TWI640370B - 使用光起始劑預處理基材之方法 - Google Patents
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- TWI640370B TWI640370B TW103118673A TW103118673A TWI640370B TW I640370 B TWI640370 B TW I640370B TW 103118673 A TW103118673 A TW 103118673A TW 103118673 A TW103118673 A TW 103118673A TW I640370 B TWI640370 B TW I640370B
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Classifications
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
- B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
- B05D3/062—Pretreatment
- B05D3/063—Pretreatment of polymeric substrates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
- C08J7/065—Low-molecular-weight organic substances, e.g. absorption of additives in the surface of the article
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
- B05D3/101—Pretreatment of polymeric substrate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Application Of Or Painting With Fluid Materials (AREA)
- Paints Or Removers (AREA)
- Polymerisation Methods In General (AREA)
- Laminated Bodies (AREA)
- General Chemical & Material Sciences (AREA)
Abstract
本發明係關於一種製備經塗佈之基材的方法，該方法包括(a)塗覆光起始劑至基材之表面上；(b)使該光起始劑曝照紫外線或紫外線可見光輻射以活化該光起始劑且形成預處理表面；及(c)將塗佈組合物施加至該預處理基材上以形成經塗佈之基材。該塗佈組合物可為含有奈米顆粒之乳液。
Description
本申請案主張2013年5月29日申請之美國臨時申請案第61/828,379號之權益。先前申請案之揭示內容被視為本申請案之揭示內容的部分(且以引用的方式併入)。
本發明係關於在塗佈之前預處理基材。
塗佈方法常常需要在塗佈之前處理基材以改良特性，諸如黏著性、濕潤均一性及基材與塗層之間的相容性。該等預處理可藉由改變表面化學性質來改變基材表面之性質。已知的預處理包括化學底塗劑、電暈暴露、電漿暴露及紫外線(UV)暴露。預處理可與塗佈步驟一起在線內進行，或可分別進行。
在Garbar等人之名稱為「製造透明導電塗層之方法(Processes for Making Transparent Conductive Coatings)」的WO 2009/149249中描述了在用自組裝乳液塗佈之前UV活化聚對苯二甲酸伸乙酯(PET)基材以形成透明導電塗層。描述了在1.1m/min.與2.7m/min.之間的線速度。
描述一種製備經塗佈之基材的方法，該方法包括(a)塗覆光起始劑至基材之表面上；(b)使該光起始劑曝照紫外線或紫外線可見光輻
射以活化該光起始劑且形成預處理表面；及(c)將塗佈組合物施加至該預處理基材上以形成經塗佈之基材。該塗佈組合物可為含有奈米顆粒的乳液。用光起始劑預處理基材能夠製備經塗佈之基材，該等經塗佈之基材具有與僅藉由曝照紫外線或紫外線可見光輻射經過預處理的基材相比更高的線速度。
本發明之一或多個實施例之細節闡述於以下描述中。本發明之其他特徵、目標及優點將根據說明書與申請專利範圍變得顯而易見。
適合基材之實例包括聚合薄膜或薄片(諸如聚酯、聚醯胺、聚醯亞胺、聚碳酸酯、聚烯烴、聚(甲基)丙烯酸酯、共聚物)及多層薄膜。基材可為剛性的或可撓的以用於卷軸式處理。
適合之光起始劑之實例包括吸收UV或UV可見光且生成自由基的分子。可使用單一光起始劑或可使用光起始劑之混合物，包括協同光起始劑系統，例如二元或H型光起始劑系統。選擇光起始劑以使得光起始劑之吸收波長與用於起始之光源(例如UV燈或LED)的發射波長重疊。
一種適用類別的光起始劑包括α-羥基酮。A此類別內之光起始劑的市售實例為可購自BASF Resins之Irgacure 184。
光起始劑可以在0.1重量%至10重量%範圍內的濃度溶解於溶劑中。當選擇溶劑或溶劑混合物時需考慮的因素包括光起始劑之溶解度、溶劑之揮發性及溶劑與基材及塗佈方法之相容性。
光起始劑溶液可藉由多種技術沈積於基材上，該等技術包括桿體展佈、浸沒、旋塗、浸漬、狹縫型擠壓式塗佈、凹板印刷式塗佈、柔性凸版印刷、噴塗或任何其他適合之技術。濕潤塗佈厚度可為1至
100μm，較佳為1至10μm。在沈積之後，視光起始劑及溶劑之選擇(例如溫度不應過高以使光起始劑揮發)而定，可在周圍條件下將光起始劑溶液乾燥或可藉由使用高溫及/或氣流加速乾燥。至於線內製程，應針對快速乾燥來選擇乾燥條件與溶劑。
在光起始劑溶液乾燥之後，將預處理基材曝照UV或可見光輻射源(諸如汞燈或LED)以活化光起始劑。輻射源之波長、強度及暴露時間((例如，藉由線速度確定)經選擇為有效的以用於活化所選擇的特定光起始劑。
在光起始劑活化之後，用所選擇的塗佈組合物塗佈基材。較佳地，最小化光起始劑活化與塗佈步驟之間的時間以保持活化之有效性，活化之有效性可隨著時間的消逝而降低。
適用於光起始劑預處理之塗料包括溶液、分散液或乳液。溶液可包括基於溶劑的塗料或可為100%固體(例如，100%單體或單體摻合物)。分散液可包括分散於溶劑中之微粒組份。塗層可包括黏著塗層、保護塗層(例如硬塗層或UV阻斷塗層)、光學塗層、導電塗層、脫模塗層、抗微生物塗層、印花及其類似者。
乳液塗層可包括自組裝成跡線與網格之網狀結構的塗層。塗覆至預處理基材上之乳液包括連續液相與分散液相，該分散液相與連續液相不混溶且在連續液相內形成分散域。在一些實施方案中，連續相比分散相蒸發地更快。適合乳液之一個實例為油包水乳液，其中水為分散液相且油提供連續相。乳液亦可呈水包油乳液的形式，其中油提供分散液相且水提供連續相。
連續相可包括有機溶劑。適合之有機溶劑可包括石油醚、己烷、庚烷、甲苯、苯、二氯乙烷、三氯乙烯、氯仿、二氯甲烷、硝基甲烷、二溴甲烷、環戊酮、環己酮或其任何混合物。較佳地，用於此連續相中之該溶劑或該等溶劑的特徵為與分散相(例如水相)相比更高
的揮發性。
用於分散液相之適合物質可包括水及/或可與水混溶的溶劑，諸如甲醇、乙醇、乙二醇、丙二醇、丙三醇、二甲基甲醯胺、二甲基乙醯胺、乙腈、二甲亞碸、N-甲基吡咯啶酮。
乳液亦可含有至少一種乳化劑、黏合劑或其任何混合物。適合之乳化劑可包括非離子與離子化合物(諸如市售的界面活性劑SPAN®-20(Sigma-Aldrich Co.,St.Louis,MO)、SPAN®-40、SPAN®-60、SPAN®-80(Sigma-Aldrich Co.,St.Louis,MO)、單油酸甘油酯、十二烷基硫酸鈉或其任何組合。適合黏合劑之實例包括改質纖維素(諸如乙基纖維素，其具有約100,000至約200,000之分子量)與改質尿素(例如，由BYK-Chemie GmbH(Wesel,Germany)生產之市售的BYK®-410、BYK®-411及BYK®-420樹脂)。
其他添加劑亦可存在於乳液調配物之油相及/或水相中。例如，添加劑可包括(但不限於)反應性或非反應性稀釋劑、去氧劑、硬塗層組份、抑制劑、穩定劑、著色劑、顏料、IR吸收劑、界面活性劑、濕潤劑、調平劑、流動控制劑、搖變或其他流變改質劑、助滑劑、分散助劑、消泡劑、保濕劑及腐蝕抑制劑。
乳液亦可包括金屬奈米顆粒。金屬奈米顆粒可包括選自(但不限於)銀、金、鉑、鈀、鎳、鈷、銅之群的導電金屬或金屬混合物(包括金屬合金)。較佳的金屬奈米顆粒包括銀、銀銅合金、銀鈀或其他銀合金，或由稱作冶金化學方法(MCP)的方法生產的金屬或金屬合金，該MCP描述於美國專利5,476,535及7,544,229中。
適合乳液的特定實例描述於美國專利第7,566,360號中，其以全文引用的方式併入本文中。此等乳液調配物通常包含在40%與80%之間的有機溶劑或有機溶劑混合物、0至3%的黏合劑、0至4%的乳化劑、2%至10%的金屬粉末及15%至55%的水或可與水混溶的溶劑。
塗佈組合物可藉由混合乳液之所有組份製備。可使用超音波處理、高剪切混合、高速混合或其他已知用於製備懸浮液與乳液之方法均勻化混合物。
可使用桿體展佈、浸沒、旋塗、浸漬、狹縫型擠壓式塗佈、凹板印刷式塗佈、柔性凸版印刷、噴塗或任何其他適合之技術將組合物塗佈於預處理基材上。在一些實施方案中，將均勻化的塗佈組合物塗佈於預處理基材上直至達到約1至200微米(例如5至200微米)之厚度。
在塗覆乳液至預處理基材上之後，在施加或不施加熱量的情況下蒸發乳液之液體部分。當液體自乳液移除時，奈米顆粒自組裝成跡線之網狀圖案，該等跡線界定對光透明的網格。
在一些實施方案中，網格為隨機成形的。在其他實施方案中，進行製程以創造具有規則圖案的網格。此類製程之一實例描述於2011年6月10日申請之名稱為「生產圖案化塗層之製程」之WO 2012/170684中，其受讓給與本申請案相同的受讓人且以全文引用的方式併入本文中。根據此製程，將組合物塗佈於預處理基材之表面上且將其乾燥以移除液體載劑，同時在塗佈及/或乾燥期間施加外力以使相對於連續相的分散域在預處理基材之所選區域中選擇性生長。施加外力引起非揮發性組份(奈米顆粒)自組裝且形成呈圖案形式之塗層，該圖案包括界定網格的跡線，該等網格具有由外力之組態確定的常規間距(例如，常規中心距)。外力之施加可例如藉由將組合物沈積於預處理基材表面上且隨後使邁耶(Mayer)棒通過組合物上方來實現。或者，可使用凹板圓柱塗覆組合物。在另一實施方案中，可將組合物沈積於預處理基材表面上，其後將微影遮罩置放於組合物上方。至於遮罩，隨著組合物乾燥，遮罩迫使組合物採用對應於遮罩圖案的圖案。
在各情況下，外力控制圖案(特定言之，經乾燥塗層中的網格之
間的中心距)。但是，界定網格之跡線的寬度不直接受外力控制。事實上，乳液特性與乾燥條件為跡線寬度之主要決定因素。以此方式，可容易地製造實質上比外力窄的線，而無困難且無需研發製程、母件及具有極細線寬之材料之費用。精細線寬可用乳化及乾燥製程產生。但是，外力可用(容易地及以低成本)以控制網狀結構之網格的尺寸、間距及定向。
在移除液體及形成自組裝層之後，可使用熱、雷射、紫外線、雷射或其他處理及/或暴露於化學物質(諸如金屬鹽、鹼或離子液體)中來燒結層。
透射率%(% T)：透射率%為在400-740nm之間的波長下以20nm的解析度通過樣本傳播的光的平均百分比，如藉由具有積分球的GretagMacbeth Color Eye 3000分光光度計(X-rite Corp,Grand Rapids,MI)所量測。一般而言，透射率%的值越高，最終塗層之品質越好。
將光起始劑溶解於丙酮中且使用具有6μm濕潤厚度的邁耶棒將光起始劑塗佈於PET基材上。在室溫下乾燥塗層1分鐘，且藉由通過具有F300S UV固化燈之系統來UV活化該塗層，該固化燈具有在LC6B輸送機上之H型燈泡(Fusion UV Systems Inc.,Gaithersburg,MD)。
以下列方式混合顯示於表2中的組份。使用超音波均質機混合除去離子水以外之所有組份直至均勻以形成分散液。然後，添加去離子水且使用超音波均質機將其混合以形成均勻的乳液。
使用邁耶棒在30μm濕潤厚度下將均勻的乳液塗佈於PET薄膜上。在50℃下乾燥經塗佈之薄膜，在該時間期間導電網狀結構自組裝且乾燥。
將E100 PET之薄片以25ft./min.(7.62m/min.)的速度通過UV系統。一片薄膜通過系統一次，另一片通過兩次且另一片通過三次。然後，用如上所述之乳液塗佈PET之薄片。
測試經塗佈之薄膜的透射率%，得到以下結果：
通過一次：61.0% T
通過兩次：75.2% T
通過三次：79.4% T。
用Irgacure 184於丙酮中之0.283wt%溶液塗佈E100 PET之薄片且如上所述將其UV活化。一片經塗佈之薄膜以25ft./min.(7.62m/min.)通過UV系統，且第二片以20ft./min.(6.10m/min.)通過。然後，用如上所述之乳液塗佈PET之薄片。
測試經塗佈之薄膜的透射率%，得到以下結果：
7.62m/min.：78.1% T
6.10m/min.：78.8% T。
將U46 PET之薄片以25ft./min.(7.62m/min.)的速度通過UV系統。一片薄膜通過系統一次，另一片通過兩次且另一片通過三次。然後，用如上所述之乳液塗佈PET之薄片。
測試經塗佈之薄膜的透射率%，得到以下結果：
通過一次：67.2% T
通過兩次：77.3% T
通過三次：81.6% T。
用Irgacure 184於丙酮中之0.283wt%溶液塗佈U46 PET之薄片且
如上所述將其UV活化。一片經塗佈之薄膜以25ft./min.(7.62m/min.)通過UV系統，第二片以35ft./min.(10.67m/min.)通過且第三片以45ft./min.(13.72m/min.)通過。然後，用如上所述之乳液塗佈PET之薄片。
測試經塗佈之薄膜的透射率%，得到以下結果：
7.62m/min.：80.5%T
10.67m/min.：80.0%T
13.72m/min.：80.2%T.
已描述本發明多個實施例。然而，應瞭解，在未悖離本發明精神及範圍下，可製作多種修改。因此，其他的實施例係在以下之申請專利範圍的範疇內。
Claims (14)
- 一種製備經塗佈之基材的方法，其包含：(a)將光起始劑塗覆至基材之表面上；(b)使該光起始劑曝照紫外線或紫外線可見光輻射以活化該光起始劑且形成預處理表面；(c)提供包含乳液之塗佈組合物，其中該乳液包括：(i)油相，其包含(a)不可與水混溶的有機溶劑或有機溶劑混合物及(b)金屬奈米顆粒；及(ii)水相，其包含水及/或可與水混溶的溶劑；及(d)將該塗佈組合物施加至該預處理表面上以形成經塗佈之基材，該經塗佈之基材包括界定網格之跡線之網狀結構，其中該些網格具有常規間距且對光透明。
- 如請求項1之方法，其中該光起始劑為α-羥基酮。
- 如請求項1之方法，其中塗覆該光起始劑之步驟包括提供包含溶劑及該光起始劑之組合物，其中該光起始劑係以該組合物0.1重量%至10重量%的量存在。
- 如請求項1之方法，其中塗覆該光起始劑之步驟包括提供包含溶劑及該光起始劑之組合物，其中該組合物係以濕潤塗佈厚度1至100μm塗覆。
- 如請求項4之方法，其中該濕潤塗佈厚度為1至10μm。
- 如請求項3之方法，其中該光起始劑為α-羥基酮。
- 如請求項4之方法，其中該光起始劑為α-羥基酮。
- 如請求項1之方法，其中施加該塗佈組合物之步驟包括塗佈該塗佈組合物於該預處理表面上直至達到1至200微米之厚度。
- 如請求項1之方法，其中該乳液進一步包括至少一種乳化劑、黏合劑或其任何混合物。
- 如請求項1之方法，其中該乳液包含在40%與80%之間的有機溶劑或有機溶劑混合物、2%至10%的金屬奈米顆粒及15%至55%的水及/或可與水混溶的溶劑。
- 如請求項1之方法，其中施加該塗佈組合物之步驟進一步包括施加外力以形成該經塗佈之基材，其中跡線之網狀結構定義具有由外力之組態確定的常規間距之該些網格。
- 如請求項1之方法，其中曝照之步驟進一步包括使該基材通過汞燈或LED。
- 如請求項1之方法，其中該光起始劑具有吸收波長，該輻射具有發射波長，且其中該吸收波長與該發射波長重疊。
- 如請求項1之方法，其中該經塗佈之基材具有至少78%透射率。
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| TW200632057A (en) * | 2004-12-22 | 2006-09-16 | Ciba Sc Holding Ag | Process for the production of strongly adherent coatings |
| TW201137063A (en) * | 2010-03-09 | 2011-11-01 | Cima Nanotech Israel Ltd | Process of forming transparent conductive coatings with sintering additives |
| TW201303511A (zh) * | 2011-06-10 | 2013-01-16 | Cima Nanotech Israel Ltd | 製造圖案化塗層之方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105324183A (zh) | 2016-02-10 |
| JP2016527074A (ja) | 2016-09-08 |
| TW201513943A (zh) | 2015-04-16 |
| US20160082473A1 (en) | 2016-03-24 |
| WO2014193904A1 (en) | 2014-12-04 |
| KR20160014040A (ko) | 2016-02-05 |
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