TWI572684B - 硬塗膜之製備方法 - Google Patents
硬塗膜之製備方法 Download PDFInfo
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- TWI572684B TWI572684B TW102119458A TW102119458A TWI572684B TW I572684 B TWI572684 B TW I572684B TW 102119458 A TW102119458 A TW 102119458A TW 102119458 A TW102119458 A TW 102119458A TW I572684 B TWI572684 B TW I572684B
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- acrylate
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- 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.
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Description
本發明係關於一種製造硬塗膜之方法。更特別地,本發明係關於製造具有高硬度的硬塗膜之方法。
此申請案主張2012年5月31日提出申請之韓國專利申請案第10-2012-0058634號、2012年5月31日提出申請之第10-2012-0058635號、2012年5月31日提出申請之第10-2012-0058636號、2012年5月31日提出申請之第10-2012-0058637號、及2013年5月30日提出申請之第10-2013-0062098號之權利。茲將先前申請案全數揭示以引用方式納入此申請案中作為參考資料。
近來,隨著行動裝置(如智慧型手機、平板電腦等)的發展,要求用於顯示器的基板變窄或變薄。通常使用機械性質極佳的玻璃或強化玻璃材料製造此行動裝置的顯示窗或前面板。但是,玻璃材料有著因其本身的重量而造成行動裝置沉重及會因外在衝擊而受損的缺點。
因此,研究塑膠樹脂膜作為玻璃的替代品。
塑膠樹脂膜因為質輕且不易破裂,所以適用於尋求較輕質且薄小化的行動裝置的趨勢。特別地,須要具有高硬度和耐磨蝕性的膜。關於此,提出具有經硬塗層塗覆之基板的結構。
考慮提高硬塗層之厚度的方法作為改良硬塗層之表面硬度的方法。欲確保硬塗層的表面硬度至可以硬塗層代替玻璃的程度,須調整硬塗層的厚度。但是,隨著硬塗層厚度的提高,其表面硬度變高,但硬塗層會因為其固化收縮而起皺或捲曲且易破裂或剝落。因此,不易將硬塗層用於實際應用。
最近,已提出數種提高硬塗膜之硬度及解決硬塗膜因其固化收縮而破裂或捲曲之問題的方法。
韓國專利申請公告第2010-0041992號提出不含單體的硬塗膜組成物,其使用包括紫外光可固化的聚胺甲酸酯丙烯酸酯低聚物之黏合劑樹脂。但是,此硬塗膜的鉛筆硬度約3H,不足以代替用於顯示器的玻璃面板。
據此,提出本發明以解決上述問題,本發明之目的係提出製造不易捲曲、翹曲或破裂之具有高硬度的硬塗膜之方法。
欲達到以上目的,本發明的一個方面係提出一種製造硬塗膜之方法,其包含下列步驟:將硬塗料組成物施用於承載基板的兩面上,該硬塗料組成物包括包含三-至六-官能性之以丙烯酸酯為基礎的單體之黏合劑、無機粒子和光引發劑;和以紫外光照射所施用的硬塗料組成物以同時使該硬塗料組成物光固化,藉此形成硬塗層。
如前述者,根據本發明之方法能夠以減少捲曲發生的方式,輕易地製造高硬度的硬塗膜。
藉此方法製造的硬塗膜具有關於硬度、耐刮性和透明性之極佳的性質。此外,其具有高加工性並因此而較不會捲曲和破裂。因此,此硬塗膜可以有用地施用於行動裝置、顯示裝置、儀器等的前面板或顯示面板。
根據本發明之一方面,本發明提出一種製造硬塗膜之方法,其包含下列步驟:將硬塗料組成物施用於承載基板的兩面上,該硬塗料組成物包括包含三-至六-官能性之以丙烯酸酯為基礎的單體之黏合劑、無機粒子和光引發劑;和以紫外光照射所施用的硬塗料組成物以同時使該硬塗料組成物光固化,藉此形成硬塗層。
本發明中,“第一”、“第二”等用以描述各構份,僅用於區分構份彼此之目的。
此外,本說明書中所用的詞彙僅用以說明本發明,不欲限制本發明。只要說明書中未明確地彼此區分,單數詞意包括複數詞意。本說明書中,“包括”、“包含”、“具有”等是指特徵、步驟、構份和彼等之組合,且必須瞭解並非事先排除一或多種其他特徵、步驟、構份和彼等之組合之存在或增加。
此外,本發明中,當提及各種構份形成於各構份“上”、“之上”或“上方”時,是指直接形成於各構份上,或指另一構份另外形成於層間、物件上或基板上。
由於本發明可經各種形式修飾,所以將詳細描述本發明之較佳的具體實施例。雖已提出這些具體實施例以用於說明,應瞭解本發明將不限於此,且嫻於此技術者將瞭解在不背離本發明之範圍和精神的情況下,各種修飾、增加和取代為可行者。
下文中,將詳細描述本發明之較佳的具體實施例。
根據本發明之具體實施例,在製造硬塗膜的方法中,首先,將包括包含三-至六-官能性之以丙烯酸酯為基礎的單體之黏合劑、無機粒子和光引發劑之硬塗料組成物施用於承載基板的兩面上。
本發明之方法中,只要是透明,任何塑膠樹脂,無論能夠伸縮與否,均可用作承載基板而使其兩面上均塗覆以硬塗料組成物,並無限制。根據本發明之具體實施例,此承載基板可包括聚對酞酸乙二酯(PET)、環烯
烴共聚物(COC)、聚丙烯酸酯(PAC)、聚碳酸酯(PC)、聚乙烯(PE)、聚甲基丙烯酸甲酯(PMMA)、聚醚醚酮(PEEK)、聚萘酸乙二酯(PEN)、聚醚醯亞胺(PEI)、聚醯亞胺(PI)、三乙醯基纖維素(TAC)、甲基丙烯酸甲酯(MMA)之類。此承載基板可為單層結構,和,必要時,可為由相同或相異材料所構成的多層結構,但無特別的限制。
根據本發明之具體實施例,此承載基板可為聚對酞酸乙二酯(PET)製成的多層基板或可為藉聚甲基丙烯酸甲酯(PMMA)和聚碳酸酯(PC)之共壓出所形成的基板。
此外,根據本發明之具體實施例,此承載基板可包括聚甲基丙烯酸甲酯(PMMA)和聚碳酸酯(PC)之共聚物。
此承載基板的厚度可為,但不限於,約30至約1,200微米,或約50至約800微米。
施用在承載基板的兩面上之硬塗料組成物包括包含三-至六-官能性之以丙烯酸酯為基礎的單體之黏合劑、無機粒子和光引發劑。
本說明書中,“以丙烯酸酯為基礎”意欲含括丙烯酸酯、甲基丙烯酸酯、和彼等之具有各種取代基的衍生物。
此黏合劑包括三-至六-官能性之以丙烯酸酯為基礎的單體。
三-至六-官能性之以丙烯酸酯為基礎的單體的例子可包括三羥甲基丙烷三丙烯酸酯(TMPTA)、乙氧基化三羥甲基丙烷三丙烯酸酯(TMPEOTA)、丙氧基化甘油三丙烯酸酯(GPTA)、季戊四醇四丙烯酸酯(PETA)、二季戊四醇六丙烯酸酯(DPHA)等。三-至六-官能性之以丙烯酸酯為基礎的單體可以單獨使用或彼等併用。
根據本發明之具體實施例,此黏合劑可以另包括單-至二-官能性之以丙烯酸酯為基礎的單體。
單-至二-官能性之以丙烯酸酯為基礎的單體的例子可包括丙烯酸羥乙酯(HEA)、甲基丙烯酸羥乙酯(HEMA)、己二醇二丙烯酸酯(HDDA)、三丙二醇二丙烯酸酯(TPGDA)、乙二醇二丙烯酸酯(EGDA)等。這些單-至二-官能性之以丙烯酸酯為基礎的單體亦可以單獨使用或彼等併用。
根據本發明之具體實施例,以100重量份硬塗料組成物計,黏合劑的含量為約35至約85重量份,或約45至約80重量份。硬塗料組成物中的黏合劑含量在以上範圍內時,可形成具有高硬度且因為其良好的加工性而不易捲曲或破裂的硬塗膜。
此外,在硬塗料組成物中,當黏合劑另包括單-至二-官能性之以丙烯酸酯為基礎的單體時,未特別限制單-至二-官能性之以丙烯酸酯為基礎的單體對三-至六-官能性之以丙烯酸酯為基礎的單體之含量比。根據本發明之具體實施例,所含括之單-至二-官能性之以丙烯酸酯為
基礎的單體和三-至六-官能性之以丙烯酸酯為基礎的單體之重量比可為約1:99至約50:50,約10:90至約50:50,或約20:80至約40:60。當所含括之單-至二-官能性之以丙烯酸酯為基礎的單體和三-至六-官能性之以丙烯酸酯為基礎的單體之重量比在以上範圍內時,硬塗層可具有高硬度和撓曲性且未損及其他物理性質,如捲曲性、耐光性等。
根據本發明之具體實施例,黏合劑可以另包括光可固化的彈性聚合物。
本說明書中,光可固化的彈性聚合物是指具有彈性並含有可藉UV照射而交聯聚合之官能基的聚合物材料。
根據本發明之具體實施例,光可固化的彈性聚合物根據ASTM D638測定之伸長率為約15%或更高,例如,約15至約200%,約20至約200%,或約20至約150%。
當本發明之硬塗料組成物另包括光可固化的彈性聚合物時,該光可固化的彈性聚合物與三-至六-官能性之以丙烯酸酯為基礎的單體交聯聚合及之後固化而形成硬塗層,硬塗層之撓曲性和耐衝擊性獲改良。
當黏合劑另包括光可固化的彈性聚合物時,未特別限制光可固化的彈性聚合物對三-至六-官能性之以丙烯酸酯為基礎的單體之含量比。但是,根據本發明之具體實施例,所含括之光可固化的彈性聚合物對三-至六-官
能性之以丙烯酸酯為基礎的單體之重量比可為約5:95至約20:80。當所含括的光可固化的彈性聚合物和三-至六-官能性之以丙烯酸酯為基礎的單體在以上重量比的範圍內時,硬塗層可被賦予高硬度和高撓曲性且未損及其他物理性質,如捲曲特性、耐光性等,且,特別地,可防止硬塗層因外在衝擊而受損,藉此而確保極佳的耐衝擊性。
根據本發明之具體實施例,此光可固化的彈性聚合物可為重量平均分子量為約1,000至約600,000克/莫耳,或約10,000至約600,000克/莫耳之聚合物或低聚物。
光可固化的彈性聚合物可為選自由聚己內酯、以胺甲酸酯丙烯酸酯為基礎的聚合物、和聚輪烷(polyrotaxane)所組成的群組中之至少一者。
在作為光可固化的彈性聚合物之聚合物中,聚己內酯係藉己內酯的開環聚合反應形成,並具有極佳的物理性質,如撓曲性、耐衝擊性、耐久性等。
以胺甲酸酯丙烯酸酯為基礎的聚合物保留胺甲酸酯鍵並具有極佳的彈性和耐久性。
聚輪烷係輪烷之聚合物,一種機械上互鎖的分子構造,其由穿透環狀原子團(巨環)之啞鈴形分子所組成。由於啞鈴(終止基)的末端大於環的內徑並防止構件脫離(因為此須要共價鍵的明顯扭曲),所以輪烷的兩個構件在動力上受到限制。
根據本發明之具體實施例,光可固化的彈性
聚合物可包括聚輪烷,該聚輪烷包含巨環且且其中之末端連結有(甲基)丙烯酸酯原子團的內酯化合物彼此鍵結;維持於該巨環內的穿透原子團;和位於該穿透原子團兩端以防止該巨環解離的終止基。
此情況中,可以無限制地使用環狀原子團(巨環),只要其尺寸能夠環繞穿透原子團即可。此環狀原子團(巨環)可包括官能基,如羥基、胺基、羧基、巰基、醛基之類,其可以與其他聚合物或化合物反應。環狀原子團(巨環)的特定例子可包括α-環糊精、β-環糊精、γ-環糊精和彼等之混合物。
此外,可以無限制地使用穿透原子團,只要
其為具有預定或更高重量且通常為直鏈即可。較佳地,聚伸烷基化合物或聚內酯化合物可用於穿透原子團。特定言之,包括具1至8個碳原子的氧伸烷基重複單元之聚氧伸烷基化合物或包括具3至10個碳原子的內酯重複單元之聚內酯化合物可用於此穿透原子團。
同時,取決於欲製造的輪烷化合物的特性,終止基可經適當調整。例如,終止基可為選自由二硝基苯基、環糊精基團、金剛烷基、三苯甲基、螢光黃基、和芘基所組成的群組中之至少一者。
由於聚輪烷的耐刮性極佳,所以當其受到外在損害時,其可具有自身恢復力。
本發明之方法中,硬塗料組成物包括無機粒子。
根據本發明之具體實施例,可以使用粒子尺寸約100奈米或更低,或約10至約100奈米,或約10至約50奈米的無機奈米粒子作為無機粒子。例如,氧化矽粒子、氧化鋁粒子、氧化鈦粒子或氧化鋅粒子可作為無機粒子。
硬塗料組成物中含括無機粒子進一步改良硬塗膜之硬度。
根據本發明之具體實施例,以100重量份該硬塗料組成物計,無機粒子的含量為約10至約60重量份,或約20至約50重量份。無機粒子的量在以上範圍內時,可以藉由添加無機粒子而改良硬塗膜之硬度且不損及硬塗料組成物的物理性質。
本發明之方法中,硬塗料組成物包括光引發劑。
根據本發明之具體實施例,光引發劑的例子可包括,但不限於,1-羥基-環己基-苯基酮、2-羥基-2-甲基-1-苯基-1-丙酮、2-羥基-1-[4-(2-羥基乙氧基)苯基]-2-甲基-1-丙酮、甲基苄醯基甲酸酯、α,α-二甲氧基-α-苯基乙醯苯、2-苄醯基-2-(二甲基胺基)-1-[4-(4-嗎啉基)苯基]-1-丁酮、2-甲基-1-[4-(甲巰基)苯基]-2-(4-嗎啉基)-1-丙酮、二苯基(2,4,6-三甲基苄醯基)氧化膦、雙(2,4,6-三甲基苄醯基)-苯基氧化膦等。此外,市售光引發劑的例子可包括Irgacure 184、Irgacure 500、Irgacure 651、Irgacure 369、Irgacure 907、Darocur 1173、Darocur
MBF、Irgacure 819、Darovur TPO、Irgacure 907、Esacure KIP 100F等。這些光引發劑可以單獨使用或以彼等之混合物使用。
根據本發明之具體實施例,相對於100重量份硬塗料組成物,光引發劑的含量為約0.5至約10重量份,或約1至約5重量份。光引發劑的存在量在以上範圍內時,可以充份進行交聯-光聚合反應且不會損及硬塗膜的物理性質。
同時,在製造根據本發明之硬塗膜的方法中,硬塗料組成物可以另包括一般使用的添加劑,如,界面活性劑、黃化抑制劑、均化劑、防污劑等。此處,未特別限制添加劑的含量,此因彼等的含量可在不損及硬塗料組成物的物理性質之情況作各種調整。
根據本發明之具體實施例,例如,硬塗料組成物可包括界面活性劑作為添加劑。此界面活性劑可為單-至二-官能性之以氟為基礎的丙烯酸酯、以氟為基礎的界面活性劑或以矽為基礎的界面活性劑。此外,硬塗料組成物可包括黃化抑制劑作為添加劑。黃化抑制劑可為二苯基甲酮化合物或苯並三唑化合物。
此外,根據本發明之方法中,硬塗料組成物可以無溶劑形式使用,但可以選擇性地另包括有機溶劑以在以硬塗料組成物塗覆承載基板之時,調整此組成物的黏度和流動性,及改良此組成物對承載基板的塗覆性。
有機溶劑的例子可包括:醇類,例如甲醇、
乙醇、異丙醇、丁醇等;烷氧基醇類,如2-甲氧基乙醇、2-乙氧基乙醇、1-甲氧基-2-丙醇等;酮類,例如丙酮、甲基乙基酮、甲基異丁基酮、甲基丙基酮、環己酮等;醚類,例如丙二醇單丙醚、丙二醇單甲醚、乙二醇單乙醚、乙二醇單丙醚、乙二醇單丁醚、二乙二醇單甲醚、二乙二醇單乙醚、二乙二醇單丙醚、二乙二醇單丁醚、二乙二醇-2-乙基己醚等;和芳族溶劑,例如苯、甲苯、二甲苯等。這些有機溶劑可以單獨使用或以彼等之混合物使用。
本發明之方法中,當有機溶劑另含括於硬塗料組成物中時,有機溶劑的添加量使得硬塗料組成物:有機溶劑的重量比為約70:30至約99:1。因此,當硬塗料組成物具有高固體含量時,硬塗料組成物的黏度提高,並因此而能夠進行厚塗覆,藉此形成具有50微米或更高之厚度的厚硬塗層。
根據本發明之具體實施例,未特別限制硬塗料組成物的黏度,只要其具有適當的流動性和塗覆性即可,但此硬塗料組成物可以因為具有相當高的固體含量而具有高黏度。例如,此硬塗料組成物所具有的25℃黏度為約100至約1,200cps,約150至約1,200cps,或約300至約1,200cps。
包括前述組份的硬塗料組成物施用在承載基板的兩面上。根據本發明之具體實施例,此硬塗料組成物可以先後施用在承載基板的正面和背面上,或可以同時施用在承載基板的兩面上。
此處,未特別限制施用硬塗料組成物的方法,只要其可用於相關領域即可。例如,可藉棒塗法(bar coating)、刮刀塗法、滾筒塗法、葉片塗法、模具塗法、微凹版印刷塗法(micro-gravure coating)、間隔塗法(comma coating)、縫隙模具塗法、澆嘴塗法(lip coating)、溶液澆鑄之類的方式施用硬塗料組成物。
此外,硬塗料組成物可以施用在承載基板的兩面上,使得藉由固化所施用的硬塗料組成物所形成的硬塗層具有約50至約300微米,約50至約150微米,約70至約100微米之厚度。根據製造本發明之硬塗膜之方法,當形成以上厚度的硬塗層時,可製造具有高硬度的硬塗膜且不會形成捲曲或破裂。
施用硬塗料組成物之後,可以選擇性地進行使得所施用的硬塗料組成物之表面安定化的程序。此程序可藉由使經硬塗料組成物塗覆的承載基板於預定溫度進行熱處理的方式進行。藉此,所施用的硬塗料組成物的表面變平,且硬塗料組成物中所含括的揮發性組份揮發,藉此安定化彼之表面。
之後,已施用硬塗料組成物的承載基板以紫外光照射以同時光固化在承載基板兩面上的硬塗料組成物,藉此形成硬塗層。
本說明書中,“同時光固化硬塗料組成物”是指施用在承載基板的兩面上的硬塗料組成物被光固化,使其固化速率彼此類似或相同,其意義並包括,當自施於承
載基板的一面上的硬塗料組成物開始固化至其固化終了所須的時間以100%表示時,施於承載基板的另一面上的硬塗料組成物被固化,且施於承載基板的兩面上的硬塗料組成物之間的時間差維持於20%或更低。
通常,以丙烯酸酯為基礎的黏合劑單體會引發固化收縮現象或因為固化收縮而造成承載基板與塗層一起捲起的現象。此捲曲現象係當平面膜散佈於平板上時,平面膜的邊緣等呈現曲線翹曲或捲起的現象,且當以丙烯酸酯為基礎的黏合劑單體於藉紫外光照射以光固化此以丙烯酸酯為基礎的黏合劑單體的程序中收縮時,發生此捲曲現象。
特別地,為了將硬塗膜用於行動終端機(如智慧型手機)的外殼或平板電腦的外殼,重要的是,改良硬塗膜的硬度至硬塗膜可代替玻璃的程度。此處,欲改良硬塗膜的硬度,基本上,必須將硬塗層的厚度提高至預定厚度,例如,50微米或更高,70微米或更高,或100微米或更高。但是,隨著硬塗層厚度的提高,固化收縮所造成的捲曲現象亦提高,使得硬塗層對承載基板之黏著降低,且硬塗膜易捲起。因此,可以另進行使得承載基板平坦化的方法,但此方法的問題在於硬塗層破裂。因此,難製造可代替玻璃且未損及彼之物理性質之具有高硬度的硬塗膜。
根據本發明之製造硬塗膜之方法,當施於承載基板的兩面上之硬塗料組成物以紫外光照射以使得所施
用的硬塗料組成物同時光固化時,能夠防止所施用的硬塗料組成物捲起,藉此製造具有極佳的物理和光學性質且未造成捲曲或破裂的硬塗膜。
例如,紫外光的照射率可為約20至約600毫焦耳/平方公分,或約50至約500毫焦耳/平方公分。未特別限制用於紫外光照射的光源,只要其可用於相關領域即可。例如,可以使用高壓汞燈、金屬鹵素燈、黑光燈、螢光燈之類作為紫外光照射的光源。當所施用的硬塗料組成物以紫外光以上述照射率照射約30秒至約15分鐘或約1至約10分鐘,此硬塗料組成物可被光固化。
根據本發明之具體實施例,承載基板對形成於承載基板之一面上的硬塗層之厚度比可為約1:0.5至約1:2,或約1:0.5至約1:1.5。當此厚度比在以上範圍內時,可形成不易捲曲或破裂之具有高硬度的硬塗膜。
藉本發明之方法得到的硬塗膜因為具有高硬度、耐刮性、透明性、耐久性、耐光性、透光率等,所以可用於各種領域。
例如,藉本發明之方法得到的硬塗膜在1公斤載重下的鉛筆硬度可為7H或更高,8H或更高,或9H或更高。
此外,摩擦試驗機放置鋼絨#0000且此鋼絨#0000在500克載重下在本發明的硬塗膜上往復摩擦400次時,在硬塗膜上形成的刮痕數為2或更低。
此外,藉本發明之方法得到之硬塗膜的透光
率為91.0%或更高,或92.0%或更高,且濁度為1.0%或更低,0.5%或更低,或0.4%或更低。
此外,當藉本發明之方法得到的硬塗膜曝於50℃或更高的溫度和80%或更高的濕度達70小時或更久並於之後置於平面上時,硬塗膜的各邊緣與平面分離的最大距離可為約1.0毫米或更低,約0.6毫米或更低,或約0.3毫米或更低。更特定言之,當硬塗膜曝於50至90℃的溫度和80至90%的濕度達70至100小時並於之後置於平面上時,硬塗膜的各邊緣與平面分離的最大距離可為約1.0毫米或更低,約0.6毫米或更低,或約0.3毫米或更低。
此外,藉本發明之方法得到之硬塗膜的初始b色值為1.0或更低。此外,當此硬塗膜藉由紫外燈而曝於UV-B下72小時或更久時,介於硬塗膜的初始b*色值和硬塗膜曝於UV-B之後的b*色值之間的差值可0.5或更低,或0.4或更低。
如前述者,藉本發明之方法得到的硬塗膜可用於各種領域。例如,本發明之硬塗膜可用於行動終端機、智慧型手機或平板電腦的觸控面板及顯示器或裝置的外殼。
下文中,將以參考以下實例的方式,更詳細地描述本發明。但是,這些實例用以說明本發明,本發明之範圍不受限於此。
在反應器中,50克經己內酯接枝的聚輪烷聚合物[A1000,Advanced Soft Material INC]與4.53克Karenz-AOI[異氰酸2-丙烯醯基乙酯,Showadenko Inc.]、20毫克二月桂酸二丁錫[DBTDL,Merck Corp.]、110毫克氫醌單甲醚和315克甲基乙基酮混合。之後,混合物於70℃反應5小時以得到聚輪烷,此聚輪烷中,具有連結至其末端的丙烯酸酯原子團之聚內酯作為巨環,而環糊精作為終止基。
所得聚輪烷的重量平均分子量為600,000克/莫耳,其伸長率是20%,此係根據ASTM D638測定。
2克丙烯酸羥乙酯(HEA)、8克的氧化矽-二季戊四醇六丙烯酸酯(DPHA)複合物(氧化矽3.2克,DPHA 4.8克)經40重量%之粒子尺寸20~30奈米的氧化矽奈米粒子分散、0.2克光引發劑(商標名稱:Darocur TPO)、0.1克以苯並三唑為基礎的黃化抑制劑(商標名稱:Tinuvin 400)和0.05克以氟為基礎的界面活性劑(商標名稱:FC4430)混合而製造硬塗料組成物。
此硬塗料組成物藉棒塗法施於尺寸為15公分×20公分且厚度為188微米的PET承載基板的兩面上。之
後,其兩面經硬塗料組成物塗覆的承載基板通過紫外光(UV)照射器之間,各個照射器放置發射290~320奈米之波長的金屬鹵素燈,且各者位於承載基板的上方和下方,以光固化此硬塗料組成物,藉此而在承載基板的兩面上形成硬塗層。
在承載基板的兩面上形成之硬塗層每一者的厚度為100微米。
2克丙烯酸羥乙酯(HEA)、8克的氧化矽-二季戊四醇六丙烯酸酯(DPHA)複合物(氧化矽3.2克,DPHA 4.8克)經40重量%之粒子尺寸20~30奈米的氧化矽奈米粒子分散、0.2克光引發劑(商標名稱:Darocur TPO)、0.1克以苯並三唑為基礎的黃化抑制劑(商標名稱:Tinuvin 400)和0.05克以氟為基礎的界面活性劑(商標名稱:FC4430)溶於2克甲基乙基酮(MEK)中以製造硬塗料組成物。
硬塗料組成物施用在尺寸為15公分×20公分且厚度為180微米的PC/PMMA共壓出承載基板上。之後,以與實例1相同的方式製造硬塗膜。
以與實例1相同的方式製造硬塗膜,但使用8克氧化矽-二季戊四醇六丙烯酸酯(DPHA)複合物(氧化
矽2.4克,DPHA 5.6克)(經30重量%之粒子尺寸20~30奈米的氧化矽奈米粒子分散)作為用於黏合劑的單體。
9克氧化矽-二季戊四醇六丙烯酸酯(DPHA)複合物(氧化矽3.6克,DPHA 5.4克)經粒子尺寸20~30奈米的氧化矽奈米粒子、1克製造例1的聚輪烷、0.2克光引發劑(商標名稱:Darocur TPO)、0.1克以苯並三唑為基礎的黃化抑制劑(商標名稱:Tinuvin 400)和0.05克以氟為基礎的界面活性劑(商標名稱:FC4430)混合而製造硬塗料組成物。
之後,以與實例1相同的方式製造硬塗膜。
以與實例4相同的方式製造硬塗膜,但使用1克以胺甲酸酯丙烯酸酯為基礎的聚合物(商標名稱:UA200PA,Shinnakamura Chemicals Corp.,重量平均分子量:2,600克/莫耳,ASTM D638測得的伸長率:170%)代替1克製造例1的聚輪烷。
以與實例4相同的方式製造硬塗膜,但使用1克以胺甲酸酯丙烯酸酯為基礎的聚合物(商標名稱:
UA340PA,Shinnakamura Chemicals Corp.,重量平均分子量:13,000克/莫耳,ASTM D638測得的伸長率:150%)代替1克製造例1的聚輪烷。
實例1至6的硬塗料組成物之組成和含量彙整於表1。
根據Japanese Standard JIS K5400評估鉛筆
硬度。此處,鉛筆硬度計在1.0公斤載重下,在各硬塗膜上往復三次,以測定未觀察到刮痕時的硬度。
載至摩擦試驗機之後,鋼絨(#0000)在0.5公斤載重下,在各硬塗膜上往復400次,計算藉此形成的刮痕數。藉下列標記評估膜的耐刮性:○代表刮痕數為2或更少,△代表刮痕數為2至低於5,而×代表刮痕數為5或更多。
硬塗膜在曝於來自UV燈的UVB 72小時之前和之後的b*色值之差異。
使用光譜儀(品牌名稱:COH-400)測定硬塗膜的透光率和濁度。
各硬塗膜切成尺寸為10公分×10公分時,在溫度85℃和濕度85%的室中儲存72小時及之後置於平面上,測定硬塗膜的各邊緣與平面分離的最大距離。
各硬塗膜纏繞在直徑3公分的圓柱形心軸上,之後測定各硬塗膜是否破裂。若各硬塗膜未破裂,則評估為OK,若其破裂則評估為X。
藉由測定22克鋼球自高度40公分處落在各硬塗膜上時,各硬塗膜是否破裂而評估各個硬塗膜的耐衝擊性。硬塗膜未破裂,則評估為OK,若其破裂則評估為X。
硬塗膜之物理性質的測定結果彙整於以下的表2。
如以上的表2所示者,能夠確定藉實例1至6之方法得到的硬塗膜皆具有良好的物理性質。
Claims (20)
- 一種製造硬塗膜之方法,其包含下列步驟:將硬塗料組成物施用於承載基板的兩面上,該硬塗料組成物包括包含三-至六-官能性之以丙烯酸酯為基礎的單體之黏合劑、無機粒子和光引發劑;和以紫外光照射所施用的硬塗料組成物以同時使該硬塗料組成物光固化,藉此形成硬塗層,其中該硬塗膜具有在1公斤載重下的鉛筆硬度為7H或更高。
- 如申請專利範圍第1項之方法,其中該三-至六-官能性之以丙烯酸酯為基礎的單體包括選自由三羥甲基丙烷三丙烯酸酯(TMPTA)、乙氧基化三羥甲基丙烷三丙烯酸酯(TMPEOTA)、丙氧基化甘油三丙烯酸酯(GPTA)、季戊四醇四丙烯酸酯(PETA)、和二季戊四醇六丙烯酸酯(DPHA)所組成的群組中之至少一者。
- 如申請專利範圍第1項之方法,其中該黏合劑另包括單-至二-官能性之以丙烯酸酯為基礎的單體。
- 如申請專利範圍第3項之方法,其中該單-至二-官能性之以丙烯酸酯為基礎的單體包括選自由丙烯酸羥乙酯(HEA)、甲基丙烯酸羥乙酯(HEMA)、己二醇二丙烯酸酯(HDDA)、三丙二醇二丙烯酸酯(TPGDA)、和乙二醇二丙烯酸酯(EGDA)所組成的群組中之至少一者。
- 如申請專利範圍第1項之方法,其中該黏合劑另包括光可固化的彈性聚合物。
- 如申請專利範圍第5項之方法,其中該光可固化的彈性聚合物根據ASTM D638測定的伸長率為15至200%。
- 如申請專利範圍第5項之方法,其中該光可固化的彈性聚合物包括選自由聚己內酯、以胺甲酸酯丙烯酸酯為基礎的聚合物、和聚輪烷(polyrotaxane)所組成的群組中之至少一者。
- 如申請專利範圍第7項之方法,其中該聚輪烷包括:巨環且其中之末端連結有(甲基)丙烯酸酯原子團的內酯化合物彼此鍵結;維持於該巨環內的穿透原子團;和位於該穿透原子團兩端以防止該巨環解離的終止基(stopper)。
- 如申請專利範圍第1項之方法,其中該承載基板包括選自由聚對酞酸乙二酯(PET)、環烯烴共聚物(COC)、聚丙烯酸酯(PAC)、聚碳酸酯(PC)、聚乙烯(PE)、聚甲基丙烯酸甲酯(PMMA)、聚醚醚酮(PEEK)、聚萘酸乙二酯(PEN)、聚醚醯亞胺(PEI)、聚醯亞胺(PI)、三乙醯基纖維素(TAC)、和甲基丙烯酸甲酯(MMA)所組成的群組中之至少一者。
- 如申請專利範圍第1項之方法,其中該硬塗料組成物藉棒塗法(bar coating)、刮刀塗法、滾筒塗法、葉片塗法、模具塗法、微凹版印刷塗法(micro-gravure coating)、間隔塗法(comma coating)、縫隙模具塗法、澆嘴塗法(lip coating)或溶液澆注方式施用。
- 如申請專利範圍第1項之方法,其中該硬塗料組成物同時施於該承載基板的兩面上。
- 如申請專利範圍第1項之方法,其中該無機粒子的粒子尺寸為100奈米或更低。
- 如申請專利範圍第1項之方法,其中該無機粒子包括選自由氧化矽奈米粒子、氧化鋁奈米粒子、氧化鈦奈米粒子和氧化鋅奈米粒子所組成的群組中之至少一者。
- 如申請專利範圍第1項之方法,其中該硬塗料組成物以100重量份該硬塗料組成物計包括35至85重量份的黏合劑、10至60重量份的無機粒子和0.5至10重量份的光引發劑。
- 如申請專利範圍第1項之方法,其中該硬塗料組成物另包括添加劑。
- 如申請專利範圍第15項之方法,其中該添加劑包括選自由單-至二-官能性之以氟為基礎的丙烯酸酯、以氟為基礎的界面活性劑、和以矽為基礎的界面活性劑所組成的群組中之至少一者。
- 如申請專利範圍第15項之方法,其中該添加劑包括含有二苯基甲酮化合物或苯並三唑化合物之黃化抑制劑。
- 如申請專利範圍第1項之方法,其中該硬塗料組成物另包括有機溶劑。
- 如申請專利範圍第1項之方法,其中該硬塗層具有50至300微米之厚度。
- 如申請專利範圍第1項之方法,其中該承載基板對該硬塗層的厚度比為1:0.5至1:2。
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