JP5201433B1 - 受容層形成用樹脂組成物ならびにそれを用いて得られる受容基材、印刷物、導電性パターン及び電気回路 - Google Patents
受容層形成用樹脂組成物ならびにそれを用いて得られる受容基材、印刷物、導電性パターン及び電気回路 Download PDFInfo
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- JP5201433B1 JP5201433B1 JP2012553136A JP2012553136A JP5201433B1 JP 5201433 B1 JP5201433 B1 JP 5201433B1 JP 2012553136 A JP2012553136 A JP 2012553136A JP 2012553136 A JP2012553136 A JP 2012553136A JP 5201433 B1 JP5201433 B1 JP 5201433B1
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- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229920006163 vinyl copolymer Polymers 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C09D133/04—Homopolymers or copolymers of esters
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Abstract
本発明は、重量平均分子量10万以上で、かつ、酸価10〜80であるビニル樹脂(A)と、水性媒体(B)と、必要に応じて水溶性樹脂(c1)及び充填材(c2)からなる群より選ばれる1種以上の成分(C)とを含有するものであり、前記ビニル樹脂(A)が水性媒体(B)に分散し、かつ、前記ビニル樹脂(A)の全量に対する前記成分(C)の含有量が0質量%〜15質量%であることを特徴とする受容層形成用樹脂組成物に関するものである。
【選択図】なし
Description
前記酸価としては、より一層優れた細線性、密着際、耐湿熱性等を付与する観点から、10〜75の範囲であることが好ましく、15〜70の範囲であることがより好ましく、25〜70の範囲であることがさらに好ましく、35〜70の範囲であることが特に好ましい。
また、前記酸基を有するビニル単量体、特に前記カルボキシル基を有するビニル単量体を、後述するアミド基を有するビニル単量体と組み合わせ使用する場合には、前記ビニル樹脂(A)の製造に使用するビニル単量体混合物の全量に対して、前記酸基を有するビニル単量体とアミド基を有するビニル単量体との合計の質量割合が、好ましくは5質量%を超え40質量%以下、より好ましくは6質量%以上35質量%以下となる範囲で使用することができる。
前記ビニル単量体(A)は、前記したビニル単量体混合物を従来から知られている方法で重合することによって製造することができるが、にじみがなく細線性に優れた導電性パターン等を形成可能な受容層を形成するうえで、乳化重合法で製造することが好ましい。
撹拌機、還流冷却管、窒素導入管、温度計、滴下漏斗を備えた反応容器に脱イオン水350質量部、ラテムルE−118B(花王(株)製:有効成分25質量%)4質量部を入れ、窒素を吹き込みながら70℃まで昇温した。
(i)PET;ポリエチレンテレフタレートフィルム(東洋紡績株式会社製 コスモシャインA4300,厚さ50μm)
(ii)PI;ポリイミドフィルム(東レ・デュポン株式会社製Kapton200H,厚さ50μm)
(iii)GL;ガラス:ガラス板,JIS R3202,厚さ2mm
ビニル単量体混合物の組成を下記表1に記載の組成にそれぞれ変更すること以外は、実施例1記載の方法と同様の方法で、不揮発分20質量%の受容層形成用樹脂組成物(I−2)〜(I−6)を調製した。
撹拌機、還流冷却管、窒素導入管、温度計、滴下漏斗を備えた反応容器に脱イオン水350質量部、ラテムルE−118B(花王(株)製:有効成分25質量%)4質量部を入れ、窒素を吹き込みながら70℃まで昇温した。
実施例2で得られた受容層形成用樹脂組成物(I−2)に水溶性樹脂として、PVA210〔株式会社クラレ製、ケン化度87モル%〜89モル%、重合度1000のポリビニルアルコール〕の10質量%水溶液を、受容層形成樹脂組成物(I−2):PVA210=300:400(固形分質量比60:40)で混合することによって、不揮発分14質量%の受容層形成用樹脂組成物(I’−1)を得た。
実施例2で得た受容層形成用樹脂組成物(I−2)に充填材として、スノーテックスO[日産化学工業(株)、コロイダルシリカ、SiO2 20%水分散体]を、受容層形成樹脂組成物(I−2):スノーテックス C=300:200(固形分質量比60:40)で混合することによって、不揮発分20質量%の受容層形成用樹脂組成物(I’−2)を得た。
ビニル単量体混合物の組成を下記表1に記載の組成にそれぞれ変更すること以外は、実施例1記載の方法と同様の方法で、不揮発分20質量%の受容層形成用樹脂組成物(I’−3)〜(I’−5)を調製した。
MMA:メタクリル酸メチル
NBMAM:N−n−ブトキシメチルアクリルアミド
BA :アクリル酸n−ブチル
MAA:メタクリル酸
AM :アクリルアミド
CHMA:メタクリル酸シクロヘキシル
L−SH:ラウリルメルカプタン
架橋剤1:メラミン系化合物[ベッカミン M−3(DIC(株)製)、トリメトキシメチルメラミン]
水溶性樹脂:PVA210〔株式会社クラレ製、ケン化度87モル%〜89モル%、重合度1000のポリビニルアルコール〕
充填材:スノーテックスO[日産化学工業(株)、コロイダルシリカ、SiO2 20%水分散体]
ビニル樹脂の酸価は、ビニル樹脂の製造に使用したビニル単量体の全量に対する酸基含有ビニル単量体の使用量に基づいて算出した計算値であり、〔酸基含有ビニル単量体が有する酸基の物質量(モル)/ビニル単量体の全質量〕×56100によって求めた値である。具体的には、実施例1でいえば、カルボキシル基を1個有するメタクリル酸(分子量86.09)7質量部に対して、ビニル単量体の全量が100質量部であるから、〔{(7/86.09)×1}/100〕×56100=46と算出できる。
前記ビニル樹脂(A)80mgとテトラヒドロフラン20mlを混合し12時間攪拌したものを測定試料として用い、ゲル・パーミエーション・クロマトグラフ法(GPC法)によって測定した。測定装置;東ソー(株)製高速液体クロマトグラフHLC−8220型、カラム;東ソー(株)製TSKgelGMH XL×4カラム、溶離液;テトラヒドロフラン、検出器;RI検出器。
前記印刷を施す前の各受容基材の表面(受容層上)にセロハン粘着テープ(ニチバン(株)製,CT405AP−24,24mm)を指で圧着した後、前記セロハン粘着テープを、受容基材の受容層表面に対して90度方向に剥離した。剥離したセロハン粘着テープの粘着面を目視で観察し、その付着物の有無に基づいて前記密着性を評価した。
[インクジェット印刷用ナノ銀インク1の調製]
ジエチレングリコールジエチルエーテル65質量部と、γ−ブチロラクトン18質量部と、テトラエチレングリコールジメチルエーテル15質量部と、テトラエチレングリコールモノブチルエーテル2質量部とからなる混合溶媒に、平均粒径30nmの銀粒子を分散させることによって、溶剤系インクジェット印刷用ナノ銀インク1を調製した。
エチレングリコール45質量部と、イオン交換水55質量部との混合溶媒に、平均粒径30nmの銀粒子を分散させることによって、水系インクジェット印刷用ナノ銀インク2を調製した。
テトラドデカンからなる溶媒に平均粒径30nmの銀粒子を分散させることによって、溶剤系インクジェット印刷用ナノ銀インク2を調製した。
銀 ペースト(ハリマ化成株式会社製 NPS)を用いた。
前記インクジェット印刷用ナノ銀インク1〜3を、それぞれ、前記支持体(i)、(ii)及び(iii)を用いて得られた3種の受容基材表面に、インクジェットプリンター(コニカミノルタIJ(株)製インクジェット試験機EB100、評価用プリンタヘッドKM512L、吐出量42pl)を用い、線幅100μm、膜厚0.5μmの直線を約1cm印刷し、次いで150℃の条件下で30分間乾燥することによって、それぞれ印刷物(導電性パターン)を得た。実施例2〜7及び比較例1〜5に記載の受容基材を用いた場合には、上記導電性インクを用いて印刷した後、前記150℃の条件で30分間乾燥工程を経ることによって、受容層に架橋構造が形成された。架橋構造が形成されたか否かは、表3及び表4中に示すように、「常温(23℃)で乾燥し、その後70℃で加熱して形成された導電性インク受容層のゲル分率」と、「更に150℃で加熱することによって形成された導電性インク受容層のゲル分率」とに基づいて判断した。すなわち、150℃で加熱して得た導電性インク受容層のゲル分率が、常温乾燥した後、70℃で加熱して得た導電性インク受容層のゲル分率(未架橋状態)と比較して、25質量%以上増加したものを、高温加熱により架橋構造が形成されたと判断した。
前記スクリーン印刷用銀ペーストを、それぞれ、前記支持体(i)、(ii)及び(iii)を用いて得られた3種の受容基材表面に、メタルメッシュ250のスクリーン版を用いて、線幅50μm、膜厚1μmの直線を約1cm印刷し、次いで150℃の条件下で30分間乾燥することによって印刷物(導電性パターン)を得た。
実施例2〜7及び比較例1〜5に記載の受容基材については、上記導電性インクを用いて印刷した後の、前記150℃の条件で30分間乾燥工程を経ることによって、受容層に架橋構造が形成された。架橋構造の有無は、前記と同様の方法で判断した。
前記した方法で得られた印刷物(導電性パターン)表面に形成された印刷部(線部)全体を、光学顕微鏡((株)キーエンス製デジタルマイクロスコープVHX−100)を用いて観察し、該印刷部のにじみの有無を確認した。
前記インクジェット印刷用ナノ銀インク1を、それぞれ、前記支持体(i)及び(ii)を用いて得られた2種の受容基材表面に、インクジェットプリンター(コニカミノルタIJ(株)製インクジェット試験機EB100、評価用プリンタヘッドKM512L、吐出量42pl)を用い、縦3cm、横1cmの長方形の範囲(面積)を、膜厚0.5μmで印刷し、次いで150℃の条件下で30分間乾燥することによって、それぞれ印刷物(導電性パターン)を得た。導電性に記載の受容基材を用いた場合には、上記インクを用いて印刷した後の、前記150℃の条件で30分間乾燥工程を経ることによって、インク受容層に架橋構造が形成された。
前記インクジェット印刷用ナノ銀インク1を、それぞれ、前記支持体(ii)を用いて得られた受容基材表面に、インクジェットプリンター(コニカミノルタIJ(株)製インクジェット試験機EB100、評価用プリンタヘッドKM512L、吐出量42pl)を用い、縦3cm、横1cmの長方形の範囲(面積)を、膜厚0.5μmで印刷し、次いで150℃の条件下で30分間乾燥することによって、それぞれ印刷物(導電性パターン)を得た。実施例2〜7及び比較例1〜5に記載の導電性インク受容基材については、上記インクを用いて印刷した後の、前記150℃の条件で30分間乾燥工程を経ることによって、受容層に架橋構造が形成された。
前記インクジェット印刷用ナノ銀インク1及び前記インクジェット印刷用ナノ銀インク2を、それぞれ、前記支持体(ii)を用いて得られた受容基材表面に、インクジェットプリンター(コニカミノルタIJ(株)製インクジェット試験機EB100、評価用プリンタヘッドKM512L、吐出量42pl)を用い、縦3cm、横1cmの長方形の範囲(面積)を、膜厚0.5μmで印刷し、次いで150℃の条件下で30分間乾燥することによって、それぞれ印刷物(導電性パターン)を得た。実施例2〜7及び比較例1〜5に記載の導電性インク受容基材については、上記インクを用いて印刷した後の、前記150℃の条件で30分間乾燥工程を経ることによって、受容層に架橋構造が形成された。
ジエチレングリコールジエチルエーテル65質量部と、γ−ブチロラクトン18質量部と、テトラエチレングリコールジメチルエーテル15質量部と、テトラエチレングリコールモノブチルエーテル2質量部とからなる混合溶媒に、平均粒径30nmの銀粒子(めっき核)を分散させることによって、溶剤系のめっき核剤1を調製した。
ジエチレングリコールジエチルエーテル65質量部と、γ−ブチロラクトン18質量部と、テトラエチレングリコールジメチルエーテル15質量部と、テトラエチレングリコールモノブチルエーテル2質量部とからなる混合溶媒に、平均粒径30nmの銀粒子(めっき核)を分散させることによって、溶剤系のめっき核剤1を調製した。
Claims (19)
- 重量平均分子量10万以上で、かつ、酸価10〜80であるビニル樹脂(A)と、水性媒体(B)と、必要に応じて水溶性樹脂(c1)及び充填材(c2)からなる群より選ばれる1種以上の成分(C)とを含有するものであり、前記ビニル樹脂(A)が水性媒体(B)に分散し、かつ、前記ビニル樹脂(A)の全量に対する前記成分(C)の含有量が0質量%〜15質量%であることを特徴とする受容層形成用樹脂組成物。
- 前記受容層形成用樹脂組成物が、導電性物質を含有する流動体を受容する層を形成するものである請求項1に記載の受容層形成用樹脂組成物。
- 前記導電性物質を含有する流動体が、導電性物質を含有する導電性インク、または、導電性物質を含有するめっき核剤である請求項2に記載の受容層形成用樹脂組成物。
- 前記ビニル樹脂(A)がビニル単量体混合物を重合して得られるものであって、前記ビニル単量体混合物が、前記ビニル単量体混合物の全量に対して酸基を有するビニル単量体を0.2質量%〜15質量%含有するものである請求項1に記載の受容層形成用樹脂組成物。
- 前記ビニル樹脂(A)がビニル単量体混合物を重合して得られるものであって、前記ビニル単量体混合物が、前記ビニル単量体混合物の全量に対して酸基を有するビニル単量体を0.2質量%〜15質量%、メタクリル酸メチルを0.01質量%〜80質量%、及び、炭素原子数2〜12のアルキル基を有する(メタ)アクリル酸アルキルエステルを5質量%〜60質量%含有するものである請求項1に記載の受容層形成用樹脂組成物。
- 前記ビニル樹脂(A)が、架橋性官能基を有するものである請求項1に記載の受容層形成用樹脂組成物。
- 前記架橋性官能基が、メチロールアミド基及びアルコキシメチルアミド基からなる群より選ばれる1種以上の熱架橋性官能基である請求項6に記載の受容層形成用樹脂組成物。
- 更に、架橋剤(D)を含有するものであって、前記架橋剤(D)が、100℃以上に加熱することによって架橋反応しうるものである請求項1または6に記載の受容層形成用樹脂組成物。
- 前記架橋剤(D)が、メラミン系化合物、エポキシ系化合物、オキサゾリン化合物、カルボジイミド化合物、及び、イソシアネート化合物からなる群より選ばれる1種以上の熱架橋剤(d1−2)である請求項8に記載の受容層形成用樹脂組成物。
- 支持体表面の一部または全部に、請求項1〜9のいずれか1項に記載の受容層形成用樹脂組成物を用いて形成された受容層を有し、前記受容層が導電性物質を含有する流動体を受容するための受容層であることを特徴とする受容基材。
- 請求項10に記載の受容基材を構成する受容層上に、導電性物質を含有する流動体によって印刷の施された印刷物。
- 前記印刷が、インクジェット印刷法、スクリーン印刷法、凸版反転印刷法またはグラビアオフセット印刷法によってなされたものである請求項11に記載の印刷物。
- 請求項10に記載の受容基材を構成する受容層上に、導電性物質を含む導電性インク、または、導電性物質からなる金属を含有するめっき核剤からなる流動体を用いて印刷の施された導電性パターン。
- 請求項10に記載の受容基材に、導電性物質を含有する導電性インク、または、導電性物質を含有するめっき核剤からなる流動体を用いて印刷し、次いで印刷の施された前記受容層に架橋構造を形成することによって得られる導電性パターン。
- 前記流動体を印刷することによって形成された印刷部の表面に、電解めっき処理または無電解めっき処理を施すことによって得られるものである請求項13または14に記載の導電性パターン。
- 請求項13または14に記載の導電性パターンを構成する、前記流動体を印刷することによって形成された印刷部の表面に、電解めっき処理を施すことによって得られる導電性パターン。
- 請求項13〜16のいずれか1項に記載の導電性パターンからなる電気回路。
- 支持体の表面の一部または全部に、請求項1〜9のいずれか1項に記載の受容層形成用樹脂組成物を塗布し、前記受容層形成用樹脂組成物が架橋反応しない条件で乾燥することによって、導電性物質を含有する流動体を受容するための受容層を形成し、次いで、前記受容層の表面に、前記導電性物質を含有する流動体を印刷し、次いで、前記印刷された受容層を加熱することによって架橋構造を形成することを特徴とする印刷物の製造方法。
- 支持体の表面の一部または全部に、請求項1〜9のいずれか1項に記載の受容層形成用樹脂組成物を塗布し、前記受容層形成用樹脂組成物が架橋反応しない条件で乾燥することによって、導電性物質を含有する流動体を受容するための受容層を形成し、次いで、前記受容層の表面に、前記導電性物質を含有する流動体を印刷することで、前記流動体中に含まれる導電性物質からなる印刷部を形成し、次いで、前記印刷された受容層を加熱することによって架橋構造を形成し、次いで前記受容層表面に形成された前記印刷部をめっき処理することを特徴とする導電性パターンの製造方法。
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JP6327443B2 (ja) * | 2013-03-19 | 2018-05-23 | Dic株式会社 | 導電性材料の製造方法及び導電性材料 |
US10150713B2 (en) | 2014-02-21 | 2018-12-11 | Terves, Inc. | Fluid activated disintegrating metal system |
JP6439973B2 (ja) * | 2014-12-24 | 2018-12-19 | Dic株式会社 | 積層体、導電性パターン及び電子回路 |
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WO2019202908A1 (ja) * | 2018-04-19 | 2019-10-24 | 富士フイルム株式会社 | パターンの製造方法、光学フィルタの製造方法、固体撮像素子の製造方法、画像表示装置の製造方法、光硬化性組成物および膜 |
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