JP2016000861A - 接合材料および接合体 - Google Patents
接合材料および接合体 Download PDFInfo
- Publication number
- JP2016000861A JP2016000861A JP2015146197A JP2015146197A JP2016000861A JP 2016000861 A JP2016000861 A JP 2016000861A JP 2015146197 A JP2015146197 A JP 2015146197A JP 2015146197 A JP2015146197 A JP 2015146197A JP 2016000861 A JP2016000861 A JP 2016000861A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- acid
- bonding material
- bonding
- joining
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 78
- 239000002245 particle Substances 0.000 claims abstract description 43
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000004332 silver Substances 0.000 claims abstract description 40
- 229910052709 silver Inorganic materials 0.000 claims abstract description 40
- 239000000126 substance Substances 0.000 claims abstract description 23
- 239000011164 primary particle Substances 0.000 claims abstract description 13
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 11
- 239000000194 fatty acid Substances 0.000 claims abstract description 11
- 229930195729 fatty acid Natural products 0.000 claims abstract description 11
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 11
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 10
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 33
- 239000002612 dispersion medium Substances 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- QEVGZEDELICMKH-UHFFFAOYSA-N Diglycolic acid Chemical compound OC(=O)COCC(O)=O QEVGZEDELICMKH-UHFFFAOYSA-N 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 239000011800 void material Substances 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 18
- 238000005304 joining Methods 0.000 abstract description 13
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- 238000006243 chemical reaction Methods 0.000 description 9
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- 230000000996 additive effect Effects 0.000 description 3
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
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- 238000007650 screen-printing Methods 0.000 description 1
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
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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
- B22F1/102—Metallic powder coated with organic material
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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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
- B23K1/0016—Brazing of electronic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B23K31/00—Processes relevant to this subclass, specially adapted for particular articles or purposes, but not covered by only one of the preceding main groups
- B23K31/02—Processes relevant to this subclass, specially adapted for particular articles or purposes, but not covered by only one of the preceding main groups relating to soldering or welding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- 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
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
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- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
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- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B23K2101/00—Articles made by soldering, welding or cutting
- B23K2101/36—Electric or electronic devices
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Abstract
【解決手段】炭素数8以下の脂肪酸で被覆され平均一次粒子径が1nm以上200nm以下の銀ナノ粒子と、平均粒子径が0.5μm以上10μm以下の銀粒子と、2以上のカルボキシル基を有する有機物質と、分散媒とを含む接合材料を提供する。
【選択図】図1
Description
炭素数8以下の脂肪酸で被覆され平均一次粒子径が10nm以上100nm以下の銀ナノ粒子と、平均粒子径が0.5μm以上10μm以下の銀粒子と、2以上のカルボキシル基を有する有機物質と、分散媒とを含む接合材料である。
前記2以上のカルボキシル基を有する有機物質が、エーテル結合を有する第1の発明に記載の接合材料である。
前記2以上のカルボキシル基を有する有機物質が、オキシジ酢酸である第1または第2の発明に記載の接合材料である。
前記銀ナノ粒子が、炭素数3以上6以下の脂肪酸で被覆されている第1ないし第3の発明のいずれかに記載の接合材料である。
複数の被接合部材が、金属として銀のみを含む接合層により接合された接合体であって、当該接合層に存在するボイド率が2.0%以下である接合体である。
本発明に係る接合材料を構成する銀ナノ粒子は、平均一次粒子径が200nm以下、好ましくは1〜150nm、一層好ましくは10〜100nmのものである。当該粒子径を有する銀ナノ粒子を使用することで、強い接合力を有した接合体を形成することができる。
還元性を有する物質を溶解させた還元液と、原料である金属塩(特に銀塩)が溶解された原料液とを準備する。
還元液と原料液とを昇温し、反応温度まで上昇させる。このとき、還元液と原料液とを、同様に加熱しておけば、反応時において反応の不均一が防止される効果があり、粒子の均一性を保つことができるので好ましい。このときに昇温させる温度は40〜80℃の範囲である。
還元液と原料液とが目的温度まで上昇したら、還元液に対して原料液を添加する。添加は突沸に注意した上で、一挙に添加することが好ましい。
還元液と原料液とを混合した後、10〜30分間程度攪拌を続け、粒子の成長を完結させる。
得られたスラリーは濾過法により固液分離する。洗浄工程は、当該濾過工程で得られたケーキに対して純水を加え、再び該純水を濾過することによって行う。本発明の製造法によれば、ナノオーダーの一次微粒子が緩やかな凝集体を形成し、反応液中に自然に沈降するため、容易に回収できる。
得られた金属(銀)塊へ60〜90℃、6〜24時間の乾燥工程を施すことで、乾燥した金属(銀)粒子塊が得られる。
銀ナノ粒子の粒子径は、透過型電子顕微鏡(TEM)写真から算出される。
具体的には、金属ナノ粒子2質量部を、シクロヘキサン96質量部とオレイン酸2質量部との混合溶液に添加し、超音波によって分散させて分散溶液を得る。得られた分散溶液を、支持膜付きCuマイクログリッドに滴下し、乾燥させることでTEM試料を作成する。作成したTEM試料であるマイクログリッドを、透過型電子顕微鏡(日本電子株式会社製JEM−100CXMark−II型)を用い、100kVの加速電圧にて、明視野で粒子を観察した像を、倍率300,000倍で撮影すれば良い。
本発明に係る接合材料を構成する銀粒子は、平均粒子径の範囲が0.5〜10μm、好ましくは0.5〜9.0μm、一層好ましくは0.5〜8.0μmの範囲の銀粒子である。銀粒子の形態については、特に制限はない。銀粒子の形態としては、球状、フレーク(鱗片)状、直方体状、立方体状、凝集体状といった様々な形態が使用できる。
本発明の接合材料は、有機物からなるフラックス成分(焼結促進成分)を添加することを特徴とする。ここでフラックス成分とは、具体的に述べれば、2以上のカルボキシル基を有する有機物質である。より好ましくは、さらにエーテル結合を有するジカルボン酸である。接合材料へ当該構成を有するフラックス成分を添加することにより、窒素を初めとした不活性雰囲気下における500℃以下の熱処理操作であっても、上述した有機物質で被覆された銀ナノ粒子を、バルク態の銀に変化させることが出来る。
本発明に係る接合材料を構成する分散媒は、銀ナノ粒子を分散させる観点から蒸気圧が低い極性溶媒とすることが好ましい。なお、この時分散媒は必ずしも一種類で構成する必要はなく、併用混合することも出来る。
上述した分散媒へ、銀ナノ粒子の焼結温度低下や密着の促進を図る添加剤や、粘度調整剤を添加することも好ましい構成である。
粘度調整剤の例としては、炭化水素溶剤、各種の脂肪酸、水溶化樹脂、水性分散樹脂、および無機バインダーがある。具体的には、ナフテン系炭化水素溶剤、オレイン酸、アクリル樹脂、マレイン酸樹脂、フマル酸樹脂、スチレン・マレイン酸共重合樹脂の高酸価樹脂、ポリエステル樹脂、ポリオレフィン樹脂、フェノキシ樹脂、ポリイミド樹脂、ポリアミド樹脂あるいは酢酸ビニル系エマルション、アクリルエマルション、合成ゴムラテックス、エポキシ樹脂、フェノール樹脂、DAP樹脂、ウレタン樹脂、フッ素樹脂、シリコーン樹脂、エチルセルロースおよびポリビニルアルコール等を添加することができる。無機バインダーの例としては、シリカゾル、アルミナゾル、ジルコニアゾル、チタニアゾルといったものを挙げることが出来る。
尤も、こうした粘度調整剤は、焼結性を改善する観点から添加量が少ない方が好ましい。そこで、当該粘度調整剤の添加剤の総量は、他成分との兼ね合いもあるが、ペーストの総質量に対して0.2〜2.0質量%、好ましくは0.3〜1.5質量%、一層好ましくは0.3〜1.0質量%とするのがよい。
本発明に係る接合材料の製造方法について説明する。当該混合物を混練脱泡機へ導入して混練し混練物を形成させる。その後、当該混練物へ機械的分散処理を行い本発明に係る接合材料を得る。
接合体の形成は、接合部が形成される一の被接合部材である基板表面へ、例えばメタルマスク、ディスペンサーまたはスクリーン印刷法により、20μm〜200μm程度の厚みで接合材料を塗布する。塗布後、低温による熱処理(以降、予備焼成という)を経た後、二の被接合部材である被接合物を貼付し、高温による熱処理工程(以降は、本焼成という。)により接合材料を金属化する。
<銀ナノ粒子の合成>
500mLビーカーを用い、硝酸銀(東洋化学株式会社製)13.4gを純水72.1gへ溶解させて原料液を調製した。
得られたソルビン酸が被覆された銀ナノ粒子凝集体乾燥粉(平均一次粒子径:100nm)45.0g(全銀中の割合は50.00質量%)を銀ナノ粒子粉とし、球状銀粒子の粉末(DOWAエレクトロニクス株式会社製 2−1C球状銀粉末:平均一次粒子径(D50)1.0μm)45.0g(全銀中の割合は50.00質量%)と、フラックスとしてオキシジ酢酸(和光純薬株式会社製:ジグリコール酸)0.05gと、分散媒としてオクタンジオール(協和発酵ケミカル社製:2−エチル−1,3−ヘキサンジオール)9.95gとを、混合し、混合物とした。
尚、オクタンジオールの沸点は244℃であり、引火点は135℃である。
メタルマスク(マスク厚50μmt)を準備し、銀めっきされた銅基板上にメタルスキージによる手印刷で、実施例1に係る接合材料(ペースト)を印刷法により塗布した。パターンは□5.5mm、50μm厚とした。
実施例1に係る接合材料の分散媒であるオクタンジオールの添加量を7.95gに変更し、さらに、粘度調整を目的としてEXXSOL D130 FLUID(エクソンモービル社製)を2.0g添加した以外は、実施例1と同様の製造工程を経て、実施例2に係る接合材料を製造した。そして、実施例1と同様の工程を経て、実施例2に係る接合体を形成し、実施例1と同様の評価を行った。評価結果を表1、2に示す。
実施例1に係る接合材料の銀粉を球状銀粒子から、フレーク銀粒子粉末(DOWAエレクトロニクス株式会社製FA−D−6:平均一次粒子径(D50)8.3μm)へ変更した以外は、実施例1と同様の製造工程を経て、実施例3に係る接合材料を製造した。そして、実施例1と同様の工程を経て、実施例3に係る接合体を形成し、実施例1と同様の評価を行った。評価結果を表1、2に示す。
実施例1に係る接合材料のソルビン酸が被覆された銀ナノ粒子凝集体乾燥粉(平均一次粒子径:100nm)から、ソルビン酸が被覆された銀ナノ粒子凝集体乾燥粉(平均一次粒子径:60nm)へ変更し、フラックスをオキシジ酢酸(和光純薬株式会社製:ジグリコール酸)0.1g、分散媒としてオクタンジオール(協和発酵ケミカル株式会社製:2−エチル−1,3−ヘキサンジオール)の添加量を9.9gと変更した以外は、実施例1と同様の製造工程を経て、実施例4に係る接合材料を製造した。そして、実施例1と同様の工程を経て、実施例4に係る接合体を形成し、実施例1と同様の評価を行った。評価結果を表1、2に示す。
実施例1に係る接合材料の分散媒であるオクタンジオールの添加量を7.45gに変更し、さらに、粘度調整を目的としてEXXSOL D130 FLUID(エクソンモービル社製)を2.0g添加し、さらに、粘度調整を目的としてオレイン酸(キシダ化学株式会社製)を0.5g添加した以外は、実施例1と同様の製造工程を経て、実施例5に係る接合材料を製造した。そして、実施例1と同様の工程を経て、実施例5に係る接合体を形成し、実施例1と同様の評価を行った。評価結果を表1、2に示す。
実施例1に係る接合材料を準備した。
そして、チップマウント前の予備焼成を実施せず、接合材料が塗布された銅基板にチップをマウントし、10MPaの加圧を施して、予備乾燥として100℃10分間加熱後、250℃まで昇温速度1℃/秒で昇温し、本焼成として250℃に達してから5分間保持することで、比較例1に係る接合体を形成し、実施例1と同様の評価を行った。評価結果を表1、2に示す。
実施例2に係る接合材料を用い、比較例1と同様の工程を経て、比較例2に係る接合体を形成し、実施例1と同様の評価を行った。評価結果を表1、2に示す。
実施例3に係る接合材料を用い、比較例1と同様の工程を経て、比較例3に係る接合体を形成し、実施例1と同様の評価を行った。評価結果を表1、2に示す。
図1に、実施例1〜3および比較例1〜3に係る接合体の接合強度を示す。図1は縦軸に接合強度(シェア強度)をとり、横軸に、実施例1−比較例1、実施例2−比較例2、実施例3−比較例3をとった棒グラフである。
実施例1−比較例1と、実施例2−比較例2と、実施例3−比較例3とは、接合材料として同組成のペーストを用い、実施例1〜3においてはチップマウント前の予備焼成を実施し、比較例1〜3においてはチップマウント前の予備焼成を実施しなかったものである。
図1より、チップマウント前の予備焼成を実施した実施例1〜3に係る接合体は、予備焼成を実施しなかった比較例1〜3に係る接合体より2.3〜6.2の接合強度を発揮することが判明した。
Claims (5)
- 炭素数8以下の脂肪酸で被覆され平均一次粒子径が10nm以上100nm以下の銀ナノ粒子と、平均粒子径が0.5μm以上10μm以下の銀粒子と、2以上のカルボキシル基を有する有機物質と、分散媒とを含む接合材料。
- 前記2以上のカルボキシル基を有する有機物質が、エーテル結合を有する請求項1に記載の接合材料。
- 前記2以上のカルボキシル基を有する有機物質が、オキシジ酢酸である請求項1または2に記載の接合材料。
- 前記銀ナノ粒子が、炭素数3以上6以下の脂肪酸で被覆されている請求項1ないし3のいずれかに記載の接合材料。
- 複数の被接合部材が、金属として銀のみを含む接合層により接合された接合体であって、当該接合層に存在するボイド率が2.0%以下である接合体。
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JP2018059192A (ja) * | 2016-09-30 | 2018-04-12 | Dowaエレクトロニクス株式会社 | 接合材およびそれを用いた接合方法 |
KR20190064605A (ko) * | 2016-09-30 | 2019-06-10 | 도와 일렉트로닉스 가부시키가이샤 | 접합재 및 그것을 사용한 접합 방법 |
KR102354209B1 (ko) | 2016-09-30 | 2022-01-20 | 도와 일렉트로닉스 가부시키가이샤 | 접합재 및 그것을 사용한 접합 방법 |
JP7007140B2 (ja) | 2016-09-30 | 2022-01-24 | Dowaエレクトロニクス株式会社 | 接合材およびそれを用いた接合方法 |
US12048964B2 (en) | 2016-09-30 | 2024-07-30 | Dowa Electronics Materials Co., Ltd. | Bonding material and bonding method using same |
WO2018124263A1 (ja) * | 2016-12-28 | 2018-07-05 | Dowaエレクトロニクス株式会社 | 接合材及びそれを用いた接合方法 |
JP2018109232A (ja) * | 2016-12-28 | 2018-07-12 | Dowaエレクトロニクス株式会社 | 接合材及びそれを用いた接合方法 |
JP2020113661A (ja) * | 2019-01-11 | 2020-07-27 | Jx金属株式会社 | 導電性塗布材料 |
JP2020113662A (ja) * | 2019-01-11 | 2020-07-27 | Jx金属株式会社 | 導電性塗布材料 |
JP2021195592A (ja) * | 2020-06-15 | 2021-12-27 | Jsr株式会社 | 組成物、銀焼結物の形成方法、接合方法、物品及び物品の製造方法 |
JP7443948B2 (ja) | 2020-06-15 | 2024-03-06 | Jsr株式会社 | 組成物、銀焼結物の形成方法、接合方法、物品及び物品の製造方法 |
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JP5986929B2 (ja) | 2016-09-06 |
CN103250236B (zh) | 2016-09-14 |
CN103250236A (zh) | 2013-08-14 |
US9486879B2 (en) | 2016-11-08 |
JP6214600B2 (ja) | 2017-10-18 |
EP2645408A1 (en) | 2013-10-02 |
KR102158290B1 (ko) | 2020-09-21 |
EP2645408A4 (en) | 2016-06-08 |
WO2012070262A1 (ja) | 2012-05-31 |
HUE043602T2 (hu) | 2019-08-28 |
KR20180004853A (ko) | 2018-01-12 |
EP2645408B1 (en) | 2019-02-27 |
KR20130129392A (ko) | 2013-11-28 |
US20130323529A1 (en) | 2013-12-05 |
KR20200067952A (ko) | 2020-06-12 |
KR102188054B1 (ko) | 2020-12-07 |
JPWO2012070262A1 (ja) | 2014-05-19 |
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