JP7367891B2 - 樹脂シート - Google Patents
樹脂シート Download PDFInfo
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- JP7367891B2 JP7367891B2 JP2023507134A JP2023507134A JP7367891B2 JP 7367891 B2 JP7367891 B2 JP 7367891B2 JP 2023507134 A JP2023507134 A JP 2023507134A JP 2023507134 A JP2023507134 A JP 2023507134A JP 7367891 B2 JP7367891 B2 JP 7367891B2
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- 150000003751 zinc Chemical class 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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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
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- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0025—Crosslinking or vulcanising agents; including accelerators
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- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- H05K1/0313—Organic insulating material
- H05K1/032—Organic insulating material consisting of one material
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
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- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
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Description
[1] 支持体と、当該支持体上に設けられた樹脂組成物層と、を有する樹脂シートであって、
樹脂組成物層が、(A)エポキシ樹脂、(B)有機溶剤、(C)無機充填材、及び(D)応力緩和材を含み、
(B)成分中の沸点120℃未満の芳香族性溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~9質量%である、樹脂シート。
[2] 樹脂組成物層中の(D)成分の含有量が、樹脂組成物層中の不揮発成分を100質量%とした場合、1質量%以上である、上記[1]に記載の樹脂シート。
[3] 樹脂組成物層中の(C)成分の含有量が、樹脂組成物層中の不揮発成分を100質量%とした場合、60質量%以上である、上記[1]又は[2]に記載の樹脂シート。
[4] 樹脂組成物層中の不揮発成分を100質量%とした場合の(C)成分の含有量(質量%)の値と(C)成分の比表面積(m2/g)の値との積が、300以上である、上記[1]~[3]の何れかに記載の樹脂シート。
[5] (B)成分中の沸点120℃未満の有機溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~30質量%である、上記[1]~[4]の何れかに記載の樹脂シート。
[6] (B)成分中の沸点220℃以上の有機溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~10質量%である、上記[1]~[5]の何れかに記載の樹脂シート。
[7] (B)成分中の芳香族性溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~9質量%である、上記[1]~[6]の何れかに記載の樹脂シート。
[8] (B)成分中の沸点120℃以上220℃未満の有機溶剤の含有量が、全(B)成分を100質量%とした場合、85質量%以上である、上記[1]~[7]の何れかに記載の樹脂シート。
[9] (D)成分が、ポリブタジエン構造及びポリカーボネート構造から選ばれる1種以上の構造を有する樹脂を含む非粒子状の応力緩和材を含む、上記[1]~[8]の何れかに記載の樹脂シート。
[10] (D)成分が、粒子状の応力緩和材を含む、上記[1]~[9]の何れかに記載の樹脂シート。
[11] 粒子状の応力緩和材の平均粒径が、10,000nm以下である、上記[10]に記載の樹脂シート。
[12] 樹脂組成物層が、(E)硬化剤をさらに含む、上記[1]~[11]の何れかに記載の樹脂シート。
[13] (E)成分が、活性エステル系硬化剤及びカルボジイミド系硬化剤から選ばれる1種以上の硬化剤を含む、上記[12]に記載の樹脂シート。
[14] (E)成分が、活性エステル系硬化剤を含む、上記[13]に記載の樹脂シート。
[15] 樹脂組成物層が、(F)硬化促進剤をさらに含む、上記[1]~[14]の何れかに記載の樹脂シート。
[16] 樹脂組成物層が、(G)ラジカル重合性化合物をさらに含む、上記[1]~[15]の何れかに記載の樹脂シート。
[17] (G)成分が、マレイミド基を有する、上記[16]に記載の樹脂シート。
[18] 支持体と接しない面を外気に露出し190℃で30分間加熱処理した後の樹脂組成物層の重量減少率が、1質量%~10質量%となる、上記[1]~[17]の何れかに記載の樹脂シート。
[19] 樹脂組成物層の硬化後の誘電正接(Df)が、10GHz、23℃で測定した場合、0.0090以下である、上記[1]~[18]の何れかに記載の樹脂シート。
[20] 樹脂組成物層の100℃における溶融粘度が、50,000poise以下である、上記[1]~[19]の何れかに記載の樹脂シート。
[21] 下記(I)及び(II)の工程を含むプリント配線板の製造方法。
(I)上記[1]~[20]の何れかに記載の樹脂シートを、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
(II)樹脂組成物層を硬化して絶縁層を形成する工程
[22] (A)エポキシ樹脂、(B)有機溶剤、(C)無機充填材、及び(D)応力緩和材を含み、
(B)成分中の沸点120℃未満の芳香族性溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~9質量%である、樹脂組成物。
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(層)と、を有する。
本発明の樹脂シートにおける樹脂組成物(層)の厚さは、特に限定されるものではないが、薄型化の観点から、好ましくは250μm以下、より好ましくは200μm以下、さらに好ましくは150μm以下、特に好ましくは100μm以下である。樹脂組成物(層)の厚さの下限は、特に限定されないが、例えば、5μm以上、10μm以上等とし得る。
本発明の樹脂シートにおける樹脂組成物(層)は、(A)エポキシ樹脂を含有する。(A)エポキシ樹脂とは、エポキシ基を有する硬化性樹脂である。
本発明の樹脂シートにおける樹脂組成物(層)は、(B)有機溶剤を含有する。ここで説明する(B)有機溶剤は、炭素原子及び酸素原子から選ばれる骨格原子で構成された分子内に炭素間二重結合及び炭素間三重結合(芳香環を構成する結合を除く)を含まない沸点250℃以下の液体化合物(常温(25℃)下において液体の化合物)である。また、ここで説明する(B)有機溶剤には、(A)エポキシ樹脂に該当するものを含めない。なお、本明細書中において沸点とは、常圧(1atm;760mmHg)下における沸点(すなわち標準沸点)を示す。(B)有機溶剤は、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。
本発明の樹脂シートにおける樹脂組成物(層)は、(C)無機充填材を含有する。(C)無機充填材は、粒子の状態で樹脂組成物(層)に含まれる。
本発明の樹脂シートにおける樹脂組成物(層)は、(D)応力緩和材を含有する。(D)応力緩和材は、柔軟性を有する樹脂を意味し、樹脂組成物(層)中で粒子の形態を維持する粒子状樹脂成分(粒子状の応力緩和材)、或いは樹脂組成物(層)に混和又は溶解する傾向のある非粒子状樹脂成分(非粒子状の応力緩和材)であり得、それらの一方のみが含まれていても又はそれらの両方が含まれていてもよく、それらを形成する樹脂成分は、樹脂そのものがゴム弾性を示す樹脂、又は他の成分と反応することによりゴム弾性を示す樹脂であり得る。ゴム弾性を示す樹脂としては、例えば、日本工業規格(JIS K7161)に準拠し、温度25℃、湿度40%RHにて、引っ張り試験を行った場合に、1GPa以下の弾性率を示す樹脂が挙げられる。
本発明の樹脂シートにおける樹脂組成物(層)は、任意成分として(E)硬化剤を含有していてもよい。(E)硬化剤は、1種類単独で用いてもよく、2種類以上を任意に組み合わせて用いてもよい。(E)硬化剤は、(A)エポキシ樹脂と反応して硬化させる機能を有し得る。ここで説明する(E)硬化剤は、上記で説明した(D)応力緩和材に該当するもの以外の成分である。
本発明の樹脂シートにおける樹脂組成物(層)は、任意成分として(F)硬化促進剤を含んでいてもよい。(F)硬化促進剤は、(B)エポキシ樹脂の硬化を促進させる硬化触媒としての機能を有する。
本発明の樹脂シートにおける樹脂組成物(層)は、任意成分として(G)ラジカル重合性化合物を含んでいてもよい。(G)ラジカル重合性化合物は、1種類単独で用いてもよく、2種類以上を任意に組み合わせて用いてもよい。ここで説明する(G)ラジカル重合性化合物は、上記で説明した(A)エポキシ樹脂、(D)応力緩和材、及び(E)硬化剤に該当するもの以外の成分である。
で表されるマレイミド化合物を含む。a単位は、それぞれ、単位毎に同一であってもよいし、異なっていてもよい。第一の実施形態におけるマレイミド化合物は、1種単独で用いてもよく、2種以上を任意の比率で組み合わせて用いてもよい。
で表される部分構造を有するマレイミド化合物を含む。第二の実施形態におけるマレイミド化合物は、1種単独で用いてもよく、2種以上を任意の比率で組み合わせて用いてもよい。
で表されるマレイミド化合物を含む。e単位、f単位及びn単位は、それぞれ、単位毎に同一であってもよいし、異なっていてもよい。
で表される部分構造としては、特に限定されるものではないが、例えば、式(D-1)~(D-3):
で表される部分構造が挙げられる。
本発明の樹脂シートにおける樹脂組成物(層)は、さらに任意成分として(H)熱可塑性樹脂を含んでいてもよい。ここで説明する(H)熱可塑性樹脂は、上記で説明した(A)エポキシ樹脂、(D)応力緩和材、(E)硬化剤、及び(G)ラジカル重合性化合物に該当するもの以外の成分である。
本発明の樹脂組成物は、さらに任意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、過酸化物系ラジカル重合開始剤、アゾ系ラジカル重合開始剤等のラジカル重合開始剤;エポキシアクリレート樹脂、ウレタンアクリレート樹脂、ウレタン樹脂、シアネート樹脂、ベンゾオキサジン樹脂、不飽和ポリエステル樹脂、フェノール樹脂、メラミン樹脂、シリコーン樹脂等のエポキシ樹脂以外の熱硬化性樹脂;有機銅化合物、有機亜鉛化合物、有機コバルト化合物等の有機金属化合物;フタロシアニンブルー、フタロシアニングリーン、アイオディングリーン、ジアゾイエロー、クリスタルバイオレット、酸化チタン、カーボンブラック等の着色剤;ハイドロキノン、カテコール、ピロガロール、フェノチアジン等の重合禁止剤;シリコーン系レベリング剤、アクリルポリマー系レベリング剤等のレベリング剤;ベントン、モンモリロナイト等の増粘剤;シリコーン系消泡剤、アクリル系消泡剤、フッ素系消泡剤、ビニル樹脂系消泡剤等の消泡剤;ベンゾトリアゾール系紫外線吸収剤等の紫外線吸収剤;尿素シラン等の接着性向上剤;トリアゾール系密着性付与剤、テトラゾール系密着性付与剤、トリアジン系密着性付与剤等の密着性付与剤;ヒンダードフェノール系酸化防止剤等の酸化防止剤;スチルベン誘導体等の蛍光増白剤;フッ素系界面活性剤、シリコーン系界面活性剤等の界面活性剤;リン系難燃剤(例えばリン酸エステル化合物、ホスファゼン化合物、ホスフィン酸化合物、赤リン)、窒素系難燃剤(例えば硫酸メラミン)、ハロゲン系難燃剤、無機系難燃剤(例えば三酸化アンチモン)等の難燃剤;リン酸エステル系分散剤、ポリオキシアルキレン系分散剤、アセチレン系分散剤、シリコーン系分散剤、アニオン性分散剤、カチオン性分散剤等の分散剤;ボレート系安定剤、チタネート系安定剤、アルミネート系安定剤、ジルコネート系安定剤、イソシアネート系安定剤、カルボン酸系安定剤、カルボン酸無水物系安定剤等の安定剤等が挙げられる。(I)その他の添加剤は、1種を単独で用いてもよく、2種以上を任意の比率で組み合わせて用いてもよい。(I)その他の添加剤の含有量は当業者であれば適宜設定できる。
本発明の樹脂シートは、支持体を有する。本発明の樹脂シートにおける支持体としては、例えば、プラスチック材料からなるフィルム、金属箔、離型紙が挙げられ、プラスチック材料からなるフィルム、金属箔が好ましい。
本発明の樹脂シートは、樹脂組成物(層)の支持体と接合していない面(即ち、支持体とは反対側の面)に、支持体に準じた保護フィルムがさらに積層されていてもよい。保護フィルムの厚さは、特に限定されるものではないが、例えば、1μm~40μmである。保護フィルムを積層することにより、樹脂組成物(層)の表面へのゴミ等の付着やキズを抑制することができる。樹脂シートは、ロール状に巻きとって保存することが可能である。樹脂シートが保護フィルムを有する場合、保護フィルムを剥がすことによって使用可能となる。
本発明の樹脂シートは、例えば、ワニス状の樹脂組成物(樹脂ワニス)を、ダイコーター等を用いて支持体上に塗布し、塗布後に乾燥を行い、支持体上に層状の樹脂組成物(層)を形成することにより、製造することができる。
ワニス状の樹脂組成物(樹脂ワニス)は、例えば、任意の調製容器に(A)エポキシ樹脂、(B)有機溶剤、(C)無機充填材、(D)応力緩和材、必要に応じて(E)硬化剤、必要に応じて(F)硬化促進剤、必要に応じて(G)ラジカル重合性化合物、必要に応じて(H)熱可塑性樹脂、及び必要に応じて(I)その他の添加剤を、任意の順で及び/又は一部若しくは全部同時に加えて混合することによって、製造することができる。また、各成分を加えて混合する過程で、温度を適宜設定することができ、一時的に又は終始にわたって、加熱及び/又は冷却してもよい。また、加えて混合する過程において又はその後に、樹脂組成物を、例えば、ミキサーなどの撹拌装置又は振盪装置を用いて撹拌又は振盪し、均一に分散させてもよい。また、撹拌又は振盪と同時に、真空下等の低圧条件下で脱泡を行ってもよい。
本発明の樹脂シートにおける樹脂組成物(層)は、(A)エポキシ樹脂、(B)有機溶剤、(C)無機充填材、及び(D)応力緩和材を含み、(B)有機溶剤中の沸点120℃未満の芳香族性溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~9質量%である。このような樹脂シートを用いることにより、ラミネート後のムラの発生を抑えることができ且つ硬化後の反りを抑制できる。
本発明の樹脂シート(樹脂組成物)は、絶縁用途の樹脂シート(樹脂組成物)、特に、絶縁層を形成するための樹脂シート(樹脂組成物)として好適に使用することができる。具体的には、絶縁層上に形成される導体層(再配線層を含む)を形成するための当該絶縁層を形成するための樹脂シート(樹脂組成物)(導体層を形成するための絶縁層形成用樹脂シート(樹脂組成物))として好適に使用することができる。また、後述するプリント配線板において、プリント配線板の絶縁層を形成するための樹脂シート(樹脂組成物)(プリント配線板の絶縁層形成用樹脂シート(樹脂組成物))として好適に使用することができ、プリント配線板の層間絶縁層を形成するため(プリント配線板の層間絶縁層用)により好適に使用することができる。また、本発明の樹脂シート(樹脂組成物)は、部品埋め込み性に良好な絶縁層をもたらすことから、プリント配線板が部品内蔵回路板である場合にも好適に使用することができる。
(1)基材に仮固定フィルムを積層する工程、
(2)半導体チップを、仮固定フィルム上に仮固定する工程、
(3)半導体チップ上に封止層を形成する工程、
(4)基材及び仮固定フィルムを半導体チップから剥離する工程、
(5)半導体チップの基材及び仮固定フィルムを剥離した面に、絶縁層としての再配線形成層を形成する工程、及び
(6)再配線形成層上に、導体層としての再配線層を形成する工程
本発明の樹脂シートは、プリント配線板の製造に用いることができる。プリント配線板は、本発明の樹脂シートにおける樹脂組成物(層)を硬化して得られる絶縁層を含む。
(I)内層基板上に、樹脂シートを、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
(II)樹脂組成物(層)を硬化(例えば熱硬化)して絶縁層を形成する工程
上記で説明したプリント配線板は、プリント配線板を含む半導体装置に用いることができる。
反応容器に、2官能性ヒドロキシ基末端ポリブタジエン(日本曹達社製「G-3000」、数平均分子量=3000、ヒドロキシ基当量=1800g/eq.)69gと、PGMEA(昭和電工社製、プロピレングリコールモノメチルエーテルアセテート)40gと、ジブチル錫ラウレート0.005gとを入れ、混合して均一に溶解させた。均一になったところで60℃に昇温し、更に撹拌しながらイソホロンジイソシアネート(エボニックデグサジャパン社製「IPDI」、イソシアネート基当量=113g/eq.)8gを添加し、約3時間反応を行った。
撹拌装置、温度計及びコンデンサーを取り付けられたフラスコに、溶剤として、PGMEA736gを仕込んだ。さらに、前記のフラスコに、ジフェニルメタンジイソシアネート100.1g(0.4モル)と、ポリカーボネートジオール(クラレ社製「C-2015N」、数平均分子量:約2000、水酸基当量=1000g/eq.、不揮発成分:100%)400g(0.2モル)とを仕込んで、70℃で4時間反応を行った。
発明協会公開技報公技番号2020-500211号の合成例1に記載の方法で合成された下記式(1)で表されるマレイミド化合物A(Mw/Mn=1.81、a’=1.47(主に1、2又は3))を準備した。
ビスフェノールA型エポキシ樹脂(三菱ケミカル社製「828EL」、エポキシ当量189g/eq.)5部、ビフェニル型エポキシ樹脂(日本化薬社製「NC3000L」、エポキシ当量271g/eq.)1部、カルボジイミド系硬化剤(日清紡ケミカル社製「V-03」、活性基当量約216、固形分50質量%のトルエン溶液)1部、クレゾールノボラック樹脂(DIC社製「KA-1160」、フェノール性水酸基当量:117g/eq.)3部、エラストマーA(固形分50質量%のPGMEA溶液)20部、マレイミド化合物(デザイナーモレキュールズ製「BMI-689」)4部、アミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C2」、平均粒径0.5μm、比表面積5.8m2/g)65部、硬化促進剤(四国化成工業社製、「1B2PZ」、1-ベンジル-2-フェニルイミダゾール)0.05部、メチルエチルケトン(MEK)10部、及びシクロヘキサノン(Anone)5部を混合し、高速回転ミキサーで均一に分散して、ワニス状の樹脂組成物(樹脂ワニス)を調製した。
カルボジイミド系硬化剤(日清紡ケミカル社製「V-03」、活性基当量約216、固形分50質量%のトルエン溶液)1部を使用せず、クレゾールノボラック樹脂(DIC社製「KA-1160」、フェノール性水酸基当量:117g/eq.)の使用量を3部から3.5部に変更し、さらにトルエン0.5部を加えたこと以外は、実施例1と同様にして、樹脂シートを作製した。
アミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C2」、平均粒径0.5μm、比表面積5.8m2/g)の使用量を65部から60部に変更し、カルボジイミド系硬化剤(日清紡ケミカル社製「V-03」、活性基当量約216、固形分50質量%のトルエン溶液)1部を使用せず、マレイミド化合物(デザイナーモレキュールズ製「BMI-689」)4部を使用せず、クレゾールノボラック樹脂(DIC社製「KA-1160」、フェノール性水酸基当量:117g/eq.)の使用量を3部から3.5部に変更し、さらにトルエン0.5部を加えたこと以外は、実施例1と同様にして、樹脂シートを作製した。
ビスフェノールA型エポキシ樹脂(三菱ケミカル社製「828EL」、エポキシ当量189g/eq.)5部、ビフェニル型エポキシ樹脂(日本化薬社製「NC3000L」、エポキシ当量271g/eq.)1部、活性エステル系硬化剤(DIC社製「HPC-8000L-65TM」、活性基当量約223、不揮発成分65質量%のトルエン:MEK=1:1の溶液)3部、トリアジン骨格含有クレゾールノボラック系硬化剤(DIC社製「LA3018-50P」、水酸基当量151、不揮発成分50%のプロピレングリコールモノメチルエーテル(PGM)溶液)2部、エラストマーA(固形分50質量%のPGMEA溶液)10部、マレイミド化合物Aを4部、アミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C2」、平均粒径0.5μm、比表面積5.8m2/g)60部、硬化促進剤(和光純薬工業社製「4-ジメチルアミノピリジン」)0.05部、メチルエチルケトン(MEK)9.48部、トルエン0.53部、及びシクロヘキサノン(Anone)5部を混合し、高速回転ミキサーで均一に分散して、ワニス状の樹脂組成物(樹脂ワニス)を調製した。こうして得られた樹脂組成物(樹脂ワニス)を用いて、実施例1と同様にして、樹脂シートを作製した。
活性エステル系硬化剤(DIC社製「HPC-8000L-65TM」、活性基当量約223、不揮発成分65質量%のトルエン:MEK=1:1の溶液)3部を使用せず、トリアジン骨格含有クレゾールノボラック系硬化剤(DIC社製「LA3018-50P」、水酸基当量151、不揮発成分50%のプロピレングリコールモノメチルエーテル(PGM)溶液)の使用量を2部から5.9部に変更し、メチルエチルケトン(MEK)の使用量を9.48部から10部に変更し、トルエン0.53部を使用しなかったこと以外は、実施例4と同様にして、樹脂シートを作製した。
アミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C2」、平均粒径0.5μm、比表面積5.8m2/g)65部の代わりにアミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C4」、平均粒径1.1μm、比表面積4.5m2/g)50部を使用し、硬化促進剤(四国化成工業社製、「1B2PZ」、1-ベンジル-2-フェニルイミダゾール)0.05部の代わりに硬化促進剤(和光純薬工業社製「4-ジメチルアミノピリジン」)0.05部を使用し、マレイミド化合物(デザイナーモレキュールズ製「BMI-689」)4部の代わりにマレイミド化合物Aを4部使用し、メチルエチルケトン(MEK)の使用量を10部から15部に変更したこと以外は、実施例1と同様にして、樹脂シートを作製した。
ビスフェノールA型エポキシ樹脂(三菱ケミカル社製「828EL」、エポキシ当量189g/eq.)3部、ビフェニル型エポキシ樹脂(日本化薬社製「NC3000L」、エポキシ当量271g/eq.)1部、ナフトールアラルキル型エポキシ樹脂(日鉄ケミカル&マテリアル社製「ESN475V」、エポキシ当量332g/eq.)2部、エラストマーB(固形分50質量%のPGMEA溶液)10部、ダウ・ケミカル日本社製「パラロイドEXL-2655」5部、活性エステル系硬化剤(エア・ウォーター社製「PC1300-02-65MA」、活性基当量約199、不揮発成分65質量%のMAK溶液)4.6部、硬化促進剤(和光純薬工業社製「4-ジメチルアミノピリジン」)0.05部、熱可塑性樹脂(三菱ケミカル社製「YX7200B35」、不揮発性分35%のAnone溶液)3部、アミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C2」、平均粒径0.5μm、比表面積5.8m2/g)50部、メチルエチルケトン(MEK)15部、ジエチレングリコールモノエチルエーテルアセテート(EDGAC)1部を混合し、高速回転ミキサーで均一に分散して、ワニス状の樹脂組成物(樹脂ワニス)を調製した。こうして得られた樹脂組成物(樹脂ワニス)を用いて、実施例1と同様にして、樹脂シートを作製した。
メチルエチルケトン(MEK)10部の代わりにトルエン10部を使用したこと以外は、実施例1と同様にして、樹脂シートを作製した。
アミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C2」、平均粒径0.5μm、比表面積5.8m2/g)の使用量を65部から40部に変更し、エラストマーA(固形分50質量%のPGMEA溶液)の使用量を20部から1部に変更し、メチルエチルケトン(MEK)10部の代わりにトルエン10部を使用したこと以外は、実施例1と同様にして、樹脂シートを作製した。
メチルエチルケトン(MEK)10部の代わりにトルエン5部を使用し、さらにジエチレングリコールモノブチルエーテル(DB)5部を加えたこと以外は、実施例1と同様にして、樹脂シートを作製した。
アミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C2」、平均粒径0.5μm、比表面積5.8m2/g)の使用量を65部から85部に変更し、カルボジイミド系硬化剤(日清紡ケミカル社製「V-03」、活性基当量約216、固形分50質量%のトルエン溶液)の使用量を1部から10部に変更し、メチルエチルケトン(MEK)10部の代わりにトルエン10.5部を使用したこと以外は、実施例1と同様にして、樹脂シートを作製した。
アミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C2」、平均粒径0.5μm、比表面積5.8m2/g)65部の代わりにアミノシラン系カップリング剤(信越化学工業社製「KBM573」)で表面処理された球形シリカ(アドマテックス社製「SO-C4」、平均粒径1.1μm、比表面積4.5m2/g)20部を使用し、メチルエチルケトン(MEK)10部の代わりにトルエン10部を使用したこと以外は、実施例1と同様にして、樹脂シートを作製した。
実施例及び比較例で作製した樹脂シートから樹脂組成物層の一部を5mg測り取り、GCMS-QP2020-NX(島津製作所製)にて250℃、10分のオーブン条件で測り取ったサンプルを処理し、サンプルライン温度260℃、トランスファーライン温度260℃、サイクルタイム55分の条件で測定した。検出された各ピークから溶剤種を特定し、予め作製しておいた検量線と照らし合わせることで、支持体付き樹脂シートの樹脂シート中に含有されている有機溶剤の種類と含有量を解析した。
実施例及び比較例で作製した樹脂シートを10cm×10cmに裁断し、これらを十分に乾燥したシリカゲルと一緒にデシケーターに入れ、30分放置した。その後、保護フィルムを剥離した状態で樹脂シートの質量(g)を測定し、その値をα1(g)とした。次に、樹脂シートを190℃のオーブンで30分加熱して、先ほど同様シリカゲルと一緒にデシケーター中で30分放冷した後に再度樹脂シートの質量(g)を測定し、その値をα2(g)とした。また、支持体のみを10cm×10cmに裁断し、それを30分間デシケーターで放置した後、支持体の質量(g)を測定し、その値をβ(g)とした。下記式(A)から樹脂シートを190℃で30分加熱処理した時の樹脂組成物層の重量減少率α(%)の値を算出した。
実施例及び比較例で作製した樹脂シートの樹脂組成物層の溶融粘度を測定した。ユー・ビー・エム社製「Rheosol-G3000」を使用して、樹脂量は1g、直径18mmのパラレルプレートを使用し、開始温度60℃から200℃まで、昇温速度5℃/分、測定温度間隔2.5℃、振動1Hz/degの測定条件にて溶融粘度を測定し、以下の評価基準で評価した。
「〇」:100℃における溶融粘度が50,000Poise以下の場合
「×」:100℃における溶融粘度が50,000Poiseを上回る場合
(1)内層基板の用意
内層回路を形成した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、基板の厚さ0.4mm、パナソニック社製「R1515A」)の両面をマイクロエッチング剤(メック社製「CZ8101」)にて1μmエッチングして銅表面の粗化処理を行った。
実施例及び比較例で作製した樹脂シートから保護フィルムを剥がして、樹脂組成物層を露出させた。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基板と接するように、内層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以下に調整した後、120℃、圧力0.74MPaにて30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60秒間熱プレスを行った。
その後、樹脂シートがラミネートされた内層基板を、130℃のオーブンに投入して30分間加熱し、次いで170℃のオーブンに移し替えて30分間加熱して、樹脂組成物層を熱硬化させて、絶縁層を形成した。その後、支持体を剥離して、絶縁層、内層基板及び絶縁層をこの順に有する硬化基板を得た。
硬化基板の両面について、樹脂シートがラミネートされた部分(積層板とは反対側の表面)の表面均一性の観察を目視にて行い、下記の評価基準で評価した。
「〇」:ムラが全く観察されず、完全に均一な表面である、もしくは樹脂シートがラミネートされた部分の外周から1cmの部分のみにムラが観察され、それより内側の部分は完全に均一な表面である場合
「×」:樹脂シートがラミネートされた部分の外周から1cmより内側の部分に、不均一な部分が観察される場合
12インチシリコンウエハ(厚さ775μm)の片面全体に、実施例及び比較例で作製した樹脂シートを、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」)を用いてラミネートし、支持体を剥離した。12インチシリコンウエハにラミネートした樹脂組成物層上に、さらに樹脂シートをラミネートすることで樹脂組成物層を2層積層し、厚さ100μmの樹脂組成物層を形成した。得られた樹脂組成物層付きシリコンウエハをオーブン中180℃および90分の条件で熱処理して、硬化した樹脂組成物層(即ち、絶縁層)付きシリコンウエハを形成した。シャドウモアレ測定装置(Akorometrix社製「ThermoireAXP」)を用いて、前記の絶縁層付きシリコンウエハの25℃での反り量を測定した。測定は、電子情報技術産業協会規格のJEITA EDX-7311-24に準拠して行った。具体的には、測定領域の基板面の全データの最小二乗法によって算出した仮想平面を基準面として、その基準面から垂直方向の最小値と最大値との差を反り量として求め、下記の評価基準で評価した。
「○」:反り量が2mm以下の場合
「×」:反り量が2mmより大きい場合
実施例及び比較例で作製した樹脂シートの一部を切り出し、180℃にて90分間加熱して、樹脂組成物層を熱硬化させた。その後、支持体を剥離し、評価用硬化物を得た。
「〇」:誘電正接(Df)が0.008以下の場合
「△」:誘電正接(Df)が0.008より大きく、0.010未満の場合
「×」:誘電正接(Df)が0.010以上の場合
Claims (21)
- 支持体と、当該支持体上に設けられた樹脂組成物層と、を有する樹脂シートであって、
樹脂組成物層が、(A)エポキシ樹脂、(B)有機溶剤、(C)無機充填材、(D)応力緩和材、及び(G)ラジカル重合性化合物を含み、
(B)成分が、沸点120℃以上220℃未満の有機溶剤を含み、
(B)成分中のトルエンの含有量が、全(B)成分を100質量%とした場合、0質量%~9質量%であり、
(B)成分中の沸点120℃未満の有機溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~30質量%である、樹脂シート。 - 支持体と、当該支持体上に設けられた樹脂組成物層と、を有する樹脂シートであって、
樹脂組成物層が、(A)エポキシ樹脂、(B)有機溶剤、(C)無機充填材、(D)応力緩和材、及び(G)ラジカル重合性化合物を含み、
(B)成分中のトルエンの含有量が、全(B)成分を100質量%とした場合、0質量%~9質量%であり、
(B)成分中の沸点120℃以上220℃未満の有機溶剤の含有量が、全(B)成分を100質量%とした場合、85質量%以上である、樹脂シート。 - 樹脂組成物層中の(D)成分の含有量が、樹脂組成物層中の不揮発成分を100質量%とした場合、1質量%以上である、請求項1又は2に記載の樹脂シート。
- 樹脂組成物層中の(C)成分の含有量が、樹脂組成物層中の不揮発成分を100質量%とした場合、60質量%以上である、請求項1~3の何れか1項に記載の樹脂シート。
- 樹脂組成物層中の不揮発成分を100質量%とした場合の(C)成分の含有量(質量%)の値と(C)成分の比表面積(m2/g)の値との積が、300以上である、請求項1~4の何れか1項に記載の樹脂シート。
- (B)成分中の沸点220℃以上の有機溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~10質量%である、請求項1~5の何れか1項に記載の樹脂シート。
- (B)成分中の芳香族性溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~9質量%である、請求項1~6の何れか1項に記載の樹脂シート。
- (D)成分が、ポリブタジエン構造及びポリカーボネート構造から選ばれる1種以上の構造を有する樹脂を含む非粒子状の応力緩和材を含む、請求項1~7の何れか1項に記載の樹脂シート。
- (D)成分が、粒子状の応力緩和材を含む、請求項1~8の何れか1項に記載の樹脂シート。
- 粒子状の応力緩和材の平均粒径が、10,000nm以下である、請求項9に記載の樹脂シート。
- 樹脂組成物層が、(E)硬化剤をさらに含む、請求項1~10の何れか1項に記載の樹脂シート。
- (E)成分が、活性エステル系硬化剤及びカルボジイミド系硬化剤から選ばれる1種以上の硬化剤を含む、請求項11に記載の樹脂シート。
- (E)成分が、活性エステル系硬化剤を含む、請求項12に記載の樹脂シート。
- 樹脂組成物層が、(F)硬化促進剤をさらに含む、請求項1~13の何れか1項に記載の樹脂シート。
- (G)成分が、マレイミド基を有する、請求項1~14の何れか1項に記載の樹脂シート。
- 支持体と接しない面を外気に露出し190℃で30分間加熱処理した後の樹脂組成物層の重量減少率が、1質量%~10質量%となる、請求項1~15の何れか1項に記載の樹脂シート。
- 樹脂組成物層の硬化後の誘電正接(Df)が、10GHz、23℃で測定した場合、0.0090以下である、請求項1~16の何れか1項に記載の樹脂シート。
- 樹脂組成物層の100℃における溶融粘度が、50,000poise以下である、請求項1~17の何れか1項に記載の樹脂シート。
- 下記(I)及び(II)の工程を含むプリント配線板の製造方法。
(I)請求項1~18の何れか1項に記載の樹脂シートを、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
(II)樹脂組成物層を硬化して絶縁層を形成する工程 - (A)エポキシ樹脂、(B)有機溶剤、(C)無機充填材、(D)応力緩和材、及び(G)ラジカル重合性化合物を含み、
(B)成分が、沸点120℃以上220℃未満の有機溶剤を含み、
(B)成分中のトルエンの含有量が、全(B)成分を100質量%とした場合、0質量%~9質量%であり、
(B)成分中の沸点120℃未満の有機溶剤の含有量が、全(B)成分を100質量%とした場合、0質量%~30質量%である、樹脂組成物。 - (A)エポキシ樹脂、(B)有機溶剤、(C)無機充填材、(D)応力緩和材、及び(G)ラジカル重合性化合物を含み、
(B)成分中のトルエンの含有量が、全(B)成分を100質量%とした場合、0質量%~9質量%であり、
(B)成分中の沸点120℃以上220℃未満の有機溶剤の含有量が、全(B)成分を100質量%とした場合、85質量%以上である、樹脂組成物。
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