激に起こりすぎ、粉体状の窒化アルミニウムが生成し
て皮膜状になりにくい傾向があるからである。In order to solve the above problems, the method for forming a composite of alumina and aluminum nitride according to the present invention firstly uses a mixture of alumina powder and aluminum powder as a base material. After forming a sprayed coating on the surface of the base material by spraying on it, heat treatment in a nitrogen atmosphere to change the aluminum component in the sprayed coating to aluminum nitride to form a coating composed of an alumina / aluminum nitride composite. To get it. In this case, the heat treatment temperature is preferably 600 to 1300 ° C. If this temperature is less than 600 ° C, the nitriding reaction is difficult to proceed sufficiently, and if it exceeds 1300 ° C, the reaction occurs too rapidly, and powdery aluminum nitride tends to be formed, and it tends to be difficult to form a film. Because there is.
【０００７】この発明にかかるアルミナと窒化アルミニ
ウムの複合体形成方法は、第２に、アルミナ粉体とカー
ボン粉体との混合物を基材上に溶射することにより前記
基材表面に溶射皮膜を形成したのち、窒素雰囲気中で熱
処理して前記溶射皮膜中のアルミナ成分の少なくとも一
部を窒化アルミニウムに変化させることによりアルミナ
・窒化アルミニウム複合体からなる皮膜を得るようにす
る。この場合、溶射皮膜の表面にカーボン粉体を塗布し
ておいて熱処理を行うことが好ましい。このようにする
と、アルミナの還元が一層良好に起きるからである。こ
のとき、カーボン粉体の塗布厚みを ０．０２mg/mm2以
上にすることが好ましい。これより薄いと、塗布効果が
あまりないからである。カーボン粉体の平均粒径は、一
般に、０．０５〜３０μm である。この大きさが適当で
あると言う理由のほかに、このような粒径のものが実用
的に入手しやすいと言う理由もある。カーボン粉体の塗
布量は溶射時に飛散して目減りするので多い目が良い。
カーボン粉体は、通常、アセトン等の溶剤と混ぜ合わせ
て懸濁液を得て、これを塗布するようにするのが良い。
第２の発明では、熱処理温度は１３００°Ｃ以上である
ことが好ましい。このような高温にしないと還元処理が
十分に起きにくいからである。In the method of forming a composite of alumina and aluminum nitride according to the present invention, secondly, a sprayed coating is formed on the surface of the base material by spraying a mixture of alumina powder and carbon powder onto the base material. After that, heat treatment is performed in a nitrogen atmosphere to change at least a part of the alumina component in the thermal spray coating to aluminum nitride to obtain a coating made of an alumina / aluminum nitride composite. In this case, it is preferable to apply carbon powder to the surface of the thermal spray coating and then perform heat treatment. This is because if this is done, the reduction of alumina will occur better. At this time, it is preferable that the coating thickness of the carbon powder is 0.02 mg / mm 2 or more. This is because if it is thinner than this, the coating effect is not so great. The average particle size of the carbon powder is generally 0.05 to 30 μm. In addition to the reason that this size is appropriate, there is also the reason that such a particle size is practically available. The coating amount of carbon powder is good because it is scattered during spraying and decreases.
The carbon powder is usually mixed with a solvent such as acetone to obtain a suspension, which is preferably applied.
In the second invention, the heat treatment temperature is preferably 1300 ° C or higher. This is because reduction treatment does not occur sufficiently unless the temperature is set to such a high temperature.
【０００８】第１の発明でも第２の発明でも、アルミナ
粉体とアルミニウム粉体、または、アルミナ粉体とカー
ボン粉体とは、単に混合して溶射しても良く、これらの
混合物を造粒してたら溶射しても良い。この発明におい
て、溶射手段に限定はないが、たとえばガス溶射ではア
ルミナが溶けにくいが、プラズマ溶射では高温が得やす
い等の理由で、プラズマ溶射を採用することが好まし
い。In both the first invention and the second invention, the alumina powder and the aluminum powder, or the alumina powder and the carbon powder may be simply mixed and sprayed, and the mixture thereof is granulated. You can spray it. In the present invention, the thermal spraying means is not limited, but it is preferable to employ plasma thermal spraying because, for example, gas thermal spraying does not easily melt alumina, but plasma thermal spraying easily obtains high temperatures.
【０００９】この発明で用いる基材の材料は、アルミナ
等のセラミックや鉄、ニッケル等の金属など溶射に耐え
るもであることが必要である。基材表面に形成する溶射
皮膜の厚みは、５０〜３００μm 程度である。第１の発
明でも第２の発明でも、アルミナ粉体の平均粒径は０．
３〜１００μm であることが好ましい。この程度に細か
い方が第２の発明では還元反応が進行しやすいと言う理
由のほかに、このような粒径のものが実用的に入手しや
すいと言う理由もある。The material of the base material used in the present invention must be resistant to thermal spraying such as ceramics such as alumina and metals such as iron and nickel. The thickness of the thermal spray coating formed on the surface of the base material is about 50 to 300 μm. In both the first invention and the second invention, the average particle size of the alumina powder is 0.
It is preferably 3 to 100 μm. In addition to the reason that the reduction reaction is more likely to proceed in the second aspect of the invention, the reason why the particle size is as fine as this is also the reason that the particles having such a particle size are practically easily available.
【００１０】アルミナ粉体の粒径もカーボン粉体の粒径
も、ともに、細かな粒径のものを造粒してこのような粒
径にした場合の粒径であっても良い。Both the particle diameter of the alumina powder and the particle diameter of the carbon powder may be the particle diameters obtained by granulating fine particle diameters to obtain such particle diameters.
【００１１】[0011]
【作用】溶射によって基材上に、アルミナ粉体とアルミ
ニウム粉体またはカーボン粉体からなる溶射皮膜を形成
したのち、窒素雰囲気中で熱処理するようにすると、ア
ルミナ・窒化アルミニウム複合体の製造工程そのものが
簡略となる。皮膜付き基板を得る場合であると、貼付け
工程も省略できる。溶射によって皮膜を基材に付着させ
るので、付着力が均一かつ強くなる。[Function] When a thermal spray coating made of alumina powder and aluminum powder or carbon powder is formed on a substrate by thermal spraying and then heat treatment is carried out in a nitrogen atmosphere, the manufacturing process of the alumina-aluminum nitride composite itself Is simplified. In the case of obtaining a film-coated substrate, the attaching step can be omitted. Since the coating is attached to the base material by thermal spraying, the adhesion becomes uniform and strong.
【００１２】この場合、溶射皮膜中では、アルミナ粉体
の粒子からなるしっかりとした骨格が出来ていて、その
隙間中にアルミニウム粉体やカーボン粉体が入り込んで
おり、したがって窒化処理や還元処理に際して窒素が皮
膜の内部深く入り込むことができ、処理効率が上がるほ
か、内部深くまでの処理も十分にできる。これに対し、
第１の発明において、このような骨格がなく、アルミニ
ウム粉末のみであると、熱処理後に直ちに、アルミニウ
ム粉末溶射皮膜の最表面が緻密な窒化アルミニウム層と
なり、そのために窒素ガスが溶射皮膜の内部に浸透しに
くく、窒化アルミニウムの生成が不充分となる。In this case, a solid skeleton made of particles of alumina powder is formed in the thermal spray coating, and aluminum powder or carbon powder is inserted into the gaps, and therefore, during nitriding treatment or reduction treatment. Nitrogen can penetrate deep inside the film, increasing the processing efficiency and sufficiently deep inside the film. In contrast,
In the first invention, if there is no such skeleton and only aluminum powder is present, the outermost surface of the aluminum powder sprayed coating becomes a dense aluminum nitride layer immediately after heat treatment, so that nitrogen gas penetrates into the sprayed coating. It is difficult to do so, and the production of aluminum nitride becomes insufficient.
【００１３】[0013]
【実施例】以下に、この発明の実施例を説明するが、こ
の発明の範囲はこれらの実施例に限定されない。 −実施例１− 平均粒径１５μm のアルミニウム粉体と平均粒径５５μ
m のアルミナ粉体とを１：１のモル比で混合してなる混
合粉体をアルゴン・水素の混合ガスを用いて出力３５kW
でアルミナ焼結基材表面にプラズマ溶射した。その膜厚
は２００μmであった。これを真空炉に入れ、窒素置換
したあと、窒素ガスを流量３００リットル／分で流しつ
つ、１０００°Ｃ、３時間の熱処理を行った。得られた
アルミナ・窒化アルミニウム複合体皮膜では、窒化物比
率が、窒化アルミニウムとアルミナ合計量の２０体積％
であった。EXAMPLES Examples of the present invention will be described below, but the scope of the present invention is not limited to these examples. -Example 1-Aluminum powder having an average particle size of 15 μm and an average particle size of 55 μm
Output of 35 kW using mixed gas of argon and hydrogen mixed powder made by mixing alumina powder of m with a molar ratio of 1: 1
Then, the surface of the alumina sintered substrate was plasma sprayed. The film thickness was 200 μm. This was placed in a vacuum furnace, and after nitrogen substitution, heat treatment was performed at 1000 ° C. for 3 hours while flowing nitrogen gas at a flow rate of 300 liters / minute. In the obtained alumina / aluminum nitride composite film, the nitride ratio was 20% by volume of the total amount of aluminum nitride and alumina.
Met.
【００１４】−実施例２− 平均粒径１５μm のアルミナ粉体と平均粒径１０μm の
カーボン粉体とを１：３のモル比で混合してなる混合粉
体をアルゴン・水素の混合ガスを用いて出力３５kWでア
ルミナ焼結基材表面にプラズマ溶射した。その膜厚は１
００μm であった。この溶射皮膜中のアルミナ粉体とカ
ーボン粉体のモル比は約１：０．３であって溶射により
カーボン粉体が飛散して約１０％に減少したことが分か
る。この溶射皮膜の表面にカーボン粉体をアセトン中に
懸濁してなる液を０．０２mg/mm2の厚みで塗布したの
ち、これを真空炉に入れ、窒素置換したあと、窒素ガス
を流量３００リットル／分で流しつつ、１５００°Ｃ、
３時間の熱処理を行った。得られたアルミナ・窒化アル
ミニウム複合体皮膜では、窒化物比率が、窒化アルミニ
ウムとアルミナ合計量の２０体積％であった。-Example 2-Alumina powder having an average particle diameter of 15 μm and carbon powder having an average particle diameter of 10 μm are mixed at a molar ratio of 1: 3, and a mixed gas of argon and hydrogen is used. Plasma sprayed on the surface of the alumina sintered substrate at an output of 35 kW. The film thickness is 1
It was 00 μm. The molar ratio of the alumina powder to the carbon powder in this sprayed coating was about 1: 0.3, and it can be seen that the carbon powder was scattered by the spraying and reduced to about 10%. A solution of carbon powder suspended in acetone was applied to the surface of this thermal spray coating at a thickness of 0.02 mg / mm 2 , and this was placed in a vacuum furnace and replaced with nitrogen, and then a nitrogen gas flow rate of 300 liters was applied. 1500 ° C, flowing at
Heat treatment was performed for 3 hours. In the obtained alumina / aluminum nitride composite film, the nitride ratio was 20% by volume of the total amount of aluminum nitride and alumina.
【００１５】[0015]
【発明の効果】この発明にかかるアルミナと窒化アルミ
ニウムの複合体形成方法は、以上にみたとおりであり、
窒化アルミニウム生成と同時に目的とする皮膜ができる
ため、製造工程数が少ない。しかも、得られた皮膜付き
基板は、接合力が強くかつ均一で薄い皮膜を有してい
る。The method for forming a composite of alumina and aluminum nitride according to the present invention is as described above.
Since the desired film is formed at the same time when aluminum nitride is produced, the number of manufacturing steps is small. Moreover, the obtained film-coated substrate has a strong and uniform bonding film.
Claims (3)
合物を基材上に溶射することにより前記基材表面に溶射
皮膜を形成したのち、窒素雰囲気中で熱処理して前記溶
射皮膜中のアルミニウム成分を窒化アルミニウムに変化
させることによりアルミナ・窒化アルミニウム複合体か
らなる皮膜を得るようにすることを特徴とするアルミナ
と窒化アルミニウムの複合体形成方法。1. A spray coating is formed on the surface of the base material by spraying a mixture of alumina powder and aluminum powder on the base material, and then heat treatment is performed in a nitrogen atmosphere to carry out an aluminum component in the spray coating. A method of forming a composite of alumina and aluminum nitride, characterized in that a film comprising an alumina / aluminum nitride composite is obtained by changing the above to aluminum nitride.
を基材上に溶射することにより前記基材表面に溶射皮膜
を形成したのち、窒素雰囲気中で熱処理して前記溶射皮
膜中のアルミナ成分の少なくとも一部を窒化アルミニウ
ムに変化させることによりアルミナ・窒化アルミニウム
複合体からなる皮膜を得るようにすることを特徴とする
アルミナと窒化アルミニウムの複合体形成方法。2. A thermal spray coating is formed on the surface of the base material by spraying a mixture of alumina powder and carbon powder on the base material, and then heat treatment is performed in a nitrogen atmosphere to heat the alumina component in the thermal spray coating. A method of forming a composite of alumina and aluminum nitride, characterized in that a film made of an alumina / aluminum nitride composite is obtained by converting at least a part of the above into aluminum nitride.
ておいて熱処理を行う請求項２記載のアルミナと窒化ア
ルミニウムの複合体形成方法。3. The method for forming a composite of alumina and aluminum nitride according to claim 2, wherein carbon powder is applied to the surface of the thermal spray coating and heat treatment is performed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3209577A JP3059250B2 (en) | 1991-08-21 | 1991-08-21 | Method for forming composite of alumina and aluminum nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3209577A JP3059250B2 (en) | 1991-08-21 | 1991-08-21 | Method for forming composite of alumina and aluminum nitride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0551285A true JPH0551285A (en) | 1993-03-02 |
| JP3059250B2 JP3059250B2 (en) | 2000-07-04 |
Family
ID=16575141
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3209577A Expired - Lifetime JP3059250B2 (en) | 1991-08-21 | 1991-08-21 | Method for forming composite of alumina and aluminum nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3059250B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6026694B1 (en) * | 2016-05-30 | 2016-11-16 | 東芝テック株式会社 | Payment device |
-
1991
- 1991-08-21 JP JP3209577A patent/JP3059250B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP3059250B2 (en) | 2000-07-04 |
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