高性能荧光/磷光混合式白光聚合物电致发光二极管的研究
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摘要
白光聚合物电致发光二极管(PLED)由于其在全彩显示和照明领域巨大的潜在应用价值，特别是其可以采用工艺简单、成本低廉的溶液加工成膜技术，聚合物发光材料的分子结构与发光颜色便于调节等优势，吸引了学术界和工业界广泛的研究兴趣，已经成为有机光电领域的一个研究热点，被誉为新一代固体照明光源。
目前，白光PLED的发光性能与基于真空蒸镀成膜技术的有机小分子电致发光二极管（OLED）相比仍然有一定的差距，主要包括发光效率、光谱稳定性和器件应用寿命等方面。因此，如要获得实际的应用，白光PLED发光性能还需要进一步提高。一般地，要想实现高效率的白光PLED，必须要充分利用发光材料的单线态和三线态激子的发光，器件的理论内量子效率达到100%。目前，高效的磷光小分子发光材料是研究的最多的材料体系之一，并且基于全磷光发射的白光PLED也实现了较高的发光效率。磷光PLED一般都是采用主客体掺杂体系结构，其发光性能一方面依赖于新型的主体和磷光客体材料的开发，另一方面需要对器件结构进行优化设计。对于主体材料，一般认为其三线态能级需要高于客体材料，同时需要具有高效、平衡的双载流子传输性能，所以开发宽带隙、双极性的主体材料是一个热点研究方向，但同时宽带隙的材料又存在合成困难和性质不稳定等缺点。鉴于此，本论文的主要研究目的就是通过采用不同聚合物主体材料和对器件结构进行优化设计，实现高性能的白光聚合物发光器件。
本论文中我们用到的主体材料有非共轭聚合物PVK、聚芴及其衍生物。PVK由于具有较高的三线态能级、良好的成膜特性、较高的玻璃转化温度和良好的空穴传输特性，是目前最常用的主体材料。目前基于PVK为主体的全磷光白光PLED的发光效率已经超过了60cd/A，功率效率达到40lm/W。聚芴类的材料由于其具有高效率、色纯度好的蓝光发射、高电荷迁移率和良好的成膜性等，在显示应用领域是一种很有吸引力的共轭聚合物。但是，以聚芴类聚合物为主体的掺杂型磷光PLED的效率普遍较低，一般认为是主体较低的三线态能级对磷光的淬灭作用。我们采用聚芴及其衍生物作为主体材料，同时在PEDOT:PSS和发光层之间引入PVK阳极缓冲层，有效地抑制了低三线态能级的聚芴类材料对磷光的淬灭，制备了一系列高性能的全磷光、荧光和磷光混合式的双层结构白光器件。这些结果大大拓宽了主体材料的选择范围，对磷光发光器件的研究具有重要意义。特别的，我们降低磷光客体材料的掺杂浓度，通过主客体间的不完全能量转移而突出了聚合物主体的深蓝光发射，填补了全磷光白光器件中深蓝光的空白，有效地拓宽了白光的发射光谱，实现了高效率、高颜色质量的白光PLED。优化后的器件最大的电流效率和功率效率分别为21.4cd/A和15.2lm/W，白光显色指数高达90。带有氨基基团的水/醇溶性的聚芴共聚物或其衍生物（如PFN）是一类具有高效电子注入特性的共轭聚合物，它可以与高功函数金属（如铝、金、银等）一起构成双层结构的阴极，器件发光效率远高于以高功函数金属为阴极器件，接近甚至超过以低功函数金属（如钡、钙等）为阴极的器件。同时，其特殊的溶解特性有助于多层结构的PLED的实现。基于PFN主体的白光PLED，其制备工艺相对简单，阴极金属采用的是相对稳定的高功函数Al，使得其在空气中具有较好的稳定性。但是其功耗较高，导致启亮电压较高，发光功率效率较低，同时发光亮度较低，成为了其在实际应用中最大的障碍。
最后，我们利用水/醇溶性共轭聚合物材料作为电子传输层，与高功函数金属Al和金属氧化物MoO3一起构成一种新型的电荷产生层（CGL），并将其成功的应用于串联式发光器件中，实现了含有两个发光单元的串联式聚合物单色光和白光发光器件。当采用带有氨基的聚芴共聚物PFN作为电子注入/传输层，Al膜厚度为5nm，MoO3厚度为10nm，绿光材料P-PPV为上下两个发光单元的发光材料时，实现了基于溶液旋涂方法的双发光单元的串联式聚合物单色发光器件，器件最大电流效率为16.65cd/A。对于串联式白光器件，我们采用PF-EP/Al (5nm)/MoO3(10nm)作为中间电荷产生层，同时基于溶液湿法处理的蓝、红光聚合物材料PFSO、PFO-DBT15作为底层器件的发光材料，而上层器件中的绿光小分子材料Alq3则采用真空蒸镀的方法，通过上下两层发光单元的颜色叠加得到白光发射。串联式白光器件的最大电流效率为7.16cd/A，最大功率效率为1.95lm/W，启亮电压为8.75V，约为上下两层器件启亮电压之和。同时，白光器件的CIE色坐标为(0.340,0.373)，其显色指数高达97，接近于白炽灯的100。
White polymer light-emitting devices (WPLEDs) have attracted intense attentionin both scientific and industrial communities due to their potential applications infull-color flat-panel displays and solid-state lighting sources, given their uniqueadvantages, such as ease of fabrication, low-cost manufacturing usingsolution-processed technology, and tunable molecule structure and emission color.Therefore, WPLEDs have become a hot research topic in the field of organicelectronics, and represent promising candidate for the next-generation of solid-statelighting sources.
On the other side, the performance of WPLEDs is much lower than that of theorganic light-emitting devices (OLEDs) based on vapor-deposition technology so far,mainly in terms of efficiencies. Therefore, it is an urgent task to improve theperformance of WPLEDs in order to meet practical applications. By harvesting bothsinglet and triplet excitons, it can allow an internal quantum efficiency approach100%.Currently, due to their high efficiency, phosphorescent emitters based on smallmolecule have received intense research interest, while the most efficient WPLEDscritically rely on these phosphorescent materials. For PLEDs based on phosphorescentemitters, host-guest doping system is usually employed, rendering the deviceperformance not only depends on the development of the host and the phosphorescentguest materials, but is also related to their device structure. For the host material, itstriplet energy level should be higher than that of guest in order to avoid triplet energyback transfer from the phosphor to the polymer host, and possess efficient andbalanced carriers transporting properties. Therefore, many researches have beenfocused on the development of host materials with wide band gap and bipolartransporting properties. However, the synthesis of materials with wide band gap is notso easy and the materials are very unstable. Herein, the purpose of this study is toinvestigate and realize efficient WPLEDs from different host materials and noveldevice structures.
The host materials used in this study including non-conjugated polymerpoly(N-vinylcarbazole)(PVK), polyfluorene and its derivatives (PFs). PVK is widelyemployed as host material due to its higher triplet energy states, good film-formingproperties, higher glass transition temperature and good hole transporting property. At present, the luminous efficiency (LE) of WPLEDs based on PVK host had exceed60cd/A, and power efficiency (PE) reached40lm/W. Polyfluorene is also an attractiveconjugated material due to its efficient, good color purity of blue emission as well asgood film-forming properties. However, its lower-lying triplet energy states canseverely quench the phosphorescent emission from the triplet guest. Here, wedemonstrate that the quench effect can be effectively suppressed by incorporating ananode buffer layer PVK between PEDOT: PSS and emitting layer. On the basis of this,a series of all-phosphorescent, hybrid (with both fluorescent and phosphorescentemission) WPLEDs based on PFs host were realized. These results broaden the rangeof options of host materials for WPLEDs and have vital significance tophosphorescent PLEDs. In particularly, when using deep blue emitting emitter as host,it can greatly broaden the white emission spectra, thus, WPLEDs with high efficiencyand good color quality can be readily achieved. When incorporating water/alcohol-soluble polyfluorene copolymers or derivatives with amino group (PFN) as electroninjection layer, devices efficiency can be further enhanced. The LE and PE of theoptimized WPLEDs reached21.4cd/A and15.2lm/W, respectively. Moreover, thecolor rendering index (CRI) was as high as90. In addition, when this type ofcopolymer is used as host, air-stable metal such as Al, Ag can be used as contactcathode, despite its higher turn-on voltage (Von).
Finally, we also investigate the realization of stacked PLED by using a newcharge generation layer (CGL) which comprising water/alcohol-soluble conjugatedpolymer, metal Al and metal oxide MoO3. By using PFN/Al/MoO3CGL and emittingmaterial P-PPV, solution-processed stacked monochromatic PLEDs with emissionfrom two sub-units are fabricated, and the peak LE reached16.65cd/A. By using red,green, blue emitting materials PFO-DBT15, Alq3and PFSO, stacked whitelight-emitting devices were also fabricated with a PF-EP/Al/MoO3CGL. Themaximum LE reaches7.16cd/A, with a maximal PE of1.95lm/W. The Vonis foundto be8.75V, which is approximately the sum of that of sub-units. Moreover, the CIEcoordinates of white emission is (0.340,0.373), with a CRI of97, very close to that ofincandescent lamp of100.
目前，白光PLED的发光性能与基于真空蒸镀成膜技术的有机小分子电致发光二极管（OLED）相比仍然有一定的差距，主要包括发光效率、光谱稳定性和器件应用寿命等方面。因此，如要获得实际的应用，白光PLED发光性能还需要进一步提高。一般地，要想实现高效率的白光PLED，必须要充分利用发光材料的单线态和三线态激子的发光，器件的理论内量子效率达到100%。目前，高效的磷光小分子发光材料是研究的最多的材料体系之一，并且基于全磷光发射的白光PLED也实现了较高的发光效率。磷光PLED一般都是采用主客体掺杂体系结构，其发光性能一方面依赖于新型的主体和磷光客体材料的开发，另一方面需要对器件结构进行优化设计。对于主体材料，一般认为其三线态能级需要高于客体材料，同时需要具有高效、平衡的双载流子传输性能，所以开发宽带隙、双极性的主体材料是一个热点研究方向，但同时宽带隙的材料又存在合成困难和性质不稳定等缺点。鉴于此，本论文的主要研究目的就是通过采用不同聚合物主体材料和对器件结构进行优化设计，实现高性能的白光聚合物发光器件。
本论文中我们用到的主体材料有非共轭聚合物PVK、聚芴及其衍生物。PVK由于具有较高的三线态能级、良好的成膜特性、较高的玻璃转化温度和良好的空穴传输特性，是目前最常用的主体材料。目前基于PVK为主体的全磷光白光PLED的发光效率已经超过了60cd/A，功率效率达到40lm/W。聚芴类的材料由于其具有高效率、色纯度好的蓝光发射、高电荷迁移率和良好的成膜性等，在显示应用领域是一种很有吸引力的共轭聚合物。但是，以聚芴类聚合物为主体的掺杂型磷光PLED的效率普遍较低，一般认为是主体较低的三线态能级对磷光的淬灭作用。我们采用聚芴及其衍生物作为主体材料，同时在PEDOT:PSS和发光层之间引入PVK阳极缓冲层，有效地抑制了低三线态能级的聚芴类材料对磷光的淬灭，制备了一系列高性能的全磷光、荧光和磷光混合式的双层结构白光器件。这些结果大大拓宽了主体材料的选择范围，对磷光发光器件的研究具有重要意义。特别的，我们降低磷光客体材料的掺杂浓度，通过主客体间的不完全能量转移而突出了聚合物主体的深蓝光发射，填补了全磷光白光器件中深蓝光的空白，有效地拓宽了白光的发射光谱，实现了高效率、高颜色质量的白光PLED。优化后的器件最大的电流效率和功率效率分别为21.4cd/A和15.2lm/W，白光显色指数高达90。带有氨基基团的水/醇溶性的聚芴共聚物或其衍生物（如PFN）是一类具有高效电子注入特性的共轭聚合物，它可以与高功函数金属（如铝、金、银等）一起构成双层结构的阴极，器件发光效率远高于以高功函数金属为阴极器件，接近甚至超过以低功函数金属（如钡、钙等）为阴极的器件。同时，其特殊的溶解特性有助于多层结构的PLED的实现。基于PFN主体的白光PLED，其制备工艺相对简单，阴极金属采用的是相对稳定的高功函数Al，使得其在空气中具有较好的稳定性。但是其功耗较高，导致启亮电压较高，发光功率效率较低，同时发光亮度较低，成为了其在实际应用中最大的障碍。
最后，我们利用水/醇溶性共轭聚合物材料作为电子传输层，与高功函数金属Al和金属氧化物MoO3一起构成一种新型的电荷产生层（CGL），并将其成功的应用于串联式发光器件中，实现了含有两个发光单元的串联式聚合物单色光和白光发光器件。当采用带有氨基的聚芴共聚物PFN作为电子注入/传输层，Al膜厚度为5nm，MoO3厚度为10nm，绿光材料P-PPV为上下两个发光单元的发光材料时，实现了基于溶液旋涂方法的双发光单元的串联式聚合物单色发光器件，器件最大电流效率为16.65cd/A。对于串联式白光器件，我们采用PF-EP/Al (5nm)/MoO3(10nm)作为中间电荷产生层，同时基于溶液湿法处理的蓝、红光聚合物材料PFSO、PFO-DBT15作为底层器件的发光材料，而上层器件中的绿光小分子材料Alq3则采用真空蒸镀的方法，通过上下两层发光单元的颜色叠加得到白光发射。串联式白光器件的最大电流效率为7.16cd/A，最大功率效率为1.95lm/W，启亮电压为8.75V，约为上下两层器件启亮电压之和。同时，白光器件的CIE色坐标为(0.340,0.373)，其显色指数高达97，接近于白炽灯的100。
White polymer light-emitting devices (WPLEDs) have attracted intense attentionin both scientific and industrial communities due to their potential applications infull-color flat-panel displays and solid-state lighting sources, given their uniqueadvantages, such as ease of fabrication, low-cost manufacturing usingsolution-processed technology, and tunable molecule structure and emission color.Therefore, WPLEDs have become a hot research topic in the field of organicelectronics, and represent promising candidate for the next-generation of solid-statelighting sources.
On the other side, the performance of WPLEDs is much lower than that of theorganic light-emitting devices (OLEDs) based on vapor-deposition technology so far,mainly in terms of efficiencies. Therefore, it is an urgent task to improve theperformance of WPLEDs in order to meet practical applications. By harvesting bothsinglet and triplet excitons, it can allow an internal quantum efficiency approach100%.Currently, due to their high efficiency, phosphorescent emitters based on smallmolecule have received intense research interest, while the most efficient WPLEDscritically rely on these phosphorescent materials. For PLEDs based on phosphorescentemitters, host-guest doping system is usually employed, rendering the deviceperformance not only depends on the development of the host and the phosphorescentguest materials, but is also related to their device structure. For the host material, itstriplet energy level should be higher than that of guest in order to avoid triplet energyback transfer from the phosphor to the polymer host, and possess efficient andbalanced carriers transporting properties. Therefore, many researches have beenfocused on the development of host materials with wide band gap and bipolartransporting properties. However, the synthesis of materials with wide band gap is notso easy and the materials are very unstable. Herein, the purpose of this study is toinvestigate and realize efficient WPLEDs from different host materials and noveldevice structures.
The host materials used in this study including non-conjugated polymerpoly(N-vinylcarbazole)(PVK), polyfluorene and its derivatives (PFs). PVK is widelyemployed as host material due to its higher triplet energy states, good film-formingproperties, higher glass transition temperature and good hole transporting property. At present, the luminous efficiency (LE) of WPLEDs based on PVK host had exceed60cd/A, and power efficiency (PE) reached40lm/W. Polyfluorene is also an attractiveconjugated material due to its efficient, good color purity of blue emission as well asgood film-forming properties. However, its lower-lying triplet energy states canseverely quench the phosphorescent emission from the triplet guest. Here, wedemonstrate that the quench effect can be effectively suppressed by incorporating ananode buffer layer PVK between PEDOT: PSS and emitting layer. On the basis of this,a series of all-phosphorescent, hybrid (with both fluorescent and phosphorescentemission) WPLEDs based on PFs host were realized. These results broaden the rangeof options of host materials for WPLEDs and have vital significance tophosphorescent PLEDs. In particularly, when using deep blue emitting emitter as host,it can greatly broaden the white emission spectra, thus, WPLEDs with high efficiencyand good color quality can be readily achieved. When incorporating water/alcohol-soluble polyfluorene copolymers or derivatives with amino group (PFN) as electroninjection layer, devices efficiency can be further enhanced. The LE and PE of theoptimized WPLEDs reached21.4cd/A and15.2lm/W, respectively. Moreover, thecolor rendering index (CRI) was as high as90. In addition, when this type ofcopolymer is used as host, air-stable metal such as Al, Ag can be used as contactcathode, despite its higher turn-on voltage (Von).
Finally, we also investigate the realization of stacked PLED by using a newcharge generation layer (CGL) which comprising water/alcohol-soluble conjugatedpolymer, metal Al and metal oxide MoO3. By using PFN/Al/MoO3CGL and emittingmaterial P-PPV, solution-processed stacked monochromatic PLEDs with emissionfrom two sub-units are fabricated, and the peak LE reached16.65cd/A. By using red,green, blue emitting materials PFO-DBT15, Alq3and PFSO, stacked whitelight-emitting devices were also fabricated with a PF-EP/Al/MoO3CGL. Themaximum LE reaches7.16cd/A, with a maximal PE of1.95lm/W. The Vonis foundto be8.75V, which is approximately the sum of that of sub-units. Moreover, the CIEcoordinates of white emission is (0.340,0.373), with a CRI of97, very close to that ofincandescent lamp of100.
引文
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