低温原子层沉积封装技术在OLED上的应用及对有机、钙钛矿太阳能电池封装的启示

doi:10.6023/A21110513

化学学报 ›› 2022, Vol. 80 ›› Issue (3): 395-422.DOI: 10.6023/A21110513 上一篇

综述

低温原子层沉积封装技术在OLED上的应用及对有机、钙钛矿太阳能电池封装的启示

周静^a, 田雪迎^a^,^b, 王斌凯^a^,^b, 张沙沙^c, 刘宗豪^a^,^*(), 陈炜^a^,^*()

a 华中科技大学武汉国家光电研究中心武汉 430074
b 华中科技大学中欧清洁与可再生能源学院武汉 430074
c 郑州大学河南先进技术研究院郑州 450001

投稿日期:2021-11-12 发布日期:2022-01-10
通讯作者: 刘宗豪, 陈炜

作者简介:

周静, 2018年于中国地质大学(武汉)获应用化学系理学士学位.目前是华中科技大学武汉国家光电研究中心2018级博士研究生, 主要研究方向为反式钙钛矿太阳能电池的稳定性研究.

田雪迎, 2019年于济南大学新能源科学与工程学院获理学士学位. 目前是华中科技大学中欧清洁与可再生能源学院2019级硕士研究生, 主要研究方向为钙钛矿太阳能电池的封装和长期稳定性研究.

王斌凯, 2019年于河北大学质量技术监督学院获管理学学士学位. 目前是华中科技大学中欧清洁与可再生能源学院2019级硕士研究生, 主要研究方向为大面积钙钛矿太阳能电池的刮涂及模组制备研究.

刘宗豪, 副教授, 2011年于华中科技大学获理学士学位, 2016年于华中科技大学获博士学位. 2015年在美国洛杉矶加利福尼亚州访学交流. 2016至2017年在北京大学做研究助理. 2017至2019年在日本冲绳理工大学研究生院做博士后. 目前是华中科技大学武汉国家光电研究中心副教授, 主要从事有机无机杂化钙钛矿光电器件性能研究.

陈炜, 教授, 于清华大学材料科学与工程系获硕士和博士学位. 2008年2010年于香港科技大学化学系做博士后. 2014年至2015年于日本国际材料化学协会做访问学者. 目前是华中科技大学武汉国家光电研究中心教授, 主要从事纳米材料的合成、基础研究和应用以及新型太阳能电池(包括钙钛矿太阳能电池)半导体薄膜的研究.

基金资助:
国家自然科学基金(51672094); 国家自然科学基金(51861145404); 国家自然科学基金(51822203); 国家自然科学基金(52002140); 国家自然科学基金(21401167); 华中科技大学自主创新研究计划基金(2018KFYRCPY003); 华中科技大学自主创新研究计划基金(2020kfyXJJS008); 湖北省自然科学基金(ZRMS2020001132); 深圳科技改革委员会(JCYJ20180507182257563)

Application of Low Temperature Atomic Layer Deposition Packaging Technology in OLED and Its Implications for Organic and Perovskite Solar Cell Packaging

Jing Zhou^a, Xueying Tian^a^,^b, Binkai Wang^a^,^b, Shasha Zhang^c, Zonghao Liu^a(), Wei Chen^a()

a Wuhan National Laboratory for Optoelectronics, Huazhong University of Science and Technology, Wuhan 430074, China
b China-EU Institute for Clean and Renewable Energy, Huazhong University of Science and Technology, Wuhan 430074, China
c Henan Institute of Advanced Technology, Zhengzhou University, Zhengzhou 450001, China

Received:2021-11-12 Published:2022-01-10
Contact: Zonghao Liu, Wei Chen
Supported by:
National Natural Science Foundation of China(51672094); National Natural Science Foundation of China(51861145404); National Natural Science Foundation of China(51822203); National Natural Science Foundation of China(52002140); National Natural Science Foundation of China(21401167); Self-determined and Innovative Research Funds of HUST(2018KFYRCPY003); Self-determined and Innovative Research Funds of HUST(2020kfyXJJS008); Natural Science Foundation of Hubei Province(ZRMS2020001132); Shenzhen Science and Technology Innovation Committee(JCYJ20180507182257563)

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摘要/Abstract

有机半导体光电器件在基础研究和工业应用方面进展迅速, 相关方向已经成为一个较为成熟的新兴领域. 然而, 这类器件中的关键有机材料存在对空气中的水、氧十分敏感的问题, 严重影响了器件的长期工作性能. 除了选择合适的传输层材料、界面层结构, 利用界面工程提高器件水氧耐受能力之外, 对器件进行可靠的封装是隔绝空气中水、氧的另一个有效手段. 原子层沉积(atomic layer deposition, ALD)是一种近乎完美的薄膜沉积封装技术, 这种技术所生长的薄膜具有独特的层-层(layer by layer)生长特性, 而且可以在低温下沉积出厚度可控、重复率高、均匀致密的薄膜, 使得该技术在半导体行业已经得到广泛应用. 在此, 我们将回顾ALD封装技术在有机发光二极管(organic light emitting diode, OLED)、有机太阳能电池(organic photovoltaics, OPV)和钙钛矿太阳能电池(perovskite solar cell, PSC)中的应用, 并进一步讨论现阶段应用于OLED的相对比较成熟的ALD封装技术, 及其对OPV和PSC封装的启示性意义.

关键词: 原子层沉积(ALD), 有机发光二极管(OLED), 有机太阳能电池(OPV), 钙钛矿太阳能电池(PSC), 封装

Organic semiconductor optoelectronic devices have made rapid development and progress in both research and industrial applications. The related directions have become a mature and emerging field. However, the organic materials in such devices usually are extremely sensitive to water vapor or oxygen existed in ambient air, which seriously affects the long-term stability of the devices. In addition to interface engineering, selecting appropriate charge (holes or electrons) transport layers and interfacial materials to improve the water and oxygen tolerance of the device and packing the device with robust encapsulation are all effective strategies to isolate the device from the water and oxygen in ambient air. Among various encapsulation technologies, atomic layer deposition (ALD) is an almost perfect encapsulation approach, which could deposit thin films in the layer-by-layer growth mode at low-temperature, with the characteristics of accurate and controllable thickness, high repeatability, excellent uniformity and high density. These characteristics make ALD to be widely used in semiconductor industry. Here, we review the progress of the applications of the ALD encapsulation techniques in organic light emitting diode (OLED) and provide further discussions on the enlightening significance of ALD encapsulation techniques in organic photovoltaics (OPV) and perovskite solar cell (PSC) encapsulations.

Key words: atomic layer deposition, organic light emitting diode, organic photovoltaics, perovskite solar cells, encapsulation

引用此文

周静, 田雪迎, 王斌凯, 张沙沙, 刘宗豪, 陈炜. 低温原子层沉积封装技术在OLED上的应用及对有机、钙钛矿太阳能电池封装的启示[J]. 化学学报, 2022, 80(3): 395-422.

Jing Zhou, Xueying Tian, Binkai Wang, Shasha Zhang, Zonghao Liu, Wei Chen. Application of Low Temperature Atomic Layer Deposition Packaging Technology in OLED and Its Implications for Organic and Perovskite Solar Cell Packaging[J]. Acta Chimica Sinica, 2022, 80(3): 395-422.

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图/表 15

图1. 三种不同的ALD工艺原理图(以ALD-Al2O3为例)

Figure 1. The schematic diagram of three different ALD processes (take ALD-Al2O3 as an example)

图2. S-ALD工艺原理图(以ALD-Al2O3为例)

Figure 2. The schematic diagram of S-ALD processes (take ALD-Al2O3 as an example)

图3. (a)有机发光二极管在水蒸气环境下工作的光学显微镜图像, 其亮度为100 cd/m2. 可以清楚地看到不发光的黑点; (b) P3HT烷基侧链的氧化机理; (c)外部铝电极的示意图, 显示了水和分子氧的两个不同的入口通道. 分子氧主要通过微孔扩散, 水主要在铝颗粒间扩散. (d)引起钙钛矿太阳能电池不稳定的因素可分为外部因素, 例如: 温度、湿度、氧气、光(包括紫外光)和电场以及内部

Figure 3. (a) Optical microscope image of an OLED working at a luminance of 100 cd/m2 under water vapor atmosphere. Non-emitting dark spots can clearly be seen. Reproduced with permission from ref. [64]. Copyright 2001, WILEY-VCH. (b) Oxidation mechanism of the P3HT alkyl side chain. Reproduced with permission from ref. [73]. Copyright 2009, Elsevier Ltd. (c) Schematic representation of the outer aluminum electrode showing the two different entrance channels for water and molecular oxygen. The molecular oxygen mainly diffuses through microscopic pinholes and water mainly diffuses in between the aluminum grains. Reproduced with permission from ref. [76]. Copyright 2012, John Wiley & Sons, Inc. (d) Factors inducing instability in perovskite solar cells can be classiﬁed as external, i.e., temperature, moisture, oxygen, light (including UV light) and electric ﬁeld, and internal. Reproduced with permission from ref. [78]. Copyright 2017, Elsevier Ltd.

Deposition temp./℃	Structure	Thickness/nm	dyads	Test temp./℃	Test temp. RH%	WVTR/ (g•m^-2•d^-1)	Bending radius/ cm	Bending cycle	WVTR change after bending/%	Ref.
80	Al₂O₃	25	1	85	85	4.50×10^-4	1.5	1000	374%	^[85]
80	Al₂O₃/cyclohexane-plasma polymer/Al₂O₃	12.5/100/12.5	1	85	85	2.70×10^-4	1.5	1000	101%	^[85]
80	Al₂O₃/Li(acac)/Al₂O₃	12.5/100/12.5	1	85	85	1.50×10^-4	1.5	1000	131%	^[85]
80	Al₂O₃/TiMO/ Al₂O₃	12.5/100/12.5	1	85	85	1.70×10^-4	1.5	1000	137%	^[85]
120	Al₂O₃/HfO₂	2/2	9	38	100	6.00×10^-6	—	—	—	^[86]
300	Al₂O₃/HfO₂	2/2	5	38	100	5.00×10^-6	—	—	—	^[86]
80	Al₂O₃/ 4MP	3/0.6	3.5	r.t.	r.t.	2.32×10^-7	—	—	—	^[87]
80	Al₂O₃	50	1	85	85	3.10×10^-4	—	—	—	^[88]
90	Al₂O₃/alucone	15/2.5	5.5	25	60	1.44×10^-4	—	—	—	^[89]
80	SAM/Al₂O₃/Ag	40/8	1	38	100	5.00×10^-5	—	—	—	^[90]
80	Al₂O₃/15% C Al₂O₃	6.7/2.5	5	85	85	3.20×10^-4	1.5	1000	186%	^[91]
60	parylene C/Al₂O₃	30/500	3	38	100	5.00×10^-5	—	—	—	^[92]
80	AMO / CYTOP	100/2000	1	60	100	1.05×10^-6	—	—	—	^[93]
80	SAOLs/Al₂O₃	10.4/20.1	5	r.t./25	r.t./40	2.99×10^-7	—	—	—	^[94]
80	SAOLs/Al₂O₃	10.4/20.1	5	85	85	1.58×10^-3	—	—	—	^[94]
40	Al₂O₃	100	1	85	85	1.84×10^-3	—	—	—	^[95]
80	ZrO₂	80	1	20	60	6.09×10^-4	—	—	—	^[84]
40	Al₂O₃	100	1	37.8	100	9.20×10^-7	—	—	—	^[95]
70	Al₂O₃/ZnO	3/3	5	30	90	4.92×10^-4	—	—	—	^[96]
70	(Al₂O₃/ZnO nano-stratified stack)/S-H nanocomposite	30/120	2.5	30	90	1.91×10^-5	3	1000	212%	^[96]
100	Al₂O₃/ZrO₂	10/10	5	50	50	3.97×10^-4	—	—	—	^[97]
80	AlOx/plasma polymer	1/20	20	85	85	3.00×10^-4	0.5	10000	≈100%	^[98]
80	Al₂O₃/TiO₂	5/5	8	85	85	2.10×10^-5	—	—	—	^[99]
60	Al₂O₃/ZnO	2/2	9	38	100	1.00×10^-6	—	—	—	^[100]
50	Al₂O₃/HfO₂	2/2	9	38	100	3.50×10^-6	—	—	—	^[100]
80	Al₂O₃/MgO	0.082/1.01	50/10	60	100	4.70×10^-6	—	—	—	^[101]
75	SiO₂	70	1	37.8	100	7.73×10^-3	—	—	—	^[80]
85	MgO/S-H nanocomposite	40/200	4.5	30	90	4.33×10^-6	—	—	—	^[102]
80	NOA63/ZrO₂/NOA63	16000/85/16000	1	20	50	9.00×10^-5	—	—	—	^[103]
80	ZrO₂/NOA63	28/16000	2	20	60	1.27×10^-4	—	—	—	^[104]
80	ZrO₂/zircone	4/1	15	20	60	3.078×10^-5	—	—	—	^[105]
70	ZnO/Al₂O₃/MgO	20/12/10	6	30	90	2.06×10^-6	0.5	—	10^-6	^[106]
70	Al₂O₃/S-H nanocomposite	60/2000	3	30	90	1.11×10^-6	1	100	—	^[107]

Deposition temp./℃	Structure	Thickness/nm	dyads	Test temp./℃	Test temp. RH%	WVTR/ (g•m^-2•d^-1)	Bending radius/ cm	Bending cycle	WVTR change after bending/%	Ref.
80	Al₂O₃	25	1	85	85	4.50×10^-4	1.5	1000	374%	^[85]
80	Al₂O₃/cyclohexane-plasma polymer/Al₂O₃	12.5/100/12.5	1	85	85	2.70×10^-4	1.5	1000	101%	^[85]
80	Al₂O₃/Li(acac)/Al₂O₃	12.5/100/12.5	1	85	85	1.50×10^-4	1.5	1000	131%	^[85]
80	Al₂O₃/TiMO/ Al₂O₃	12.5/100/12.5	1	85	85	1.70×10^-4	1.5	1000	137%	^[85]
120	Al₂O₃/HfO₂	2/2	9	38	100	6.00×10^-6	—	—	—	^[86]
300	Al₂O₃/HfO₂	2/2	5	38	100	5.00×10^-6	—	—	—	^[86]
80	Al₂O₃/ 4MP	3/0.6	3.5	r.t.	r.t.	2.32×10^-7	—	—	—	^[87]
80	Al₂O₃	50	1	85	85	3.10×10^-4	—	—	—	^[88]
90	Al₂O₃/alucone	15/2.5	5.5	25	60	1.44×10^-4	—	—	—	^[89]
80	SAM/Al₂O₃/Ag	40/8	1	38	100	5.00×10^-5	—	—	—	^[90]
80	Al₂O₃/15% C Al₂O₃	6.7/2.5	5	85	85	3.20×10^-4	1.5	1000	186%	^[91]
60	parylene C/Al₂O₃	30/500	3	38	100	5.00×10^-5	—	—	—	^[92]
80	AMO / CYTOP	100/2000	1	60	100	1.05×10^-6	—	—	—	^[93]
80	SAOLs/Al₂O₃	10.4/20.1	5	r.t./25	r.t./40	2.99×10^-7	—	—	—	^[94]
80	SAOLs/Al₂O₃	10.4/20.1	5	85	85	1.58×10^-3	—	—	—	^[94]
40	Al₂O₃	100	1	85	85	1.84×10^-3	—	—	—	^[95]
80	ZrO₂	80	1	20	60	6.09×10^-4	—	—	—	^[84]
40	Al₂O₃	100	1	37.8	100	9.20×10^-7	—	—	—	^[95]
70	Al₂O₃/ZnO	3/3	5	30	90	4.92×10^-4	—	—	—	^[96]
70	(Al₂O₃/ZnO nano-stratified stack)/S-H nanocomposite	30/120	2.5	30	90	1.91×10^-5	3	1000	212%	^[96]
100	Al₂O₃/ZrO₂	10/10	5	50	50	3.97×10^-4	—	—	—	^[97]
80	AlOx/plasma polymer	1/20	20	85	85	3.00×10^-4	0.5	10000	≈100%	^[98]
80	Al₂O₃/TiO₂	5/5	8	85	85	2.10×10^-5	—	—	—	^[99]
60	Al₂O₃/ZnO	2/2	9	38	100	1.00×10^-6	—	—	—	^[100]
50	Al₂O₃/HfO₂	2/2	9	38	100	3.50×10^-6	—	—	—	^[100]
80	Al₂O₃/MgO	0.082/1.01	50/10	60	100	4.70×10^-6	—	—	—	^[101]
75	SiO₂	70	1	37.8	100	7.73×10^-3	—	—	—	^[80]
85	MgO/S-H nanocomposite	40/200	4.5	30	90	4.33×10^-6	—	—	—	^[102]
80	NOA63/ZrO₂/NOA63	16000/85/16000	1	20	50	9.00×10^-5	—	—	—	^[103]
80	ZrO₂/NOA63	28/16000	2	20	60	1.27×10^-4	—	—	—	^[104]
80	ZrO₂/zircone	4/1	15	20	60	3.078×10^-5	—	—	—	^[105]
70	ZnO/Al₂O₃/MgO	20/12/10	6	30	90	2.06×10^-6	0.5	—	10^-6	^[106]
70	Al₂O₃/S-H nanocomposite	60/2000	3	30	90	1.11×10^-6	1	100	—	^[107]

表1. 各种OLED封装膜的性能总结

Table 1. Summary of the properties of various OLED encapsulation film

表1. 各种OLED封装膜的性能总结

Table 1. Summary of the properties of various OLED encapsulation film

图4. (a)装有紫外线灯的ALD系统原理图. 冷镜和热镜分别反射紫外线和可见光/红外辐射. 注意, 热镜可以防止衬底温度升高. (b)分别通过热ALD和UV-ALD获得的100 nm厚Al2O3膜的WVTR的MOCON测试结果. 随着时间的推移, WVTR值达到一个恒定的水平, 这个水平通过MOCON测试指定为最终的WVTR值. 使用MOCON仪器的检出限为1.00×10-3 g•m-2•d-1. (c)低碳富Al2O3薄膜的WVTR; (d)低碳富Al2O3薄膜弯曲试验的WVTR; (e)三层多层膜弯曲试验的WVTR; (f)五层多层膜弯曲试验的WVTR

Figure 4. (a) Schematic diagram of an ALD system equipped with a UV lamp. Cold mirror and hot mirror reflect UV radiation and visible/IR radiation, respectively. Note that the hot mirror prevents the substrate temperature from increasing. (b) MOCON test results to obtain the WVTR for the 100 nm thick Al2O3 barrier films by thermal ALD and UV-ALD. With time, WVTR values reach a constant level that is assigned as the final WVTR value by MOCON test. The detection limit of the MOCON instrument used was 1.00×10-3 g•m-2•d-1. Reproduced with permission from ref. [95]. Copyright 2017, The Royal Society of Chemistry. (c) WVTR of Low-carbon and rich Al2O3 Films, (d) WVTR of Low-carbon and rich Al2O3 Films with Bending. (e) WVTR of three-layer multiple barrier films with bending test, (f) WVTR of five-layer multiple barrier films with bending test. Reproduced with permission from ref. [91]. Copyright 2018, The Korean Physical Society.

图5. (a)浸没在水中的Al2O3保护装置的标准化PCE的发展. 插图显示在水中放置1 h后, 有Al2O3(右)层和没有Al2O3(左)层的器件的照片; (b) 存储在大气环境中对照器件(黑色)和具有TiO2界面层的器件(红色), 具有TiO2界面层和Al2O3封装层的器件(蓝色)以及具有TiO2界面层和叠层Al2O3封装层的器件(绿色)的标准化PCE的演变; (c)封装工艺示意图; (d)封装前后钙钛矿太阳能电池的效率; (e)在高湿度环境下, 有或没有封装的钙钛矿太阳能电池标准化PCE随时间的演变

Figure 5. (a) Evolution of normalized PCE for the Al2O3 protected devices immersed in water. The inset picture shows photographs of the devices with Al2O3 (right) and without Al2O3 (left) layers after being kept in water for an hour; (b) evolution of normalized PCE of the control devices (black), devices with TiO2 interface layer (red), devices with TiO2 interface layer and Al2O3 encapsulation layer (blue) and devices with TiO2 interface layer and stacked Al2O3 encapsulation layer (green) stored in an ambient environment. Reproduced with permission from ref. [113]. Copyright 2018, American Chemical Society. (c) Schematic diagram of the encapsulation process; (d) efficiency of the perovskite solar cells before and after encapsulation; (e) time evolution of normalized PCE for the perovskite solar cells with and without encapsulation under a high-humidity environment. Reproduced with permission from ref. [124]. Copyright 2019, Elsevier Ltd.

ALD cycles	O₃-Al₂O₃			H₂O-Al₂O₃
ALD cycles	η_initial	η_{350 h}	%η_retention	η_initial	η_{350 h}	%η_retention
90	2.36	0.82	35	2.50	0.01	0.4
120	2.47	1.13	46	2.76	0.05	2
150	2.52	1.61	64	2.64	0.74	28
210	2.69	2.35	87	2.78	0.91	33

表2. 用沉积在140 ℃的90、120、150和210个循环的Al2O3封装的OPV的初始效率(ηinitial)、350 h后的效率(η350 h)和350 h后保留的初始效率百分比(%ηretention)

Table 2. The initial efficiency (ηinitial), efficiency after 350 h (η350 h) and percentage of initial efficiency retained after 350 h (%ηretention) for OPVs encapsulated with 90, 120, 150, and 210 cycles of Al2O3 deposited at 140 ℃. Reprinted with permission from Ref. [3], Copyright (2010) Elsevier B.V.

图6. (a)通过XRR测量的ALD Al2O3的密度; (b)通过SE测量的折射率; (c)具有代表性的MAPbI3-xClx薄膜光学图像; (d)、(e)和(f)为分别暴露于O3、H2O和乙酸(AA)的MAPbI3-xClx膜; (g)相应薄膜的XRD谱图

Figure 6. (a) Densities of ALD Al2O3 measured via XRR and (b) refractive index measured through SE. Reproduced with permission from ref. [88]. Copyright 2019, Elsevier Ltd and Techna Group S.r.l. (c) Optical image of representative as-deposited MAPbI3-xClx thin film. (d), (e), and (f) MAPbI3-xClx films exposed to O3, H2O, and acetic acid (AA), respectively. (g) XRD spectra of corresponding films. Reproduced with permission from ref. [120]. Copyright 2013, The Royal Society of Chemistry.

图7. OLED分别用Al2O3, 纳米复合层和玻璃盖封装的寿命表征. (a)电压随时间的变化; (b)归一化发光强度随时间变化, 起始光强为1000 cd/m2. 内置图片: OLED活性区域的光学照片. (I) 300 h后未封装器件; (II)玻璃封装的器件; (III) Al2O3封装的器件; (IV)纳米复合层封装1000 h后. (c) OLED器件分别用PE-ALD做钝化层和玻璃封装的J-V曲线, 内置为OLED的结构示意图; (d)有没有PE-ALD钝化的OLED器件在60 ℃, 90%RH条件下发光区域随时间的变化; (e) Ca导电率在较高空气温度和湿度下随时间的变化; (f)叠层Al2O3/MgO不同循环数沉积的器件发光强度随时间的变化.

Figure 7. Lifetime characteristics of Al2O3, NL and glass lid encapsulated OLEDs compared to an OLED without encapsulation (constant-current mode). (a) Voltage-time characteristics. (b) Normalized luminance-time characteristics. Starting luminance 1000 cd/m2. Inset: Photographs of active OLED areas. (I) Without encapsulation taken after 300 h. (II) With glass lid encapsulation, (III) with Al2O3 encapsulation and (IV) with NL encapsulation taken after 1000 h. Reproduced with permission from ref. [131]. Copyright 2009, American Institute of Physics. (c) J-V characteristics of the OLED devices prepared with PE-ALD-based passivation layers and glass-encapsulated devices. The inset shows a schematic configuration of the OLED. (d) The emitting area over time, measured in OLED devices passivated with or without PE-ALD-based films at 60 ℃ and 90% RH. Reproduced with permission from ref. [163]. Copyright 2015, the Owner Societies. (e) The conductivity of Ca with respect to corrosion time under high ambient temperature and humidity. (f) TE-OLEDs luminescence versus continuous operation times for laminated Al2O3/MgO with different cyclic deposition. Reproduced with permission from ref. [101]. Copyright 2016, IOP Publishing Ltd.

图8. (a)不同封装条件下的器件分解情况. 除了标准样, 其余所有器件的测试在空气28 ℃, 60%湿度条件下进行. 器件的初始效率波动范围为3.1%~3.7%. Al2O3/HfO2纳米复合层的沉积经历了反应物停留浸泡的过程. (b)六个封装的OPV器件暴露在空气中的平均值和标准偏差归一化的光伏参数随时间的变化. 虚线和点线分别代表了最好的和最差的器件随时间的变化. 右下角的图是封装后的OPV器件的结构示意图.

Figure 8. (a) Degradation profiles of the devices with various encapsulations. All profiles except for that of the control were measured over storage in air at 28 ℃ with 60% relative humidity. The initial PCE of the devices ranged from 3.1% to 3.7%. The Al2O3/HfO2 nanolaminated films were made with the with-soak process. Reproduced with permission from ref. [155]. Copyright 2009, Elsevier B.V. (b) Average values (symbols) and standard deviation error bars of normalized photovoltaic performance parameters of 6 encapsulated OPVs as a function of time exposure to air. The dashed lines and dotted lines represent temporal evolution for the best and worse OPV device, respectively. The bottom-right panel is a schematic of an encapsulated OPV device. Reproduced with permission from ref. [59]. Copyright 2016, IOP Publishing Ltd.

图9. (a)在Si基底上沉积MgO/S-H纳米复合层4.5个周期的扫描电镜(SEM)截面图; (b)导电率随时间变化的归一化曲线. 依据每一个样品的初始导电率归一化. 黑色的矩形和红色的圆圈分别代表玻璃和薄膜封装. 薄膜封装的样品曲线趋势完美跟随玻璃封装的样品. 内置图展示了Ca测试的示意图; (c)以MLD:ALD循环数比为1:25在Si基底上沉积的4MP/Al2O3膜的透射电子显微镜(TEM)截面图; (d)在85%RH 85 ℃100 nm厚的 Al2O3 薄膜里面不同4MP层的数量条件下Ca导电率随时间的变化. 这个数量代表多层膜里单层4MP的数量, Ca测试百分比的计算是以Ca位点总数为144个情况下, 每次氧化的Ca点的数量.

Figure 9. (a) SEM cross section image of MgO/S-H nanocomposite 4.5 dyads on a Si wafer; (b) normalized conductance curves versus time. Conductance is normalized by the initial value in each sample. The black solid rectangle and red open circle mean glass and thin film encapsulation, respectively. The thin film encapsulated sample perfectly follows the trend of glass lid encapsulation. The inset shows a schematic diagram of the Ca test. Reproduced with permission from ref. [102]. Copyright 2013, Elsevier B.V. (c) A Cross-sectional TEM image of 4MP/Al2O3 multilayered film grown on a Si wafer with MLD:ALD ratio of 1:25. (d) Ca test yield vs time with the variation of a number of 4MP layers in 100 nm-thick Al2O3 thin films under 85% RH at 85 ℃. The number at the legend stands for the number of 4MP monolayers within the multilayered films. Ca test yield (%) was calculated as [(number of Ca dot oxidized at each time)/(total number of Ca dots, 144)]×100. Reproduced with permission from ref. [87]. Copyright 2019, Elsevier B.V.

图10. (a)三个周期有机/无机复合膜最优结构的扫描电镜截面图; (b)多层薄膜的WVTR值随循环周期数的变化; (c)右)封装的PSC器件的结构示意图, 左)封装层的扫描电镜截面图; (d)在50 ℃/50%RH加速老化测试条件下, 器件效率随叠层循环周期数的变化; (e)初始钙钛矿太阳能电池的J-V特性曲线; (f)四个周期的TFE薄膜封装的钙钛矿太阳能电池器件随时间变化的反扫曲线

Figure 10. (a) SEM cross-sectional image of the optimized organic/inorganic hybrid multilayer with 3 dyads; (b) WVTR of the optimized multilayers with respect to the increase of the dyad numbers. Reprinted with permission from ref. [38], Copyright (2014) Wiley Periodicals, Inc. (c) Right) Schematic illustration of the encapsulated PSC, and left) The cross-sectional SEM image of the TFE. (d) Shelf life of PSC encapsulated with 1—4 layers of multilayer TFE under an accelerated condition of 50 ℃, 50% RH. The numbers in legend indicate the WVTR of each TFE with unit of g•m-2•d-1. J-V characteristics of (e) pristine PSC and (f) the PSC encapsulated with 4-dyad TFE with respect to the time lapse with reverse scan. Reproduced with permission from ref. [171]. Copyright 2017, Wiley-VCH

图11. (a)三种不同聚合物的光透过率比较; (b)AMO与不同的聚合物复合成的薄膜, Ca膜归一化电导率随时间的变化; (c)封装前后的器件浸泡在不同化学药品里的光学照片; (d)每一种结构层的示意图. IS(无机层/基底), EIS(环氧树脂涂层/无机层/基底), EZIS(环氧树脂-ZrP纳米复合涂层/无机层/基底)

Figure 11. (a) Comparison of transmittance for three kinds of polymer films; (b) the normalized change of electrical conductance of Ca film with composite film of AMO and different polymer as a function of time; (c) photographic images of encapsulated TE-OLEDs before and after chemical agent bath; (d) a schematic diagram of each layered structure; IS (inorganic layer/substrate), EIS (epoxy coating/inorganic layer/substrate), and EZIS (epoxy-ZrP nanocomposite coating/inorganic layer/substrate). Reproduced with permission from ref. [93]. Copyright 2017, Elsevier B.V.

Device structure	Deposition temperature/℃	WVTR/ (g•m^-2•d^-1)	PCE/%	Aging condition and stablity tests	Ref.
ITO/PEDOT:PSS/MAPbI₃/PCBM/ ALD ZnO/Ag NWs/50 nm ALD Al₂O₃ coated PET	100	9×10^-4	10.55	being exposed to ambience (30 ℃, 65% relative humidity) for more than 40 d	^[131]
FTO/bl-TiO₂/mp-TiO₂/(FAPbI₃)_0.87-(MAPbBr₃)_0.13/PTAA/Au/ALD Al₂O₃/pV3D3	60	1×10^-4	18.2±1.3	maintained 97% of its original efficiency after 300 h of exposure at 50 ℃ and 50% RH.	^[171]
FTO/ALD-NiO/Cs_0.05MA_0.95PbI₃/ PCBM/BCP/ALD-AZO/Ag /50 nm ALD Al₂O₃	100	—	18.4	maintaining 86.7% of the initial PCE under continuous1 Sun illumination at 85 ℃ in ambient air with constant near maximum power point over 500 h	^[160]
ITO/NIO/CH₃NH₃PbI₃/PC₆₁BM/ALD TiO₂/Ag/60 nm ALD Al₂O₃	60	—	—	93% of the initial PCE remained after being stored in ambient for a thousand hours	^[113]
FTO/bl-TiO₂/mp-TiO₂/MAPbI₃/Spiro-OMeTAD/Au/16 nm ALD Al₂O₃	60	—	17.4	exhibited a final PCE of 12.4% after more than 2250 h of storage underambient conditions (from original PCE=16.4%)	^[132]
FTO/bl-TiO₂/mp-TiO₂/(FAPbI₃)_0.85-(MAPbBr₃)_0.15/PTAA/Au/50 nm Al₂O₃	95	1.84×10^-2	15.3	with less than 4% drop in PCE after 7500 h (>10 months) of exposure to 50%RH under room temperature.	^[194]
ITO/SnO₂/MAPbI₃/Spiro-MeOTD/Ag/Alucone/ALD Al₂O₃	50	1.3×10^-5	17.01	at 80% relative humidity and 30 ℃ for over 2000 h while preserving 96% of its initial performance	^[124]
FTO/SnO₂/(FA_0.83MA_0.17)_0.95Cs_0.05-PbI_2.5Br_0.5/Spiro-OMeTAD/Au/300 cycles ALD Al₂O₃	75	—	19.4	retaining 84% of its initial efficiency by the end of 300 d stored in ambient conditions	^[124,133]

Device structure	Deposition temperature/℃	WVTR/ (g•m^-2•d^-1)	PCE/%	Aging condition and stablity tests	Ref.
ITO/PEDOT:PSS/MAPbI₃/PCBM/ ALD ZnO/Ag NWs/50 nm ALD Al₂O₃ coated PET	100	9×10^-4	10.55	being exposed to ambience (30 ℃, 65% relative humidity) for more than 40 d	^[131]
FTO/bl-TiO₂/mp-TiO₂/(FAPbI₃)_0.87-(MAPbBr₃)_0.13/PTAA/Au/ALD Al₂O₃/pV3D3	60	1×10^-4	18.2±1.3	maintained 97% of its original efficiency after 300 h of exposure at 50 ℃ and 50% RH.	^[171]
FTO/ALD-NiO/Cs_0.05MA_0.95PbI₃/ PCBM/BCP/ALD-AZO/Ag /50 nm ALD Al₂O₃	100	—	18.4	maintaining 86.7% of the initial PCE under continuous1 Sun illumination at 85 ℃ in ambient air with constant near maximum power point over 500 h	^[160]
ITO/NIO/CH₃NH₃PbI₃/PC₆₁BM/ALD TiO₂/Ag/60 nm ALD Al₂O₃	60	—	—	93% of the initial PCE remained after being stored in ambient for a thousand hours	^[113]
FTO/bl-TiO₂/mp-TiO₂/MAPbI₃/Spiro-OMeTAD/Au/16 nm ALD Al₂O₃	60	—	17.4	exhibited a final PCE of 12.4% after more than 2250 h of storage underambient conditions (from original PCE=16.4%)	^[132]
FTO/bl-TiO₂/mp-TiO₂/(FAPbI₃)_0.85-(MAPbBr₃)_0.15/PTAA/Au/50 nm Al₂O₃	95	1.84×10^-2	15.3	with less than 4% drop in PCE after 7500 h (>10 months) of exposure to 50%RH under room temperature.	^[194]
ITO/SnO₂/MAPbI₃/Spiro-MeOTD/Ag/Alucone/ALD Al₂O₃	50	1.3×10^-5	17.01	at 80% relative humidity and 30 ℃ for over 2000 h while preserving 96% of its initial performance	^[124]
FTO/SnO₂/(FA_0.83MA_0.17)_0.95Cs_0.05-PbI_2.5Br_0.5/Spiro-OMeTAD/Au/300 cycles ALD Al₂O₃	75	—	19.4	retaining 84% of its initial efficiency by the end of 300 d stored in ambient conditions	^[124,133]

表3. ALD-Al2O3封装在不同的PSCS器件结构中, 沉积温度、WVTR、PCE的封装器件及稳定性的试验结果

Table 3. ALD-Al2O3 encapsulation in different device structures of PSCS,including deposition temperature, WVTR, PCE of the encapsulated devices and the results of the stability tests

表3. ALD-Al2O3封装在不同的PSCS器件结构中, 沉积温度、WVTR、PCE的封装器件及稳定性的试验结果

Table 3. ALD-Al2O3 encapsulation in different device structures of PSCS,including deposition temperature, WVTR, PCE of the encapsulated devices and the results of the stability tests

Material	Temperature/℃	WVTR/ (g•m^-2•d^-1)	J_sc/ (mA•cm^-2)	PCE/%	Lifetime	Cycle	Thickness/nm	Ref.
ITO/PEDOT:PSS/ Polymer:PCBM/Ca/Al	80	—	5.31	1.93	300 h/72%	1000	100(Al₂O₃)	^[137]
ITO/PEDOT:PSS/ rrP3HT:PC₇₀BM/Yb/Al	70	—	—	—	250 min/95%	3000	330(Al₂O₃)	^[136]
ITO/PEIE/P3HT:ICBA/ MoO₃/Ag	30	—	9	3	>1400 h/88%	—	10(TiO₂)/10(Al₂O₃)/ 400(SiN_x)/30(Al₂O₃)/ 10(TiO₂)	^[59]
ITO/PEDOT:PSS/ P3HT:PCBM/AlO_x/Pt	100	—	7	2.9	>2000 h/30%	999	≤100	^[112,135]
OPV	90	1.29×10^-5	—	—	—	—	500(pV4D4)/35(Al₂O₃)/200(pV4D4)/35(Al₂O₃)/200(pV4D4)/35(Al₂O₃)	^[38]
ITO/PEDOT:PSS/ P3HT:PCBM/Al	100	<5×10^-4	8.3	3.1	>450 h/50%	480	27(AlO_x/HfO_x cycle 30)	^[37]
ITO/MoO_x/ClAlPc/ ClAlPc:C₆₀/C₆₀/BCP/Ag	100	<5×10^-4	—	1.7	>1200 h/10%	480	27(AlO_x/HfO_x cycle 30)	^[37]
ITO/PEDOT:PSS/ P3HT:PCBM/Al	140	—	9.15	2.7	500 h/80%	210	18(Al₂O₃)	^[119]
ITO/PEDOT:PSS/ P3HT:PCBM/Al	140	—	9.98	3.66	640 h/50%	104	26(Al₂O₃/HfO₂ cycle 52)+UV-curable epoxy resin film	^[195]
ITO/pentacene/C₆₀/ BCP/Al	100	—	11.1	2.8	6145 h/94%	—	200(Al₂O₃)	^[134]

表4. 不同ALD封装的有机太阳能电池的光伏性能总结

Table 4. Photovoltaic performance summary of organic solar cells with different ALD encapsulation

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低温原子层沉积封装技术在OLED上的应用及对有机、钙钛矿太阳能电池封装的启示

Application of Low Temperature Atomic Layer Deposition Packaging Technology in OLED and Its Implications for Organic and Perovskite Solar Cell Packaging

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