有机添加剂在金属卤化钙钛矿发光二极管中的应用

黎振超; 陈梓铭; 邹广锐兴; 叶轩立; 曹镛

doi:10.7498/aps.68.20190307

摘要

近年来, 金属卤化钙钛矿凭借其优异的光电特性以及可低成本溶液加工的优势得到了学界的广泛关注, 成为了光电子领域的研究热点, 其中, 钙钛矿发光二极管是该领域的一大重要研究方向. 由于钙钛矿材料具有荧光量子效率高、带隙连续可调、发光半峰宽窄等优点, 钙钛矿发光二极管在短短5年时间内, 实现了外量子效率从不足1%到超过20%的重大突破, 成为了发展速度最快的发光技术. 在这5年的发展历程中, 学界主要集中于解决如何实现钙钛矿成膜和结晶过程的控制、如何提高钙钛矿薄膜的荧光量子效率, 以及如何改善钙钛矿发光二极管的稳定性等问题. 而在众多解决方案中, 有机添加剂的使用被认为是一种简单且有效的策略. 本文通过文献综述, 回顾了有机添加剂在钙钛矿发光二极管领域的整体发展和应用情况, 并着重讨论了小分子与聚合物添加剂在钙钛矿中的具体作用, 最后分析了当前钙钛矿发光二极管面临的问题, 并对其未来发展进行了展望.

关键词:

Abstract

In recent years, metal halide perovskites have received extensive attention due to their superior optoelectronic properties and solution processability, which also become a research hotspot in the field of optoelectronics. Among all the perovskite optoelectronics applications, perovskite light-emitting diode (LED) becomes one of the important research topics because it is likely to be used in the next-generation display technique. Based on the high photoluminescence quantum yield (PLQY), facilely tunable bandgaps, and sharp emission of perovskite material, the external quantum efficiency of perovskite LED has increased from less than 1% to over 20% within only five years, showing the most rapid development speed in the LED field. During the 5-year exploration of perovskite LEDs, researchers have focused their efforts on how to realize the crystal-growth control in the perovskite film formation process, enhance PLQY of the perovskite films, and improve the performance of perovskite LEDs. Among all the approaches, the utilization of organic additives including small molecules and polymers proves to be an effective strategy. Here, in this article, we review the recent advances in metal halide perovskite LEDs based on the strategy of organic-additive treatment. We also analyze and discuss the interaction between organic additive and perovskite crystal as well as its influence on the performance of perovskite LED. In the end, we discuss the challenges remaining in perovskite LEDs and the prospects for perovskite LEDs.

Keywords:

作者及机构信息

华南理工大学材料科学与工程学院, 发光材料与器件国家重点实验室, 广州　510640

通信作者: 陈梓铭, mszimingchen@yahoo.com ; 叶轩立, msangusyip@scut.edu.cn ;

基金项目: 国家重点研发计划(批准号: 2017YFA0206600)、国家自然科学基金(批准号: 21761132001, 51573057, 91733302)和中国博士后科学基金(批准号：2019M650197)资助的课题.

Authors and contacts

State Key Laboratory of Luminescent Materials and Devices, School of Materials Science and Engineering, South China University of Technology, Guangzhou 510640, China

Corresponding author: Chen Zi-Ming, mszimingchen@yahoo.com ; Yip Hin-Lap, msangusyip@scut.edu.cn ;

Funds: Project supported by the National Key R&D Program of China (Grant No. 2017YFA0206600), the National Natural Science Foundation of China (Grant Nos. 21761132001, 51573057, 91733302), and the China Postdoctoral Science Foundation (Grant No. 2019M650197).

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施引文献

图 1 (a)立方相钙钛矿晶体结构; (b) A位阳离子尺寸与钙钛矿容忍因子的关系^[15]; (c) n值不同的RP型二维钙钛矿在 $ \left\langle 100\right\rangle$ 方向上的排列方式^[16]; (d) n值不同的DJ型二维钙钛矿在 $\left\langle 100\right\rangle $ 方向上的排列方式^[17]

Fig. 1. (a) Crystal structure of cubic perovskite; (b) relationship between sizes of A cations and tolerance factor of perovskite ^[15]; (c) the $\left\langle 100\right\rangle $ oriented layered perovskite series, named as (RNH₃)₂A_n_–1B_nX_3n+1 ^[16]; (d) the $ \left\langle 100\right\rangle$ oriented layered perovskite series, named as (NH₃-R-NH₃)A_n_–1B_nX_3n+1 ^[17]

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图 2 (a)倒装钙钛矿LED器件结构; (b)正装钙钛矿LED器件结构; (c)倒装钙钛矿LED中各功能层的能级及钙钛矿LED的工作机理

Fig. 2. (a) Inverted architecture of a perovskite LED; (b) conventional architecture of a perovskite LED; (c) energy levels of different layers in a perovskite LED and working mechanism of perovskite LEDs.

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图 3 (a)钙钛矿中常用的小分子与聚合物有机添加剂的化学式汇总; (b)向钙钛矿中引入添加剂的两种方法

Fig. 3. (a) Summary of chemical structure of small molecule and polymer additives applied in perovskite; (b) schematic diagram of two approaches to introducing organic additives into the perovskite layer.

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图 4 (a)不同浓度的POEA与MAPbBr₃制备的钙钛矿薄膜的扫描电子显微镜(SEM)图与维度调控示意图^[33]; (b)不同浓度的POEA与MAPbBr₃制备的钙钛矿薄膜的XRD图案^[33]; (c)不同浓度的POEA与MAPbBr₃制备的钙钛矿薄膜PL以及器件EL的色坐标图^[33]

Fig. 4. (a) SEM images of perovskite films fabricated from MAPbBr₃ precursor solutions with different ratio of POEA and a schematic diagram of structural change of perovskite from bulk to layered structure upon increasing POEA concentration ^[33]; (b) XRD pattern of perovskite thin films fabricated from MAPbBr₃ precursor solutions with different ratio of POEA ^[33]; (c) color coordinates of the EL of perovskite LEDs and PL of perovskite films plotted in the CIE chromaticity diagram ^[33].

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图 5 (a)不同浓度的PEABr与CsPbCl_0.9Br_2.1制备的薄膜的PL光谱图^[29]; (b)不同浓度的PEABr与CsPbCl_0.9Br_2.1制备的LED的EL光谱图^[29]; (c) $\left\langle n \right\rangle $ = 3准二维钙钛矿不同时间尺度的PL光谱^[23]; (d) $\left\langle n \right\rangle $ = 5准二维钙钛矿晶粒间的电荷转移^[23]; (e)多晶PEA₂MA_n_–1Pb_nI₃_n₊₁准二维钙钛矿的电荷转移示意图^[23]; (f) PA₂(CsPbBr₃)_n_–1PbBr₄钙钛矿薄膜的吸收与PL光谱^[34]; (g) PA₂(CsPbBr₃)_n_–1PbBr₄钙钛矿LED的EL光谱与工作电压为6 V时的照片^[34]; (h) PA₂(CsPbBr₃)_n_–1PbBr₄量子阱中的电荷转移示意图^[34]; (i)基于钙钛矿量子阱的钙钛矿LED能级图^[24]; (j)钙钛矿多量子阱结构的级联式能量传递效应示意图^[24]

Fig. 5. (a) PL spectra of CsPbCl_0.9Br_2.1 thin films with different ratios of PEABr ^[29]; (b) EL spectra of CsPbCl_0.9Br_2.1 thin films with different ratios of PEABr ^[29]; (c) PL for an $\left\langle n \right\rangle $ = 3 perovskite at different timescales ^[23]; (d) the carrier transfer process in $ \left\langle n \right\rangle$ = 5 perovskite crystals ^[23]; (e) carrier transfer process in multi-phase PEA₂MA_n_–1Pb_nI_3n+1 perovskite crystals ^[23]; (f) UV-Vis absorption and PL spectra of the PA₂(CsPbBr₃)_n_–1PbBr₄ film ^[34]; (g) EL spectrum of PeLEDs fabricated with PA₂(CsPbBr₃)_n_–1PbBr₄ film and the photograph of a working device at 6 V ^[34]; (h) schematic diagram of charge carrier cascade in PA₂(CsPbBr₃)_n_–1PbBr₄ MQWs ^[34]; (i) flat-band energy level diagram of the PeLED with perovskite MQWs ^[24]; (j) schematic diagram of cascade energy transfer in perovskite multi quantum wells ^[24].

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图 6 (a) NMA₂FAPb₂I₇薄膜的激发功率密度依赖PLQE曲线^[24]; (b)不同组分的NMA₂FA_n_–1Pb_nI₃_n₊₁薄膜的激发功率密度依赖PLQE曲线^[36]; (c)不同组分的NMA₂(FA_xCs_1–_x)Pb₂I₇薄膜的激发功率密度依赖PLQE曲线^[38]; (d)三维与二维量子阱钙钛矿薄膜的激发功率密度依赖PLQE曲线^[39]; (e)不同组分的NMA₂FA_n_–1Pb_nI₃_n₊₁制备器件的EQE-电流密度曲线^[36]; (f)不同组分的NMA₂(FA_xCs_1–_x)Pb₂I₇制备器件的EQE-电流密度曲线^[38]; (g) PBA₂Cs_n_–1Pb_nI₃_n₊₁薄膜的激发功率密度依赖PLQE曲线^[40]; (h) PBA₂Cs_n_–1Pb_nI₃_n₊₁制备器件的EQE-电流密度曲线^[40]

Fig. 6. (a) Excitation-intensity-dependent PLQE of the NMA₂FAPb₂I₇ thin film ^[24]; (b) excitation-intensity-dependent PLQE of NMA₂FA_n_–1Pb_nI_3n+1 thin films with different composition ^[36]; (c) excitation-intensity-dependent PLQE of NMA₂(FA_xCs_1–x)Pb₂I₇ thin films with different composition ^[38]; (d) excitation-intensity-dependent PLQE of perovskite with three-dimensional and two-dimensional quantum wells ^[39]; (e) EQE versus current density curves of NMA₂FA_n_–1Pb_nI_3n+1 thin films with different composition ^[36]; (f) EQE versus current density curves of NMA₂(FA_xCs_1–x)Pb₂I₇ thin films with different composition ^[38]; (g) excitation-intensity-dependent PLQE of PBA₂Cs_n_–1Pb_nI_3n+1 thin films ^[40]; (h) EQE versus current density curves of PBA₂Cs_n_–1Pb_nI_3n+1 thin films ^[40].

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图 7 (a)经过含有不同浓度TPBi的氯仿作为反溶剂处理的MAPbBr₃薄膜的SEM图以及晶粒尺寸分布曲线^[47]; (b)不同比例的PEABr与CsPbBr₃制备的钙钛矿薄膜的表面与横截面SEM图^[50]; (c)不同比例的卵磷脂添加剂与CsPbBr₃制备的钙钛矿薄膜的表面SEM图^[51]; (d)有或没有冠醚添加剂处理的40% PEABr+CsPbBr₃的二维掠入射小角XRD与表面SEM图^[52]

Fig. 7. (a) SEM images of MAPbBr₃ films treated with different concentration of TPBi and grain size distribution graph of MAPbBr₃ films treated with TPBi or not ^[47]; (b) top-view and cross-section SEM images of CsPbBr₃ perovskite films prepared with different PEABr:CsPbBr₃ molar ratios ^[50]; (c) top-view SEM images of CsPbBr₃ perovskite films prepared with different concentration of lecithin additive^[51]; (d) two-dimensional grazing incidence XRD and SEM images of CsPbBr₃ + 40% PEABr with or without adding crown additive^[52].

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图 8 (a)不同浓度PVP与MAPbBr₃混合后的薄膜SEM图^[60]; (b)不同浓度PEOXA与MAPbI₃混合后的薄膜SEM图^[8]; (c)不同浓度PEOXA与MAPbI₃所制备器件的EQE与电流密度曲线^[8]; (d)加入45% PEOXA的CsPbBr_0.6I_2.4薄膜在不同退火温度下的XRD图案^[61]; (e)加入45% PEOXA的CsPbBr_0.6I_2.4薄膜的TEM图^[61]; (f)聚合物诱导的原位钙钛矿纳米晶形成过程示意图^[61]

Fig. 8. (a) SEM images of MAPbI₃ films with different ratio of PVP^[60]; (b) SEM images of MAPbI₃ films with different ratio of PEOXA^[8]; (c) EQE versus current density curves of MAPbI₃ films with different ratio of PEOXA^[8]; (d) XRD patterns of CsPbBr_0.6I_2.4 films with 45% PEOXA annealed at different temperatures^[61]; (e) TEM image of CsPbBr_0.6I_2.4 films with 45% PEOXA^[61]; (f) schematic diagram of polymer-induced in situ perovskite nanocrystal formation process^[61].

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图 9 (a)钙钛矿LED截面的STEM图^[27]; (b)钙钛矿薄膜的表面SEM图^[27]; (c)钙钛矿薄膜的AFM高度图^[27]; (d)具有自散射钙钛矿亚微米结构可提高光取出效率的示意图^[27]; (e) 5-氨基戊酸在ZnO-PEIE表面发生脱水反应机理示意图^[27]

Fig. 9. (a) STEM image of the fabricated device^[27]; (b) top-view SEM image of the perovskite^[27]; (c) AFM height image of the perovskite^[27]; (d) schematic diagram of the enhanced light outcoupling efficiency originated by the submicrometre-scale structure of perovskite^[27]; (e) dehydration reaction of 5AVA on top of the ZnO-PEIE surface^[27].

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图 10 (a) MAPbI₃钙钛矿中各种类型点缺陷的形成能与转变能级计算值^[70]; (b) MAPbBr₃钙钛矿中激子辐射复合效率与双分子辐射复合效率随载流子密度的变化^[78]; (c)常用的路易斯碱含有的官能团类型

Fig. 10. (a) Calculated formation energies and transition energy levels of various point defects in MAPbI₃ ^[70]; (b) calculated carrier density dependence of radiative efficiency for excitonic emission and bimolecular emission in MAPbBr₃ ^[78]; (c) structures of various Lewis base passivating materials in perovskite.

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图 11 (a)没有添加剂处理的MAPbBr₃钙钛矿薄膜的共聚焦PL图^[80]; (b)乙二胺处理的MAPbBr₃钙钛矿薄膜的共聚焦PL图^[80]; (c)添加TBAB前后的CsPbBr₃钙钛矿薄膜的时间分辨荧光衰减曲线^[81]; (d)添加TBAB前后的CsPbBr₃钙钛矿薄膜的温度依赖荧光强度曲线^[81]; (e) BCP修饰前后的LED缺陷密度-能量分布曲线^[82]; (f)不同浓度的5-氨基戊酸添加剂对FA_0.47Cs_0.53Pb(I_0.87Br_0.13)₃的激发功率密度依赖PLQY曲线^[83]; (g)不同浓度PEABr修饰的CsPbCl_0.9Br_2.1薄膜的缺陷密度与PLQY^[29]; (h)不同浓度PEABr修饰的CsPbCl_0.9Br_2.1薄膜的荧光寿命测试^[29]

Fig. 11. (a) Confocal PL image of MAPbBr₃ thin film without amine treatment ^[80]; (b) confocal PL image of MAPbBr₃ thin film with EDA treatment ^[80]; (c) PL decay curves for pure CsPbBr₃ and TBAB:CsPbBr₃ films ^[81]; (d) temperature-dependent PL intensities of pristine CsPbBr₃ and TBAB:CsPbBr₃ films ^[81]; (e) trap density versus energies for PeLEDs with and without BCP molecules ^[82]; (f) excitation-intensity-dependent PLQE of FA_0.47Cs_0.53Pb(I_0.87Br_0.13)₃ thin films with different ratio of 5AVA ^[83]; (g) trap densities and PLQYs of CsPbCl_0.9Br_2.1 thin films with different ratios of PEABr ^[29]; (h) PL lifetime measurement of CsPbCl_0.9Br_2.1 perovskites with various concentrations of PEABr ^[29].

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图 12 (a)基于NMA₂FAPb₂I₇钙钛矿的LED寿命测试, 测试条件为10 mA·cm^–2^[24]; (b)基于NMA₂CsPb₂I₆Cl钙钛矿的LED寿命测试, 测试条件为10 mA·cm^{–2 [35]}; (c)基于NMA₂FA_0.93Cs_0.07Pb₂I₇钙钛矿的LED寿命测试, 测试条件为10 mA·cm^{–2 [38]}; (d)基于(BIZ)₂FA_n_–1Pb_nBr₃_n₊₁钙钛矿的LED寿命测试, 测试条件为5 mA·cm^{–2 [90]}; (e)基于FPMAI-MAPb_0.6Sn_0.4I₃钙钛矿不同测试时间的EL光谱, 测试条件为1 mA·cm^{–2 [91]}; (f)基于FPMAI-MAPb_0.6Sn_0.4I₃钙钛矿不同测试时间的归一化EL强度, 测试条件分别为0.5, 1, 5 mA·cm^{–2 [91]}; (g)基于PEAI-CsSnI₃钙钛矿的LED寿命测试, 测试条件为10 mA cm^{–2 [39]}; (h)基于NEA-CsPbI₃钙钛矿的LED放置稳定性与连续工作稳定性测试^[92]

Fig. 12. (a) Stability test for the NMA₂FAPb₂I₇ based LED under a constant current density of 10 mA·cm^–2[24]; (b) normalized EQE for the NMA₂CsPb₂I₆Cl based LED tested under a constant current density of 10 mA·cm^–2[35]; (c) normalized EQE for the NMA₂FA_0.93Cs_0.07Pb₂I₇ based LED tested under a constant current density of 10 mA·cm^–2[38]; (d) stability test for the (BIZ)₂FA_n_–1Pb_nBr_3n+1 based LED under a constant current density of 5 mA·cm^–2[90]; (e) EL spectra at different measuring time under a constant current density of 1 mA·cm^–2 for the FPMAI-MAPb_0.6Sn_0.4I₃ based LED ^[91]; (f) normalized EL intensity of FPMAI-MAPb_0.6Sn_0.4I₃ based LED under constant current densities of 0.5, 1, and 5 mA·cm^–2[91]; (g) stability test for the PEAI-CsSnI₃ based LED under a constant current density of 10 mA·cm^–2[39]; (h) storage and continuous operating stability test for the NEA-CsPbI₃ based LED ^[92].

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图 13 (a)不同处理方式的CsPbBr₃钙钛矿LED在大气中的亮度衰减曲线^[100]; (b)加入Tween20前后的钙钛矿LED的亮度衰减曲线^[101]; (c)钙钛矿LED的亮度随拉伸次数的变化^[102]; (d) 45% PEOXA修饰的CsPbBr_0.6I_2.4钙钛矿LED的EL光谱^[61]; (e) 45% PEOXA修饰的CsPbBr_0.6I_2.4钙钛矿LED的亮度衰减曲线^[61]; (f)经过poly-HEMA修饰的钙钛矿LED的稳定性测试^[104]

Fig. 13. (a) Stability test of the PeLEDs based on pristine CsPbBr₃, CsPbBr₃-PEO, and CsPbBr₃-PEO-CF films at ambient conditions ^[100]; (b) stability test of the PeLEDs based on pristine CsPbBr₃ and Tween 20:CsPbBr₃ films ^[101]; (c) luminance of the device after repetitive stretching cycles for strain of 0–40% ^[102]; (d) EL spectra of the CsPbBr_0.6I_2.4 LED with 45% PEOXA measuring at different voltages ^[61]; (e) stability test of CsPbBr_0.6I_2.4 LED with 45% PEOXA ^[61]; (f) stability test for the poly-HEMA based PeLED under a constant current density of 0.1 mA·cm^{–2 [104]}.

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有机添加剂在金属卤化钙钛矿发光二极管中的应用