JP2017108116A - ウエハ積層体及びその製造方法 - Google Patents
ウエハ積層体及びその製造方法 Download PDFInfo
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- JP2017108116A JP2017108116A JP2016221110A JP2016221110A JP2017108116A JP 2017108116 A JP2017108116 A JP 2017108116A JP 2016221110 A JP2016221110 A JP 2016221110A JP 2016221110 A JP2016221110 A JP 2016221110A JP 2017108116 A JP2017108116 A JP 2017108116A
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Abstract
Description
〔1〕
透明基板と、該基板上に形成された接着剤層と、更に該接着剤層に、回路面を有する表面が対向するように積層されたウエハとを備えたウエハ積層体であって、上記接着剤が、上記基板側に配設された遮光性を有する第1の硬化樹脂層(A)と、上記ウエハ側に配設された熱硬化性樹脂組成物の硬化物からなる第2の硬化樹脂層(B)とを含むことを特徴とするウエハ積層体。
〔2〕
遮光性を有する第1の硬化樹脂層(A)が、波長500nmにおける透過率が15%以下であり、波長500nm以下に大きな吸収を有する〔1〕に記載のウエハ積層体。
〔3〕
第1の硬化樹脂層(A)が、下記一般式(1)で示される繰り返し単位を有するポリマーを含有する樹脂組成物の硬化物からなる〔1〕又は〔2〕に記載のウエハ積層体。
〔4〕
上記樹脂組成物が、更に架橋剤、酸発生剤、及び有機溶剤のうちいずれか1つ以上のものを含有する〔3〕に記載のウエハ積層体。
〔5〕
第2の硬化樹脂層(B)が、シリコーン樹脂重合体及び/又はエポキシ樹脂重合体を主成分とする熱硬化性樹脂組成物の硬化物からなり、該硬化物の25℃での樹脂モジュラスが10〜1,000MPaである〔1〕〜〔4〕のいずれかに記載のウエハ積層体。
〔6〕
熱硬化性樹脂組成物が、フェノール変性シリコーン樹脂及び/又はエポキシ変性シリコーン樹脂を主成分とする〔5〕に記載のウエハ積層体。
〔7〕
フェノール変性シリコーン樹脂を主成分とする熱硬化性樹脂組成物が、下記一般式(2)で示される繰り返し単位を有する重量平均分子量が3,000〜500,000のフェノール変性シリコーン樹脂100質量部に対して、架橋剤として1分子中に平均して2個以上のエポキシ基を有するエポキシ化合物から選ばれるいずれか1種以上を0.1〜50質量部含有する組成物である〔6〕に記載のウエハ積層体。
〔8〕
エポキシ変性シリコーン樹脂を主成分とする熱硬化性樹脂組成物が、下記一般式(4)で示される繰り返し単位を有する重量平均分子量が3,000〜500,000のエポキシ変性シリコーン樹脂100質量部に対して、架橋剤として1分子中に平均して2個以上のフェノール基を有するフェノール化合物及び1分子中に平均して2個以上のエポキシ基を有するエポキシ化合物から選ばれるいずれか1種以上を0.1〜50質量部含有する組成物である〔6〕に記載のウエハ積層体。
〔9〕
第1の硬化樹脂層(A)の膜厚が0.1〜30μmであり、第2の硬化樹脂層(B)の膜厚が1〜200μmである〔1〕〜〔8〕のいずれかに記載のウエハ積層体。
〔10〕
透明基板に接着剤層を介してウエハの回路形成面を接合して〔1〕〜〔9〕のいずれかに記載のウエハ積層体を製造する方法であって、
(a)透明基板に直接遮光性を有する第1の硬化樹脂層(A)又は第1の硬化樹脂層(A)形成用の樹脂組成物層(A')を形成する工程、
(b)この形成された硬化樹脂層(A)又は樹脂組成物層(A')上に、更に第2の硬化樹脂層(B)形成用の熱硬化性樹脂組成物層(B')を形成する工程、
(c)この熱硬化性樹脂組成物層(B')にウエハの回路形成面を減圧下に接合する工程、
(d)上記熱硬化性樹脂組成物層(B')の熱硬化を行って第2の硬化樹脂層(B)を形成すると共に、第1の硬化樹脂層(A)との接着を行う工程、又は樹脂組成物層(A')を用いた場合は熱硬化性樹脂組成物層(B')と同時に熱硬化を行って第1及び第2の硬化樹脂層(A)、(B)を形成して接着を行う工程、
(e)接合した上記ウエハの回路非形成面を研削又は研磨する工程
を含むことを特徴とするウエハ積層体の製造方法。
〔11〕
透明基板に接着剤層を介してウエハの表面回路形成面を接合して〔1〕〜〔9〕のいずれかに記載のウエハ積層体を製造する方法であって、
(a)透明基板に直接遮光性を有する第1の硬化樹脂層(A)又は第1の硬化樹脂層(A)形成用の樹脂組成物層(A')を形成する工程、
(b')ウエハの表面回路形成面に第2の硬化樹脂層(B)形成用の熱硬化性樹脂組成物層(B')を形成する工程、
(c')上記透明基板上の第1の硬化樹脂層(A)又は樹脂組成物層(A')とウエハ上の熱硬化性樹脂組成物層(B')とを減圧下に接合する工程、
(d)上記熱硬化性樹脂組成物層(B')の熱硬化を行って第2の硬化樹脂層(B)を形成すると共に、第1の硬化樹脂層(A)との接着を行う工程、又は樹脂組成物層(A')を用いた場合は熱硬化性樹脂組成物層(B')と同時に熱硬化を行って第1及び第2の硬化樹脂層(A)、(B)を形成して接着を行う工程、
(e)接合した上記ウエハの回路非形成面を研削又は研磨する工程
を含むことを特徴とするウエハ積層体の製造方法。
本発明のウエハ積層体は、図1に示したように、透明基板1に接して形成された第1の硬化樹脂層(A)3aと、この層(A)と接して形成された第2の硬化樹脂層(B)3bの2層の接着剤層3を介して、ウエハ2と積層されたウエハ積層体である。
透明基板としては、ガラス基板、石英基板が用いられ、その厚さは、通常300〜1,000μm、特に500〜800μmである。
第1の硬化樹脂層(A)は、500nm以下の波長に対して大きな吸収を有する硬化樹脂層(遮光層)であり、かつ、耐熱性や接着性、耐薬品性等の特徴を保持するため、下記一般式(1)で示される構造を繰り返し単位として有するポリマーとこのポリマーを熱反応によって架橋させる架橋剤とを含有する樹脂組成物の硬化物から構成される。なお、500nm以下の波長に対して大きな吸収を有するとは、波長500nm以下の吸収率が80%以上であることを示す。
Q−CHO (6)
(式中、Qは水素原子又は置換基を有してもよい炭素数1〜30、特に1〜10の1価の有機基である。)
架橋剤としては、分子内に2個以上の官能基を有するエポキシ化合物やエポキシ樹脂、更には、メチロールメラミン等のアミノ樹脂が好適に用いられ、これらの架橋剤と上記ポリマーとの架橋反応を促進させるため、触媒を添加することが好ましい。
(S-)(N+(R17R18R19R20)) (8)
(式中、R17、R18、R19、R20はそれぞれ水素原子、炭素数1〜12の直鎖状、分岐状又は環状のアルキル基、アルケニル基、オキソアルキル基又はオキソアルケニル基、炭素数6〜20のアリール基、又は炭素数7〜12のアラルキル基又はアリールオキソアルキル基を示し、これらの基の水素原子の一部又は全部がアルコキシ基によって置換されていてもよい。R17、R18、R19、R20はこれらが結合する窒素原子と共に環を形成してもよく、環を形成する場合には、炭素数3〜10のアルキレン基であるか、又は式中の窒素原子を環の中に有する複素芳香族環を形成する。S-はα位の少なくとも1つがフッ素化されたスルホン酸、又はパーフルオロアルキルイミド酸若しくはパーフルオロアルキルメチド酸である。)
本発明で用いられるヒンダードフェノール系化合物は、特に限定されるものではないが、以下に挙げるヒンダードフェノール系化合物が好ましい。
1,3,5−トリメチル−2,4,6−トリス(3,5−ジ−t−ブチル−4−ヒドロキシベンジル)ベンゼン(商品名:IRGANOX 1330)、2,6−ジ−t−ブチル−4−メチルフェノール(商品名:Sumilizer BHT)、2,5−ジ−t−ブチル−ハイドロキノン(商品名:Nocrac NS-7)、2,6−ジ−t−ブチル−4−エチルフェノール(商品名:Nocrac M-17)、2,5−ジ−t−アミルハイドロキノン(商品名:Nocrac DAH)、2,2'−メチレンビス(4−メチル−6−t−ブチルフェノール)(商品名:Nocrac NS-6)、3,5−ジ−t−ブチル−4−ヒドロキシ−ベンジルフォスフォネート−ジエチルエステル(商品名:IRGANOX 1222)、4,4'−チオビス(3−メチル−6−t−ブチルフェノール)(商品名:Nocrac 300)、2,2'−メチレンビス(4−エチル−6−t−ブチルフェノール)(商品名:Nocrac NS-5)、4,4'−ブチリデンビス(3−メチル−6−t−ブチルフェノール)(アデカスタブAO-40)、2−t−ブチル−6−(3−t−ブチル−2−ヒドロキシ−5−メチルベンジル)−4−メチルフェニルアクリレート(商品名:Sumilizer GM)、2−[1−(2−ヒドロキシ−3,5−ジ−t−ペンチルフェニル)エチル]−4,6−ジ−t−ペンチルフェニルアクリレート(商品名:Sumilizer GS)、2,2'−メチレンビス[4−メチル−6−(α−メチル−シクロヘキシル)フェノール]、4,4'−メチレンビス(2,6−ジ−t−ブチルフェノール)(商品名:シーノックス226M)、4,6−ビス(オクチルチオメチル)−o−クレゾール(商品名:IRGANOX 1520L)、2,2'−エチレンビス(4,6−ジ−t−ブチルフェノール)、オクタデシル−3−(3,5−ジ−t−ブチル−4−ヒドロキシフェニル)プロピオネート(商品名:IRGANOX 1076)、1,1,3−トリス−(2−メチル−4−ヒドロキシ−5−t−ブチルフェニル)ブタン(商品名:アデカスタブAO-30)、テトラキス[メチレン−(3,5−ジ−t−ブチル−4−ヒドロキシハイドロシンナメート)]メタン(商品名:アデカスタブ AO−60)、トリエチレングリコールビス[3−(3−t−ブチル−5−メチル−4−ヒドロキシフェニル)プロピオネート](商品名:IRGANOX 245)、2,4−ビス−(n−オクチルチオ)−6−(4−ヒドロキシ−3,5−ジ−t−ブチルアニリノ)−1,3,5−トリアジン(商品名:IRGANOX 565)、N,N'−ヘキサメチレンビス(3,5−ジ−t−ブチル−4−ヒドロキシ−ヒドロシンナマミド)(商品名:IRGANOX 1098)、1,6−ヘキサンジオール−ビス[3−(3,5−ジ−t−ブチル−4−ヒドロキシフェニル)プロピオネート](商品名:IRGANOX 259)、2,2−チオ−ジエチレンビス[3−(3,5−ジ−t−ブチル−4−ヒドロキシフェニル)プロピオネート](商品名:IRGANOX 1035)、3,9−ビス[2−[3−(3−t−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオニルオキシ]1,1−ジメチルエチル]2,4,8,10−テトラオキサスピロ[5.5]ウンデカン(商品名:Sumilizer GA-80)、トリス−(3,5−ジ−t−ブチル−4−ヒドロキシベンジル)イソシアヌレート(商品名:IRGANOX 3114)、ビス(3,5−ジ−t−ブチル−4−ヒドロキシベンジルホスホン酸エチル)カルシウム/ポリエチレンワックス混合物(50:50)(商品名:IRGANOX 1425WL)、イソオクチル−3−(3,5−ジ−t−ブチル−4−ヒドロキシフェニル)プロピオネート(商品名:IRGANOX 1135)、4,4'−チオビス(6−t−ブチル−3−メチルフェノール)(商品名:Sumilizer WX-R)、6−[3−(3−t−ブチル−4−ヒドロキシ−5−メチルフェニル)プロポキシ]−2,4,8,10−テトラ−t−ブチルジベンズ[d,f][1,3,2]ジオキサフォスフェピン(商品名:Sumilizer GP)等。
本発明で用いられるヒンダードアミン系化合物は、特に限定されるものではないが、以下に挙げるヒンダードアミン系化合物が好ましい。
p,p'−ジオクチルジフェニルアミン(商品名:IRGANOX 5057)、フェニル−α−ナフチルアミン(商品名:Nocrac PA)、ポリ(2,2,4−トリメチル−1,2−ジヒドロキノリン)(商品名:Nocrac 224、224-S)、6−エトキシ−2,2,4−トリメチル−1,2−ジヒドロキノリン(商品名:Nocrac AW)、N,N'−ジフェニル−p−フェニレンジアミン(商品名:Nocrac DP)、N,N'−ジ−β−ナフチル−p−フェニレンジアミン(商品名:Nocrac White)、N−フェニル−N'−イソプロピル−p−フェニレンジアミン(商品名:Nocrac 810NA)、N,N'−ジアリル−p−フェニレンジアミン(商品名:Nonflex TP)、4,4'−(α,α−ジメチルベンジル)ジフェニルアミン(商品名:Nocrac CD)、p,p−トルエンスルフォニルアミノジフェニルアミン(商品名:Nocrac TD)、N−フェニル−N'−(3−メタクロリルオキシ−2−ヒドロキシプロピル)−p−フェニレンジアミン(商品名:Nocrac G1)、N−(1−メチルヘプチル)−N'−フェニル−p−フェニレンジアミン(商品名:Ozonon 35)、N,N'−ジ−sec−ブチル−p−フェニレンジアミン(商品名:Sumilizer BPA)、N−フェニル−N'−1,3−ジメチルブチル−p−フェニレンジアミン(商品名:Antigene 6C)、アルキル化ジフェニルアミン(商品名:Sumilizer 9A)、コハク酸ジメチル−1−(2−ヒドロキシエチル)−4−ヒドロキシ−2,2,6,6−テトラメチルピペリジン重縮合物(商品名:Tinuvin 622LD)、ポリ[[6−(1,1,3,3−テトラメチルブチル)アミノ−1,3,5−トリアジン−2,4−ジイル][(2,2,6,6−テトラメチル−4−ピペリジル)イミノ]ヘキサメチレン[(2,2,6,6−テトラメチル−4−ピペリジル)イミノ]](商品名:CHIMASSORB 944)、N,N'−ビス(3−アミノプロピル)エチレンジアミン−2,4−ビス[N−ブチル−N−(1,2,2,6,6−ペンタメチル−4−ピペリジル)アミノ]−6−クロロ−1,3,5−トリアジン縮合物(商品名:CHIMASSORB 119FL)、ビス(1−オクチロキシ−2,2,6,6−テトラメチル−4−ピペリジル)セバケート(商品名:TINUVIN 123)、ビス(2,2,6,6−テトラメチル−4−ピペリジル)セバケート(商品名:TINUVIN 770)、2−(3,5−ジ−t−ブチル−4−ヒドロキシベンジル)−2−n−ブチルマロン酸ビス(1,2,2,6,6−ペンタメチル−4−ピペリジル)(商品名:TINUVIN 144)、ビス(1,2,2,6,6−ペンタメチル−4−ピペリジル)セバケート(商品名:TINUVIN 765)、テトラキス(1,2,2,6,6−ペンタメチル−4−ピペリジル)1,2,3,4−ブタンテトラカルボキシレート(商品名:LA-57)、テトラキス(2,2,6,6−テトラメチル−4−ピペリジル)1,2,3,4−ブタンテトラカルボキシレート(商品名:LA-52)、1,2,3,4−ブタンテトラカルボン酸と1,2,2,6,6−ペンタメチル−4−ピペリジノール及び1−トリデカノールとの混合エステル化物(商品名:LA-62)、1,2,3,4−ブタンテトラカルボン酸と2,2,6,6−テトラメチル−4−ピペリジノール及び1−トリデカノールとの混合エステル化物(商品名:LA-67)、1,2,3,4−ブタンテトラカルボン酸と1,2,2,6,6−ペンタメチル−4−ピペリジノール及び3,9−ビス(2−ヒドロキシ−1,1−ジメチルエチル)−2,4,8,10−テトラオキサスピロ[5.5]ウンデカンとの混合エステル化物(商品名:LA-63P)、1,2,3,4−ブタンテトラカルボン酸と2,2,6,6−テトラメチル−4−ピペリジノール及び3,9−ビス(2−ヒドロキシ−1,1−ジメチルエチル)−2,4,8,10−テトラオキサスピロ[5.5]ウンデカンとの混合エステル化物(商品名:LA-68LD)、(2,2,6,6−テトラメチレン−4−ピペリジル)−2−プロピレンカルボキシレート(商品名:アデカスタブLA-82)、(1,2,2,6,6−ペンタメチル−4−ピペリジル)−2−プロピレンカルボキシレート(商品名:アデカスタブLA-87)等。
本発明で用いられる有機リン化合物は、特に限定されるものではないが、以下に挙げる有機リン化合物が好ましい。
ビス(2,4−ジ−t−ブチルフェニル)[1,1−ビフェニル]−4,4'−ジイルビスホスファイト、9,10−ジヒドロ−9−オキサ−10−ホスファフェナントレン−10−オキサイド(商品名:SANKO-HCA)、トリエチルホスファイト(商品名:JP302)、トリ−n−ブチルホスファイト(商品名:JP304)、トリフェニルホスファイト(商品名:アデカスタブTPP)、ジフェニルモノオクチルホスファイト(商品名:アデカスタブC)、トリ(p−クレジル)ホスファイト(商品名:Chelex-PC)、ジフェニルモノデシルホスファイト(商品名:アデカスタブ135A)、ジフェニルモノ(トリデシル)ホスファイト(商品名:JPM313)、トリス(2−エチルヘキシル)ホスファイト(商品名:JP308)、フェニルジデシルホスファイト(アデカスタブ517)、トリデシルホスファイト(商品名:アデカスタブ3010)、テトラフェニルジプロピレングリコールジホスファイト(商品名:JPP100)、ビス(2,4−ジ−t−ブチルフェニル)ペンタエリスリトールジホスファイト(商品名:アデカスタブPEP-24G)、トリス(トリデシル)ホスファイト(商品名:JP333E)、ビス(ノニルフェニル)ペンタエリスリトールジホスファイト(商品名:アデカスタブPEP-4C)、ビス(2,6−ジ−t−ブチル−4−メチルフェニル)ペンタエリスリトールジホスファイト(商品名:アデカスタブPEP-36)、ビス[2,4−ジ(1−フェニルイソプロピル)フェニル]ペンタエリスリトールジホスファイト(商品名:アデカスタブPEP-45)、トリラウリルトリチオホスファイト(商品名:JPS312)、トリス(2,4−ジ−t−ブチルフェニル)ホスファイト(IRGAFOS 168)、トリス(ノニルフェニル)ホスファイト(商品名:アデカスタブ1178)、ジステアリルペンタエリスリトールジホスファイト(商品名:アデカスタブPEP-8)、トリス(モノ,ジノニルフェニル)ホスファイト(商品名:アデカスタブ329K)、トリオレイルホスファイト(商品名:Chelex-OL)、トリステアリルホスファイト(商品名:JP318E)、4,4'−ブチリデンビス(3−メチル−6−t−ブチルフェニルジトリデシル)ホスファイト(商品名:JPH1200)、テトラ(C12−C15混合アルキル)−4,4'−イソプロピリデンジフェニルジホスファイト(商品名:アデカスタブ1500)、テトラ(トリデシル)−4,4'−ブチリデンビス(3−メチル−6−t−ブチルフェノール)ジホスファイト(商品名:アデカスタブ260)、ヘキサ(トリデシル)−1,1,3−トリス(2−メチル−5−t−ブチル−4−ヒドロキシフェニル)ブタン−トリホスファイト(商品名:アデカスタブ522A)、水添ビスフェノールAホスファイトポリマー(HBP)、テトラキス(2,4−ジ−t−ブチルフェニルオキシ)−4,4'−ビフェニレン−ジ−ホスフィン(商品名:P-EPQ)、テトラキス(2,4−ジ−t−ブチル−5−メチルフェニルオキシ)−4,4'−ビフェニレン−ジ−ホスフィン(商品名:GSY-101P)、2−[[2,4,8,10−テトラキス(1,1−ジメチルエチル)ジベンゾ[d,f][1.3.2]ジオキサフォスフェピン−6−イル]オキシ]−N,N−ビス[2−[[2,4,8,10−テトラキス(1,1−ジメチルエチル)ジベンゾ[d,f][1.3.2]ジオキサフォスフェピン−6−イル]オキシ]−エチル]エタナミン(商品名:IRGAFOS 12)、2,2'−メチレンビス(4,6−ジ−t−ブチルフェニル)オクチルホスファイト(商品名:アデカスタブHP-10)等。
本発明で用いられる有機硫黄化合物は、特に限定されるものではないが、以下に挙げる有機硫黄化合物が好ましい。
ジラウリル−3,3'−チオジプロピオネート(商品名:Sumilizer TPL-R)、ジミリスチル−3,3'−チオジプロピオネート(商品名:Sumilizer TPM)、ジステアリル−3,3'−チオジプロピオネート(商品名:Sumilizer TPS)、ペンタエリスリトールテトラキス(3−ラウリルチオプロピオネート)(商品名:Sumilizer TP-D)、ジトリデシル−3,3'−チオジプロピオネート(商品名:Sumilizer TL)、2−メルカプトベンズイミダゾール(商品名:Sumilizer MB)、ジトリデシル−3,3'−チオジプロピオネート(商品名:アデカスタブAO-503A)、1,3,5−トリス−β−ステアリルチオプロピオニルオキシエチルイソシアヌレート、3,3'−チオビスプロピオン酸ジドデシルエステル(商品名:IRGANOX PS 800FL)、3,3'−チオビスプロピオン酸ジオクデシルエステル(商品名:IRGANOX PS 802FL)等。
第2の硬化樹脂層(B)は、耐熱性等の観点から、エポキシ樹脂、ポリイミド樹脂、シリコーン樹脂、フェノール樹脂から選ばれるが、500nmを超える波長に対して高透明性であることが必須であり、かつ、ガラス等の透明基板とシリコンウエハという異種の基板を貼り合わせる目的のため、そのソリ抑制の観点から、その硬化後の硬化物の25℃での樹脂モジュラスが10〜1,000MPa(1GPa)であることが好ましい。このような点から、第2の硬化樹脂層(B)の形成には、シリコーン樹脂重合体及び/又はエポキシ樹脂重合体を主成分とする熱硬化性樹脂組成物を用いることが好ましく、特にフェノール変性シリコーン樹脂、エポキシ変性シリコーン樹脂が好適である。
このフェノール変性シリコーン樹脂の例として下記一般式(2)で示される構造を有する樹脂、エポキシ変性シリコーン樹脂の例として下記一般式(4)で示される構造を有する樹脂が特に好ましい。
本発明のウエハ積層体の製造方法は、透明基板と半導体回路等を有するウエハ、接着層として前述の硬化樹脂層(A)、硬化樹脂層(B)の2層とからなる接着層を用いることを特徴とする。
本発明のウエハ積層体の製造方法は、下記(a)〜(e)の工程を有する。
工程(a)は、透明基板に上述した遮光性を有する第1の硬化樹脂層(A)を直接形成する工程である。層(A)を形成し得る組成物の溶液をスピンコート、ロールコータなどの方法により透明基板に形成でき、この場合、その溶剤の揮発条件に応じて80〜200℃、好ましくは100〜180℃の温度で、予めプリベークを行ったのち、使用に供される。またフィルム状で透明基板に形成することもできる。
工程(b)は、透明基板上に形成された第1の硬化樹脂層(A)又は樹脂組成物層(A')上に、更に第2の硬化樹脂層(B)形成用の熱硬化性樹脂組成物層(B')を形成する工程であり、工程(b')は、該熱硬化性樹脂組成物層(B')をウエハの回路面を有する表面に形成する工程である。
熱硬化性樹脂組成物層(B')は透明基板に形成された第1の層(A)又は(A')上、又はウエハ上に、層(A)又は(A')と同様に溶液をスピンコートあるいはフィルム状でラミネートすることにより形成、プリベークできる。
工程(c)は、熱硬化性樹脂組成物層(B')にウエハの回路形成面を減圧下に接合する工程であり、工程(c')は、透明基板上の第1の硬化樹脂層(A)又は樹脂組成物層(A')とウエハ上の熱硬化性樹脂組成物層(B')とを減圧下に接合する工程である。
層(A)又は(A')と(B')が形成された透明基板とウエハは、これらの層を介して、接合された基板として形成される。このとき、好ましくは40〜200℃、より好ましくは60〜180℃の温度領域で、この温度にて減圧下、この基板を均一に圧着することで、ウエハが透明基板と接合したウエハ積層体が形成される。
ウエハ貼り合わせ装置としては、市販のウエハ接合装置、例えばEVG社のEVG520IS、850TB、SUSS社のXBC300等が挙げられる。
工程(d)は、工程(c)で接合させた透明基板−ウエハ積層体の層(B')又は(A')と(B')の熱硬化を行い硬化樹脂層(A)と(B)との接着を行う工程であり、上記ウエハ積層体が形成された後、120〜220℃、好ましくは150〜200℃で10分〜4時間、好ましくは30分〜2時間加熱することによって、樹脂層(B)の硬化を行う。
工程(e)は、回路非形成面を研削したウエハ加工体、即ち、裏面研削によって薄型化されたウエハ加工体の回路非形成面に加工を施す工程である。ウエハの裏面研削・研磨は特に限定されず公知の研削・研磨技術によって加工される。例えば、ウエハに冷却水を供給しながら砥石(例えばダイヤモンド砥石)により研削する。また、既存の(株)DISCO製、表面研削盤DAG810が使用されてもよい。研磨は、ウエハの裏面を化学機械研磨(CMP)等を用いて研磨されることが好ましい。
撹拌機、温度計、窒素置換装置及び還流冷却器を具備したフラスコ内に9,9'−ビス(3−アリル−4−ヒドロキシフェニル)フルオレン(M−1)43.1g、平均構造式(M−3)で示されるオルガノハイドロジェンシロキサン29.5g、トルエン135g、塩化白金酸0.04gを仕込み、80℃に昇温した。その後、1,4−ビス(ジメチルシリル)ベンゼン(M−5)17.5gを1時間掛けてフラスコ内に滴下した。このとき、フラスコ内温度は、85℃まで上昇した。滴下終了後、更に80℃で2時間熟成し、次いでトルエンを留去すると共に、シクロヘキサノンを80g添加して、樹脂固形分濃度50質量%のシクロヘキサノンを溶剤とする樹脂溶液を得た。この樹脂溶液中の樹脂の分子量をGPCにより測定すると、ポリスチレン換算で重量平均分子量45,000であった。
更にこの樹脂溶液50gに、架橋剤としてエポキシ架橋剤であるEOCN-1020(日本化薬(株)製)を7.5g、硬化触媒として、BSDM(ビス(t−ブチルスルホニル)ジアゾメタン)(和光純薬工業(株)製)を0.2g、更に、酸化防止剤として、テトラキス[メチレン−(3,5−ジ−t−ブチル−4−ヒドロキシハイドロシンナメート)]メタン(商品名:アデカスタブAO-60)を0.1g添加し、1μmのメンブレンフィルターで濾過して、熱硬化性樹脂組成物溶液(B−1)を得た。
撹拌機、温度計、窒素置換装置及び還流冷却器を具備した5Lフラスコ内にエポキシ化合物(M−2)84.1gをトルエン600gに溶解後、化合物(M−3)294.6g、化合物(M−4)25.5gを加え、60℃に加温した。その後、カーボン担持白金触媒(5質量%)1gを投入し、内部反応温度が65〜67℃に昇温するのを確認後、更に、90℃まで加温し、3時間熟成した。次いで室温まで冷却後、メチルイソブチルケトン(MIBK)600gを加え、本反応溶液をフィルターにて加圧濾過することで白金触媒を取り除いた。この樹脂溶液中の溶剤を減圧留去すると共に、プロピレングリコールモノメチルエーテルアセテート(PGMEA)270gを添加して、樹脂固形分濃度60質量%のPGMEAを溶剤とする樹脂溶液を得た。この樹脂溶液中の樹脂の分子量をGPCにより測定すると、ポリスチレン換算で重量平均分子量28,000であった。
更にこの樹脂溶液100gに4官能フェノール化合物であるTEP−TPA(旭有機材工業(株)製)を9g、テトラヒドロ無水フタル酸(新日本理化(株)製、リカシッドHH-A)0.2gを添加し、1μmのメンブレンフィルターで濾過して、熱硬化性樹脂組成物溶液(B−2)を得た。
1,000mLのフラスコに化合物(M−6)として1,5−ジヒドロキシナフタレン80g(0.50モル)、化合物(M−7)として2−ヒドロキシ−6−ナフトアルデヒド51.6g(0.30モル)、更にメチルセロソルブ145gを加え、70℃で撹拌しながら20質量%パラトルエンスルホン酸メチルセロソルブ溶液20gを添加した。温度を85℃に上げ6時間撹拌後、室温に冷却し、酢酸エチル800mLで希釈した。分液ロートに移し変え、脱イオン水200mLで洗浄を繰り返し、反応触媒と金属不純物を除去した。得られた溶液を減圧濃縮した後、残渣に酢酸エチル600mLを加え、ヘキサン2,400mLでポリマーを沈殿させた。沈殿したポリマーを濾別、回収後、減圧乾燥して、下記構造式を繰り返し単位として有するポリマー(1)を得た。GPCにより分子量(Mw)、分散度(Mw/Mn)を求め、1H−NMR分析によりポリマー中の比率を以下のように求めた。
1,000mLのフラスコに化合物(M−6)として1,5−ジヒドロキシナフタレン80g(0.50モル)、化合物(M−8)としてパラホルムアルデヒド9.0g(0.30モル)、更にメチルセロソルブ145gを加え、70℃で撹拌しながら20質量%パラトルエンスルホン酸メチルセロソルブ溶液20gを添加した。温度を85℃に上げ6時間撹拌後、室温に冷却し、酢酸エチル800mLで希釈した。分液ロートに移し変え、脱イオン水200mLで洗浄を繰り返し、反応触媒と金属不純物を除去した。得られた溶液を減圧濃縮した後、残渣に酢酸エチル600mLを加え、ヘキサン2,400mLでポリマーを沈殿させた。沈殿したポリマーを濾別、回収後、減圧乾燥して、下記構造式を繰り返し単位として有するポリマー(2)を得た。GPCにより分子量(Mw)、分散度(Mw/Mn)を求め、1H−NMR分析によりポリマー中の比率を以下のように求めた。
1,000mLのフラスコに化合物(M−9)として1−ヒドロキシナフタレン72g(0.50モル)、化合物(M−7)として2−ヒドロキシ−6−ナフトアルデヒド51.6g(0.30モル)、更にメチルセロソルブ145gを加え、70℃で撹拌しながら20質量%パラトルエンスルホン酸メチルセロソルブ溶液20gを添加した。温度を85℃に上げ6時間撹拌後、室温に冷却し、酢酸エチル800mLで希釈した。分液ロートに移し変え、脱イオン水200mLで洗浄を繰り返し、反応触媒と金属不純物を除去した。得られた溶液を減圧濃縮した後、残渣に酢酸エチル600mLを加え、ヘキサン2,400mLでポリマーを沈殿させた。沈殿したポリマーを濾別、回収後、減圧乾燥して、下記構造式を繰り返し単位として有するポリマー(3)を得た。GPCにより分子量(Mw)、分散度(Mw/Mn)を求め、1H−NMR分析によりポリマー中の比率を以下のように求めた。
1,000mLのフラスコに化合物(M−10)として2−メチルヒドロキベンゼン32.4g(0.30モル)、化合物(M−7)として2−ヒドロキシ−6−ナフトアルデヒド51.6g(0.30モル)、更にメチルセロソルブ145gを加え、70℃で撹拌しながら20質量%パラトルエンスルホン酸メチルセロソルブ溶液20gを添加した。温度を85℃に上げ6時間撹拌後、室温に冷却し、酢酸エチル800mLで希釈した。分液ロートに移し変え、脱イオン水200mLで洗浄を繰り返し、反応触媒と金属不純物を除去した。得られた溶液を減圧濃縮した後、残渣に酢酸エチル600mLを加え、ヘキサン2,400mLでポリマーを沈殿させた。沈殿したポリマーを濾別、回収後、減圧乾燥して、下記構造式を繰り返し単位として有するポリマー(4)を得た。GPCにより分子量(Mw)、分散度(Mw/Mn)を求め、1H−NMR分析によりポリマー中の比率を以下のように求めた。
直径200mm(厚さ:500μm)のガラス板に対しA−1、A−1'、A−2、A−3、A−4の溶液をスピンコート後、ホットプレートにて250℃で5分間加熱することにより、硬化樹脂層(A)に対応する材料を表1に示す膜厚で成膜した。
その後、この接合された基板に対し、下記試験を行った。実施例の結果を表1に示す。なお、下記の順で評価を実施した。
200mmのウエハ接合は、EVG社製ウエハ接合装置EVG520ISを用いて行った。接合温度は表1に記載の値、接合時のチャンバー内圧力は10-3mbar以下、荷重は5kNで実施した。
接合後、一旦、180℃で1時間オーブンを用いて基板を加熱し、層(B)の硬化を実施したのち、室温まで冷却し、その後の界面の接着状況を目視及び光学顕微鏡それぞれで確認し、界面での気泡などの異常が発生しなかった場合を良好と評価して「○」で示し、異常が発生した場合を不良と評価して「×」で示した。
グラインダー((株)DISCO製DAG810)でダイヤモンド砥石を用いてシリコンウエハの裏面研削を行った。最終基板厚50μmまでグラインドした後、光学顕微鏡(100倍)にてクラック、剥離等の異常の有無を調べた。異常が発生しなかった場合を良好と評価して「○」で示し、異常が発生した場合を不良と評価して「×」で示した。
シリコンウエハを裏面研削した後の積層体を窒素雰囲気下の150℃オーブンに2時間入れた後、外観異常の有無を調べた。外観異常が発生しなかった場合を良好と評価して「○」で示し、ボイド、ウエハ膨れ、ウエハ破損等の外観異常が発生した場合を不良と評価して「×」で示した。
樹脂溶液A−1、A−1'、A−2、A−3、A−4をそれぞれ厚み500μmのガラス基板に膜厚0.3μmでスピンコート後、250℃で5分間の熱硬化を行い、硬化樹脂層(A)を形成し、その透過率(波長500nm)を分光光度計(U-4100形、(株)日立ハイテクサイエンス製)を用いて測定した。透過率が15%以下の場合を良好として「○」で示し、15%よりも高い場合を不良として「×」で示した。また、分光光度計(U-4100形)を用いて波長500nm以下の吸収率を測定した。本発明の範囲内の樹脂層は、波長500nm以下の吸収率が80%以上をいずれも示していた。
更に上記硬化樹脂層(A)を形成し、そのガラス基板に対し、模擬太陽光(波長350nm以下をカット)500万ルクスを照射後の透過率(波長500nm)を再度測定した。透過率15%以下を「○」、15%より高い場合を「×」として評価した。
2 ウエハ
3 接着剤層
3a 第1の硬化樹脂層(A)
3b 第2の硬化樹脂層(B)
Claims (11)
- 透明基板と、該基板上に形成された接着剤層と、更に該接着剤層に、回路面を有する表面が対向するように積層されたウエハとを備えたウエハ積層体であって、上記接着剤が、上記基板側に配設された遮光性を有する第1の硬化樹脂層(A)と、上記ウエハ側に配設された熱硬化性樹脂組成物の硬化物からなる第2の硬化樹脂層(B)とを含むことを特徴とするウエハ積層体。
- 遮光性を有する第1の硬化樹脂層(A)が、波長500nmにおける透過率が15%以下であり、波長500nm以下に大きな吸収を有する請求項1に記載のウエハ積層体。
- 上記樹脂組成物が、更に架橋剤、酸発生剤、及び有機溶剤のうちいずれか1つ以上のものを含有する請求項3に記載のウエハ積層体。
- 第2の硬化樹脂層(B)が、シリコーン樹脂重合体及び/又はエポキシ樹脂重合体を主成分とする熱硬化性樹脂組成物の硬化物からなり、該硬化物の25℃での樹脂モジュラスが10〜1,000MPaである請求項1〜4のいずれか1項に記載のウエハ積層体。
- 熱硬化性樹脂組成物が、フェノール変性シリコーン樹脂及び/又はエポキシ変性シリコーン樹脂を主成分とする請求項5に記載のウエハ積層体。
- フェノール変性シリコーン樹脂を主成分とする熱硬化性樹脂組成物が、下記一般式(2)で示される繰り返し単位を有する重量平均分子量が3,000〜500,000のフェノール変性シリコーン樹脂100質量部に対して、架橋剤として1分子中に平均して2個以上のエポキシ基を有するエポキシ化合物から選ばれるいずれか1種以上を0.1〜50質量部含有する組成物である請求項6に記載のウエハ積層体。
- エポキシ変性シリコーン樹脂を主成分とする熱硬化性樹脂組成物が、下記一般式(4)で示される繰り返し単位を有する重量平均分子量が3,000〜500,000のエポキシ変性シリコーン樹脂100質量部に対して、架橋剤として1分子中に平均して2個以上のフェノール基を有するフェノール化合物及び1分子中に平均して2個以上のエポキシ基を有するエポキシ化合物から選ばれるいずれか1種以上を0.1〜50質量部含有する組成物である請求項6に記載のウエハ積層体。
- 第1の硬化樹脂層(A)の膜厚が0.1〜30μmであり、第2の硬化樹脂層(B)の膜厚が1〜200μmである請求項1〜8のいずれか1項に記載のウエハ積層体。
- 透明基板に接着剤層を介してウエハの回路形成面を接合して請求項1〜9のいずれか1項に記載のウエハ積層体を製造する方法であって、
(a)透明基板に直接遮光性を有する第1の硬化樹脂層(A)又は第1の硬化樹脂層(A)形成用の樹脂組成物層(A')を形成する工程、
(b)この形成された硬化樹脂層(A)又は樹脂組成物層(A')上に、更に第2の硬化樹脂層(B)形成用の熱硬化性樹脂組成物層(B')を形成する工程、
(c)この熱硬化性樹脂組成物層(B')にウエハの回路形成面を減圧下に接合する工程、
(d)上記熱硬化性樹脂組成物層(B')の熱硬化を行って第2の硬化樹脂層(B)を形成すると共に、第1の硬化樹脂層(A)との接着を行う工程、又は樹脂組成物層(A')を用いた場合は熱硬化性樹脂組成物層(B')と同時に熱硬化を行って第1及び第2の硬化樹脂層(A)、(B)を形成して接着を行う工程、
(e)接合した上記ウエハの回路非形成面を研削又は研磨する工程
を含むことを特徴とするウエハ積層体の製造方法。 - 透明基板に接着剤層を介してウエハの表面回路形成面を接合して請求項1〜9のいずれか1項に記載のウエハ積層体を製造する方法であって、
(a)透明基板に直接遮光性を有する第1の硬化樹脂層(A)又は第1の硬化樹脂層(A)形成用の樹脂組成物層(A')を形成する工程、
(b')ウエハの表面回路形成面に第2の硬化樹脂層(B)形成用の熱硬化性樹脂組成物層(B')を形成する工程、
(c')上記透明基板上の第1の硬化樹脂層(A)又は樹脂組成物層(A')とウエハ上の熱硬化性樹脂組成物層(B')とを減圧下に接合する工程、
(d)上記熱硬化性樹脂組成物層(B')の熱硬化を行って第2の硬化樹脂層(B)を形成すると共に、第1の硬化樹脂層(A)との接着を行う工程、又は樹脂組成物層(A')を用いた場合は熱硬化性樹脂組成物層(B')と同時に熱硬化を行って第1及び第2の硬化樹脂層(A)、(B)を形成して接着を行う工程、
(e)接合した上記ウエハの回路非形成面を研削又は研磨する工程
を含むことを特徴とするウエハ積層体の製造方法。
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JP2015191940A (ja) * | 2014-03-27 | 2015-11-02 | 富士フイルム株式会社 | 積層体、保護層形成用組成物、キット、および、半導体デバイスの製造方法 |
US20150325465A1 (en) * | 2014-05-08 | 2015-11-12 | Tokyo Ohka Kogyo Co., Ltd. | Supporting member separation method |
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CN106800909B (zh) | 2021-05-28 |
US10453732B2 (en) | 2019-10-22 |
EP3173453B1 (en) | 2020-09-30 |
EP3173453A1 (en) | 2017-05-31 |
KR20170061607A (ko) | 2017-06-05 |
KR102543122B1 (ko) | 2023-06-14 |
JP6610510B2 (ja) | 2019-11-27 |
US20170154802A1 (en) | 2017-06-01 |
TW201736109A (zh) | 2017-10-16 |
CN106800909A (zh) | 2017-06-06 |
TWI693161B (zh) | 2020-05-11 |
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