JP7491668B2 - 樹脂組成物 - Google Patents
樹脂組成物 Download PDFInfo
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- JP7491668B2 JP7491668B2 JP2019023744A JP2019023744A JP7491668B2 JP 7491668 B2 JP7491668 B2 JP 7491668B2 JP 2019023744 A JP2019023744 A JP 2019023744A JP 2019023744 A JP2019023744 A JP 2019023744A JP 7491668 B2 JP7491668 B2 JP 7491668B2
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- 238000000790 scattering method Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 125000003003 spiro group Chemical group 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 125000002298 terpene group Chemical group 0.000 description 1
- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- SWAXTRYEYUTSAP-UHFFFAOYSA-N tert-butyl ethaneperoxoate Chemical compound CC(=O)OOC(C)(C)C SWAXTRYEYUTSAP-UHFFFAOYSA-N 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- GHPYAGKTTCKKDF-UHFFFAOYSA-M tetraphenylphosphanium;thiocyanate Chemical compound [S-]C#N.C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 GHPYAGKTTCKKDF-UHFFFAOYSA-M 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical class SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- JLGNHOJUQFHYEZ-UHFFFAOYSA-N trimethoxy(3,3,3-trifluoropropyl)silane Chemical compound CO[Si](OC)(OC)CCC(F)(F)F JLGNHOJUQFHYEZ-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
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Description
[1] スパッタで導体層が形成されるための絶縁層の形成用の樹脂組成物であって、
(A-1)液状又は半固形状の熱硬化性樹脂、及び
(B)熱可塑性樹脂、を含み、
(C)無機充填材を含まないか又は含み、
(C)無機充填材の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、50質量%以下であり、
(C)無機充填材の比表面積が40m2/g以上である、樹脂組成物。
[2] 樹脂成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、50質量%以上である、[1]に記載の樹脂組成物。
[3] (A-1)成分が、エポキシ樹脂、(メタ)アクリル樹脂、アミン系樹脂、及びアリル系樹脂から選ばれる少なくとも1種である[1]又は[2]に記載の樹脂組成物。
[4] (A-1)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、5質量%以上30質量%以下である、[1]~[3]のいずれかに記載の樹脂組成物。
[5] (B)成分が、ポリイミド樹脂、ポリカーボネート樹脂及びフェノキシ樹脂から選ばれる少なくとも1種である、[1]~[4]のいずれかに記載の樹脂組成物。
[6] (B)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、10質量%以上50質量%以下である、[1]~[5]のいずれかに記載の樹脂組成物。
[7] (C)成分が、シリカである、[1]~[6]のいずれかに記載の樹脂組成物。
[8] (A-2)固形状の熱硬化性樹脂をさらに含む、[1]~[7]のいずれかに記載の樹脂組成物。
[9] (A-2)成分が、シアネートエステル系樹脂、カルボジイミド系樹脂、及びマレイミド樹脂の少なくともいずれかである、[8]に記載の樹脂組成物。
[10] 多層プリント配線板の絶縁層の形成用である、[1]~[9]のいずれかに記載の樹脂組成物。
[11] スパッタで導体層が形成されるための絶縁層の形成用の樹脂シートであって、
支持体と、該支持体上に設けられた、樹脂組成物を含む樹脂組成物層とを含み、
樹脂組成物が、(A)熱硬化性樹脂、及び(B)熱可塑性樹脂を含み、(C)無機充填材を含まないか又は含み、(C)無機充填材の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、50質量%以下であり、(C)無機充填材の比表面積が40m2/g以上であり、
樹脂組成物層の最低溶融粘度が100poise以上4000poise以下である樹脂シート。
[12] 支持体と、該支持体上に設けられた[1]~[10]のいずれかに記載の樹脂組成物を含む樹脂組成物層とを含む、樹脂シート。
[13] [1]~[10]のいずれかに記載の樹脂組成物の硬化物、もしくは請求項11又は12に記載の樹脂シートの樹脂組成物層の硬化物により形成された絶縁層を含む、プリント配線板。
[14] (1)内層基板上に、[11]又は[12]に記載の樹脂シートの樹脂組成物層が内層基板と接合するように積層する工程、
(2)樹脂組成物層を熱硬化して絶縁層を形成する工程、
(3)絶縁層に穴あけする工程、及び
(4)絶縁層上にスパッタにより導体層を形成する工程、を含む、プリント配線板の製造方法。
[15] [13]に記載のプリント配線板を含む、半導体装置。
本発明の樹脂組成物は、(A-1)液状又は半固形状の熱硬化性樹脂、及び(B)熱可塑性樹脂、を含み、(C)無機充填材を含まないか又は含み、(C)無機充填材の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、50質量%以下であり、(C)無機充填材の比表面積が40m2/g以上である。また、本発明の樹脂組成物は、スパッタで導体層を形成されるための絶縁層の形成用の樹脂組成物として好適である。このような樹脂組成物を用いることにより、スパッタによる導体層形成において、ビア底ボイドの発生を抑制することが可能な硬化物を得ることができ、かつ、フィルム取扱い性に優れた樹脂シートが得られるようになる。さらには、スパッタによる導体層形成においては、無機充填材に起因する凸凹などの不均一な粗化面や、銅配線と絶縁層の熱膨張のミスマッチによる歪みが、微細配線形成の歩留まりに大きく影響する傾向にあるが、このような樹脂組成物を用いることにより、算術平均粗さRaが低く、線熱膨張係数が低い硬化物を得ることが可能であり、微細配線形成にも寄与する。
(A)熱硬化性樹脂としては、配線板の絶縁層を形成する際に使用される熱硬化性樹脂を用いることができる。このような熱硬化性樹脂としては、例えば、エポキシ樹脂、(メタ)アクリル樹脂、マレイミド樹脂、フェノール系樹脂、ナフトール系樹脂、ベンゾオキサジン系樹脂、活性エステル系樹脂、シアネートエステル系樹脂、カルボジイミド系樹脂、アミン系樹脂、アリル系樹脂、酸無水物系樹脂等が挙げられる。用語「(メタ)アクリル樹脂」とは、アクリル樹脂及びメタクリル樹脂を包含する。
恒温水槽:
攪拌機、ヒーター、温度計、自動温度調節器(±0.1℃で温度制御が可能なもの)を備えたもので深さ150mm以上のものを用いる。
なお、後述する実施例で用いた熱硬化性樹脂の判定では、いずれもヤマト科学社製の低温恒温水槽(型式BU300)と投入式恒温装置サーモメイト(型式BF500)の組み合わせを用い、水道水約22リットルを低温恒温水槽(型式BU300)に入れ、これに組み付けられたサーモメイト(型式BF500)の電源を入れて設定温度(20℃又は60℃)に設定し、水温を設定温度±0.1℃にサーモメイト(型式BF500)で微調整したが、同様の調整が可能な装置であればいずれも使用できる。
試験管としては、図1に示すように、内径30mm、高さ120mmの平底円筒型透明ガラス製のもので、管底から55mmおよび85mmの高さのところにそれぞれ標線11A、12Bが付され、試験管の口をゴム栓13aで密閉した液状判定用試験管10aと、同じサイズで同様に標線が付され、中央に温度計を挿入・支持するための孔があけられたゴム栓13bで試験管の口を密閉し、ゴム栓13bに温度計14を挿入した温度測定用試験管10bを用いる。以下、管底から55mmの高さの標線を「A線」、管底から85mmの高さの標線を「B線」という。
温度計14としては、JIS B7410(1982)「石油類試験用ガラス製温度計」に規定する凝固点測定用のもの(SOP-58目盛範囲0~100℃)を用いるが、0~100℃の温度範囲が測定できるものであればよい。
温度60±5℃の大気圧下で24時間以上放置した試料を、図1(a)に示す液状判定用試験管10aと図1(b)に示す温度測定用試験管10bにそれぞれ11A線まで入れる。2本の試験管10a、10bを低温恒温水槽に12B線が水面下になるように直立させて静置する。温度計は、その下端が11A線よりも30mm下となるようにする。
試料温度が設定温度±0.1℃に達してから10分間そのままの状態を保持する。10分後、液状判断用試験管10aを低温恒温水槽から取り出し、直ちに水平な試験台の上に水平に倒し、試験管内の液面の先端が11A線から12B線まで移動した時間をストップウォッチで測定し、記録する。
20℃において、測定された時間が90秒を超え、60℃において、測定された時間が90秒以内のものを半固形状と判定する。
60℃において、測定された時間が90秒を超えるものを固体状と判定する。
以下、(A-1)成分及び(A-2)成分について説明する。
樹脂組成物は、(A-1)成分として、液状又は半固形状の熱硬化性樹脂を含む。(A-1)成分が樹脂組成物中に含まれることで、最低溶融粘度を低下させることができるとともに埋め込み性を向上させることができ、その結果フィルム取扱い性を向上させることができる。
樹脂組成物は、任意の成分として、さらに(A-2)成分として、固形状の熱硬化性樹脂を含んでいてもよい。(A-2)成分が樹脂組成物中に含まれることで、フィルム取扱い性をより向上させることができる。
樹脂組成物は、(B)熱可塑性樹脂を含有する。(B)成分としての熱可塑性樹脂を樹脂組成物が含有することで、フィルム取扱い性を向上させることができる。また、(B)熱可塑性樹脂を樹脂組成物に含有させることで、硬化物の線熱膨張係数を低下させることも可能となる。
R31及びR32は、それぞれ独立して、ハロゲン原子、シアノ基、ニトロ基、又は-X33-R33を示し、
X33は、それぞれ独立して、単結合、-NR33’-、-O-、-S-、-CO-、-SO2-、-NR33’CO-、-CONR33’-、-OCO-、又は-COO-を示し、
R33は、それぞれ独立して、置換又は無置換のアルキル基、又は置換又は無置換のアルケニル基を示し、
R33’は、それぞれ独立して、水素原子、置換又は無置換のアルキル基、又は置換又は無置換のアルケニル基を示し、
Yは、単結合、或いは炭素原子、酸素原子、硫黄原子及び窒素原子から選ばれる1~100個の骨格原子を有するリンカー構造を示し、
n10及びm10は、それぞれ独立して、0~3の整数を示す。]
で表される化合物が挙げられる。
樹脂組成物は、(C)無機充填材を含有するか又は含まない。但し、(C)無機充填材の含有量は、樹脂組成物中の不揮発成分を100質量%とした場合、50質量%以下である。(C)成分として無機充填材と含有する場合、(C)無機充填材の比表面積が40m2/g以上である。(C)無機充填材の比表面積とは、樹脂組成物に含まれる無機充填材全体の比表面積を表す。
樹脂組成物は、任意の成分として、更に、(D)硬化促進剤を含んでいてもよい。
樹脂組成物は、上述した成分以外に、任意の成分として、更にその他の添加剤を含んでいてもよい。このような添加剤としては、例えば、増粘剤、消泡剤、レベリング剤、密着性付与剤等の樹脂添加剤;重合開始剤などが挙げられる。これらの添加剤は、1種類単独で用いてもよく、2種類以上を組み合わせて用いてもよい。それぞれの含有量は当業者であれば適宜設定できる。
本発明の樹脂組成物は、埋め込み性に優れるという特性を示す。よって、フィルム取扱い性に優れる樹脂シートをもたらす。埋め込み性の測定の具体例は、樹脂シートを、ガラス布基材エポキシ樹脂両面銅張積層板(銅箔の厚さ3μm、基板厚み0.15mm、三菱ガス化学社製「HL832NSF LCA」、255×340mmサイズ)にラミネートし、樹脂組成物層を100℃で20分間、その後180℃で30分間熱硬化させ絶縁層を形成し評価基板を作製する。デジタルマイクロスコープを用いて、評価基板の配線パターン上における任意に設定した1cm角を3点観察し、直径10μm以上の外観欠点であるボイドを測定する。このときボイドの数は通常0個である。前記の埋め込み性の評価の詳細は、後述する実施例に記載の方法に従って測定することができる。
本発明の樹脂シートは、支持体と、該支持体上に設けられた、樹脂組成物を含む樹脂組成物層とを含み、樹脂組成物が、(A)熱硬化性樹脂、及び(B)熱可塑性樹脂を含み、(C)無機充填材を含まないか又は含み、(C)無機充填材の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、50質量%以下であり、(C)無機充填材の比表面積が40m2/g以上であり、樹脂組成物層の最低溶融粘度が100poise以上4000poise以下である。
本発明のプリント配線板は、本発明の樹脂組成物の硬化物により形成された絶縁層を含む。本発明の樹脂組成物は、スパッタで導体層を形成するための絶縁層を形成するための樹脂組成物として好適に使用することができる。このため、導体層はスパッタにて形成することが好ましい。
(1)内層基板上に、樹脂シートの樹脂組成物層が内層基板と接合するように積層する工程
(2)樹脂組成物層を熱硬化して絶縁層を形成する工程
(3)絶縁層に穴あけする工程
(4)絶縁層上にスパッタにより導体層を形成する工程
本発明の半導体装置は、本発明のプリント配線板を含む。本発明の半導体装置は、本発明のプリント配線板を用いて製造することができる。
(A)熱硬化性樹脂の液状、半固形状、及び固形状の判定は、危険物の試験及び性状に関する省令(平成元年自治省令第1号)の別紙第2の「液状の確認方法」に準じて行った。「液状の確認方法」は上記したとおりに行った。結果を以下に示す。
「630」三菱ケミカル社製;液状
「ELM-100」住友化学社製;液状
「A-DOG」新中村化学工業社製;液状
「A-A」日本化薬社製;液状
「L-DAIC」四国化成社製;液状
「ALP-d」JFEケミカル社製;液状
「YX4000」三菱ケミカル社製;固形状
「BA230S75」ロンザジャパン社製;固形状
「V-03」日清紡ケミカル社製;固形状
「MIR-3000-70MT」日本化薬社製;固形状
BET全自動比表面積測定装置(マウンテック社製Macsorb HM-1210)を使用して、無機充填材表面に窒素ガスを吸着させ、BET多点法を用いて比表面積を算出することで無機充填材の比表面積を測定した。
有機溶剤に分散した無機充填材については、60℃の乾燥炉中で12時間乾燥し、有機溶剤を揮発させたもので比表面積の測定を実施した。結果を以下に示す。
「YA050C-MJE」アドマテックス社製、メタクリルシランによる表面処理;61.8m2/g
「UFP-30」デンカ社製;30.7m2/g
環流冷却器を連結した水分定量受器、窒素導入管、及び攪拌器を備えた、500mLのセパラブルフラスコを用意した。このフラスコに、4,4’-オキシジフタル酸無水物(ODPA)20.3g、γ-ブチロラクトン200g、トルエン20g、及び、5-(4-アミノフェノキシ)-3-[4-(4-アミノフェノキシ)フェニル]-1,1,3-トリメチルインダン29.6gを加えて、窒素気流下で45℃にて2時間攪拌して、反応を行った。次いで、この反応溶液を昇温し、約160℃に保持しながら、窒素気流下で縮合水をトルエンとともに共沸除去した。水分定量受器に所定量の水がたまっていること、及び、水の流出が見られなくなっていることを確認した。確認後、反応溶液を更に昇温し、200℃で1時間攪拌した。その後、冷却して、1,1,3-トリメチルインダン骨格を有するポリイミド樹脂を含むポリイミド溶液(不揮発分20質量%)を得た。得られたポリイミド樹脂は、下記式(X1)で表される繰り返し単位及び下記式(X2)で示す繰り返し単位を有していた。また、前記のポリイミド樹脂の重量平均分子量は、12,000であった。
グリシジルアミン型エポキシ樹脂(三菱ケミカル社製「630」、エポキシ当量95g/eq.)3部、合成例1で作製したポリイミド樹脂を30部、無機充填材(アドマッテクス社製「YA050C-MJE」、比表面積61.8m2/g、平均粒径50nm、不揮発分50質量%のMEK溶液)20部、ビフェニル型エポキシ樹脂(三菱ケミカル社製「YX4000」、エポキシ当量約190g/eq.)5部、ビスフェノールAジシアネートのプレポリマー(ロンザジャパン社製「BA230S75」、シアネート当量約232g/eq.、不揮発分75質量%のMEK溶液)20部、硬化促進剤(コバルト(III)アセチルアセトン「(Co(acac)3-1M」、不揮発分1質量%のMEK溶液)0.5部を、ミキサーを用いて均一に分散して、樹脂ワニスを得た。
下記表に示す配合割合で各成分を配合した以外は実施例1と同様にして、ミキサーを用いて均一に分散して、樹脂組成物及び樹脂シートを得た。
(1)硬化物性評価用サンプルの調製
予め作製した各実施例及び各比較例の樹脂シートを、200℃で90分間熱硬化させたのち、支持体を剥がすことで硬化物性評価用サンプルを作製した。
硬化物性評価用サンプルを、幅約5mm、長さ約15mmの試験片に切断し、熱機械分析装置(Thermo Plus TMA8310、リガク社製)を使用して、引張加重法で熱機械分析を行った。試験片を前記装置に装着後、荷重1g、昇温速度5℃/分の測定条件にて連続して2回測定した。2回目の測定における30℃から150℃までの線熱膨張係数(ppm)を算出した。
予め作製した各実施例及び各比較例の樹脂シートの樹脂組成物層について、動的粘弾性測定装置(ユー・ビー・エム社製「Rheosol-G3000」)を使用して溶融粘度を測定した。試料樹脂組成物1gについて、直径18mmのパラレルプレートを使用して、開始温度60℃から200℃まで昇温速度5℃/分にて昇温し、測定温度間隔2.5℃、振動1Hz、歪み5degの測定条件にて動的粘弾性率を測定し、最も低くなる溶融粘度(最低溶融粘度)を評価値とした。
(1)内層回路基板の下地処理
内層回路基板として、L/S=15μm/15μmの配線パターンにて形成された回路導体(銅)を両面に有するガラス布基材エポキシ樹脂両面銅張積層板(銅箔の厚さ18μm、基板厚み0.15mm、三菱ガス化学社製「HL832NSF LCA」、255×340mmサイズ)を用意した。
予め作製した各実施例及び各比較例の樹脂シートから保護フィルムを剥がし、バッチ式真空加圧ラミネーター(ニッコー・マテリアルズ社製、2ステージビルドアップラミネーター、CVP700)を用いて、樹脂組成物層が内層回路基板と接するように、内層回路基板の両面にラミネートした。ラミネートは、30秒間減圧して気圧を13hPa以下とし、100℃、圧力0.74MPaにて45秒間圧着させることにより実施した。次いで、100℃、圧力0.5MPaにて75秒間熱プレスを行った。
樹脂組成物層がラミネートされた内層回路基板を、100℃のオーブンに投入後30分間、次いで180℃のオーブンに移し替えた後30分間熱硬化して絶縁層を形成し、支持体を剥離することで、評価用基板を作製した。
デジタルマイクロスコープ(ハイロックス社製「DIGITAL MICROSCOPE KH-8700」)を用いて、評価用基板の配線パターン上における任意に設定した1cm角を3点観察し、その中に、直径10μm以上の外観欠点であるボイドが1個以上あった場合を「×」とし、0個の場合を「○」とした。ボイドがないことで埋め込み性が優れることを表す。
(2)のうち、樹脂シートを内層回路基板にラミネートした際、樹脂シートの外周部から染み出た樹脂の長さを「染み出し量」と規定する。任意の10点の染み出し量を測定し、その平均が0.5mm以上5mm以下である場合を「〇」とし、0.5mm未満又は5mmを超える場合を「×」とした。染み出し量が範囲内であることで基板作製時の制御の容易性を表す。
評価用基板の絶縁層に粗化処理としてのデスミア処理を行った。なお、デスミア処理としては、下記の湿式デスミア処理を実施した。
膨潤液(アトテックジャパン社製「スウェリングディップ・セキュリガントP」、ジエチレングリコールモノブチルエーテル及び水酸化ナトリウムの水溶液)に60℃で5分間、次いで酸化剤溶液(アトテックジャパン社製「コンセントレート・コンパクトCP」、過マンガン酸カリウム濃度約6%、水酸化ナトリウム濃度約4%の水溶液)に80℃で20分間、最後に中和液(アトテックジャパン社製「リダクションソリューション・セキュリガントP」、硫酸水溶液)に40℃で5分間、浸漬した後、80℃で15分間乾燥した。これを粗化基板とする。
非接触型表面粗さ計(ビーコインスツルメンツ社製WYKO NT3300)を用いて、VSIコンタクトモード、50倍レンズにより測定範囲を121μm×92μmとして得られる数値により、粗化基板の算術表面粗さ(Ra)の値(nm)を求めた。また10点の平均値を求めることにより測定した。
(1)内層回路基板の下地処理
内層回路基板として、L/S=2μm/2μmの配線パターンにて形成された回路導体(銅)を両面に有するガラス布基材エポキシ樹脂両面銅張積層板(銅箔の厚さ3μm、基板厚み0.15mm、三菱ガス化学社製「HL832NSF LCA」、255×340mmサイズ)を用意した。
予め作製した各実施例及び各比較例の樹脂シートから保護フィルムを剥がし、バッチ式真空加圧ラミネーター(ニッコー・マテリアルズ社製、2ステージビルドアップラミネーター、CVP700)を用いて、樹脂組成物層が内層回路基板と接するように、内層回路基板の両面にラミネートした。ラミネートは、30秒間減圧して気圧を13hPa以下とし、100℃、圧力0.74MPaにて45秒間圧着させることにより実施した。次いで、100℃、圧力0.5MPaにて75秒間熱プレスを行った。
樹脂組成物層がラミネートされた内層回路基板を、100℃のオーブンに投入後30分間、次いで180℃のオーブンに移し替えた後30分間熱硬化して絶縁層を形成し、支持体を剥離することで、ボイド評価用基板を作製した。
支持体を剥離して絶縁層の表面を露出させ、UV-YAGレーザー加工機(ビアメカニクス社製「LU-2L212/M50L」)を使用して、絶縁層に下記条件でビアホールを形成した。
条件:パワー0.25W、ショット数20、狙いトップ径20μm
ボイド評価用基板の絶縁層に粗化処理としてのデスミア処理を行った。なお、デスミア処理としては、下記の湿式デスミア処理を実施した。
膨潤液(アトテックジャパン社製「スウェリングディップ・セキュリガントP」、ジエチレングリコールモノブチルエーテル及び水酸化ナトリウムの水溶液)に60℃で5分間、次いで酸化剤溶液(アトテックジャパン社製「コンセントレート・コンパクトCP」、過マンガン酸カリウム濃度約6%、水酸化ナトリウム濃度約4%の水溶液)に80℃で20分間、最後に中和液(アトテックジャパン社製「リダクションソリューション・セキュリガントP」、硫酸水溶液)に40℃で5分間、浸漬した後、80℃で15分間乾燥した。これを粗化基板とする。
スパッタリング装置(キャノンアネルバ社製「E-400S」)を用いて、チタン層(厚さ30nm)、次いで銅層(厚さ300nm)を形成した。得られた基板を、150℃にて30分間加熱してアニール処理を行った後に、セミアディティブ法に従って、エッチングレジストを形成し、露光・現像によるパターン形成の後に、硫酸銅電解めっきを行い、25μmの厚さで導体層を形成した。導体パターン形成後、200℃にて60分間加熱してアニール処理を行った。得られたプリント配線板を「評価基板A」と称する。
FIB-SEM複合装置(SIIナノテクノロジー社製「SMI3050SE」)を用いて、評価基板Aのビアホールの断面観察を行った。詳細には、ビアを垂直に観察できる断面をFIB(集束イオンビーム)により削り出し、ビア底の界面近傍の断面SEM画像(観察幅40μm)を確認した。各評価基板Aにつき、無作為に選んだ10箇所のビアの断面観察を行い、10箇所全てのビア底でボイドが発生していないものを「○」、1つでもあるものを「×」とした。
630:グリシジルアミン型エポキシ樹脂(三菱ケミカル社製、エポキシ当量約95g/eq.、液状の熱硬化性樹脂)
ELM-100:グリシジルアミン型エポキシ樹脂(住友化学社製、液状の熱硬化性樹脂)
A-DOG:ジオキサンアクリルモノマー(新中村化学工業社製、(メタ)アクリロイル基当量163g/eq.、液状の熱硬化性樹脂)
A-A:アミン系樹脂(日本化薬社製、「カヤハードA-A」、液状の熱硬化性樹脂)
L-DAIC:アリル系樹脂(四国化成社製、液状の熱硬化性樹脂)
ALP-d:アリル系樹脂(JFEケミカル社製、液状の熱硬化性樹脂)
合成例1:合成例1で製造したポリイミド樹脂
YL7553BH30:フェノキシ樹脂(三菱ケミカル社製、固形分30質量%のMEK(メチルエチルケトン)とシクロヘキサノンの1:1溶液)
FPC0220:カーボネート樹脂(三菱瓦斯化学社製)
YA050C-MJE:シリカ(アドマテックス社製、固形分50質量%のMEK溶液、比表面積61.8m2/g、平均粒径50nm)
UFP-30:シリカ(デンカ社製、比表面積30.7m2/g)
YX4000:ビフェニル型エポキシ樹脂(三菱ケミカル社製、、エポキシ当量約190g/eq.、固形状の熱硬化性樹脂)
BA230S75:ビスフェノールAジシアネートのプレポリマー(ロンザジャパン社製、シアネート当量約232g/eq.、不揮発分75質量%のMEK溶液、固形状の熱硬化性樹脂)
V-03:カルボジイミド系硬化剤(日清紡ケミカル社製、活性基当量約216g/eq.、不揮発分50質量%のトルエン溶液、固形状の熱硬化性樹脂)
MIR-3000-70MT:マレイミド樹脂(日本化薬社製、不揮発分70質量%のMEK/トルエン混合、固形状の熱硬化性樹脂)
Co(acac)3-1M:硬化促進剤(コバルト(III)アセチルアセトン、不揮発分1質量%のMEK溶液)
1B2PZ-10M:1-ベンジル-2-フェニルイミダゾール(固形分10質量%のMEK溶液)
パーブチルC:過酸化物系硬化促進剤(日油社製)
Claims (11)
- 内層基板と接合するように内層基板上に積層され、スパッタで導体層が形成されるための絶縁層の形成用の樹脂組成物であって、
(A-1)液状又は半固形状の熱硬化性樹脂、
(A-2)マレイミド樹脂を含む固形状の熱硬化性樹脂、及び
(B)熱可塑性樹脂、を含み、
(C)無機充填材を含まないか又は含み、
(A-1)成分が、アミン系樹脂、アリル系樹脂、及び4員環以上の環状構造を有する(メタ)アクリル樹脂から選ばれる少なくとも1種を含み、
(C)無機充填材の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、40質量%以下であり、
(C)無機充填材の比表面積が40m2/g以上であり、
(A-1)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、1質量%以上40質量%以下である、樹脂組成物。 - 樹脂成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、50質量%以上である、請求項1に記載の樹脂組成物。
- (B)成分が、ポリイミド樹脂、ポリカーボネート樹脂及びフェノキシ樹脂から選ばれる少なくとも1種である、請求項1又は2に記載の樹脂組成物。
- (B)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、10質量%以上50質量%以下である、請求項1~3のいずれか1項に記載の樹脂組成物。
- (C)成分が、シリカである、請求項1~4のいずれか1項に記載の樹脂組成物。
- 多層プリント配線板の絶縁層の形成用である、請求項1~5のいずれか1項に記載の樹脂組成物。
- 内層基板と接合するように内層基板上に積層され、スパッタで導体層が形成されるための絶縁層の形成用の樹脂シートであって、
支持体と、該支持体上に設けられた、樹脂組成物を含む樹脂組成物層とを含み、
樹脂組成物が、(A-1)液状又は半固形状の熱硬化性樹脂、(A-2)マレイミド樹脂を含む固形状の熱硬化性樹脂、及び(B)熱可塑性樹脂を含み、(C)無機充填材を含まないか又は含み、(A-1)成分が、アミン系樹脂、アリル系樹脂、及び4員環以上の環状構造を有する(メタ)アクリル樹脂から選ばれる少なくとも1種を含み、(C)無機充填材の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、40質量%以下であり、(C)無機充填材の比表面積が40m2/g以上であり、(A-1)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、1質量%以上40質量%以下であり、
樹脂組成物層の最低溶融粘度が100poise以上4000poise以下である樹脂シート。 - 支持体と、該支持体上に設けられた請求項1~6のいずれか1項に記載の樹脂組成物を含む樹脂組成物層とを含む、樹脂シート。
- 請求項1~6のいずれか1項に記載の樹脂組成物の硬化物、もしくは請求項7又は8に記載の樹脂シートの樹脂組成物層の硬化物により形成された絶縁層を含む、プリント配線板。
- (1)内層基板上に、請求項7又は8に記載の樹脂シートの樹脂組成物層が内層基板と接合するように積層する工程、
(2)樹脂組成物層を熱硬化して絶縁層を形成する工程、
(3)絶縁層に穴あけする工程、及び
(4)絶縁層上にスパッタにより導体層を形成する工程、を含む、プリント配線板の製造方法。 - 請求項9に記載のプリント配線板を含む、半導体装置。
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