JPH0798706B2 - Surface treatment method for non-oxide ceramics - Google Patents
Surface treatment method for non-oxide ceramicsInfo
- Publication number
- JPH0798706B2 JPH0798706B2 JP15591292A JP15591292A JPH0798706B2 JP H0798706 B2 JPH0798706 B2 JP H0798706B2 JP 15591292 A JP15591292 A JP 15591292A JP 15591292 A JP15591292 A JP 15591292A JP H0798706 B2 JPH0798706 B2 JP H0798706B2
- Authority
- JP
- Japan
- Prior art keywords
- oxide ceramics
- oxide
- ceramics
- surface treatment
- fine particles
- 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.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5127—Cu, e.g. Cu-CuO eutectic
Description
【０００１】[0001]
【産業上の利用分野】本発明は非酸化物セラミックスの
表面処理方法に係り、詳しくは非酸化物セラミックスを
接合剤あるいはメタライジング剤と強固に接着させる上
で非酸化物セラミックスの表面に例えばＣｕＡｌ2 Ｏ4
あるいはＣｕＡｌＯ2 の酸化物層を形成する非酸化物セ
ラミックスの表面処理方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a surface treatment method for non-oxide ceramics, and more specifically, for strongly adhering non-oxide ceramics to a bonding agent or a metallizing agent, for example, CuAl on the surface of non-oxide ceramics. 2 O 4
Alternatively, it relates to a surface treatment method for non-oxide ceramics which forms an oxide layer of CuAlO 2 .
【０００２】[0002]
【従来の技術】セラミックスは高耐熱性、高硬度という
特徴を有しているが、その反面、機械的・熱的衝撃に弱
い欠点がある。これを補うのに金属と組み合わせたり、
あるいは同じセラミックスでも特性の異なるものを組み
合わせると用途が拡大する。このようにセラミックス
と、セラミックスまたは金属との複合化技術（接合技
術）はセラミックス加工技術の重要な要素技術の１つに
なっている。2. Description of the Related Art Ceramics have the characteristics of high heat resistance and high hardness, but on the other hand, they have the drawback of being weak against mechanical and thermal shocks. To supplement this, combine with metal,
Or if the same ceramics with different characteristics are combined, the application will be expanded. As described above, the technique of combining ceramics with ceramics or metal (joining technique) is one of the important elemental techniques of the ceramics processing technique.
【０００３】ところで、セラミックス同志、セラミック
スと金属との接合方法としては、ＰｂＯ、ＣａＯ、Ａｌ
2 Ｏ3 、ＭｇＯなどの金属酸化物を含むペースト物を接
合剤として用いる方法、あるいはＴｉ系、Ｚｒ系、Ｂｅ
系、Ｎｉ系などの活性金属を含んだペースト状の接合剤
を用いる方法、またＭｏ−Ｍｎ系、Ｍｏ系、Ｗ系等の高
融点金属を被接合材表面でメタライジングし、その表面
にＮｉメッキ、そして金属ろうを付着し、更にもう一方
の被接合材表面にＮｉメッキした後、高温度で接合する
方法が使用されている。By the way, as a method for joining ceramics to each other and ceramics and metals, PbO, CaO, Al
A method of using a paste containing a metal oxide such as 2 O 3 or MgO as a bonding agent, or Ti-based, Zr-based, Be
System, a method using a paste-like bonding agent containing an active metal such as Ni system, or metallizing a refractory metal such as Mo-Mn system, Mo system, W system on the surface of the material to be bonded, and Ni A method is used in which plating, metal brazing is adhered, Ni is plated on the surface of the other material to be bonded, and then bonding is performed at a high temperature.
【０００４】また、他の方法として非酸化物セラミック
スの表面に酸化物層を形成し、該セラミックスと接合剤
との接着性を改善する試みがなされている。例えば、特
公昭６４−４６６８によると、非酸化物セラミックスを
酸化雰囲気中で１０００〜１３００°Ｃの温度で数時間
加熱することにより、非酸化物セラミックス表面にＡｌ
2 Ｏ3 のような酸化物層を形成することが開示されてい
る。As another method, an attempt has been made to form an oxide layer on the surface of non-oxide ceramics to improve the adhesion between the ceramics and the bonding agent. For example, according to Japanese Examined Patent Publication No. 64-4668, by heating non-oxide ceramics in an oxidizing atmosphere at a temperature of 1000 to 1300 ° C. for several hours, Al is applied to the surface of the non-oxide ceramics.
Forming an oxide layer such as 2 O 3 is disclosed.
【０００５】[0005]
【発明が解決しようとする課題】しかし、従来の非酸化
物セラミックスの表面に酸化物層を形成する方法では、
高温雰囲気下で長時間放置して酸化物層を形成しなけれ
ばならず、またセラミックスに損傷を与えやすく、経済
的にも不利な方法であった。本発明はこのような諸問題
を解決するものであり、比較的低い温度で、また短時間
で、しかも任意の場所に酸化物層を形成して接合剤ある
いはメタライジン剤との接着力を向上してなる非酸化物
セラミックスの表面処理方法を提供することを目的とす
る。However, in the conventional method for forming the oxide layer on the surface of the non-oxide ceramics,
This is an economically disadvantageous method because it is necessary to leave the oxide layer for a long time in a high temperature atmosphere to form an oxide layer, and ceramics are easily damaged. The present invention solves these problems, and improves the adhesive strength with a bonding agent or a metallizing agent by forming an oxide layer at an arbitrary location at a relatively low temperature for a short time. An object of the present invention is to provide a surface treatment method for the non-oxide ceramics.
【０００６】[0006]
【課題を解決するための手段】即ち、本発明の非酸化物
セラミックスの表面処理方法では、Ｃｕ，Ｃｕ2 Ｏもし
くはＣｕＯから選ばれた粒径０．１μｍ以下の微粒子を
非酸化物セラミックスの表面に付着させた後、酸化雰囲
気下で熱処理を行うことにより非酸化物セラミックスの
表面に酸化物層を設けた点にある。粒径０．１μｍ以下
のＣｕ，Ｃｕ2 ＯもしくはＣｕＯから選ばれた微粒子
は、溶剤に溶けた高分子のペースト物中に分散してい
る。また、上記酸化物層は主としてＣｕＡｌ2 Ｏ4 ある
いはＣｕＡｌＯ2 である。That is, in the surface treatment method for non-oxide ceramics according to the present invention, fine particles having a particle size of 0.1 μm or less selected from Cu, Cu 2 O or CuO are added to the surface of non-oxide ceramics. This is because the oxide layer is formed on the surface of the non-oxide ceramics by performing a heat treatment in an oxidizing atmosphere after the deposition. Fine particles selected from Cu, Cu 2 O or CuO having a particle size of 0.1 μm or less are dispersed in a polymer paste dissolved in a solvent. The oxide layer is mainly CuAl 2 O 4 or CuAlO 2 .
【０００７】 本発明で使用するＣｕもしくはＣｕ2 Ｏ
から選ばれた微粒子は、以下の方法によって得ることが
できる。即ち、まず高分子材料を融解後、これにより生
じた蒸発物を基材面の上で急速固化して熱力学的に非平
衡化した高分子層を形成し、この高分子層の表面に銅膜
を密着させた後、高分子が平衡状態になるまで緩和さ
せ、該銅膜から微粒子化したＣｕもしくはＣｕ2 Ｏを高
分子層内に浸透させると共に分散させ、これをｍ−クレ
ゾール、１，２−ジクロロエタン、アセトン等の溶剤に
溶かしてペースト物にしたものである。この微粒子を分
散した高分子複合物は、微粒子が凝集せずに独立した状
態で分離分散し、しかも微粒子が高分子層に安定した状
態で分散しているので、経時安定性に優れている。Cu or Cu 2 O used in the present invention
The fine particles selected from can be obtained by the following method. That is, first, after melting the polymer material, the vaporized material generated thereby is rapidly solidified on the surface of the base material to form a thermodynamically non-equilibrium polymer layer, and a copper layer is formed on the surface of the polymer layer. After the film was brought into close contact, the polymer was relaxed until it reached an equilibrium state, finely divided Cu or Cu 2 O was permeated from the copper film into the polymer layer and dispersed therein, and m-cresol, 1 , 2 , It is made into a paste by dissolving it in a solvent such as 2-dichloroethane or acetone. The polymer composite in which the fine particles are dispersed is excellent in stability over time because the fine particles are not dispersed but aggregated and dispersed independently, and the fine particles are stably dispersed in the polymer layer.
【０００８】ここで使用する高分子材料としては、熱可
塑性高分子であり、例えばナイロン６、ナイロン６６、
ナイロン１１、ナイロン１２、ナイロン６９、高密度ポ
リエチレン（ＨＤＰＥ）、低密度ポリエチレン（ＬＤＰ
Ｅ）、ポリフッ化ビニリデン（ＰＶＤＦ）、ポリ塩化ビ
ニル、ポリオキシメチレンなどが挙げられ、特に限定さ
れない。The polymer material used here is a thermoplastic polymer such as nylon 6, nylon 66,
Nylon 11, Nylon 12, Nylon 69, High Density Polyethylene (HDPE), Low Density Polyethylene (LDP)
E), polyvinylidene fluoride (PVDF), polyvinyl chloride, polyoxymethylene and the like are mentioned, but not particularly limited.
【０００９】また、本発明で使用する非酸化物セラミッ
クスは、窒化アルミニウム（ＡｌＮ）、窒化珪素（Ｓｉ
3 Ｎ4 ）、炭化珪素（ＳｉＣ）からなる。The non-oxide ceramics used in the present invention are aluminum nitride (AlN) and silicon nitride (Si).
3 N 4 ) and silicon carbide (SiC).
【００１０】しかして、本発明方法では、まず非酸化物
セラミックスの粉体とＣｕ，Ｃｕ2ＯもしくはＣｕＯの
微粒子を含む高分子複合物を混合し、７００〜９００°
Ｃの酸化雰囲気中で、約１分〜６０分間焼成する。また
他の方法としては非酸化物セラミックスの板体の上にＣ
ｕ，Ｃｕ2 ＯもしくはＣｕＯの微粒子を含むペースト物
を塗布し、７００〜９００°Ｃの酸化雰囲気中で、約１
分〜６０分間焼成する。更に、他の方法としては非酸化
物セラミックスの板体の上にＣｕを真空蒸着、スパッタ
リングあるいは溶融噴霧によって付着し、７００〜９０
０°Ｃの酸化雰囲気中で、約１分〜６０分間焼成する。
この結果、非酸化物セラミックスの表面、特にＣｕ，Ｃ
ｕ2 ＯもしくはＣｕＯから選ばれた微粒子を付着したと
ころのみに、酸化物層が形成される。とりわけ、非酸化
物セラミックスの表面に形成されたＣｕＡｌ2 Ｏ4 ある
いはＣｕＡｌＯ2 の酸化物層は、接合剤との接着力を向
上することができる。In the method of the present invention, however, first, a non-oxide ceramic powder and a polymer composite containing Cu, Cu 2 O or CuO particles are mixed, and the temperature is 700 to 900 °.
Baking is performed in an oxidizing atmosphere of C for about 1 to 60 minutes. As another method, C on a non-oxide ceramic plate is used.
Apply a paste containing fine particles of u, Cu 2 O or CuO, and apply in an oxidizing atmosphere at 700 to 900 ° C for about 1
Bake for minutes to 60 minutes. Further, as another method, Cu is deposited on the plate body of non-oxide ceramics by vacuum deposition, sputtering, or melt spraying, and the temperature is 700 to 90.
Baking is performed in an oxidizing atmosphere at 0 ° C. for about 1 to 60 minutes.
As a result, the surface of non-oxide ceramics, especially Cu, C
The oxide layer is formed only where the fine particles selected from u 2 O or CuO are attached. In particular, the CuAl 2 O 4 or CuAlO 2 oxide layer formed on the surface of the non-oxide ceramics can improve the adhesive force with the bonding agent.
【００１１】[0011]
【作用】即ち、本発明によると、非酸化物セラミックス
の表面にＣｕ，Ｃｕ2 ＯもしくはＣｕＯの粒径０．１μ
ｍの微粒子を付着させた後、比較的低温でかつ短時間で
焼成しても、微粒子の粒径が小さいために該セラミック
スの表面には例えばＣｕＡｌ2 Ｏ4 あるいはＣｕＡｌＯ
2 の酸化物層が形成される。そして、この酸化物層の表
面に、例えばＣｕあるいはＣｕ2 Ｏの粉体とバインダー
からなるメタライジング剤を塗布して焼成すると、本発
明により得られたＣｕＡｌ2 Ｏ4 あるいはＣｕＡｌＯ2
の酸化物層が非酸化物セラミックスとメタライズ膜の両
方に化学的に結合するため、非酸化物セラミックスとメ
タライズ膜との接着力が向上する。また、比較的低温で
かつ短時間で焼成して非酸化物セラミックスの表面に酸
化物層を形成することができるため、被接合材である非
酸化物セラミックスの基板の熱劣化を避けることもでき
る。According to the present invention, the particle size of Cu, Cu 2 O or CuO is 0.1 μm on the surface of the non-oxide ceramics.
Even if the fine particles of m are adhered and then fired at a relatively low temperature for a short time, the particle diameter of the fine particles is small, so that, for example, CuAl 2 O 4 or CuAlO is formed on the surface of the ceramic.
Two oxide layers are formed. Then, a metallizing agent composed of, for example, Cu or Cu 2 O powder and a binder is applied to the surface of the oxide layer and fired to obtain CuAl 2 O 4 or CuAlO 2 obtained by the present invention.
Since the oxide layer is chemically bonded to both the non-oxide ceramics and the metallized film, the adhesive force between the non-oxide ceramics and the metallized film is improved. Further, since the oxide layer can be formed on the surface of the non-oxide ceramics by firing at a relatively low temperature for a short time, it is possible to avoid thermal deterioration of the substrate of the non-oxide ceramics which is the material to be joined. .
【００１２】[0012]
【実施例】次に、本発明を具体的な実施例により更に詳
細に説明する。 （Ｃｕ2 Ｏ微粒子を含んだ高分子複合物の作成）真空蒸
着装置により、ナイロン１１ペレットをタングステンボ
ード中に入れ、１０-6Ｔｏｒｒに減圧する。次いで、電
極間に電圧を印加してタングステンボードを真空中で加
熱して、ポリマーを融解させ、取り付け台の上部に設置
した基材（ガラス板）上に、１０-4〜１０-6Ｔｏｒｒの
真空度で約１μｍ／分の速度で厚さ約５μｍの蒸着膜で
ある高分子層を得た。更に、銅をタングステン線に巻き
付け加熱融解して１０-4〜１０-6Ｔｏｒｒの真空下で蒸
着を行い、高分子層の上に銅蒸着膜を付着し、この積層
膜が付着したガラス板を真空蒸着装置から取り出し、１
２０℃に保持した恒温槽中に１０分間放置して複合物を
得た。その結果、膜表面の赤色が無くなり、膜全体が透
明黄緑色に変化した。Next, the present invention will be described in more detail with reference to specific examples. (Preparation of Polymer Composite Containing Cu 2 O Fine Particles) Nylon 11 pellets are put into a tungsten board and decompressed to 10 −6 Torr by a vacuum vapor deposition apparatus. Next, a voltage is applied between the electrodes to heat the tungsten board in a vacuum to melt the polymer, and 10 -4 to 10 -6 Torr of the polymer is melted on the base material (glass plate) placed on the upper part of the mounting table. A polymer layer as a vapor-deposited film having a thickness of about 5 μm was obtained at a rate of vacuum of about 1 μm / min. Further, copper is wrapped around a tungsten wire, heated and melted, and vapor-deposited under a vacuum of 10 −4 to 10 −6 Torr. Take out from the vacuum vapor deposition device, 1
The composite was obtained by leaving it in a constant temperature bath kept at 20 ° C. for 10 minutes. As a result, the red color on the surface of the film disappeared and the entire film changed to transparent yellow-green.
【００１３】このように得られた試料を入射角０．５°
の薄膜Ｘ線回折装置（理学電気社製ＲＩＮＴ１２００）
を用いて、同試料のＸ線回折パターンを測定した。この
Ｘ線回折パターンでは、銅はＣｕ2 Ｏ（酸化銅）に変化
し、この微粒子がナイロン１１中に分散していることが
判った。The sample obtained in this manner was used for the incident angle of 0.5 °.
Thin film X-ray diffractometer (RINT1200 manufactured by Rigaku Denki Co., Ltd.)
Was used to measure the X-ray diffraction pattern of the same sample. In this X-ray diffraction pattern, it was found that copper changed to Cu 2 O (copper oxide), and the fine particles were dispersed in nylon 11.
【００１４】また、Ｃｕ2 Ｏの微粒子の粒子径を透過型
電子顕微鏡写真から観察すると、その平均粒子径は約１
０ｎｍであり、また添加量は１８ｖｏｌ％であった。ナ
イロン１１中にＣｕ2 Ｏを１８ｖｏｌ％微粒化分散させ
た高分子複合物をｍ−クレゾールに重量比１：１で溶か
したペースト物にした。When the particle size of Cu 2 O particles is observed from a transmission electron micrograph, the average particle size is about 1
It was 0 nm, and the added amount was 18 vol%. A polymer composite having 18 vol% Cu 2 O atomized and dispersed in nylon 11 was dissolved in m-cresol at a weight ratio of 1: 1 to obtain a paste.
【００１５】実施例１〜７ 表１に示した焼成条件にしたがって窒化アルミニウム粉
（粒径１μｍ）とＣｕ2 Ｏ微粒子（粒径１０ｎｍ）を分
散させた高分子複合物の混合物を焼成した。窒化アルミ
ニウム粉とＣｕ2 Ｏ微粒子の重量比は２０／１である。
焼成後の試料を前述と同じ入射角０．５°の薄膜Ｘ線回
折装置を用いて、これらの試料のＸ線回折パターンを測
定した結果を図１、図２に示す。これによると、８００
°Ｃ以上の温度では焼成時間１０分という短時間にＣｕ
Ａｌ2 Ｏ4 が生成する。特に、１０００°Ｃでは酸化反
応が急激に進行し、窒化アルミニウムおよびＣｕＯが全
てＣｕＡｌ2 Ｏ4 およびＡｌ2 Ｏ3 に変化している。ま
た、焼成温度７００°Ｃの場合、１０分間の焼成時間で
はＣｕＡｌ2 Ｏ4 が認められなかったが、焼成時間を３
０分まで増加させるとＣｕＡｌ2 Ｏ4 が生成することが
判る。Examples 1 to 7 According to the firing conditions shown in Table 1, a mixture of polymer composites in which aluminum nitride powder (particle diameter 1 μm) and Cu 2 O fine particles (particle diameter 10 nm) were dispersed was fired. The weight ratio of aluminum nitride powder to Cu 2 O fine particles is 20/1.
1 and 2 show the results of measuring the X-ray diffraction patterns of the samples after firing using the thin film X-ray diffractometer having the same incident angle of 0.5 ° as described above. According to this, 800
At temperatures above ° C, Cu was burned in a short time of 10 minutes.
Al 2 O 4 is produced. Particularly, at 1000 ° C., the oxidation reaction rapidly progresses, and aluminum nitride and CuO are all changed to CuAl 2 O 4 and Al 2 O 3 . Further, when the firing temperature was 700 ° C., CuAl 2 O 4 was not observed in the firing time of 10 minutes, but the firing time was 3
It can be seen that CuAl 2 O 4 is produced when the content is increased to 0 minutes.
【００１６】[0016]
【表１】 [Table 1]
【００１７】実施例８〜９、比較例１〜２ 表２の内容にしたがって窒化アルミニウム焼結体基板の
表面にＣｕ2 Ｏ微粒子を塗布し焼成した。塗布方法はＣ
ｕ2 Ｏ微粒子を分散した高分子複合物のペースト物をナ
イフを用いて窒化アルミニウム焼結体基板の表面に塗布
した。焼成後の試料表面に、Ｃｕ粉／Ｃｕ2 Ｏ粉／ナイ
ロン１１の有機バインダーからなる導体路形成ペースト
を塗布し、１０-3Ｔｏｒｒの減圧下、８００°Ｃ、５分
間、空気中で焼成を行ってメタライズ膜を形成した。得
られたメタライズ膜と窒化アルミニウム焼結体との接着
強度を表２に示す。この接着強度の測定方法において
は、まず窒化アルミニウム焼結体基板の表面にに２×２
ｍｍのメタライズ膜を作り、このメタライズ膜にハンダ
付けによってＬ字型に曲げた直径０．８ｍｍの銅線を接
着し、この銅線を引っ張ることによってメタライズ膜の
接着強度を測定した。Examples 8-9, Comparative Examples 1-2 According to the contents of Table 2, Cu 2 O fine particles were applied to the surface of the aluminum nitride sintered substrate and baked. The coating method is C
The paste of the polymer composite in which the u 2 O particles were dispersed was applied to the surface of the aluminum nitride sintered body substrate using a knife. A conductor path forming paste made of an organic binder of Cu powder / Cu 2 O powder / nylon 11 is applied to the surface of the sample after baking, and baking is performed in air at 800 ° C. for 5 minutes under a reduced pressure of 10 −3 Torr. Then, a metallized film was formed. Table 2 shows the adhesive strength between the obtained metallized film and the aluminum nitride sintered body. In this method of measuring the adhesive strength, first, 2 × 2 is formed on the surface of the aluminum nitride sintered body substrate.
A metallized film having a diameter of 0.8 mm was formed, a copper wire having a diameter of 0.8 mm which was bent into an L shape by soldering was adhered to the metallized film, and the adhesive strength of the metallized film was measured by pulling the copper wire.
【００１８】[0018]
【表２】 [Table 2]
【００１９】この結果、窒化アルミニウム焼結体基板の
表面の目的とする位置に酸化物層を形成することによっ
て、窒化アルミニウム焼結体基板とメタライズ膜の接着
強度が向上していることが判る。As a result, it is understood that the adhesion strength between the aluminum nitride sintered body substrate and the metallized film is improved by forming the oxide layer at the desired position on the surface of the aluminum nitride sintered body substrate.
【００２０】実施例１０〜１１、比較例３〜４ 表３の内容に従って窒化ケイ素（Ｓｉ3 Ｎ4 ）焼結体、
炭化ケイ素（ＳｉＣ）焼結体の焼成を行った。前述と同
じＸ線回折法による分析結果を図３、図４に示す。Examples 10-11, Comparative Examples 3-4 Silicon nitride (Si 3 N 4 ) sintered bodies according to the contents of Table 3,
The silicon carbide (SiC) sintered body was fired. The results of analysis by the same X-ray diffraction method as described above are shown in FIGS.
【００２１】[0021]
【表３】 [Table 3]
【００２２】これによると、窒化アルミニウムに限ら
ず、窒化ケイ素、炭化ケイ素等の非酸化物セラミックス
もＣｕ2 Ｏ微粒子を塗布、焼成することによって比較的
容易に酸化物層を形成することができる。According to this method, not only aluminum nitride but also non-oxide ceramics such as silicon nitride and silicon carbide can form the oxide layer relatively easily by coating and firing Cu 2 O fine particles.
【００２３】[0023]
【発明の効果】以上のように本発明の非酸化物セラミッ
クスの表面処理方法では、非酸化物セラミックスの表面
に比較的低い温度で、しかも任意の場所に酸化物層を形
成することによって、接合剤との接着力を向上すること
ができる。また、比較的低温でかつ短時間で焼成して非
酸化物セラミックスの表面に酸化物層を形成することが
できるため、被接合材である非酸化物セラミックスの基
板の熱劣化を避けることもできる。As described above, according to the surface treatment method for non-oxide ceramics of the present invention, bonding is performed by forming an oxide layer on the surface of non-oxide ceramics at a relatively low temperature and at an arbitrary position. The adhesive strength with the agent can be improved. In addition, since the oxide layer can be formed on the surface of the non-oxide ceramics by firing at a relatively low temperature for a short time, it is possible to avoid thermal deterioration of the substrate of the non-oxide ceramics as the material to be joined. .
【図１】実施例１〜実施例５における焼成後の試料のＸ
線回折パターンを示す図である。FIG. 1 is X of a sample after firing in Examples 1 to 5.
It is a figure which shows a line diffraction pattern.
【図２】実施例２、実施例６そして実施例７における焼
成後の試料のＸ線回折パターンを示す図である。FIG. 2 is a diagram showing X-ray diffraction patterns of samples after firing in Examples 2, 6 and 7.
【図３】実施例１０、比較例３における焼成後の試料の
Ｘ線回折パターンを示す図である。FIG. 3 is a diagram showing an X-ray diffraction pattern of samples after firing in Example 10 and Comparative Example 3.
【図４】実施例１１、比較例４における焼成後の試料の
Ｘ線回折パターンを示す図である。FIG. 4 is a diagram showing X-ray diffraction patterns of samples after firing in Example 11 and Comparative Example 4.
Claims (4)
れた粒径０．１μｍ以下の微粒子を非酸化物セラミック
スの表面に付着させた後、酸化雰囲気下で熱処理を行う
ことにより非酸化物セラミックスの表面に酸化物層を設
けたことを特徴とする非酸化物セラミックスの表面処理
方法。1. Non-oxide ceramics are prepared by depositing fine particles having a particle size of 0.1 μm or less selected from Cu, Cu 2 O or CuO on the surface of non-oxide ceramics, and then performing heat treatment in an oxidizing atmosphere. A method for surface treatment of non-oxide ceramics, characterized in that an oxide layer is provided on the surface of.
しくはＣｕＯから選ばれた微粒子は、溶剤に溶けた高分
子のペースト物中に分散している請求項１記載の非酸化
物セラミックスの表面処理方法。2. The non-oxide ceramics according to claim 1, wherein the fine particles selected from Cu, Cu 2 O or CuO having a particle diameter of 0.1 μm or less are dispersed in a polymer paste dissolved in a solvent. Surface treatment method.
ムである請求項１記載の非酸化物セラミックスの表面処
理方法。3. The surface treatment method for non-oxide ceramics according to claim 1, wherein the non-oxide ceramics is aluminum nitride.
る酸化物層が、主としてＣｕＡｌ2 Ｏ4 あるいはＣｕＡ
ｌＯ2 である請求項３記載の非酸化物セラミックスの表
面処理方法。4. The oxide layer formed on the surface of the non-oxide ceramic is mainly CuAl 2 O 4 or CuA.
10. The method for surface treatment of non-oxide ceramics according to claim 3, which is 10 2 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15591292A JPH0798706B2 (en) | 1992-05-21 | 1992-05-21 | Surface treatment method for non-oxide ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15591292A JPH0798706B2 (en) | 1992-05-21 | 1992-05-21 | Surface treatment method for non-oxide ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06321663A JPH06321663A (en) | 1994-11-22 |
| JPH0798706B2 true JPH0798706B2 (en) | 1995-10-25 |
Family
ID=15616233
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15591292A Expired - Fee Related JPH0798706B2 (en) | 1992-05-21 | 1992-05-21 | Surface treatment method for non-oxide ceramics |
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| Country | Link |
|---|---|
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| EP1241148B1 (en) * | 2001-03-16 | 2008-07-09 | Electrovac, Fabrikation Elektrotechnischer Spezialartikel Gesellschaft M.B.H. | Aluminium nitride substrate and method of preparing this substrate for joining with a copper foil |
| US20070231590A1 (en) * | 2006-03-31 | 2007-10-04 | Stellar Industries Corp. | Method of Bonding Metals to Ceramics |
| CN108249948B (en) * | 2016-12-29 | 2020-10-20 | 比亚迪股份有限公司 | Aluminum nitride ceramic and preparation method and application thereof |
| KR102017081B1 (en) * | 2018-06-25 | 2019-09-02 | (주)윈스 | A conductive ceramic composition having excellent electric-conductivity |
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1992
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| Publication number | Publication date |
|---|---|
| JPH06321663A (en) | 1994-11-22 |
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