JP6162885B2 - 部分的に酸化した金属粒子を含む改良焼結ペースト - Google Patents
部分的に酸化した金属粒子を含む改良焼結ペースト Download PDFInfo
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- JP6162885B2 JP6162885B2 JP2016511071A JP2016511071A JP6162885B2 JP 6162885 B2 JP6162885 B2 JP 6162885B2 JP 2016511071 A JP2016511071 A JP 2016511071A JP 2016511071 A JP2016511071 A JP 2016511071A JP 6162885 B2 JP6162885 B2 JP 6162885B2
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- RQFLGKYCYMMRMC-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O RQFLGKYCYMMRMC-UHFFFAOYSA-N 0.000 description 1
- 229960002446 octanoic acid Drugs 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 229940114930 potassium stearate Drugs 0.000 description 1
- MQOCIYICOGDBSG-UHFFFAOYSA-M potassium;hexadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCC([O-])=O MQOCIYICOGDBSG-UHFFFAOYSA-M 0.000 description 1
- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 229940045870 sodium palmitate Drugs 0.000 description 1
- 229940080350 sodium stearate Drugs 0.000 description 1
- GGXKEBACDBNFAF-UHFFFAOYSA-M sodium;hexadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCC([O-])=O GGXKEBACDBNFAF-UHFFFAOYSA-M 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- ZTUXEFFFLOVXQE-UHFFFAOYSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCC(O)=O ZTUXEFFFLOVXQE-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
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- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
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- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
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- B23K35/24—Selection of soldering or welding materials proper
- B23K35/28—Selection of soldering or welding materials proper with the principal constituent melting at less than 950 degrees C
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- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
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- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
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- B23K35/3613—Polymers, e.g. resins
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- B23K2103/00—Materials to be soldered, welded or cut
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- B23K2103/00—Materials to be soldered, welded or cut
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- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/08—Non-ferrous metals or alloys
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- B23K2103/00—Materials to be soldered, welded or cut
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- B23K2103/00—Materials to be soldered, welded or cut
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- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/50—Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
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Description
(a)金属粒子と、
(b)式I:R1−COR2(I)で表される有機化合物であって、
式中、R1は8〜32個の炭素原子を有する脂肪族残基であり、R2は−OM部分または−X−R3部分を含み、Mはカチオンであり、XはO、S、N−R4から成る群から選択され、R3は水素原子または脂肪族残基であり、R4は水素原子または脂肪族残基である、有機化合物と、
を含み、
有機化合物(b)中に存在する炭素の、金属粒子(a)中に存在する酸素に対するモル比が3〜50の範囲である、混合物である。
本発明による混合物は金属粒子を含む。
さらに、本発明の焼結ペーストは、式I:R1COR2(I)によって表される有機化合物を含み、式中、R1は、8〜32個、好ましくは10〜24個、特に好ましくは12〜18個の炭素原子を有する脂肪族残基であり、分枝状または非分枝状であってもよい。さらに、R1はヘテロ原子を含んでもよい。R2は−OM部分または−X−R3部分のいずれかを含み、Mはカチオンであり、Xは、O、S、およびN−R4から成る群から選択され、R3は水素原子または脂肪族残基であり、R4は水素原子または脂肪族残基である。これに関して、XはO、N、またはSであることが好ましく、Oが特に好ましい。
本発明による焼結性混合物は、焼結ペーストとして存在でき、その後、通常は付加的な分散剤(c)を含む。金属ペースト用の一般的な分散剤が、焼結ペースト用に考えられる。
酸素原子を含む有機ポリマーの添加も、さらに焼結性を高めることが意外なことにわかった。
さらに、本発明による混合物は、通例の界面活性剤、消泡剤、結着剤、または粘度調節剤のようなその他の原料成分を含むことができる。好ましくは、混合物は湿潤剤を含むことができる。
(a)好ましくは、銀、銅、アルミニウム、およびニッケルから成る群から選択される、特に銀の、75〜90重量%の金属粒子と、
(b)好ましくは、脂肪酸、脂肪酸塩、および脂肪酸エステルから成る群から選択される、特に脂肪酸の、さらに好ましくは金属粒子(a)上でコーティングとして存在する、0.05〜3.0重量%の有機化合物(b)と、
(c)好ましくは、アルコールの群から、特にテルピネオールから選択される、6〜30重量%の分散剤と、
(d)適用可能な場合、0.05〜1.0重量%のセルロース、特にエチルセルロースと、を含み、
有機化合物(b)に含まれる炭素の金属粒子(a)に含まれる酸素に対するモル比が5〜40の範囲であり、好ましくは10〜35、より好ましくは12〜30、特に好ましくは15〜25の範囲であり、これらの特定された重量はそれぞれ、焼結性混合物の総重量に関わるものである。
本発明の主題の一つは、本発明による混合物の生成方法でもあり、金属粒子(a)、有機化合物(b)、および適用可能な場合、分散剤(c)が混合される。
少なくとも第1の成分、第2の成分、および本発明による混合物を含む交互重ね配置を提供する工程であって、混合物を、第1の成分と第2の成分との間に位置付ける工程、および
交互重ね配置を焼結する工程。
a)本発明による混合物を成分の成分表面に適用する工程、
b)混合物が第1の成分と前記第2の成分との間に位置するように適切に第2の成分を配置することによって交互重ね配置を提供する工程、
c)交互重ね配置を焼結する工程。
最初に、金属ペースト1〜13を、表1に記載の量比で、原料成分を混合して生成した。
ペーストを20〜25℃でステンシル印刷によって適用し、ステンシルは厚さ75μmで、印刷面積は10×10mmであった。ピッチ角60度の鋼製スキージを用いた。印刷速度は50mm/sであった。
圧力焼結は、焼結ペーストを金/ニッケルの表面を含んだ成分に適用した後(焼結ペーストは金側に接触した)または銅の表面に適用した後に行った。その後、焼結ペーストを、TiNiAg金属被覆を有するシリコン成分に接触させ、それぞれの圧力(プロセス圧力)で、240℃で3分間焼結させた。
無圧力焼結は、焼結ペーストを金/ニッケルの表面を含んだ成分に適用した後(焼結ペーストは金側に接触した)または銅の表面に適用した後に行った。その後、焼結ペーストを、TiNiAg金属被覆を有するシリコン成分に接触させた。次の加熱プロファイルを無圧力焼結で用いた。焼結される接触部位を、30分間にわたって25℃〜160℃で徐々に加熱し、その後、160℃で30分間維持した。次に、5分間にわたって最終温度230℃まで温度を徐々に上昇させ、その後60分間、この温度に維持した。その後、温度を50分間にわたって30℃まで徐々に下げた。
焼結性は2つの等しく重み付けした評価基準によって測定した。
焼結された接触部位は、5つの平行なカットラインを、水平方向および垂直方向に有した。それぞれのカットライン間の長さは1mmであった。
シリコン成分に結合した基板を、図1および2に示すようにローラーに取り付けた。図1および2において、焼結層(4)によって基板(ニッケル/金成分または銅成分)(1)に対して焼結されたシリコン成分(3)を、直径2cmのローラー(2)に取り付けた。その複合体を右から左に進めてローラー上で曲げた。図1は、シリコン成分(3)が基板に完全に接着しているので、非常に良い結果(グレード=1)の曲げ試験を示している。
Claims (18)
- (a)金属粒子と、
(b)式I:R1−COR2(I)で表される有機化合物であって、
式中、R1は8〜32個の炭素原子を有する脂肪族残基であり、R2は−OM部分または−X−R3部分を含み、Mはカチオンであり、XはO、S、N−R4から成る群から選択され、R3は水素原子または脂肪族残基であり、R4は水素原子または脂肪族残基である、有機化合物と、
酸素原子を含む付加的なポリマーと、を含み、
有機化合物(b)中に存在する炭素の、金属粒子(a)中に存在する酸素に対するモル比が3〜50の範囲であり、該酸素原子を含む付加的なポリマーがセルロースである、混合物。 - 金属粒子(a)の少なくとも1つの金属が、銀、銅、ニッケル、アルミニウム、合金、およびそれらの混合物から成る群から選択される、請求項1記載の混合物。
- 金属粒子(a)の少なくとも1つの金属が、銀、銅、および銅と銀の混合物から成る群から選択される、請求項1または2の混合物。
- 有機化合物(b)が、C8〜C30の脂肪酸である、請求項1〜3のいずれか1項に記載の混合物。
- 有機化合物(b)が、オクタン酸、ステアリン酸、ラウリン酸、パルミチン酸、およびそれらの混合物から成る群から選択される、請求項1〜4のいずれか1項に記載の混合物。
- 有機化合物(b)が、粒子(a)上でコーティングの形態で存在する、請求項1〜5のいずれか1項に記載の混合物。
- 化合物(b)が、粒子(a)および化合物(b)の総重量に対して、0.1〜4.0重量%の量で存在する、請求項1〜6のいずれか1項に記載の混合物。
- 金属粒子(a)が、金属粒子(a)の重量に対して、0.01〜0.15重量%の酸素含有量を有する、請求項1〜7のいずれか1項に記載の混合物。
- 有機化合物(b)に含まれる炭素の、金属粒子に含まれる酸素に対するモル比が4〜45である、請求項1〜8のいずれか1項に記載の混合物。
- (c)分散剤をさらに含む、請求項1〜9のいずれか1項に記載の混合物。
- 分散剤(c)が、α−テルピネオール、β−テルピネオール、γ−テルピネオール、δ−テルピネオール、前述のテルピネオールの混合物、N−メチル−2−ピロリドン、エチレングリコール、ジメチルアセトアミド、1−トリデカノール、2−トリデカノール、3−トリデカノール、4−トリデカノール、5−トリデカノール、6−トリデカノール、イソトリデカノール、二塩基性エステル、好ましくはグルタル酸のジメチルエステル、アジピン酸のジメチルエステル、コハク酸のジメチルエステル、またはそれらの混合物、グリセリン、ジエチレングリコール、トリエチレングリコール、およびそれらの混合物から成る群から選択される、請求項10記載の混合物。
- 金属粒子(a)、有機化合物(b)、および適用可能な場合、分散剤(c)が混合されることを特徴とする、請求項1〜11のいずれか1項に記載の混合物の生成方法。
- 少なくとも第1の成分、第2の成分、および請求項1〜11のいずれか1項に記載の混合物を含む交互重ね配置を提供する工程であって、前記混合物を、前記第1の成分と前記第2の成分との間に位置付ける工程と、
前記交互重ね配置を焼結する工程と、
を含む、少なくとも2つの成分の結合方法。 - 前記焼結する工程が、180℃〜250℃の温度で行われる、請求項13記載の結合方法。
- 前記焼結が0MPa〜30MPaのプロセス圧力で行われる、請求項13または14に記載の結合方法。
- 前記成分の少なくとも1つが金属表面を有し、それらの上に前記混合物が適用される、請求項13〜15のいずれか1項に記載の結合方法。
- a)請求項1〜11のいずれか1項に記載の混合物を第1の成分の成分表面に適用する工程と、
b)前記混合物が前記第1の成分と第2の成分との間に位置するように適切に第2の成分を配置することによって交互重ね配置を提供する工程と、
c)前記交互重ね配置を焼結する工程と、
を含む、請求項13〜16のいずれか1項に記載の結合方法。 - 前記混合物が適用される前記成分の表面のうちの少なくとも1つが、非貴金属の表面であることを特徴とする、請求項13〜17のいずれか1項に記載の結合方法。
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EP3009211B1 (de) | 2015-09-04 | 2017-06-14 | Heraeus Deutschland GmbH & Co. KG | Metallpaste und deren verwendung zum verbinden von bauelementen |
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