JPWO2013061527A1 - 接合用組成物 - Google Patents
接合用組成物 Download PDFInfo
- Publication number
- JPWO2013061527A1 JPWO2013061527A1 JP2013540626A JP2013540626A JPWO2013061527A1 JP WO2013061527 A1 JPWO2013061527 A1 JP WO2013061527A1 JP 2013540626 A JP2013540626 A JP 2013540626A JP 2013540626 A JP2013540626 A JP 2013540626A JP WO2013061527 A1 JPWO2013061527 A1 JP WO2013061527A1
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- bonding
- composition
- metal
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- bonding composition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
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Abstract
Description
無機粒子と、前記無機粒子の表面の少なくとも一部に付着しているアミン及び/又はカルボン酸を含む有機物と、を含み、
熱分析によって室温から200℃まで加熱したときの重量減少率が33%〜69%であり、かつ、200℃から300℃まで加熱したときの重量減少率が24%〜50%であること、
を特徴とする接合用組成物を提供する。
更に、上記の本発明の接合用組成物は、金属同士の接合に用いるのが好ましい。
本実施形態の金属コロイドを含んでなる接合用組成物は、
金属粒子と、
前記金属粒子の表面の少なくとも一部に付着しているアミン及び/又はカルボン酸を含む有機物と、を含み、
熱分析によって室温から200℃まで加熱したときの重量減少率が33%〜69%であり、かつ、200℃から300℃まで加熱したときの重量減少率が24%〜50%であること、
を特徴とする。
本実施形態の接合用組成物の金属粒子としては、特に限定されるものではないが、本実施形態の接合用組成物を用いて得られる接着層の導電性を良好かつ安定にすることができるため、亜鉛よりもイオン化傾向が小さい(貴な)金属であるのが好ましい。
D=Kλ/Bcosθ
ここで、K:シェラー定数(0.9)、λ:X線の波長、B:回折線の半値幅、θ:ブラッグ角である。
本実施形態の接合用組成物において、金属粒子の表面の少なくとも一部に付着している有機物、即ち、金属コロイド粒子中の「有機物」は、いわゆる分散剤として上記金属粒子とともに実質的に金属コロイド粒子を構成する。当該有機物には、金属中に最初から不純物として含まれる微量有機物、後述する製造過程で混入して金属成分に付着した微量有機物、洗浄過程で除去しきれなかった残留還元剤、残留分散剤等のように、金属粒子に微量付着した有機物等は含まれない概念である。なお、上記「微量」とは、具体的には、金属コロイド粒子中1質量%未満が意図される。
モノアミンとしては、オレイルアミン、ヘキシルアミン、ブチルアミン、ペンチルアミン、ヘキシルアミン、オクチルアミン、ドデシルアミン等のアルキルアミン(C2-20程度の直鎖状アルキルアミン、側鎖を有していてもよい。)、シクロペンチルアミン、シクロヘキシルアミン等のシクロアルキルアミン、アニリン等のアリルアミン等の第1級アミン、ジプロピルアミン、ジブチルアミン、ピペリジン、ヘキサメチレンイミン等の第2級アミン、トリプロピルアミン、ジメチルプロパンジアミン、シクロヘキシルジメチルアミン、ピリジン、キノリン等の第3級アミン等が挙げられる。
本実施形態の接合用組成物には、上記の成分に加えて、本発明の効果を損なわない範囲で、使用目的に応じた適度な粘性、密着性、乾燥性又は印刷性等の機能を付与するために、分散媒や、例えばバインダーとしての役割を果たすオリゴマー成分、樹脂成分、有機溶剤(固形分の一部を溶解又は分散していてよい。)、界面活性剤、増粘剤又は表面張力調整剤等の任意成分を添加してもよい。かかる任意成分としては、特に限定されない。
次に、本実施形態の金属コロイドを含んでなる接合用組成物を製造するためには、主成分としての、有機物で被覆された金属粒子(金属コロイド粒子)を調製する。
本実施形態の接合用組成物を用いれば、加熱を伴う部材同士の接合において高い接合強度を得ることができる。即ち、上記接合用組成物を第1の被接合部材と第2の被接合部材との間に塗布する接合用組成物塗布工程と、第1の被接合部材と第2の被接合部材との間に塗布した接合用組成物を、所望の温度(例えば300℃以下、好ましくは150〜200℃)で焼成して接合する接合工程と、により、第1の被接合部材と第2の被接合部材とを接合することができる。この際、加圧することもできるが、特に加圧しなくとも十分な接合強度を得ることができるのも本発明の利点のひとつである。また、焼成を行う際、段階的に温度を上げたり下げたりすることもできる。また、予め被接合部材表面に界面活性剤又は表面活性化剤等を塗布しておくことも可能である。
トルエン(和光純薬工業(株)製特級)200mLにヘキシルアミン(東京化成工業(株)製EPグレード)15gを加え、マグネティックスターラーにてよく攪拌した。攪拌を行いながら、硝酸銀(和光純薬工業(株)製特級)10gを加え、硝酸銀が溶解したところでオレイン酸(和光純薬工業(株)製一級)5g及びヘキサン酸(和光純薬工業(株)製特級)10gを順次添加し、硝酸銀のトルエン溶液を調製した。
(1)熱分析
上記で得た接合用組成物約10mgについて、リガク(株)製の熱重量分析装置を用いて熱分析試験を行った。加熱は、室温(25℃)から550℃までを10℃/分でチッ素気流中において上昇させて行い、重量減少を測定した。そして、初期値(室温)から500℃までの減少値(≒組成物中の全有機物量)を基準として、200℃までに減少した重量減少率と、200℃から300℃の間に減少した重量減少率を計算で求めた。
上記で得た接合用組成物をダイボンダー(ハイソル社製)を用いて、表面に金メッキを施したアルミナ板(50mm角)に少量載せ、その上に、市販の青色LEDチップ(ジェネライツ社製、底面積600ミクロン×600ミクロン)を積層した。その際、外力を加えて加圧することはしなかった。
更に、上記で得た接合用組成物中に含まれる金属粒子の粒径測定を広角X線回折法で測定した。理学電機(株)製のRINT−UltimaIIIを用いて、回折法で2θが30〜80°の範囲で測定した。得られた回折スペクトルのうち最大の強度を示す約38°(111面)の測定値をシェラー式に代入し、粒径(より正確には結晶子径)を求めた。
エバポレーターを用いた加熱処理の後に、分散媒としてのテルピネオール(和光純薬工業(株)製)を10質量%になるように添加した以外は、実施例1と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
エバポレーターを用いた加熱の際の加熱時間を60分間にした以外は、実施例1と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
エバポレーターを用いた加熱処理に代えて、未処理銀粒子組成物を大気雰囲気下150℃のオーブンに15分間入れることで加熱処理した以外は、実施例1と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
エバポレーターを用いた加熱の際の加熱温度を80℃にし、加熱時間を30分間にした以外は、実施例1と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
エバポレーターを用いた加熱の際の加熱温度を40℃にし、加熱時間を90分間にした以外は、実施例1と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
オレイン酸及びヘキサン酸の量をそれぞれ半分にした以外は、実施例1と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
遠心分離にて銀粒子を完全に沈降させただけでその後の加熱処理による有機物の量を調整を行わずに接合用組成物とした以外は、実施例1と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
未処理銀粒子組成物にエバポレーターによる加熱処理をせず、その後、洗浄工程として、少量(10mL)のトルエンを添加し銀粒子を再度分散させ、更に250mLのメタノール中に銀粒子を沈降させ、その後、遠心分離して銀粒子を完全に沈降させてこれを接合用組成物としたこと以外は実施例1と同様にして、接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
上記比較例6の洗浄工程を2回行った以外は、上記比較例6と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
上記比較例6の洗浄工程を3回行った以外は、上記比較例6と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表1に示した。
トルエン(和光純薬工業(株)製特級)300mLにヘキシルアミン(東京化成工業(株)製EPグレード)50gを加え、マグネティックスターラーにてよく攪拌した。攪拌を行いながら、硝酸銀(和光純薬工業(株)製特級)10gを加え、硝酸銀が溶解したところでオレイン酸(和光純薬工業(株)製一級)10g及びヘキサン酸(和光純薬工業(株)製特級)5gを順次添加し、硝酸銀のトルエン溶液を調製した。
(1)熱分析
上記評価試験1の熱分析と同様の方法で熱分析を行った。結果を表2に示した。
上記評価試験1の接合強度測定と同様の方法で積層体を作製し、得られた積層体を、200℃に調整した熱風循環式オーブンに入れ、大気雰囲気下で、120分間の加熱による焼成処理を行った以外は、上記評価試験1の接合強度測定と同様の方法で接合強度測定を行った。即ち、積層体の底面積に対して5MPaの応力に耐えるかどうかで接合強度試験を行い、耐えた場合を「1」、剥離が見られた場合を「2」と指数で評価した。また、剥離時の接合強度を積層体(チップ)の底面積で除してMPaで求めた。結果を表2に示した。なお、ここで、200℃にて接合強度を求めたのは、省エネルギーの観点から、市場及び顧客のニーズが、焼成条件の低温化に進んでいるからである。
更に、上記で得た接合用組成物中に含まれる金属粒子の粒径測定を、上記評価試験1の粒測定と同様の方法で行った。結果を表2に示した。
未処理銀粒子組成物を大気雰囲気下200℃のオーブンに20分間入れることで加熱処理した以外は、実施例5と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表2に示した。
未処理銀粒子組成物を大気雰囲気下250℃のオーブンに10分間入れることで加熱処理した以外は、実施例5と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表2に示した。
未処理銀粒子組成物を大気雰囲気下350℃のオーブンに5分間入れることで加熱処理した以外は、実施例5と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表2に示した。
エバポレーターを用いた加熱処理に代えて、未処理銀粒子組成物を大気雰囲気下150℃のオーブンに15分間入れることで加熱処理した以外は、実施例5と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表2に示した。
ダイヤフラムポンプを用いて数分間減圧して少量残存していたメタノールをよく蒸発させただけで、その後の加熱処理による有機物の量の調整を行わなかった以外は、実施例5と同様にして接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表2に示した。
ヘキシルアミンを20g、オレイン酸を1.5gとした以外は、実施例5と同様にして未処理銀粒子組成物を得、その後、実施例6と同様にして、大気雰囲気下200℃のオーブンに20分間入れることで加熱処理して接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表2に示した。
ヘキシルアミンを20g、オレイン酸を2.5gとした以外は、実施例5と同様にして未処理銀粒子組成物を得、その後、実施例6と同様にして、大気雰囲気下200℃のオーブンに20分間入れることで加熱処理して接合用組成物を調製し、熱分析及び接合強度測定を行った。結果を表2に示した。
Claims (4)
- 無機粒子と、前記無機粒子の表面の少なくとも一部に付着しているアミン及び/又はカルボン酸を含む有機物と、を含み、
熱分析によって室温から200℃まで加熱したときの重量減少率が33%〜69%であり、かつ、200℃から300℃まで加熱したときの重量減少率が24%〜50%であること、
を特徴とする接合用組成物。 - 前記無機粒子の結晶子径が4〜40nmであること、
を特徴とする請求項1に記載の接合用組成物。 - 前記無機粒子が、金、銀、銅、ニッケル、ビスマス、スズ又は白金族元素よりなる群から選択される少なくとも1種の金属の粒子であること、
を特徴とする請求項1又は2に記載の接合用組成物。 - 金属製の被接合部材同士の接合に用いられること、
を特徴とする請求項1〜3のうちのいずれかに記載の接合用組成物。
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JP6262139B2 (ja) * | 2012-10-12 | 2018-01-17 | バンドー化学株式会社 | 接合用組成物 |
JP6153076B2 (ja) * | 2013-05-22 | 2017-06-28 | 株式会社豊田中央研究所 | 金属ナノ粒子ペースト、それを含有する接合材料、及びそれを用いた半導体装置 |
JPWO2015162881A1 (ja) * | 2014-04-25 | 2017-04-13 | バンドー化学株式会社 | 接合用組成物及びそれを用いた金属接合体 |
JP6387794B2 (ja) * | 2014-11-05 | 2018-09-12 | 株式会社豊田中央研究所 | 有機被覆金属ナノ粒子及びその製造方法 |
TWI585915B (zh) * | 2014-12-12 | 2017-06-01 | Heterogeneous bonding heat dissipation substrate with thick metal plate | |
CN107207911B (zh) * | 2015-01-29 | 2021-01-01 | 阪东化学株式会社 | 接合用组合物及电子零件接合体 |
JP6072117B2 (ja) * | 2015-03-30 | 2017-02-01 | Jx金属株式会社 | 銅微粒子ペースト及びその製造方法 |
WO2017204238A1 (ja) * | 2016-05-26 | 2017-11-30 | 株式会社大阪ソーダ | 導電性接着剤 |
EP3466564B1 (en) * | 2016-05-31 | 2021-07-21 | Hitachi, Ltd. | Metal joining material, production method for same, and method for producing metal joined body using same |
US11515281B2 (en) * | 2019-04-22 | 2022-11-29 | Panasonic Holdings Corporation | Bonded structure and bonding material |
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2012
- 2012-10-09 WO PCT/JP2012/006468 patent/WO2013061527A1/ja active Application Filing
- 2012-10-09 EP EP12843695.3A patent/EP2772328B1/en not_active Not-in-force
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US20140312285A1 (en) | 2014-10-23 |
EP2772328A4 (en) | 2015-08-05 |
WO2013061527A1 (ja) | 2013-05-02 |
EP2772328A1 (en) | 2014-09-03 |
JP6021816B2 (ja) | 2016-11-09 |
TW201321467A (zh) | 2013-06-01 |
EP2772328B1 (en) | 2019-07-03 |
TWI583768B (zh) | 2017-05-21 |
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