TWI668278B - 用於半導體奈米粒子之阻氣塗層 - Google Patents

用於半導體奈米粒子之阻氣塗層 Download PDF

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TWI668278B
TWI668278B TW106131181A TW106131181A TWI668278B TW I668278 B TWI668278 B TW I668278B TW 106131181 A TW106131181 A TW 106131181A TW 106131181 A TW106131181 A TW 106131181A TW I668278 B TWI668278 B TW I668278B
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沃，康-都安
耐吉 皮凱特
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英商納諾柯技術有限公司
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Abstract

本發明係關於一種用短波長UV輻射固化之薄矽氮烷塗層，其為極透明的，呈現良好的阻氧特性且對含量子點之膜中的量子點損害最小。

Description

用於半導體奈米粒子之阻氣塗層
本發明大體上係關於半導體奈米粒子-亦稱為「量子點」(QD)。 更特定言之，其係關於應用於含QD之膜、珠粒及其類似物之塗層以保護QD免受有害環境因素，尤其氧氣及濕氣。
相關技術之描述，包括 37 CFR 1.97 及 1.98 中揭示之資訊 . 當用於顯示器及照明應用中時，量子點受益於氣體阻擋囊封。在一個尤其較佳方法中，QD首先分散於高度相容材料(諸如有機兩親媒性大分子或聚合物)中以形成防止量子點凝聚之內相，由此保持量子點之光學效能。內相隨後囊封於具有較低透氧性之外相樹脂中。 美國專利第9,708,532號揭示量子點之多相聚合物膜。QD吸附於分散在外聚合物相內之主體基質中。主體基質係疏水性的且與QD之表面相容。主體基質亦可包括防止QD凝聚之骨架材料。外聚合物通常係更具親水性的且防止氧氣與QD接觸。美國專利第9,680,068號亦揭示含有量子點之多相聚合物膜。膜具有主要疏水性聚合物之域及主要親水性聚合物之域。大體上更穩定於疏水性基質內之QD主要分散於膜之疏水性域內。親水性域傾向於在排除氧氣時有效。 該等有機二相樹脂展示更佳的阻氧特性，但不足以使諸如可在背光單元(BLU)中碰到之高溫及高濕度下照射下的量子點安定化，因為氧氣仍可通過囊封劑遷移至量子點之表面，其可導致光氧化且引起量子產率下降。目前實踐係將含量子點的樹脂包夾於兩個阻擋膜之間。嵌入有QD之聚合物珠粒對於安定化更具有挑戰性，因為其需要薄無機塗層之保形層(例如Al2 O3 )。使用原子層沈積(ALD)方法塗覆珠粒或其類似物極其耗時且難以擴大規模。此外，在ALD塗覆之後已觀測到顯著降低的量子產率(QY)。 矽氮烷類塗層係珠粒上之阻擋膜及無機塗層兩者的替代物。矽氮烷係具有由共價鍵接合之矽及氮原子之直鏈或分支鏈的矽及氮的氫化物。該等化合物之有機衍生物亦被稱為矽氮烷。其類似於矽氧烷類，用-NH-替換-O-。其個別名稱視化學結構中矽原子之數目而定。舉例而言，六甲基二矽氮烷(或雙(三甲基矽烷基)胺；[(CH3 )3 Si]2 NH)含有兩個結合至氮原子之矽原子。 矽氮烷塗層之熱固化已由申請人測試。然而，已發現熱固化對QD造成顯著損害。熱固化矽氮烷塗層不足以使膜或珠粒中之量子點安定化。因此，測試UV可固化矽氮烷而非熱固化矽氮烷以使對量子點之損害降至最低。
已發現，用短波長UV輻射固化之薄矽氮烷塗層係極透明的，呈現良好的阻氧特性且對量子點造成的損害最小。本方法並沒有ALD耗時且可用於含QD之膜及聚合物或含量子點之無機珠粒的大規模生產。 已發現，在量子點嵌入於二相樹脂系統中時，矽氮烷塗層作用尤佳。 預期二相樹脂系統之使用可尤其在矽氮烷進行UV固化時增強量子點之穩定性。 在一測試中，製備具有大致100 µm白色樹脂層的10 cm × 10 cm可剝離膜，該白色樹脂層包含層合於125 µm阻擋膜之間的發綠螢光CFQD®量子點[Nanoco技術有限公司(Nanoco Technologies Ltd.)，Manchester UK]。未改質之膜用作對照樣品。測試樣品藉由以下製備：剝離阻擋膜中之一者，塗佈表面，因此膜上曝露有UV可固化矽氮烷塗層[聚(全氫矽氮烷(perhydrosilazane))；CAS號：90387-00-1 ENCS號：(2)-3642]，且隨後曝露矽氮烷前驅體至UV輻射。隨後評估經矽氮烷塗佈之膜的光學及壽命可靠度。此方法可延伸至含有嵌入量子點之塗層聚合物珠粒。 經矽氮烷塗佈之含QD的膜在超薄裝置(例如行動電話)中係尤其有利的，因為相對於先前技術之阻擋塗層而言，需要矽氮烷之相對薄層。
相關申請案之交叉參考： 本申請案主張2016年9月12日申請的美國臨時專利申請案第62/393,325號之權益，該申請案之內容以全文引用的方式併入本文中。 在本發明之一個特定例示性實施例中，使用二相樹脂系統製備100微米厚的QD膜。含有521 nm PLmax 、43 nm FWHM及80% QY之綠光量子點的樹脂層層合於兩個125微米阻擋膜(I-Component有限公司(I-Component Co. Ltd.)，S. Korea)之間。膜展示對阻擋膜的極佳黏著力或單面可剝離，該單面視含QD之樹脂接觸的哪面阻擋膜而定。可剝離QD膜之裸露面隨後塗佈有矽氮烷前驅體，如圖1中所展示。旋塗用於此特定研究但亦可使用浸塗或噴霧以控制矽氮烷塗層之厚度(參見圖1)。狹縫式塗佈亦可行且較佳可用於工業規模生產。經塗佈之膜隨後烘烤(80℃，3 min)以在用短波長UV輻射(172 nm氙準分子燈；＞100 mV/cm2 ；2至6 mm輻射間隙)以不同量照射之前移除溶劑。矽氮烷塗層之厚度可藉由改變矽氮烷濃度及旋轉或浸漬的速度(若分別使用旋塗或浸塗)來控制。二相樹脂系統可提供對於量子點之增強的保護，以免受UV固化輻射之損害。 現參看圖3，各種含QD之膜的穩定性測試結果以圖形格式呈現。圖形A係針對囊封於兩個市售阻擋膜(I-Component有限公司)之間的QD二相系統膜作為對照。圖形B係針對僅在一面具有市售阻擋膜(I-Component有限公司)之QD膜。圖形C係針對在一面具有市售阻擋膜(I-Component有限公司)且在另一面具有用高量[7 J/cm2 ] UV輻射固化之200 nm矽氮烷塗層的QD膜。圖形D係針對在一面具有市售阻擋膜(I-Component有限公司)且在另一面具有用低量[4 J/cm2 ]固化之200 nm矽氮烷塗層的QD膜。圖形E係針對在一面具有市售阻擋膜(I-Component有限公司)且在另一面具有用高量[7 J/cm2 ] UV輻射固化之100 nm矽氮烷塗層的QD膜。圖形F係針對在一面具有市售阻擋膜(I-Component有限公司)且在另一面具有用低量[4 J/cm2 ] UV輻射固化之100 nm矽氮烷塗層的QD膜。 表1呈現對照膜(樣品A，囊封於兩個市售阻擋膜之間的QD膜)及一面上具有市售阻擋膜且另一面上無阻擋或矽氮烷塗層之膜的某些光學資料。對照膜展示61%之高QY及45%之EQE，而一面上不具有阻擋之QD膜(樣品B)的QY及EQE僅分別為40%及32%，表明市售阻擋膜保護量子點免受(光)氧化。然而，經矽氮烷塗佈之膜的QY比對照稍微更低，其指示塗佈方法對量子點具有某些負面影響。具有較薄矽氮烷塗層之膜(樣品E及F)比具有較厚矽氮烷塗層之膜展示較高的QY及EQE，其表明可存在對於QD膜的最佳矽氮烷塗層厚度。 表 1 . 圖2中所展示之含QD之膜的量子產率及量子效率。 上文之QD膜在光測試上之壽命藉由在60℃及90%相對濕度下，用具有106 mW/cm2 之強度的450 nm藍光照射此等膜進行。監測QD發射峰值強度對比時間(圖3)。在無氣體阻擋層下，樣品B中綠光QD在數小時內完全衰減，而對照膜及經矽氮烷塗佈之膜表現彼此類似，亦即綠光量子點在500小時之後保持穩定。綠光量子點在較厚經矽氮烷塗佈之膜中相比於在具有較薄矽氮烷塗層之膜中的彼等而言更穩定。具有矽氮烷塗層之QD膜的穩定性表明矽氮烷塗層之阻氧特性等同於市售阻擋膜之阻氧特性或甚至更佳。應注意，固化UV輻射之量不影響QY及/或EQE，且經矽氮烷塗佈之膜的穩定性證實短UV固化對較薄阻擋塗層的優點(此因其低穿透深度而使對量子點的損害降至最低)。 亦有可能塗佈含QD之聚合物珠粒或其他具有矽氮烷之三維物件(諸如LED蓋及其類似物)。含量子點之珠粒可在固化製程進行之前在例如使用惰性氣體或矽氮烷前驅體之非溶劑的流體化床中用矽氮烷前驅體塗佈。 前述呈現體現本發明原理之系統的特定實施例。熟習此項技術者將能夠設計替代方式及變化，即使其未明確地揭示於本文中，但因此體現彼等原理且因此在本發明之範疇內。儘管已展示且描述本發明之特定實施例，但其並不意欲限制本專利覆蓋之內容。熟習此項技術者將理解可在不背離如由隨附申請專利範圍字面上及等效地涵蓋之本發明的範疇的情況下進行各種變化及修改。
圖1係根據本發明實施例之用於含量子點之膜的矽氮烷的製備的示意性圖示。 圖2係含QD之膜的橫截面圖，其測試結果呈現於圖3中。 圖3含有展示對於各種含量子點之膜的綠色QD發射峰值強度、LED強度及外部量子效率(EQE)的變化對比時間(相對於初始值)的圖形。 圖4A展示經取代之矽氮烷的大體化學結構。 圖4B係一個特定代表性多環矽氮烷之化學結構。 圖4C係另一矽氮烷之化學結構。在下文所報導之某些試驗中，在所用特定矽氮烷中，R8 、R9 及R10 =H。

Claims (19)

  1. 一種螢光膜，其包含：含量子點之層，其具有第一側面及對置之第二側面；及矽氮烷塗層，其在該含量子點之層之該第一側面及該第二側面中的至少一者上，其中該含量子點之層包含嵌入於具有疏水性域及親水性域之二相樹脂系統中的量子點。
  2. 如請求項1之螢光膜，其進一步包含在該含量子點之層的該第一側面及該第二側面兩者上的矽氮烷塗層。
  3. 如請求項1之螢光膜，其中該矽氮烷塗層係在該含量子點之層的該第一側面上且進一步包含在該含量子點之層的該第二側面上的阻擋膜。
  4. 如請求項1之螢光膜，其中該含量子點之層在由藍光源照射時產生綠光。
  5. 一種螢光珠粒，其包含：含量子點之主體；及在該含量子點之主體上的矽氮烷塗層。
  6. 一種用於發光二極體(LED)的螢光蓋，其包含：含量子點之主體，其具有上表面、對置底表面及至少一個側面；及矽氮烷塗層，其在該含量子點之主體之該上表面、該底表面及該至少一個側面中之至少一者上。
  7. 如請求項6之用於LED的螢光蓋，其中該矽氮烷塗層係在該含量子點之主體之該上表面、該底表面及該至少一個側面中之每一者上。
  8. 如請求項6之用於LED的螢光蓋，其中該含量子點之主體係經配置以使得該底表面由該LED照射，且該上表面在該蓋安裝於含有該LED之封裝上時發射由該等量子點產生的螢光。
  9. 如請求項6之用於LED的螢光蓋，其中該含量子點之主體包含嵌入於樹脂中的量子點。
  10. 一種用於塗覆矽氮烷塗層至包含量子點之薄膜的方法，該方法包含：塗覆矽氮烷前驅體至包含量子點之該薄膜的至少一個側面上；及藉由使具有塗覆至其上之矽氮烷前驅體的該薄膜曝露至紫外(UV)輻射來固化該矽氮烷前驅體，其中該包含量子點之薄膜包含嵌入於具有疏水性域及親水性域之二相樹脂系統中的量子點。
  11. 如請求項10之方法，其中該UV輻射係短波長UV輻射。
  12. 如請求項11之方法，其中該UV輻射具有約172nm之波長。
  13. 如請求項10之方法，其中使具有矽氮烷前驅體塗覆至其上的該薄膜曝露於約7J/cm2的強度下的該UV輻射。
  14. 如請求項10之方法，其中該矽氮烷前驅體係全氫矽氮烷。
  15. 如請求項10之方法，其進一步包括加熱已塗覆矽氮烷前驅體之該薄膜至足以大體上移除溶解該等矽氮烷前驅體之溶劑的溫度及時間。
  16. 如請求項15之方法，其中該加熱以移除該溶劑係在約80℃下進行約3分鐘。
  17. 一種用於塗覆矽氮烷塗層至包含量子點之聚合物珠粒的方法，該方法包含：使包含量子點之該等聚合物珠粒流體化；塗覆矽氮烷前驅體至包含量子點之該等流體化聚合物珠粒；及藉由使具有塗覆至其上之矽氮烷前驅體的該等聚合物珠粒曝露至紫外(UV)輻射來固化該矽氮烷前驅體。
  18. 如請求項17之方法，其中使該等聚合物珠粒流體化包含使用惰性氣體使該等聚合物珠粒流體化。
  19. 如請求項17之方法，其中使該等聚合物珠粒流體化包含使用該等矽氮烷前驅體之非溶劑使該等聚合物珠粒流體化。
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