JPWO2011048765A1 - 半導体封止用エポキシ樹脂組成物、半導体装置及び離型剤 - Google Patents
半導体封止用エポキシ樹脂組成物、半導体装置及び離型剤 Download PDFInfo
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- JPWO2011048765A1 JPWO2011048765A1 JP2011537117A JP2011537117A JPWO2011048765A1 JP WO2011048765 A1 JPWO2011048765 A1 JP WO2011048765A1 JP 2011537117 A JP2011537117 A JP 2011537117A JP 2011537117 A JP2011537117 A JP 2011537117A JP WO2011048765 A1 JPWO2011048765 A1 JP WO2011048765A1
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- H01L2924/19041—Component type being a capacitor
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Abstract
Description
このような状況下、従来の未酸化の銅表面に対する接着性が優れている半導体封止材でも、表面状態の異なる酸化銅に対しては接着性が劣る場合が多く、樹脂封止後の型抜き時や半田リフロー時に剥離を起こす問題が出てきている。
剥離を抑制するためのインサート品と封止材樹脂との接着性は、金型に対する離型性と相反する指標であるため、接着性を向上させると離型性が劣り、成形性が低下するといった問題があった。電子部品の高集積化による、銅フレームの酸化が問題になる以前は接着性と離型性を両立するために、酸化ポリエチレンワックス及び、αオレフィンとマレイン酸との共重合体の半エステル化物を離型剤として添加する手法が提案されている。(例えば、特許文献1、2参照。)この手法によれば、未酸化の銅に対する接着性と離型性には優れるものの、酸化ポリエチレンワックスを併用しているため、酸化された銅フレームに対する封止樹脂の接着力が低下する問題点があった。またαオレフィン部分が炭素原子25個分以下と短い共重合体離型剤(例えば、特許文献3参照。)では連続成形性(エアベントブロック等の離型性)が劣る問題点があった。
[1]
(A)エポキシ樹脂、
(B)硬化剤、
(C)無機充填材、及び
離型剤、を含有し、
前記離型剤は、(D)炭素数28〜60のα−オレフィンと無水マレイン酸との共重合体を、炭素数10〜25の長鎖脂肪族アルコールでエステル化した化合物を含有する、半導体封止用エポキシ樹脂組成物。
[2]
更に下記一般式(I)で示される、シロキサン付加重合体変性物を含む、[1]に記載の半導体封止用エポキシ樹脂組成物。
[3]
前記(D)炭素数28〜60のα−オレフィンと無水マレイン酸との共重合体を、炭素数10〜25の長鎖脂肪族アルコールでエステル化した化合物の含有量が、前記離型剤の総量100質量%に対して、55質量%以上100質量%以下である、[1]または[2]に記載の半導体封止用エポキシ樹脂組成物。
[4]
前記シロキサン付加重合体変性物の含有量が、前記半導体封止用エポキシ樹脂組成物の総量100質量%に対して、0.1質量%以上2質量%以下である、[2]に記載の半導体封止用エポキシ樹脂組成物。
[5]
前記(A)エポキシ樹脂が、ビフェニル型エポキシ樹脂、パラキシリレン型エポキシ樹脂、及びビフェニレン骨格を有するフェノールアラルキル型エポキシ樹脂からなる群から選択される少なくとも一種を含む、[1]から[4]のいずれか1項に記載の半導体封止用エポキシ樹脂組成物。
[6]
銅含有リードフレームを備える半導体装置における半導体素子の封止に用いる、[1]から[5]のいずれか1項に記載の半導体封止用エポキシ樹脂組成物。
[7]
[1]から[6]のいずれか1項に記載の半導体封止用エポキシ樹脂組成物の硬化物で、半導体素子が封止されていることを特徴とする半導体装置。
[8]
(D)炭素数28〜60のα−オレフィンと無水マレイン酸との共重合体を、炭素数10〜25の長鎖脂肪族アルコールでエステル化した化合物を含有する、離型剤。
[9]
半導体封止用エポキシ樹脂組成物に用いる、[8]に記載の離型剤。
[10]
前記半導体封止用エポキシ樹脂組成物は、銅含有リードフレームを備える半導体装置における半導体素子の封止に用いる、[9]に記載の離型剤。
以下、各成分について詳述する。
本発明において用いられる(A)エポキシ樹脂としては、半導体封止用エポキシ樹脂組成物に一般に使用されているもので特に制限はないが、例えば、フェノールノボラック型エポキシ樹脂、オルソクレゾールノボラック型エポキシ樹脂をはじめとするフェノール、クレゾール、キシレノール、レゾルシン、カテコール、ビスフェノールA、ビスフェノールF等のフェノール類及び/又はα−ナフトール、β−ナフトール、ジヒドロキシナフタレン等のナフトール類とホルムアルデヒド、アセトアルデヒド、プロピオンアルデヒド、ベンズアルデヒド、サリチルアルデヒド等のアルデヒド基を有する化合物とを酸性触媒下で縮合又は共縮合させて得られるノボラック樹脂をエポキシ化したもの、ビスフェノールA、ビスフェノールF、ビスフェノールS、ビスフェノールA/D等のジグリシジルエーテル、アルキル置換又は非置換のビフェノールのジグリシジルエーテルであるビフェニル型エポキシ樹脂、フェノール類及び/又はナフトール類とジメトキシパラキシレン又はビス(メトキシメチル)ビフェニルから合成されるフェノールアラルキル樹脂のエポキシ化物、スチルベン型エポキシ樹脂、ハイドロキノン型エポキシ樹脂、フタル酸、ダイマー酸等の多塩基酸とエピクロルヒドリンの反応により得られるグリシジルエステル型エポキシ樹脂、ジアミノジフェニルメタン、イソシアヌル酸等のポリアミンとエピクロルヒドリンの反応により得られるグリシジルアミン型エポキシ樹脂、ジシクロペンタジエンとフェノ−ル類の共縮合樹脂のエポキシ化物であるジシクロペンタジエン型エポキシ樹脂、ナフタレン環を有するエポキシ樹脂、トリフェノールメタン型エポキシ樹脂、トリメチロールプロパン型エポキシ樹脂、テルペン変性エポキシ樹脂、オレフィン結合を過酢酸等の過酸で酸化して得られる線状脂肪族エポキシ樹脂、脂環族エポキシ樹脂、及びこれらのエポキシ樹脂をシリコーン、アクリロニトリル、ブタジエン、イソプレン系ゴム、ポリアミド系樹脂等により変性したエポキシ樹脂などが挙げられ、これらを単独で用いても2種以上を組み合わせて用いてもよい。
本発明に係る(A)エポキシ樹脂の含有量は、半導体封止用エポキシ樹脂組成物の総量100質量%に対して、とくに限定されないが、0.8質量%以上12質量%以下であることが好ましく、1.5質量%以上10質量%以下であることがより好ましい。
中でも、低粘度化、低吸湿性の観点から、下記一般式(V)で示されるビフェニレン骨格を有するフェノールアラルキル樹脂が好ましい。
本発明に係る硬化剤(B)の含有量は、特に限定されるものではないが、半導体封止用エポキシ樹脂組成物の総量100質量%に対して、0.8質量%以上12質量%以下であることが好ましく、1.5質量%以上10質量%以下であることがより好ましい。
(C)無機充填剤の配合量は、成形性、吸湿性、線膨張係数の低減及び強度向上の観点から、半導体封止用エポキシ樹脂組成物の総量100質量%に対して80質量%以上が好ましく、82〜96質量%の範囲がより好ましく、86〜92質量%がさらに好ましい。下限値未満では信頼性が低下する傾向があり、上限値を超えると成形性が低下する傾向がある。
(D)化合物に用いられるα−オレフィンの炭素数が下限値未満では、連続成形性(離型性)が劣り、上限値を超えると酸化銅に対する接着性が低下する。
(D)化合物に用いられる一価のアルコールの炭素数が下限値未満では、連続成形性(離型性)が劣り、上限値を超えると酸化銅に対する接着性が低下する。
(D)化合物には、未反応のα−オレフィンを0〜33質量%含んでも連続成形性及び酸化銅に対する接着性は変化しないが、含有量が上限値を超えると成形品表面の汚れ(パッケージ汚れ)が顕著になる傾向がある。
(D)化合物の配合量は、特に制限はないが、(A)エポキシ樹脂の総量100質量%に対して0.5〜10質量%が好ましく、1〜5質量%がより好ましい。配合量が下限値未満では離型性が低下する傾向があり、上限値を超えると、酸化銅に対する接着性が不十分となる傾向がある。
また、(D)化合物の含有量は、離型剤の総量100質量%に対して、特に限定されないが、55質量%以上100質量%以下が好ましい。このような範囲とすることにより、良好な酸化銅に対する接着性と離型性が実現できる。
Mg1−XAlX(OH)2(CO3)X/2・mH2O (VIII)
(0<X≦0.5、mは正の整数)
陰イオン交換体の配合量は、ハロゲンイオン等のイオン性不純物を捕捉できる十分な量であれば特に制限はないが、(A)エポキシ樹脂の総量100質量%に対して0.1〜30質量%が好ましく、1〜10質量%がより好ましく、2〜5質量%がさらに好ましい。配合量が下限値未満ではイオン性不純物の捕捉が不十分になる傾向があり、上限値を超えた場合それ以下に比べて効果に大差がないため経済的に不利である。
上記カップリング剤の配合量は、(C)無機充填剤の総量100質量%に対して0.05〜5質量%であることが好ましく、0.1〜2.5質量%がより好ましい。下限値未満では耐湿性が低下する傾向があり、上限値を超えるとパッケージの成形性が低下する傾向がある。
また、本発明の半導体封止用エポキシ樹脂組成物は、各種有機溶剤に溶かして液状半導体封止用エポキシ樹脂組成物として使用することもでき、この液状半導体封止用エポキシ樹脂組成物を板又はフィルム上に薄く塗布し、樹脂の硬化反応が余り進まないような条件で有機溶剤を飛散させることによって得られるシートあるいはフィルム状の半導体封止用エポキシ樹脂組成物として使用することもできる。
図1は、本発明に係る半導体封止用エポキシ樹脂組成物を用いた半導体装置の一例について、断面構造を示した図である。ダイパッド3上に、ダイボンド材硬化体2を介して半導体素子1が2段に積層されて固定されている。半導体素子1の電極パッドと銅リードフレーム5との間は金線4によって接続されている。半導体素子1は、封止用樹脂組成物の硬化体6によって封止されている。銅リードフレーム5としては、半導体装置の技術分野において一般的に使用される汎用の銅含有リードフレームが好ましい。この銅含有リードフレームとしては、銅を含む限り特に限定されず、少なくとも表面に銅を含むリードフレームや、銅合金のリードフレームまたは銅からなるリードフレームなどが好ましい。
また、素子を直接樹脂封止する一般的な封止方法ばかりではなく、素子に直接半導体封止用エポキシ樹脂組成物が接触しない形態である中空パッケージの方式もあり、中空パッケージ用の半導体封止用エポキシ樹脂組成物としても好適に使用できる。
また、本発明の半導体封止用エポキシ樹脂組成物は、酸化銅に対する接着性、離型性、連続成形性等に優れ、この半導体封止用エポキシ樹脂組成物を用いてIC、LSI等の電子部品を封止すれば信頼性に優れた半導体装置を得ることができる。
1−オクタコセン、1−トリアコンテン、1−テトラコンテン、1−ペンタコンテン、1−ヘキサコンテン等の混合物と無水マレイン酸との共重合物(三菱化学株式会社製、商品名ダイヤカルナ(登録商標)30)、300g及びステアリルアルコール、140gをトルエン、500mlに溶解して110℃で8時間反応させた後、160℃まで段階的に昇温しながらトルエンを除去し、減圧下160℃で6時間反応を行うことにより未反応成分を除去し、目的のモノエステル化率100モル%の化合物1、489gを得た。分子量は、テトラヒドロフランを溶離液として、ポリスチレン換算のゲル浸透クロマトグラフィーにより測定したところ、数平均分子量(Mn)=4100、分子量分布(Mw/Mn)=3.52であり、未反応のステアリルアルコール残留量は化合物1全体の1%以下であった。
ステアリルアルコールの代わりに1−ドデカノール97gを添加したことを除いては合成例1に記載の方法によって、モノエステル化率100モル%の化合物2、385gを得た。分子量は、テトラヒドロフランを溶離液として、ポリスチレン換算のゲル浸透クロマトグラフィーにより測定したところ、数平均分子量(Mn)=3800、分子量分布(Mw/Mn)=3.81であり、未反応の1−ドデカノール残留量は化合物2全体の1%以下であった。
ステアリルアルコールの代わりにベヘニルアルコール(花王株式会社製、商品名カルコール220−80)170gを添加したことを除いては合成例1に記載の方法によって、モノエステル化率100モル%の化合物3、458gを得た。分子量は、テトラヒドロフランを溶離液として、ポリスチレン換算のゲル浸透クロマトグラフィーにより測定したところ、数平均分子量(Mn)=4400、分子量分布(Mw/Mn)=3.55であり、未反応のベヘニルアルコール残留量は化合物3全体の1%以下であった。
1−エイコセン、1−ドコセン、1−テトラコセンの混合物(出光興産株式会社製、商品名リニアレン2024)、180gと無水マレイン酸、58gをトルエン、500mlに溶解し、110℃で加熱しながら20分毎にBPO、0.16gを3回に分けて添加した。BPOを添加終了後、反応溶液をさらに7時間110℃で加熱した。この共重合物のトルエン溶液にステアリルアルコール162gを添加して110℃で8時間反応させた後、160℃まで段階的に昇温しながらトルエンを除去し、減圧下160℃で6時間反応を行うことにより未反応成分を除去し、目的のモノエステル化率100モル%の化合物4、380gを得た。分子量は、テトラヒドロフランを溶離液として、ポリスチレン換算のゲル浸透クロマトグラフィーにより測定したところ、数平均分子量(Mn)=9800、分子量分布(Mw/Mn)=2.63であり、未反応のステアリルアルコール残留量は化合物4全体の1%以下であった。
ステアリルアルコールの代わりに1−オクタノール、68gを添加したことを除いては合成例1に記載の方法によって、モノエステル化率100モル%の化合物5、340gを得た。分子量は、テトラヒドロフランを溶離液として、ポリスチレン換算のゲル浸透クロマトグラフィーにより測定したところ、数平均分子量(Mn)=3700、分子量分布(Mw/Mn)=3.80であり、未反応の1−オクタノール残留量は化合物5全体の1%以下であった。
ステアリルアルコールの代わりにオクタコサノール(株式会社素材機能研究所製、商品名ポリコサノール(米糠由来))、214gを添加したことを除いては合成例1に記載の方法によって、モノエステル化率100モル%の化合物6、506gを得た。分子量は、テトラヒドロフランを溶離液として、ポリスチレン換算のゲル浸透クロマトグラフィーにより測定したところ、数平均分子量(Mn)=4800、分子量分布(Mw/Mn)=3.91であり、未反応のオクタコサノール残留量は化合物6全体の1%以下であった。
(A)成分のエポキシ樹脂:
エポキシ当量185、融点108℃のビフェニル型エポキシ樹脂(ジャパンエポキシ株式会社製、商品名エピコートYX−4000K)、
エポキシ当量237、軟化点52℃のパラキシリレン型エポキシ樹脂(日本化薬社製、商品名NC2000)、
エポキシ当量273、軟化点52℃のビフェニレン骨格を有するフェノールアラルキル型エポキシ樹脂(ビフェニルアラルキル型エポキシ樹脂と略す)(日本化薬社製、商品名NC−3000L)
(B)成分の硬化剤:
水酸基当量199、軟化点64℃のビフェニレン骨格を有するフェノールアラルキル型フェノール樹脂(ビフェニルアラルキル樹脂と略す)(明和化成株式会社製、商品名MEH−7851SS)
(C)成分の無機充填剤:
平均粒径10.8μm、比表面積5.1m2/gの球状溶融シリカ(電気化学工業株式会社製、商品名デンカ溶融シリカ(DF)球形粉末タイプ(グレード FB-105))
(D)成分の離型剤:
上記合成例で得られた化合物1〜6、その他の離型剤として酸化ポリエチレンワックス(クラリアント社製、商品名PED191)、モンタン酸系ワックス(クラリアント社製、商品名リコワックスE)、α−オレフィンモノマー(Chevron Phillips Chemical Company製、商品名Alpha Olefin C30+)
(E)成分の硬化促進剤:
トリフェニルホスフィンとp−ベンゾキノンとの付加物(北興化学株式会社製、商品名TPP−BQ)
シロキサン付加重合体変性物:
シリコーンオイルA(下記式(IX)で表される化合物(東レ・ダウコーニング株式会社製、BY−750、分子量約1500)とビスフェノールA型エポキシ樹脂(ジャパンエポキシレジン株式会社製、JER(登録商標)YL−6810(エポキシ当量172g/eq、融点45℃)12質量部を140℃で加温溶融し、G1−1を6質量部、トリフェニルホスフィンを0.15質量部添加して、140℃にて30分間溶融混合して得た溶融反応物)
着色剤:カーボンブラック(三菱化学株式会社製、商品名カーボン#5)
上記成分をそれぞれ表1及び表2に示す質量部で配合し、混練温度100℃、混練時間30分の条件で二軸混練して冷却後粉砕し、半導体封止用エポキシ樹脂組成物を作製した。なお比較例4及び5の化合物1及び化合物4と酸化ポリエチレンワックスはビフェニル型エポキシ樹脂と170℃、6時間の条件で予備混練して用いた。
(1)接着性
酸化銅基材とタブレット化した半導体封止用エポキシ樹脂組成物を175℃、70kg/cm2、2分の条件で一体成形して切頭体状の成形品(上径2mm×下径3mm×厚さ3mm)を得た後、得られた各成形品の基材を固定し、半導体封止用エポキシ樹脂組成物の硬化部位を横方向から押し、そのトルク(N)を測定した。
(2)離型荷重
離型時荷重評価用金型は、トランスファー成形型として上型、中型、下型からなる。図2に成形後の中型の平面概略図を示した。成形後に中型に付着する成形品の形状は、直径14.0mm、高さ1.5mm厚である。図2において、11は中型を示し、12はカルを示し、13はランナーを示す。14は成形品を示し、15はエアベントを示す。16は取っ手、17はプッシュプルゲージ挿入用の穴を、それぞれ示す。
図2に示す離型時荷重評価用金型を用いて金型温度175℃、注入圧力6.9MPa、硬化時間1分で評価用材料をトランスファー成形した。成形後に中型11に付着した円形の成形品14に、中型の上部の穴17からプッシュブルゲージを当て(図3参照)、成形品を突き出した際にかかる荷重を測定した。続けて評価用材料を20ショット成形した後半の10ショットの成形品について測定を行い、その平均値を離型荷重として評価した。
(3)連続成形性(エアベントブロック、型汚れ及びパッケージ汚れ)
低圧トランスファー自動成形機(第一精工株式会社製、GP−ELF)を用いて、金型温度175℃、注入圧力9.8MPa、硬化時間70秒で、80ピンクワッドフラットパッケージ(80pQFP;Cu製リードフレーム、パッケージ外寸:14mm×20mm×2mm厚、パッドサイズ:6.5mm×6.5mm、チップサイズ6.0mm×6.0mm×0.35mm厚)を、連続で400ショットまで封止成形した。
エアベントブロックは50ショット毎に金型を目視により観察することで、エアベントブロックの有無を確認し、次の4段階で評価した。
A:400ショットまで問題なし
B:300ショットまでにエアベントブロック発生
C:200ショットまでにエアベントブロック発生
D:100ショットまでにエアベントブロック発生
型汚れについては、400ショットの金型を観察し、ゲート口からの汚れの広がり具合の程度から、次の5段階に評価した。
A:汚れなし
B:汚れの広がりがパッケージ表面の10面積%以下
C:汚れの広がりがパッケージ表面の10面積%超〜20面積%以下
D:汚れの広がりがパッケージ表面の20面積%超〜50面積%以下
E:汚れの広がりがパッケージ表面の50面積%超
パッケージ汚れについては400ショットのパッケージを観察し、ゲート口からの汚れの広がり具合の程度から、次の5段階に評価した。
A:汚れなし
B:汚れの広がりがパッケージ表面の10面積%以下
C:汚れの広がりがパッケージ表面の10面積%超〜20面積%以下
D:汚れの広がりがパッケージ表面の20面積%超〜50面積%以下
E:汚れの広がりがパッケージ表面の50面積%超
Claims (10)
- (A)エポキシ樹脂、
(B)硬化剤、
(C)無機充填材、及び
離型剤、を含有し、
前記離型剤は、(D)炭素数28〜60のα−オレフィンと無水マレイン酸との共重合体を、炭素数10〜25の長鎖脂肪族アルコールでエステル化した化合物を含有する、半導体封止用エポキシ樹脂組成物。 - 前記(D)炭素数28〜60のα−オレフィンと無水マレイン酸との共重合体を、炭素数10〜25の長鎖脂肪族アルコールでエステル化した化合物の含有量が、前記離型剤の総量100質量%に対して、55質量%以上100質量%以下である、請求項1または2に記載の半導体封止用エポキシ樹脂組成物。
- 前記シロキサン付加重合体変性物の含有量が、前記半導体封止用エポキシ樹脂組成物の総量100質量%に対して、0.1質量%以上2質量%以下である、請求項2に記載の半導体封止用エポキシ樹脂組成物。
- 前記(A)エポキシ樹脂が、ビフェニル型エポキシ樹脂、パラキシリレン型エポキシ樹脂、及びビフェニレン骨格を有するフェノールアラルキル型エポキシ樹脂からなる群から選択される少なくとも一種を含む、請求項1から4のいずれか1項に記載の半導体封止用エポキシ樹脂組成物。
- 銅含有リードフレームを備える半導体装置における半導体素子の封止に用いる、請求項1から5のいずれか1項に記載の半導体封止用エポキシ樹脂組成物。
- 請求項1から6のいずれか1項に記載の半導体封止用エポキシ樹脂組成物の硬化物で、半導体素子が封止されていることを特徴とする半導体装置。
- (D)炭素数28〜60のα−オレフィンと無水マレイン酸との共重合体を、炭素数10〜25の長鎖脂肪族アルコールでエステル化した化合物を含有する、離型剤。
- 半導体封止用エポキシ樹脂組成物に用いる、請求項8に記載の離型剤。
- 前記半導体封止用エポキシ樹脂組成物は、銅含有リードフレームを備える半導体装置における半導体素子の封止に用いる、請求項9に記載の離型剤。
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MY156340A (en) * | 2010-03-25 | 2016-02-15 | Sumitomo Bakelite Co | Epoxy resin composition for semiconductor encapsulation, and semiconductor device using the same |
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WO2014116996A1 (en) * | 2013-01-25 | 2014-07-31 | Washington State University Research Foundation | Derivatives of fatty esters, fatty acids and rosins |
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WO2022118749A1 (ja) * | 2020-12-03 | 2022-06-09 | 住友ベークライト株式会社 | 封止用樹脂組成物および半導体装置 |
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