JP7270204B2 - 皮膜の製造方法及びプリント配線板 - Google Patents
皮膜の製造方法及びプリント配線板 Download PDFInfo
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- JP7270204B2 JP7270204B2 JP2018211258A JP2018211258A JP7270204B2 JP 7270204 B2 JP7270204 B2 JP 7270204B2 JP 2018211258 A JP2018211258 A JP 2018211258A JP 2018211258 A JP2018211258 A JP 2018211258A JP 7270204 B2 JP7270204 B2 JP 7270204B2
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- AUONHKJOIZSQGR-UHFFFAOYSA-N oxophosphane Chemical compound P=O AUONHKJOIZSQGR-UHFFFAOYSA-N 0.000 description 1
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- 239000013034 phenoxy resin Substances 0.000 description 1
- 229920006287 phenoxy resin Polymers 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 230000002165 photosensitisation Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 229940086066 potassium hydrogencarbonate Drugs 0.000 description 1
- 235000011118 potassium hydroxide Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- FYNROBRQIVCIQF-UHFFFAOYSA-N pyrrolo[3,2-b]pyrrole-5,6-dione Chemical class C1=CN=C2C(=O)C(=O)N=C21 FYNROBRQIVCIQF-UHFFFAOYSA-N 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000001062 red colorant Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 125000006158 tetracarboxylic acid group Chemical group 0.000 description 1
- 150000000000 tetracarboxylic acids Chemical class 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- NIUZJTWSUGSWJI-UHFFFAOYSA-M triethyl(methyl)azanium;chloride Chemical compound [Cl-].CC[N+](C)(CC)CC NIUZJTWSUGSWJI-UHFFFAOYSA-M 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- HVYVMSPIJIWUNA-UHFFFAOYSA-N triphenylstibine Chemical compound C1=CC=CC=C1[Sb](C=1C=CC=CC=1)C1=CC=CC=C1 HVYVMSPIJIWUNA-UHFFFAOYSA-N 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 150000007964 xanthones Chemical class 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
- C08F2/50—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light with sensitising agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
- G03F7/028—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds with photosensitivity-increasing substances, e.g. photoinitiators
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
- G03F7/028—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds with photosensitivity-increasing substances, e.g. photoinitiators
- G03F7/029—Inorganic compounds; Onium compounds; Organic compounds having hetero atoms other than oxygen, nitrogen or sulfur
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
- G03F7/028—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds with photosensitivity-increasing substances, e.g. photoinitiators
- G03F7/031—Organic compounds not covered by group G03F7/029
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
- G03F7/032—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds with binders
- G03F7/033—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds with binders the binders being polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. vinyl polymers
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/09—Photosensitive materials characterised by structural details, e.g. supports, auxiliary layers
- G03F7/105—Photosensitive materials characterised by structural details, e.g. supports, auxiliary layers having substances, e.g. indicators, for forming visible images
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/20—Exposure; Apparatus therefor
- G03F7/2002—Exposure; Apparatus therefor with visible light or UV light, through an original having an opaque pattern on a transparent support, e.g. film printing, projection printing; by reflection of visible or UV light from an original such as a printed image
- G03F7/2004—Exposure; Apparatus therefor with visible light or UV light, through an original having an opaque pattern on a transparent support, e.g. film printing, projection printing; by reflection of visible or UV light from an original such as a printed image characterised by the use of a particular light source, e.g. fluorescent lamps or deep UV light
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/28—Applying non-metallic protective coatings
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Structural Engineering (AREA)
- Architecture (AREA)
- Inorganic Chemistry (AREA)
- Materials For Photolithography (AREA)
- Non-Metallic Protective Coatings For Printed Circuits (AREA)
Description
カラム:SHODEX KF-800P,KF-005,KF-003,KF-001の4本直列、
移動相:THF、
流量:1ml/分、
カラム温度:45℃、
検出器:RI、
換算:ポリスチレン。
(1-1)合成例A-1及び合成例B-1
還流冷却器、温度計、空気吹き込み管及び攪拌機を取付けた四つ口フラスコ内に、表1中の「第一反応」欄に示す成分を加えて、これらをエアバブリング下で攪拌することで混合物を調製した。この混合物をフラスコ内でエアバブリング下で攪拌しながら、「反応条件」欄に示す反応温度及び反応時間で加熱した。これにより、中間体の溶液を調製した。
・エポキシ化合物1:式(7)で示され、式(7)中のR1~R8がすべて水素であるエポキシ当量250g/eqのビスフェノールフルオレン型エポキシ化合物。
・エポキシ化合物2:クレゾールノボラック型エポキシ樹脂(新日鉄住金化学株式会社製、品番YDC-700-5、エポキシ当量203g/eq)。
後掲の表に示す成分の一部を3本ロールで混練してから、後掲の表に示す全成分をフラスコ内で撹拌混合することで、感光性樹脂組成物を得た。なお、表に示される成分の詳細は次の通りである。また、以下の光重合開始剤において、特定の波長に対し「光を吸収しない」とは、光重合開始剤の吸収スペクトルにおいて、「光重合開始剤の350nm以上370nm以下の波長範囲の曲線下面積に対する、各波長範囲の曲線下面積が2%未満である」ことを意味する。例えば、光重合開始剤Bが、「400nm以上415nm以下の波長の光を吸収しない」とは、光重合開始剤Bの吸収スペクトルにおいて、「光重合開始剤Bの350nm以上370nm以下の波長範囲の曲線下面積に対する、400nm以上415nm以下の波長範囲の曲線下面積が2%未満である」ことを意味する。
・不飽和化合物A:トリメチロールプロパントリアクリレート。
・不飽和化合物B:ジペンタエリストールペンタアクリレートとジペンタエリストールヘキサアクリレートの混合体(日本化薬株式会社製、品番KAYARAD DPHA)。
・光重合開始剤A:2,4,6-トリメチルベンゾイル-ジフェニル-フォスフィンオキサイド(BASF社製、品番Irgacure TPO);アシルフォスフィンオキサイド系光重合開始剤。305nm以上325nm以下の波長の光と、350nm以上370nm以下の波長の光と、370nmより長く400nm未満の波長の光と、400nm以上415nm以下の波長の光と、を吸収する特性を有する。
・光重合開始剤B:2-メチル-1-(4-メチルチオフェニル)-2-モルフォリノプロパン-1-オン(BASF社製、品番Irgacure 907);α‐アミノアルキルフェノン系光重合開始剤。305nm以上325nm以下の波長の光と、350nm以上370nm以下の波長の光と、370nmより長く400nm未満の波長の光と、を吸収する特性を有する。400nm以上415nm以下の波長の光を吸収しない。
・光重合開始剤C:エタノン,1-[9-エチル-6-(2-メチルベンゾイル)-9H-カルバゾール-3-イル]-,1-(O-アセチルオキシム)(BASF社製、品番Irgacure OXE 02);オキシムエステル系光重合開始剤。305nm以上325nm以下の波長の光と、350nm以上370nm以下の波長の光と、370nmより長く400nm未満の波長の光と、を吸収する特性を有する。400nm以上415nm以下の波長の光を吸収しない。
・光重合開始剤D:1-ヒドロキシ-シクロヘキシル-フェニル-ケトン(BASF社製、品番Irgacure 184);α-ヒドロキシアルキルフェノン系光重合開始剤。305nm以上325nm以下の波長の光と、350nm以上370nm以下の波長の光と、370nmより長く400nm未満の波長の光と、を吸収する特性を有する。400nm以上415nm以下の波長の光を吸収しない。
・光重合開始剤E:2,4-ジエチルチオキサントン(日本化薬株式会社製、品番KAYACURE-DETX-S);水素引き抜き型光重合開始剤。305nm以上325nm以下の波長の光と、350nm以上370nm以下の波長の光と、370nmより長く400nm未満の波長の光と、400nm以上415nm以下の波長の光と、を吸収する特性を有する。
・光重合開始剤F:4,4’-ビス(ジエチルアミノ)ベンゾフェノン;水素引き抜き型光重合開始剤。305nm以上325nm以下の波長の光と、350nm以上370nm以下の波長の光と、370nmより長く400nm未満の波長の光と、400nm以上415nm以下の波長の光と、を吸収する特性を有する。
・エポキシ樹脂A:ビフェニル型結晶性エポキシ樹脂(三菱化学株式会社製の品名YX-4000、融点105℃、エポキシ当量187g/eq)。
・エポキシ樹脂Bの溶液:長鎖炭素鎖含有ビスフェノールA型エポキシ樹脂(DIC製、品番EPICLON EXA-4816、液状樹脂、エポキシ当量410g/eq)を固形分90%でジエチレングリコールモノエチルエーテルアセテートに溶解させた溶液(固形分90%換算のエポキシ当量は、455.56g/eq)。
・エポキシ樹脂Cの溶液:クレゾールノボラック型エポキシ樹脂(新日鉄住金化学株式会社製の品名YDCN-704、軟化点87~97℃、エポキシ当量208g/eq)を固形分70%でジエチレングリコールモノエチルエーテルアセテートに溶解させた溶液(固形分70%換算のエポキシ当量は、297.14g/eq)。
・黒色着色剤:カーボンブラック分散液、平均粒子径100~300nm、顔料分20%、固形分25%、分散溶剤:プロピレングリコールモノメチルエーテルアセテート。
・青色着色剤:フタロシアニンブルー分散液、平均粒子径100~300nm、顔料分20%、固形分25%、分散溶剤:プロピレングリコールモノメチルエーテルアセテート。
・黄色着色剤:ニッケル錯体顔料分散液、平均粒子径100~300nm、顔料分20%、固形分25%、分散溶剤:プロピレングリコールモノメチルエーテルアセテート。
・メラミン:日産化学工業株式会社製、微粉メラミン;感光性樹脂組成物中において平均粒子径8μmで分散。
・酸化防止剤:ヒンダードフェノール系酸化防止剤(BASF社製、品番IRGANOX 1010)。
・硫酸バリウム:堺化学工業株式会社製、品番バリエースB30。
・ベントナイト:レオックス社製、品番ベントンSD-2。
・有機フィラーの分散液:平均一次粒子径0.07μmのカルボキシル基を有する架橋ゴム(NBR)、JSR株式会社製、品番XER-91-MEK、架橋ゴムの含有割合15重量%のメチルエチルケトン分散液、酸価10.0mgKOH/g。
・カップリング剤:3-グリシドキシプロピルトリメトキシシラン。
・消泡剤:信越化学工業株式会社製、品番KS-66。
・界面活性剤:DIC製、品番メガファックF-477。
・溶剤:メチルエチルケトン。
上記(2)で調製した感光性樹脂組成物を用いて、次のように試験サンプル(塗膜)を作製した。
(4-1)吸光度特性
各実施例の感光性樹脂組成物をポリエチレンテレフタレート製のフィルム上にアプリケータで塗布してから、95℃で25分加熱することで乾燥させることにより、フィルム上に厚み10μmの乾燥塗膜を形成した。ポリエチレンテレフタレート製のフィルム上に形成された各実施例の乾燥塗膜を、紫外可視近赤外分光光度計(株式会社島津製作所製の品番UV-3100PC)にセットして、乾燥塗膜の300~800nmの吸収スペクトルを測定した。リファレンスには、基材であるポリエチレンテレフタレート製のフィルムを使用した。得られた吸収スペクトルより、[波長305~325nmにおける吸光度の最大値]/[波長350~370nmにおける吸光度の最大値]の値(すなわち350nm以上370nm以下の波長範囲での光の最大吸光度に対する、305nm以上325nm以下の波長範囲での光の最大吸光度の比の値)を求め、以下の基準で評価した。
○:[波長305~325nmにおける吸光度の最大値]/[波長350~370nmにおける吸光度の最大値]の値が3以上である。
×:[波長305~325nmにおける吸光度の最大値]/[波長350~370nmにおける吸光度の最大値]の値が3未満である。
上記(3)で作製した各実施例の試験サンプル(塗膜)に露光してから現像することで、皮膜に形成された孔の形状を評価した。具体的には、各実施例の試験サンプル(塗膜)に、ポリエチレンテレフタレート製のフィルム上から、直径60μmの円形形状の非露光部を有する石英ガラスのネガマスクを直接当てがった状態で、光学フィルタ及びネガマスクを介して塗膜に400mJ/cm2の条件で光を照射した。塗膜に光を照射するための光源は、超高圧水銀灯を使用した。超高圧水銀灯が発する光の発光スペクトルは、図1に示すように横軸を波長(単位nm)及び縦軸を相対強度(単位%)として、波長と相対強度とが図1に示すとおりである。下記の露光条件(条件A~F)で光を照射した。なお、露光後、現像前に、塗膜からポリエチレンテレフタレート製のフィルムを剥離した。
光源から発せられる光を、280nm以上415nm以下の波長範囲の光のみを透過させる光学フィルタを通過させてから、塗膜に照射した。
光源から発せられる光を、280nm以上370nm以下の波長範囲の光のみを透過させる光学フィルタを通過させてから、塗膜に照射した。
光源から発せられる光を、光学フィルタを通過させずに、塗膜に照射した。
光源から発せられる光を、350nm以上370nm以下の波長範囲の光のみを透過させる光学フィルタを通過させてから、塗膜に照射した。
光源から発せられる光を、350nm以上415nm以下の波長範囲の光のみを透過させる光学フィルタを通過させてから、塗膜に照射した。
光源から発せられる光を、280nm以上325nm以下の波長範囲の光のみを透過させる光学フィルタを通過させてから、塗膜に照射した。
A:内径の差が4μm未満である。
B:内径の差が4μm以上、6μm未満である。
C:内径の差が6μm以上、8μm未満である。
D:内径の差が8μm以上、10μm未満である。
E:内径の差が10μm以上である。
F:塗膜を十分に光硬化させることができなかったため、孔を形成できなかった。
テストピースにおける導体配線(くし型電極)にDC12Vのバイアス電圧を印加しながら、テストピースを130℃、85%R.H.の試験環境下に100時間曝露した。この試験環境下における硬化物からなる層のくし型電極間の電気抵抗値を常時測定し、その結果を次のように評価した。
A:試験開始時から100時間経過するまでの間、電気抵抗値が常に106Ω以上を維持した。
B:試験開始時から70時間経過するまでは電気抵抗値が常に106Ω以上を維持したが、試験開始時から100時間経過する前に電気抵抗値が106Ω未満となった。
C:試験開始時から70時間経過する前に電気抵抗値が106Ω未満となった。
室温下でテストピースを10%の硫酸水溶液に30分間浸漬した後、硬化物からなる層の外観を観察した。その結果を次に示すように評価した。
A:硬化物からなる層にふくれ、剥離、変色等の異常が認められない。
B:硬化物からなる層にふくれ、剥離、変色等の異常が僅かに認められる。
C:硬化物からなる層にふくれ、剥離、変色等の異常が顕著に認められる。
室温下でテストピースを濃度10質量%の水酸化ナトリウム水溶液に1時間浸漬した後、硬化物からなる層の外観を観察した。その結果を次に示すように評価した。
A:硬化物からなる層にふくれ、剥離、変色等の異常が認められない。
B:硬化物からなる層にふくれ、剥離、変色等の異常が僅かに認められる。
C:硬化物からなる層にふくれ、剥離、変色等の異常が顕著に認められる。
水溶性フラックス(ロンドンケミカル社製、品番LONCO 3355-11)を、テストピースの硬化物からなる層に塗布し、続いて硬化物からなる層を260℃の溶融はんだ浴に10秒間浸漬してから水洗した。この処理を3回繰り返してから、硬化物からなる層の外観を観察し、その結果を次に示すように評価した。
A:硬化物からなる層にふくれ、剥離、変色等の異常が認められない。
B:硬化物からなる層にふくれ、剥離、変色等の異常が僅かに認められる。
C:硬化物からなる層にふくれ、剥離、変色等の異常が顕著に認められる。
市販のメッキ液を用いて、テストピースに無電解ニッケルメッキと無電解金メッキを順次施してから、メッキ層及び硬化物からなる層の状態を確認した。
A:メッキ層の形成前後で硬化物からなる層に外観の変化が認められず、メッキの潜り込みも認められず、セロハン粘着テープ剥離試験には硬化物からなる層の剥離は認められなかった。
B:メッキ層の形成前後で硬化物からなる層に外観の変化が認められないが、セロハン粘着テープ剥離試験には硬化物からなる層の一部剥離が認められる。
C:メッキ層の形成後に硬化物からなる層の浮き上がりが認められ、セロハン粘着テープ剥離試験には硬化物からなる層の剥離が認められる。
2 絶縁層
3 導電層
31 第一の導体配線
4 塗膜
5 非露光部
6 孔
7 層間絶縁層
8 第二の導体配線
9 ホールメッキ
10 スルーホール
11 プリント配線板
40 皮膜
Claims (10)
- 感光性樹脂組成物を基材上に配置することで、前記基材上に塗膜を形成する工程と、
前記塗膜に光源が発する光を、280nmより短く200nm以上の波長範囲内の光、及び415nmより長く500nm以下の波長範囲内の光をカットする光学フィルタを通過させてから照射して露光する工程と、
前記露光後の前記塗膜をアルカリ溶液で現像する工程と、を含む、
皮膜の製造方法であって、
前記感光性樹脂組成物は、カルボキシル基含有樹脂(A)と、エチレン性不飽和結合を一分子中に少なくとも一つ有する不飽和化合物(B)と、光重合開始剤(C)と、エポキシ樹脂(D)と、を含有し、
前記光重合開始剤(C)の光の吸収スペクトルは、
350nm以上370nm以下の波長範囲内にある第一の吸収と、
370nmより長く415nm以下の波長範囲内にある第二の吸収とを有し、
前記露光する工程で塗膜に照射する光のスペクトルは、
350nm以上370nm以下の波長範囲内で前記第一の吸収の波長と重複する波長にある第一の強度分布と、
370nmより長く415nm以下の波長範囲内で前記第二の吸収の波長と重複する波長にある第二の強度分布と、
305nm以上325nm以下の波長範囲内にある第三の強度分布とを有し、
かつ200nm以上500nm以下の波長範囲の曲線下面積に対する、280nmより短く200nmまでの波長範囲の曲線下面積と、415nmより長く500nmまでの波長範囲の曲線下面積との合計の百分比は、5%以下であり、
前記光重合開始剤(C)は、アシルフォスフィンオキサイド系光重合開始剤(C1)、α-アミノアルキルフェノン系光重合開始剤(C2)、及びオキシムエステル系光重合開始剤(C3)からなる群から選択される少なくとも一種を含有する、
皮膜の製造方法。 - 前記第二の吸収は、400nmより長く415nm以下の波長範囲内にある吸収を少なくとも含み、
前記第二の強度分布は、400nmより長く415nm以下の波長範囲内で前記第二の吸収の波長と重複する波長にある強度分布を少なくとも含む、
請求項1に記載の皮膜の製造方法。 - 前記光重合開始剤(C)の光の吸収スペクトルは、305nm以上325nm以下の波長範囲内にある第三の吸収を更に有し、
前記第三の強度分布は、305nm以上325nm以下の波長範囲内で前記第三の吸収の波長と重複する波長にある強度分布を少なくとも含む、
請求項1又は2に記載の皮膜の製造方法。 - 前記塗膜の光の吸収スペクトルにおける、350nm以上370nm以下の波長範囲での最大吸光度に対する、305nm以上325nm以下の波長範囲での最大吸光度は、3倍以上である、
請求項1から3のいずれか一項に記載の皮膜の製造方法。 - 前記光源は、メタルハライドランプ、高圧水銀灯、及び超高圧水銀灯からなる群から選択される少なくとも一種である、
請求項1から4のいずれか一項に記載の皮膜の製造方法。 - 前記光重合開始剤(C)は、水素引き抜き型光重合開始剤(C4)を含む、
請求項1から5のいずれか一項に記載の皮膜の製造方法。 - 前記カルボキシル基含有樹脂(A)は、エチレン性不飽和基を有するカルボキシル基含有樹脂を含む、
請求項1から6のいずれか一項に記載の皮膜の製造方法。 - 前記感光性樹脂組成物は、ビスフェノールフルオレン骨格を有する成分を含む、
請求項1から7のいずれか一項に記載の皮膜の製造方法。 - 前記感光性樹脂組成物は、更に着色顔料(E)を有する、
請求項1から8のいずれか一項に記載の皮膜の製造方法。 - 導電層と、前記導電層に重なる絶縁層とを備え、
前記絶縁層は、請求項1から9のいずれか一項に記載の皮膜の製造方法で製造した皮膜を含む、
プリント配線板。
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