JPH0624854A - Ceramics-metal joining body - Google Patents
Ceramics-metal joining bodyInfo
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- JPH0624854A JPH0624854A JP17691992A JP17691992A JPH0624854A JP H0624854 A JPH0624854 A JP H0624854A JP 17691992 A JP17691992 A JP 17691992A JP 17691992 A JP17691992 A JP 17691992A JP H0624854 A JPH0624854 A JP H0624854A
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- metal
- nitride
- ceramic
- active metal
- ceramics
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、セラミックス部材と金
属部材との接合体に係り、特に耐冷熱サイクル特性に優
れたセラミックス−金属接合体に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a bonded body of a ceramic member and a metal member, and more particularly to a ceramic-metal bonded body excellent in cold-heat cycle resistance.
【０００２】[0002]
【従来の技術】窒化物系セラミックス材料は、一般に、
軽量でかつ高硬度を有する、電気絶縁性に優れる、耐熱
性や耐食性に優れる等という特徴を有しており、これら
の特徴を生かして構造用材料や電気部品用材料等として
利用されている。ところで、例えば窒化物系セラミック
ス材料を構造材として使用する場合、セラミックス材料
は本来脆性材料であるため、金属材料と接合して用いる
ことが一般的である。一方、窒化物系セラミックス材料
の高電気絶縁性という特性を利用して、電子部品の搭載
基板等として使用する際にも、電気回路の形成等を目的
として、金属と接合することが行われている。このよう
に、窒化物系セラミックス材料の実用化を考えた場合、
金属材料との接合が重要な技術となる。2. Description of the Related Art Nitride-based ceramic materials are generally
It is lightweight and has high hardness, is excellent in electrical insulation, and is excellent in heat resistance and corrosion resistance. By making use of these characteristics, it is used as a structural material, a material for electric parts and the like. By the way, when a nitride-based ceramic material is used as a structural material, the ceramic material is generally a brittle material, and therefore it is generally used by being joined to a metal material. On the other hand, by utilizing the high electric insulation property of the nitride-based ceramic material, even when it is used as a mounting substrate for electronic parts, it is bonded to a metal for the purpose of forming an electric circuit. There is. In this way, when considering the practical application of nitride ceramic materials,
Joining with metal materials is an important technology.
【０００３】上述したような窒化物系セラミックス部材
と金属部材との接合方法としては、従来から、MoやW 等
の高融点金属を用いる方法や、IVa 族元素や Va 族元素
のような活性金属を用いる方法等が知られており、中で
も、高強度、高封着性、高信頼性等が得られることか
ら、活性金属法が多用されている。As a method of joining the above-mentioned nitride ceramics member and the metal member, conventionally, a method of using a refractory metal such as Mo or W or an active metal such as an IVa group element or a Va group element has been used. There are known methods of using an active metal method, and among them, the active metal method is widely used because high strength, high sealing property, high reliability and the like can be obtained.
【０００４】上記活性金属法は、Ti、Zr、Hf、Nb等の金
属元素が窒化物系セラミックス材料に対して濡れやす
く、反応しやすいことを利用した接合法であり、具体的
には活性金属を添加したろう材を用いたろう付け法や、
窒化物系セラミックス部材と金属部材との間に活性金属
の箔や粉体を介在させ、加熱接合する方法（固相拡散接
合）等として利用されている。また、被接合体となる金
属部材として、活性金属を直接使用することも行われて
いる。一般的に、取扱い性や処理のしやすさ等から、Cu
とAgとの共晶ろう材（Ag:72wt%）にTi等の活性金属を添
加し、これをセラミックス部材と金属部材との間に介在
させ、適当な温度で熱処理して接合する方法が多用され
ている。The above-mentioned active metal method is a bonding method utilizing the fact that metal elements such as Ti, Zr, Hf, and Nb easily wet and react with the nitride ceramic material. Brazing method using a brazing filler metal containing
It is used as a method (solid phase diffusion bonding) of heat-bonding by interposing an active metal foil or powder between a nitride ceramics member and a metal member. In addition, an active metal is also used directly as a metal member to be bonded. In general, due to the ease of handling and processing, Cu
An active metal such as Ti is added to a eutectic brazing filler metal (Ag: 72 wt%) of Ag and Ag, and this is interposed between the ceramic member and the metal member, and heat treatment is performed at an appropriate temperature to join them. Has been done.
【０００５】[0005]
【発明が解決しようとする課題】ところで、窒化物系セ
ラミックス部材と金属部材との接合部品には、高接合強
度が求められる一方、セラミックス材料の熱膨張率は金
属材料のそれに比べて小さいため、この熱膨張差に起因
する欠点の発生を抑制することが強く求められている。
すなわち、熱膨張率が大きく異なるセラミックス材料と
金属材料とを接合すると、接合後の冷却過程で熱膨張差
に起因する残留応力が生じ、外部応力との相乗によって
接合強度が大幅に低下したり、また接合後の冷却過程や
冷熱サイクルの付加によって応力の最大点からクラック
が発生したり、さらにはセラミックス材料が破壊される
等の問題を招いてしまう。By the way, while high joining strength is required for the joining parts of the nitride ceramics member and the metal member, the coefficient of thermal expansion of the ceramic material is smaller than that of the metal material, There is a strong demand for suppressing the occurrence of defects due to this difference in thermal expansion.
That is, when a ceramic material and a metal material having greatly different coefficients of thermal expansion are joined, residual stress caused by the difference in thermal expansion occurs in the cooling process after joining, and the joint strength is significantly reduced due to synergism with external stress, Further, due to the cooling process after joining and the addition of a cooling / heating cycle, cracks may occur from the maximum stress point, and further, the ceramic material may be broken.
【０００６】このような点に対して、上述した従来の活
性金属ろう材を用いた接合方法では、比較的接合強度が
高い接合体は得られるものの、冷熱サイクル等の付加に
対して十分な信頼性を有する接合体を再現性よく得るま
でには至っていないのが現状である。例えば、窒化物系
セラミックス部材上に銅板等を活性金属ろう材を用いて
接合したものを、半導体素子等の搭載用基板として用い
ているが、近年の半導体素子の高集積化や大電力化によ
って、半導体素子からの放熱量は飛躍的に増大してお
り、搭載基板側への熱伝達量が増加していることから、
冷熱サイクル等に対する信頼性の向上が強く望まれてい
る。On the other hand, in the above-mentioned conventional joining method using an active metal brazing material, a joined body having a relatively high joining strength can be obtained, but it is sufficiently reliable against the addition of a cooling / heating cycle or the like. At present, it has not been possible to obtain a bonded body with good reproducibility. For example, a product obtained by joining a copper plate or the like onto a nitride-based ceramic member by using an active metal brazing material is used as a mounting substrate for semiconductor elements or the like. , The amount of heat radiated from the semiconductor element has increased dramatically, and since the amount of heat transfer to the mounting board side has increased,
There is a strong demand for improvement in reliability with respect to cooling and heating cycles.
【０００７】本発明は、このような課題を解決するため
になされたもので、高接合強度を満足すると共に、冷熱
サイクル等の付加に対して高い信頼性が得られるセラミ
ックス−金属接合体を提供することを目的としている。The present invention has been made to solve the above problems, and provides a ceramic-metal bonded body which satisfies a high bonding strength and is highly reliable against the addition of a heat cycle or the like. The purpose is to do.
【０００８】[0008]
【課題を解決するための手段と作用】本発明のセラミッ
クス−金属接合体は、窒化物系セラミック部材と、Ti、
Zr、HfおよびNbから選ばれた少なくとも 1種の活性金属
を含む Ag-Cu系ろう材層を介して、前記窒化物系セラミ
ックス部材に接合された金属部材とを具備するセラミッ
クス−金属接合体において、前記窒化物系セラミック部
材側の接合界面には、前記活性金属を含む化合物の直径
100nm以下の球状粒子が層状に存在することを特徴とし
ている。Means and Actions for Solving the Problems A ceramic-metal bonded body of the present invention comprises a nitride ceramic member, Ti,
A ceramic-metal bonded body comprising a metal member bonded to the nitride ceramic member through an Ag-Cu brazing material layer containing at least one active metal selected from Zr, Hf and Nb. , The diameter of the compound containing the active metal at the bonding interface on the nitride ceramic member side.
It is characterized in that spherical particles having a size of 100 nm or less are present in layers.
【０００９】本発明に用いられる窒化物系セラミックス
部材としては、窒化アルミニウム、窒化ケイ素、サイア
ロン等が例示される。また、窒化物系セラミックス部材
自体の材料特性は、特に限定されるものではないが、特
に破壊靭性値ＫICが4.5MPa・m1/2 以上のものを用いる
ことが好ましい。本発明のセラミックス−金属接合体
は、ろう材層自体の構成によって、耐冷熱サイクル特性
や接合強度の向上を図ったものであるが、さらに破壊靭
性値ＫICが4.5MPa・m 1/2 以上の窒化物系セラミックス
部材を用いることにより、より一層耐冷熱サイクル特性
の向上を図ることができる。すなわち、窒化物系セラミ
ックス部材の破壊靭性値ＫICが4.5MPa・m1/2 以上であ
ると、冷熱サイクル等が接合体に付加された際に、窒化
物系セラミックス部材にクラックが生じることが抑制さ
れる。Examples of the nitride ceramic member used in the present invention include aluminum nitride, silicon nitride and sialon. The material properties of the nitride-based ceramic member itself are not particularly limited, but it is particularly preferable to use one having a fracture toughness value K IC of 4.5 MPa · m 1/2 or more. The ceramic-metal bonded body of the present invention is intended to improve the thermal cycle resistance and the bonding strength by the constitution of the brazing material layer itself, but the fracture toughness value K IC is more than 4.5 MPa · m 1/2. By using the above-mentioned nitride-based ceramic member, it is possible to further improve the cold-heat cycle resistance. That is, if the fracture toughness value K IC of the nitride-based ceramics member is 4.5 MPa · m 1/2 or more, cracks may occur in the nitride-based ceramics member when a thermal cycle or the like is applied to the bonded body. Suppressed.
【００１０】また、金属部材は、用途に応じて各種の金
属材料から適宜選択すればよく、例えば構造材料として
は、鋼材、耐熱合金、超硬合金等が例示され、また電子
部品材料としては、Cu、Cu合金、Ni、Ni合金、W 、Mo等
が例示される。Further, the metal member may be appropriately selected from various metal materials according to the application, and examples of the structural material include steel materials, heat-resistant alloys, cemented carbides, and the like, and electronic component materials include Examples include Cu, Cu alloys, Ni, Ni alloys, W 2 and Mo.
【００１１】本発明のセラミックス−金属接合体は、上
述したような窒化物系セラミックス部材と金属部材と
を、 Ag-Cuの共晶組成（72wt%Ag-28wt%Cu)もしくはその
近傍の組成を主とし、これにTi、Zr、HfおよびNbから選
ばれた少なくとも 1種の活性金属を適量配合した Ag-Cu
系ろう材により接合したものである。そして、本発明の
セラミックス−金属接合体においては、窒化物系セラミ
ックス部材側の接合界面に、上記ろう材中の活性金属と
窒化物系セラミックス部材との反応生成物である化合物
粒子を層状に存在させていると共に、この化合物粒子の
形状を直径 100nm以下の球状にコントロールしている。
上記化合物は、主に活性金属の窒化物からなるものであ
る。In the ceramic-metal bonded body of the present invention, the above-described nitride ceramic member and the metal member have the eutectic composition of Ag-Cu (72 wt% Ag-28 wt% Cu) or a composition in the vicinity thereof. Mainly, Ag-Cu containing an appropriate amount of at least one active metal selected from Ti, Zr, Hf and Nb
It is joined with a brazing filler metal. In the ceramic-metal bonded body of the present invention, compound particles, which are reaction products of the active metal in the brazing material and the nitride-based ceramic member, are layered at the bonding interface on the nitride-based ceramic member side. At the same time, the shape of the compound particles is controlled to be spherical with a diameter of 100 nm or less.
The above compounds are mainly composed of active metal nitrides.
【００１２】上記活性金属の化合物粒子層は、上述した
ように、窒化物系セラミックス部材との反応によるもの
であり、このような反応物を窒化物系セラミックス部材
側の接合界面に連続して層状に形成することにより、安
定して高接合強度が得られる。そして、さらに化合物粒
子の形状を直径 100nm以下の球状とすることにより、こ
の活性金属の化合物粒子層が応力緩和層として有効に機
能するため、冷熱サイクルの付加等によって窒化物系セ
ラミックス部材にクラックが生じることを抑制すること
ができる。すなわち、直径 100nm以下の微粒子状の活性
金属を含む化合物は応力緩和効果が大きく、熱応力によ
る窒化物系セラミックス部材のクラック発生を有効に阻
止する。例えば、活性金属を含む化合物粒子が直径 100
nmを超えるような粗大粒子や異形粒子となると、応力緩
和効果が低下して、耐冷熱サイクル特性の十分な向上を
図ることができなくなる。As described above, the active metal compound particle layer is formed by the reaction with the nitride-based ceramic member, and such a reaction product is continuously layered at the bonding interface on the nitride-based ceramic member side. By forming it, stable high bonding strength can be obtained. Further, by further making the shape of the compound particles spherical with a diameter of 100 nm or less, the compound particle layer of the active metal effectively functions as a stress relaxation layer. This can be suppressed. That is, a compound containing a particulate active metal having a diameter of 100 nm or less has a large stress relaxation effect, and effectively prevents cracking of the nitride-based ceramic member due to thermal stress. For example, a compound particle containing an active metal has a diameter of 100
If coarse particles or irregular-shaped particles exceeding nm are used, the stress relaxation effect decreases, and it becomes impossible to sufficiently improve the cold-heat cycle resistance.
【００１３】なお、 TiNのような活性金属の窒化物自体
は脆性材料であり、あまり層厚が厚くなると逆にクラッ
クの起点となる恐れがあるため、活性金属の化合物粒子
層の厚さは 3μm 以下とすることが好ましい。また、層
厚があまり薄いと一様に形成することが困難となるた
め、 1μm 以上とすることが好ましい。The active metal nitride itself such as TiN is a brittle material, and if the layer thickness is too thick, it may start cracking. Therefore, the active metal compound particle layer has a thickness of 3 μm. The following is preferable. Further, if the layer thickness is too thin, it becomes difficult to form the layer uniformly, so the thickness is preferably 1 μm or more.
【００１４】本発明に用いられる Ag-Cu系ろう材は、前
述したように、 Ag-Cuの共晶組成もしくはその近傍の組
成を主とし、これにTi、Zr、HfおよびNbから選ばれた少
なくとも 1種の活性金属を適量配合したものである。上
記活性金属は、熱処理温度（接合温度）で活性化し、窒
化物系セラミックス部材と反応して窒化物となり、接合
強度や耐冷熱サイクル特性の向上に寄与するものであ
る。ただし、あまり多量に添加すると、接合強度は増大
するものの、冷熱サイクルが付加された際にクラックの
発生原因となる恐れがあるため、10重量％未満とするこ
とが好ましい。一方、活性金属の配合量があまり少ない
と、十分な接合強度が得られないため、 1重量％以上と
することが好ましい。また、ろう材の主体となる Ag-Cu
合金は、基本的には共晶組成を満足するものとするが、
全ろう材成分中のCu量が15重量％〜35重量％程度であれ
ば同様な効果を得ることができる。As described above, the Ag-Cu brazing material used in the present invention is mainly composed of a eutectic composition of Ag-Cu or a composition in the vicinity thereof, and is selected from Ti, Zr, Hf and Nb. It contains a proper amount of at least one active metal. The active metal is activated at the heat treatment temperature (bonding temperature) and reacts with the nitride-based ceramic member to form a nitride, which contributes to improvement in bonding strength and cold / heat cycle resistance. However, if added in an excessively large amount, the bonding strength will increase, but it may cause cracks when a cooling / heating cycle is applied, so the content is preferably less than 10% by weight. On the other hand, if the amount of the active metal compounded is too small, sufficient bonding strength cannot be obtained, so the content is preferably 1% by weight or more. In addition, Ag-Cu, which is the main brazing material,
The alloy basically satisfies the eutectic composition,
Similar effects can be obtained if the Cu content in all brazing filler metal components is about 15% by weight to 35% by weight.
【００１５】本発明のセラミックス−金属接合体は、例
えば以下のようにして製造される。まず、窒化物系セラ
ミックス部材と金属部材とを用意し、上述したような活
性金属を含む Ag-Cu系ろう材をペースト化したものを窒
化物系セラミックス部材側に塗布する。ここで、本発明
で規定するように、活性金属を含む化合物の粒子層を窒
化物系セラミックス部材側の接合界面に形成するには、
ろう材ペーストを窒化物系セラミックス部材側に塗布す
ることが重要である。ろう材ペーストを金属部材側に塗
布したのでは、塗布したペースト層の表面に、接合工程
までの間に微量な酸素が付着し、この酸素が活性金属が
窒化物系セラミックス部材側に移行することを妨げる。
よって、窒化物系セラミックス部材側に化合物粒子層を
一様に形成することが困難となる。The ceramic-metal bonded body of the present invention is manufactured, for example, as follows. First, a nitride ceramics member and a metal member are prepared, and a paste of the above-described Ag—Cu brazing material containing an active metal is applied to the nitride ceramics member side. Here, as defined in the present invention, in order to form a particle layer of a compound containing an active metal at the bonding interface on the nitride ceramics member side,
It is important to apply the brazing paste to the nitride ceramics member side. When the brazing paste is applied to the metal member side, a small amount of oxygen adheres to the surface of the applied paste layer until the bonding process, and this oxygen causes the active metal to migrate to the nitride ceramic member side. Interfere with.
Therefore, it becomes difficult to uniformly form the compound particle layer on the nitride ceramics member side.
【００１６】なお、上述した Ag-Cu系ろう材の使用形態
としては、Ag、Cuおよび活性金属を含むペーストとして
使用することが好ましいが、必ずしも箔の積層体のよう
な状態で使用することを除外するものではない。The Ag-Cu brazing material described above is preferably used as a paste containing Ag, Cu and an active metal, but is not necessarily used in the form of a foil laminate. It does not exclude.
【００１７】次に、ろう材ペーストを塗布した窒化物系
セラミックス部材と金属部材とを積層し、真空中または
アルゴン雰囲気のような不活性雰囲気中にて、 Ag-Cu共
晶が形成される温度で熱処理し、この共晶液相および活
性金属とセラミックス部材との反応等を利用して、窒化
物系セラミックス部材と金属部材とを接合する。Next, the nitride ceramics member coated with the brazing paste and the metal member are laminated, and the temperature at which an Ag-Cu eutectic crystal is formed in a vacuum or an inert atmosphere such as an argon atmosphere. Then, the nitride ceramics member and the metal member are joined together by utilizing the reaction between the eutectic liquid phase and the active metal and the ceramics member.
【００１８】この際、一般的には接合温度は 800℃〜 9
50℃程度で、接合時間（加熱時間）は 1分〜20分程度で
あるが、活性金属と窒化物系セラミックス部材との反応
物である化合物粒子を、窒化物系セラミックス部材側の
接合界面に層状に存在させると共に、化合物粒子の形状
を直径 100nm以下の微粒子状を維持させるためには、87
0℃〜 920℃程度の比較的高温側で、 1分〜 3分程度の
短時間で処理することが好ましい。このように、高温で
の短時間処理によってろう付けを行うことにより、活性
金属を含む化合物粒子の粒成長を抑制することができ、
微粒子状態を維持することが可能となる。さらに、活性
金属を含む化合物粒子を微粒子状態で層状に存在させる
ための条件としては、真空度を上げたり、アルゴン雰囲
気中の酸素や窒素の濃度を低下させることが必要であ
る。At this time, generally, the joining temperature is 800 ° C to 9 ° C.
The bonding time (heating time) is about 1 to 20 minutes at about 50 ° C, but the compound particles, which are the reaction product of the active metal and the nitride-based ceramics member, do not adhere to the bonding interface on the nitride-based ceramics member side. In order to maintain the compound particles in the form of layers and maintaining the shape of the compound particles as fine particles with a diameter of 100 nm or less, 87
It is preferable to perform the treatment at a relatively high temperature side of about 0 ° C to 920 ° C in a short time of about 1 minute to 3 minutes. Thus, by performing brazing by high-temperature short-time treatment, it is possible to suppress the grain growth of compound particles containing an active metal,
It becomes possible to maintain a fine particle state. Furthermore, as conditions for allowing the compound particles containing an active metal to exist in a layered state in the form of fine particles, it is necessary to increase the degree of vacuum and reduce the concentrations of oxygen and nitrogen in the argon atmosphere.
【００１９】[0019]
【実施例】次に、本発明の実施例について説明する。EXAMPLES Next, examples of the present invention will be described.
【００２０】実施例１ まず、窒化物系セラミックス部材として厚さ0.8mmtの板
状の窒化アルミニウム焼結体、および金属部材として厚
さ0.3mmtの銅板（無酸素銅）を用意した。一方、重量比
でAg:Cu:Ti=70.6:27.4:2.0のろう材を用意し、このろう
材に樹脂バインダおよび分散媒を適量加え、十分に混合
して接合用ペーストを作製した。Example 1 First, a 0.8 mm-thick plate-shaped aluminum nitride sintered body was prepared as a nitride ceramics member, and a 0.3 mm-thick copper plate (oxygen-free copper) was prepared as a metal member. On the other hand, a brazing material having a weight ratio of Ag: Cu: Ti = 70.6: 27.4: 2.0 was prepared, a resin binder and a dispersion medium were added to the brazing material in appropriate amounts, and they were sufficiently mixed to prepare a bonding paste.
【００２１】次に、窒化アルミニウム焼結体の一方の主
面に、上記した接合用ペーストをスクリーン印刷し、乾
燥させた後、接合用ペーストの塗布層上に銅板を積層、
配置した。この後、上記積層物に対して真空中にて、 9
00℃× 2分（昇温速度：20℃／分、降温：炉冷）の温度
プロファイルで熱処理を施し、窒化アルミニウム焼結体
と銅板とをろう材層を介して接合し、目的とするセラミ
ックス−金属接合体を得た。Next, the above-mentioned bonding paste is screen-printed on one main surface of the aluminum nitride sintered body and dried, and then a copper plate is laminated on the coating layer of the bonding paste.
I placed it. After that, the above laminate is placed in a vacuum and
Heat treatment is performed with a temperature profile of 00 ° C x 2 minutes (temperature increase rate: 20 ° C / minute, temperature decrease: furnace cooling), the aluminum nitride sintered body and the copper plate are joined together via a brazing material layer, and the target ceramic -A metal joint was obtained.
【００２２】比較例１ 上記実施例１において、接合用ペーストを銅板側に塗布
する以外は、同一条件でセラミックス−金属接合体を作
製した。Comparative Example 1 A ceramic-metal bonded body was prepared under the same conditions as in Example 1 except that the bonding paste was applied to the copper plate side.
【００２３】比較例２ 上記実施例１において、熱処理条件を窒素雰囲気中、 9
00℃× 2分（昇温速度：20℃／分、降温：炉冷）と変更
する以外は、実施例１と同様にしてセラミックス−金属
接合体を作製した。Comparative Example 2 In the above-mentioned Example 1, the heat treatment conditions were as follows:
A ceramic-metal bonded body was produced in the same manner as in Example 1 except that the temperature was changed to 00 ° C. × 2 minutes (temperature rising rate: 20 ° C./minute, temperature decrease: furnace cooling).
【００２４】上記実施例１および比較例１、２で作製し
た各セラミックス−金属接合体（窒化アルミニウム−
銅）の接合部を透過型電子顕微鏡（ＴＥＭ）によって観
察した。図１に、実施例１によるセラミックス−金属接
合体の接合部のＴＥＭ写真を模式的に示す。図１から明
らかなように、実施例１によるセラミックス−金属接合
体では、窒化アルミニウム側の接合界面に TiN粒子が層
状に存在していることを確認した。この TiN粒子層の厚
さは約 1μm で、また TiN粒子は直径 100nm以下の球状
微粒子であった。一方、比較例１によるセラミックス−
金属接合体では、窒化アルミニウム側の接合界面に TiN
層が形成されていたが、この TiN層はとぎれている部分
が存在し、またその厚さは約 3μm であった。また、比
較例２によるセラミックス−金属接合体では、窒化アル
ミニウム側の接合界面に TiN層が形成されていたが、 T
iN粒子は直径 100nmを超える粗大粒子であった。Each ceramic-metal bonded body (aluminum nitride-made) produced in Example 1 and Comparative Examples 1 and 2 above.
The copper) joint was observed by a transmission electron microscope (TEM). FIG. 1 schematically shows a TEM photograph of the bonded portion of the ceramic-metal bonded body according to Example 1. As is clear from FIG. 1, in the ceramic-metal bonded body according to Example 1, it was confirmed that TiN particles exist in layers at the bonding interface on the aluminum nitride side. The thickness of the TiN particle layer was about 1 μm, and the TiN particles were spherical particles with a diameter of 100 nm or less. On the other hand, the ceramic according to Comparative Example 1
In the metal bonded body, TiN is formed at the bonding interface on the aluminum nitride side.
Although a layer was formed, this TiN layer had a discontinuous portion and its thickness was about 3 μm. Further, in the ceramic-metal bonded body according to Comparative Example 2, the TiN layer was formed at the bonding interface on the aluminum nitride side.
The iN particles were coarse particles with a diameter of more than 100 nm.
【００２５】次に、上記実施例１および比較例１、２で
作製した各セラミックス−金属接合体の特性を以下のよ
うにして評価した。まず、各セラミックス−金属接合体
に対して冷熱サイクル試験(TCT) を施した。 TCTは -40
℃×30分＋RT×10分＋ 125℃×30分＋RT℃×10分を 1サ
イクルとした。 TCT後の特性は、銅板のピール強度の測
定と窒化アルミニウム焼結体のファインクラックの有無
により判定した。なお、窒化アルミニウム焼結体のファ
インクラックの有無は、銅板およびろう材層をエッチン
グ除去し、蛍光浸透探傷(PT)検査を実施することにより
判定した。Next, the characteristics of each ceramic-metal bonded body produced in Example 1 and Comparative Examples 1 and 2 were evaluated as follows. First, each ceramic-metal bonded body was subjected to a thermal cycle test (TCT). TCT is -40
One cycle consists of ℃ × 30 minutes + RT × 10 minutes + 125 ° C × 30 minutes + RT ° C × 10 minutes. The properties after TCT were judged by measuring the peel strength of the copper plate and the presence or absence of fine cracks in the aluminum nitride sintered body. The presence or absence of fine cracks in the aluminum nitride sintered body was determined by removing the copper plate and the brazing material layer by etching and conducting a fluorescent penetrant inspection (PT) test.
【００２６】TCT前の接合強度は、実施例１によるセラ
ミックス−金属接合体が10kgf/mm、比較例１によるもの
が 8kgf/mm、比較例２によるものが 5kgf/mmと、比較例
によるものは接合強度が低かった。 TCT 100サイクル後
においては、実施例１によるセラミックス−金属接合体
では 9kgf/mmと強度低下がほとんどなかったのに対し、
比較例２によるものでは 3kgf/mmと強度が低下した。ま
た、この TCT 100サイクル後のファインクラックの有無
を上記した方法で判定したところ、実施例１のセラミッ
クス−金属接合体では TCT 100サイクル後においてもク
ラックは認められなかったのに対し、比較例２のセラミ
ックス−金属接合体では微細なクラックが発生してい
た。さらに、実施例１によるセラミックス−金属接合体
は、 TCT200サイクル後においてもクラックは確認され
なかった。The bonding strength before TCT is 10 kgf / mm for the ceramic-metal bonded body according to Example 1, 8 kgf / mm for Comparative Example 1 and 5 kgf / mm for Comparative Example 2, and the comparative example has The bonding strength was low. After 100 cycles of TCT, the ceramic-metal bonded body according to Example 1 showed almost no strength reduction of 9 kgf / mm, whereas
In Comparative Example 2, the strength was reduced to 3 kgf / mm. Further, when the presence or absence of fine cracks after 100 cycles of this TCT was judged by the above-mentioned method, no cracks were observed even after 100 cycles of TCT in the ceramic-metal bonded body of Example 1, whereas in Comparative Example 2 In the ceramic-metal bonded body of No. 3, fine cracks were generated. Further, in the ceramic-metal bonded body according to Example 1, no crack was confirmed even after 200 cycles of TCT.
【００２７】[0027]
【発明の効果】以上説明したように、本発明のセラミッ
クス−金属接合体によれば、窒化物系セラミックス部材
側の接合界面に、活性金属と窒化物系セラミックス部材
との反応物である化合物の球状微粒子を層状に存在させ
ており、この微細な化合物球状粒子が大きな応力緩和効
果を有しているため、安定して高接合強度が得られると
共に、冷熱サイクルの付加等によって窒化物系セラミッ
クス部材にクラックが生じることを抑制することができ
る。よって、高接合強度を有すると共に、冷熱サイクル
に対して優れた信頼性を示すセラミックス−金属接合体
を、再現性よく提供することが可能となる。As described above, according to the ceramic-metal bonded body of the present invention, the compound which is the reaction product of the active metal and the nitride-based ceramic member is formed at the bonding interface on the nitride-based ceramic member side. Since the spherical fine particles are present in a layered state and the fine compound spherical particles have a large stress relaxation effect, a stable high bonding strength can be obtained, and a nitride-based ceramic member can be obtained by adding a heat cycle. It is possible to suppress the occurrence of cracks in the. Therefore, it becomes possible to provide a ceramic-metal bonded body having high bonding strength and excellent reliability with respect to a thermal cycle with good reproducibility.
【図１】本発明の一実施例によるセラミックス−金属接
合体の接合部のＴＥＭ写真を模式的に示す図である。FIG. 1 is a diagram schematically showing a TEM photograph of a bonded portion of a ceramics-metal bonded body according to an example of the present invention.
Claims (2)
およびNbから選ばれた少なくとも 1種の活性金属を含む
Ag-Cu系ろう材層を介して、前記窒化物系セラミックス
部材に接合された金属部材とを具備するセラミックス−
金属接合体において、 前記窒化物系セラミック部材側の接合界面には、前記活
性金属を含む化合物の直径 100nm以下の球状粒子が層状
に存在することを特徴とするセラミックス−金属接合
体。1. A nitride ceramic member and Ti, Zr, Hf
And at least one active metal selected from Nb
Ceramics comprising a metal member bonded to the nitride ceramics member via an Ag-Cu brazing material layer-
In the metal-bonded body, spherical particles having a diameter of 100 nm or less of the compound containing the active metal are layered at the bonding interface on the side of the nitride-based ceramic member, in a layered structure.
体において、 前記活性金属を含む化合物は、主に前記活性金属の窒化
物からなることを特徴とするセラミックス−金属接合
体。2. The ceramic-metal bonded body according to claim 1, wherein the compound containing the active metal is mainly composed of a nitride of the active metal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17691992A JP3495051B2 (en) | 1992-07-03 | 1992-07-03 | Ceramic-metal joint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17691992A JP3495051B2 (en) | 1992-07-03 | 1992-07-03 | Ceramic-metal joint |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0624854A true JPH0624854A (en) | 1994-02-01 |
| JP3495051B2 JP3495051B2 (en) | 2004-02-09 |
Family
ID=16022061
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17691992A Expired - Lifetime JP3495051B2 (en) | 1992-07-03 | 1992-07-03 | Ceramic-metal joint |
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| Country | Link |
|---|---|
| JP (1) | JP3495051B2 (en) |
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