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Perovskite quantum dot color conversion Micro-LEDs: progress in stability and patterning
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摘要
微型发光二极管 (Micro light-emitting diode，Micro-LED)显示具有优异的显示性能和光电性质，被称为“下一代”终极显示技术。为了满足近眼显示需求，Micro-LED需要进一步微缩与集成化。随着微纳级图案化技术的不断革新，荧光色转换层法表现出低制造成本等显著优势，相较于三色芯片法，更适合应用于对色域、分辨率有更高要求的虚拟/增强现实显示应用。钙钛矿量子点是最有前景的荧光色转换材料，然而自身晶格固有的不稳定性和外界环境因素刺激共同导致的结构降解是一大问题。另外，如何制备与Micro-LED芯片阵列相匹配的微米级荧光阵列图案是至关重要的。为此，本文首先讲述了造成钙钛矿量子点结构不稳定性的原因；其次，总结了配体交换、离子掺杂、表面包覆和化学交联等方案在提升钙钛矿量子点稳定性方面的应用；最后，总结了光刻技术和喷墨打印技术在制备高分辨率钙钛矿量子点荧光阵列的最新研究进展。
Abstract
Micro light-emitting diode (Micro-LED) display is considered the "next-generation" ultimate display technology due to its excellent display performance and optoelectronic properties. In order to meet the requirements of near-eye display applications, further miniaturization and integration of Micro-LED are necessary. With the continuous innovation of micro/nanopatterning technology, the fluorescent color conversion layer method has significant advantages such as low manufacturing cost. Compared to the three-color chip method, it is more suitable for virtual/augmented reality display applications that demand higher color gamut and resolution. Perovskite quantum dots (PQDs) are the most promising fluorescent color conversion materials. However, the inherent lattice instability of PQDs and degradation caused by external environmental factors pose significant challenges. Furthermore, it is crucial to develop micro-scale fluorescent array patterns that match the Micro-LED chip array. Therefore, this paper first discusses the factors that affect the structural instability of perovskite quantum dots. Then, it summarizes the applications of strategies such as ligand exchange, ion doping, surface coating, and chemical cross-linking in enhancing the stability of perovskite quantum dots. Finally, the latest research progress for fabricating high-resolution perovskite quantum dot fluorescent arrays using photolithography and inkjet printing techniques is summarized.
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Overview
Overview: Micro-LEDs, as microscale light-emitting diode displays, are widely regarded as the ultimate choice for next-generation display technology due to their exceptional display performance and optoelectronic properties. Through miniaturization and high integration, Micro-LEDs have surpassed LCD and OLED technologies. Currently, the methods employed to achieve full-color Micro-LEDs primarily involve the use of trichromatic chips and photoluminescent quantum dot (PQD) conversion layers. However, one of the major challenges faced by the trichromatic chip approach is large-scale transfer technology, which affects transfer efficiency, precision, and yield. Moreover, the demand for ultra-high pixel density displays has led to a further reduction in Micro-LED chip size, increasing the difficulty of chip transfer and resulting in high manufacturing costs. Additionally, the impact of sidewall damage during the fabrication process on the performance of small-sized Micro-LEDs cannot be overlooked. In recent years, the fabrication of patterned full-color Micro-LED displays using PQDs conversion layers has garnered significant attention. However, a PQD possess ionic properties and low surface energy, making them highly susceptible to the external environment, including water, oxygen, heat, and light. The high dissociation of long-chain surface ligands leads to increased surface defects and particle aggregation, severely impacting the performance of PQD-based Micro-LED displays. To overcome these challenges, several strategies have been proposed, including ligand exchange, ion doping, surface encapsulation, and chemical cross-linking. These methods effectively passivate surface defects of PQDs, enhance lattice stability, and suppress non-radiative recombination pathways. By employing stability-enhancing techniques such as strong ligand bonding, lattice adjustment, organic/inorganic shell encapsulation, and covalent cross-linking, ion diffusion in PQDs can be inhibited, thereby improving their environmental stability. For achieving exceptional full-color Micro-LEDs, these stability-enhancing approaches can be combined with photolithography and inkjet printing techniques to fabricate PQDs conversion layers with high resolution, stability, and luminance. This review begins by elucidating the causes of structural instability in PQDs. Subsequently, it summarizes the applications of ligand exchange, ion doping, surface encapsulation, and chemical cross-linking in enhancing the stability of perovskite quantum dots. Finally, the latest research advancements in photolithography and inkjet printing techniques for fabricating high-resolution perovskite quantum dot fluorescent arrays are presented. By synthesizing these findings, this comprehensive review specifically emphasizes the strategies employed to enhance the stability and performance of patterned Micro-LED displays with perovskite quantum dot conversion layers.
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图 2 (a)卤化物钙钛矿典型ABX3晶体结构示意图[33]； (b) CsPbI3相变的可能途径[39]； (c) CsPbI3光氧化机制[43]； (d)水与钙钛矿晶体相互作用示意图[47]； (e) CsPbBr3光诱导团聚示意图[45]
Figure 2. (a) Schematic of a typical ABX3 crystal structure of halide perovskite[33] ; (b) Possible pathways for phase transitions of CsPbI3[39] ; (c) Photo-oxidation mechanism of CsPbI3[43]; (d) Schematic of the interaction between water and PNCs[47]; (e) Schematic of photo-induced agglomeration of CsPbBr3[45]
图 3 (a) CsPbI3-DDAB和CsPbI3-OA/OLA结构图[52]； (b) CsPbI3-DDAB和CsPbI3-OA/OLA的PLQY稳定性[52]； (c) CsPbI3-DDAB在黑暗环境中存放60天后的TEM图[52]； (d) HI诱导的5AVA配体与OA/OLA配体原位交换策略图[54]； (e) 两性离子配体 (磺基甜菜碱、磷胆碱和γ-氨基酸)钝化示意图[58]； (f) DDAB和DLPS双配体钝化策略[59]； (g) 三种量子点在自然环境下的PL稳定性[59]
Figure 3. (a) Structure of CsPbI3-DDAB and CsPbI3-OA/OLA[52]; (b) PLQY stability of CsPbI3-DDAB and CsPbI3-OA/OLA[52]; (c) TEM image of CsPbI3-DDAB after 60 days of storage in a dark environment[52]; (d) Strategy of HI-induced in situ exchange strategy of 5AVA ligand with OA/OLA ligand[54]; (e) Schematic of the passivation of amphipathic ionic ligands (sulfobetaine, phosphocholine and γ-aminoacids)[58]; (f) DDAB and DLPS dual ligand passivation strategies[59]; (g) PL stability of three QDs in natural environments[59]
图 4 (a)原位合成Ni2+掺杂的CsPbI3 PQD示意图[75]； (b)未掺杂和掺镍CsPbI3 PQD 的PLQY随存储时间的变化[75]； (c) Zn2+掺杂CsMnCl3 PQD的稳定机制[77]； (d)不同Zn/Mn质量比的PLQY[77]； (e)掺杂NdCl3的CsPbBr3 PQD制备流程图[79]； (f)不同掺杂的CsPbBr3 PQD在自然环境下的PLQY稳定性[79]
Figure 4. (a) Schematic diagram of in-situ synthesized Ni2+ doped CsPbI3 PQD[75]; (b) Variation of PLQY with storage time for undoped and Ni-doped CsPbI3 PQD[75]; (c) Stabilization mechanism of Zn2+ doped CsMnCl3 PQD[77]; (d) PLQY at different Zn/Mn mass ratios[77]; (e) Process flowchart for the preparation of CsPbBr3 PQDs doped with NdCl3[79]; (f) PLQY stability of CsPbBr3 PQDs with different dopants in a natural environment[79]
图 5 (a) CsPbBr3/LLPDE结构示意图[83]； (b) CsPbBr3和CsPbBr3/LLPDE在自然环境下的降解实验[83]； (c) CsPbBr3和CsPbBr3/LLPDE在365 nm光照射下的降解实验[83]； (d) 可聚合CsPbX3 PQD墨水制备流程图[87]； (e) 配体交换与ALD-Al2O3封装流程图[97]； (f) CsPbBr3/CdS和CsPbBr3/Cs4PbBr6封装方法和能量图[103]； (g) 各种QD材料在水环境 (左图)和365 nm光环境 (右图)下的降解实验[103]
Figure 5. (a) Schematic structure of CsPbBr3/LLPDE[83]; (b) Degradation of CsPbBr3 and CsPbBr3/LLPDE in natural environment[83]; (c) Degradation of CsPbBr3 and CsPbBr3/LLPDE under 365 nm light irradiation[83]; (d) Flowchart for preparation of polymerisable CsPbX3 PQD ink[87]; (e) Ligand exchange and ALD-Al2O3 encapsulation flowchart[97]; (f) CsPbBr3/CdS and CsPbBr3/Cs4PbBr6 encapsulation methods and energy maps[103]; (g) Degradation of various QD materials in aqueous environment (left) and 365 nm light environment (right)[103]
图 6 (a) 层状双金属氢氧化物纳米片中制备CsPbBr3 PQD示意图[107]； (b) CsPbBr3和LDH-CP-CsPbBr3在高温下的PL稳定[107]； (c) 在疏水性二氧化硅气凝胶上原位生长CsPbBr3 QDs示意图[108]； (d) PQD在高温下加热1小时后的PL稳定性[108]； (e) CsPbBr3 PQD复合材料的设计示意图[109]； (f) CsPbBr3 PQD复合材料加热-冷却循环的荧光特性[109]； (g) 添加乙基纤维素的PQD在自然环境下的PL稳定性[110]
Figure 6. (a) Schematic diagram of the preparation of CsPbBr3 perovskite PQD in LHD nanosheets[107]; (b) PL stability of CsPbBr3 and LDH-CP-CsPbBr3 at high temperatures[107]; (c) Schematic diagram of in-situ growth of CsPbBr3 QDs on hydrophobic silica aerogel[108]; (d) PL stability of PQDs after heating at high temperatures for 1 hour[108]; (e) Design schematic of CsPbBr3 PQD composite materials[109]; (f) Fluorescence characteristics of CsPbBr3 PQD composite materials during heating-cooling cycles[109]; (g) PL stability of PQDs with the addition of ethyl cellulose in a natural environment[110]
图 7 (a)光刻掩膜法制备PQD薄膜示意图[113]； (b)特征尺寸小至3 µm的PQD阵列[113]； (c)光刻剥离法制备PQD薄膜示意图[114]； (d)半径尺寸为5 µm的PQD点阵[114]； (e)利用溴化铅配合物原位制造PQD图案示意图[115]； (f)分辨率高达2450 PPI的PQD荧光阵列[115]； (g) PZ配体光图案化机制[116]； (h)线距为4 µm的高分辨率PQD图案[116]
Figure 7. (a) Schematic diagram of PQD thin film preparation using photolithographic masking method[113]; (b) PQD array with feature sizes as small as 3 µm[113]; (c) Schematic diagram of PQD thin film preparation using photolithographic peeling method[114]; (d) PQD dot array with a radius size of 5 µm[114]; (e) Schematic diagram of in-situ fabrication of PQD patterns using lead bromide complex[115]; (f) PQD fluorescence array with a resolution of up to 2450 PPI [115]; (g) Photopatterning mechanism of PZ ligands[116]; (h) High-resolution PQD pattern with a line spacing of 4 µm[116]
图 8 (a) PTMP与PQD的反应机制 (上图)和直接光刻制备PQD图案示意图 (下图)[119]； (b)分辨率达12700 PPI的PQD荧光阵列[119]； (c)微孔填充法制备PQD荧光阵列示意图[120]； (d)像素尺寸2 µm的高分辨率PQD荧光阵列[120]； (e)高分辨率双色PQD图案[120]
Figure 8. (a) Reaction mechanism between PTMP and PQD (top) and schematic diagram of direct photolithographic fabrication of PQD patterns (bottom)[119]; (b) PQD fluorescence array with a resolution of 12700 PPI[119]; (c) Schematic diagram of PQD fluorescence array prepared by microsphere filling method[120]; (d) High-resolution PQD fluorescence array with pixel size of 2 µm[120]; (e) High-resolution dual-color PQD pattern[120].
图 9 (a)气溶胶喷墨打印技术制备PQD颜色转换层示意图[125]； (b)线宽为13 µm的PQD图案[125]； (c) EHD喷墨打印示意图[126]； (d)分辨率为10 µm的PQD图案[126]； (e)分辨率为2540 DPI的红色PQD荧光阵列[127]； (f)子像素直径为10 µm的全彩PQD颜色转换层[127]； (g)通过配体交换和EHD喷墨打印工艺制备红色PQD荧光阵列示意图[127]
Figure 9. (a) Schematic diagram of PQD color conversion layer prepared by aerosol inkjet printing technique[125]; (b) PQD pattern with a line width of 13 µm [125]; (c) Schematic diagram of EHD inkjet printing[126]; (d) PQD pattern with a resolution of 10 µm [126]; (e) Red PQD fluorescence array with a resolution of 2540 DPI [127]; (f) Full-color PQD color conversion layer with subpixel diameter of 10 µm [127]; (g) Schematic diagram of red PQD fluorescence array prepared by ligand exchange and EHD inkjet printing process[127]
图 10 (a)墨水制备和印刷示意图[129]； (b)分辨率高达22718 DPI的PQD荧光阵列[129]； (c)线宽小于2 µm的混合QD纳米环Micro-LED制备流程[130]； (d)线宽为1.65 µm的QD图案[130]； (e)直径为1 µm、2 µm、3 µm的钙钛矿点阵图案[131]
Figure 10. (a) Schematic diagram of ink preparation and printing[129]; (b) PQD fluorescence array with a resolution of up to 22718 DPI[129]; (c) Fabrication process of mixed QD nanoring Micro-LED with line width less than 2 µm[130]; (d) QD pattern with a line width of 1.65 µm[130]; (e) Patterns of perovskite dot arrays with diameters of 1 µm, 2 µm, and 3 µm[131]
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