JP2019038997A - 樹脂シートおよび粘着剤層付樹脂シート - Google Patents
樹脂シートおよび粘着剤層付樹脂シート Download PDFInfo
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- JP2019038997A JP2019038997A JP2018143561A JP2018143561A JP2019038997A JP 2019038997 A JP2019038997 A JP 2019038997A JP 2018143561 A JP2018143561 A JP 2018143561A JP 2018143561 A JP2018143561 A JP 2018143561A JP 2019038997 A JP2019038997 A JP 2019038997A
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Abstract
Description
主面Aおよび主面Bが厚みdで対抗している樹脂シートであって、
JIS K 6767:1999に記載の圧縮硬さの測定方法に準じて測定した厚みd方向の23±5℃における50%圧縮荷重が20N/cm2以下であり、
23℃におけるポアソン比が0.10以下であり、
23℃において厚みd方向に20%圧縮した際の厚み回復率が40%以上である。
本発明の一つの実施形態における樹脂シートは、主面Aおよび主面Bが厚みdで対抗している樹脂シートである。具体的には、図1に示すように、本発明の樹脂シート1000は、主面A100と、主面B200が厚みdで対抗している。
本発明の一つの実施形態である粘着剤層付樹脂シートは、本発明の一つの実施形態である樹脂シートと粘着剤層を有する。粘着剤層は、樹脂シートの一方の側に備えられていてもよいし、両方の側に備えられていてもよい。粘着剤層は、1層のみであってもよいし、2層以上であってもよい。
JIS K 6767に記載されている圧縮硬さ測定法に準じて測定した。測定対象のシートを30mm×30mmに切り出し、厚み10mmに調整して(例えば、シート厚みが0.2mmの場合は50枚積層させることで)シート状の試験片とした。なお、このとき30mm×30mm×10mmの試験片は略直方体となるようした。次に、この試験片を、23±5℃、圧縮速度:10mm/minで、厚み方向に、圧縮率が50%になるまで圧縮したときの応力(N)を単位面積(1cm2)当たりに換算し、50%圧縮荷重とした。
マイクロオートグラフ((株)島津製作所社製、MST−200NX)のサンプル設置面に、測定対象のシートを10mm×10mmに切り出し、厚み1mmに調整して(例えば、シート厚みが0.2mmの場合は5枚積層させることで)シート状の試験片とした。なお、このとき10mm×10mm×1mmの試験片は略直方体となるようした。試験片に対してカメラが正対するような位置にカメラを設置した。すなわち、カメラから見たときに、試験片の10mmの辺が最も長く映るようにカメラを設置した。23℃にて、オートグラフの圧縮治具を速度10mm/minで動かし、試験片の厚みが0.2mmになるまで圧縮した。そのときの画像から、圧縮前に10mmだった辺の圧縮後の長さX(mm)を求め、下記式によりポアソン比を求めた。
ポアソン比=│{(X−10)/10}/{(0.2−1)/1}│
(「│(数値A)│」は、数値Aの絶対値を表す。)
測定対象のシートを10mm×10mmに切り出し、厚み1mmに調整して(例えば、シート厚みが0.2mmの場合は5枚積層させることで)シート状の試験片とした。なお、このとき10mm×10mm×1mmの試験片は略直方体となるようした。圧縮試験機((株)島津製作所社製、マイクロサーボ)を用いて、23℃にて、厚み方向に、初期厚み(1mm)に対して20%の厚みに1分間圧縮し、圧縮解除し、圧縮解除1秒後の厚みの回復挙動を、高速度カメラを用いて撮影した。厚み回復率は、圧縮解除1秒後の厚みの初期厚みに対する割合として表した。
測定対象の発泡体樹脂のシートの流れ方向(MD)と平行に切断した際の断面をマイクロスコープ(Keyence製、VHX−900F、リング照明OP−72404、倍率100倍)で観察し、撮影された断面セル画像を、画像処理ソフト「ImageJ」を用いて、しきい値「75」で二値化した際のセル壁の割合(白部分となる)を「セル壁比率」とした。
測定対象の発泡体樹脂のシートのMD方向(流れ方向)に対する直交方向に平行に、カッターにて測定対象の発泡体樹脂のシートの主面(延長する面)に対して垂直方向(厚み方向)に切断し、平滑な断面を作成した。これら断面をデジタルマイクロスコープ(Keyence製、VHX−500)により、測定対象の発泡体樹脂のシートのセルの拡大画像を取り込み、同計測器の解析ソフト(三谷商事(株)製、Win ROOF)を用いて、画像解析することにより、平均セル径(μm)を求めた。拡大画像内のセルのうち、面積の大きいものから10個のセルを解析に用いて平均直径を算出し、これを平均セル径とした。
測定対象の発泡体樹脂のシートを、40mm×40mmサイズに打ち抜き、試験片とし、試験片の寸法を測定した。また、測定端子φ20mmの1/100ダイヤルゲージにて厚みを測定した。これらの値から測定対象のシートの体積を算出した。次に、測定対象のシートの質量を、最小目盛り0.01g以上の上皿天秤にて測定した。これらの値から、測定対象のシートの見掛け密度を算出した。
見掛け密度(g/cm3)=試験片の質量/試験片の体積
十分な体積の発泡体を切り出して積層した後、加熱機能を有する真空プレス機を用いて1分間圧縮することにより、厚み0.3mmの樹脂シートを得た。加熱温度は発泡体樹脂の融点付近で未溶融や熱劣化の無い範囲で設定を行った。
熱伝導率の測定は図2((a)が正面図、(b)が側面図)に示す熱特性評価装置を用いて行った。具体的には、1辺が20mmの立方体となるように形成されたアルミニウム製(A5052、熱伝導率:140W/m・K)の一対のブロック(ロッドと称する場合もある)L間に、熱伝導性粘着剤S(20mm×20mm)を挟み込み、一対のブロックLを接着シートで貼り合わせた。そして、一対のブロックLが上下となるように発熱体(ヒーターブロック)Hと放熱体(冷却水が内部を循環するように構成された冷却ベース板)Cとの間に配置した。具体的には、上側のブロックLの上に発熱体Hを配置し、下側のブロックLの下に放熱体Cを配置した。この際、熱伝導性粘着剤Sで貼りあわされた一対のブロックLは、発熱体Hおよび放熱体Cを貫通する一対の圧力調整用ネジTの間に位置している。なお、圧力調整用ネジTと発熱体Hとの間にはロードセルRが配置されており、圧力調整用ネジTを締めこんだ際の圧力が測定されるように構成されており、斯かる圧力を熱伝導性粘着シートSに加わる圧力として用いた。具体的には、この試験において、圧力調整用ネジTを、熱伝導性粘着剤Sに加わる圧力が25N/cm2(250kPa)となるように締めこんだ。また、下側のブロックLおよび熱伝導性粘着剤Sを放熱体C側から貫通するように接触式変位計の3本のプローブP(直径1mm)を設置した。この際、プローブPの上端部は、上側のブロックLの下面に接触した状態になっており、上下のブロックL間の間隔(熱伝導性粘着剤Sの厚み)を測定可能に構成されている。発熱体Hおよび上下のブロックLには温度センサーDを取り付けた。具体的には、発熱体Hの1箇所に温度センサーDを取り付け、各ブロックLの5箇所に上下方向に5mm間隔で温度センサーDをそれぞれ取り付けた。測定はまず初めに、圧力調整用ネジTを締めこんで、熱伝導性粘着剤Sに圧力を加え、発熱体Hの温度を80℃に設定するともに、放熱体Cに20℃の冷却水を循環させた。そして、発熱体Hおよび上下のブロックLの温度が安定した後、上下のブロックLの温度を各温度センサーDで測定し、上下のブロックLの熱伝導率(W/m・K)と温度勾配から熱伝導性粘着剤Sを通過する熱流束を算出するとともに、上下のブロックLと熱伝導性粘着剤Sとの界面の温度を算出した。そして、これらを用いて圧力における熱伝導率(W/m・K)および熱抵抗(cm2・K/W)を、下記の熱伝導率方程式(フーリエの法則)を用いて算出した。
Q=−λgradT
R=L/λ
Q:単位面積あたりの熱流速
gradT:温度勾配
L:シートの厚み
λ:熱伝導率
R:熱抵抗
厚み2mmのポリカーボネート(PC)板より形成したステージに熱電対を備えたセラミックヒーター(25mm角)を設置した。測定対象のシートを25mm×25mmに切断し、セラミックヒーター上に貼り合せた後、上から筐体とするPC板(160mm×160mm×2mm)を組付けた。筐体のPC板とセラミックヒーター間の隙間は0.2mmに設定し、PC板の左半分に0.1mmのPETフィルムを貼り合わせ、隙間には0.1mmの段差をつけた。セラミックヒーターに2Aの電流を流して加熱し、5分後のセラミックヒーターの温度を熱電対で測定し、筐体表面温度をサーモグラフィー(NEC製、TH7800)にて測定した。サーモグラフィーにて測定した熱分布画像を、レポート作成プログラム(NEC三栄社製、NS9200)にて解析を行い、ヒーターの中心部から左右に9mmずつ離れた点の温度を観測した。PETフィルムが入っている側をA、入っていない側をBとし、A−Bの値を部分的な加熱評価の指標とした。
熱伝導性粘着剤の熱伝導率および熱抵抗の測定は、図2((a)が正面図、(b)が側面図)に示す熱特性評価装置を用いて行った。具体的には、1辺が20mmの立方体となるように形成されたアルミニウム製(A5052、熱伝導率:140W/m・K)の一対のブロック(ロッドと称する場合もある)L間に、熱伝導性粘着剤S(20mm×20mm)を挟み込み、一対のブロックLを接着シートで貼り合わせた。そして、一対のブロックLが上下となるように発熱体(ヒーターブロック)Hと放熱体(冷却水が内部を循環するように構成された冷却ベース板)Cとの間に配置した。具体的には、上側のブロックLの上に発熱体Hを配置し、下側のブロックLの下に放熱体Cを配置した。この際、熱伝導性粘着剤Sで貼りあわされた一対のブロックLは、発熱体Hおよび放熱体Cを貫通する一対の圧力調整用ネジTの間に位置している。なお、圧力調整用ネジTと発熱体Hとの間にはロードセルRが配置されており、圧力調整用ネジTを締めこんだ際の圧力が測定されるように構成されており、斯かる圧力を熱伝導性粘着シートSに加わる圧力として用いた。具体的には、この試験において、圧力調整用ネジTを、熱伝導性粘着剤Sに加わる圧力が25N/cm2(250kPa)となるように締めこんだ。また、下側のブロックLおよび熱伝導性粘着剤Sを放熱体C側から貫通するように接触式変位計の3本のプローブP(直径1mm)を設置した。この際、プローブPの上端部は、上側のブロックLの下面に接触した状態になっており、上下のブロックL間の間隔(熱伝導性粘着剤Sの厚み)を測定可能に構成されている。発熱体Hおよび上下のブロックLには温度センサーDを取り付けた。具体的には、発熱体Hの1箇所に温度センサーDを取り付け、各ブロックLの5箇所に上下方向に5mm間隔で温度センサーDをそれぞれ取り付けた。測定はまず初めに、圧力調整用ネジTを締めこんで、熱伝導性粘着剤Sに圧力を加え、発熱体Hの温度を80℃に設定するともに、放熱体Cに20℃の冷却水を循環させた。そして、発熱体Hおよび上下のブロックLの温度が安定した後、上下のブロックLの温度を各温度センサーDで測定し、上下のブロックLの熱伝導率(W/m・K)と温度勾配から熱伝導性粘着剤Sを通過する熱流束を算出するとともに、上下のブロックLと熱伝導性粘着剤Sとの界面の温度を算出した。そして、これらを用いて圧力における熱伝導率(W/m・K)および熱抵抗(cm2・K/W)を、下記の熱伝導率方程式(フーリエの法則)を用いて算出した。
Q=−λgradT
R=L/λ
Q:単位面積あたりの熱流速
gradT:温度勾配
L:シートの厚み
λ:熱伝導率
R:熱抵抗
粘着剤原料の粘度は、BM粘度計(No.4ロータ、12rpm、測定温度23℃)によって測定した。
熱伝導性粘着剤を、幅10mm、長さ60mmに切断して試料とし、JIS K 6767に準じて引張試験を実施した。試料からベースフィルムおよびカバーフィルムを剥がし、23℃、50%RH雰囲気下、万能引張試験機「TCM−1kNB」(ミネベア社製)を用い、チャック間距離20mm、引っ張り速度300mm/minで応力−ひずみ曲線を測定した。測定された、応力−ひずみ曲線から、下記式により、引張強さおよび伸びを計算した。また、得られた応力−ひずみ曲線の初期の立ち上がりの部分に接線を引き、その接線が100%伸びに相当するときの荷重(N)を試料の断面積(mm2)で割って、引張弾性率(MPa)とした。
引張強さ(MPa)=試料が破断するまでの最大荷重(N)/試料の断面積(mm2)
伸び(%)={(破断時の試料のチャック間長さ(mm)−20(mm))/20(mm)}×100
熱伝導性粘着剤のベースフィルム(またはカバーフィルム)を剥がして、厚み25μmのPETフィルムを貼り合わせ、これを幅20mm、長さ150mmに切断して評価用サンプルとした。評価用サンプルから残りのカバーフィルム(またはベースフィルム)を剥がし、23℃、50%RH雰囲気下で、熱伝導性粘着剤をアルミニウム板(#1050)に貼り付け、PETフィルムの上から2kgローラーを1往復させて、熱伝導性粘着剤をアルミニウム板に押し付けた。23℃で30分間養生した後、万能引張試験機「TCM−1kNB」(ミネベア社製)を用い、剥離角度90度、引っ張り速度300mm/分で、90度剥離接着力を、JIS Z 0237に準じて測定した。
熱伝導性粘着剤を用いて、JIS K 7312に準じて、下記条件にて試験を実施した。詳しくは、熱伝導性粘着剤を幅20mm、長さ20mmに切断し、厚みが4mmになるように積層させたものを評価用サンプルとして、アスカーC硬度計(高分子計器社製)で、23℃、50%RH雰囲気下において、アスカーC硬度計の加圧面を密着させてから30秒後の硬さ(アスカーC硬度)を測定した。
熱伝導性粘着剤を、20mm×10mmの大きさに裁断した後、25μm厚のPETフィルムに貼付けて、サンプルとした。次いで、23℃、50%RH環境下で、サンプルの上端部10mm×20mmの部分を、剥離面をステンレス鋼(SUS304BA)板の下端部に載置して、2kgのローラーで1往復することにより、熱伝導性粘着剤をステンレス鋼板に貼着した。その後、80℃環境下で、30分間、静置して貼着(接着)状態を安定させた(養生)後、ステンレス鋼板の上端部を固定して、サンプルの下端部に300gのおもりを80℃の条件で垂下した。そして、80℃環境下で、1時間放置させたときの、サンプルのステンレス鋼に対するズレ量(移動距離)を測定した。
ポリプロピレン(メルトフローレート(MFR):0.35g/10min):52重量部、熱可塑性オレフィン系エラストマー(エチレン−プロピレン共重合体エラストマー)と軟化剤(パラフィン系伸展油)の混合物(MFR(230℃):6g/10分、JIS A硬度:79度、軟化剤をポリオレフィン系エラストマー100重量部に対して30重量部配合):48重量部、カーボンブラック(商品名「旭♯35」、旭カーボン(株)製):5重量部、水酸化マグネシウム:10重量部、ステアリン酸モノグリセリド:3重量部、および脂肪酸アミド(ラウリン酸ビスアミド):1重量部を、(株)日本製鋼所(JSW)製の二軸混練機にて、200℃の温度で混練した後、ストランド状に押出し、水冷後ペレット状に成形した。このペレットを、(株)日本製鋼所製の単軸押出機に投入し、220℃の雰囲気下、13(注入後12)MPaの圧力で、二酸化炭素ガスを注入した。二酸化炭素ガスは、ペレット全量に対して5.6重量%の割合で注入した。二酸化炭素ガスを十分飽和させた後、発泡に適した温度まで冷却し、ダイから円筒状に押出して、発泡体の内側表面を冷却するマンドレルと、押出機の環状ダイから押し出された円筒状の発泡体の外側表面を冷却する発泡体冷却用エアリングの間を通過させ、直径の一部を切断してシート状に展開して長尺発泡体原反を得た。この長尺発泡体原反を所定の幅に切断し(スリット加工)、連続スライス装置(スライスライン)を用いて、1面ずつ表面の低発泡層を剥がしとり、樹脂発泡体(1)(厚み:0.30mm)を得た。
(株)日本製鋼所(JSW)製の二軸混練機にて混練する材料を、ポリプロピレン(メルトフローレート(MFR):0.45g/10min):42重量部、熱可塑性オレフィン系エラストマー(エチレン−プロピレン共重合体エラストマー)と軟化剤(パラフィン系伸展油)の混合物(MFR(230℃):6g/10分、JIS A硬度:79度、軟化剤をポリオレフィン系エラストマー100重量部に対して30重量部配合):55重量部、カーボンブラック(商品名「旭♯35」、旭カーボン(株)製):1重量部、水酸化マグネシウム:10重量部、ステアリン酸モノグリセリド:1.2重量部、および脂肪酸アミド(ラウリン酸ビスアミド):2.5重量部とした以外は、実施例1と同様にして、樹脂発泡体(2)、樹脂シート(2)を得た。
(樹脂発泡体(3)、樹脂シート(3)の製造)
(株)日本製鋼所(JSW)製の二軸混練機にて混練する材料を、ポリプロピレン(メルトフローレート(MFR):0.40g/10min):52重量部、熱可塑性オレフィン系エラストマー(エチレン−プロピレン共重合体エラストマー)と軟化剤(パラフィン系伸展油)の混合物(MFR(230℃):6g/10分、JIS A硬度:79度、軟化剤をポリオレフィン系エラストマー100重量部に対して30重量部配合):48重量部、カーボンブラック(商品名「旭♯35」、旭カーボン(株)製):5重量部、水酸化マグネシウム:10重量部、ステアリン酸モノグリセリド:3重量部、および脂肪酸アミド(ラウリン酸ビスアミド):1重量部とした以外は、実施例1と同様にして、樹脂発泡体(3)、樹脂シート(3)を得た。
単量体として、アクリル酸2−エチルヘキシル:90重量部、N−ビニル−2−ピロリドン(NVP):10重量部を配合し、混合して単量体の混合物を得た。得られた混合物に、光重合開始剤として、2,2−ジメトキシ−1,2−ジフェニルエタン−1−オン(商品名「イルガキュアー651」、BASF社製):0.05重量部と、1−ヒドロキシシクロヘキシルフェニルケトン(商品名「イルガキュアー184」、BASF社製):0.05重量部とを配合した。その後、混合物に紫外線を照射して、粘度(BH粘度計、No.5ロータ、10rpm、測定温度30℃)が約20Pa・sになるまで重合し、単量体の一部が重合した単量体の部分重合物(シロップ状)を調製した。得られた単量体の部分重合物:100重量部に、多官能単量体として、ジペンタエリスリトールヘキサアクリレート(商品名「KAYARAD DPHA−40H」、日本化薬社製)0.05重量部と、分散剤として、商品名「プライサーフA212E」(第一工業製薬社製)3.4重量部とを配合し、混合して、単量体組成物を調製した。
次いで、得られた単量体組成物に、第1熱伝導性粒子として、平均粒子径(体積基準)1μm、最大粒子径(体積基準)10μm未満の水酸化アルミ粉末(商品名「ハイジライトH−42」、形状:破砕状、昭和電工社製):100重量部と、第2熱伝導性粒子として、平均粒子径(体積基準)8μm、最小粒子径(体積基準)30μm以上の水酸化アルミ粉末(商品名「ハイジライトH−32」、形状:破砕状、昭和電工社製):100重量部とを配合し、混合して粘着剤原料を調製した。粘着剤原料の粘度(BM粘度計、No.4ロータ、12rpm、測定温度23℃)を表3に示す。
得られた粘着剤原料を、片面に剥離処理が施されているベースフィルム(ポリエチレンテレフタレートフィルム、商品名「ダイアホイルMRF38」、三菱化学ポリエステルフィルム社製)の剥離処理面に、乾燥および硬化後の厚みが50μmとなるように塗布した。次いで、ベースフィルムとの間に粘着剤原料の塗膜を挟むように、粘着剤原料の塗膜の上に、カバーフィルム(ベースフィルムと同じフィルム)を配置した。次いで、粘着剤原料に、紫外線(照度約5mW/cm2)を両側(ベースフィルム側およびカバーフィルム側)から3分間照射した。これにより、粘着剤原料中の単量体を重合させて、厚み50μmの熱伝導性粘着剤(3)を作製した。
得られた熱伝導性粘着剤(3)の伸び、引張弾性率、90度剥離接着力、保持力、硬さ、熱伝導率、熱抵抗を、表3に示す。
(粘着剤層付樹脂シート(3)の製造)
得られた樹脂シート(3)と熱伝導性粘着剤(3)を重ね、プレス圧力を0.2MPaに調整した小型ラミネータの樹脂ロール間を2m/minの速度で通過させることにより、粘着剤層付樹脂シート(3)を得た。
ポリオレフィン系樹脂としての直鎖状低密度ポリエチレン(日本ポリエチレン株式会社製「カーネルKF370」、密度:0.905g/cm3、融点(DSC法)Tm:97℃):100重量部、熱分解型発泡剤としてのアゾジカルボンアミド:15重量部、および、分解温度調整剤としての酸化亜鉛:2.0質量部を押出機に供給して130℃で溶融混練し、厚み約0.3mmの長尺シート状のポリオレフィン系樹脂組成物を押出した。次に、得られた長尺シート状のポリオレフィン系樹脂組成物を、その両面に加速電圧500kVの電子線を5.0Mrad照射して架橋した後、熱風および赤外線ヒーターにより250℃に保持された発泡炉内に連続的に送り込んで加熱して発泡させるとともに、発泡させながらMDの延伸倍率を3.0倍、TDの延伸倍率を2.0倍として延伸させることにより、厚み0.2mmの樹脂発泡体(4)からなる樹脂シート(4)を得た。
ハードセグメントとしてのポリブチレンテレフタレートとソフトセグメントとしてのポリエーテルとのブロック共重合体(商品名「ペルプレン P−90BD」、東洋紡株式会社製、230℃のメルトフローレート:3.0g/10min):100重量部、アクリル系滑剤(商品名「メタブレンL−1000」、三菱レイヨン株式会社製):3重量部、シランカップリング剤で表面処理加工されているハードクレー(商品名「ST−301」、白石カルシウム株式会社製):0.5重量部、カーボンブラック(商品名「旭♯35」、旭カーボン株式会社製):5重量部、および、エポキシ系アクリル樹脂(エポキシ変性アクリル系ポリマー、重量平均分子量:50000、エポキシ当量:1200g/eq、粘度:2850mPa・s):1重量部を、二軸混練機(日本製鋼所(JSW)社製)により、220℃の温度で混練した後、ストランド状に押出し、水冷後ペレット状に切断して成形した。そして、ペレット状の樹脂組成物を得た。
このペレット状の樹脂組成物を単軸押出機(日本製鋼所社(JSW)製)に投入し、240℃の雰囲気中、17(注入後13)MPaの圧力で、二酸化炭素ガスをペレット状の樹脂組成物全量(100重量%)に対して、3.3重量%の割合で注入した。二酸化炭素ガスを十分飽和させた後、発泡に適した温度まで冷却後、ダイから押出して、発泡体の内側表面を冷却するマンドレルと、押出機の環状ダイから押し出された円筒状の発泡体の外側表面を冷却する発泡体冷却用エアリングの間を通過させ、直径の一部を切断してシート状に展開して長尺発泡体原反を得た。この長尺発泡体原反を所定の幅に切断し(スリット加工)、連続スライス装置(スライスライン)を用いて、1面ずつ表面の低発泡層を剥がしとり、樹脂発泡体(5)(厚み:0.30mm)を得た。
EPDM(「EPT3045」、三井化学社製、ジエン含量4.7重量%):40重量部、EPDM(「EP−24」、JSR社製、ジエン含量4.5重量%):60重量部、顔料としてカーボンブラック(「旭#50」、旭カーボン社製):15重量部、加硫助剤として酸化亜鉛(三井金属鉱業社製):4重量部、滑剤としてステアリン酸(「粉末ステアリン酸さくら」、日油社製):5重量部、充填材として炭酸カルシウム(「N重質炭酸カルシウム」、丸尾カルシウム社製):120重量部、軟化剤としてパラフィン(「パラペレ130」、谷口石油社製、融点:54.4〜57.2℃、針入度:50以下):10重量部、アスファルトとしてブローンアスファルト10−20(新日本石油社製、軟化点:135〜142℃、針入度(25℃):10〜20):100重量部、パラフィン系オイルとしてパラフィン系プロセスオイル(ダイアナプロセスオイルPW−90、出光興産社製、密度:0.85〜0.89g/cm3、動粘度(40℃):75.0〜105.0cSt):40重量部、および、加硫促進剤としてチオウレア系加硫促進剤(N,N’−ジブチルチオ尿素、「ノクセラーBUR」、大内新興化学社製):1重量部を配合し、3L加圧ニーダにて混練し、一次混和物を調製した。
ポリプロピレン(メルトフローレート(MFR):0.35g/10min):52重量部、熱可塑性オレフィン系エラストマー(エチレン−プロピレン共重合体エラストマー)と軟化剤(パラフィン系伸展油)の混合物(MFR(230℃):6g/10分、JIS A硬度:79度、軟化剤をポリオレフィン系エラストマー100重量部に対して30重量部配合):48重量部、カーボンブラック(商品名「旭♯35」、旭カーボン(株)製):5重量部、水酸化マグネシウム:10重量部、ステアリン酸モノグリセリド:3重量部、および脂肪酸アミド(ラウリン酸ビスアミド):1重量部を、(株)日本製鋼所(JSW)製の二軸混練機にて、200℃の温度で混練した後、ストランド状に押出し、水冷後ペレット状に成形した。このペレットを、(株)日本製鋼所製の単軸押出機に投入し、220℃の雰囲気下、13(注入後12)MPaの圧力で、二酸化炭素ガスを注入した。二酸化炭素ガスは、ペレット全量に対して5.6重量%の割合で注入した。二酸化炭素ガスを十分飽和させた後、発泡に適した温度まで冷却し、ダイから円筒状に押出して、発泡体の内側表面を冷却するマンドレルと、押出機の環状ダイから押し出された円筒状の発泡体の外側表面を冷却する発泡体冷却用エアリングの間を通過させ、直径の一部を切断してシート状に展開して長尺発泡体原反を得た。この長尺発泡体原反を所定の幅に切断し(スリット加工)、連続スライス装置(スライスライン)を用いて、1面ずつ表面の低発泡層を剥がしとり、樹脂発泡体(7)(厚み:0.20mm)を得た。
実施例7で得られた樹脂シート(7)(すなわち、樹脂発泡体(7))と実施例3で得られた熱伝導性粘着剤(3)を重ね、プレス圧力を0.2MPaに調整した小型ラミネータの樹脂ロール間を2m/minの速度で通過させることにより、粘着剤層付樹脂シート(8)を得た。
ポリプロピレン(メルトフローレート(MFR):0.35g/10min):52重量部、熱可塑性オレフィン系エラストマー(エチレン−プロピレン共重合体エラストマー)と軟化剤(パラフィン系伸展油)の混合物(MFR(230℃):6g/10分、JIS A硬度:79度、軟化剤をポリオレフィン系エラストマー100重量部に対して30重量部配合):48重量部、カーボンブラック(商品名「ケッチェンブラックEC−600JD」、粒径D50=0.04μm、中空シェル構造、BET比表面積=1270m2/g、ライオン・スペシャリティ・ケミカルズ株式会社製):5重量部、カーボンナノチューブ(商品名「K−Nanos 100P」、チューブ径=10nm、チューブ長さ=1.5μm、アスペクト比=150、Korea Kumho Petrochemical製):7重量部、水酸化マグネシウム:10重量部、およびステアリン酸モノグリセリド:1重量部を、(株)日本製鋼所(JSW)製の二軸混練機にて、200℃の温度で混練した後、ストランド状に押出し、水冷後ペレット状に成形した。このペレットを、(株)日本製鋼所製の単軸押出機に投入し、220℃の雰囲気下、13(注入後12)MPaの圧力で、二酸化炭素ガスを注入した。二酸化炭素ガスは、ペレット全量に対して5.6重量%の割合で注入した。二酸化炭素ガスを十分飽和させた後、発泡に適した温度まで冷却し、ダイから円筒状に押出して、発泡体の内側表面を冷却するマンドレルと、押出機の環状ダイから押し出された円筒状の発泡体の外側表面を冷却する発泡体冷却用エアリングの間を通過させ、直径の一部を切断してシート状に展開して長尺発泡体原反を得た。この長尺発泡体原反を所定の幅に切断し(スリット加工)、連続スライス装置(スライスライン)を用いて、1面ずつ表面の低発泡層を剥がしとり、樹脂発泡体(9)(厚み:0.30mm)を得た。
実施例9で得られた樹脂シート(9)(すなわち、樹脂発泡体(9))と実施例3で得られた熱伝導性粘着剤(3)を重ね、プレス圧力を0.2MPaに調整した小型ラミネータの樹脂ロール間を2m/minの速度で通過させることにより、粘着剤層付樹脂シート(10)を得た。
アクリルエマルション溶液(固形分量55%、アクリル酸エチル−アクリル酸ブチル−アクリロニトリル共重合体(重量比45:48:7)):100重量部、脂肪酸アンモニウム系界面活性剤(ステアリン酸アンモニウムの水分散液、固形分量33%)(界面活性剤A):1.6重量部、カルボキシベタイン型両性界面活性剤(「アモーゲンCB−H」、第一工業製薬社製)(界面活性剤B):1.6重量部、オキサゾリン系架橋剤(「エポクロスWS−500」日本触媒社製、固形分量39%):6重量部、顔料(カーボンブラック)(「NAF−5091」大日精化工業社製):2重量部、ポリアクリル酸系増粘剤(アクリル酸エチル−アクリル酸共重合体(アクリル酸20重量%)、固形分量28.7%):0.8重量部をディスパー(「ロボミックス」プライミクス社製)で撹拌混合して起泡化した。この発泡組成物を、剥離処理をしたPET(ポリエチレンテレフタレート)フィルム(厚さ:38μm、商品名「MRF♯38」三菱樹脂社製)上に塗布し、70℃で4.5分、140℃で4.5分乾燥させ、樹脂発泡体(11)(厚み:0.20mm)を得た。
実施例11で得られた樹脂シート(11)(すなわち、樹脂発泡体(11))と実施例3で得られた熱伝導性粘着剤(3)を重ね、プレス圧力を0.2MPaに調整した小型ラミネータの樹脂ロール間を2m/minの速度で通過させることにより、粘着剤層付樹脂シート(12)を得た。
市販のグラファイトシート(商品名「グラフィニティー25μm」、カネカ社製、厚み:25μm)を8枚積層したシート(C1)を得た。
100 主面A
200 主面B
Claims (9)
- 主面Aおよび主面Bが厚みdで対抗している樹脂シートであって、
JIS K 6767:1999に記載の圧縮硬さの測定方法に準じて測定した厚みd方向の23±5℃における50%圧縮荷重が20N/cm2以下であり、
23℃におけるポアソン比が0.10以下であり、
23℃において厚みd方向に20%圧縮した際の厚み回復率が40%以上である、
樹脂シート。 - 前記樹脂シートが樹脂発泡体から構成される、請求項1に記載の樹脂シート。
- 前記樹脂発泡体が、ポリエチレン、ポリプロピレン、ポリエステル、EPDM、アクリル系樹脂から選ばれる少なくとも1種を含む、請求項2に記載の樹脂シート。
- 前記樹脂発泡体が、化学的発泡方法、物理的発泡方法から選ばれる少なくとも1種である発泡方法によって形成される、請求項2または3に記載の樹脂シート。
- セル壁比率が5%〜80%である、請求項2から4までのいずれかに記載の樹脂シート。
- 平均セル径が40μm〜500μmである、請求項2から5までにいずれかに記載の樹脂シート。
- 見かけ密度が0.01g/cm3〜0.5g/cm3である、請求項2から6までのいずれかに記載の樹脂シート。
- 熱伝導率が0.05W/mK〜0.35W/mKである、請求項2から7までのいずれかに記載の樹脂シート。
- 請求項1から8までのいずれかに記載の樹脂シートと粘着剤層を有する、粘着剤層付樹脂シート。
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KR20220024261A (ko) * | 2020-01-02 | 2022-03-03 | 주식회사 휴비스 | 폴리에스테르 발포시트 및 이의 제조방법 |
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