JP6494047B2 - 金属粉末を製造するための方法 - Google Patents
金属粉末を製造するための方法 Download PDFInfo
- Publication number
- JP6494047B2 JP6494047B2 JP2016564060A JP2016564060A JP6494047B2 JP 6494047 B2 JP6494047 B2 JP 6494047B2 JP 2016564060 A JP2016564060 A JP 2016564060A JP 2016564060 A JP2016564060 A JP 2016564060A JP 6494047 B2 JP6494047 B2 JP 6494047B2
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- Prior art keywords
- silver
- powder
- sintering
- copper
- acid
- Prior art date
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- 238000000034 method Methods 0.000 claims description 48
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Description
塩基性金属塩溶液を準備するステップと;
塩基性金属塩溶液を還元剤と接触させ、それから金属粉末を沈殿させるステップと;
沈殿した金属粉末を溶媒から回収するステップと
を含む方法を提供する。
金属は、銀を含み;
還元剤は、ヒドラジンを含み、
方法は、
塩基性金属塩溶液を還元剤と接触させるステップの後に、塩基性金属塩溶液をオレイン酸キャッピング剤と接触させるステップと、
回収された沈殿した金属粉末を、オレイン酸キャッピング剤の存在下で、ボールミルを使用して少なくとも30分間粉砕するステップと
を更に含む。
銅粒子から酸化物層をエッチングするステップと;
ガルバニめっきを使用して銅粒子に銀コーティングを適用するステップと
を含む。
銅粉末を準備するステップと;
銅粉末を、ポリマー及び/又はポリアミンの存在下で、ボールミルを使用して粉砕するステップと
を含む方法を提供する。
500nmから10μmのD50;及び
2g/cm3を超えるタップ密度
を有する金属粉末であって、銀、銅及びそれらの1つ又は複数の合金の1つ又は複数を含む金属粉末を提供する。
本明細書に記載のような金属粉末と;
結合剤と;
溶媒と;
任意選択で、レオロジー調節剤及び/又は有機銀化合物及び/又は活性剤及び/又は界面活性剤及び/又は湿潤剤及び/又は過酸化水素若しくは有機過酸化物と
を含む、焼結用ペーストを提供する。
1から15wt%の結合剤;及び/又は
1から30wt%の溶媒;及び/又は
5wt%までのレオロジー調節剤;及び/又は
10wt%までの有機銀化合物;及び/又は
2wt%までの活性剤;及び/又は
6wt%までの界面活性剤;及び/又は
2wt%までの過酸化水素若しくは有機過酸化物
を含む。
本明細書に記載のような金属粉末と;
有機銀化合物と;
溶媒と;
任意選択で、活性剤及び/又はレオロジー調節剤及び/又は界面活性剤及び/又は過酸化水素若しくは有機過酸化物と
を含む焼結用ペーストを提供する。
1から30wt%の溶媒;及び/又は
50wt%まで、好ましくは0.1から25wt%、より好ましくは0.1から10wt%、更により好ましくは0.1から9wt%の有機銀化合物;及び/又は
5wt%までのレオロジー調節剤;及び/又は
2wt%までの活性剤;及び/又は
6wt%までの界面活性剤;及び/又は
2wt%までの過酸化水素若しくは有機過酸化物
を含む。
(i)本明細書に記載の焼結用フィルムを、接合されるダイと基板との間に配置するステップと;
(ii)焼結用フィルムを焼結するステップと
を含み、焼結するステップは、圧力の印加なしで行われる、ダイ取付け方法を提供する。
(a)焼結用フィルムをダイに適用して、ダイ側及び焼結用フィルム側を有するアセンブリを形成するステップと;
(b)アセンブリのフィルム側を基板と接触させるステップと
を含む。
(i)本明細書に記載の焼結用フィルムを、接合されるダイと基板との間に配置するステップと;
(ii)焼結用フィルムを焼結するステップと
を含み、焼結するステップは、0.1から40MPaの圧力を印加しながら行われる、ダイ取付け方法を提供する。
(i)本明細書に記載の焼結用フィルムを、接合される2つ以上のウエハの間に配置するステップと;
(ii)焼結用フィルムを焼結するステップと
を含み、焼結するステップは、圧力の印加なしで行われる、ウエハ結合方法を提供する。
本明細書に記載の焼結用フィルムを基板に適用して、焼結用フィルム側及び基板側を有するアセンブリを形成するステップと;
アセンブリの焼結用フィルム側を部品と接触させるステップと;
アセンブリを、50から200℃の温度に加熱するステップと;
アセンブリに、1から5MPaの圧力を、0.1秒から60分間印加するステップと;
基板を焼結用フィルムから分離するステップと
を含む方法を提供する。
本明細書に記載のような金属粉末、又は本明細書に記載のような焼結用ペースト若しくはフィルムを、接合される2つ以上の加工対象物の近くに提供するステップと;
金属粉末又は焼結用ペースト若しくはフィルムを加熱して、少なくとも部分的に金属を焼結するステップと
を含む方法を提供する。
本明細書に記載の方法に従って、金属粉末を調製するステップと;
金属粉末を、結合剤、溶媒、並びに任意選択でレオロジー調節剤及び/又は有機銀化合物及び/又は活性剤及び/又は過酸化物と混合するステップと
を含む方法を提供する。
無加圧焼結
標準的なSMTラインにおける処理可能性
平坦で均一な表面形態
15MPaを超えるダイシェア強度平均
界面破壊モードがない
室温安定性=最低1カ月
熱サイクル:1000サイクルまでの許容される接合部強度(−40℃から+125℃、10分の滞留時間)。
ニードル及び噴射分注可能
フィルム形態因子
高いダイシェア強度(15から45MPa)
高い熱伝導率(>100W/mK)
ピン転写可能
良好な高温特性
実施例1
化学プロセスにおいて、420gの硝酸銀を、2100gの脱イオン水に撹拌により溶解した。これに420gのDMFを添加し、継続的に撹拌した。この溶液に、2つの別個の溶液、(1)325gのトリエチルアミン及び460gのホルムアルデヒドの混合物、並びに(2)200gの脱イオン水中の30gの水酸化ナトリウムの溶液を、同時に添加した。この直後に、新しく調製したオレイン酸ナトリウム溶液(6.3gのオレイン酸を、200gの水中の1.3gの水酸化ナトリウムの溶液に添加した)を添加した。混合物を1時間撹拌し、その後粉末を濾過し、濾液のpHが中性となるまで水及びアセトンで洗浄した。次いで、粉末を炉内で70℃で8時間乾燥させた。
実施例2及び3
化学プロセスにおいて、420gの硝酸銀を、1500gの脱イオン水に撹拌により溶解した。これに、400gの脱イオン水中の89gの水酸化ナトリウムの溶液を添加すると、褐色の不均質溶液が生じた。反応混合物に、1890gの脱イオン水中の126gの水和ヒドラジンの溶液を添加し、これに続いて、新しく調製したオレイン酸ナトリウム溶液(6.3gのオレイン酸を、210gの水中の1.3gの水酸化ナトリウムの溶液に添加した)を添加した。混合物を1時間撹拌し、その後粉末を濾過し、濾液のpHが中性となるまで水及びアセトンで洗浄した。次いで、粉末を炉内で70℃で8時間乾燥させた。
実施例4
1140gの硝酸銅(II)三水和物を、6.9gの界面活性剤(DAXAD)を含有する1550gの脱イオン水に、30分間撹拌することにより溶解した。電子温度計を有するホットプレート上に反応混合物を維持した。pHが8になるまで、1380mLの30%アンモニア溶液を上記溶液に添加した。溶液を10分間撹拌した。温度を70℃に設定した。所望の温度に達した後、1970mLの60%水和ヒドラジンを毎分30mLの速度で添加し、30分間継続的に撹拌した。発泡を低減するために、間隔をおいて最少量のエタノールを添加した。温度を85℃に設定した。その温度に達した後、溶液を2.5時間撹拌した。粉末を沈降させ、上澄みをデカンテーションすることにより収集した。これを水及びアセトンで洗浄し、フォーミングガス(90〜95%窒素:5〜10%水素)環境中で、50℃で8時間炉内で乾燥させた。
実施例5〜7
500gの微粉砕された銅粉末(Cu1)を、300gの蒸留水、25gのPEG400、2.25gのトリエチレンテトラミンの溶液に添加した。これを十分に混合して均質混合物を得、2.2kgの1.6mmサイズのジルコニアビーズを有するアトライターボールミル内に全て移した。粉砕を、(a)Cu3を得るために45分間、(b)Cu4を得るために1時間、及び(c)Cu5を得るために2時間継続した。機械的プロセスの後、混合物をビーズと共にビーカーに入れ、水を使用して銅フレークをビーズから分離した。これを、青色の上澄みが消えるまで水及びアセトンの混合物で洗浄し、次いでアセトンで洗浄した。銅フレークを、その酸化を回避するためにフォーミングガス(90〜95%窒素:5〜10%水素)環境中で50℃で乾燥させた。
実施例8
Agコーティングプロセス:1kgの微粉砕された市販の銅粉末(Cu1)を、2kgの脱イオン水に添加した。これに、50gのPEG−400を添加し、混合物を10分間十分に撹拌すると、均質形態が得られた。上記スラリーを、一定撹拌下で3Lのトリエチレンテトラミンに添加した。この混合物を1.5時間撹拌した。10kgの氷冷水を反応器に添加した。次いでこれを、更に15分間撹拌した。220gの硝酸銀及び660gのクエン酸を、5kgの蒸留水に溶解し、上記反応混合物を一定撹拌下で徐々に(約20分で)添加した。完全に添加した後、反応混合物を更に1時間撹拌した。反応の完了後、混合物を沈降させ、上澄みの青色溶液をデカンテーションし、上澄みが完全に無色となるまで沈降したAgCuを水で洗浄し、続いてアセトンで洗浄した。粉末を炉内で50〜60℃で乾燥させた。
実施例9
Agコーティングプロセス:100gのファセット状銅粉末(Cu2)を、350gの水に入れ、適切な分散体となるように十分撹拌した。これに、350gの水、22.75gの硫酸アンモニウム及び20mLの水酸化アンモニウムの混合物を添加し、15分間撹拌した。上澄みをデカンテーションし、5gのPEG、350gの水及び350gのトリエチルテトラアミンをこれに速やかに添加し、1.5時間撹拌した。これに1kgの水を添加し、続いて250gの水中の26.4gのAgNO3及び22gのクエン酸の溶液を滴下により添加し、1時間撹拌した。粉末を、無色溶液が得られるまでアセトンで洗浄した。粉末を炉内で50〜60℃で乾燥させた。
実施例10〜12
Ag及び有機コーティングプロセス:フレーク状銅粒子Cu3〜5を、フレーク状AgCu粒子の調製に使用した。Agコーティング及び有機コーティングプロセスは、球状AgCu1に関して説明されたものと同じである。
Claims (12)
- 銀粉末を製造するための方法であって、
塩基性銀塩溶液を準備するステップと;
前記塩基性銀塩溶液をヒドラジン、ホルムアルデヒド及びホウ化水素の1つ又は複数を含む還元剤と接触させ、それから銀粉末を沈殿させるステップと;
前記塩基性銀塩溶液を前記還元剤と接触させるステップの後に、前記塩基性銀塩溶液を第1のキャッピング剤と接触させるステップと;
沈殿した銀粉末を前記溶媒から回収するステップと;
少なくとも30分間、第2のキャッピング剤の存在下で、ボールミルを使用して前記回収された沈殿した銀粉末を粉砕するステップと、を含み、
前記製造された銀粉末が、500nmから10μmのD50、及び2g/cm3を超えるタップ密度を有し、
前記第1のキャッピング剤及び前記第2のキャッピング剤が、ラウリン酸、パルミチン酸、ステアリン酸、イソステアリン酸及びオレイン酸の1つ又は複数を含むことを特徴とする方法。 - 前記還元剤が、ヒドラジン及びホウ化水素を含む請求項1に記載の方法。
- 前記粉砕するステップが、少なくとも90分間行われる請求項1に記載の方法。
- 銅粉末を製造する方法であって、
塩基性銅塩溶液を準備するステップと;
前記塩基性銅塩溶液をヒドラジン、ホルムアルデヒド及びホウ化水素の1つ又は複数を含む還元剤と接触させ、それから銅粉末を沈殿させるステップと;
前記塩基性銅塩溶液を前記還元剤と接触させるステップの後に、前記塩基性銅塩溶液をキャッピング剤と接触させるステップと;
沈殿した銅粉末を前記溶媒から回収するステップと;
少なくとも30分間、ポリマー又はポリアミンの存在下で、ボールミルを使用して前記回収された沈殿した銅粉末を粉砕するステップと、を含み、
前記製造された銅粉末が、500nmから10μmのD50、及び2g/cm 3 を超えるタップ密度を有し、
前記キャッピング剤が、ラウリン酸、パルミチン酸、ステアリン酸、イソステアリン酸及びオレイン酸の1つ又は複数を含むことを特徴とする方法。 - 前記粉末を形成する粒子に銀コーティングを適用するステップを更に含み、
前記銀コーティングを適用するステップが、
銅粒子から酸化物層をエッチングするステップと;
ガルバニめっきを使用して前記銅粒子に銀コーティングを適用するステップと
を含む請求項4に記載の方法。 - 前記銀コーティングされた粒子に脂肪酸コーティングを適用するステップを更に含む請求項5に記載の方法。
- 前記製造された銀粉末が、3g/cm 3 を超えるタップ密度を有する請求項1に記載の方法。
- 前記製造された銀粉末が、3.5g/cm 3 から5.5g/cm 3 のタップ密度を有する請求項7に記載の方法。
- 前記塩基性銀塩溶液が、7を超えるpHを示す請求項1に記載の方法。
- 前記塩基性銀塩溶液が、界面活性剤を含む請求項1に記載の方法。
- 前記製造された銀粉末が、3μmから6μmのD90、0.9μmから2μmのD50、及び0.3μmから0.8μmのD10のサイズ分布を示す請求項1に記載の方法。
- 前記製造された銅粉末が、4μmから15μmのD90、2μmから10μmのD50、及び0.5μmから3μmのD10のサイズ分布を示す請求項4に記載の方法。
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JP6920029B2 (ja) | 2016-04-04 | 2021-08-18 | 日亜化学工業株式会社 | 金属粉焼結ペースト及びその製造方法、導電性材料の製造方法 |
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KR102075199B1 (ko) * | 2017-03-31 | 2020-02-07 | 주식회사 솔루에타 | 구리합금 제조방법 및 구리합금을 원료로 하는 호일 제조방법 |
DE102017207210A1 (de) * | 2017-04-28 | 2018-10-31 | Skz-Kfe Ggmbh | Verfahren zur additiven Herstellung eines Bauteils sowie additiv hergestelltes Bauteil |
US11929341B2 (en) * | 2018-06-26 | 2024-03-12 | Alpha Assembly Solutions Inc. | Nano copper paste and film for sintered die attach and similar applications |
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BR112016024827A2 (pt) | 2014-04-23 | 2017-08-15 | Alpha Metals | método para fabricar pó de metal |
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MX2016013818A (es) | 2017-05-30 |
CN106457404B (zh) | 2020-02-21 |
WO2015162405A1 (en) | 2015-10-29 |
US10130995B2 (en) | 2018-11-20 |
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