有机电致荧光、磷光器件的性能优化与OLED封装技术的研究
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摘要
有机电致发光器件具有自发光、响应快、全固态、制备工艺简单、高效率、宽视角、超薄、耐高低温、柔性等优点，被誉为第三代显示技术。但是，目前OLED的制造成本高、发光效率需进一步地提高、物理机理认识的不足，这严重地影响了OLEDs器件的在显示领域的应用步伐，针对上述问题，本论文在红光荧光器件的制备工艺和新型磷光发光器件制备及器件封装方面进行了一系列的探索性和创新性的工作，具体包括：
1．采用正交实验法，深入细致的考察制备基于DCJTB红光OLED器件的五个主要参数包括HTL厚度、EML厚度、ETL厚度、DCJTB掺杂浓度、Rubrene掺杂浓度对OLED的亮度、效率等特性的影响。用Keithly2400、PR650及光具座搭建的测试平台测试了OLED的I～V、V～B性能，同时评价了OLED的V～η特性，优化出的红光OLED的最优结构参数是：HTL厚度为40nm、EML厚度为40nm、ETL厚度为20nm、DCJTB掺杂浓度为1 wt％、Rubrene掺杂浓度为30、vt％。按优化的参数制备出的红光OLED器件，当外加电压23.5V时，器件的亮度达到了8650cd／m~2，最高电流效率为2.58cd／A，对应的电压为6.8V。
2．分析了磷光发光材料相对荧光材料的优势，进而详细叙述了磷光材料掺杂与荧光材料掺杂在能量转移方面原理上的不同，即F(o|¨)rster理论和Dexter理论。合成了六种新型铱金属配合物磷光材料，将其中的两种材料用于多层磷光器件的制备，优化了器件发光层的层厚和掺杂浓度，制备出了高性能的磷光器件。
3．给出了一种是具有强的空间位阻效应的新型铂金属配合物磷光材料(ppy)pt(bcam)，该材料的发光光谱的主峰为624nm，为橙红色的光；设计了勿需掺杂的发光层器件结构，简化了磷光器件的制备工艺，为磷光OLED器件的大生产提供了思路，这也是本论文创新点之一。
4．分析了OLED器件失效的原因，提出了OLED器件失效的电解池模型，介绍了三种封装技术(常规盖板封装、真空封装及多层薄膜封装)，其中，真空封装技术是我们自行提出的方案。我们采用了典型结构的OLED器件(ITO／CuPc／NPB／Alq_3／LiF／Al)进行寿命实验，分别采用三种封装技术对其进行了实际封装。并选择了钙膜腐蚀法来验证与比较三种封装技术的实际效果，得出了理想的封装方案。
Organic light-emitting diodes (OLEDs) possess many advantages, such asself-emission, fast response, full solid device, easy fabrication, high efficiency, wideview-angle, super-thin thickness. OLEDs are considered as the most ideal and potentialdisplay technology in 21~(st) century. However, currently there are also some shortcomingsto prevent it from large scale commercial application such as high fabrication cost, lowlumiance efficiency and indistinct understanding about device mechanism. Aiming atthose problems, some basic and systematic works have been performed to focus on thefabrication process to obtain high performance red fluorescent OLED device and highefficiency phosphorescent OLEDs in this work. The encapsulation technology of OLEDis also studied.
1. The red fluorsecent OLED based on DCJTB was fabricated. There are fiveparameters affecting the properties of fluoresecent OLED and orthogonal test tableL_(16((4~5) was used to carried out the systematic study. The parameters includes: Thethickness of HTL, thickness of EML, thickness of ETL, doped concentration of DCJTB,doped concentration of Rubrene. The optimum structure for the OLED devices isITO/HIL(50nm)/HTL(40nm)/EML(40nm)/ETL(20nm)/LiF(1nm)/Al(100nm), the dopedconcentration of DCJTB & Rubrene are 1 wt%, 30 wt%, respectively. The luminance(L)-current density (J)-bias voltage (V) characteristics were recorded simultaneouslywith the measurement of a PR650 spectroscan spectrometer by combining thespectrometer with a Keithley 2400 programmable voltage-current source. Thebrightness of OLED prepared with parameters mentioned above is 8650cd/m~2 under thevoltage of 23.5v, and relative efficiency is 2.58 cd/A @ 6.8v.
2. The advantage of organic electro-phosphorescent materials is discussedcomparing with that of organic fluorescent materials. And the differences of energytransferring mechanism in the doping status between the organic electro-phosphorescentmaterials and organic fluorescent materials are also introduced. They are the theories ofF(o|¨)rster energy transfer and Dexter energy transfer. Novel six kinds of phosphorescent materials have been designed and synthesized based Ir. two kinds of phosphorescentmaterials are choosed and relative multilayer devices are fabricated. The thickness ofEML and doping concentration of phosphorescent OLED were optimized. At the sametime the high efficiency phosphorescent OLED was fabricated.
3. a novel phosphorescent OLEDs with pure phosphorescent materials as theemitting layer based on new materials platinum(Ⅱ) (2-phenylpyridinato-N,C2)(3-benzoyl-camphor) [(ppy)pt(bcam)] with red light emission is demonstrated. Becausethe molecular structure of this kind of phosphorescent materials has the3-benzoyl-camphor group with strong steric hindrance effect. It enormously simplifiesthe fabrication processes. The methods can be adapted to the mass production ofphosphorescent OLED; it is the one of novel idea in this dissertation.
4. The reasons of the OLED degradation were discussed, and the electrolytic cellmodel to explain the OLED degration is proposed. The three kinds of encapsulationtechnologies are also introduced; they are conventional encapsulation with backplane,vacuum encapsulation with backplane and multi-layer thin film encapsulation; amongthem, the vacuum encapsulation with backplane technology was proposed by us. OLEDdevice of classical structure with ITO/CuPc/NPB/Alq_3/LiF/Al, which was used to studyOLED degradation, is adopted. The OLED devices with three encapsulation methodshave been encapsulated, respectively. The calcium film etching method is choosed tostudy the results of three encapsulations. A good scheme through experimental testresult is obtained.
1．采用正交实验法，深入细致的考察制备基于DCJTB红光OLED器件的五个主要参数包括HTL厚度、EML厚度、ETL厚度、DCJTB掺杂浓度、Rubrene掺杂浓度对OLED的亮度、效率等特性的影响。用Keithly2400、PR650及光具座搭建的测试平台测试了OLED的I～V、V～B性能，同时评价了OLED的V～η特性，优化出的红光OLED的最优结构参数是：HTL厚度为40nm、EML厚度为40nm、ETL厚度为20nm、DCJTB掺杂浓度为1 wt％、Rubrene掺杂浓度为30、vt％。按优化的参数制备出的红光OLED器件，当外加电压23.5V时，器件的亮度达到了8650cd／m~2，最高电流效率为2.58cd／A，对应的电压为6.8V。
2．分析了磷光发光材料相对荧光材料的优势，进而详细叙述了磷光材料掺杂与荧光材料掺杂在能量转移方面原理上的不同，即F(o|¨)rster理论和Dexter理论。合成了六种新型铱金属配合物磷光材料，将其中的两种材料用于多层磷光器件的制备，优化了器件发光层的层厚和掺杂浓度，制备出了高性能的磷光器件。
3．给出了一种是具有强的空间位阻效应的新型铂金属配合物磷光材料(ppy)pt(bcam)，该材料的发光光谱的主峰为624nm，为橙红色的光；设计了勿需掺杂的发光层器件结构，简化了磷光器件的制备工艺，为磷光OLED器件的大生产提供了思路，这也是本论文创新点之一。
4．分析了OLED器件失效的原因，提出了OLED器件失效的电解池模型，介绍了三种封装技术(常规盖板封装、真空封装及多层薄膜封装)，其中，真空封装技术是我们自行提出的方案。我们采用了典型结构的OLED器件(ITO／CuPc／NPB／Alq_3／LiF／Al)进行寿命实验，分别采用三种封装技术对其进行了实际封装。并选择了钙膜腐蚀法来验证与比较三种封装技术的实际效果，得出了理想的封装方案。
Organic light-emitting diodes (OLEDs) possess many advantages, such asself-emission, fast response, full solid device, easy fabrication, high efficiency, wideview-angle, super-thin thickness. OLEDs are considered as the most ideal and potentialdisplay technology in 21~(st) century. However, currently there are also some shortcomingsto prevent it from large scale commercial application such as high fabrication cost, lowlumiance efficiency and indistinct understanding about device mechanism. Aiming atthose problems, some basic and systematic works have been performed to focus on thefabrication process to obtain high performance red fluorescent OLED device and highefficiency phosphorescent OLEDs in this work. The encapsulation technology of OLEDis also studied.
1. The red fluorsecent OLED based on DCJTB was fabricated. There are fiveparameters affecting the properties of fluoresecent OLED and orthogonal test tableL_(16((4~5) was used to carried out the systematic study. The parameters includes: Thethickness of HTL, thickness of EML, thickness of ETL, doped concentration of DCJTB,doped concentration of Rubrene. The optimum structure for the OLED devices isITO/HIL(50nm)/HTL(40nm)/EML(40nm)/ETL(20nm)/LiF(1nm)/Al(100nm), the dopedconcentration of DCJTB & Rubrene are 1 wt%, 30 wt%, respectively. The luminance(L)-current density (J)-bias voltage (V) characteristics were recorded simultaneouslywith the measurement of a PR650 spectroscan spectrometer by combining thespectrometer with a Keithley 2400 programmable voltage-current source. Thebrightness of OLED prepared with parameters mentioned above is 8650cd/m~2 under thevoltage of 23.5v, and relative efficiency is 2.58 cd/A @ 6.8v.
2. The advantage of organic electro-phosphorescent materials is discussedcomparing with that of organic fluorescent materials. And the differences of energytransferring mechanism in the doping status between the organic electro-phosphorescentmaterials and organic fluorescent materials are also introduced. They are the theories ofF(o|¨)rster energy transfer and Dexter energy transfer. Novel six kinds of phosphorescent materials have been designed and synthesized based Ir. two kinds of phosphorescentmaterials are choosed and relative multilayer devices are fabricated. The thickness ofEML and doping concentration of phosphorescent OLED were optimized. At the sametime the high efficiency phosphorescent OLED was fabricated.
3. a novel phosphorescent OLEDs with pure phosphorescent materials as theemitting layer based on new materials platinum(Ⅱ) (2-phenylpyridinato-N,C2)(3-benzoyl-camphor) [(ppy)pt(bcam)] with red light emission is demonstrated. Becausethe molecular structure of this kind of phosphorescent materials has the3-benzoyl-camphor group with strong steric hindrance effect. It enormously simplifiesthe fabrication processes. The methods can be adapted to the mass production ofphosphorescent OLED; it is the one of novel idea in this dissertation.
4. The reasons of the OLED degradation were discussed, and the electrolytic cellmodel to explain the OLED degration is proposed. The three kinds of encapsulationtechnologies are also introduced; they are conventional encapsulation with backplane,vacuum encapsulation with backplane and multi-layer thin film encapsulation; amongthem, the vacuum encapsulation with backplane technology was proposed by us. OLEDdevice of classical structure with ITO/CuPc/NPB/Alq_3/LiF/Al, which was used to studyOLED degradation, is adopted. The OLED devices with three encapsulation methodshave been encapsulated, respectively. The calcium film etching method is choosed tostudy the results of three encapsulations. A good scheme through experimental testresult is obtained.
引文
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