JP2018190540A - 金属粉焼結ペースト及びその製造方法、ならびに導電性材料の製造方法 - Google Patents
金属粉焼結ペースト及びその製造方法、ならびに導電性材料の製造方法 Download PDFInfo
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- JP2018190540A JP2018190540A JP2017090197A JP2017090197A JP2018190540A JP 2018190540 A JP2018190540 A JP 2018190540A JP 2017090197 A JP2017090197 A JP 2017090197A JP 2017090197 A JP2017090197 A JP 2017090197A JP 2018190540 A JP2018190540 A JP 2018190540A
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- metal powder
- powder sintered
- sintered paste
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- 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
- B22F7/00—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
- 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
- B22F7/062—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 involving the connection or repairing of preformed parts
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- 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
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- B22—CASTING; POWDER METALLURGY
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- 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
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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- 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
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
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Abstract
【解決手段】平均粒径(メジアン径)が0.3μm〜5μmの銀の粒子を主成分として含み、CV値(標準偏差/平均値)が5%未満の無機スペーサー粒子を更に含み、実質的に樹脂を含まない金属粉焼結ペーストを提供する。
【選択図】なし
Description
また金属粉焼結ペーストにおいて、金属粉として金を含まない場合、発光素子の実装によく用いられる金錫共晶半田に比べて安価である。
本実施形態の金属粉焼結ペーストに用いる金属粒子は、銀の粒子が主成分である。すなわち、金属粒子における前記銀の粒子の含有率は、例えば70質量%以上、好ましくは80質量%以上、よりこのましくは90質量%以上であることを意味する。なお、銀の粒子には、例えば10質量%以下、好ましくは7質量%以下、より好ましくは5質量%以下の酸化銀の粒子を含んでもよい。
本実施形態の金属粉焼結ペーストはCV値(標準偏差/平均値)が5%未満の無機スペーサー粒子を含む。前記無機スペーサー粒子は、シリカから成るのが好ましい。前記無機スペーサー粒子が無機物から成るため、前記金属粉焼結ペーストの焼成時に熱分解する恐れが低い。また、前記無機スペーサー粒子が無機物から成るため、前記金属粉焼結ペーストの焼成時に、焼結を阻害する揮発分が発生しない。
1/(材料A重量比/材料A比重+材料B重量比/材料B比重+・・)・・[式1]
さらに金属粉焼結ペーストの厚みは、スペーサーを用いる場合、スペーサーの直径に相当すると考えられる。このため、下記の式2によりチップ下ペースト体積が計算できる。
チップ下ペースト体積=チップ面積×スペーサー直径・・[式2]
チップ下ペースト体積に式1で求められるペースト比重を掛ける事でチップ下ペースト重量が計算できるので、下記の式3によりチップ下スペーサー総体積が求まる。
チップ下スペーサー総体積
=チップ下ペースト体積×ペースト比重×スペーサー重量比/スペーサー比重・・[式3]
上限濃度設定のためのスペーサー体積%は以下の式4で計算できる。
粒子濃度(体積%)=チップ下スペーサー総体積×100/チップ下ペースト体積・・[式4]
さらに、スペーサー粒子体積は下記の式5により粒径から計算できる。
スペーサー粒子体積=4×π×(粒径/2)×(粒径/2)×(粒径/2)/3・・[式5]
下記の式6で下限濃度設定のための粒子濃度(pcs/チップ面積)が求まる。
粒子濃度(pcs/チップ面積)=チップ下スペーサー総体積/スペーサー粒子体積・・[式6]
上記の計算はスペーサー重量比から粒子濃度を求めているが、計算を逆にすれば任意の粒子濃度に相当するスペーサー重量比を求められる。
本実施形態の金属粉焼結ペーストにはアニオン性の界面活性剤が含まれても良い。アニオン性による電界により、一般にマイナスの表面電位を持つ銀や金といった電極に対して、アニオン性の界面活性剤が電界による耐ブリード性を発揮することにより、基板底面への漏れや汚染によるワイヤーボンド不良が改善され、安定した電子部品の製造が可能になる。
R1O(CH2CH(R2)O)n1CH2COOR3 (I)
[式中、R1は炭素数7以上の直鎖または分岐のあるアルキル基であり、R2は−Hまたは−CH3または−CH2CH3、−CH2CH2CH3のいずれかであり、R3は−Hまたはアルカリ金属であり、n1は2〜5の範囲である。]
R11−C(O)N(R12)(CH2)n2COOR13 (II)
[式中、R11は、炭素数7以上の直鎖または分岐のあるアルキル基であり、R12は−Hまたは−CH3または−CH2CH3、−CH2CH2CH3のいずれかであり、R13は−H、NH+(C2H4OH)3またはアルカリ金属であり、n2は1〜5の範囲である。]
R21−CH=CH−(CH2)n3COOR22 (III)
[式中、R21は、炭素数7以上の直鎖または分岐のあるアルキル基であり、R22は−Hまたはアルカリ金属であり、n3は1〜10の範囲である。]
R31−COOR32 (IV)
[式中、R31は、OHまたはCOOR33(R33は、アルカリ金属である)で任意に置換された炭素数7以上の直鎖または分岐のあるアルキル基またはアルコキシ基であり、R32は−Hまたはアルカリ金属である。]
R41−SO3R42 (V)
[式中、R41は、OHまたはCOOR43(R43は、アルキル基である)で任意に置換された炭素数7以上の直鎖または分岐のあるアルキル基、アラルキル基もしくはアルケニル基またはアラルキル基であり、R42は、−Hまたはアルカリ金属である。]
R61−O−PO(OR62)OR63 (VII)
[式中、R61及びR62は、直鎖または分岐のあるアルキル基であり、R63は、−Hまたはアルカリ金属である。]
本実施形態の金属粉焼結ペーストは、分散媒として有機溶剤を含む事が好ましい。銀の粒子を有機溶剤に均一に分散する事で、印刷やディスペンスといった手法により効率的に高品質な塗布が可能になるからである。
本実施形態の金属粉焼結ペーストは、実質的に樹脂を含まない。前記樹脂としては、エポキシ樹脂やフェノール樹脂等の結合剤、ポリアミド樹脂などの硬化剤が挙げられる。
また、CV値(標準偏差/平均値)が5%未満の無機スペーサー粒子と、平均粒径(メジアン径)が0.3μm〜5μmの銀の粒子とを混合することを含み、ただし実質的に樹脂とは混合しない金属粉焼結ペーストの製造方法について以下に説明する。なお、前記無機スペーサー粒子、銀の粒子および樹脂については、前記金属粉焼結ペーストにおいて説明したとおりである。
170℃60分の大気オーブンによる焼成によって電気抵抗が6μΩ・cm以下の導電性材料が得られる金属粉焼結ペーストが好ましい。
また、金属粉焼結ペーストを焼成する工程を含む本実施形態の導電性材料の製造方法について説明する。この方法において金属粉焼結ペーストは、本実施形態の金属粉焼結ペーストである。
前記焼成は、非酸化性雰囲気下、大気下、真空雰囲気下、酸素もしくは混合ガス雰囲気下などの雰囲気下等で行ってもよいが、酸素、オゾン又は大気雰囲気下で行われるのが好ましい。この雰囲気下で焼成すれば、銀の熱拡散が加速され、より高い焼結強度を有する導電性材料(焼結体)が得られるからである。
本実施形態の導電性材料は、本実施形態の金属粉焼結ペーストを焼成して得られる。本実施形態の導電性材料は、電気抵抗値が50μΩ・cm以下であるのが好ましい。電気抵抗が低いほど、電極として用いる場合には電力のロスが抑えられ、また放熱性に優れるためである。電気抵抗値は、10μΩ・cm以下であるのがより好ましく、6μΩ・cm以下であるのがさらに好ましい。
本実施形態の金属粉焼結ペーストを用いて、チップと基板を接合する方法は、
前記金属粉焼結ペーストを前記基板上に塗布し、
前記金属粉焼結ペーストの上に前記チップを配置し、
前記金属粉焼結ペーストと前記チップが配置された前記基板を加熱し、前記金属粉焼結ペーストを焼結させて前記チップと前記基板を接合させる工程を含む。
前記加熱は、非酸化性雰囲気下、大気下、真空雰囲気下、酸素もしくは混合ガス雰囲気下、気流中などの雰囲気下等で行ってもよいが、酸素、オゾン又は大気雰囲気下で行われるのが好ましい。この雰囲気下で加熱すれば、銀の熱拡散が加速され、より高い焼結強度を有する導電性材料(焼結体)が得られるからである。
有機溶剤である2−エチル−1,3−ヘキサンジオール(0.57g)とジエチレングリコールモノブチルエーテル(0.14g)および、アニオン性液状界面活性剤(三洋化成工業株式会社製、製品名「ビューライトLCA−H」、ラウレス−5−カルボン酸、25℃で液状、0.09g)を、自転・公転ミキサー(商品名「あわとり錬太郎AR−250」、株式会社シンキー製)にて1分間攪拌、次いで15秒間脱泡のサイクルを1サイクル用いて攪拌し、溶剤混合物を得た。
有機溶剤である2−エチル−1,3−ヘキサンジオール(0.57g)とジエチレングリコールモノブチルエーテル(0.14g)および、アニオン性液状界面活性剤(三洋化成工業株式会社製、製品名「ビューライトLCA−H」、ラウレス−5−カルボン酸、25℃で液状、0.09g)を自転・公転ミキサー(商品名「あわとり錬太郎AR−250」、株式会社シンキー製)にて1分間攪拌、次いで15秒間脱泡のサイクルを1サイクル用いて攪拌し、溶剤混合物を得た。
真球状シリカスペーサー(宇部エクシモ製、製品名「ハイプレシカTS」、平均粒径(メジアン径)が31.14μm、CV値が1.92%、0.03g)の代わりに真球状シリカスペーサー(宇部エクシモ製、製品名「ハイプレシカTS」、コールターカウンターによる測定で平均粒径(メジアン径)が50.8μm、CV値が1.1%、0.09g)を用いた以外は、実施例1と同様に行い、金属粉焼結ペースト(10g)を得た(銀の粒子の含有量は、91.0質量%、スペーサー粒子濃度は214pcs/チップ面積で2.62体積%)。
比較例1、実施例1または2において得られた金属粉焼結ペーストを、表面に金を有する銅フレームにディスペンス法を用いて塗布し、裏面に銀電極を有し、外形4650μm×2300μm、厚み400μmの、窒化アルミを基材とするサブマウントチップをその上へマウントした。サブマウントチップには半導体発光素子が実装されている。金属粉焼結ペーストを介してサブマウントチップがマウントされた基板を、大気オーブンを用いて185℃で120分加熱し、その後、冷却した。冷却後に、サブマウント表面とフレーム表面の高さの差を光学式の測定顕微鏡で測定し、サブマウント厚みよりペースト厚みを算出した。その後、加熱後の金属粉焼結ペーストを介してサブマウントチップがマウントされた基板の半量を、85℃、85%の高温高湿槽に24時間投入し、260℃、10秒のリフローパスを実施するサイクルを計2サイクル実施した。その後、リフロー前とリフロー後の両サンプルを、基板からサブマウントチップを剥す方向に剪断力をかけ、サブマウントチップが剥離したときの強度を接合強度として測定した。
Claims (14)
- 平均粒径(メジアン径)が0.3μm〜5μmの銀の粒子を主成分として含み、
CV値(標準偏差/平均値)が5%未満の無機スペーサー粒子を更に含み、
実質的に樹脂を含まない金属粉焼結ペースト。 - 前記無機スペーサー粒子がシリカから成ることを特徴とする、請求項1に記載の金属粉焼結ペースト。
- 前記無機スペーサー粒子の平均粒径(メジアン径)が10〜60μmである事を特徴とする、請求項1または2に記載の金属粉焼結ペースト。
- 前記銀の粒子は、フレーク状である請求項1〜3のいずれか一項に記載の金属粉焼結ペースト。
- 前記銀の粒子は、平均粒径(メジアン径)が0.3μm未満の粒子の含有量が5質量%以下である請求項1〜4のいずれか一項に記載の金属粉焼結ペースト。
- 前記銀の粒子は、平均粒径(メジアン径)が0.5μm以下の粒子の含有量が15質量%以下である請求項5に記載の金属粉焼結ペースト。
- 分散媒として有機溶剤を更に含む請求項1〜6のいずれか一項に記載の金属粉焼結ペースト。
- 前記有機溶剤の沸点が、150〜250℃の範囲である請求項7に記載の金属粉焼結ペースト。
- 前記金属粉焼結ペーストの焼結後の導電性材料の電気抵抗が6μΩ・cm以下である請求項1〜8のいずれか一項に記載の金属粉焼結ペースト。
- 前記銀の粒子の含有量が、前記ペーストに対して70質量%以上である請求項1〜9のいずれか一項に記載の金属粉焼結ペースト。
- CV値(標準偏差/平均値)が5%未満の無機スペーサー粒子と、平均粒径(メジアン径)が0.3μm〜5μmの銀の粒子とを混合することを含み、ただし実質的に樹脂とは混合しない金属粉焼結ペーストの製造方法。
- 請求項1〜10のいずれか一項に記載の金属粉焼結ペーストを焼成する工程を含む導電性材料の製造方法。
- 前記焼成が、160℃〜300℃の範囲の温度で行われる請求項12に記載の導電性材料の製造方法。
- 前記焼成は、160℃〜250℃で30〜120分の大気オーブン中で行われる請求項12に記載の導電性材料の製造方法。
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