Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/10661
標題: 塑膠基材阻氣性鍍膜之設計、製作與應用
Design, Fabrication and Applications of Gas Barrier Coatings on Polymer Substrates
作者: 陳采寧
Chen, Tsai-Ning
關鍵字: barrier;阻氣層;silicon nitride;parylene;calcium test;polymer solar cell;氮化矽;聚-對二甲苯;鈣測法;高分子太陽能電池
出版社: 材料科學與工程學系所
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摘要: 
軟性電子因為具有低製程溫度、重量輕且可沉積在塑膠基板上等優點,除了將帶來更人性化、行動化與個人化的便利新科技外,同時也將大幅改變21世紀人類的生活型態。然而,如同其他前瞻技術一樣,使用塑膠基板製作有機元件仍面臨許多尚待解決之問題。其中,有機半導體對水氣及氧氣非常敏感,尤其是當電流通過有機半導體材料時,其電氣特性會迅速的衰退。這亦是有機半導體之主動電子元件,如有機發光二極體、有機太陽能電池及有機薄膜電晶體,一直無法順利發展的原因之一。為提升有機元件之壽命,本論文主要探討並分析不同類型(氮化矽、氧化矽與聚-對二甲苯)及結構(單層與多層)之阻氣層薄膜,沉積在聚碳酸酯(PC)塑膠基板上之特性。如何製備與軟性基材之間附著力良好、表面粗糙度低、水/氧氣透過率低且機械性質佳之透明阻障膜是本論文之主要目標。
首先,利用氧氣、氮氣及氬氣電漿對軟性基材PC進行表面預處理,經研究後發現,利用高密度氬氣電漿對PC基材預處理60秒後,基板之表面粗糙度由原始之~ 1.71 nm下降至~0.89 nm,因為基板的表面粗糙度會影響沈積在上方薄膜之品質,在經氬氣電漿處理後之基板上,利用電漿輔助化學氣相沈積系統製備單層氮化矽薄膜,其氧氣透過率可由原始之0.61 cm3/m2/day下降至0.1 cm3/m2/day (為MOCON機台所能量測之極限值)。此外,在調變單層氮化矽的製程參數中,薄膜於不同製程溫度下,其特性有顯著之變化,經濕蝕刻法觀察後發現,當沉積溫度由80°C提升至240°C,薄膜內部之缺陷間距推估由125 μm上升至450 μm。然而,單層膜並無法達到有機發光二極體顯示器的嚴苛要求,即水氣透過率< 10-6 g/m2/day與氧氣透過率< 10-3 cm3/m2/day。於是,氮化矽/聚-對二甲苯、氮化矽/氧化矽/聚-對二甲苯與氮化矽/氧化矽多層結構被用來進一步降低水氧氣透過率。其中,將氮化矽薄膜之沉積溫度由80°C提高至200°C,四對氮化矽/聚-對二甲苯多層膜結構之水氣透過率可由7.9×10-4 g/m2/day降至7.41×10-6 g/m2/day。於80°C之低溫製程下,研究發現有機層之厚度與無機膜之薄膜內應力是影響多層膜特性之決定性因素。藉由鈣測試法得知,在25°C,相對溼度40%之測試條件下,重複堆疊多對之氮化矽/氧化矽/聚-對二甲苯多層鍍膜於PC基材上,可將PC之水氣透過率由原始之20 g/m2/day降至2.5×10-7 g/m2/day,經5000次撓曲後,水氣透過率約為4.3×10-6 g/m2/day。為了簡化製程,本文亦探討氮化矽/氧化矽多層膜之特性,經調變多層膜之薄膜內應力,鍍製六對之氮化矽/氧化矽於PC上,可將水氣透過率降至3.1×10-6 g/m2/day,經5000次撓曲後,略微上升至3.5×10-5 g/m2/day,平均可見光穿透率~87%。
最後,本研究將六對之氮化矽/氧化矽多層膜結構實際應用於高分子太陽能元件之封裝。其中,主動層使用聚(3-己烷噻吩)[poly(3-hexylthiophene); P3HT]與碳六十之衍生物([6,6]-phenyl C61-butyric acid methyl ester; PCBM),以塊材異質接面結構(Bulk Heterojunction)製作。探討溶液濃度、溶質比與溶劑退火條件,對主動層之影響,以獲得穩定且最佳化之高分子太陽能元件。另外,特別針對阻障層鍍製過程中,可能產生之影響進行討論。比較最佳化元件在有無阻氣層封裝之情況下,經室外測試,無阻氣層封裝之元件壽命約為50小時,有阻氣層封裝之元件在經過1500小時後,仍具有原始效率50%之光電轉換效率。

Flexible organic light emitting displays (OLEDs) and polymer solar cells (PSCs) are expected to become next-generation electronic devices. These devices require high-performance substrates with a low permeability, high optical transparency, optimum film stress, low surface roughness, good mechanical behavior, and long-term chemical, thermal and environmental stability. Among these requirements, moisture and oxygen permeation could degrade and reduce the performance and durability of electronic devices. In order to achieve OLEDs' lifetime of tens of thousands of hours, the water vapor transmission rate (WVTR) must be <10-6 g/m2/day and the oxygen transmission rate (OTR) must be <10-3 cm3/m2/day. These extreme low transmission rates are several orders of magnitude smaller than those of any polymer substrates, and they can also be several orders of magnitude smaller than what can be measured using commercial equipment (MOCON) designed for this purpose. For these reasons, this dissertation has focused on developing transparent barrier materials on polymer substrates with ultra-low permeabilities and the calcium degradation test for measuring the low permeation. To improve the surface state of polymer substrates, Ar, N2, and O2 plasma-treated polycarbonate (PC) substrates have been investigated. The roughness of Ar plasma-treated PC substrates was decreased from 1.71 to 0.89 nm and, thus, the OTR of silicon nitride (SiNx) coatings on PC decreased from 0.61 to 0.1 cm3/m2/day. For a single barrier film, the growth temperature was found to have significant effects on film's properties. A wet etching process was performed to visualize the defect distribution in the barrier film. After 120 min of etching, the average defect spacing increased from 125 to 450 μm with increasing growth temperature from 80 and 240°C. However, the single barrier film deposited by plasma-enhanced chemical vapor deposition was not sufficient for the strict requirement and multilayer barrier structures were proposed for further reducing the permeability.
Multilayer structures composed of SiNx and parylene thin films were deposited onto flexible Industry Technology Research Institute polyimide with high glass transition temperature. Under room temperature and RH 50%, four SiNx/parylene stacks with the SiNx films deposited at 80 and 200°C were demonstrate to decrease the water vapor transmission rate to 7.9×10-4 and 7.41×10-6 g/m2/day, respectively. As a result, ultra-low permeation can be achieved with less repeating barrier stacks by using high temperature deposited SiNx films in the barrier structures. SiOx films were added into the barrier structures for improving the performance of low temperature deposited barrier structures. OLEDs capped with two SiNx/SiOx/parylene(NOP) stacks deposited at 80°C showed no dark spots and exhibited better emissions than single NOP layers after 100 h under 25°C, 40% RH. However, a lateral leakage was observed in the parylene layer and resulted in increasing permeation and poor adhesion between organic and inorganic layers. By encapsulating the parylene layer, the WVTR can reach 2.5×10-7 g/m2/day as calculated by a calcium test. After being flexed for 5000 times, the WVTR value can keep ~4.3×10-6 g/m2/day. To simplify the growth process, transparent barrier structures consisting of SiNx/SiOx stacks was studied. The internal stress of barrier films was adjusted to prevent the stress-induced cracks during the multilayer deposition process. The WVTR value of the optimum barrier structure can reduce to 3.12×10-6 g/m2/day calculated by a calcium test (100 days at 25°C, 40% relative humidity). After bending for 5000 times in a compressive mode, the WVTR value can keep below 3.54×10-5 g/m2/day. Therefore, this barrier structure was applied for the encapsulation of bulk heterojunction PSCs. After barrier encapsulation, the outside testing experiment shows that the halflife of the devices can be prolonged from ~50 to ~1500 h.
URI: http://hdl.handle.net/11455/10661
Appears in Collections:材料科學與工程學系

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