Research Progress on the Formation Mechanism and Prevention of Black Spot in Organic Light-Emitting Devices
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摘要:
有机电致发光器件（OLEDs）由于具有主动发光、响应速度快、视角宽、且与柔性电子兼容等优秀特性而在显示行业广受关注，然而由于器件对水氧非常敏感，一旦跟水氧接触就会失效，其中黑点的形成是影响器件成品率的一大原因。相关研究提出了几种黑点形成机制但并没有特定模型，此外，黑点形成相对模糊且不可预测。为了减少和防止黑点的形成，本文总结了黑点的形成原因，讨论了黑点的形成机制，并给出了黑点预防措施。
Abstract:Organic light-emitting devices (OLEDs) have attracted wide attention in the display industry owing to their excellent characteristics, such as active luminescence, fast response time, wide viewing angle, and compatibility with flexible electronics. Nevertheless, organic luminescent materials are vulnerable to environmental moisture and oxygen, and they fail once they come in contact with water and oxygen. The formation of black spots is one of the main factors affecting the product yields of these devices. Relevant studies have proposed several mechanisms for the formation of black spots; however, there is no specific model. In addition, current models of the formation of black spots are relatively vague and unpredictable. To reduce and prevent the formation of black spots, this study summarizes the causes of black spot formation, discusses the formation mechanism of black spots, and provides preventive measures.
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图 1 OLEDs中的颗粒与针孔：(a) 未刺破膜层的外部颗粒和灰尘[12]；(b) 膜层中尖刺和针孔[12]；(c) 已刺破膜层的有机颗粒[13-14]；(d) 已刺破膜层的外来颗粒[13-14]
Figure 1. Particles and pinholes in OLEDs: (a) External particles and dust that have not punctured the film[12]; (b) Spikes and pinholes in the membrane[12]; (c) Organic particles that have punctured the membrane[13-14]; (d) Foreign particles that have punctured the membrane[13-14]
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图 3 黑点在水氧下的生长机制和形貌：(a) OLEDs在水汽下工作时黑点形成的机理[20]；(b) 纯氧环境和无偏压下的黑点生长机理[20]；(c) 黑点及黑点周围灰色晕[23-24]；(d) OLEDs与水相互作用过程[23-24]；(e) 黑点在水氧下的生长机里[3, 14]
Figure 3. The growth mechanism of black spots under the action of water and oxygen and the morphology of black spots: (a) mechanism of dark spot formation during operation of an OLED underwater vapor atmosphere[20]; (b) dark spot growth mechanism for an unbiased device under a pure oxygen atmosphere[20]; (c) the grey halo around the black spot[23-24]; (d) the processes of water interaction in the OLEDs[23-24]; (e) growth mechanism of black spots under water and oxygen[3, 14]
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图 4 潮湿环境会诱导有机物结晶形成黑点：(a) Alq3薄膜的透射偏光显微镜照片[6]；(b) Alq3与水反应过程及产物[25]；
Figure 4. Humid environments induce the crystallization of organic matter, leading to the formation of black spots: (a) transmission polarization micrograph of an Alq3 film [6]; (b) reaction of Alq3 complex with water to form 8-Hq and other products[25]
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图 5 局部高电流导致黑点的形成：(a) 黑点生长过程及机理[27]；(b) 正常工作时电流走向[9]；(c) 电流流向短路[9]；(d) 大电流沿圆周方向冲入短路[9]；(e) 缺陷中心会产生累积的铝金属原子[9]；(f) 圆形边界处的铝阴极会变得足够薄，无法注入电子越过边界界限[9]；(g) 黑点光学图片[9]
Figure 5. Localized high current leads to the formation of black spots: (a) Illustration of a propagation mechanism of dark spots[27]; (b) Current direction during normal operation[9]; (c) Diversion of current flow into short circuit[9]; (d) Large electric current dashed into the short circuit in a circular manner[9]; (e) Accumulated al metal atoms will be created at the center of the defect, and (f) Al cathode at the circular boundary will become thin enough and not able to inject electrons to cross the boundary limit[9]; (g) Optical micrographs showing dark spot[9]
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图 8 不同阻挡层下水氧渗透路径：(a) 从针孔通过[54]；(b) 从晶界处通过[55-56]；(c) 从裂纹处通过[57-58]；(d) 从薄膜中直接渗透[61]
Figure 8. Infiltration paths of water and oxygen in different barrier layers: (a) water and oxygen molecules pass through the pinhole[54]; (b) water and oxygen molecules pass through the grain boundaries[55-56]; (c) water and oxygen molecules pass through the crack[57-58]; (d) water and oxygen molecules permeate directly through the barrier[61]
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表 1 黑点形成原因总结
Table 1 Summary of the formation reasons of black spot
Device Architecture Structure of black spot Test conditions Causes of black spot formation Ref. ITO//NPB/Alq3/Mg: Ag Circular aggregates At 100% relative humidity for 2 h Humidity-induced crystallization of Alq3 [6] ITO/TPD/Alq3/Mg/Ag Rounded Voltage: 4.5 V (Current density: 3–5 mA/cm2) Particle [13] ITO/NPB/Alq3(Qd-doped) /Alq3/Al Round with a nucleus in the center Voltage: 5 V (Current density: 5 mA/cm2) Concentrated current [15] ITO/PEDOT: PSS/PPV/ (Ca/Ag) Round with a nucleus in the center 20℃/50% RH Particle/Pinhole [16-18] ITO/CuPc/NPD/Alq3/ Mg: Ag Circumferential and raised at the center nucleus Exposure to the air Pinhole [19] ITO/CuPc/NPD/Alq3/Li/Al Gray ring around the core area 75% RH Permeated with oxygen Particle [20] ITO/ PEDOT: PSSLEP/BaAl Circular black spot (25–80)℃ (50–90)% RH Pinhole [21] ITO/Alq3/LiF/Al Gray ring around the core area 20℃/50% RH Voltage: (2.5–6.5)V Pinhole [23] ITO/PEDOT: PSS/LEP/ BaAl Gray ring around the core area Voltage: 4 V 50% RH Pinhole [24] ITO/MEH-PPV/Al Circumferential and raised at the center nucleus Current density: 100 mA/cm2 Surface defects High current density [27] ITO/a-NPD/Alq3/Al Circumferential and raised at the center nucleus Voltage: 6–10 V (Current density: 500 mA/cm2) High current density [28] ITO/a-NPB/Alq3/Al Domed Voltage: 32 V Roughness of ITO surface [29] ITO/PEDOT: PSS/polyfluorene/Al Black dot with white outer ring H2O/O2 < 0.01 ppm Voltage: 3.2 V Roughness of ITO surface High current density [30] Ag/PEDOT: PSS/MEH-PPV/Alq3/LiF/Al Sparkling Voltage: 5 V (Current density: 150 mA/cm2) High current density [31] ITO/TPD/ Alq3/Al Corrugated High voltage density: 3×106 V/cm High current density [32] 
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表 2 薄膜封装阻隔性能总结
Table 2 Summary of the barrier properties of thin film encapsulation
Materials Fabrication method Fabrication condition and materials Thickness/nm Test temperature/(℃) and humidity/ RH(%) WVTR/(g/m2∙day) Ref. SiNx PE-CVD (Ar/SiH4/N2/NH3) RT, Plasma 100 60/85 2×10-2 [67] Al2O3/TiO2 PE-ALD (TMA/TDMAT/O2)100℃ (22.1/0.225)×123 60/90 9.16×10-5 [69] Al2O3/ZrO2 RP-ALD (TMA/TEMAZr/O2) 225℃, Plasma 100 50/50 9.9×10-4 [70] (Al2O3/Parylene)3 ALD/CVD (TMA/H2O/N2/Parylene) 60℃ 1590 38/100 < 10-5 [75] Al2O3 ALD (TMA/H2O)120℃ 25 38 /85 1.7×10-5 [77] Al2O3–PI hybrid ALI (TMA/PI/H2O/Ar)100℃ 22 ± 2 85/85 < 10−7 [77] Al2O3 ALD (TMA/O3)100℃ 50 50/50 2.0×10-5 [78] Al2O3 PE-ALD (TMA/O2)100℃, Plasma 50 50/50 3.0×10-4 [78] Al2O3 ALD (TMA/O3)80℃ 60 20/60 8.7×10-6 [79] Al2O3 PE-ALD (TMA/ O2)100℃, Plasma 50 60/90 3.8×10-4 [80] SiNx ICP-CVD (SiH4/N2/Ar)40℃, Plasma 100 38/100 5×10−2 [81] SiNx PE-CVD (SiH4/N2/NH3) 180℃, Plasma 500 85/85 3×10−2 [82] SiNx L-PECVD (SiH4/NH3/He) 85℃, Plasma/Ion beam 300 37.8/100 5.0×10-5 [84] Al2O3/SiOx ALD (TMA/Silanol/H2O) 175℃ 26/60 RT/100 5×10-5 [85] Al2O3/SiNx: H PE-ALD/ PE-CVD (TMA/O2)25℃, Plasma (SiH4/N2/NH3)110℃, Plasma 40/300 20/50 4×10-6 [86] SiNx/SiOx PE-CVD (SiH4/NH/N2O)250℃ - - 1.0×10-2 [87] Parylene/SiNx/SiOx PE-CVD (SiH4/NH/N2O /Parylene)80℃, Preheating 120℃ 150/50/50 25/40 5.2×10-3 [87] 3(SiOx/SiNx)+Parylene +3(SiOx/SiNx stacks) PE-CVD (SiH/NH/N2O/Parylene) 80℃/120℃ 750 25/40 2.5× 10-7 [87]
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