JP2018171636A - 接合用成形体及びその製造方法 - Google Patents
接合用成形体及びその製造方法 Download PDFInfo
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- JP2018171636A JP2018171636A JP2017071964A JP2017071964A JP2018171636A JP 2018171636 A JP2018171636 A JP 2018171636A JP 2017071964 A JP2017071964 A JP 2017071964A JP 2017071964 A JP2017071964 A JP 2017071964A JP 2018171636 A JP2018171636 A JP 2018171636A
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- molded body
- bonding
- core
- activator
- precursor
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- 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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- B22F1/17—Metallic particles coated with metal
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Abstract
Description
図1に示すように、本発明の第1の実施形態の接合用成形体1は、CuコアSnシェル粉末2をプレス成形して厚さ20〜400μmのペレット状又はシート状に作製される。
接合用成形体の原料となるCuコアSnシェル粉末2は、図1(a)の拡大図に示すように、Cuからなるコア2aと、このコア2aを被覆するSnからなるシェル2bとにより構成される。このCuコアSnシェル粉末2の平均粒径は0.5〜50μm、好ましくは1.0〜20μmである。平均粒径が下限値である0.5μm未満では、プレス成形又は後述するロール圧延成形をする際に、均一な密度の成形体前駆体を作ることが困難であるだけでなく、25℃などの通常の材料を取り扱う温度下では二層構造粒子のCuとSn界面でCuの拡散が数時間で進行することが知られており、接合加熱時にSn液相が生成する前の昇温途中で外殻のSnのほぼ全量がCu6Sn5となってしまい、接合性能が悪化する不具合がある。一方、平均粒径が上限値の50μmを超えると、接合加熱時にSnが溶融し一体化しやすくなるが、CuとSnが相互拡散して金属間化合物を形成するのに多くの時間を必要とし、本発明の効果の一つである短時間接合が実現できなくなる不具合がある。また、二層構造の粉末の中心に配置されるCuの粒径より薄い成形体前駆体を得る場合には、外殻のSnだけでなくCuも変形させる必要があるが、CuはSnより硬く変形しにくいため、平均粒径が上限値の50μmを超えると、最表面にCuが露出して、Cuが酸化して濡れ性が悪くなり、また表面部のSnの存在割合が減少するため、接合に関与する液相のSnが接合面に出にくく、接合性を悪化させる不具合がある。ここで、粉末の平均粒径(体積基準)はレーザー回折散乱法(堀場製作所社製、LA960)により測定した値である。
図1(b)及び(c)に示すように、窒素、アルゴンのような不活性ガス雰囲気下、CuコアSnシェル粉末2を一軸プレス機10でプレス成形を行って成形体前駆体3を作製する。一軸プレス機10は、金型となるダイ10a、上パンチ10b及び下パンチ10cを有する。この一軸プレス機10により、成形体前駆体3を製造するには、先ずダイ10aに下パンチ10cを組み合わせた状態で、CuコアSnシェル粉末2を所定量秤量し、ダイ10aの上パンチ挿入孔から下パンチ10c上に投入する(図1(b))。図示しないが、治具でCuコアSnシェル粉末2を上からタッピングして略均等な厚さとする。次に上パンチ10bをダイ10aに挿入して下降させる(図1(c))。この上パンチ10bの加圧力により、CuコアSnシェル粉末2は変形して、粉末間の絡み合いや接着が起こって独立した成形体前駆体3になる。このようにして、一軸プレス機10でCuコアSnシェル粉末2を一軸プレスして20〜400μmの所定の厚さとなるように成形する。成形圧力は、CuコアSnシェル粉末2の粒径や組成で変化するため、それぞれの微細粉末の粒径、組成、形状に応じた圧力とするため、個別に限定することができないが、10〜1000MPaの範囲でプレス成形する。このとき、成形体前駆体3の断面を観察してCuとSnの金属成分以外から構成される空隙部の面積が5%〜0.1%となるように投入粉末量を決定し、上記所定の厚さとなるように圧力調整する。図示しないが、上記空隙部は閉空孔及び開空孔から構成される。圧縮された集合体である成形体前駆体中、コアのCuを符号2aで示す(図1(c))。
図1(e)に示すように、成形体前駆体内部の粉末表面の酸化物を除去するための液状の活性剤含有物4を容器5に貯える。なお、液状の活性剤含有物の粘度は10-2〜10Pa・sに調整する。窒素、アルゴンのような不活性ガス雰囲気下、貯えた活性剤含有物4中に、上記得られた成形体前駆体3を浸漬する。活性剤含有物4は、活性剤成分を含有するフラックスであるか、又は活性剤成分を含有する溶剤である。活性剤としては、ハロゲン化水素酸アミン塩が好ましく、具体的には、トリエタノールアミン、ジフェニルグアニジン、エタノールアミン、ブチルアミン、アミノプロパノール、ポリオキシエチレンオレイルアミン、ポリオキシエチレンラウレルアミン、ポリオキシエチレンステアリルアミン、ジエチルアミン、トリエチルアミン、メトキシプロピルアミン、ジメチルアミノプロピルアミン、ジブチルアミノプロピルアミン、エチルヘキシルアミン、エトキシプロピルアミン、エチルヘキシルオキシプロピルアミン、ビスプロピルアミン、イソプロピルアミン、ジイソプロピルアミン、ピペリジン、2,6−ジメチルピペリジン、アニリン、メチルアミン、エチルアミン、ブチルアミン、3−アミノ−1−プロペン、イソプロピルアミン、ジメチルヘキシルアミン、シクロヘキシルアミン等のアミンの塩化水素酸塩又は臭化水素酸塩が挙げられる。この中でシクロヘキシルアミン臭化水素酸塩が好ましい。
窒素、アルゴンのような不活性ガス雰囲気下、上記活性剤含有物中に浸漬した成形体前駆体3を容器5とともに減圧する。減圧(真空度)は、活性剤含有物の粘度や活性剤含有物に使用される溶剤の蒸気圧に応じて変化させるが、活性剤含有物に用いられる溶剤のうち25℃における蒸気圧が最も高い値に対して2倍以上の真空度で、0.1〜5kPaの範囲に設定し、この減圧下で成形体前駆体から気体発生が認められなくなるまでの時間、30〜600秒間保持する。これにより、成形体前駆体3内部の開空孔に存在する気体を膨張させ、開空孔から脱気する。真空度及び減圧時間が上記範囲の下限値未満では上記脱気が十分に行われない。真空度及び減圧時間が上記範囲の上限値を超えた場合には、蒸気圧の高い溶媒が揮発して開空孔内に充填させる活性剤含有物の組成が大きくずれて、期待する酸化防止や表面酸化膜除去の機能が発揮されない不具合がある。上記減圧を行った後で、上記不活性ガス雰囲気下のまま、容器5とともに活性剤含有物中に浸漬した成形体前駆体3を常圧に300〜1200秒間かけて復圧する。これにより、活性剤含有物4が成形体前駆体3内部の開空孔に充填される。復圧して開空孔に活性剤含有物を充填した後、成形体前駆体を容器から取り出し、不活性ガス雰囲気下、成形体前駆体の表面に付着した活性剤含有物を拭き取って除去し、必要により乾燥することにより、図1(f)に示される接合用成形体1が得られる。
図2に示すように、本発明の第2の実施形態の接合用成形体6は、第1の実施形態と同一のCuコアSnシェル粉末2(図2(a))をロール圧延成形して厚さ20〜400μmのシート状又はペレット状に作製される。
図2(b)に示すように、窒素、アルゴンのような不活性ガス雰囲気下、CuコアSnシェル粉末2を粉末圧延機20で粉末ロール圧延成形を行って成形体前駆体7を作製する。粉末圧延機20は一対の円柱状のロール20a、20bとこれらのロール上面に接して設けられたホッパー20cを有する。ロール20aとロール20bは互いに逆方向に回転し、図2ではホッパー20cに投入されるCuコアSnシェル粉末2を下方に圧延し、圧延体はガイドローラ20d〜20gで水平方向に案内されるように構成される。ロール圧延時の圧力は、線圧となり、実際に圧延成形されるCuコアSnシェル粉末に印加される圧力の確認及び管理が難しいため、圧力は限定することができないが、第1の実施形態の一軸プレス成形と同様に成形体前駆体7が20〜400μmの所定の厚さとなるようにロール間ギャップを調整するとともに成形体前駆体7の断面を観察して空隙部が5%〜0.1%になるようにホッパー20cによるCuコアSnシェル粉末2の投入量を調整する。図示しないが、上記空隙部は閉空孔及び開空孔から構成される。圧縮された集合体である成形体前駆体中、コアのCuを符号2aで示す(図2(b))。
第2の実施形態の活性剤含有物は、第1の実施形態の活性剤含有物と同一であり、また図2(d)及び(e)に示すように、ロール圧延成形後の成形体前駆体の活性剤含有物中への浸漬方法及び成形体前駆体内部の開空孔への活性剤含有物の充填方法は、第1の実施形態と同様であるため、繰返しの説明を省略する。このようにして、第2の実施形態の接合用成形体6が得られる。図2(d)及び(e)において、各要素の符号は、図1(e)及び(f)に示した要素に付した符号と同一である。
次に上記第1及び第2の実施形態の方法で製造された接合用成形体を用いてシリコンチップ素子を銅板の基板に接合して、シリコンチップ素子を基板に実装する一例について説明する。先ず上記接合用成形体を銅板上に配置し、接合用成形体の上に2.5mm□の裏面をAuスパッタしたシリコンチップ素子を搭載する。次に接合炉、例えばマルコム社製、SRS−1Cを用い、窒素ガス雰囲気下で、0.1〜100MPaの荷重を加えながら、最高温度250〜350℃条件で1〜15分間加熱保持処理する。この接合加熱により接合用成形体中の活性剤が粉末の外殻のSn層の酸化物を除去することにより、Snが短時間で溶融し、CuとSnの相互拡散によりコアのCuを囲むようにCu−Snの金属間化合物(IMC)が形成されて、シリコンチップ素子と銅板とが高い接合強度で接合する。
平均粒径が0.5μmであって、Cu割合が75質量%かつSnの割合が25質量%のCuコアSnシェル粉末を用意した。ここでCuコアSnシェル粉末のCuとSnの組成割合は、ICP発光分光法(Thermo Fisher Scientific社製、iCAP-6500 Duo)により測定した。またコアシェル構造の結晶構造が主としてCu及びSnから構成されることは、粉末X線回折法(PANalytical社製、多目的X線回折装置Empyrean)により確認した。上記CuコアSnシェル粉末を金型を用いて500MPaで300秒間一軸プレスし、厚さ100μmで3mm□のペレット状の成形体前駆体を得た。
実施例2〜5及び比較例1、2では、表1に示すように、接合用成形体を作製するためのCuコアSnシェル粉末の平均粒径について、実施例1とは異なる平均粒径のCuコアSnシェル粉末を用いて、実施例1と同様にして接合用成形体を得た。
実施例6〜9及び比較例3、4では、表1に示すように、接合用成形体を作製するためのCuコアSnシェル粉末のCuとSnの組成について、実施例1とは異なるCuとSnの組成のCuコアSnシェル粉末を用いて、実施例1と同様にして接合用成形体を得た。
実施例10〜13及び比較例5、6では、表1に示すように、接合用成形体を作製するときの一軸プレス成形するときの成形荷重について、実施例1とは異なる成形荷重で、実施例1と同様にして接合用成形体を得た。荷重を加えた時間は実施例1と同一の300秒間であった。
実施例14〜17及び比較例7、8では、表2に示すように、CuコアSnシェル粉末の金型に投入する量を変えて、得られる接合用成形体の厚さについて、実施例1とは厚さになるようにした。それ以外は、実施例1と同様にして接合用成形体を得た。
実施例18〜22及び比較例9、10では、表2に示すように、成形方法をロール圧延成形に変更し、粉末圧延機のロール間ギャップを調整して、得られる接合用成形体の厚さについて、実施例1とは厚さになるようにした。それ以外は、実施例1と同様にして接合用成形体を得た。
実施例1〜22及び比較例1〜10で得られた32種類の接合用成形体をそれぞれ銅板上に載せ、ここに裏面をAuスパッタした2.5mm□のシリコンチップ素子を搭載した。シリコンチップ素子に1MPaの荷重を加えて銅板に密着させた状態で、リフロー炉を用いて、窒素雰囲気下、最高温度300℃で5分間保持して、銅板とシリコンチップ素子を接合し、32種類の接合サンプルを得た。これらの接合サンプルについて、次に述べる方法により、初期接合強度試験と冷熱サイクル試験を行い、評価した。その評価結果を表1及び表2に示す。
接合強度はダイシェアテスタ(エー・アンド・デイ社製、テンシロン万能試験機RTF−1310)により、32種類の接合サンプルの銅板をそれぞれ固定し、シリコンチップ素子側面から銅板と平行方向に力を加え、シリコンチップ素子が剥がれる際の力又は破壊された際の力(単位はニュートン、N)を計測し、この値を接合面積2.5mm×2.5mm=6.25mm2で除した値を接合強度(単位はMPa)とした。
32種類の接合サンプルを冷熱サイクル試験機(エスペック社製、冷熱衝撃試験装置TSA―73ES)にそれぞれ入れ、下限温度−40℃、上限温度200℃に設定し、降温と昇温を1000回繰り返し、上記(1)の初期接合強度と同様の方法で接合強度を測定し、初期接合強度で除したものを冷熱サイクル特性とした。これは1.00であれば初期強度を維持したことを意味し、0.50であれば初期強度の半分に低下していることを意味する。
2 CuコアSnシェル粉末
2a コア(Cu)
2b シェル(Sn)
3、7 成形体前駆体
4 活性剤含有物
Claims (2)
- CuコアSnシェル粉末の圧縮された集合体により構成された接合用成形体であって、
前記接合用成形体の表面部及び内部の開空孔に前記粉末表面の酸化物を除去するための活性剤含有物が存在し、
前記接合用成形体がCuを55〜95質量%の割合でかつSnを45〜5質量%の割合でそれぞれ含有し、
前記接合用成形体が20〜400μmの厚さを有することを特徴とする接合用成形体。 - 不活性ガス雰囲気下、平均粒径が0.5〜50μmのCuコアSnシェル粉末を10〜1000MPaの圧力でプレス成形又はロール圧延成形して厚さ20〜400μmのペレット状又はシート状の成形体前駆体を得る工程と、
不活性ガス雰囲気下、前記粉末表面の酸化物を除去するための液状の活性剤含有物を容器に貯えて前記活性剤含有物中に前記成形体前駆体を浸漬する工程と、
不活性ガス雰囲気下、前記浸漬した成形体前駆体を前記容器とともに減圧して前記成形体前駆体内部の開空孔から前記開空孔に存在する気体を脱気する工程と、
不活性ガス雰囲気下、前記開空孔から気体を脱気した前記成形体前駆体を常圧に復圧して前記開空孔に活性剤含有物を充填する工程と、
前記開空孔に活性剤含有物が充填された成形体前駆体の表面に付着した余剰の活性剤含有物を除去して接合用成形体を得る工程とを含み、
前記CuコアSnシェル粉末がCuを55〜95質量%の割合でかつSnを45〜5質量%の割合でそれぞれ含有することを特徴とする接合用成形体の製造方法。
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