TWI671345B - 樹脂組成物及其可靠性評估的方法以及包含此組成物的色彩轉換膜 - Google Patents
樹脂組成物及其可靠性評估的方法以及包含此組成物的色彩轉換膜 Download PDFInfo
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- TWI671345B TWI671345B TW107117250A TW107117250A TWI671345B TW I671345 B TWI671345 B TW I671345B TW 107117250 A TW107117250 A TW 107117250A TW 107117250 A TW107117250 A TW 107117250A TW I671345 B TWI671345 B TW I671345B
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0041—Optical brightening agents, organic pigments
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0025—Crosslinking or vulcanising agents; including accelerators
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/01—Hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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Abstract
本申請案提供一種樹脂組成物、一種其可靠性評估的方
法及一種包含此組成物的色彩轉換膜,所述樹脂組成物藉由所述樹脂組成物的二級結構轉變濃度及弛豫時間有效地抑制光漂白現象且達成優異的外部阻擋性質及光學性質。
Description
[相關申請案的交叉參考]
本申請案主張於2017年5月19日提出申請的韓國專利申請案第10-2017-0062427號的優先權,所述韓國專利申請案的揭露內容全文併入本案供參考。
本發明是有關於一種樹脂組成物、一種其可靠性評估的方法及一種包含此組成物的色彩轉換膜。
電視(TV)正變得具有高影像品質、更纖薄且更複雜並且面積擴大。高效能及高影像品質有機發光二極體(organic light-emitting diode,OLED)電視仍存在價格競爭力的問題,且因此市場尚未真正開放。因此,繼續努力以類似地確保OLED及液晶顯示器(liquid crystal display,LCD)的優點。
傳統的LCD設置有含有用於著色的染料的色彩轉換膜,其中諸多無機螢光物質已被用作染料,但由於無機螢光物質
具有窄色域(color gamut),因此存在色彩轉換率降低的問題,且最近已經嘗試研究使用有機螢光物質代替無機螢光物質來改善此問題。
然而,大部分有機螢光物質易於被外部因素(例如水分)氧化而造成光漂白(photobleaching)現象,且因此存在色彩轉換膜的光學特性劣化的問題。
本申請案提供一種能夠達成優異的光學特性的樹脂組成物、一種其可靠性評估的方法及一種含有此組成物的色彩轉換膜。
本申請案是有關於一種樹脂組成物的可靠性評估的方法。所述可靠性評估的方法可例如為應用於例如LCD等顯示裝置的發光的樹脂組成物的可靠性評估的方法。此外,舉例而言,所述組成物的經固化產物可應用於顯示裝置的背光單元。
一種示例性可靠性評估的方法是包含聚合物樹脂及有機螢光物質的樹脂組成物的可靠性評估的方法。所述樹脂組成物可滿足以下方程式1,或者可根據方程式2具有20毫秒(ms)或大於20毫秒的弛豫時間(relaxation time,λ):
[方程式2]
在以上方程式1中,當在25℃的溫度及10s-1的剪切速率下根據所述樹脂組成物的濃度量測所述樹脂組成物的相對黏度且量測值示於相對黏度根據濃度變化的曲線圖中時,CE表示在曲線梯度的拐點處的濃度。
在以上方程式2中,在其中使用延伸黏度計卡百利(CaBER)在25℃的溫度下將所述樹脂組成物密封於同軸且垂直設置的一對圓形板之間且上部板在50毫秒的時間內在垂直方向上升高了40毫米(mm)並保持不變的狀態下,D1表示由所述樹脂組成物形成的細絲的初始直徑,D(t)表示所述細絲在斷裂時間(breakup time,t)處的直徑,且k表示比例常數。比例常數k可為例如-10與10之間的數。
根據以上方程式1的方法所量測的曲線梯度的拐點可為一或多個,但本文中的用語「拐點(inflection point)」意指當樹脂組成物的濃度為5重量%(wt%)或大於5重量%時曲線梯度第一次變化的點。
在以上方程式1中,樹脂組成物的濃度增大的實際情況意指樹脂組成物中的固體含量增加。另外,用語「相對黏度」意指相較於對照組量測的相對黏度,其中對照組可為黏度為例如0.8厘泊(cP)的溶劑。在一個實例中,黏度為0.8厘泊的溶劑可具有1的相對黏度。此外,用於量測黏度的設備無特別限制,但例如可
使用已知的流變計來量測。
在本申請案中,用語「曲線的拐點處的濃度」可以與樹脂組成物的二級結構轉變濃度(CE)相同的含義來使用。
圖1為示出根據方程式1的在本申請案的實例及比較例中製備的樹脂組成物的二級結構轉變濃度的曲線圖。
圖2為示意性地示出一種使用延伸黏度計CaBER量測細絲直徑的方法的圖。
參照圖1,二級結構轉變濃度(CE)意指樹脂組成物在A區的拐點處的濃度。
參照圖2中的B部分,以上方程式2中的D1表示在延伸黏度計的上部板在50毫秒的時間內在垂直方向上升高了40毫米並保持不變的狀態下由樹脂組成物形成的細絲的初始直徑。參照圖2中的C部分,由樹脂組成物形成的細絲的直徑隨著時間過去而逐漸減小並斷裂,其中D(t)表示在細絲即將斷裂前的直徑。
此處,用語「初始直徑」意指緊接延伸黏度計的上部板在50毫秒的時間內在垂直方向上升高了40毫米之後的由樹脂組成物形成的細絲的直徑。用語「直徑」意指在上部板與下部板之間的實質上中點處量測的直徑,且「實質上中點」意指包括在上部板與下部板之間的中點處±5毫米的誤差範圍的點。
「斷裂時間(breakup time,t)」意指自緊接延伸黏度計的上部板在垂直方向上升高了40毫米之後至細絲的直徑隨著時間過去逐漸減小至即將完全斷裂之前所花費的時間。用於量測細絲
的直徑的設備可為各種各樣的,且舉例而言,細絲直徑的變化可使用雷射測微計(laser micrometer)即時量測。
此外,在本說明書中,用語「弛豫時間(relaxation time,λ)」意指樹脂組成物自斷裂時間返回至平衡狀態所花費的時間。具體而言,當上部板在垂直方向上升高時,樹脂組成物中的聚合物鏈已被展開並斷裂,然後隨著時間逐漸鬆弛以返回至原始聚合物鏈的形式,其中弛豫時間意指展開的聚合物鏈返回至原始形式所花費的時間。
在一個實例中,可藉由比較二或更多種樹脂組成物的固體含量及弛豫時間來執行可靠性評估的方法。
在示例性可靠性評估準則中,可評估得到,當在以上方程式1中的樹脂組成物的二級結構轉變濃度(CE)更低或根據方程式2的弛豫時間(λ)變得更長時,因此樹脂組成物具有更高的可靠性。此外,當生產此種樹脂組成物作為色彩轉換膜時,可評估得到色彩轉換膜具有優異的耐光性。
在一個實施例中,由以上方程式1表示的固體含量可為30重量%或小於30重量%、25重量%或小於25重量%、24重量%或小於24重量%、23重量%或小於23重量%、22重量%或小於22重量%或者21重量%或小於21重量%。固體含量的下限無特別限制,其可為例如0.001重量%或大於0.001重量%、0.01重量%或大於0.01重量%、0.1重量%或大於0.1重量%或者1.0重量%或大於1.0重量%。在本申請案中,用語「固體含量」被解釋為相同
於樹脂組成物的濃度。另外,由以上方程式2表示的弛豫時間可為20毫秒或大於20毫秒、23毫秒或大於23毫秒、25毫秒或大於25毫秒或者26毫秒或大於26毫秒。弛豫時間的上限無特別限制,其可為例如1000毫秒或小於1000毫秒、500毫秒或小於500毫秒或者100毫秒或小於100毫秒。
本申請案的樹脂組成物具有以下優點:藉由將根據以上方程式1或方程式2的各參數控制成處於特定範圍內,聚合物樹脂中的有機螢光物質在生產膜時被均勻地分散,藉此特定區之間的效能的變化為小,且聚合物樹脂亦具有優異的保護有機螢光物質免受水分及氧影響的能力,藉此可防止有機螢光物質降低光學特性的問題。具體而言,當將樹脂組成物被生產成膜時,有機螢光物質與水分及氧發生反應而造成光漂白(photobleaching)現象的問題可被最小化,藉此確保膜的優異的耐光性。
構成樹脂組成物的材料無特別限制,只要滿足上述物理性質即可。示例性樹脂組成物可包含聚合物樹脂及有機螢光物質。為了在以上範圍內對由以上方程式1表示的樹脂組成物的二級結構轉變濃度(CE)或者由以上方程式2表示的弛豫時間(λ)進行調整,可對聚合物樹脂及其溶劑進行合適地選擇,藉此可在生產膜時提供在高溫及高濕度下具有優異的耐性可靠性且能夠在達成優異的防潮效能的同時易於達成期望的光學特性的色彩轉換膜。
在一個實例中,本申請案的聚合物樹脂可為熱塑性樹脂
或熱固性樹脂。用語「熱固性樹脂」意指可藉由適當的熱量施加或老化(aging)製程被固化的樹脂。
在本申請案中,熱塑性樹脂的具體種類無特別限制。在一個實例中,作為熱塑性樹脂,舉例而言,可使用聚(甲基)丙烯酸系列,例如聚甲基丙烯酸甲酯(polymethylmethacrylate,PMMA);聚碳酸酯系列(polycarbonate,PC)、聚苯乙烯系列(polystyrene,PS)、聚伸芳基系列(polyarylene,PAR)、聚胺基甲酸酯系列(熱塑性聚胺基甲酸酯(thermoplastic polyurethane,TPU)、苯乙烯-丙烯腈系列(styrene-acrylonitrile,SAN)、聚偏二氟乙烯系列(polyvinylidene fluoride,PVDF)、聚乙烯醇系列(polyvinyl alcohol,PVA)、改質的聚偏二氟乙烯系列(modified-PVDF)等。可包括該些樹脂中的一者或者二或更多者。
在一個實例中,慮及與以下所述種類的溶劑的優異的相互作用(interaction),熱塑性樹脂可為聚(甲基)丙烯酸聚合物。構成聚(甲基)丙烯酸聚合物的(甲基)丙烯酸酯單體的實例如下。在本說明書中,用語「(甲基)丙烯酸」可意指丙烯酸或甲基丙烯酸。(甲基)丙烯酸酯單體可藉由(甲基)丙烯酸烷基酯來舉例說明,且例如可藉由具有含有1至20個碳原子的烷基的(甲基)丙烯酸烷基酯來舉例說明,例如(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸異丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸第三丁酯、(甲基)丙烯酸第二丁酯、(甲基)丙烯酸戊基酯、(甲基)丙烯酸己基酯、(甲基)丙烯酸2-乙基己基酯、(甲基)丙烯酸
2-乙基丁酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸異辛酯、(甲基)丙烯酸異壬酯、(甲基)丙烯酸月桂酯或(甲基)丙烯酸十四烷基酯等。(甲基)丙烯酸烷基酯可在烷基中具有1至20個、1至15個、1至10個、1至8個、1至5個或1至3個碳原子,但並非僅限於此。
另外,本申請案的聚(甲基)丙烯酸聚合物除(甲基)丙烯酸烷基酯以外,亦可包括包含(甲基)丙烯酸作為單體的聚合物。在一個實例中,本申請案的聚合物樹脂可為含有(甲基)丙烯酸烷基酯作為聚合單元的聚合物與含有(甲基)丙烯酸作為聚合單元的聚合物的混合物。在此混合物的情形中,以含有(甲基)丙烯酸烷基酯作為聚合單元的聚合物的100重量份計,可包含50重量份至150重量份、60重量份至140重量份、70重量份至130重量份、75重量份至125重量份、83重量份至118重量份或88重量份至110重量份的量的含有(甲基)丙烯酸作為聚合單元的聚合物。
在本申請案的實施例中,熱塑性樹脂可具有介於約100,000至2,000,000、150,000至1,500,000或300,000至1,000,000範圍內的重量平均分子量。熱固性樹脂可具有介於約100,000至2,000,000、150,000至1,500,000或300,000至1,000,000範圍內的重量平均分子量。本文中的用語「重量平均分子量」意指藉由凝膠滲透層析法(gel permeation chromatograph,GPC)量測的轉換為標準聚苯乙烯的值。
在一個實例中,熱固性樹脂無特別限制,只要其滿足以
上所提及的方程式1或方程式2所示的特徵範圍即可。在一個實例中,熱固性樹脂可包含至少一個熱固性官能基。舉例而言,熱固性樹脂可包含例如環氧基、縮水甘油基、異氰酸酯基、羥基、羧基或醯胺基等至少一個熱可固化官能基作為可經過固化而表現出黏附性質者。此種樹脂的具體種類可包括丙烯酸樹脂、聚酯樹脂、異氰酸酯樹脂、酯樹脂、醯亞胺樹脂或環氧樹脂等,但並非僅限於此。
在本申請案的實施例中,樹脂組成物可更包含固化劑。舉例而言,樹脂組成物可更包含能夠與熱固性樹脂發生反應以形成交聯結構等的熱固化劑。
在一個實例中,可依據樹脂中所含有的官能基的類型來選擇及使用適當類型的固化劑。在一個實例中,熱固化劑可包括胺固化劑、咪唑固化劑、酚固化劑、磷固化劑、三嗪固化劑、硫醇系固化劑、異氰脲酸系固化劑或酸酐固化劑。
在本申請案中,有機螢光物質無特別限制,只要有機螢光物質是能夠含有螢光組分以藉由利用光進行刺激來發光且具有耐光性的有機材料即可,其可包括例如聚芳香烴,例如萘、蒽、稠四苯、稠五苯、苝、滌綸(terylene)、誇特銳烯(quaterylene)、菲及芘,其可經例如羥基、胺基、羧基或鹵素元素取代;雜環化合物衍生物,例如吡啶、喹啉、吖啶、吲哚、色胺酸、咔唑、二苯並呋喃、二苯並噻吩、呫噸、若丹明(rhodamine)、焦寧(pyronine)、螢光素(fluorescein)、曙紅(eosin)及香豆素等。
在一個實例中,有機螢光物質可為艾樂科(Alexa)350、Alexa 430、AMCA、氟硼螢(BODIPY)630/650、BODIPY 650/665、BODIPY-FL、BODIPY-R6G、BODIPY-TMR、BODIPY-TRX、喀斯喀特藍(Cascade Blue)、Cy3、Cy5、6-FAM、螢光素異硫氰酸酯、HEX、6-JOE、俄勒岡綠(Oregon Green)488、俄勒岡綠500、俄勒岡綠514、太平洋藍(Pacific Blue)、REG、若丹明綠(Rhodamine Green)、若丹明紅(Rhodamine Red)、瑞諾格蘭菲(Renographin)、ROX、TAMRA、TET、四甲基若丹明或德克薩斯紅(Texas Red)。
在一個實施例中,以聚合物樹脂的100重量份計,可包含0.1重量份至10重量份、0.5重量份至5重量份、1重量份至4重量份或1.5重量份至3重量份的量的有機螢光物質。
本申請案中的樹脂組成物可更包含溶劑。溶劑可為依據上述聚合物樹脂的種類而表現出優異的相互作用(interaction)的溶劑,其可藉由方程式1或方程式2來選擇。舉例而言,溶劑可為選自由以下組成的群組中的一者或者二或更多者:甲苯、二甲苯、丙酮、氯仿、各種醇系溶劑、甲基乙基酮(methyl ethyl ketone,MEK)、甲基異丁基酮(methyl isobutyl ketone,MIBK)、乙酸乙酯(ethyl acetate,EA)、乙酸丁酯、二甲基甲醯胺(dimethylformamide,DMF)、二甲基乙醯胺(dimethylacetamide,DMAc)、二甲基亞碸(dimethylsulfoxide,DMSO)、N-甲基-吡咯啶酮(N-methyl-pyrrolidone,NMP)、環己酮、丙二醇甲基乙基乙酸酯(propylene glycol methylethyl acetate,PGMEA)及二噁烷
(dioxane),且本申請案的樹脂組成物可依據聚合物樹脂的種類而選擇並包含滿足方程式1或方程式2的溶劑。
以聚合物樹脂的100重量份計,可包含100重量份至500重量份、150重量份至450重量份、200重量份至400重量份或250重量份至350重量份的量的溶劑,但並非僅限於此。
在一個實例中,本申請案的樹脂組成物包含聚合物樹脂、有機螢光物質及溶劑,但重要的是慮及所述三種組分之間的相互作用來選擇各組分,且因此,可藉由根據上述方程式1或方程式2的參數是否滿足特定範圍來確定所述三種組分中在固化之後的可靠性,例如混合特性、分散性及耐光性。
舉例而言,當聚合物樹脂中的聚合物組分之間的相互作用較聚合物樹脂與溶劑之間的相互作用強時,即使樹脂組成物與溶劑混合,聚合物組分亦可趨於凝聚。在另一實例中,即使組成物中的聚合物樹脂的含量過高,聚合物組分亦可趨於凝聚。此種趨勢可藉由在以下將闡述的色彩轉換膜中形成裂縫且有機螢光物質與被引入裂縫中的氧或水分發生反應而造成光漂白(photobleaching)現象。亦即,在樹脂組成物及包含此組成物的色彩轉換膜中,當聚合物樹脂與溶劑之間的相互作用弱時,方程式1的二級結構轉變濃度或方程式2的弛豫時間不滿足以上所提及的特定範圍。
另一方面,當聚合物樹脂與溶劑之間的相互作用強時,即使聚合物樹脂在所述組成物中以高含量進行配製,分散性亦為
優異的,且當將其生產成以下所述的色彩轉換膜時,可因優異的阻擋性質而防止光學特性因有機螢光物質而被降低的問題。
本申請案亦是有關於一種樹脂組成物。樹脂組成物可為根據上述可靠性評估的方法而被評估為分散性及耐光性優異的樹脂組成物。
示例性樹脂組成物包含聚合物樹脂及有機螢光物質,其可滿足以下方程式1,或者可根據方程式2具有20毫秒或大於20毫秒的弛豫時間(relaxation time,λ)。
在以上方程式1中,當在25℃的溫度及10s-1的剪切速率下根據所述樹脂組成物的濃度量測所述樹脂組成物的相對黏度且量測值示於相對黏度根據濃度變化的曲線圖中時,CE表示在曲線梯度的拐點處的濃度。
在以上方程式2中,在其中使用延伸黏度計CaBER在25℃的溫度下將所述樹脂組成物密封於同軸且垂直設置的一對圓形板之間且上部板在50毫秒的時間內在垂直方向上升高了40毫米並保持不變的狀態下,D1表示由所述樹脂組成物形成的細絲的初始直徑,D(t)表示所述細絲在斷裂時間(breaking time,t)處的
直徑,且k表示比例常數。比例常數k可為例如-10與10之間的數。
本申請案亦是有關於一種色彩轉換膜。示例性色彩轉換膜可具有包含上述樹脂組成物的色彩轉換層。色彩轉換膜包含二級結構轉變濃度或弛豫時間處於上述特定範圍內的樹脂組成物,藉此可達成色彩轉換層的優異的外部阻擋性質以防止有機螢光物質的效能退化。具體而言,構成色彩轉換層的聚合物樹脂藉由形成顯示出低透氧性及低透濕性的結構而具有優異的保護有機螢光物質免受水分及氧影響的能力,藉此可防止因有機螢光物質與水分或氧發生反應而造成光漂白(photobleaching)現象的問題。
本申請案的色彩轉換膜可更包括位於所述色彩轉換層的至少一側上的保護膜或障壁膜。作為保護膜及障壁膜,可使用此項技術中已知的保護膜及障壁膜,且舉例而言,可使用聚對苯二甲酸乙二醇酯(polyethylene terephthalate,PET)膜。
本申請案亦是有關於一種包括以上所提及的色彩轉換膜的背光單元。背光單元除包括色彩轉換膜以外,可具有此項技術中已知的背光單元構型。
示例性背光單元包括側鏈型光源、環繞光源的反射板、對自光源直接發出或自反射板反射的光進行引導的導光板、設置於導光板的一側上的反射層以及設置於與面對導光板的反射層的側相對的一側上的色彩轉換膜。另外,光源亦可用作直接型以及側鏈型,且反射板或反射層亦可根據需要被省略或替換為另一結
構,且若需要,則可進一步提供額外的膜,例如光擴散膜、聚光膜或亮度增強膜。
本申請案提供一種樹脂組成物、一種其可靠性評估的方法及一種包含此組成物的色彩轉換膜,所述樹脂組成物藉由所述樹脂組成物的二級結構轉變濃度及弛豫時間有效地抑制光漂白現象且達成優異的外部阻擋性質及光學性質。
A‧‧‧區
B、C‧‧‧部分
圖1為示出根據方程式1的在本申請案的實例及比較例中製備的樹脂組成物的二級結構轉變濃度的曲線圖。
圖2為示意性地示出一種使用延伸黏度計CaBER量測細絲直徑的方法的圖。
以下,將藉由根據本發明的實例及不是根據本發明的比較例更詳細地闡述本發明,但本發明的範圍不受以下實例限制。
實例1
(1)樹脂組成物的製備
向可密封的500毫升反應容器中,引入了74.5重量份二甲基甲醯胺(DMF,西格瑪奧德里奇公司(Sigma Aldrich))、0.5重量份BODIPY-FL(賽默飛世爾公司(Thermo Fisher))及25重量份聚甲基丙烯酸甲酯與聚甲基丙烯酸以5:5的重量比進行混合的混合物,並在室溫下攪拌了約1小時以製備均勻的樹脂組成物。
(2)色彩轉換膜的生產
將以上所製備的樹脂組成物施加至脫模PET的脫模表面並在130℃的烘箱中乾燥(5個標準大氣壓(atm))了3分鐘,以生產包括厚度為50微米的色彩轉換層的色彩轉換膜。對於以紫外射線在2焦/平方公分(J/cm2)(基於A區的100毫瓦/平方公分(mW/cm2))下在氮氣氣氛下對所生產的膜進行了照射的樣本,量測了物理性質。
(3)二級結構轉變濃度(CE)的量測
依據在實例中製備的樹脂組成物的濃度(固體含量),量測了樹脂組成物的相對黏度。當繪製隨著濃度而變化的所量測的相對黏度後,量測了在曲線梯度的拐點處的固體含量。使用黏彈性計(動態混合流變計(dynamic hybrid rheometer),DHR,TA儀器公司(TA Instruments))在10s-1的剪切速率條件下在25℃下量測了黏度,且藉由將所量測的黏度與黏度為0.8厘泊(cP)的對照樣本進行比較而計算出相對黏度,且結果示於圖1中。參照圖1,溶劑A表示在實例1中用作溶劑的二甲基甲醯胺(DMF)。
實例2
(1)樹脂組成物的製備
向可密封的500毫升反應容器中,引入了74.5重量份二甲基甲醯胺(DMF,西格瑪奧德里奇公司(Sigma Aldrich))、0.5重量份BODIPY-FL(賽默飛世爾公司(Thermo Fisher))及25重量份聚甲基丙烯酸甲酯與聚甲基丙烯酸以5:5的重量比進行混合
的混合物,並在室溫下攪拌了約1小時以製備均勻的樹脂組成物。
(2)色彩轉換膜的生產
將以上所製備的樹脂組成物施加至脫模PET的脫模表面並在130℃的烘箱中乾燥(5個標準大氣壓)了3分鐘,以生產包括厚度為50微米的色彩轉換層的色彩轉換膜。對於以紫外射線在2焦/平方公分(基於A區的100毫瓦/平方公分)下在氮氣氣氛下對所生產的膜進行了照射的樣本,量測了物理性質。
(3)弛豫時間(relaxation time,λ)量測
如圖2所示,對於在實例2中製備的樹脂組成物溶液,使用延伸黏度計CaBER量測了弛豫時間。在25℃的溫度下將樹脂組成物密封於同軸且垂直設置的一對圓形板之間。在其中上部板在50毫秒的時間內在垂直方向上升高了40毫米並保持不變的狀態下,使用雷射測微計(laser micrometer)即時量測了由樹脂組成物形成的細絲的直徑。當結果示出為直徑隨著時間變化的曲線圖時,量測了斷裂時間處的梯度,且根據上述方程式2量測了弛豫時間(relaxation time,λ)。使用矩陣實驗室(MATLAB)程式計算出弛豫時間。
比較例1
除了使用丙二醇甲基乙基乙酸酯(PGME)替代了二甲基甲醯胺(DMF)以外,以與實例1相同的方式生產了樹脂組成物及色彩轉換膜。
對於樹脂組成物,如在實例1中一樣量測了二級結構轉
變濃度(CE),且結果示於圖1中。參照圖1,溶劑B表示在比較例1中用作溶劑的丙二醇甲基乙基乙酸酯(PGME)。
比較例2
除了使用四氫呋喃(THF)替代了二甲基甲醯胺(DMF)以外,以與實例1相同的方式生產了樹脂組成物及色彩轉換膜。
對於樹脂組成物,如在實例1中一樣量測了二級結構轉變濃度(CE)。
比較例3
除了使用丙二醇甲基乙基乙酸酯(PGME)替代了二甲基甲醯胺(DMF)以外,以與實例1相同的方式生產了樹脂組成物及色彩轉換膜。
對於樹脂組成物,如在實例2中一樣量測了弛豫時間(relaxation time,λ)。
比較例4
除了使用四氫呋喃(THF)替代了二甲基甲醯胺(DMF)以外,以與實例1相同的方式生產了樹脂組成物及色彩轉換膜。
對於樹脂組成物,如在實例2中一樣量測了弛豫時間(relaxation time,λ)。
量測結果歸納並闡述於下表1及表2中。
[表2]
在以上實例及比較例中,當聚合物樹脂為聚甲基丙烯酸甲酯及聚甲基丙烯酸時,對當溶劑類型變化時是否滿足方程式1或方程式2進行了評估,藉此可選擇適合於特定聚合物樹脂的溶劑。
關於在實例及比較例中生產的色彩轉換膜的耐光性評估,當樹脂組成物的二級結構轉變濃度(CE)更低且弛豫時間更長時,顯示出優異的耐光性。
Claims (9)
- 一種包含聚合物樹脂及有機螢光物質的樹脂組成物的可靠性評估的方法,其中所述樹脂組成物滿足以下方程式1,或者根據以下方程式2具有20毫秒或大於20毫秒的弛豫時間(λ): 在以上方程式1中,當在25℃的溫度及10s-1的剪切速率下根據所述樹脂組成物的濃度量測所述樹脂組成物的相對黏度且量測值示於所述相對黏度根據所述濃度變化的曲線圖中時,CE表示在所述曲線圖梯度的拐點處的濃度,其中所述相對黏度是相較於黏度為0.8厘泊的溶劑來量測,且所述黏度為0.8厘泊的溶劑的所述相對黏度為1,且在以上方程式2中,在其中使用延伸黏度計卡百利在25℃的溫度下將所述樹脂組成物密封於同軸且垂直設置的一對圓形板之間且上部板在50毫秒的時間內在垂直方向上升高了40毫米並保持不變的狀態下,D1表示由所述樹脂組成物形成的細絲的初始直徑,D(t)表示所述細絲在斷裂時間(t)處的直徑,且k表示比例常數。
- 如申請專利範圍第1項所述的可靠性評估的方法,其中所述聚合物樹脂是熱固性樹脂或熱塑性樹脂。
- 如申請專利範圍第1項所述的可靠性評估的方法,其中所述有機螢光物質包含聚芳香烴或雜環化合物衍生物。
- 如申請專利範圍第1項所述的可靠性評估的方法,其中以所述聚合物樹脂的100重量份計,含有0.1重量份至10重量份的量的所述有機螢光物質。
- 如申請專利範圍第1項所述的可靠性評估的方法,其中所述樹脂組成物更包含溶劑。
- 如申請專利範圍第5項所述的可靠性評估的方法,其中所述溶劑包括選自由以下組成的群組中的一者或者二或更多者:甲苯、二甲苯、丙酮、氯仿、各種醇系溶劑、甲基乙基酮(MEK)、甲基異丁基酮(MIBK)、乙酸乙酯(EA)、乙酸丁酯、二甲基甲醯胺(DMF)、二甲基乙醯胺(DMAc)、二甲基亞碸(DMSO)、N-甲基-吡咯啶酮(NMP)、環己酮、丙二醇甲基乙基乙酸酯(PGMEA)及二噁烷。
- 一種樹脂組成物,包含聚合物樹脂及有機螢光物質,且滿足以下方程式1,或者根據以下方程式2具有20毫秒或大於20毫秒的弛豫時間(λ):[方程式2]在以上方程式1中,當在25℃的溫度及10s-1的剪切速率下根據所述樹脂組成物的濃度量測所述樹脂組成物的相對黏度且量測值示於所述相對黏度根據所述濃度變化的曲線圖中時,CE表示在所述曲線圖梯度的拐點處的濃度,其中所述相對黏度是相較於黏度為0.8厘泊的溶劑來量測,且所述黏度為0.8厘泊的溶劑的所述相對黏度為1,且在以上方程式2中,在其中使用延伸黏度計卡百利在25℃的溫度下將所述樹脂組成物密封於同軸且垂直設置的一對圓形板之間且上部板在50毫秒的時間內在垂直方向上升高了40毫米並保持不變的狀態下,D1表示由所述樹脂組成物形成的細絲的初始直徑,D(t)表示所述細絲在斷裂時間(t)處的直徑,且k表示比例常數。
- 一種色彩轉換膜,具有包含如申請專利範圍第7項所述的樹脂組成物的色彩轉換層。
- 如申請專利範圍第8項所述的色彩轉換膜,更包括位於所述色彩轉換層的至少一側上的保護膜或障壁膜。
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