JP2022113748A - 積層体および電子部品の製造方法 - Google Patents
積層体および電子部品の製造方法 Download PDFInfo
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- JP2022113748A JP2022113748A JP2022090759A JP2022090759A JP2022113748A JP 2022113748 A JP2022113748 A JP 2022113748A JP 2022090759 A JP2022090759 A JP 2022090759A JP 2022090759 A JP2022090759 A JP 2022090759A JP 2022113748 A JP2022113748 A JP 2022113748A
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- silicone gel
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- reaction
- gel
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Abstract
Description
を有する電子部品の製造方法により、上記課題を解決できる事を見出し、本発明に到達した。この場合、シート状部材は硬化反応性シリコーンゲルの硬化物と接合体を形成して実質的に一体化しており、シート状部材を剥離することによって、それに追従する硬化物もほぼ同時に電子部品上から分離される。
本積層体は硬化反応性のシリコーンゲルを備えることを特徴とする。当該、シリコーンゲルは、電子部品等の基材を各種処理から保護することができ、非流動性のゲル状を呈し、加熱、高エネルギー線の照射等に応答して硬化反応を起こし、硬化反応前よりも保型性が高く、離型性に優れたハードな硬化層に変化する。シリコーンゲル層は、層状であれば、とくにその形状は限定されないが、後述する電子部品の製造用途に用いる場合、実質的に平坦なシリコーンゲルであることが好ましい。シリコーンゲル層の厚みについても特に限定されるものではないが、平均厚みが10~500μmの範囲、25~300μmの範囲または30~200μmの範囲であってよい。平均厚みが10μm未満では基材である電子部品等の凹凸に由来する間隙(ギャップ)が埋まりにくく、500μmを超えると、特に電子部品製造用途において、電子部品の仮留/加工時の配置目的でシリコーンゲル層を使用する場合には、不経済となることがある。また、当該硬化反応性シリコーンゲルの外観は特に制限されるものではないが、電子部品の処理やダイシング(個片化)を行う場合には、透明乃至半透明であることが好ましく、後述するシリコーンゲルは色材等を添加しない限り、ほぼ透明乃至半透明なゲルおよび硬化物を形成する。
(i)120~200℃でのシリコーンゲルの加熱操作:ヒドロシリル化反応硬化型、過酸化物硬化反応型、またはそれらの組み合わせ
(ii)シリコーンゲルへの紫外線の照射操作:高エネルギー線照射によるラジカル反応硬化型、光活性型白金錯体硬化触媒を用いたヒドロシリル化反応硬化型、またはそれらの組み合わせ
(iii)上記の(i)および(ii)の硬化操作、硬化機構および条件の組み合わせ、特に同時または時差をおいての硬化操作の組み合わせを含む。
シリコーンゲル層を積層する基材は凹凸があってよく、シリコーンゲル層により当該凹凸が隙間なく充填乃至追従され、平坦なシリコーンゲル層を形成していることが特に好ましい。本発明の硬化反応性シリコーンゲル層は柔軟で変形性、追従性に優れるため、凹凸のある基材に対しても間隙を生じにくく、乖離やシリコーンゲル表面の変形などの問題を生じにくいという利点がある。シリコーンゲル層を積層する目的は特に制限されるものではないが、基材が電子部品である場合、当該シリコーンゲル層の積層箇所を各種処理から選択的に保護できるほか、柔軟なシリコーンゲル層により物理的な衝撃・振動からの保護等を図ってもよい。
本発明の積層体は、上記の通り、基材として1個以上の電子部品を有することが好ましい。電子部品は、特にその種類は制限されるものではないが、半導体チップの素体となる半導体ウェハ、セラミックス素子(セラミックコンデンサ含む)、半導体チップおよび発光半導体チップが例示され、同一または異なる2個以上の電子部品の上に硬化反応性のシリコーンゲル層が配置されたものであってもよい。本発明の積層体における硬化反応性シリコーンゲル層は、ゲル状であり、かつ、硬化条件を選択可能なので、ある程度高温となる温度領域で取り扱った場合であっても、硬化反応が殆ど進行せず、適度に柔軟かつ追従性・変形性に優れるため、安定かつ平坦な面を形成することができ、さらに、当該シリコーンゲルが積層面を各種処理から選択的に保護するほか、電子部品の製造工程における振動や衝撃を緩和するため、当該シリコーンゲルを積層した電子部品を定位置に安定的に保持し、電子部品に対して各種パターン形成等の処理およびダイシング等の加工処理を行った場合であっても、基材の表面凹凸や電子部品の位置ずれ、振動変位(ダンピング)に伴う電子部品の加工不良が発生しにくいという利点を有する。なお、ゲルによる電子部品等の保持は、ゲルの粘弾性に由来するものであり、ゲル自体の弱い粘着力によるものと、ゲルの変形による電子部品の担持の両方を含む。
これらの電子部品は、積層体を形成する前に化学的または物理的な処理が行われていてもよく、電子部品にシリコーンゲルを積層した後に、上記処理を行うものであっても良い。電子部品のうち、シリコーンゲルを積層した箇所は、これらの処理から選択的に保護されうるため、所望とする化学的または物理的処理を、電子部品の特定箇所のみに施すことが可能である。特に、本発明では、シリコーンゲルが局所的、ピンポイントであっても、効率よくその硬化物を分離できるため、電子部品の選択的な保護に特に有用である。これらの電子部品への処理は、少なくとも部分的に電子回路または電極パターン、導電膜、絶縁膜等を形成する事が含まれるが、これらに限定されるものではない。上記処理にあたっては、従来公知の手段を特に制限なく用いることができ、真空蒸着法、スパッタ法、電気めっき法、化学めっき法(無電解めっき法含む)、エッチング法、印刷工法またはリフトオフ法に形成されていてもよい。本発明の積層体を電子部品の製造に用いる場合、硬化反応性シリコーンゲルを積層した上で、電子部品の電子回路、電極パターン、導電膜、絶縁膜等を形成することが特に好ましく、任意で当該積層体を個片化(ダイシング)してもよい。上記のとおり、シリコーンゲル層を用いることで、これらの電子部品の加工不良が抑制される。なお、処理に当たっては、基材である電子部品とシリコーンゲル層の上下左右関係は所望により選択することができる。
シート状部材は、少なくとも部分的に接着層を備えており、前記の硬化反応性シリコーンゲル上に、接着層を介して積層されることを特徴とする。当該接着層を介してシリコーンゲルと密着していることで、特に硬化反応性シリコーンゲルが硬化物を形成する際に、シート状部材と当該硬化物は接合体を形成し、実質的に一体として基材上から分離することができる。硬化反応性シリコーンゲルを硬化してなる硬化物は、分離に用いる機械装置の種類により、破損の問題や剥離工程の複雑化といった問題の原因になりうるものであるが、シート状部材と一体化したシリコーンゲルの硬化物は、局所的乃至ピンポイントであっても容易に分離でき、かつ、簡便、迅速かつ確実に基材上から分離することができ、特に工業的生産工程において、作業時間の短縮および工数の削減という著しい優位性を実現する。
本発明の積層体は、基材上にシリコーンゲル、および接着層を介してシート状部材を積層してなるものであり、所望により、シリコーンゲルの原料組成物である硬化性シリコーン組成物を目的となる基材上に塗布してゲル状に硬化させることで製造可能である。同様に、シリコーンゲルは、所望の剥離層を備えたシート状基材上に形成させ、剥離層からシリコーンゲル層を分離し、他の基材上に転写し、さらに、接着層を介してシート状部材を積層することによっても製造可能である。シリコーンゲルの積層は、基材の全面でも局所的であっても行うことができ、ピンポイントでの基材保護も可能である。
および、基材上で当該硬化性シリコーン組成物をゲル状に一次硬化させることにより、硬化反応性シリコーンゲル層を形成する工程(A-2)、および
硬化反応性シリコーンゲル層に接着層を介してシート状部材を積層する工程(A-3)
を有する製造方法により得ることができる。
剥離層上で当該硬化性シリコーン組成物をゲル状に一次硬化させることにより、硬化反応性シリコーンゲル層を形成する工程(B-2)、
前記工程で得た積層体のシリコーンゲル層を、上記の基材Rとは異なる、少なくとも1種類の基材上に配置し、基材Rのみを除去する工程(B-3)、および
硬化反応性シリコーンゲル層に接着層を介してシート状部材を積層する工程(B-4)
を有する製造方法により得ることができる。なお、この場合、積層体のシリコーンゲル層であって、上記の基材Rとは異なる、少なくとも1種類の基材に対向する面には、その密着性及び接着性を改善する目的で、基材と対向するシリコーンゲル面に、プライマー処理、コロナ処理、エッチング処理、プラズマ処理等の表面処理がなされていてもよく、かつ好ましい。当該密着性の改善により、基材Rを容易に分離できる利点がある。
硬化反応性のシリコーンゲル層は実質的に平坦であることが好ましいが、その原料となる硬化性シリコーン組成物を、通常の方法で剥離層を有する基材上に塗布すると、特に硬化後のシリコーンゲル層の厚みが50μm以上となる場合には、その塗布面が凹んだ不均一な表面を形成して、得られるシリコーンゲル層表面が不均一となる場合がある。しかしながら、当該硬化性シリコーン組成物およびシリコーンゲル層に対して剥離層を有する基材を適用し、未硬化の塗布面を各々の剥離層を備えたシート状基材(上記の基材R;セパレータ)で挟み込み、物理的に均一化された平坦化層を形成することで、平坦化された硬化反応性のシリコーンゲル層を得ることができる。なお、上記の平坦化層の形成にあたっては、剥離層を有するセパレータ間に未硬化の硬化性シリコーン組成物が塗布されてなる積層体を、ロール圧延等の公知の圧延方法を用いて圧延加工することが好ましい。
本発明の積層体を構成する硬化反応性シリコーンゲル層は、硬化性シリコーン組成物をゲル状に一次硬化させてなるものである。上記のとおり、シリコーンゲル層を形成するための一次硬化反応は、シリコーンゲル自体の二次硬化反応と異なる硬化反応機構であってもよく、同一の硬化反応機構であってもよい。一方、100℃以下でのシリコーンゲル層の安定性の見地から、硬化性シリコーン組成物を室温~100℃の温度範囲においてゲル状に硬化させることが好ましい。
上式中、R1は同じかまたは異なる、脂肪族不飽和結合を有さない一価炭化水素基であり、メチル基またはフェニル基が好ましい。R2はアルキル基であり、脱アルコール縮合反応性のアルコキシ基を構成するため、メチル基、エチル基またはプロピル基であることが好ましい。R3はケイ素原子に結合するアルキレン基であり、炭素原子数2~8のアルキレン基が好ましい。aは0~2の整数であり、pは1~50の整数である。脱アルコール縮合反応性の見地から、最も好適には、aは0であり、トリアルコキシシリル基含有基であることが好ましい。なお、上記のアルコキシシリル基含有基に加えて、ヒドロシリル化反応性の官能基または光重合反応性の官能基を同一分子内に有してもよい。
本発明に係るシリコーンゲル層は、硬化性シリコーン組成物をヒドロシリル化反応硬化型、脱水縮合反応硬化型、脱アルコール縮合反応硬化型または高エネルギー線照射によるラジカル反応硬化型の硬化機構によりゲル状に硬化されていることが好ましい。特に、100℃以下の低温下でヒドロシリル化反応硬化型または室温下での高エネルギー線照射によるラジカル反応硬化型または高エネルギー線照射によるヒドロシリル化反応硬化型が好適である。
上記のとおり、本発明の積層体は電子部品の製造に有用であり、基材である電子部品上にシリコーンゲルを形成して、安定かつ平坦で、応力緩和性に優れた電子部品の配置面を形成することにより、その後に当該電子部品に対して化学的乃至物理的処理を行った場合であっても、当該シリコーンゲルを積層した部分は、各種処理から選択的に保護され、かつ、電子部品の製造時における基材の表面凹凸や電子部品の位置ずれ、振動変位(ダンピング)に伴う電子部品の加工不良が発生しにくいという利益を実現しうる。また、前記のシート状部材が接着層を介して積層されたシリコーンゲルを硬化させることにより、当該シート状部材とシリコーンゲルの硬化物が接合して一体化し、シリコーンゲルのみを硬化させた場合には硬化物の効率的な剥離が難しいような局所的な配置であっても、両者をほぼ同時に、簡便、迅速、かつ、確実に電子部品上から剥離することができ、しかもシリコーンゲル等の残留物(糊残り)に由来する不良品が発生しにくいという利点を有する。
工程(I):電子部品、硬化反応性シリコーンゲルおよび接着層を有するシート状部材を有する積層体を作成する 工程、
工程(II):工程(I)の後、電子部品に対して、1種類以上の化学的乃至物理的処理(電子回路の形成、電極パターンの形成、導電膜の形成 および絶縁膜の形成から選ばれる1種類以上の処理を含むが、これらに限定されない)を行う工程、
工程(III):工程(II)の後、硬化反応性シリコーンゲルを硬化する工程、
工程(IV):工程(III)の後、シート状部材および硬化反応性シリコーンゲルの硬化物を、実質的に同時に電子部品から分離する工程
を有するものである。なお、工程(I)における積層体の形成工程は任意であり、硬化性シリコーン組成物を基材である電子部品上に塗布してゲル状に一次硬化させてもよく、別途形成した硬化反応性シリコーンゲルを基材である電子部品上に転写しても良い。
工程(I’):電子部品上に硬化反応性シリコーンゲルを積層する工程、
工程(II’):工程(I’)の後、電子部品に対して、1種類以上の化学的乃至物理的処理(電子回路の形成、電極パターンの形成、導電膜の形成 および絶縁膜の形成から選ばれる1種類以上の処理を含むが、これらに限定されない)を行う工程、
工程(III’):工程(II’)の後、硬化反応性シリコーンゲル上に接着層を有するシート状部材を積層する工程 、
工程(IV’):工程(III’)の後、硬化反応性シリコーンゲルを硬化する工程、
工程(V’):工程(IV’)の後、シート状部材および硬化反応性シリコーンゲルの硬化物を、実質的に同時に電子部品から分離する工程。
・成分(A1-2):両末端ビニルジメチルシロキシ基封鎖、ジメチルシロキサンポリマー(シロキサン重合度:約315,ビニル基の含有量:約0.22重量%)
・・成分(A1-3):両末端トリメチルシロキシ基封鎖、ジメチルシロキサン-ビニルメチルシロキサンコポリマー (シロキサン重合度:約816,ビニル基の含有量: 約0.29重量%)
・成分(A2):ビニルジメチルシロキシ基封鎖Q単位からなる樹脂状オルガノポリシロキサン (ビニル基の含有量: 約4.1重量%)
・成分(B1):両末端ハイドロジェンジメチルシロキシ基封鎖ジメチルシロキサンポリマー(シロキサン重合度:約20,ケイ素結合水素基の含有量: 0.12重量%)
<ヒドロシリル化反応抑制剤>
・成分(C1):1,3,5,7-テトラメチル-1,3,5,7-テトラビニル-シクロテトラシロキサン(ビニル基の含有量:30.2重量%)。
<フィラー>
・成分(D1):ヘキサメチルジシラザン処理シリカ微粒子(日本アエロジル製、商品名「アエロジル200V」)
<硬化剤>
・成分(E1):白金-ジビニルテトラメチルジシロキサン錯体のビニルシロキサン溶液(白金金属濃度で約0.6重量%)
・成分(E2):2,5-ジメチル-2,5-ジ(t-ブチルパーオキシ)ヘキサン-両末端トリメチルシロキシ基封鎖シロキサンポリマー混合物(2,5-ジメチル-2,5-ジ(t-ブチルパーオキシ)ヘキサン濃度で約50重量%)
成分A1-1(9.76重量%)、A1-2(5.93重量%)、A1-3(60.42重量%)、A2(6.61重量%)、B1(13.02重量%)、C1(0.10重量%)、D1(2.08重量%)、E1(0.07重量%)およびE2(2.00重量%)を均一に混合することにより、硬化性液状シリコーン組成物を調製した。その際、ビニル基1モル当たり、成分(B1)のケイ素原子結合水素原子(Si-H)が0.85モルとなる量とした。なお、本実施例では上記成分に加え、剥離性確認を容易にする目的で適当量の着色材を使用した。
<組成:実施例2>
成分A1-1(9.87重量%)、A1-3(66.27重量%)、A2(6.69重量%)、B1(8.74重量%)、C1(0.10重量%)、D1(6.25重量%)、E1(0.07重量%)およびE2(2.00重量%)を均一に混合することにより、硬化性液状シリコーン組成物を調製した。その際、ビニル基1モル当たり、成分(B1)のケイ素原子結合水素原子(Si-H)が0.56モルとなる量とした。なお、本実施例では上記成分に加え、剥離性確認を容易にする目的で適当量の着色材を使用した。
硬化前液状シリコーン組成物を80℃で2時間かけて加熱することにより、ヒドロシリル化反応を進行させてゲル状物を得た。得られた硬化反応性シリコーンゲルは着色材を欠いた状態では透明であった。
上記で作製した硬化反応性シリコーンゲルをさらに窒素中150℃(実施例2)もしくは170℃(実施例1)で1時間かけて二次硬化させることで二次硬化物を得た。
硬化反応性シリコーンゲル
アルミニウム製容器(直径50mm)に、硬化前液状シリコーン組成物を厚さ約1.5mmとなるように投入し、上記条件にて得られた硬化反応性シリコーンゲルから直径8mmとなるように試験体を切り出し使用した。MCR302粘弾性測定装置(Anton Paar社製)を用い、直径8mmのパラレルプレートに切り出したサンプルを貼り付け測定を行った。23℃にて、周波数0.01~10Hzの範囲で、ひずみ0.5%の条件で行った。
実施例1:0.1Hzでの貯蔵弾性率は6.1×104Pa、損失正接(損失弾性率/貯蔵弾性率)は0.03であった。
実施例2:0.1Hzでの貯蔵弾性率は3.9×104Pa、損失正接(損失弾性率/貯蔵弾性率)は0.05であった。
上記同様、アルミニウム製容器を用い、硬化反応性シリコーンゲルを作製した。さらに上記作製条件にて硬化させることで二次硬化物が得られた。得られた二次硬化物から直径8mmとなるように試験体を切り出し使用した。MCR302(アントンパール社製)を用い、直径8mmのパラレルプレートに切り出したサンプルを貼り付け測定を行った。23℃にて、周波数0.01~10Hzまで、ひずみ0.1%の条件で行った。
実施例1:0.1Hzでの貯蔵弾性率は1.0×105Paであった。
実施例2:0.1Hzでの貯蔵弾性率は8.4×104Paであった。
硬化前液状シリコーン組成物を基板上に室温にてスピンコートし、上記条件にて基板上に硬化性ゲル層を作製した。
得られた硬化性ゲル層に粘着テープ(日東電工社製、ニトフロン No.903UL)を貼り付け、窒素中150℃もしくは170℃で1時間かけて硬化反応性シリコーンゲルを二次硬化させた。
上記で作製した二次硬化物を含む基板上から粘着テープを剥がし、二次硬化物が粘着テープ側へ転写されることを目視で確認した。
粘着テープを用いない他は、上記同様の条件で、硬化前液状シリコーン組成物を基板上に室温にてスピンコートし、基板上に硬化性ゲル層を作製し、窒素中150℃もしくは170℃で1時間かけて硬化反応性シリコーンゲルを二次硬化させた。しかしながら、粘着テープがない場合、二次硬化物を効率的に基材から剥がす(=分離する)ことができなかった。
アルミ基板上にプライマーXおよびY(共にダウコーニング社製)を薄膜塗布した。その上に実施例2に記載の硬化前液状シリコーン組成物を約230μmとなるように塗布し、上記同様に硬化させエラストマーを得た。さらに、得られたエラストマー上に粘着テープ(no. 336、日東電工社製)を張り合わせ、窒素雰囲気下150℃で1時間かけて加熱することにより粘着層との反応を行った。30分保存後、RTC1210(オリエンテック社製)を用いて、23℃、相対湿度50%の条件で、300mm/minの速度で180度ピール試験を行った。ピール強度は165N/mで、剥離モードが凝集破壊であった。一方、窒素雰囲気下150℃で1時間かけて加熱後、上記同様に粘着テープを張り合わせた場合、ピール強度は135N/mで、剥離モードが界面剥離であった。従って、上記の二次硬化反応により、硬化反応性エラストマーと粘着テープ界面で強固な結合が形成されていることが確認された。このような結合体は、粘着テープと一体として基材上から除去可能である。
Claims (8)
- (L1)基材、
(L2)前記基材上に積層された硬化反応性シリコーンゲル、および
(L3)前記硬化反応性シリコーンゲル上に、接着層を介して積層されたシート状部材
を含有し、
前記接着層は、ヒドロシリル化反応硬化性のシリコーン系接着剤、過酸化物硬化性のシリコーン系接着剤、高エネルギー線硬化性のシリコーン系接着剤、またはこれらから選ばれる2種類以上のシリコーン系接着剤からなり、該接着層は、前記前記硬化反応性シリコーンゲルの硬化物と接合体を形成し、前記基材から前記シート状部材を分離しようとした際に、該接着層の破壊モードが凝集破壊となるような強固な接着を形成している積層体。 - 上記(L1)基材が、(L1-E)電子部品である、請求項1に記載の積層体。
- 上記(L1)基材が、1種類以上の化学的乃至物理的処理が施されている(L1-E)電子部品である、請求項1または請求項2に記載の積層体。
- 上記(L2)の硬化反応性シリコーンゲルの損失係数tanδが、23℃~100℃において、0.01~1.00の範囲にあることを特徴とする、請求項1~請求項3のいずれか1項に記載の積層体。
- 上記(L2)の硬化反応性シリコーンゲルを硬化反応させて得られる硬化反応性シリコーンゲルの硬化物の貯蔵弾性率G’curedが、硬化前のシリコーンゲルの貯蔵弾性率G’gelに比べて50%以上上昇することを特徴とする、請求項1~請求項4のいずれか1項に記載の積層体。
- 上記(L3)のシート状部材が、接着フィルムである、請求項1~請求項5のいずれか1項に記載の積層体。
- 上記(L3)のシート状部材が、上記(L2)の硬化反応性シリコーンゲルの硬化反応により、硬化反応性シリコーンゲルの硬化物と接合物を形成することを特徴とする、請求項1~請求項6のいずれか1項に記載の積層体。
- 上記(L3)のシート状部材に、プライマー処理、コロナ処理、エッチング処理、プラズマ処理のいずれかの表面処理がなされている、請求項1~7のいずれか1項に記載の積層体。
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