JPWO2019021637A1 - 金属接合積層体の製造方法 - Google Patents
金属接合積層体の製造方法 Download PDFInfo
- Publication number
- JPWO2019021637A1 JPWO2019021637A1 JP2018530164A JP2018530164A JPWO2019021637A1 JP WO2019021637 A1 JPWO2019021637 A1 JP WO2019021637A1 JP 2018530164 A JP2018530164 A JP 2018530164A JP 2018530164 A JP2018530164 A JP 2018530164A JP WO2019021637 A1 JPWO2019021637 A1 JP WO2019021637A1
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- Prior art keywords
- bonded
- bonding composition
- bonding
- silver
- metal
- Prior art date
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- Granted
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- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
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- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/31—Structure, shape, material or disposition of the layer connectors after the connecting process
- H01L2224/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
- H01L2224/321—Disposition
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- H01L2224/32221—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
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- H01L2224/732—Location after the connecting process
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Abstract
Description
上記接合用組成物は、銀粒子及び有機成分を含有するものであれば特に限定されないが、塗布しやすいようにペースト状であることが好ましい。また、マイグレーションを起こりにくくするために、銀粒子以外に、イオン化列が水素より貴である金属、すなわち金、銅、白金、パラジウム等の粒子が併用されてもよい。
上記工程(1)では、第一の被接合体に接合用組成物を塗布する。ここで、「塗布」とは、接合用組成物を面状に塗布する場合も線状に塗布(描画)する場合も含む概念である。塗布されて、加熱により焼成される前の状態の接合用組成物からなる塗膜の形状は、所望する形状にすることが可能である。したがって、加熱による焼結後の本実施形態の接合材(銀粒子焼結層)12は、面状及び線状のいずれであってもよく、第一の被接合体上において連続していても不連続であってもよい。
上記工程(2)では、塗布した接合用組成物(塗膜)を加熱乾燥する。第一の被接合体に塗布された接合用組成物は、塗布性(印刷性)及びポットライフ(可使時間)を確保するために有機成分の量が多くされており、そのまま第二の被接合体を押し付け加熱焼結させると、生成する銀粒子焼結層中に空隙(ボイド)が多く発生してしまう。そこで、接合用組成物に第二の被接合体を押し付ける前に、工程(2)において接合用組成物を加熱乾燥し、接合用組成物中の有機成分の含有量を予め低減する。このとき、接合用組成物中の有機成分の含有量を少なくし過ぎると、第二の被接合体が接合用組成物と充分に密着しないため、ボイドや剥離が発生してしまう。そこで、工程(2)における加熱乾燥(予備乾燥)は、加熱乾燥された接合用組成物中の有機成分の含有量が4質量%以上となるように行われる。また、生成する銀粒子焼結層中にボイドが発生することを抑制する観点からは、加熱乾燥された接合用組成物中の有機成分の含有量は6質量%以下とされることが好ましい。
上記工程(3)では、加熱乾燥された接合用組成物に第二の被接合体を押し付ける。第二の被接合体は、1MPa以下の荷重で押し付けられることが好ましい。押し付け荷重が1MPaを超えると、パワー半導体チップ11等の第二の被接合体へのダメージ(表面の傷つきや割れ)が懸念される。押し付け荷重は0.05MPa以上であることが好ましい。押し付け荷重が0.05MPa未満であると、密着不足となり剥離してしまうおそれがある。上記工程(3)における第二の被接合体の押し付けを行う方法は特に限定されず、従来公知のさまざまな方法が適用可能であるが、加熱乾燥された接合用組成物(乾燥塗膜)を均一に加圧する方法が好ましい。
上記工程(4)では、接合用組成物を加熱して焼結させ、銀粒子焼結層を形成する。工程(2)の予備加熱では、有機成分のうち、主に分散媒が揮発し、銀粒子に付着させた分散剤等は接合用組成物内に残存するが、工程(4)における加熱により、接合用組成物中の有機成分の大部分又は全てが揮発する。本実施形態においては、接合用組成物がバインダー成分を含む場合は、接合材の強度向上及び被接合部材間の接合強度向上等の観点から、バインダー成分も焼結することになるが、場合によっては、各種印刷法へ適用するために接合用組成物の粘度を調整することをバインダー成分の主目的として、焼成条件を制御してバインダー成分を全て除去してもよい。銀粒子焼結層は、高い接合強度と高い信頼性を得るという点で有機成分の残存量は少ない方がよく、有機成分を実質的に含有しないことが好ましいが、本発明の効果を損なわない範囲で有機成分の一部が残存していても構わない。銀粒子焼結層中の有機成分の含有量は、1質量%未満であることが好ましい。
3−メトキシプロピルアミン2.0gをマグネティックスターラーで充分に撹拌を行いながら、シュウ酸銀3.0gを添加し、増粘させた。得られた粘性物質を恒温槽に入れて反応させた後、レブリン酸を10g添加して更に反応させ、懸濁液を得た。次に、懸濁液の分散媒を置換するため、メタノールを加えて撹拌後、遠心分離によりレブリン酸で表面が被覆された銀粒子を沈殿させて分離し、上澄みを捨てた。この操作をもう一度繰り返した。このレブリン酸で表面を被覆された銀粒子1gとミクロン銀粒子(福田金属箔粉工業社製、Ag−HWQ1.5)1gに、分散媒としてトリデカノールを0.05g、ブチルカルビトールアセテートを0.06g、リシノール酸を0.005g加えて撹拌混合し、銀粒子及び有機成分を含有する接合用組成物Aを得た。
焼成処理を窒素雰囲気下で実施したことと、銀メッキした銅板の代わりに希硫酸にて超音波洗浄した無垢銅板を使用したこと以外は実施例1と同様にして金属接合積層体を作製した。
トリデカノール0.05g及びブチルカルビトールアセテート0.06gの代わりにヘキシルカルビトール0.2gを添加して接合用組成物Bを得たことと、予備乾燥の時間を15分間に変えたこと以外は実施例1と同様にして金属接合積層体を作製した。
焼成処理を窒素雰囲気下で実施したことと、銀メッキした銅板の代わりに希硫酸にて超音波洗浄した無垢銅板を使用したこと以外は実施例3と同様にして金属接合積層体を作製した。
焼成処理における最高温度を280℃にしたこと以外は実施例3と同様にして金属接合積層体を作製した。
予備乾燥における温度と時間を100℃5分間にしたこと以外は実施例3と同様にして金属接合積層体を作製した。
3−メトキシプロピルアミンの代わりに3−エトキシプロピルアミン1.5gとジグリコールアミン0.4gを添加して接合用組成物Cを得たこと以外は実施例3と同様にして金属接合積層体を作製した。
焼成処理を窒素雰囲気下で実施したことと、銀メッキした銅板の代わりに希硫酸にて超音波洗浄した無垢銅板を使用したこと以外は実施例7と同様にして金属接合積層体を作製した。
3−メトキシプロピルアミン8.0gとドデシルアミン0.40gを混合し、マグネティックスターラーで充分に撹拌してアミン混合液を調製した。アミン混合液に、撹拌を行いながらシュウ酸銀6.0gと銀粒子(三井金属鉱業社製、還元粉、D50(メジアン径)=1.5μm)10gを添加し、増粘させた。得られた粘性物質を恒温槽に入れ、反応させ、懸濁液を得た。懸濁液の分散媒を置換するため、メタノールを加えて撹拌後、遠心分離により銀微粒子で表面を被覆された銀粒子を沈殿させて分離し、上澄みを捨てた。この操作をもう一度繰り返した。この銀微粒子で表面を被覆された銀粒子15gに、分散媒としてトリデカノールを0.4g、ブチルカルビトールアセテートを0.4g、リシノール酸を0.01g加えて撹拌混合し、接合用組成物Dを得た。接合用組成物Dを得たこと以外は実施例1と同様にして金属接合積層体を作製した。
予備乾燥を行わなかったこと以外は実施例1と同様にして金属接合積層体を作製した。
予備乾燥を行わなかったこと以外は実施例3と同様にして金属接合積層体を作製した。
予備乾燥における温度と時間を100℃10分間にしたこと以外は実施例3と同様にして金属接合積層体を作製した。
実施例及び比較例で作製した接合用組成物を用いて下記評価試験を行った。その結果を表1に示した。
日立ハイテクノロジーズ社製の走査型電子顕微鏡(型番:S4800)を用いて200000倍で撮影した写真から、50〜100個程度の粒子の粒径の算術平均値を算出する方法にて銀粒子の平均粒径を得た。
予備乾燥の前後で接合用組成物の質量を測定し、得られた質量を基に、下記式を用いて予備乾燥後の有機成分の含有量を算出した。
有機成分の揮発量(g)=塗布した接合用組成物の質量(g)−予備乾燥後の接合用組成物の質量(g)
予備乾燥後の有機成分の含有量(質量%)={有機成分の添加量(g)−有機成分の揮発量(g)/塗布した接合用組成物の質量(g)}×100
常温にてボンドテスター(レスカ社製)を用いて接合強度試験を行った。
金属接合積層体を研磨にて断面を露出させ、走査型電子顕微鏡にて断面観察を行った。得られた電子顕微鏡写真から、銀粒子焼結層内の空隙の面積を銀粒子焼結層の全体の面積で割って空隙率を算出した。空隙率が20%以下は○、21〜30%は△、31%以上は×とした。また、空隙率の値に関わらず、大きな空隙が存在したり、接合した界面が剥離したりしているものは×とした。
12 接合材
13 銅張絶縁基板
13a 基材
13b Cu層
14 放熱材
15 ヒートシンク
16 ワイヤーボンド
Claims (5)
- 第一の被接合体と第二の被接合体とが銀粒子焼結層により接合された金属接合積層体の製造方法であって、
前記第一の被接合体に、銀粒子及び有機成分を含有する接合用組成物を塗布する工程(1)と、
塗布した前記接合用組成物を加熱乾燥する工程(2)と、
加熱乾燥された前記接合用組成物に前記第二の被接合体を押し付ける工程(3)と、
前記接合用組成物を加熱して焼結させ、前記銀粒子焼結層を形成する工程(4)とを含み、
前記工程(2)で加熱乾燥された前記接合用組成物中の前記有機成分の含有量は4質量%以上であることを特徴とする金属接合積層体の製造方法。 - 前記銀粒子焼結層の空隙率は、20体積%以下であることを特徴とする請求項1に記載の金属接合積層体の製造方法。
- 前記工程(2)では、25℃以上、100℃以下の温度で加熱乾燥することを特徴とする請求項1又は2に記載の金属接合積層体の製造方法。
- 前記工程(3)では、前記第二の被接合体を1MPa以下の荷重で押し付けることを特徴とする請求項1〜3のいずれかに記載の金属接合積層体の製造方法。
- 前記工程(4)では、前記第一の被接合体と前記第二の被接合体とを無加圧下で接合することを特徴とする請求項1〜4のいずれかに記載の金属接合積層体の製造方法。
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