JP2013195733A - 感光性導電ペースト - Google Patents
感光性導電ペースト Download PDFInfo
- Publication number
- JP2013195733A JP2013195733A JP2012063163A JP2012063163A JP2013195733A JP 2013195733 A JP2013195733 A JP 2013195733A JP 2012063163 A JP2012063163 A JP 2012063163A JP 2012063163 A JP2012063163 A JP 2012063163A JP 2013195733 A JP2013195733 A JP 2013195733A
- Authority
- JP
- Japan
- Prior art keywords
- photosensitive
- conductive paste
- conductive
- acrylate
- pattern
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002245 particle Substances 0.000 claims abstract description 38
- 239000000945 filler Substances 0.000 claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 239000000758 substrate Substances 0.000 claims description 26
- 239000002253 acid Substances 0.000 claims description 22
- 238000000576 coating method Methods 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 13
- 239000003999 initiator Substances 0.000 claims description 10
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 7
- 229910001887 tin oxide Inorganic materials 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000004020 conductor Substances 0.000 claims description 2
- 238000000059 patterning Methods 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 description 17
- 239000000178 monomer Substances 0.000 description 16
- 239000002904 solvent Substances 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000001723 curing Methods 0.000 description 11
- 238000011161 development Methods 0.000 description 11
- 230000018109 developmental process Effects 0.000 description 11
- 238000001035 drying Methods 0.000 description 11
- 238000000034 method Methods 0.000 description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 8
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 7
- -1 2-methylbenzoyl Chemical group 0.000 description 7
- 230000009477 glass transition Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 6
- VVBLNCFGVYUYGU-UHFFFAOYSA-N 4,4'-Bis(dimethylamino)benzophenone Chemical compound C1=CC(N(C)C)=CC=C1C(=O)C1=CC=C(N(C)C)C=C1 VVBLNCFGVYUYGU-UHFFFAOYSA-N 0.000 description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- 238000007334 copolymerization reaction Methods 0.000 description 6
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229920002799 BoPET Polymers 0.000 description 5
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 150000002923 oximes Chemical class 0.000 description 5
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 4
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011246 composite particle Substances 0.000 description 4
- 239000011162 core material Substances 0.000 description 4
- 125000004386 diacrylate group Chemical group 0.000 description 4
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 4
- 229920001721 polyimide Polymers 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- WDQMWEYDKDCEHT-UHFFFAOYSA-N 2-ethylhexyl 2-methylprop-2-enoate Chemical compound CCCCC(CC)COC(=O)C(C)=C WDQMWEYDKDCEHT-UHFFFAOYSA-N 0.000 description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 3
- 229920006243 acrylic copolymer Polymers 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229940116333 ethyl lactate Drugs 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 2
- YIKSHDNOAYSSPX-UHFFFAOYSA-N 1-propan-2-ylthioxanthen-9-one Chemical compound S1C2=CC=CC=C2C(=O)C2=C1C=CC=C2C(C)C YIKSHDNOAYSSPX-UHFFFAOYSA-N 0.000 description 2
- BTJPUDCSZVCXFQ-UHFFFAOYSA-N 2,4-diethylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC(CC)=C3SC2=C1 BTJPUDCSZVCXFQ-UHFFFAOYSA-N 0.000 description 2
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 2
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 description 2
- INQDDHNZXOAFFD-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOC(=O)C=C INQDDHNZXOAFFD-UHFFFAOYSA-N 0.000 description 2
- UHFFVFAKEGKNAQ-UHFFFAOYSA-N 2-benzyl-2-(dimethylamino)-1-(4-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=C(N2CCOCC2)C=CC=1C(=O)C(CC)(N(C)C)CC1=CC=CC=C1 UHFFVFAKEGKNAQ-UHFFFAOYSA-N 0.000 description 2
- BQZJOQXSCSZQPS-UHFFFAOYSA-N 2-methoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OC)C(=O)C1=CC=CC=C1 BQZJOQXSCSZQPS-UHFFFAOYSA-N 0.000 description 2
- RZVINYQDSSQUKO-UHFFFAOYSA-N 2-phenoxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC1=CC=CC=C1 RZVINYQDSSQUKO-UHFFFAOYSA-N 0.000 description 2
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- ZWMAYLMVFSCMMS-UHFFFAOYSA-N 4-ethynyl-n,n-dimethylaniline Chemical group CN(C)C1=CC=C(C#C)C=C1 ZWMAYLMVFSCMMS-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- DQFBYFPFKXHELB-UHFFFAOYSA-N Chalcone Natural products C=1C=CC=CC=1C(=O)C=CC1=CC=CC=C1 DQFBYFPFKXHELB-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
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- 239000005977 Ethylene Substances 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
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- LGPAKRMZNPYPMG-UHFFFAOYSA-N (3-hydroxy-2-prop-2-enoyloxypropyl) prop-2-enoate Chemical compound C=CC(=O)OC(CO)COC(=O)C=C LGPAKRMZNPYPMG-UHFFFAOYSA-N 0.000 description 1
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- Manufacturing Of Printed Circuit Boards (AREA)
Abstract
【解決手段】導電性粒子(A)、感光性成分(B)、光重合開始剤(C)、および針状フィラー(D)を含み、前記針状フィラー(D)のアスペクト比が1.5〜50の範囲内であることを特徴とする感光性導電ペーストとする。
【選択図】なし
Description
本発明の感光性導電ペーストに含まれる導電性粒子(A)はAg、Au、Cu、Pt、Pb、Sn、Ni、Al、W、Mo、酸化ルテニウム、Cr、Ti、およびインジウムの少なくとも1種を含むことが好ましく、これらの導電性粒子を単独、合金、あるいは混合粉末として用いることができる。また、上述の成分で絶縁性粒子または導電性粒子の表面を被膜した導電性粒子も同様に用いることができる。中でも導電性の観点からAg、CuおよびAuが好ましく、コスト、安定性の観点からAgがより好ましい。
本発明の感光性導電ペーストに含まれる不飽和二重結合を有し、酸価が30〜250mgKOH/gの範囲内である感光性成分(B)としては、分子内に不飽和二重結合を少なくとも一つ以上有するモノマー、オリゴマーもしくはポリマーのことをいい、1種または2種以上使用することができる。
光重合開始剤(C)の添加量としては、不飽和二重結合を有し、酸価が30〜250mgKOH/gの範囲内である感光性成分(B)100重量部に対し、好ましくは0.05〜30重量部の範囲で添加され、より好ましくは、5〜20重量部である。感光性成分(B)100重量部に対する光重合開始剤(C)の添加量を5重量部以上とすることにより、特に露光部の硬化密度が増加し、現像後の残膜率を高くすることができる。また、感光性成分(B)100重量部に対する光重合開始剤(C)の添加量を20重量部以下とすることで、特に光重合開始剤(C)による塗布膜上部での過剰な光吸収を抑制し、導電パターンが逆テーパー形状となり基材との接着性が低下することを抑制することができる。
チタン酸バリウム、チタン酸ジルコン酸鉛、マイカ、合成マイカ、モンモリナイト、バーミキュライト、炭素繊維、ケブラー繊維、チタン酸カリウム、ゾノトライト、硫酸バリウム、二硫化モリブデン、タルク、テフロン粉、塩基性硫酸マグネシウム、硫酸マグネシウム、シリカ、炭酸カルシウム、ガラスバルーン、シラスバルーン、シリカバルーン、樹脂バルーン、木炭、酸化チタン、ハイドロタルサイト、水酸化アルミニウム、水酸化マグネシウム、酸化アンチモン、ホウ酸、ホウ酸亜鉛、炭酸亜鉛、赤リン、ベーマイト、炭酸リチウム、酸化セリウム、銀イオン肝持ゼオライト、金属フタロシアニン、カテキン、シリカゲル、ゼオライト、セピオライト、ウォラストナイト、ホウ酸アルミニウム、PMF(Processed Mineral Filler)、ドーソナイト、セリサイト、ガラスフレーク、クレー、ハイドロタルサイト、ケイ酸カルシウム等が挙げられるが、これらに限定されない。テトラポット型も針状フィラー(D)に含まれる。これらの針状フィラーを単独あるいは混合粉末として利用できる。また、上述の絶縁性粒子または導電性粒子の表面を導電性物質で被膜した導電性粒子も同様に用いることができる。具体的には、酸化チタンやチタン酸カリウム等のチタン化合物の表面に酸化スズ系またはカーボン系の導電材料をコーティングしたものが好ましいが、これらに限定されない。
針状フィラー(D)アスペクト比はSEMもしくはTEM画像から100個の粒子のアスペクト比を求め、その平均値とした。
PETフィルム上に感光性導電ペーストを乾燥厚みが10μmになるように塗布、90℃の乾燥オーブンで10分間乾燥し、一定のラインアンドスペース(L/S)で配列する直線群を1つのユニットとし、L/Sの値が異なる9種類のユニットを有する透光パターンを有するフォトマスクを介して露光、現像、そして130℃で1時間キュアすることによって導電パターンを得た。各ユニットのL/Sの値は500/500、250/250、100/100、50/50、40/40、30/30、25/25、20/20、15/15とした(それぞれライン幅(μm)/間隔(μm)を表す)。パターンを光学顕微鏡により観察し、パターン間に残渣がなく、かつパターン剥がれのない最小のL/Sの値を持つパターンを確認し、この最小のL/Sの値を現像可能なL/Sとした。
<比抵抗率の評価方法>
PETフィルム上に導電ペーストを乾燥厚みが10μmになるように塗布、90℃の乾燥オーブンで10分間乾燥し、図1に示すパターンの透光部Aを有するフォトマスクを介して露光し、現像そして140℃で1時間乾燥オーブンでキュアすることによって比抵抗率測定用導電性パターンを得た。導電性パターンのライン幅は0.400mm、ライン長さは80mmである。得られたパターンの端部を表面抵抗計でつなぎ、表面抵抗値を測定し、下記の計算式に当てはめて比抵抗率を算出した。なお膜厚の測定は触針式段差計“サーフコム1400”(商品名、(株)東京精密製)を用いて行った。膜厚の測定はランダムに3箇所の位置にて測り、その3点の平均値を膜厚とした。測長は1mm、走査速度は0.3mm/sとした。線幅はパターンを光学顕微鏡でランダムに3箇所の位置を観察し、画像データを解析して得られた3点の平均値を線幅とした。
比抵抗率=表面抵抗値×膜厚×線幅/ライン長
<ITOとの接続信頼性評価方法>
PETフィルムにITOが全面スパッタされた透明導電フィルム上に導電ペーストを乾燥厚みが10μmになるように塗布し、90℃の乾燥オーブンで10分間乾燥し、図2に示すパターンの透光部Aを有するフォトマスクを介して露光し、現像そして140℃で1時間乾燥オーブンでキュアすることによってITOとの接続信頼性評価サンプルを得た。導電性パターンのライン幅は100μm、ライン間は5mm、端子部は直径2mmの円形である。得られたサンプルの端子部をテスターでつなぎ、初期抵抗を測定した後、85℃、85%RHの恒温恒湿槽“LU−113”(商品名、エスペック(株))に500h投入した。その後、取り出したサンプルの端子部を再度テスターでつなぎ抵抗値を測定し、下記式を用いて抵抗変化率を算出し、1.3以下のものを○、1.3より大きいものは×とした。
<平均粒子径の測定>
導電性粒子径(A)の平均粒子径は、HORIBA社製動的光散乱式粒度分布計により体積平均粒子径を測定した。
・不飽和二重結合を有し、酸価が30〜250mgKOH/gの範囲内である感光性成分(B)
(合成例1)不飽和二重結合を有し、酸価が30〜250mgKOH/gの範囲内である感光性成分 B−1
エチルアクリレート(EA)/メタクリル酸2−エチルヘキシル(2−EHMA)/スチレン(St)/アクリル酸(AA)の共重合体(共重合比率:20重量部/40重量部/20重量部/15重量部)にグリシジルメタクリレート(GMA)を5重量部付加反応させたもの
窒素雰囲気の反応容器中にジエチレングリコールモノエチルエーテルアセテート150gを仕込みオイルバスを用いて80℃まで昇温した。これに、エチルアクリレート20g、メタクリル酸2−エチルヘキシル40g、スチレン20g、アクリル酸15g、2,2’−アゾビスイソブチロニトリル0.8gおよびジエチレングリコールモノエチルエーテルアセテート10gからなる混合物を1時間かけて滴下した。滴下終了後、さらに6時間重合反応を行った。その後、ハイドロキノンモノメチルエーテル1gを添加して重合反応を停止した。引き続きグリシジルメタクリレート5g、トリエチルベンジルアンモニウムクロライド1gおよびジエチレングリコールモノエチルエーテルアセテート10gからなる混合物を0.5時間かけて滴下した。滴下終了後、さらに2時間付加反応を行った。得られた反応溶液をメタノールで精製することで未反応不純物を除去し、さらに24時間真空乾燥することで感光性成分B−1を得た。得られた感光性成分B−1の酸価は103mgKOH/g、式(1)より求めたガラス転移温度は21.7℃であった。
(合成例2)不飽和二重結合を有し、酸価が30〜250mgKOH/gの範囲である感光性成分 B−2
エチレンオキサイド変性ビスフェノールAジアクリレートFA−324A(製品名、日立化成工業株式会社製)/EA/AAの共重合体(共重合比率:50重量部/10重量部/15重量部)にグリシジルメタクリレート(GMA)を5重量部付加反応させたもの
窒素雰囲気の反応容器中にジエチレングリコールモノエチルエーテルアセテート150gを仕込みオイルバスを用いて80℃まで昇温した。これに、エチレンオキサイド変性ビスフェノールAジアクリレートFA−324Aを50g、エチルアクリレート20g、アクリル酸15g、2,2’−アゾビスイソブチロニトリル0.8gおよびジエチレングリコールモノエチルエーテルアセテート10gからなる混合物を1時間かけて滴下した。滴下終了後、さらに6時間重合反応を行った。その後、ハイドロキノンモノメチルエーテル1gを添加して重合反応を停止した。引き続きグリシジルメタクリレート5g、トリエチルベンジルアンモニウムクロライド1gおよびジエチレングリコールモノエチルエーテルアセテート10gからなる混合物を0.5時間かけて滴下した。滴下終了後、さらに2時間付加反応を行った。得られた反応溶液をメタノールで精製することで未反応不純物を除去し、さらに24時間真空乾燥することで感光性成分B−2を得た。得られた感光性成分B−2の酸価は96mgKOH/g、式(1)より求めたガラス転移温度は19.9℃であった。
・光重合開始剤(C)
IRGACURE 369(商品名、チバジャパン株式会社製)
・ 針状フィラー粒子(D)
針状フィラー粒子(D−1)
FT−1000(商品名、石原産業株式会社製、酸化チタンからなる芯材をアンチモンドープ酸化スズで被覆した複合粒子、アスペクト比12.9、平均繊維径0.13μm)
針状フィラー粒子(D−2)
デントールWK500(商品名、大塚化学株式会社製、チタン酸カリウム繊維からなる心材をアンチモンドープ酸化スズで被覆した複合粒子、アスペクト比23.3、平均繊維径 0.3μm)
針状フィラー粒子(D−3)
FTL−200(商品名、石原産業株式会社製、酸化チタン、アスペクト比33.5、平均繊維径0.25μm)
針状フィラー粒子(D−4)
MOS(商品名、宇部興産株式会社製、アスペクト比42.4、平均繊維径0.2μm)
針状フィラー粒子(D−5)
デントールWK500B(商品名、大塚化学株式会社製、チタン酸カリウム繊維からなる心材をアンチモンドープ酸化スズで被覆した複合粒子、アスペクト比60.5、平均繊維径 0.1μm)
針状フィラー粒子(D−6)
ET−500W(商品名、石原産業株式会社製、酸化チタンからなる芯材をアンチモンドープ酸化スズで被覆した複合粒子、アスペクト比1.1、体積平均粒子径0.3μm)
・モノマー:ライトアクリレートBP−4EA(共栄社化学株式会社製)
・溶剤:ジエチレングリコールモノエチルエーテルアセテート(東京化成工業株式会社製)
実施例1
100mlクリーンボトルに化合物B−1を10.0g、光重合開始剤IRGACURE369(チバジャパン株式会社製)を2.0g、ライトアクリレートBP−4EA(共栄社化学株式会社製)を2.0g、ジエチレングリコールモノエチルエーテルアセテートを8.0gいれ、“あわとり錬太郎”(商品名、ARE−310、株式会社シンキー社製)で混合し、感光性樹脂溶液22.0g(固形分63.6重量%)を得た。
得られた感光性樹脂溶液22.0gと平均粒子径2μmのAg粒子を93.7g、FT−1000(石原産業株式会社製)を1.91g混ぜ合わせ、3本ローラー“EXAKT M−50”(商品名、EXAKT社製)を用いて混練し、117.61gの感光性導電ペーストを得た。
表1に示す組成の感光性導電ペーストを実施例1と同様の方法で製造し、評価結果を表1に示した。
表1に示す組成の感光性導電ペーストを実施例1と同様の方法で製造し、評価結果を表2に示した。
B、C サンプル短辺
D 導電パターン
E ポリイミドフィルム
Claims (5)
- 導電性粒子(A)、感光性成分(B)、光重合開始剤(C)、および針状フィラー(D)を含み、前記針状フィラー(D)のアスペクト比が1.5〜50の範囲内であることを特徴とする感光性導電ペースト。
- 前記針状フィラー(D)が、酸化スズ系またはカーボン系の導電材料をコーティングして導電処理していることを特徴とする請求項1記載の感光性導電ペースト。
- 前記導電性粒子(A)の体積平均粒子径が0.1〜10μmの範囲であることを特徴とする請求項1または2記載の感光性導電ペースト。
- 感光性成分(B)が、不飽和二重結合を有し、酸価が30〜250mgKOH/gの範囲内であることを特徴とする請求項1〜3のいずれかに記載の感光性導電ペースト。
- 請求項1〜4のいずれかに記載の感光性導電ペーストを基板上に塗布し、乾燥し、露光し、現像した後に100℃以上300℃以下の温度でキュアすることを特徴とする導電パターンの製造方法。
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