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TWI743032B - 用於封裝量子點之多層聚合物複合材料 - Google Patents

用於封裝量子點之多層聚合物複合材料 Download PDF

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Publication number
TWI743032B
TWI743032B TW105106559A TW105106559A TWI743032B TW I743032 B TWI743032 B TW I743032B TW 105106559 A TW105106559 A TW 105106559A TW 105106559 A TW105106559 A TW 105106559A TW I743032 B TWI743032 B TW I743032B
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Prior art keywords
polymer composite
composite material
item
patent application
quantum dots
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TW105106559A
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TW201700513A (zh
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志峰 白
賈布摩 朱
成仁慶
詹姆士 泰勒
Original Assignee
美商陶氏全球科技責任有限公司
美商羅門哈斯電子材料有限公司
南韓商羅門哈斯電子材料韓國公司
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Abstract

一種聚合物複合材料，其包括量子點及至少一種式(I)化合物之聚合單元
Figure 105106559-A0202-11-0001-1
其中R1為氫或甲基且R2為C6-C20脂族多環取代基。

Description

用於封裝量子點之多層聚合物複合材料
本發明係關於一種用於製備含有量子點之多層聚合物複合材料之方法。
半導體量子點(QD)提供顯著不同於塊體材料之光學吸收及發射(光致發光PL或電致發光EL)特性。隨著粒度減小，有效能帶隙(Eg)或可用能級增加，且產生藍移之PL光譜。相同材料內藉由粒度依賴性量子限制效應之此光譜可調諧性為優於習知塊體半導體之關鍵優勢。由於其獨特光學性質，QD在多種顯示及照明應用中引起巨大關注。大多數QD具有無機殼體，其具有較大帶隙材料以將電子及電洞對限制於核心區域內且防止任何表面電荷狀態。外部殼體隨後由有機配位體覆蓋以減少殼體之俘獲狀態，所述俘獲狀態可能會導致量子產率(QY)降低。有機配位體幫助QD分散於有機/水性溶劑中。包圍QD之典型有機配位體具有相對長的烷基鏈，其提供於非極性溶劑或單體中之高溶解度。不幸地，QD在光吸收/轉換過程期間極易受光氧化影響。此外，當配位體不相容時，濕氣可能具有類似影響。QD典型地封裝於聚合物基質中以保護其免於水及氧氣之不良作用。舉例而 言，US2010/0084629揭示多種聚合物作為封裝劑。然而，此參考文獻未揭示本文所描述之聚合物組合物。
本發明提供一種聚合物複合材料，其包括量子點及式(I)化合物之聚合單元
Figure 105106559-A0202-12-0002-3
其中R1為氫或甲基且R2為C6-C20脂族多環取代基。
除非另外規定，否則百分比為重量百分比(重量%)，且溫度以℃為單位。除非另外規定，否則操作在室溫(20-25℃)下進行。沸點在大氣壓(約101kPa)下量測。術語「(甲基)丙烯酸酯」意謂丙烯酸酯或甲基丙烯酸酯。量子點在本領域中為眾所周知的，參見例如US2012/0113672。
在本發明之一個較佳實施例中，聚合物複合材料為多層組合件之一部分，所述多層組合件在聚合物複合材料之各側上亦包括外層。較佳地，外層為氧氣障壁，其亦抑制濕氣之通過。較佳地，外層包括聚合物薄膜，較佳包括聚對苯二甲酸伸乙酯(PET)、聚芳基醚酮、聚醯亞胺、聚烯烴、聚碳酸酯、聚甲基丙烯酸甲酯(PMMA)、聚苯乙烯或其組合之聚合物薄膜。較佳地，外層進一步包括氧化物或氮化物，較佳矽氧化物、二氧化鈦、氧化鋁、矽氮化物或其組合。較佳地，氧化物或氮 化物塗佈於聚合物薄膜之面向QD層之表面上。較佳地，各外層包括厚度為25至150微米(較佳50至100微米)之聚合物薄膜及厚度為10至100nm(較佳30至70nm)之氧化物/氮化物層。在本發明之一些較佳實施例中，外層包括至少兩個聚合物薄膜層及/或至少兩個氧化物/氮化物層；不同層可能具有不同組成。較佳地，外層具有極低氧氣透過率(OTR，<10-1cc/m2/天)及低水蒸氣透過率(WVTR，<10-2g/m2/天)。較佳地，外層中之聚合物薄膜具有60至200℃、較佳至少90℃、較佳至少100℃之Tg。
較佳地，本發明之聚合物複合材料之厚度為10至500微米、較佳至少20微米、較佳至少30微米、較佳至少40微米；較佳不超過400微米、較佳不超過300微米、較佳不超過200微米、較佳不超過150微米。較佳地，各外層之厚度為20至100微米、較佳25至75微米。
較佳地，本發明之聚合物複合材料藉由使藉由混合單體、QD及其他視情況選用之添加劑製備之樹脂自由基聚合而製備。較佳地，樹脂在固化之前藉由典型方法(例如旋轉塗佈、狹縫塗佈、凹版印刷、噴墨及噴塗)塗佈於第一外層上。較佳地，固化藉由將樹脂暴露於紫外光或熱量、較佳紫外光、較佳UVA範圍中之紫外光而引發。
較佳地，R2為C7-C17脂族多環取代基，較佳地，R2為C8-C15脂族多環取代基。較佳地，R2為橋連多環取代基；較佳雙環、三環或四環取代基；較佳雙環或三環取代基。較佳地，R2為飽和脂族取代基。R2之較佳結構包含例如金剛烷、雙環[2,2,1]烷、雙環[2,2,2]烷、雙環[2,1,1]烷及三環癸烷(例 如，三環[5,2,1,02,6]癸烷)；此等結構可經烷基、烷氧基、羥基或(甲基)丙烯酸酯取代(即，式(I)化合物可具有至少兩個、較佳不超過兩個(甲基)丙烯酸酯取代基)；較佳地，烷基及烷氧基具有一至六個、較佳一至四個碳原子。三環癸烷及雙環[2,2,1]烷為尤佳的，特別為三環[5,2,1,02,6]癸烷、二甲醇二甲基丙烯酸酯及丙烯酸異冰片酯。較佳地，內層包括具有一個(甲基)丙烯酸酯取代基之式(I)化合物及具有兩個(甲基)丙烯酸酯取代基之式(I)化合物的聚合單元；較佳地，重量比分別為100：1至1：5、較佳10：1至1：2。
較佳地，本發明之聚合物複合材料包括0.01至5重量%、較佳至少0.03重量%、較佳至少0.05重量%、較佳不超過4重量%、較佳不超過3重量%、較佳不超過2重量%之量子點。較佳地，量子點包括CdS、CdSe、CdTe、ZnS、ZnSe、ZnTe、HgS、HgSe、HgTe、GaN、GaP、GaAs、InP、InAs或其組合。
較佳地，包圍量子點之無機部分之配位體具有非極性組分。較佳配位體包含例如三辛基氧化膦、十二硫醇及脂肪酸鹽(例如，硬脂酸鹽、油酸鹽)。
可併入至本發明之聚合物複合材料中之其他添加劑包含uv穩定劑、抗氧化劑、改良光提取之散射劑及增加黏度之增稠劑(例如，丙烯酸胺基甲酸酯寡聚物)。較佳增稠劑包含丙烯酸胺基甲酸酯、纖維素醚、纖維素丙烯酸酯、聚苯乙烯聚合物、聚苯乙烯嵌段共聚物、丙烯酸樹脂及聚烯烴彈性體。較佳地，聚苯乙烯、丙烯酸及聚烯烴增稠劑具有50,000至400,000、較佳100,000至200,000之Mw。較佳地， 纖維素醚具有1,000至100,000之Mw。
丙烯酸胺基甲酸酯寡聚物可為聚酯型、聚醚型、聚丁二烯型或聚己內酯型。其可具有雙官能、三官能、六官能反應性。寡聚物之黏度在50C下可在1000至200,000cPs範圍內。對於非極性配位體QD，聚丁二烯型為較佳的。
較佳地，第一內層包括1至60重量%、較佳至少5重量%、較佳至少10重量%、較佳不超過50重量%、較佳不超過40重量%之丙烯酸胺基甲酸酯。
聚合物複合材料之較佳形式包含例如薄膜、珠粒、條帶、桿、方塊及板。聚合物複合材料適用於多種應用，包含例如顯示、照明及醫療應用。較佳顯示應用包含公眾訊息顯示器、標牌、電視、監視器、行動電話、平板電腦、膝上型電腦、汽車儀錶盤及手錶。
實例
實例之樣品製備
藉由在兩個i-Component PET障壁薄膜之間層壓樹脂調配物來製備所有樣品。將約2mL樹脂分配於底部薄膜上，且用間隙塗佈棒基於所要薄膜厚度用間隙設置(10密耳-12密耳)塗覆頂部。除非另外指出，否則在Fusion UV F300S固化系統中用UVA 400mJ/cm2固化樣品。藉由用測微計量測固化薄膜且隨後減去障壁薄膜厚度來測定薄膜厚度。用Hamamatsu C9920-02G積分球量測光致發光量子產率(PLQY)、峰值發射波長(PWL)及發射峰之半高全寬(FWHM)。藉由對裸背光單元上老化之1"×1"樣品進行圖像分析來測定邊緣入口。
實例1：將線性脂族單體與環脂族單體比較
固化條件：UVA 400mJ/cm2×4次
Figure 105106559-A0202-12-0006-4
1.如US7588828中所描述之無鎘量子點
CN996寡聚物為來自Sartomer America之脂族丙烯酸胺基甲酸酯寡聚物。
塗層厚度：
Figure 105106559-A0202-12-0006-6
在1000Cd/m2藍色BLU之後的邊緣入口損壞
Figure 105106559-A0202-12-0006-8
實例2：具有抗氧化劑(IRGAFOS 168)及光穩定劑(TINUVIN 5100)之樹脂之實例
Figure 105106559-A0202-12-0007-10
BR-641D寡聚物為來自Dymax之聚丁二烯丙烯酸胺基甲酸酯寡聚物。
TIPURE 706可購自Dupont。
固化：400mJ/cm2，單程
Figure 105106559-A0202-12-0007-12
Figure 105106559-A0202-12-0007-13
實例3：
用聚合物黏度改性劑(KRATON G1650)製備之樹脂之實例
Figure 105106559-A0202-12-0007-35
Zoco101可購自Zochem。
Figure 105106559-A0202-12-0008-15
Figure 105106559-A0202-12-0008-16
實例4：
用各種比率之環脂族單體製備之樹脂的實例
Figure 105106559-A0202-12-0008-18
Figure 105106559-A0202-12-0008-19
Figure 105106559-A0202-12-0008-20
在60℃/90%相對濕度中儲存之後的邊緣入口損壞(mm)
Figure 105106559-A0202-12-0009-21
實例5：
用小負載量之線性脂族單體作為相容添加劑製備之樹脂的實例
Figure 105106559-A0202-12-0009-23
Figure 105106559-A0202-12-0009-24
Figure 105106559-A0202-12-0009-25
實例6：用兩種不同量子點混合物製備之樹脂之實例
Figure 105106559-A0202-12-0010-26
Figure 105106559-A0202-12-0010-27
將固化膜置放於基於藍色LED之背光單元(BLU)之光導板與稜鏡薄膜/亮度提昇薄膜之間。使用GL Spectis分光輻射度計量測BLU光譜。基於BLU光譜及可用彩色濾光片資料集計算最終光譜之色彩座標及色域覆蓋率。
Figure 105106559-A0202-12-0010-28
Figure 105106559-A0202-12-0010-29
Figure 105106559-A0202-12-0010-30
藉由最大峰值強度標準化之波長依賴性發射光譜
Figure 105106559-A0202-12-0011-31
Figure 105106559-A0202-12-0012-36

Claims (7)

  1. 一種聚合物複合材料，其包括量子點及至少一種式(I)化合物之聚合單元
    Figure 105106559-A0305-02-0015-1
     其中R1為氫或甲基且R2為C7-C17橋連多環取代基，前提為該至少一種式(I)化合物之該聚合單元為非離子性；以及所述聚合物複合材料包括重量比分別為100：1至1：5的具有一個(甲基)丙烯酸酯取代基之式(I)化合物及具有兩個(甲基)丙烯酸酯取代基之式(I)化合物。
  2. 如申請專利範圍第1項之聚合物複合材料，其中R2具有雙環[2,2,1]烷或三環癸烷環系統。
  3. 如申請專利範圍第2項之聚合物複合材料，其中所述量子點包括CdS、CdSe、CdTe、ZnS、ZnSe、ZnTe、HgS、HgSe、HgTe、GaN、GaP、GaAs、InP、InAs或其組合。
  4. 如申請專利範圍第3項之聚合物複合材料，其進一步包括丙烯酸胺基甲酸酯、纖維素醚、纖維素丙烯酸酯、聚苯乙烯聚合物、聚苯乙烯嵌段共聚物、丙烯酸樹脂或聚烯烴彈性體。
  5. 如申請專利範圍第3項之聚合物複合材料，其進一步包括散射劑。
  6. 如申請專利範圍第5項之聚合物複合材料，其進一步包括抗氧化劑或UV光穩定劑。
  7. 如申請專利範圍第3項之聚合物複合材料，其為薄膜。
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