基于荧光与磷光复合的白光有机电致发光器件研究
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摘要
有机电致发光器件(OLED)因为具备发光效率高、驱动电压低、响应速度快、可视化角度大、可实现柔性化等优点，已经被普遍认为是下一代全彩显示与固体照明的主流技术。OLED发展至今仍然存在一些问题需要进一步研究与完善。在效率方面，蓝色OLED的效率普遍较低，磷光OLED在高亮度下效率下降严重；在光源品质方面，OLED的显色指数需要进一步提高。本论文从以上提出的问题出发，结合OLED的基本理论、发光机理与过程开展了一系列基础与应用研究。主要研究内容包括以下方面：
(1)在蓝色荧光OLED研究中，由于蓝光器件的效率相比绿光与红光器件较低，同时又缺乏深蓝光的材料，使得深蓝光器件成为OLED发展的最大阻碍。首先，对一种发射峰为452nm的新型蓝色荧光材料6,12-bis{[N-(3,4-dimethylphenyl)-N-(2,4,5-trimethylphenyl)]amino}chrysene(BmPAC)进行了初步研究。在以BmPAC为发光客体的OLED器件中，获得了最高发光亮度12500cd/m~2，在电流密度为23mA/cm~2的情况下获得了最大电流效率4.89cd/A，同时器件的电致发光峰为456nm，CIE坐标为(0.16,0.17)。然后将BmPAC与黄光染料搭配，制备了白光OLED。在发光层结构为黄光发光层-阻隔层-蓝光发光层的器件中，启亮电压为4V，在1300cd/m~2亮度下获得了最大电流效率36.11cd/A和最大功率效率22.78lm/W，电流效率在100cd/m~2和1000cd/m~2亮度下下降为34.59cd/A和35.61cd/A。随着亮度的增加，器件的发光光谱基本稳定，相对于黄光，蓝光的发射强度只有轻微的下降，器件的发光光谱为暖白光，最高显色指数为45。在发光层结构为蓝光发光层-阻隔层-黄光发光层-阻隔层-蓝光发光层的器件中，启亮电压降为2.5V，最大电流效率和最大功率效率分别提高到40.9cd/A和49.4lm/W，电流效率在100cd/m~2和1000cd/m~2亮度下下降为37.3cd/A和33.1cd/A，同时器件的最高显色指数提高至53。我们把这种改善归因于使用双蓝光发光层可以得到最好的载流子平衡。最后在9,10-di(2-naphthyl)anthracene (ADN):1-4-di-[4-(N,N-di-phenyl)amino]styryl-benzene (DSA-ph)的发光层中共掺入质量比为1%的深蓝光BD-3染料，通过与无共掺杂的器件相比，器件的发光效率和工作寿命都得到改善与提高，我们把这种提高归因于载流子平衡的改善和激子复合区域的扩宽。共掺杂方法使得ADN本来比空穴迁移率高的电子迁移率降低，从而得到更好的载流子平衡。
(2)在磷光OLED器件中，由于在高亮度下产生大量的三重态激子，会发生三重态-三重态激子淬灭，导致严重的效率滚降现象。首先分别使用双主体掺杂的发光层、双发光层、双主体掺杂的空间阻隔层三种方法研究对效率滚降的改善作用。以Ir(ppy)3为发光客体的绿色磷光OLED器件为研究对象，在使用双主体掺杂的发光层的器件中获得最大电流效率和功率效率分别为26.23cd/A和31.67lm/W，使用双发光层的器件中获得最大电流效率和功率效率分别为29.14cd/A和22.29lm/W，使用双主体掺杂的空间阻隔层的器件中获得最大的电流效率和功率效率分别为50.38cd/A和29.29lm/W。相对其它方法，使用空间阻隔层可以获得最高的发光效率和最轻微的效率滚降。双主体掺杂的空间阻隔层可以最大程度上实现促进载流子向发光层输运与扩宽激子的复合区域。然后研究了使用超薄发光层对磷光OLED的发光效率和效率滚降现象的改善作用。比较使用超薄发光层和普通厚度发光层的器件，通过仔细调节超薄发光层与阻隔层的厚度，我们获得了显色指数高达80的白光OLED，并且最高电流效率29.2cd/A在1000cd/m~2亮度下仅下降到22.8cd/A。而使用普通厚度发光层的器件最高显色指数不足40，最高电流效率只有15.8cd/A，在1000cd/m~2亮度下下降到11.4cd/A。我们把这种提高与改善归因于超薄发光层不仅可以促进载流子的注入与传输，而且超薄发光层中形成的岛状形貌可以为激子的复合提供足够大的空间，极大程度上减少了三重态-三重态激子之间的湮灭。
(3)高显色指数是白光OLED能够应用到高品质照明光源中的关键因素。我们研究了具有双波段、三波段、与四波段电致发光光谱的三种类型白光OLED。在双波段白光器件中获得了较为稳定的白光发射，CIE坐标在(0.47,0.42)附近，最高显色指数为45，同时器件在100cd/m~2亮度下的电流效率为34.59cd/A。对于三波段的白光OLED，最大电流效率为27.29cd/A，最高显色指数为88，在所有亮度下色温低于2800K。对于四波段的白光OLED，在亮度从100cd/m~2变化到5000cd/m~2的过程中，发光光谱从冷白光变化至暖白光，实现了色温可调，并且在5000cd/m~2的亮度下获得了显色指数为89的类太阳光光谱。我们证明了增加发光峰的数目可以扩大发光光谱在可见光区域的覆盖范围，从而实现显色指数的提高，尤其重点研究了黄光发射的增加对白光OLED光源品质的影响。
Organic Light-Emitting Diodes (OLEDs) have been considered as nextgeneration full color displays and solid-state lighting sources, because of their highluminous efficiency, low driving voltage, fast response, wide visual angle, andflexible characteristics, etc. There still are some issues which need to be investigatedand improved in OLED. For the efficiency, the blue OLEDs are not as good as theirgreen and red counterparts, the phosphorescent OLEDs have serious efficiencyroll-off at high luminance. For the quality of lighting sources, the color renderingindex (CRI) of OLEDs needs to be improved further. In this thesis, based on theissues mentioned above, we develop fundamental and applicable research combiningOLEDs theory, electroluminescent mechanism and process. Some results have beenobtained as follows:
(1) The efficiency and lifetime of blue-light-emitting devices are usually not asgood as those of their green and red counterparts. Additionally, it is difficult togenerate high-performance pure/deep blue emission devices. These two reasonsindicate that the blue devices become the biggest impediment for the development ofwhite OLEDs. First, we assess a novel fluorescence dye named6,12-bis{[N-(3,4-dimethylphenyl)-N-(2,4,5-trimethylphenyl)]amino}chrysene(BmPAC) with emission peak of452nm. We fabricate blue OLED using BmPAC asemitter, the highest luminescence of12500cd/m~2is obtained, and the maximumcurrent efficiency reaches4.89cd/A at current density of23mA/cm~2. The emissionpeak of blue OLED is located at456nm, with CIE coordinates of (0.16,0.17). Thenwe combine orange dye with BmPAC to fabricate white OLED, with the emittinglayer (EML) structure of orange EML-interlayer-blue EML. The turn-on voltage forwhite OLED is4V, the maximum current efficiency and power efficiency are36.11cd/A and22.78lm/W at1300cd/m~2, and the current efficiency rolls off to34.59cd/A and35.61cd/A at100cd/m~2and1000cd/m~2, respectively. The spectra which are warm white lights, are almost stable with the increase of luminance. We only finda slight decrease of blue emission with the increasing brightness, and the highestCRI of45is obtained. We change the EML structure to be blue EML-interlayer-orange EML-interlayer-blue EML to improve the performance of white OLED. Theturn-on voltage is reduced to2.5V, the maximum current efficiency and powerefficiency are enhanced to40.9cd/A and49.4lm/W, respectively. The currentefficiency is37.3cd/A at100cd/m~2, or33.1cd/A at1000cd/m~2. Meanwhile a higherCRI of53is realized. We attribute the improvement to better balance of hole andelectron charges by using double blue EMLs. Finally, we demonstrate efficient blueorganic light-emitting diode with the EML structure of1,4-bis[N-(1-naphthyl)-N'-phenylamino]-4,4'-diamine/9,10-di(2-naphthyl)anthracene(ADN):1-4-di-[4-(N,N-di-phenyl)amino]styryl-benzene (DSA-ph). Improvedefficiencies and longer operational lifetime are obtained by co-doping astyrylamine-based deep blue dopant BD-3(0.1wt%) into the emitting layer of ADNdoped with DSA-ph compared to the case of non-co-doping. This is due to theimproved charge balance and expansion of exciton recombination zone. The bettercharge balance is obtained by reducing the electron mobility of ADN which is higherthan the hole mobility in the case of non-co-doping.
(2) Utilization of phosphorescent emitters may solve the problem of achievingefficient emissions. A large number of triplet excitons formed at high luminance cancause serious triplet-triplet annihilation, which results in roll-off phenomenon inphosphorescent OLEDs. Mixed host EML, double EMLs, and interlayer betweentwo adjacent EMLs structures are employed here to improve the roll-off problem,respectively. We employ Ir(ppy)3as green emitter for phosphorescent OLEDs. Formixed host EML structure device, the maximum current efficiency of26.23cd/A andthe maximum power efficiency of31.67lm/W are obtained respectively. For doubleEMLs structure device, the maximum current efficiency of29.14cd/A and themaximum power efficiency of22.29lm/W are obtained respectively. For interlayer between two adjacent EMLs structure device, the maximum current efficiency of50.38cd/A and the maximum power efficiency of29.29lm/W are obtainedrespectively. Compared with the other two methods, using interlayer can result in thehighest efficiency and slightest roll-off. Employing mixed host EML structure couldimprove the transport of carriers into EML and expand the recombination zone. Thenwe report successful fabrication of efficient and high-color-rendering phosphorescentwhite OLED by employing ultra-thin red emitter-spacer layer-ultra-thin greenemitter architecture. By fine-tuning the thicknesses of emitting layers and spacerlayer, we obtain white OLED with a high CRI of80and high luminance efficiencyof29.2cd/A which only rolls off to22.8cd/A at1000cd/m~2. A typical WOLED forcomparison exhibits a CRI below40and maximum luminance efficiency of15.8cd/A which decreases to11.4cd/A at1000cd/m~2. We attribute the improvement tothe island-like morphology generated by deposition of ultra-thin film. This allowssufficient space for exciton formation and possibility of minimizing triplet-tripletannihilation.
(3) High CRI is crucial for white OLED which can be applied in thehigh-quality lighting sources. We develop three types of white OLEDs with two-,three-and four-peak electroluminescence spectra. For two-peak OLED, a luminanceefficiency of34.59cd/A at100cd/m~2with a CRI of45and almost stable whiteemission with CIE coordinates around (0.47,0.42) are obtained. For three-peakOLED, highest CRI of88and correlated color temperature (CCT) below2800K atvarious brightness and a maximum luminance efficiency of27.29cd/A are realized.For four-peak OLED, color-temperature tunable white emission in the luminancerange of100cd/m~2to5000cd/m~2is obtained, the spectra turns from cold whiteemission to warm white emission with the change of luminance. Additionally, asunlight-like spectrum with a highest CRI of89is realized at5000cd/m~2. Wedemonstrate that to increase the number of emission wavebands could expand thecoverage area of visible light for the spectra of OLEDs, which results in higher CRI. Especially, we focus on the role of orange component on how to enhance the qualityof lighting source.
(1)在蓝色荧光OLED研究中，由于蓝光器件的效率相比绿光与红光器件较低，同时又缺乏深蓝光的材料，使得深蓝光器件成为OLED发展的最大阻碍。首先，对一种发射峰为452nm的新型蓝色荧光材料6,12-bis{[N-(3,4-dimethylphenyl)-N-(2,4,5-trimethylphenyl)]amino}chrysene(BmPAC)进行了初步研究。在以BmPAC为发光客体的OLED器件中，获得了最高发光亮度12500cd/m~2，在电流密度为23mA/cm~2的情况下获得了最大电流效率4.89cd/A，同时器件的电致发光峰为456nm，CIE坐标为(0.16,0.17)。然后将BmPAC与黄光染料搭配，制备了白光OLED。在发光层结构为黄光发光层-阻隔层-蓝光发光层的器件中，启亮电压为4V，在1300cd/m~2亮度下获得了最大电流效率36.11cd/A和最大功率效率22.78lm/W，电流效率在100cd/m~2和1000cd/m~2亮度下下降为34.59cd/A和35.61cd/A。随着亮度的增加，器件的发光光谱基本稳定，相对于黄光，蓝光的发射强度只有轻微的下降，器件的发光光谱为暖白光，最高显色指数为45。在发光层结构为蓝光发光层-阻隔层-黄光发光层-阻隔层-蓝光发光层的器件中，启亮电压降为2.5V，最大电流效率和最大功率效率分别提高到40.9cd/A和49.4lm/W，电流效率在100cd/m~2和1000cd/m~2亮度下下降为37.3cd/A和33.1cd/A，同时器件的最高显色指数提高至53。我们把这种改善归因于使用双蓝光发光层可以得到最好的载流子平衡。最后在9,10-di(2-naphthyl)anthracene (ADN):1-4-di-[4-(N,N-di-phenyl)amino]styryl-benzene (DSA-ph)的发光层中共掺入质量比为1%的深蓝光BD-3染料，通过与无共掺杂的器件相比，器件的发光效率和工作寿命都得到改善与提高，我们把这种提高归因于载流子平衡的改善和激子复合区域的扩宽。共掺杂方法使得ADN本来比空穴迁移率高的电子迁移率降低，从而得到更好的载流子平衡。
(2)在磷光OLED器件中，由于在高亮度下产生大量的三重态激子，会发生三重态-三重态激子淬灭，导致严重的效率滚降现象。首先分别使用双主体掺杂的发光层、双发光层、双主体掺杂的空间阻隔层三种方法研究对效率滚降的改善作用。以Ir(ppy)3为发光客体的绿色磷光OLED器件为研究对象，在使用双主体掺杂的发光层的器件中获得最大电流效率和功率效率分别为26.23cd/A和31.67lm/W，使用双发光层的器件中获得最大电流效率和功率效率分别为29.14cd/A和22.29lm/W，使用双主体掺杂的空间阻隔层的器件中获得最大的电流效率和功率效率分别为50.38cd/A和29.29lm/W。相对其它方法，使用空间阻隔层可以获得最高的发光效率和最轻微的效率滚降。双主体掺杂的空间阻隔层可以最大程度上实现促进载流子向发光层输运与扩宽激子的复合区域。然后研究了使用超薄发光层对磷光OLED的发光效率和效率滚降现象的改善作用。比较使用超薄发光层和普通厚度发光层的器件，通过仔细调节超薄发光层与阻隔层的厚度，我们获得了显色指数高达80的白光OLED，并且最高电流效率29.2cd/A在1000cd/m~2亮度下仅下降到22.8cd/A。而使用普通厚度发光层的器件最高显色指数不足40，最高电流效率只有15.8cd/A，在1000cd/m~2亮度下下降到11.4cd/A。我们把这种提高与改善归因于超薄发光层不仅可以促进载流子的注入与传输，而且超薄发光层中形成的岛状形貌可以为激子的复合提供足够大的空间，极大程度上减少了三重态-三重态激子之间的湮灭。
(3)高显色指数是白光OLED能够应用到高品质照明光源中的关键因素。我们研究了具有双波段、三波段、与四波段电致发光光谱的三种类型白光OLED。在双波段白光器件中获得了较为稳定的白光发射，CIE坐标在(0.47,0.42)附近，最高显色指数为45，同时器件在100cd/m~2亮度下的电流效率为34.59cd/A。对于三波段的白光OLED，最大电流效率为27.29cd/A，最高显色指数为88，在所有亮度下色温低于2800K。对于四波段的白光OLED，在亮度从100cd/m~2变化到5000cd/m~2的过程中，发光光谱从冷白光变化至暖白光，实现了色温可调，并且在5000cd/m~2的亮度下获得了显色指数为89的类太阳光光谱。我们证明了增加发光峰的数目可以扩大发光光谱在可见光区域的覆盖范围，从而实现显色指数的提高，尤其重点研究了黄光发射的增加对白光OLED光源品质的影响。
Organic Light-Emitting Diodes (OLEDs) have been considered as nextgeneration full color displays and solid-state lighting sources, because of their highluminous efficiency, low driving voltage, fast response, wide visual angle, andflexible characteristics, etc. There still are some issues which need to be investigatedand improved in OLED. For the efficiency, the blue OLEDs are not as good as theirgreen and red counterparts, the phosphorescent OLEDs have serious efficiencyroll-off at high luminance. For the quality of lighting sources, the color renderingindex (CRI) of OLEDs needs to be improved further. In this thesis, based on theissues mentioned above, we develop fundamental and applicable research combiningOLEDs theory, electroluminescent mechanism and process. Some results have beenobtained as follows:
(1) The efficiency and lifetime of blue-light-emitting devices are usually not asgood as those of their green and red counterparts. Additionally, it is difficult togenerate high-performance pure/deep blue emission devices. These two reasonsindicate that the blue devices become the biggest impediment for the development ofwhite OLEDs. First, we assess a novel fluorescence dye named6,12-bis{[N-(3,4-dimethylphenyl)-N-(2,4,5-trimethylphenyl)]amino}chrysene(BmPAC) with emission peak of452nm. We fabricate blue OLED using BmPAC asemitter, the highest luminescence of12500cd/m~2is obtained, and the maximumcurrent efficiency reaches4.89cd/A at current density of23mA/cm~2. The emissionpeak of blue OLED is located at456nm, with CIE coordinates of (0.16,0.17). Thenwe combine orange dye with BmPAC to fabricate white OLED, with the emittinglayer (EML) structure of orange EML-interlayer-blue EML. The turn-on voltage forwhite OLED is4V, the maximum current efficiency and power efficiency are36.11cd/A and22.78lm/W at1300cd/m~2, and the current efficiency rolls off to34.59cd/A and35.61cd/A at100cd/m~2and1000cd/m~2, respectively. The spectra which are warm white lights, are almost stable with the increase of luminance. We only finda slight decrease of blue emission with the increasing brightness, and the highestCRI of45is obtained. We change the EML structure to be blue EML-interlayer-orange EML-interlayer-blue EML to improve the performance of white OLED. Theturn-on voltage is reduced to2.5V, the maximum current efficiency and powerefficiency are enhanced to40.9cd/A and49.4lm/W, respectively. The currentefficiency is37.3cd/A at100cd/m~2, or33.1cd/A at1000cd/m~2. Meanwhile a higherCRI of53is realized. We attribute the improvement to better balance of hole andelectron charges by using double blue EMLs. Finally, we demonstrate efficient blueorganic light-emitting diode with the EML structure of1,4-bis[N-(1-naphthyl)-N'-phenylamino]-4,4'-diamine/9,10-di(2-naphthyl)anthracene(ADN):1-4-di-[4-(N,N-di-phenyl)amino]styryl-benzene (DSA-ph). Improvedefficiencies and longer operational lifetime are obtained by co-doping astyrylamine-based deep blue dopant BD-3(0.1wt%) into the emitting layer of ADNdoped with DSA-ph compared to the case of non-co-doping. This is due to theimproved charge balance and expansion of exciton recombination zone. The bettercharge balance is obtained by reducing the electron mobility of ADN which is higherthan the hole mobility in the case of non-co-doping.
(2) Utilization of phosphorescent emitters may solve the problem of achievingefficient emissions. A large number of triplet excitons formed at high luminance cancause serious triplet-triplet annihilation, which results in roll-off phenomenon inphosphorescent OLEDs. Mixed host EML, double EMLs, and interlayer betweentwo adjacent EMLs structures are employed here to improve the roll-off problem,respectively. We employ Ir(ppy)3as green emitter for phosphorescent OLEDs. Formixed host EML structure device, the maximum current efficiency of26.23cd/A andthe maximum power efficiency of31.67lm/W are obtained respectively. For doubleEMLs structure device, the maximum current efficiency of29.14cd/A and themaximum power efficiency of22.29lm/W are obtained respectively. For interlayer between two adjacent EMLs structure device, the maximum current efficiency of50.38cd/A and the maximum power efficiency of29.29lm/W are obtainedrespectively. Compared with the other two methods, using interlayer can result in thehighest efficiency and slightest roll-off. Employing mixed host EML structure couldimprove the transport of carriers into EML and expand the recombination zone. Thenwe report successful fabrication of efficient and high-color-rendering phosphorescentwhite OLED by employing ultra-thin red emitter-spacer layer-ultra-thin greenemitter architecture. By fine-tuning the thicknesses of emitting layers and spacerlayer, we obtain white OLED with a high CRI of80and high luminance efficiencyof29.2cd/A which only rolls off to22.8cd/A at1000cd/m~2. A typical WOLED forcomparison exhibits a CRI below40and maximum luminance efficiency of15.8cd/A which decreases to11.4cd/A at1000cd/m~2. We attribute the improvement tothe island-like morphology generated by deposition of ultra-thin film. This allowssufficient space for exciton formation and possibility of minimizing triplet-tripletannihilation.
(3) High CRI is crucial for white OLED which can be applied in thehigh-quality lighting sources. We develop three types of white OLEDs with two-,three-and four-peak electroluminescence spectra. For two-peak OLED, a luminanceefficiency of34.59cd/A at100cd/m~2with a CRI of45and almost stable whiteemission with CIE coordinates around (0.47,0.42) are obtained. For three-peakOLED, highest CRI of88and correlated color temperature (CCT) below2800K atvarious brightness and a maximum luminance efficiency of27.29cd/A are realized.For four-peak OLED, color-temperature tunable white emission in the luminancerange of100cd/m~2to5000cd/m~2is obtained, the spectra turns from cold whiteemission to warm white emission with the change of luminance. Additionally, asunlight-like spectrum with a highest CRI of89is realized at5000cd/m~2. Wedemonstrate that to increase the number of emission wavebands could expand thecoverage area of visible light for the spectra of OLEDs, which results in higher CRI. Especially, we focus on the role of orange component on how to enhance the qualityof lighting source.
引文
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