JP6645185B2 - 硬化膜付き透明基材の製造方法 - Google Patents
硬化膜付き透明基材の製造方法 Download PDFInfo
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- JP6645185B2 JP6645185B2 JP2015521461A JP2015521461A JP6645185B2 JP 6645185 B2 JP6645185 B2 JP 6645185B2 JP 2015521461 A JP2015521461 A JP 2015521461A JP 2015521461 A JP2015521461 A JP 2015521461A JP 6645185 B2 JP6645185 B2 JP 6645185B2
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- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
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- 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
- G03F7/027—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
- 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
- G03F7/20—Exposure; Apparatus therefor
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
- G06F3/044—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means
- G06F3/0443—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means using a single layer of sensing electrodes
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
- G06F3/044—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means
- G06F3/0446—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means using a grid-like structure of electrodes in at least two directions, e.g. using row and column electrodes
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
- G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
- G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
- G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
- G06F2203/04111—Cross over in capacitive digitiser, i.e. details of structures for connecting electrodes of the sensing pattern where the connections cross each other, e.g. bridge structures comprising an insulating layer, or vias through substrate
-
- 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
- H05K3/285—Permanent coating compositions
- H05K3/287—Photosensitive compositions
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- Chemical & Material Sciences (AREA)
- Human Computer Interaction (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials For Photolithography (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
Description
酸価=0.1×Vf×56.1/(Wp×I/100)
式中、VfはKOHの滴定量(mL)を示し、Wpは測定したバインダーポリマーを含有する溶液の重量(g)を示し、Iは測定したバインダーポリマーを含有する溶液中の不揮発分の割合(質量%)を示す。
水酸基価=(A−B)×f×56.11×0.5/試料(g)+酸価
式中、Aは空試験に用いた0.5mol/L水酸化カリウムのエタノール溶液の量(mL)を示し、Bは滴定に用いた0.5mol/L水酸化カリウムのエタノール溶液の量(mL)を示し、fはファクターを示す。
本実施形態に係る電子部品は、本実施形態に係る硬化膜付き透明基材を備える。硬化膜付き透明基材は、透明基材上に、本実施形態に係る感光性樹脂組成物の硬化物(硬化膜等)を備えている。本実施形態に係る電子部品において、硬化膜は、例えば、保護部材(保護膜等)、絶縁部材(絶縁膜等)などとして用いることもできる。
撹拌機、還流冷却器、不活性ガス導入口及び温度計を備えたフラスコに、表1に示す(1)を仕込み、窒素ガス雰囲気下で80℃に昇温し、反応温度を80℃±2℃に保ちながら、表1に示す(2)を4時間かけて均一に滴下した。(2)の滴下後、80℃±2℃で6時間撹拌を続け、重量平均分子量が約65,000、酸価が78mgKOH/gのバインダーポリマーの溶液(固形分45質量%)(A1)を得た。
上記(A1)と同様にし、重量平均分子量が約80,000、酸価が115mgKOH/gのバインダーポリマーの溶液(固形分45質量%)(A2)を得た。
上記(A1)と同様にし、重量平均分子量が約60,000、酸価が91mgKOH/gのバインダーポリマーの溶液(固形分45質量%)(A3)を得た。
上記(A1)と同様にし、重量平均分子量が約90,000、酸価が91mgKOH/gのバインダーポリマーの溶液(固形分45質量%)(A4)を得た。
GPC条件
ポンプ:日立 L−6000型(株式会社日立製作所製、製品名)
カラム:Gelpack GL−R420、Gelpack GL−R430、Gelpack GL−R440(以上、日立化成株式会社製、製品名)
カラム仕様:直径10.7mm × 300mm
溶離液:テトラヒドロフラン
試料濃度:NV(不揮発分濃度)50質量%の樹脂溶液を120mg採取、5mLのTHFに溶解
注入量:200μL
圧力:4.9MPa
測定温度:40℃
流量:2.05mL/分
検出器:日立 L−3300型RI(株式会社日立製作所製、製品名)
酸価は、次のようにして測定した。まず、バインダーポリマーの溶液を、130℃で1時間加熱し、揮発分を除去して、固形分を得た。そして、酸価を測定すべきポリマー1.0gを精秤した後、このポリマーにアセトンを30g添加し、これを均一に溶解した。次いで、指示薬であるフェノールフタレインをその溶液に適量添加して、0.1NのKOH水溶液を用いて滴定を行った。そして、バインダーポリマーのアセトン溶液を中和するのに必要なKOHのmg数を次式により算出し、酸価を求めた。
酸価=0.1×Vf×56.1/(Wp×I/100)
式中、VfはKOHの滴定量(mL)を示し、Wpは測定したポリマー溶液の重量(g)を示し、Iは測定したポリマー溶液中の不揮発分の割合(質量%)を示す。
[硬化膜を形成するための感光性樹脂組成物溶液(V−1)の調製]
表2に示す材料を、攪拌機を用いて15分間混合し、硬化膜を形成するための感光性樹脂組成物溶液(V−1)を調製した。
支持フィルムとして厚さ50μmのポリエチレンテレフタレートフィルムを使用し、感光性樹脂組成物溶液(V−1)を支持フィルム上にコンマコーターを用いて均一に塗布し、100℃の熱風対流式乾燥機で3分間乾燥して溶剤を除去し、感光性樹脂組成物からなる感光層(感光性樹脂組成物層)を形成した。得られた感光層の厚さは5μmであった。
得られた感光性エレメント(E−1)のカバーフィルムであるポリエチレンフィルムをはがしながら、厚さ1mmのガラス基板上に、感光層が接するようにラミネータ(日立化成株式会社製、商品名:HLM−3000型)を用いて、ロール温度120℃、基板送り速度1m/分、圧着圧力(シリンダ圧力)4×105Pa(厚さが1mm、縦10cm×横10cmの基板を用いたため、このときの線圧は9.8×103N/m)の条件でラミネートして、ガラス基板上に、感光層及び支持フィルムが積層された積層体を作製した。
得られた感光性エレメント(E−1)の保護フィルムであるポリエチレンフィルムをはがしながら、厚さ0.7mmのガラス基板(b*:0.1〜0.2)上に、感光層が接するようにラミネータ(日立化成株式会社製、商品名:HLM−3000型)を用いて、ロール温度120℃、基板送り速度1m/分、圧着圧力(シリンダ圧力)4×105Pa(厚さが1mm、縦10cm×横10cmの基板を用いたため、この時の線圧は9.8×103N/m)の条件でラミネートして、ガラス基板上に、感光層及び支持体フィルムが積層された基板を作製した。
得られた感光性エレメント(E−1)のカバーフィルムであるポリエチレンフィルムをはがしながら、スパッタ銅付きポリイミドフィルム(東レフィルム加工株式会社製)上に、感光層が接するようにラミネータ(日立化成株式会社製、商品名:HLM−3000型)を用いて、ロール温度120℃、基板送り速度1m/分、圧着圧力(シリンダ圧力)4×105Pa(厚さが1mm、縦10cm×横10cmの基板を用いたため、この時の線圧は9.8×103N/m)の条件でラミネートして、スパッタ銅上に、感光層及び支持フィルムが積層された積層体を作製した。
A : 保護膜表面に全く変化なし。
B : 保護膜表面にごくわずかな痕跡が見えるが、銅は変化なし。
C : 保護膜表面に痕跡が見えるが、銅は変化なし。
D : 保護膜表面に痕跡があり、かつ銅が変色する。
評価用試料の表面状態を観察したところ、保護膜表面に全く変化なく評価はAであった。
得られた感光性エレメント(E−1)のポリエチレンフィルムをはがしながら、厚さ50μmのポリエチレンテレフタレートフィルム上に、感光層が接するようにロール温度100℃、基板送り速度0.6m/分、圧着圧力(シリンダ圧力)0.5MPaの条件でラミネートし、ポリエチレンテレフタレートフィルム上に感光層および支持フィルムが積層された積層体を作製した。
A : ≦φ2.0mmの円筒を用い、保護膜にクラックなし。
B : φ3.0〜φ4.0mmの円筒を用い、保護膜にクラックなし。
C : ≧φ5.0の円筒を用い、保護膜にクラックなし。
評価用試料の保護膜表面状態を観察したところ、φ2.0mmの円筒を用いてもクラックが見られなかったため、評価はAであった。
得られた感光性樹脂組成物溶液(V−1)を厚さ50μmのポリエチレンテレフタレートフィルム上に、アプリケータを用いて均一に塗布し、厚み40μmの感光性エレメント(E−2)を作製した。得られた感光性エレメント(E−2)をNo.5Cろ紙(アドバンテック製)上に感光層が接するようにロール温度80℃、基板送り速度0.6m/分、圧着圧力(シリンダ圧力)0.5MPaの条件でラミネートし、No.5Cろ紙上に感光層およびポリエチレンテレフタレートフィルムが積層した積層体を作製した。
A : 透湿度≦450(g/m2・24h)である。
B : 450<透湿度≦550(g/m2・24h)である。
C : 550<透湿度≦650(g/m2・24h)である。
D : 透湿度>650(g/m2・24h)である。
実施例1においては、透湿度が450(g/m2・24h)未満であったため、評価はAであった。
表3(表中の数値の単位は質量部)に示す感光性樹脂組成物溶液を用いた以外は、実施例1と同様に感光性エレメントを作製し、塩水噴霧試験、マンドレル試験、透湿度測定を行った。表3に示すように、実施例1〜4においては、耐塩水性評価、マンドレル試験、透湿度測定のいずれも良好な結果であった。
(A1):メタクリル酸/メタクリル酸メチル/アクリル酸エチル=12/58/30(質量比)、酸価78(mgKOH/g)
(A2):メタクリル酸/メタクリル酸メチル/アクリル酸エチル=17.5/52.5/30(質量比)、酸価115(mgKOH/g)
(A3):メタクリル酸/メタクリル酸メチル/アクリル酸エチル=14/56/30(質量比)、酸価91(mgKOH/g)
(A4):メタクリル酸/メタクリル酸メチル/アクリル酸エチル=14/61/25(質量比)、酸価91(mgKOH/g)
(B)成分:光重合性化合物
T−1420(T):ジトリメチロールプロパンテトラアクリレート(日本化薬株式会社製)
その他の光重合性化合物
A−TMMT:ペンタエリスリトールテトラアクリレート(新中村化学工業株式会社製)
TMPTA:トリメチロールプロパントリアクリレート(日本化薬株式会社製)、
RP−1040:EO変性ペンタエリスリトールテトラアクリレート(日本化薬株式会社製)
BPE−500:エトキシ化ビスフェノールAジメタクリレート(新中村化学工業株式会社製)
4G:ポリエチレングリコール#200ジメタクリレート(新中村化学工業株式会社製)
(C)成分:光重合開始剤
OXE01:1,2−オクタンジオン,1−[4−(フェニルチオ)−,2−(o−ベンゾイルオキシム)](BASF株式会社製、商品名:IRGACURE OXE 01)
その他AW−500:2,2’−メチレン−ビス(4−エチル−6−Tert−ブチルフェノール)(アンテージW−500、川口化学株式会社製)
SH−30:有機変性シリコーンオイル(東レ・ダウコーニング株式会社製)
メチルエチルケトン:東燃化学株式会社製
Claims (3)
- 支持フィルムと、該支持フィルム上に設けられた感光層と、を備える感光性エレメントを用意する工程と、
前記感光性エレメントの前記感光層を、タッチパネルの額縁領域に銅を含む引き出し配線を有するタッチパネル用透明基材上にラミネートする工程と、
ラミネートされた前記感光層の所定部分を活性光線の照射により硬化させた後に前記感光層の前記所定部分以外を除去し、前記引き出し配線の一部又は全部を被覆する前記感光層の硬化物からなる硬化膜を形成する工程と、を備え、
前記感光層が、バインダーポリマー、ジトリメチロールプロパン由来の骨格を有する(メタ)アクリレート化合物を含む光重合性化合物、及び光重合開始剤を含有する感光性樹脂組成物からなり、厚さが3〜8μmであり、可視光線透過率が90%以上であり、
前記バインダーポリマーの重量平均分子量が、30,000〜150,000であり、
前記バインダーポリマーの含有量が、前記バインダーポリマー及び前記光重合性化合物の合計量100質量部に対して、55〜65質量部であり、
前記光重合性化合物の含有量が、前記バインダーポリマー及び前記光重合性化合物の合計量100質量部に対して、35〜45質量部であり、
前記透明基材がフレキシブルディスプレイ基板である、硬化膜付き透明基材の製造方法。 - 前記(メタ)アクリレート化合物が4以上の(メタ)アクリロイル基を有する化合物である、請求項1に記載の硬化膜付き透明基材の製造方法。
- 前記光重合開始剤がオキシムエステル化合物及び/又はホスフィンオキサイド化合物を含有する、請求項1又は2に記載の硬化膜付き透明基材の製造方法。
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US10935891B2 (en) | 2017-03-13 | 2021-03-02 | Holo, Inc. | Multi wavelength stereolithography hardware configurations |
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