JP2019178270A - 硬化性組成物、その硬化物およびこれを有する電子部品 - Google Patents
硬化性組成物、その硬化物およびこれを有する電子部品 Download PDFInfo
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- JP2019178270A JP2019178270A JP2018069210A JP2018069210A JP2019178270A JP 2019178270 A JP2019178270 A JP 2019178270A JP 2018069210 A JP2018069210 A JP 2018069210A JP 2018069210 A JP2018069210 A JP 2018069210A JP 2019178270 A JP2019178270 A JP 2019178270A
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- Prior art keywords
- meth
- curable composition
- acrylate
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- compound
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- 239000003999 initiator Substances 0.000 claims abstract description 14
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 58
- -1 methacryloyl group Chemical group 0.000 description 56
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Landscapes
- Ink Jet Recording Methods And Recording Media Thereof (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Non-Metallic Protective Coatings For Printed Circuits (AREA)
Abstract
Description
そこで、インクジェットプリンターの適用の初期には、スクリーン印刷用のソルダーレジストインキ(樹脂組成物)を、希釈剤で希釈して10〜150mPa・s(25℃)程度の低粘度としてインクジェットプリンターに用いる方法が検討された(特許文献1および2)。
インクジェット法適用のための低粘度化の要求と、レジストインキとして本来必要な耐熱性、耐薬品性、密着性、硬度等の物性を得るという要求の双方を満足する樹脂組成物を得るために、種々の開発が行われる中、たとえば特許文献3および4の硬化性組成物が提案された。これらの硬化性組成物は、低分子量の硬化性化合物と比較的少量のフィラーを用いることにより、インクジェットに適する粘度を有し、かつレジスト膜として必要な所望の特性を具備するものとされている。
以下、本発明の硬化性組成物の構成成分を説明する。
本発明の硬化性組成物は(A)モース硬度が5以上のフィラーを含む。
本発明において、エチレン性不飽和基を有する多分岐状のオリゴマー又はポリマーは、多分岐状のオリゴマー又はポリマー(1分子中に複数の分岐鎖を有するオリゴマー又はポリマーのことをいう)骨格にエチレン性不飽和基を少なくとも1つ有する化合物である。エチレン性不飽和基は、(メタ)アクリロイル基などの官能基に由来するものであり、1分子内に複数種のエチレン性不飽和基を有していてもよい。なお、(メタ)アクリロイル基は、アクリロイル基とメタクリロイル基の両方を含む概念である。
デンドリマーの製造方法は特に限定されず、中心コア分子に世代ごとに分子を結合させて分岐を形成するダイバージェント法、予め合成した枝部分をコア分子に結合させるコンバージェント法、2以上の反応点Bを有する分岐部分と別の反応点Aを有するつなぎ部分とを1分子内に持つモノマーABxを用いて1段階で合成する方法など公知の製造方法を採用することができる。
本発明の硬化性組成物には、熱硬化成分を加えることができる。熱硬化成分を加えることにより密着性や耐熱性が向上することが期待できる。本発明に用いられる熱硬化成分としては、メラミン樹脂、ベンゾグアナミン樹脂、メラミン誘導体、ベンゾグアナミン誘導体等のアミノ樹脂、ブロックイソシアネート化合物、シクロカーボネート化合物、環状(チオ)エーテル基を有する熱硬化成分、ビスマレイミド、カルボジイミド樹脂等の公知の熱硬化性樹脂が使用できる。特に好ましいのは、耐熱性に優れる点より、ブロックイソシアネート化合物である。
(D)光重合開始剤としては、エネルギー線の照射により、(メタ)アクリレートを重合させることが可能なものであれば、特に制限はなく、ラジカル重合開始剤が使用できる。
[(メタ)アクリレートモノマー]
本発明の硬化性組成物は上記の(B)エチレン性不飽和基を有する多分岐状のオリゴマーおよび多分岐状ポリマーのいずれか1種類以上とは別の(メタ)アクリレートモノマーを含むことができる。
I.組成物の調整
表1に示す割合(単位:質量部)で各成分を配合し、これをディゾルバーで攪拌した。その後ビーズミルを用いて1mmのジルコニアビーズにて分散を2時間行い、本発明の組成物(実施例1〜5)および比較組成物(比較例1〜2)を得た。
上記各組成物について、以下に示す特性試験を行った。その結果を表1に示す。
実施例および比較例の硬化性組成物の25℃、100rpmにおける粘度を、コーンプレート型粘度計(東機産業社製TVH−33H)にて測定し、下記基準による評価結果を表1に記載した。
× 150mPa・sを超過
厚さ50μmのポリイミドフィルム上に、各実施例および比較例の硬化性組成物を、アプリケータを用いて塗布し、UV露光(高圧水銀灯500mJ/cm2)を行った。硬化性組成物の塗膜が完全に硬化したことを確認して、ポリイミドフィルムと硬化塗膜の積層体を、3cmx3cm(縦×横)に切り出してサンプル(乾燥膜厚:15μm)とした。各サンプルを、硬化塗膜面を上面として、水平な作業台上に静置し、作業台から上昇した地上から上昇したサンプルの四端の高さを定規で測定し、四端の高さの平均値を求めた。同様の試験をサンプルごとに3回行い、3回の試験の平均値を求めた。下記基準による評価結果を表1に記載した。
○ 四端の合計高さの平均値が6mm超過、10mm未満
× 四端の合計高さの平均値が10mm以上
各実施例および比較例の硬化性組成物を、アプリケーターを使って-銅箔上に塗布し、UV露光(高圧水銀灯500mJ/cm2)を行い、次いで150℃の熱風循環式乾燥炉にて60分間熱処理を行い、硬化塗膜サンプル(膜厚25um)を得た。得られた硬化塗膜の表面における鉛筆硬度をJIS 5600−5−4に準拠して測定を行った。測定結果を表1に示す。
上記3.鉛筆硬度評価に用いたものと同様の硬化塗膜サンプルを、JIS C−5012の方法に準拠してはんだフロート法によるはんだ耐熱性試験に付した。260℃のはんだ槽に10秒間浸漬後、各サンプルをはんだ層から取り出して自然冷却した後、プロピレングリコールモノメチルエーテルアセテートで洗浄し、乾燥した。この試験を3回繰返した後、塗膜の状態を目視観察した後、上記で得られためっきされた基板硬化塗膜の密着性をJIS K 5600−5−6に準拠したクロスカットテープピールリング試験を実施し、以下の基準にて評価した。
〇 クロスカットした部分にわずかにチッピングが見られた。
× 塗膜が完全に剥離した
上記3.鉛筆硬度評価に用いたものと同様の硬化塗膜サンプルをニッケル0.5μm、金0.03μmの条件でめっきを行ない、得られた硬化塗膜表面状態の観察を行った。その後、セロハン粘着テープによるピーリング試験を行い、更に塗膜の状態を目視観察した。評価基準は以下のとおりである。
× 剥離が生じた
*2 ビスコート#1000、大阪有機化学工業株式会社製
*3 BI 7982、Baxenden Chemicals 社製
*4 Omnirad TPO、IGM Resins社製
*5 Omnirad 819、IGM Resins社製
*6 IRGANOX 1010、BASF ジャパン社製
*7 4HBA、日本化成株式会社製
*8 KAYARAD R-604、日本化薬株式会社製
*9 A-NOD-N、新中村化学工業株式会社製
*10 PA-100、昭和化学工業株式会社製
本発明の組成物は、射出性、低反り性、鉛筆硬度、はんだ耐熱性および金めっき耐性の
全てにおいて優れていることが示された。
Claims (6)
- (A)モース硬度が5以上のフィラーと、
(B)エチレン性不飽和基を有する多分岐状のオリゴマーまたは多分岐状ポリマーのいずれか1種以上と、
(C)熱硬化性化合物と、
(D)光重合開始剤と、
を含むことを特徴とするインクジェット用硬化性組成物。 - 前記(B)エチレン性不飽和基を有する多分岐状オリゴマーまたは多分岐状ポリマーの(メタ)アクリロイル基数が6を超過する請求項1に記載の硬化性組成物。
- 前記(A)モース硬度が5以上のフィラーの含有率が、硬化性組成物の総質量の10質量%以上であることを特徴とする請求項1または2に記載の硬化性組成物。
- 前記(C)熱硬化性化合物が、ブロックイソシアネートであることを特徴する請求項1から3のいずれか1項に記載の硬化性組成物。
- 請求項1〜4のいずれか1項に記載の硬化性組成物の硬化物。
- 請求項5に記載の硬化物を有することを特徴とする電子部品。
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