JP2004255416A - Joining method for carbon based copper composite material and ceramics or copper - Google Patents

Joining method for carbon based copper composite material and ceramics or copper Download PDF

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JP2004255416A
JP2004255416A JP2003049030A JP2003049030A JP2004255416A JP 2004255416 A JP2004255416 A JP 2004255416A JP 2003049030 A JP2003049030 A JP 2003049030A JP 2003049030 A JP2003049030 A JP 2003049030A JP 2004255416 A JP2004255416 A JP 2004255416A
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carbon
copper
composite material
copper composite
based copper
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JP4108505B2 (en
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Aritoshi Sugaya
有利 菅谷
Tsugio Masuda
次男 増田
Takashi Kato
崇 加藤
Hiroyuki Yamagishi
弘幸 山岸
Masami Ogura
正巳 小倉
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Honda Motor Co Ltd
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Honda Motor Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an inexpensive joining method for a carbon based copper composite material and ceramics or for a carbon based copper composite material and copper which can enhance adhesiveness. <P>SOLUTION: Materials to be joined are heated to 900 °C in the nitrogen gas atmosphere. Mg powder 12 is sublimed and turned into Mg (a gas). Then, the Mg reacts with the atmosphere N<SB>2</SB>and generates Mg<SB>3</SB>N<SB>2</SB>. The Mg<SB>3</SB>N<SB>2</SB>has the strong reduction action and exerts the action to remove an oxide film. Heating is conducted in an atmosphere of nitrogen, which is inexpensive and has no danger of explosion. Accordingly, costs for joining can be significantly reduced. <P>COPYRIGHT: (C)2004,JPO&NCIPI

Description

【０００１】
【発明の属する技術分野】
本発明は炭素基銅複合材とセラミックスとの接合方法又は炭素基銅複合材と銅との接合方法の改良に関する。
【０００２】
【従来の技術】
ある種のパワーモジュール（特にそれのヒートシンク）に、炭素部材とセラミックス又は金属を接合して一体化した構造のものが実用化されている。このときの接合、一体化が異種材料同士の場合に問題となる。
【０００３】
例えば、ボルトで一体化した場合には、ボルトから離れた部位に隙間が発生しやすく、高い密着性が得られない。
ろう付けや半田付けで一体化しようとすると、ろうや半田が炭素部材やセラミックス又は金属から剥がれやすい。すなわち、炭素部材はろう材や半田と濡れ性が悪く、接合性が悪い。また、セラミックス又は金属の表面に薄い酸化物膜が存在し、この酸化物膜がろうや半田との濡れ性が悪く、接合を阻害する。
【０００４】
以上のボルト締めやろう付け法によらぬ接合方法が各種提案されてきた。
すなわち、ろう材を使用せずにＴｉにより接合する技術が提案されている（例えば、特許文献１。）。
また、ろう材を使用せずにＴｉ及び水素ガスの使用により接合する技術が提案されている（例えば、特許文献２。）。
【０００５】
【特許文献１】
特開平９−２０８３３５号公報（請求項９）
【特許文献２】
特開昭５９−１３７３７３公報（特許請求の範囲第９項、第１１項）
【０００６】
特許文献１の請求項９に「炭素部材の表面に予めＴｉ膜を形成する工程と、次に前記Ｔｉ膜の表面にＣｕとＭｎ又はＣｕとＰを主成分とする組成物を配置する工程と、次にこれを非酸化性雰囲気中で前記組成物の融点以上に加熱する工程によって前記炭素部材の表面に金属化膜を形成することを特徴とする炭素部材の複合化方法。」との記載がある。
【０００７】
特許文献２の特許請求の範囲第９項に「接合するときの加熱雰囲気は、Ｈ２ガス中・・・以下省略」との記載がある。
また、特許文献２の特許請求の範囲第１１項に「接合するときの加熱雰囲気は、Ｎ２ガス中・・・以下省略」との記載がある。
【０００８】
【発明が解決しようとする課題】
特許文献１に記載されたＴｉは、炭素部材のＣと反応してＴｉＣになり、良好な接合性を発揮することが知られている。
しかし、本発明者らの研究では、Ｔｉの表面に薄い酸化物膜が存在する。この酸化物膜はＣとＴｉとの接触を妨害する。その為に、Ｃ＋Ｔｉの反応が不活発になり、接合不良を引き起こすことが分かった。
【０００９】
この点、特許文献２に記載のＨ２ガスは還元性に富み、酸化物膜を破壊して、Ｃ＋Ｔｉの反応を促す作用をなす。
しかし、Ｈ２ガスは高価であり、また、爆発しやすいガスであるため、その管理コストが嵩む。
【００１０】
また、本発明者らの研究では特許文献２に記載のＮ２ガスはＴｉと反応してＴｉＮを生成し、このＴｉＮがＣとＴｉとの接触を妨害し、接合不良を引き起こすことが分かった。
【００１１】
そこで、本発明の目的は低コストで且つ接着性を高めることのできる炭素基銅複合材とセラミックスとの接合方法又は炭素基銅複合材と銅との接合方法を提供することにある。
【００１２】
【課題を解決するための手段】
上記目的を達成するために請求項１は、炭素基銅複合材とセラミックスとの接合方法又は炭素基銅複合材と銅との接合方法において、炭素基銅複合材とセラミックスとの間又は炭素基銅複合材と銅との間に、Ｔｉ並びにＭｇを含む接合材を介在させ、この多層体を窒素ガス雰囲気下で前記接合材の融点以上の温度に加熱し、生成したＭｇ３Ｎ２で炭素基銅複合材の銅表面やセラミックス又は銅表面の酸化物膜を還元し、Ｔｉと炭素との結合を促して炭素基銅複合材とセラミックス又は銅を接合することを特徴とする。
【００１３】
接合材にＴｉのみならずＭｇを加えたことを特徴とする。Ｍｇ（固体）は加熱すると昇華してＭｇ（ガス）になり、雰囲気の窒素と結合してＭｇ３Ｎ２になる。このＭｇ３Ｎ２は、標準生成エネルギーの観点からＴｉＮより安定する。この結果、ＴｉＮの生成を抑えることができる。
【００１４】
加えて、Ｍｇ３Ｎ２は強い還元作用を発揮し、炭素基銅複合材の銅表面やセラミックス又は銅表面の酸化物膜を還元し、除去する。酸化物膜が除去されて濡れ性の増したセラミックス又は銅に、ＴｉＮ化しないＴｉが良好に浸透し、ＴｉＣなどが生成できるため、接着性を格段に高めることができる。
【００１５】
加熱雰囲気は、窒素であり、窒素は安価であり、爆発の危険もない。従って、本発明によれば、接合に要するコストを大幅に下げることができる。
【００１６】
請求項２では、接合材は、Ｔｉを含む銅合金箔と、この箔の両面に配置したＭｇ又はＭｇ合金と、からなることを特徴とする。
Ｔｉを含む銅合金箔は、入手容易であり且つ粉末に比較して取扱いが容易である。従って、請求項２によれば、接合に要するコストを更に下げることができる。
【００１７】
請求項３では、融点以上の温度は、８８５℃〜１０８３℃であることを特徴とする。
Ｃｕ組成が８０％を超えるＴｉ系銅合金の融点は８８５℃であるので、加熱温度が８８５℃未満では接合材の溶融が不十分となり接着不良が起こる。また、加熱温度が１０８３℃を超えると、炭素基銅複合材から銅が流れ出し、製品品質が低下する。
接着不良を回避すると共に製品品質を良好に保つために、加熱温度は８８５℃〜１０８３℃の範囲に留める。
【００１８】
【発明の実施の形態】
本発明の実施の形態を添付図に基づいて以下に説明する。
図１（ａ）〜（ｄ）は本発明での材料準備からるつぼ充填までの作用説明図（第１実施例）である。
（ａ）において、セラミックスとしてのＳｉ３Ｎ４板１１と、接合材を構成するためのＭｇ粉末１２と、接合材を構成するためのＣｕＴｉ合金箔１３と、炭素基銅複合材１４とからなる出発材料を準備する。炭素基銅複合材１４は、図面ではＣ／Ｃｕと表記する。
【００１９】
ＣｕＴｉ合金箔１３は、例えば８０μｍの板を用いる。ＣｕＴｉ合金箔１３は厚すぎると熱伝導が悪くなり、ヒートシンク等の接合としては好ましくない。従って、厚さは製造が可能であれば、より薄くすることが望ましい。
ＣｕＴｉ合金箔１３は、例えばＴｉが３質量％で残りがＣｕの合金を用いる。
【００２０】
（ｂ）において、るつぼ１５に、先ずＳｉ３Ｎ４板１１を置き、このＳｉ３Ｎ４板１１に１０ｍｇ／ｃｍ２の割合でＭｇ粉末１２を載せる。１０ｍｇ／ｃｍ２は、５〜２０ｍｇ／ｃｍ２の範囲から選択することができる。５ｍｇ／ｃｍ２未満では還元作用が弱くなり、２０ｍｇ／ｃｍ２を超えるとＭｇの溶融が多くなりすぎる。
【００２１】
（ｃ）において、ＣｕＴｉ合金箔１３を載せ、このＣｕＴｉ合金箔１３に１０ｍｇ／ｃｍ２の割合でＭｇ粉末１２を載せる。
【００２２】
（ｄ）において、炭素基銅複合材１４を載せる。これで、るつぼ１５への充填が完了する。さらには、炭素基銅複合材１４に別のセラミックス製ウエイト（図示せず。）を載せ、１ｋｇ／ｃｍ２程度の押し圧を付与することが望ましい。接合をより確実にすることができるからである。
【００２３】
図２は本発明での加熱要領図（第１実施例）であり、加熱手段２１や窒素ガス吹込み手段２２やガス抜き手段２３を備えた加熱炉２０に、るつぼ１５を装入する。そして、炉内の空気を窒素ガスに置換して、窒素ガス雰囲気にする。次に、加熱手段２１にて炉内を９００℃まで加熱し、９００℃に保持する。
【００２４】
９００℃は、８８５〜１０８３℃の範囲で変更することが可能である。Ｃｕ組成が８０％を超えるＴｉ系銅合金の融点は８８５℃であるので、加熱温度が８８５℃未満では接合材の溶融が不十分となり接着不良が起こる。また、加熱温度が１０８３℃を超えると、炭素基銅複合材から銅が流れ出し、製品品質が低下する。
上記加熱により加熱炉２０内及びるつぼ１５内で次の反応が起こる。
【００２５】
【化１】

Figure 2004255416
【００２６】
▲１▼式に示すとおりに、Ｍｇ粉末１２が、昇華してＭｇ（ガス）となる。すると、▲２▼式に示すとおりに、Ｍｇが雰囲気のＮ２と反応してＭｇ３Ｎ２が生成する。このＭｇ３Ｎ２は強い還元作用を発揮する。
【００２７】
ＣｕＴｉ合金箔１３に含まれるＴｉが雰囲気のＮ２と反応するか否かを検討する。前記Ｍｇ３Ｎ２は、標準生成エネルギーの観点からＴｉＮより安定する。不安定なＴｉＮは仮に生成したとしてもその形で存在することはない。そのため安定したＭｇ３Ｎ２が主として生成し、不安定なＴｉＮは実質的に生成しない。Ｔｉの形で存在すれば、Ｔｉは濡れ性促進剤としての役割を果たす。
【００２８】
ところで、図１（ａ）において、セラミックスとしてのＳｉ３Ｎ４板１１には表面に酸化物膜としてのＳｉＯ２が存在する。
ＣｕＴｉ合金箔１３には、表面に酸化物膜としてのＴｉＯ２及び／又はＣｕＯ（酸化第２銅）が存在する。
炭素基銅複合材１４の銅表面には、ＣｕＯ（酸化第２銅）が存在すると、考えられる。
【００２９】
以上の酸化物膜ＳｉＯ２、ＴｉＯ２、ＣｕＯは次の反応（Ｍｇ３Ｎ２による還元反応）により、Ｓｉ、Ｔｉ、Ｃｕに変化し、実質的に酸化物膜が除去される。
【００３０】
【化２】
Figure 2004255416
【００３１】
すなわち、▲３▼式により酸化物膜ＳｉＯ２が除去され、▲４▼式により酸化物膜ＴｉＯ２が除去され、▲５▼式により酸化物膜ＣｕＯが除去される。これで、Ｓｉ３Ｎ４板１１及び炭素基銅複合材１４は溶融金属（溶融接合材）との濡れ性が高まる。
【００３２】
９００℃の加熱により、溶融金属（溶融接合材）はＳｉ３Ｎ４板１１及び炭素基銅複合材１４に浸透し、良好な接着が行える。特に接着が困難な炭素基銅複合材１４においては、ＴｉＣの生成により結合力を高めることができる。
【００３３】
図３は本発明方法で製造した接合体の断面図（第１実施例）であり、接合体２５は、Ｓｉ３Ｎ４板１１と、ＣｕＴｉ合金箔１３と、炭素基銅複合材１４とからなるが、炭素基銅複合材１４はＣｕＴｉ合金箔１３を介してＳｉ３Ｎ４板１１に強固に接合できた接合物である。
【００３４】
図１において、セラミックスとしてのＳｉ３Ｎ４板１１は、ＳｉＮ、ＳｉＯ２や、ＡｌＮ、Ａｌ２Ｏ３やＴｉＣであってもよい。その理由は次の通りである。
Ｓｉ３Ｎ４、ＳｉＯ２での酸化物膜はＳｉＯ２であり、上記▲３▼式により還元できる。ＡｌＮ、Ａｌ２Ｏ３での酸化物膜はＡｌ２Ｏ３であり、同様にＭｇ３Ｎ２での還元が可能である。ＴｉＣでの酸化物膜はＴｉＯ２であり、上記▲４▼式により還元できる。
すなわち、セラミックスは酸化物、窒化物、炭化物、硼化物など何れでもよい。
【００３５】
以上に説明した第１実施例の別実施例を次に説明する。別実施例としての第２実施例は、前記第１実施例と重複する部分が多いが、正確を期すために詳しく説明する。
図４（ａ）〜（ｄ）は本発明での材料準備からるつぼ充填までの作用説明図（第２実施例）である。
（ａ）において、銅板２６と、接合材を構成するためのＭｇ粉末１２及びＣｕＴｉ合金箔１３と、炭素基銅複合材１４とからなる出発材料を準備する。
【００３６】
ＣｕＴｉ合金箔１３は、例えば８０μｍの板を用いる。
ＣｕＴｉ合金箔１３は、例えばＴｉ３質量％で残りがＣｕの合金を用いる。
【００３７】
（ｂ）において、るつぼ１５に、先ず銅板２６を置き、この銅板２６に１０ｍｇ／ｃｍ２の割合でＭｇ粉末１２を載せる。
（ｃ）において、ＣｕＴｉ合金箔１３を載せ、このＣｕＴｉ合金箔１３に１０ｍｇ／ｃｍ２の割合でＭｇ粉末１２を載せる。
（ｄ）において、炭素基銅複合材１４を載せる。これで、るつぼ１５への充填が完了する。
【００３８】
図５は本発明での加熱要領図（第２実施例）であり、加熱手段２１や窒素ガス吹込み手段２２やガス抜き手段２３を備えた加熱炉２０に、るつぼ１５を装入する。そして、炉内の空気を窒素ガスに置換して、窒素ガス雰囲気にする。次に、加熱手段２１にて炉内を９００℃まで加熱し、９００℃に保持する。
【００３９】
上記加熱により加熱炉２０内及びるつぼ１５内で次の反応が起こる。
【００４０】
【化３】
Figure 2004255416
【００４１】
▲６▼式に示すとおりに、Ｍｇ粉末１２が、昇華してＭｇ（ガス）となる。すると、▲７▼式に示すとおりに、Ｍｇが雰囲気のＮ２と反応してＭｇ３Ｎ２が生成する。このＭｇ３Ｎ２は強い還元作用を発揮する。
【００４２】
ところで、図４（ａ）において、銅板２６には表面に酸化物膜としてのＣｕＯが存在する。
ＣｕＴｉ合金箔１３には、表面に酸化物膜としてのＴｉＯ２及び／又はＣｕＯが存在する。
炭素基銅複合材１４の銅表面には、ＣｕＯが存在すると、考えられる。
【００４３】
以上の酸化物膜ＴｉＯ２、ＣｕＯは次の反応（Ｍｇ３Ｎ２による還元反応）により、Ｔｉ、Ｃｕに変化し、実質的に酸化物膜が除去される。
【００４４】
【化４】
Figure 2004255416
【００４５】
すなわち、▲８▼式により酸化物膜ＴｉＯ２が除去され、▲９▼式により酸化物膜ＣｕＯが除去される。これで、銅板２６及び炭素基銅複合材１４は溶融金属との濡れ性が高まる。
【００４６】
９００℃での加熱により、溶融金属（溶融接合材）はＳｉ３Ｎ４板１１及び炭素基銅複合材１４に浸透し、良好な接着が行える。特に接着が困難な炭素基銅複合材１４においては、ＴｉＣの生成により結合力を高めることができる。
【００４７】
図６は本発明方法で製造した接合体の断面図（第２実施例）であり、接合体２７は、銅板２６と、炭素基銅複合材１４とからなる。図５に示したＣｕＴｉ合金箔１３は銅板２６と一体化するために実質的に２層になった。炭素基銅複合材１４は一体化したＣｕＴｉ合金箔１３を介して銅板２６に強固に接合できた接合物である。
【００４８】
尚、実施例では、接合材としてＣｕＴｉ合金箔にＭｇ粉末を組合わせが接合材はＣｕＴｉＭｇ合金箔であってもよい。又は接合材はＣｕ粉末＋Ｔｉ粉末＋Ｍｇ粉末からなる金属粉末混合物に置換えることもできる。
ＣｕＴｉＭｇ合金箔は取扱いの点で最良である。ＣｕＴｉ合金箔にＭｇ粉末を組合わせたものは、Ｍｇ粉末が入手容易である点からコストダウンに好適である。
【００４９】
【発明の効果】
本発明は上記構成により次の効果を発揮する。
請求項１は、接合材にＴｉのみならずＭｇを加えたことを特徴とする。Ｍｇ（固体）は加熱すると昇華してＭｇ（ガス）になり、雰囲気の窒素と結合してＭｇ３Ｎ２になる。このＭｇ３Ｎ２は、標準生成エネルギーの観点からＴｉＮより安定する。この結果、ＴｉＮの生成を抑えることができる。
【００５０】
加えて、Ｍｇ３Ｎ２は強い還元作用を発揮し、炭素基銅複合材の銅表面やセラミックス又は銅表面の酸化物膜を還元し、除去する。酸化物膜が除去されて濡れ性の増したセラミックス又は銅に、ＴｉＮ化しないＴｉが良好に浸透し、ＴｉＣなどが生成できるため、接着性を格段に高めることができる。
【００５１】
加熱雰囲気は、窒素であり、窒素は安価であり、爆発の危険もない。従って、本発明によれば、接合に要するコストを大幅に下げることができる。
従って、請求項１によれば、低コストで且つ接着性を高めることのできる炭素基銅複合材とセラミックスとの接合方法又は炭素基銅複合材と銅との接合方法を提供することができる。
【００５２】
請求項２では、接合材は、Ｔｉを含む銅合金箔と、この箔の両面に配置したＭｇ又はＭｇ合金と、からなることを特徴とする。Ｔｉを含む銅合金箔は、入手容易であり且つ粉末に比較して取扱いが容易である。従って、請求項２によれば、接合に要するコストを更に下げることができる。
【００５３】
請求項３では、融点以上の温度は、８８５℃〜１０８３℃であることを特徴とする。加熱温度が８８５℃未満では接合材の溶融が不十分となり接着不良が起こる。また、加熱温度が１０８３℃を超えると、炭素基銅複合材から銅が流れ出し、製品品質が低下する。
接着不良を回避すると共に製品品質を良好に保つために、加熱温度は８８５℃〜１０８３℃の範囲に留める。
【図面の簡単な説明】
【図１】本発明での材料準備からるつぼ充填までの作用説明図（第１実施例）
【図２】本発明での加熱要領図（第１実施例）
【図３】本発明方法で製造した接合体の断面図（第１実施例）
【図４】本発明での材料準備からるつぼ充填までの作用説明図（第２実施例）
【図５】本発明での加熱要領図（第２実施例）
【図６】本発明方法で製造した接合体の断面図（第２実施例）
【符号の説明】
１１…セラミックスとしてのＳｉ３Ｎ４板、１２…接合材を構成するためのＭｇ粉末、１３…接合材を構成するためのＣｕＴｉ合金箔、１４…炭素基銅複合材、２０…加熱炉、２１…加熱手段、２２…窒素ガス吹込み手段、２５、２７…接合体、２６…銅板。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an improvement in a method for joining a carbon-based copper composite and ceramics or a method for joining a carbon-based copper composite and copper.
[0002]
[Prior art]
2. Description of the Related Art A power module (particularly, a heat sink thereof) having a structure in which a carbon member and a ceramic or metal are joined and integrated has been put to practical use. At this time, the joining and the integration become problematic when different materials are used.
[0003]
For example, when integrated with a bolt, a gap is likely to be generated in a portion away from the bolt, and high adhesion cannot be obtained.
When trying to integrate by brazing or soldering, the brazing or solder is easily peeled off from the carbon member, ceramics or metal. That is, the carbon member has poor wettability with brazing material and solder, and poor bondability. In addition, a thin oxide film exists on the surface of ceramics or metal, and this oxide film has poor wettability with solder or solder, and inhibits bonding.
[0004]
Various joining methods that do not rely on the bolting or brazing methods described above have been proposed.
That is, a technique of joining with Ti without using a brazing material has been proposed (for example, Patent Document 1).
Further, a technique of joining by using Ti and hydrogen gas without using a brazing material has been proposed (for example, Patent Document 2).
[0005]
[Patent Document 1]
JP-A-9-208335 (Claim 9)
[Patent Document 2]
JP-A-59-137373 (Claims 9 and 11)
[0006]
Claim 9 of Patent Document 1 states that “a step of forming a Ti film in advance on the surface of a carbon member, and a step of disposing a composition mainly composed of Cu and Mn or Cu and P on the surface of the Ti film. And a step of heating the composition in a non-oxidizing atmosphere to a temperature equal to or higher than the melting point of the composition to form a metallized film on the surface of the carbon member. " There is.
[0007]
In claim 9 of Patent Document 2, there is a description that “the heating atmosphere at the time of joining is in H 2 gas...
Further, in claim 11 of Patent Document 2, there is a description that “the heating atmosphere for bonding is in N 2 gas...
[0008]
[Problems to be solved by the invention]
It is known that Ti described in Patent Literature 1 reacts with C of a carbon member to become TiC and exhibits good bonding properties.
However, in the study of the present inventors, a thin oxide film exists on the surface of Ti. This oxide film hinders the contact between C and Ti. For this reason, it was found that the reaction of C + Ti became inactive, causing poor bonding.
[0009]
In this regard, the H 2 gas described in Patent Document 2 is rich in reducing properties and has an effect of destroying an oxide film and promoting the reaction of C + Ti.
However, H 2 gas is expensive, also because it is an Explosive Gas, increase its management costs.
[0010]
In addition, in the study of the present inventors, it has been found that the N 2 gas described in Patent Document 2 reacts with Ti to generate TiN, and this TiN interferes with the contact between C and Ti to cause a bonding failure. .
[0011]
Therefore, an object of the present invention is to provide a method of joining a carbon-based copper composite material and ceramics or a method of joining a carbon-based copper composite material and copper at a low cost and capable of improving the adhesiveness.
[0012]
[Means for Solving the Problems]
In order to achieve the above object, a first aspect of the present invention relates to a method of joining a carbon-based copper composite and ceramics or a method of joining a carbon-based copper composite and copper, wherein the method comprises the steps of: A bonding material containing Ti and Mg is interposed between the copper composite material and the copper, and the multilayer body is heated to a temperature equal to or higher than the melting point of the bonding material in a nitrogen gas atmosphere, and carbon is generated using the generated Mg 3 N 2 . The method is characterized in that an oxide film on a copper surface or a ceramic or copper surface of the base copper composite material is reduced, and a bond between Ti and carbon is promoted to join the carbon-based copper composite material and ceramics or copper.
[0013]
It is characterized by adding Mg as well as Ti to the joining material. When heated, Mg (solid) sublimates into Mg (gas) and combines with nitrogen in the atmosphere to form Mg 3 N 2 . This Mg 3 N 2 is more stable than TiN in terms of standard energy of formation. As a result, generation of TiN can be suppressed.
[0014]
In addition, Mg 3 N 2 exerts a strong reducing action, and reduces and removes the copper surface of the carbon-based copper composite, ceramics, or an oxide film on the copper surface. Ti, which is not converted to TiN, satisfactorily penetrates into the ceramic or copper having increased wettability after the oxide film is removed, and TiC or the like can be generated, so that the adhesiveness can be significantly improved.
[0015]
The heating atmosphere is nitrogen, which is inexpensive and has no danger of explosion. Therefore, according to the present invention, the cost required for joining can be significantly reduced.
[0016]
According to a second aspect of the present invention, the bonding material is made of a copper alloy foil containing Ti and Mg or a Mg alloy disposed on both sides of the foil.
Copper alloy foils containing Ti are easily available and easier to handle than powders. Therefore, according to the second aspect, the cost required for joining can be further reduced.
[0017]
According to a third aspect, the temperature equal to or higher than the melting point is 885 ° C. to 1083 ° C.
Since the melting point of a Ti-based copper alloy having a Cu composition exceeding 80% is 885 ° C., if the heating temperature is lower than 885 ° C., the bonding material is insufficiently melted, resulting in poor adhesion. On the other hand, when the heating temperature exceeds 1083 ° C., copper flows out of the carbon-based copper composite material, and the product quality deteriorates.
The heating temperature is kept in the range of 885 ° C. to 1083 ° C. in order to avoid poor adhesion and keep good product quality.
[0018]
BEST MODE FOR CARRYING OUT THE INVENTION
An embodiment of the present invention will be described below with reference to the accompanying drawings.
1 (a) to 1 (d) are operation explanatory views (first embodiment) from material preparation to crucible filling in the present invention.
In FIG. 1A, an Si 3 N 4 plate 11 as a ceramic, a Mg powder 12 for forming a bonding material, a CuTi alloy foil 13 for forming a bonding material, and a carbon-based copper composite material 14. Prepare starting materials. The carbon-based copper composite material 14 is described as C / Cu in the drawings.
[0019]
As the CuTi alloy foil 13, for example, a plate of 80 μm is used. If the thickness of the CuTi alloy foil 13 is too large, the heat conduction becomes poor, which is not preferable for joining a heat sink or the like. Therefore, it is desirable to make the thickness thinner if it can be manufactured.
As the CuTi alloy foil 13, for example, an alloy containing 3% by mass of Ti and remaining Cu is used.
[0020]
In (b), first, the Si 3 N 4 plate 11 is placed on the crucible 15, and the Mg powder 12 is placed on the Si 3 N 4 plate 11 at a rate of 10 mg / cm 2 . 10 mg / cm 2 may be selected from the range of 5 to 20 mg / cm 2. If it is less than 5 mg / cm 2 , the reducing action will be weak, and if it exceeds 20 mg / cm 2 , the melting of Mg will be too large.
[0021]
In (c), the CuTi alloy foil 13 is placed, and the Mg powder 12 is placed on the CuTi alloy foil 13 at a rate of 10 mg / cm 2 .
[0022]
In (d), the carbon-based copper composite material 14 is placed. Thus, the filling of the crucible 15 is completed. Further, it is desirable to place another ceramic weight (not shown) on the carbon-based copper composite material 14 and apply a pressing pressure of about 1 kg / cm 2 . This is because bonding can be more reliably performed.
[0023]
FIG. 2 is a heating procedure diagram (first embodiment) according to the present invention, in which a crucible 15 is charged into a heating furnace 20 provided with a heating means 21, a nitrogen gas blowing means 22 and a degassing means 23. Then, the air in the furnace is replaced with nitrogen gas to make a nitrogen gas atmosphere. Next, the inside of the furnace is heated to 900 ° C. by the heating means 21 and maintained at 900 ° C.
[0024]
900 ° C. can be changed in the range of 885 to 1083 ° C. Since the melting point of a Ti-based copper alloy having a Cu composition exceeding 80% is 885 ° C., if the heating temperature is lower than 885 ° C., the bonding material is insufficiently melted, resulting in poor adhesion. On the other hand, when the heating temperature exceeds 1083 ° C., copper flows out of the carbon-based copper composite material, and the product quality deteriorates.
The following reaction occurs in the heating furnace 20 and the crucible 15 by the above heating.
[0025]
Embedded image
Figure 2004255416
[0026]
As shown in the equation (1), the Mg powder 12 sublimates into Mg (gas). Then, ▲ 2 ▼ as shown in Equation, Mg reacts with N 2 atmosphere Mg 3 N 2 is produced. This Mg 3 N 2 exerts a strong reducing action.
[0027]
Ti contained in CuTi alloy foil 13 to consider whether to react with N 2 atmosphere. Mg 3 N 2 is more stable than TiN from the viewpoint of standard energy of formation. Unstable TiN, if produced, does not exist in that form. Therefore, stable Mg 3 N 2 is mainly generated, and unstable TiN is not substantially generated. When present in the form of Ti, Ti serves as a wetting promoter.
[0028]
Incidentally, in FIG. 1A, SiO 2 as an oxide film exists on the surface of the Si 3 N 4 plate 11 as a ceramic.
The CuTi alloy foil 13 has TiO 2 and / or CuO (copper oxide) as an oxide film on the surface.
It is considered that CuO (copper oxide) exists on the copper surface of the carbon-based copper composite material 14.
[0029]
The above oxide films SiO 2 , TiO 2 , and CuO are changed to Si, Ti, and Cu by the next reaction (reduction reaction with Mg 3 N 2 ), and the oxide film is substantially removed.
[0030]
Embedded image
Figure 2004255416
[0031]
That is, the oxide film SiO 2 is removed by the formula (3), the oxide film TiO 2 is removed by the formula (4), and the oxide film CuO is removed by the formula (5). Thus, the wettability of the Si 3 N 4 plate 11 and the carbon-based copper composite material 14 with the molten metal (the molten bonding material) is increased.
[0032]
By heating at 900 ° C., the molten metal (molten joining material) penetrates into the Si 3 N 4 plate 11 and the carbon-based copper composite material 14 and good adhesion can be performed. In particular, in the carbon-based copper composite material 14 in which adhesion is difficult, the bonding force can be increased by generation of TiC.
[0033]
FIG. 3 is a cross-sectional view (first embodiment) of a joined body manufactured by the method of the present invention. A joined body 25 is made of a Si 3 N 4 plate 11, a CuTi alloy foil 13, and a carbon-based copper composite material 14. However, the carbon-based copper composite material 14 is a bonded article that can be firmly bonded to the Si 3 N 4 plate 11 via the CuTi alloy foil 13.
[0034]
In FIG. 1, the Si 3 N 4 plate 11 as a ceramic may be SiN, SiO 2 , AlN, Al 2 O 3, or TiC. The reason is as follows.
The oxide film of Si 3 N 4 and SiO 2 is SiO 2 and can be reduced by the above formula (3). The oxide film of AlN and Al 2 O 3 is Al 2 O 3 , and can be similarly reduced with Mg 3 N 2 . The oxide film of TiC is TiO 2 and can be reduced by the above formula (4).
That is, the ceramics may be any of oxides, nitrides, carbides, borides, and the like.
[0035]
Next, another embodiment of the first embodiment described above will be described. The second embodiment as another embodiment has many portions overlapping with the first embodiment, but will be described in detail for accuracy.
4 (a) to 4 (d) are operation explanatory views (second embodiment) from material preparation to crucible filling in the present invention.
1A, a starting material including a copper plate 26, an Mg powder 12 and a CuTi alloy foil 13 for forming a bonding material, and a carbon-based copper composite material 14 is prepared.
[0036]
As the CuTi alloy foil 13, for example, a plate of 80 μm is used.
As the CuTi alloy foil 13, for example, an alloy of 3% by mass of Ti and the remainder of Cu is used.
[0037]
In (b), first, a copper plate 26 is placed on the crucible 15, and the Mg powder 12 is placed on the copper plate 26 at a rate of 10 mg / cm 2 .
In (c), the CuTi alloy foil 13 is placed, and the Mg powder 12 is placed on the CuTi alloy foil 13 at a rate of 10 mg / cm 2 .
In (d), the carbon-based copper composite material 14 is placed. Thus, the filling of the crucible 15 is completed.
[0038]
FIG. 5 is a heating procedure diagram (second embodiment) according to the present invention. The crucible 15 is charged into a heating furnace 20 provided with a heating means 21, a nitrogen gas blowing means 22 and a degassing means 23. Then, the air in the furnace is replaced with nitrogen gas to make a nitrogen gas atmosphere. Next, the inside of the furnace is heated to 900 ° C. by the heating means 21 and maintained at 900 ° C.
[0039]
The following reaction occurs in the heating furnace 20 and the crucible 15 by the above heating.
[0040]
Embedded image
Figure 2004255416
[0041]
As shown in the equation (6), the Mg powder 12 sublimates into Mg (gas). Then, ▲ 7 ▼ as shown in Equation, Mg reacts with N 2 atmosphere Mg 3 N 2 is produced. This Mg 3 N 2 exerts a strong reducing action.
[0042]
By the way, in FIG. 4A, CuO as an oxide film exists on the surface of the copper plate 26.
The CuTi alloy foil 13 has TiO 2 and / or CuO as an oxide film on the surface.
It is considered that CuO exists on the copper surface of the carbon-based copper composite 14.
[0043]
The above oxide films TiO 2 and CuO are changed to Ti and Cu by the next reaction (reduction reaction with Mg 3 N 2 ), and the oxide film is substantially removed.
[0044]
Embedded image
Figure 2004255416
[0045]
That is, the oxide film TiO 2 is removed by the formula (8), and the oxide film CuO is removed by the formula (9). Thereby, the copper plate 26 and the carbon-based copper composite material 14 have high wettability with the molten metal.
[0046]
By heating at 900 ° C., the molten metal (fused joining material) permeates the Si 3 N 4 plate 11 and the carbon-based copper composite material 14, and good adhesion can be performed. In particular, in the carbon-based copper composite material 14 in which adhesion is difficult, the bonding force can be increased by the generation of TiC.
[0047]
FIG. 6 is a cross-sectional view (second embodiment) of a joined body manufactured by the method of the present invention. A joined body 27 is composed of a copper plate 26 and a carbon-based copper composite material 14. The CuTi alloy foil 13 shown in FIG. 5 has substantially two layers to be integrated with the copper plate 26. The carbon-based copper composite material 14 is a joint that can be firmly joined to the copper plate 26 via the integrated CuTi alloy foil 13.
[0048]
In the embodiment, a CuTi alloy foil is combined with Mg powder as a joining material, but the joining material may be a CuTiMg alloy foil. Alternatively, the joining material can be replaced with a metal powder mixture consisting of Cu powder + Ti powder + Mg powder.
CuTiMg alloy foil is best in terms of handling. A combination of the CuTi alloy foil and the Mg powder is suitable for cost reduction because the Mg powder is easily available.
[0049]
【The invention's effect】
The present invention has the following effects by the above configuration.
Claim 1 is characterized in that not only Ti but also Mg is added to the joining material. When heated, Mg (solid) sublimates into Mg (gas) and combines with nitrogen in the atmosphere to form Mg 3 N 2 . This Mg 3 N 2 is more stable than TiN in terms of standard energy of formation. As a result, generation of TiN can be suppressed.
[0050]
In addition, Mg 3 N 2 exerts a strong reducing action, and reduces and removes the copper surface of the carbon-based copper composite, ceramics, or an oxide film on the copper surface. Ti, which is not converted to TiN, satisfactorily penetrates into the ceramic or copper having increased wettability after the oxide film is removed, and TiC or the like can be generated, so that the adhesiveness can be significantly improved.
[0051]
The heating atmosphere is nitrogen, which is inexpensive and has no danger of explosion. Therefore, according to the present invention, the cost required for joining can be significantly reduced.
Therefore, according to the first aspect, it is possible to provide a method of joining a carbon-based copper composite material and ceramics or a method of joining a carbon-based copper composite material and copper at a low cost and capable of improving adhesion.
[0052]
According to a second aspect of the present invention, the bonding material is made of a copper alloy foil containing Ti and Mg or a Mg alloy disposed on both sides of the foil. Copper alloy foils containing Ti are easily available and easier to handle than powders. Therefore, according to the second aspect, the cost required for joining can be further reduced.
[0053]
According to a third aspect, the temperature equal to or higher than the melting point is 885 ° C. to 1083 ° C. If the heating temperature is lower than 885 ° C., the bonding material is not sufficiently melted, resulting in poor bonding. On the other hand, when the heating temperature exceeds 1083 ° C., copper flows out of the carbon-based copper composite material, and the product quality deteriorates.
The heating temperature is kept in the range of 885 ° C. to 1083 ° C. in order to avoid poor adhesion and keep good product quality.
[Brief description of the drawings]
FIG. 1 is a diagram illustrating the operation from material preparation to crucible filling in the present invention (first embodiment).
FIG. 2 is a view showing a heating procedure in the present invention (first embodiment).
FIG. 3 is a cross-sectional view of a joined body manufactured by the method of the present invention (first embodiment).
FIG. 4 is a diagram illustrating the operation from material preparation to crucible filling in the present invention (second embodiment).
FIG. 5 is a heating procedure diagram in the present invention (second embodiment).
FIG. 6 is a sectional view of a joined body manufactured by the method of the present invention (second embodiment).
[Explanation of symbols]
11: Si 3 N 4 plate as ceramics, 12: Mg powder for forming a bonding material, 13: CuTi alloy foil for forming a bonding material, 14: carbon-based copper composite material, 20: heating furnace, 21 ... heating means, 22 ... nitrogen gas blowing means, 25, 27 ... joined body, 26 ... copper plate.

Claims (3)

炭素基銅複合材とセラミックスとの接合方法又は炭素基銅複合材と銅との接合方法において、炭素基銅複合材とセラミックスとの間又は炭素基銅複合材と銅との間に、Ｔｉ並びにＭｇを含む接合材を介在させ、この多層体を窒素ガス雰囲気下で前記接合材の融点以上の温度に加熱し、生成したＭｇ３Ｎ２で炭素基銅複合材の銅表面やセラミックス又は銅表面の酸化物膜を還元し、Ｔｉと炭素との結合を促して炭素基銅複合材とセラミックス又は銅を接合することを特徴とする炭素基銅複合材とセラミックス又は銅との接合方法。In the method of bonding the carbon-based copper composite material and the ceramic or the method of bonding the carbon-based copper composite material and the copper, between the carbon-based copper composite material and the ceramic or between the carbon-based copper composite material and the copper, Ti and This multilayer body is heated to a temperature equal to or higher than the melting point of the bonding material under a nitrogen gas atmosphere with a bonding material containing Mg interposed therebetween, and the generated Mg 3 N 2 is used to form a copper surface or a ceramic or copper surface of a carbon-based copper composite material. Bonding the carbon-based copper composite material to ceramics or copper by reducing the oxide film and bonding the Ti and carbon to each other to bond the carbon-based copper composite material to ceramics or copper. 前記接合材は、Ｔｉを含む銅合金箔と、この箔の両面に配置したＭｇ又はＭｇ合金と、からなることを特徴とする請求項１記載の炭素基銅複合材とセラミックス又は銅との接合方法。2. The bonding between a carbon-based copper composite material and ceramics or copper according to claim 1, wherein the bonding material is made of a copper alloy foil containing Ti and Mg or a Mg alloy disposed on both surfaces of the foil. Method. 前記融点以上の温度は、８８５℃〜１０８３℃であることを特徴とする請求項１又は請求項２記載の炭素基銅複合材とセラミックス又は銅との接合方法。The method according to claim 1 or 2, wherein the temperature equal to or higher than the melting point is 885 ° C to 1083 ° C.
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