TW202033680A - 聚合物-多金屬氧酸鹽複合塗佈液及其應用 - Google Patents
聚合物-多金屬氧酸鹽複合塗佈液及其應用 Download PDFInfo
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Abstract
本發明揭露一種聚合物-多金屬氧酸鹽複合塗佈液,其包含一溶劑、一聚合物或二種以上聚合物交纏,以及一多金屬氧酸鹽,其中,聚合物或二種以上聚合物交纏結構與多金屬氧酸鹽之重量比例範圍為1:0.001~1:0.09。上述複合塗佈液可用以製造載子傳遞薄膜,以及具備載子傳遞薄膜的有機電子裝置。
Description
本案主張2018年9月17日申請之美國臨時專利申請案第62/732,165號的優先權,其揭露的全部內容引用併入本案。
本發明係關於一種複合塗佈液,特別是一種聚合物-多金屬氧酸鹽複合塗佈液及其應用。
有機電子裝置包含有機光伏裝置、有機光感測裝置、有機發光二極體以及有機薄膜電晶體(OTFT),近年來在新製程開發下發展興盛,特別是溶液加工法不需要真空環境,低操作溫度,具有成本低、可大面積卷對卷生產等優勢。
以有機光伏裝置的結構為例,通常包括透明基板、透明電極(例如ITO)、載子傳遞層一、主動層、載子傳遞層二、金屬電極(例如鋁或銀),其中用於電洞傳遞之載子傳遞材料主要有聚合物和金屬氧化物兩大類。金屬氧化物例如:氧化鉬、氧化釩、氧化鎳、氧化鎢等因具有能階匹配、材料穩定性高等優點。但傳統的金屬氧化物薄膜多採用真空蒸鍍方法沉積,與基於溶液態的印刷塗佈方法不相容,也不利於大面積卷對卷生產。
另一類常用於電洞傳遞的材料為聚合物,主要是poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate),即PEDOT:PSS導電聚合物,它是已商業化廣泛使用的一類材料。該材料可良好分散於水性溶劑中,可大面積塗佈、易於搭配各種塗佈或印刷技術進行使用,且成膜品質高。但是與使用金屬氧化物的電洞傳遞層的有機光伏裝置相比,PEDOT:PSS始終由於載子傳遞特性與能階匹配性上不及蒸鍍型之金屬氧化物,顯著降低終端產品的光電效能。
綜合上述,仍需要學界與業界大力投入開發,以便於開發兼
顧適合大面積生產,以及維持高光電效能的電洞傳遞層材料。
本發明之一目的在於提供一種含有PMA:PEDOT:PSS的複合塗佈液。
本發明之另一目的在於提供一種兼顧適合大面積生產,以及維持高光電效能的電洞傳遞層材料。
第一A圖至第一C圖顯示載子傳遞薄膜的成膜品質。
第二A圖至第二D圖顯示PMA濃度如何影響有機光伏裝置的光電性能。
第三A圖至第三D圖顯示使用PMA:PEDOT:PSS載子傳遞薄膜的元件光電性能與單獨使用PEDOT:PSS載子傳遞薄膜的元件光電性能比較。
本文所用之填充因子(FF),係指實際最大可獲得功率(Pm或Vmp * Jmp)與理論(非實際可獲得)功率之比值((Jsc * Voc)。因此,填充因子可由下式決定:FF=(Vmp * Jmp)/(Voc * Jsc)其中Jmp及Vmp分別表示在最大功率點(Pm)之電流密度及電壓,該點係藉由變化電路中的電阻直到J * V為最大值而得;Jsc及Voc分別表示開路電流及開路電壓。填充因子是評價太陽電池的關鍵參數。
本文所用之開路電壓(Voc),係在無連接外部負載下元件的陽極與陰極之間的電位差。
本文所用之太陽電池的功率轉換效率(PCE),係指從入射光轉變為電力的功率百分比。太陽電池的功率轉換效率(PCE)可藉由最大
功率點(Pm)除以標準測試條件下(STC)入射光輻射照度(E;W/m2)及太陽電池的表面積(Ac;m2)而算出。STC通常指在溫度25℃、輻射照度為1000W/m2之AM(air mass)1.5G光譜。
本文所用之構件(例如一薄膜層),若其包含一個或一個以上的可吸收光子而產生用以產生光電流的激子之化合物,可被視為「光活性」。
本文所用之「溶液加工」,係指化合物(例如聚合物)、材料或組成物可用於溶液態的製程,例如旋轉塗佈、印刷法(例如噴墨印刷、凹版印刷、凸版印刷等)、噴塗法、狹縫塗佈、滴鑄法、浸塗法及刮刀塗佈法。
如本文所用之「退火」,係指在環境中或在減壓或加壓下,對半結晶聚合物膜進行一定持續時間的沉積後熱處理,「退火溫度」,係指該退火過程中該聚合物膜或該聚合物與其他分子之混合薄膜可進行小規模分子運動及重新排列之溫度。不受任何特定理論束縛,據信退火可在可能的情況下導致聚合物膜中的結晶度的增加,提升聚合物膜或該聚合物與其他分子之混合薄膜之材料載子遷移率,並形成分子交互排列而達到有效電子與電洞之獨立傳遞路徑之效果。
本發明之第一實施例揭示一聚合物-多金屬氧酸鹽複合塗佈液,其包含一溶劑、一聚合物或二種以上聚合物交纏結構,以及一多金屬氧酸鹽,其中,聚合物或二種以上聚合物交纏結構與多金屬氧酸鹽之重量比例範圍為1:0.001~1:0.09。較佳者,聚合物或二種以上聚合物交纏結構聚合物與多金屬氧酸鹽之重量比例範圍為1:0.005~1:0.03。
於一實施態樣中,聚合物交纏結構為poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)(PEDOT:PSS)。
於另一實施態樣中,多金屬氧酸鹽選自含有鉬、鎢、釩中的任意一種或者兩種以上的組合的多金屬氧酸鹽。較佳者,多金屬氧酸鹽為phosphomolybdic acid(PMA)。
藉由聚合物交纏結構與多金屬氧酸鹽之間均勻混合,可降低多金屬氧酸鹽的團聚現象,提高成膜均勻性。同時,金屬氧酸鹽也具有調
節聚合物交纏結構的功函數,進而改變有機電子裝置應用性能的功能。
於又一實施態樣中,前述之多金屬氧酸鹽於複合塗佈液中的濃度範圍為0.01~0.8mg/ml。較佳者,濃度範圍為0.05~0.2mg/ml。。
於本實施例中,溶劑選自下列一種或者兩種以上的組合:甲醇、乙醇、正丙醇、異丙醇、正丁醇、叔丁醇、乙二醇以及乙二醇單甲醚。
本發明之第二實施例揭示一載子傳遞薄膜,前述之載子傳遞薄膜係由第一實施例中所述之複合塗佈液所形成。
本發明之第三實施例揭示一有機電子裝置,包含一第一電極(透明電極)、一第一載子傳遞層、一主動層、一第二載子傳遞層、一第二電極,前述第一載子傳遞層位於第一電極與主動層之間,第二載子傳遞層位於主動層與第二電極之間,前述第二載子傳遞層如第二實施例所述之載子傳遞薄膜。此外,有機電子裝置包含有機光伏裝置、有機光感測裝置、有機發光二極體以及有機薄膜電晶體(OTFT)。
範例1:聚合物交纏結構-多金屬氧酸鹽複合塗佈液製備
a.試劑A-將2mg之polyoxometalate系列化合物(如phosphomolybdic acid,PMA)溶解於1ml的極性溶劑中(如2-propanol)
b.將試劑A與試劑B-poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)(PEDOT:PSS)溶液以體積比1:9進行混合(例:1ml試劑A加入9ml試劑B,其中試劑B之PEDOT:PSS固含量約1% in H2O,故9ml(9g)PEDOT:PSS solution中內約含90mg PEDOT:PSS固體)
c.每10ml之試劑A與試劑B混合溶液中,PEDOT:PSS(固體)對polyoxometalate(固體)的重量比為90mg:2mg=1:0.022
d.每10ml之試劑A與試劑B混合溶液中,含有2mg PMA。PMA於溶液中之濃度為2mg/10ml=0.20mg/ml。
範例2:有機光伏裝置的製造及測試
使用具有~15Ω/□的薄層電阻的預圖案化的ITO塗覆的玻璃作為基板。依順序在肥皂去離子水、去離子水、丙酮及異丙醇中超音波震盪處理,在每個步驟中清洗15分鐘。用UV-ozone清潔器進一步處理洗滌過的基材30分鐘。將ZnO(二乙基鋅溶液,在甲苯中15wt%,用四氫呋喃稀釋)的頂塗層,以5000_rpm的旋轉速率30秒旋轉塗佈在ITO基板上,然後在空氣中在150℃下烘烤20分鐘。在o-xylene中製備主動層溶液。主動層材料為共軛聚合物與富勒烯衍生物之混合物,主動層材料濃度為35mg ml-1。為將主動層材料完全溶解,主動層溶液需在加熱板上以120℃下攪拌至少1小時。隨後將主動層材料回復至室溫進行旋轉塗佈。最後將塗佈完成之主動層薄膜在120℃下退火5分鐘。然後將範例1所提供之試劑A與試劑B之混合溶液塗佈或印刷於主動層上,並乾燥之以便於形成載子傳遞薄膜。
關於載子傳遞薄膜的成膜品質請參考表一所列不同配方,以及第一A圖、第一B圖與第一C圖,第一A圖係配方A於光伏元件主動層上所製成薄膜,第一B圖係配方B於光伏元件主動層上所製成薄膜,第一C圖係配方D於光伏元件主動層上所製成薄膜。影響成膜品質最重要的因素是PMA在PEDOT:PSS溶液中的濃度,表一中控制組是完全沒有PMA的PEDOT:PSS溶液,溶液沒有膠化(gelled)情形,成膜完整。配方A與配方B由於PMA濃度偏高(0.83與0.67mg/ml)且試劑A(溶劑為醇類)與試劑B(溶劑為水)之混合比例亦較相近(1:5與1:2),因此可發現在醇類溶劑與水及PMA與PEDOT:PSS交替作用下,混合溶液發生膠化現象,無法形成完整薄膜,請參考第一A圖與第一B圖。而配方C雖然試劑A與試劑B(之混合比例已提高至1:10,但由於試劑A中的PMA含量相對較高(10mg/ml),整體PMA於試劑B內的含量為0.91mg/ml,同樣無法得到理想的膜面,也顯見PMA含量對成膜性之重要。配方D的試劑A與試劑B比例調整為1:9,PMA於試劑B內之濃度調低至0.80mg/ml,可以發現混合溶液雖然發生膠化現象,但是速度較慢,可以形成完整薄膜。
隨後沉積100nm厚度之銀作為上電極。使用環氧樹脂在手套箱內封裝所有元件。使用class AAA太陽光模擬器,在1000W/m2的AM1.5G光強度下測量元件J-V特性。此處用於校正光強度之校正電池乃採用具有KG5濾波片的標準矽二極體,並於使用前先經過第三方校正。此實驗使用Keithley 2400 source meter儀器記錄J-V特性。電池面積為4mm2,並由金屬遮罩對準元件進行面積定義。
範例3:有機光伏裝置的效能分析
關於PMA濃度如何影響光電性能請參考表二、第二A圖、第二B圖、第二C圖與第二D圖,第二A圖顯示當PMA濃度維持在0.1mg/ml以上,裝置的開路電壓(Voc)也一直維持在0.8V左右。第二B圖顯示當PMA濃度在0.01mg/ml-0.2mg/ml之間,裝置的開路電流(Jsc)可以維持在15mA/cm2以上。第二C圖顯示當PMA濃度在0.2mg/ml以上,裝置的填充因子(FF)可以維持在72%以上。第二D圖顯示當PMA濃度在0.01mg/ml-0.3mg/ml之間,裝置的功率轉換效率(PCE)可以維持在8.4%以上。
再請參閱第三A圖至第三D圖,方塊數據是控制組配方製成有機光伏裝置,圓圈數據係配方E製成有機光伏裝置,可以發現使用
PMA:PEDOT:PSS載子傳遞薄膜的元件光電性能優於單獨使用PEDOT:PSS載子傳遞薄膜的元件光電性能。此外,使用PMA:PEDOT:PSS載子傳遞薄膜的元件在長時間工作中的穩定性都能維持良好。
Claims (10)
- 一聚合物-多金屬氧酸鹽複合塗佈液(polymer-polyoxometalate composite ink),該複合塗佈液包含:一溶劑;一聚合物或二種以上聚合物交纏結構;以及一多金屬氧酸鹽,其中,該聚合物或二種以上聚合物交纏結構與該多金屬氧酸鹽之重量比例範圍為1:0.001~1:0.09。
- 如申請專利範圍第1項所述之聚合物-多金屬氧酸鹽複合塗佈液,其中該聚合物或二種以上聚合物交纏結構與該多金屬氧酸鹽之重量比例範圍為1:0.005~1:0.03。
- 如申請專利範圍第1項所述之聚合物-多金屬氧酸鹽複合塗佈液,其中該多金屬氧酸鹽於該複合塗佈液中的濃度範圍為0.01~0.8mg/ml。
- 如申請專利範圍第1項所述之聚合物-多金屬氧酸鹽複合塗佈液,其中該多金屬氧酸鹽於該複合塗佈液中的濃度範圍為0.05~0.2mg/ml。
- 如申請專利範圍第1項所述之聚合物-多金屬氧酸鹽複合塗佈液,其中該二種以上聚合物交纏結構為poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)(PEDOT:PSS)。
- 如申請專利範圍第1項所述之聚合物-多金屬氧酸鹽複合塗佈液,其中,該多金屬氧酸鹽選自含有鉬、鎢、釩中的任意一種或者兩種以上的組合的多金屬氧酸鹽。
- 如申請專利範圍第1項所述之聚合物-多金屬氧酸鹽複合塗佈液,其中該多金屬氧酸鹽為phosphomolybdic acid(PMA)。
- 如申請專利範圍第1項所述之聚合物-多金屬氧酸鹽複合塗佈液,其中該溶劑選自下列一種或者兩種以上的組合:甲醇、乙醇、正丙醇、異丙醇、正丁醇、叔丁醇、乙二醇以及乙二醇單甲醚。
- 一載子傳遞薄膜,該載子傳遞薄膜係由如申請專利範圍第1項所述之聚合物-多金屬氧酸鹽複合塗佈液所形成。
- 一有機電子裝置,包含:一第一電極,該第一電極係為透明電極;一第一載子傳遞層;一主動層,其中,該第一載子傳遞層位於該第一電極與該主動層之間;一第二載子傳遞層;以及一第二電極,其中,該第二載子傳遞層位於該主動層與該第二電極之間,該第二載子傳遞層如申請專利範圍第9項所述之載子傳遞薄膜。
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