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Synthesis and Properties of Materials | Updated：2022-10-19
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In -situ Synthesis and Performance of Sodium Chloride/ Cesium Lead Bromide Perovskite Composite Film Enhanced Publication- Chinese Journal of Luminescence Vol.43, Issue 8, (2022)
- Affiliations：College of Optical and Electronic Technology， China Jiliang University,Hangzhou,China,310018
- Author bio：
- Funds：National Natural Science Foundation of China(62075203;51832005;12104431;51702339);Preeminence Youth Science Fund Project of Zhejiang Province(LR19F050001);Key Research and Development Program of Zhejiang Province(2021C05005);The Fundamental Research Funds for The Provincial Universities of Zhejiang Province(2022YW02)
- DOI：10.37188/CJL.20220129 CLC： O482.31
Published：05 August 2022，
Received：10 April 2022，
Revised：25 April 2022，
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戴克城,翟玥,吴娜等.氯化钠/铯铅溴钙钛矿复合薄膜的原位制备及性能[J].发光学报,2022,43(08):1188-1197.
DAI Ke-cheng,ZHAI Yue,WU Na,et al.In-situ Synthesis and Performance of Sodium Chloride/ Cesium Lead Bromide Perovskite Composite Film[J].Chinese Journal of Luminescence,2022,43(08):1188-1197.
戴克城,翟玥,吴娜等.氯化钠/铯铅溴钙钛矿复合薄膜的原位制备及性能[J].发光学报,2022,43(08):1188-1197. DOI： 10.37188/CJL.20220129.
DAI Ke-cheng,ZHAI Yue,WU Na,et al.In-situ Synthesis and Performance of Sodium Chloride/ Cesium Lead Bromide Perovskite Composite Film[J].Chinese Journal of Luminescence,2022,43(08):1188-1197. DOI： 10.37188/CJL.20220129.
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"data": "全无机铯铅卤钙钛矿因其优异的光电性能受到广泛关注。然而，薄膜较差的稳定性和制备中大量昂贵且有毒有机溶剂的使用，严重阻碍了其商业化应用进程。在本工作中，水溶液被用作配制含氯化钠（NaCl）的钙钛矿前驱液的溶剂。通过一步溶液法获得原位生长的NaCl/CsPbBr"
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"data": "All-inorganic cesium lead halide perovskite film has received extensive attention due to their excellent photoelectric properties. However， the poor stability of the perovskite film and the use of numerous expensive as well as toxic organic solvents during the preparation process severely hinder its commercial application process. In this work， aqueous solution is used as the solvent to prepare a perovskite precursor solution containing with sodium chloride（NaCl）. The "
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"data": "。近年来，将其作为荧光转换薄膜以实现全彩化显示的应用已被提出并得到了广泛研究"
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"data": "。通常，钙钛矿薄膜的制备主要以溶液旋涂法和化学气相沉积法为主"
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"data": "。然而，这些方法普遍存在着有机溶剂大量使用、原材料浪费、制备时间长及成本高等问题。此外，获得的钙钛矿薄膜也会不可避免地在其表面及晶界处形成大量缺陷，进而使得薄膜具有较差的荧光发射及稳定性"
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"data": "。因此，为了满足实际应用需求，通过简便低成本的方法获得具有高荧光性能及稳定性的钙钛矿荧光转换薄膜是十分必要的。"
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"data": "在过去的几年中，已有研究表明通过使用具有特殊官能团的有机分子或疏水性有机聚合物对钙钛矿进行表面处理，可以钝化缺陷并在表面形成保护层，进而大幅提高其光物理性能。吴等利用4,4'-二溴三苯胺（DBTPA）对MAPbI"
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"data": "和DBTPA中的π体系间的相互作用，最终促使钙钛矿的热稳定性得到提高"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "15",
"type": "bibr",
"rid": "R15",
"data": [
{
"name": "text",
"data": "15"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。不同于有机分子后处理策略，采用一步合成法具有更加简便、高效的优势。魏等通过一步溶液旋涂法构建了CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "-MABr准核-壳结构钙钛矿薄膜，归功于MABr壳层对CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "晶体中缺陷态的钝化及对过量电子注入的阻挡，该薄膜表现出优异的光电性能"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "16",
"type": "bibr",
"rid": "R16",
"data": [
{
"name": "text",
"data": "16"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。此外，钟等使用溶剂蒸发法原位制备了MAPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "/聚偏二氟乙烯（PVDF）复合薄膜，该复合薄膜不仅展现出增强的光致发光性能，同时也具有提高的湿度和紫外光照稳定性"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "17",
"type": "bibr",
"rid": "R17",
"data": [
{
"name": "text",
"data": "17"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。基于CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿量子点的过饱和重结晶和乙烯-醋酸乙烯共聚物（EVA）在甲苯中的溶解，李等通过一步法制备了柔性CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "/EVA复合薄膜"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "18",
"type": "bibr",
"rid": "R18",
"data": [
{
"name": "text",
"data": "18"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。得益于EVA基质对钙钛矿量子点的有效保护，薄膜在空气和水溶液中具有长期稳定的发光性能。由此可见，采用一步合成法对钙钛矿进行原位盐/聚合物复合是改善钙钛矿薄膜荧光性能及稳定性的有效策略。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "本文采用价格低廉的无机盐（氯化钠）作为修饰剂，使用水溶液代替有机溶剂来配制钙钛矿前驱体溶液，并在二甲基亚砜溶液的协同作用下通过一步合成法原位制备了NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜。系统研究了原料配比、二甲基亚砜用量及合成温度对薄膜结构和性能的影响。使用时间分辨荧光光谱对薄膜荧光性能的改善进行了分析。此外，还对所制备的薄膜进行了热稳定性及环境稳定性测试。"
}
]
}
]
},
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"data": {
"title": [
{
"name": "text",
"data": "2 实 验"
}
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"level": "1",
"id": "s2"
}
},
{
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"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "2.1 材料"
}
],
"level": "2",
"id": "s2a"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "溴化铯（CsBr，99.5%）、溴化铅（PbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "，99.0%）、氯化钠（NaCl，99.5%）、二甲基亚砜（DMSO，99%，GC）和无水乙醇（≥99.5%，无水级，水分≤0.005%）均购于上海阿拉丁生化科技股份有限公司。上述试剂均为购买后直接使用，无额外的提纯过程。去离子水（DI water，18.25 MΩ·cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "）是通过纯水提纯系统获得的。玻璃基板购买于连云港楚天石英制品有限公司。玻璃基板在使用前先依次经过无水乙醇、去离子水超声清洗10 min，取出后再使用无水乙醇、去离子水各清洗一遍，之后置于真空干燥箱中干燥待用。"
}
]
}
]
},
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"data": {
"title": [
{
"name": "text",
"data": "2.2 NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜的原位制备"
}
],
"level": "2",
"id": "s2b"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "钙钛矿前驱液的制备：将CsBr（85.1 mg）、 PbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "（146.8 mg）和30 mL去离子水放入50 mL烧杯中，在85 ℃加热平台上恒温搅拌2 h至反应物完全溶解，此时前驱液呈澄清状（该条件下制备的前驱液描述为Perovskite solution，简写为PS）。对于复合薄膜样品的前驱液（简写为PS+NaCl），则是在上述反应液中进一步加入NaCl（3 000 mg）来制备，此时NaCl的用量达到了其在溶液中的最大溶解度。具体的配制参数如"
},
{
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"data": {
"text": "表1",
"type": "table",
"rid": "T1",
"data": [
{
"name": "text",
"data": "表1"
}
]
}
},
{
"name": "text",
"data": "所示。"
}
]
},
{
"name": "table",
"data": {
"id": "T1",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "表1"
}
],
"title": [
{
"name": "text",
"data": "配制不同前驱液所需试剂"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Tab.1"
}
],
"title": [
{
"name": "text",
"data": "Reagents needed for the preparation of different precursor solution"
}
]
}
],
"note": [],
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"data": [
{
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"data": "CsBr/mg"
}
]
},
{
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"data": [
{
"name": "text",
"data": "PbBr"
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"data": [
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"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "/mg"
}
]
},
{
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"data": [
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"name": "text",
"data": "NaCl/mg"
}
]
},
{
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"data": [
{
"name": "text",
"data": "H"
},
{
"name": "sub",
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{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "O/mL"
}
]
}
]
],
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[
{
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{
"name": "text",
"data": "PS"
}
]
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{
"name": "text",
"data": "85.1"
}
]
},
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"align": "center",
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"name": "text",
"data": "146.8"
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]
},
{
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"name": "text",
"data": "0"
}
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},
{
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{
"name": "text",
"data": "30"
}
]
}
],
[
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"data": "PS+NaCl"
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"data": "85.1"
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"data": "146.8"
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},
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"data": "3 000"
}
]
},
{
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"data": "30"
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"data": "NaCl/CsPbBr"
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}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜的原位制备：如"
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"text": "图1",
"type": "fig",
"rid": "F1",
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"data": "图1"
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]
}
},
{
"name": "text",
"data": "所示，将上述在85 ℃下溶解好的前驱液快速滴加在玻璃基板上，然后置于90 ℃的真空干燥箱中进行热处理，最终得到NaCl/CsPbBr"
},
{
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"data": [
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"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜。在该过程中，DMSO溶液也用于钙钛矿复合薄膜的制备。如"
},
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"text": "图1",
"type": "fig",
"rid": "F1",
"data": [
{
"name": "text",
"data": "图1"
}
]
}
},
{
"name": "text",
"data": "（b）所示，首先在玻璃基板上滴加DMSO溶液，然后进行前驱液的滴加，最终形成去离子水/DMSO的混合溶剂。最后将基板置于真空干燥箱中进行热处理（加热温度分别为50，60，70，80，90，100 ℃），随着溶剂挥发速率的不同而形成具有不同结晶性的钙钛矿复合薄膜。"
},
{
"name": "xref",
"data": {
"text": "表2",
"type": "table",
"rid": "T2",
"data": [
{
"name": "text",
"data": "表2"
}
]
}
},
{
"name": "text",
"data": "总结了制备不同类型铯铅溴钙钛矿薄膜时所用的原料配比，其中只使用PS前驱液制备的薄膜定义为S1；使用PS+NaCl前驱液制备的复合薄膜定义为S2；使用PS+NaCl前驱液及DMSO溶液制备的复合薄膜定义为S3。"
}
]
},
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"lang": "zh",
"label": [
{
"name": "text",
"data": "图1"
}
],
"title": [
{
"name": "text",
"data": "（a）原位合成法制备NaCl/CsPbBr"
},
{
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"data": [
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"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜；（b）DMSO协同作用制备过程示意图。"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.1"
}
],
"title": [
{
"name": "text",
"data": "（a）Schematic diagram of "
},
{
"name": "italic",
"data": [
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"name": "text",
"data": "in-situ"
}
]
},
{
"name": "text",
"data": " synthesis NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3 "
}
]
},
{
"name": "text",
"data": "perovskite composite film. （b）DMSO synergistic preparation process"
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"data": "2.3 样品表征与测试"
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},
{
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"data": [
{
"name": "text",
"data": "光学显微镜照片是通过奥林巴斯（Olympus）荧光显微镜采集获得的。SEM以及元素mapping通过日本HITACHI公司的SU9010 FE-SEM冷场发射扫描电子显微镜测试获得。TEM及HR-TEM图像通过日本JEOL公司的JEM-2100F测试获得。采用X射线衍射仪（XRD，德国D2 PHASER）对样品的晶体结构进行表征。使用日立F-4600荧光分光光度计对样品的荧光发射光谱进行测试。绝对荧光量子效率由滨松C11347绝对量子效率光谱仪获得，激发波长为365 nm。使用单光子计数荧光寿命光谱仪（英国HORIBA公司Tempro型）获得样品的时间相关发射光谱。"
}
]
}
]
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"title": [
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"name": "text",
"data": "3.1 原料配比对NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜形貌、晶体结构和荧光性能的影响"
}
],
"level": "2",
"id": "s3a"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "采用原位合成法制备铯铅溴钙钛矿薄膜的过程中，原料的不同配比会对其形貌和晶体结构产生影响。首先使用荧光显微镜对90 ℃真空条件下制备薄膜样品的形貌进行研究，如"
},
{
"name": "xref",
"data": {
"text": "图2",
"type": "fig",
"rid": "F2",
"data": [
{
"name": "text",
"data": "图2"
}
]
}
},
{
"name": "text",
"data": "所示。"
},
{
"name": "xref",
"data": {
"text": "图2",
"type": "fig",
"rid": "F2",
"data": [
{
"name": "text",
"data": "图2"
}
]
}
},
{
"name": "text",
"data": "（a）为使用PS前驱液制备的钙钛矿薄膜的荧光显微镜照片，从中可以看到所形成的钙钛矿晶体具有明显团聚的现象且呈现不规则分布。当在前驱液中加入NaCl后，获得的样品分布较均匀，同时形成的钙钛矿晶体具有较小的粒径（"
},
{
"name": "xref",
"data": {
"text": "图2",
"type": "fig",
"rid": "F2",
"data": [
{
"name": "text",
"data": "图2"
}
]
}
},
{
"name": "text",
"data": "（b））。进一步引入DMSO后（DMSO与PS+NaCl前驱液体积比为1∶1），样品的形貌发生明显改变，展现出单一分散的“花状”形貌，如"
},
{
"name": "xref",
"data": {
"text": "图2",
"type": "fig",
"rid": "F2",
"data": [
{
"name": "text",
"data": "图2"
}
]
}
},
{
"name": "text",
"data": "（c）所示。晶粒形貌的改变可能是由于DMSO的引入使得前驱液中溶质的溶解性和溶剂的挥发速率发生变化，进而影响了晶体的成核及生长。蓝光激发下S3薄膜明亮的绿光发射照片证明了NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合结构的形成（"
},
{
"name": "xref",
"data": {
"text": "图2",
"type": "fig",
"rid": "F2",
"data": [
{
"name": "text",
"data": "图2"
}
]
}
},
{
"name": "text",
"data": "（d））。"
}
]
},
{
"name": "fig",
"data": {
"id": "F2",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图2"
}
],
"title": [
{
"name": "text",
"data": "利用不同前驱液制备的S1（a）、S2（b）和S3（c）钙钛矿薄膜的荧光显微镜照片；（d）蓝光激发下S3薄膜的荧光显微镜照片。"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.2"
}
],
"title": [
{
"name": "text",
"data": "Fluorescence microscope images of S1（a）， S2（b） and S3（c） perovskite films prepared with different precursor solutions. （d）Fluorescence microscope image of S3 perovskite film with excitation of blue light."
}
]
}
],
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"data": [
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"data": {
"text": "图3",
"type": "fig",
"rid": "F3",
"data": [
{
"name": "text",
"data": "图3"
}
]
}
},
{
"name": "text",
"data": "（a）~（c）的SEM图像呈现出不同原料配比条件下制备的S1、S2和S3薄膜的表面形貌，其形貌特征与光学显微镜照片结果一致。然而，随着NaCl的复合以及DMSO溶液的引入，薄膜表面均匀性逐渐降低，这一现象也可以从插图展现的薄膜的宏观照片中观察到。为了更好地证明NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合结构的形成，选取了S3薄膜中分散的“花状”晶粒进行元素mapping表征分析，如"
},
{
"name": "xref",
"data": {
"text": "图3",
"type": "fig",
"rid": "F3",
"data": [
{
"name": "text",
"data": "图3"
}
]
}
},
{
"name": "text",
"data": "（d）~（i）所示。从图中可以清楚地观察到Na、Cl、Cs、Pb和Br元素的存在。相较于Cs、Pb和Br元素的分布，Na和Cl元素的含量明显较多，且均匀分布于整个“花状”结构中，表明NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合结构已成功制备。"
}
]
},
{
"name": "fig",
"data": {
"id": "F3",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图3"
}
],
"title": [
{
"name": "text",
"data": "利用不同前驱液制备的S1（a）、S2（b）和S3（c）钙钛矿薄膜的SEM图像，其中左下角的插图为薄膜的宏观照片；（d）~（i）S3薄膜中单个晶粒的元素mapping图像。"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.3"
}
],
"title": [
{
"name": "text",
"data": "SEM images of S1（a）， S2（b） and S3（c） perovskite films prepared with different precursor solutions， and the illustration on the lower left is the macro-photo of films. （d）-（i）Element mapping images of single grain in S3 perovskite film."
}
]
}
],
"subcaption": [],
"note": [],
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{
"name": "p",
"data": [
{
"name": "text",
"data": "为了进一步证实NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合结构的形成，对S3薄膜进行了TEM图像表征，如"
},
{
"name": "xref",
"data": {
"text": "图4",
"type": "fig",
"rid": "F4",
"data": [
{
"name": "text",
"data": "图4"
}
]
}
},
{
"name": "text",
"data": "（a）所示。从图中可以清楚地观察到钙钛矿晶体均匀地复合在NaCl晶体中，其晶粒尺寸大约为22.2 nm。"
},
{
"name": "xref",
"data": {
"text": "图4",
"type": "fig",
"rid": "F4",
"data": [
{
"name": "text",
"data": "图4"
}
]
}
},
{
"name": "text",
"data": "（b）是相关的HR-TEM图像，图中存在位于不同区域的清晰的晶格条纹。其中0.294 nm的晶格间距与CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿晶体的（200）晶面一致，而0.285 nm的晶格间距与NaCl晶体的（200）相关"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "19",
"type": "bibr",
"rid": "R19",
"data": [
{
"name": "text",
"data": "19"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "，这一结果也与"
},
{
"name": "xref",
"data": {
"text": "图4",
"type": "fig",
"rid": "F4",
"data": [
{
"name": "text",
"data": "图4"
}
]
}
},
{
"name": "text",
"data": "（c）测得的XRD结果相符合。"
}
]
},
{
"name": "fig",
"data": {
"id": "F4",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图4"
}
],
"title": [
{
"name": "text",
"data": "（a）~（b）S3钙钛矿薄膜的TEM及HR-TEM图像；（c）S1、S2和S3钙钛矿薄膜的XRD图谱。"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.4"
}
],
"title": [
{
"name": "text",
"data": "（a）-（b）TEM and HR-TEM images of S3 perovskite films. （c）XRD patterns of S1， S2 and S3 perovskite films."
}
]
}
],
"subcaption": [],
"note": [],
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"data": [
{
"name": "xref",
"data": {
"text": "图4",
"type": "fig",
"rid": "F4",
"data": [
{
"name": "text",
"data": "图4"
}
]
}
},
{
"name": "text",
"data": "（c）显示了S1、S2和S3薄膜的XRD衍射图谱。当只使用PS前驱液时，所制备的S1薄膜在15.3°、21.6°、26."
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": " "
}
]
},
{
"name": "text",
"data": "1°和30.8°处呈现明显的衍射峰，分别对应于CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿（PDF#18-0364）的（100）、（110）、（111）和（200）晶面。此外，在11.8°、23.6°、35.6°和48.0°处也存在着明显的CsPb"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "Br"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "5"
}
]
},
{
"name": "text",
"data": "钙钛矿衍射峰（PDF#25-0211），表明使用该前驱液制备的S1薄膜具有由CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "和CsPb"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "Br"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "5"
}
]
},
{
"name": "text",
"data": "钙钛矿构成的混相晶体结构。通常，PbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "在水溶液中具有较低的溶解度，随着水溶液的不断挥发，其析出速度要明显大于CsBr，进而在钙钛矿晶体形成过程中产生较高的铅离子浓度，最终形成混合晶相"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "20",
"type": "bibr",
"rid": "R20",
"data": [
{
"name": "text",
"data": "20"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。在前驱液中加入NaCl后，除了CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "和CsPb"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "Br"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "5"
}
]
},
{
"name": "text",
"data": "钙钛矿特征峰外，在S2薄膜中还可以观察到位于27.4°、31.8°、45.6°和56.6°处的新的衍射峰，这些新的衍射峰与立方相的NaCl晶体结构相关（PDF#05-0628）。随后，DMSO的进一步引入提高了PbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "在体系中的溶解度，使得S3薄膜中钙钛矿的相纯度得以提高，在图谱中只能观察到CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿和NaCl晶体的特征衍射峰。值得注意的是，NaCl晶体的最强衍射峰由S2薄膜的（200）晶面转变为S3薄膜的（222）晶面，表明DMSO的使用对体系中NaCl晶体的生长方向产生一定的影响，这与"
},
{
"name": "xref",
"data": {
"text": "图2",
"type": "fig",
"rid": "F2",
"data": [
{
"name": "text",
"data": "图2"
}
]
}
},
{
"name": "text",
"data": "中晶粒形貌发生改变相符合。此外，我们也发现S3薄膜中CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿（111）晶面的衍射峰位置较S1薄膜相比向大角度方向有0.1°的偏移，表明在CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿晶体中可能有少量的Cl"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-"
}
]
},
{
"name": "text",
"data": "离子引入，进而使得相关衍射峰位置发生改变。对S2和S3薄膜来说，DMSO的引入使28.6°位置的钙钛矿衍射峰有少许的大角度方向偏移。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "随后，在室温下分别对S1、S2和S3薄膜的光学性能进行研究。在365 nm光激发下，所制备薄膜的荧光发射光谱如"
},
{
"name": "xref",
"data": {
"text": "图5",
"type": "fig",
"rid": "F5",
"data": [
{
"name": "text",
"data": "图5"
}
]
}
},
{
"name": "text",
"data": "（a）所示。从图中可以看到，S1薄膜在大约537 nm处具有一个较弱的荧光发射峰。根据文献报道，CsPb"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "Br"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "5"
}
]
},
{
"name": "text",
"data": "钙钛矿的带隙值为3.87 eV"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "21",
"type": "bibr",
"rid": "R21",
"data": [
{
"name": "text",
"data": "21"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "，因而该发射峰只与CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿相关。引入NaCl后，S2薄膜的荧光发射峰位置蓝移到524 nm处，同时发射峰强度明显增强。DMSO的使用进一步增强了S3薄膜中钙钛矿晶体的荧光发射，其发射峰位于约522 nm处，证实DMSO对钙钛矿晶体相纯度的改善。光谱的蓝移和发射的增强一方面是由于薄膜中团聚的钙钛矿晶体的减少引起的"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "22",
"type": "bibr",
"rid": "R22",
"data": [
{
"name": "text",
"data": "22"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "，另一方面也可能与钙钛矿晶体中氯离子的少量引入相关。薄膜的荧光发射特性也可以使用绝对荧光量子效率结果来表征，如"
},
{
"name": "xref",
"data": {
"text": "图5",
"type": "fig",
"rid": "F5",
"data": [
{
"name": "text",
"data": "图5"
}
]
}
},
{
"name": "text",
"data": "（b）所示。在365 nm光激发下，S1、S2和S3薄膜的荧光量子效率值分别为0.8%，6.7%和22.7%。"
}
]
},
{
"name": "fig",
"data": {
"id": "F5",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图5"
}
],
"title": [
{
"name": "text",
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"data": "所占的比例。根据拟合结果获得的相关寿命常量以及根据公式（"
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"data": "所示。在375 nm光激发下，S1、S2和S3薄膜的平均寿命分别为0.9，19.7，24.8 ns。NaCl/CsPbBr"
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"data": "钙钛矿复合薄膜荧光量子效率的提高和平均寿命的延长表明钙钛矿中的部分缺陷位点（如溴空位或表面铅的悬键）受到了NaCl晶体的有效钝化，进而减少了非辐射复合途径"
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"data": "26"
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"data": "48.91"
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"data": "3.2 DMSO用量对NaCl/CsPbBr"
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"data": "钙钛矿复合薄膜晶体结构和荧光性能的影响"
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"data": "上述研究表明DMSO的使用能够改善复合薄膜中钙钛矿晶体的相纯度，为了获得高性能的NaCl/CsPbBr"
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{
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"data": "钙钛矿复合薄膜，我们进一步研究了DMSO用量对薄膜结构和性能的影响。在90 ℃热处理条件下，使用不同比例的DMSO与PS+NaCl前驱液（体积比分别为1∶4、1∶3、1∶2和1∶1）制备薄膜的XRD图谱如"
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"text": "图6",
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"data": "图6"
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"data": "（a）所示。除立方相的NaCl晶体衍射峰外，与CsPbBr"
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"data": "钙钛矿相关的衍射峰也可以在图谱中找到，表明DMSO的用量不会影响最终NaCl/CsPbBr"
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{
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"data": "钙钛矿复合薄膜的形成。此外，NaCl晶体的晶面衍射峰强度随着DMSO用量的增加发生了明显的改变。当DMSO与PS+NaCl前驱液体积比低于1∶3时，（200）晶面相关的衍射峰强度达到最强，这与未使用DMSO时制备的S2薄膜的最强衍射峰晶面一致。当DMSO与PS+NaCl前驱液体积比高于1∶2时，NaCl晶体的最强衍射峰转变为相应的（222）晶面。这一结构变化说明DMSO的用量会影响NaCl/CsPbBr"
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{
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"data": "钙钛矿复合薄膜中NaCl晶体的生长过程。"
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"title": [
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"data": "不同DMSO与PS+NaCl前驱液用量条件下（体积比分别为1∶4，1∶3，1∶2和1∶1）制备的NaCl/CsPbBr"
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{
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"data": "钙钛矿复合薄膜的XRD图谱（a）、发射光谱（b）、荧光量子效率（c）和时间分辨荧光光谱（d）。"
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"data": "Fig.6"
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"title": [
{
"name": "text",
"data": "XRD patterns（a）， emission spectra（b）， photoluminescence quantum yield（c） and time-resolved fluorescent spectra（d） of NaCl/CsPbBr"
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"data": "3 "
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]
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{
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"data": "perovskite composite films prepared with different volume ratios of DMSO and PS+NaCl precursor solution（volume ratios is 1∶4， 1∶3， 1∶2 and 1∶1 respectively）."
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"data": "随后，使用荧光发射光谱、绝对荧光量子效率和时间相关荧光寿命测试对四种复合薄膜的荧光性能进行分析。"
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"data": "（b）是365 nm光激发下薄膜的荧光发射光谱。可以观察到，复合薄膜在绿光区域具有单一的荧光发射特性，且发射峰位置随着DMSO用量的增加逐渐从526 nm蓝移到522 nm。同时，其荧光发射峰强度随着DMSO浓度的增大呈现出先增加后减少的趋势，在DMSO与PS+NaCl前驱液体积比为1∶2时，复合薄膜的荧光发射峰强度达到最强，此时发射峰位置为522 nm。光谱的轻微蓝移与钙钛矿晶粒中Cl"
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"data": "离子的掺杂量相关。从XRD图谱（"
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"text": "图 6",
"type": "fig",
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"data": "图 6"
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"data": "（a））中可以发现，随着DMSO用量的增加，位于28.4°处CsPbBr"
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{
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"data": "钙钛矿相关衍射峰的位置逐渐向大角度方向偏移，表明钙钛矿晶体中Cl"
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"data": "-"
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"data": "离子的引入。"
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"text": "图6",
"type": "fig",
"rid": "F6",
"data": [
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"data": "图6"
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"data": "（c）为在365 nm光激发下测得的复合薄膜的荧光量子效率结果。当DMSO与PS+NaCl前驱液体积比为1∶4、1∶3、1∶2和1∶1时，NaCl/CsPbBr"
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"data": "钙钛矿复合薄膜的荧光量子效率分别为29.5%、43.4%、48.2%和22.7%。"
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"text": "图6",
"type": "fig",
"rid": "F6",
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"data": "图6"
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},
{
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"data": "（d）为在375 nm光激发下获得的荧光衰减光谱。所有的衰减曲线都可以使用双指数函数很好地拟合，相关的寿命常量如"
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"data": {
"text": "表4",
"type": "table",
"rid": "T4",
"data": [
{
"name": "text",
"data": "表4"
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{
"name": "text",
"data": "所示。随着DMSO用量的增加，薄膜的平均寿命呈现出先增大后减小的趋势，平均寿命值分别为31.2，38.2，40.6，24.8 ns。其中，与载流子辐射复合相关的较慢的衰减过程（"
},
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"data": "2"
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]
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{
"name": "text",
"data": "）所占的比例逐渐从1∶4的58.41%增加到1∶2的71.81%，而与载流子猝灭相关的较快的衰减过程（"
},
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"data": [
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}
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},
{
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"data": "1"
}
]
},
{
"name": "text",
"data": "）所占比例逐渐从1∶4的41.59%降低到1∶2的28.19%。这一结果表明DMSO的适量使用可以减少NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜中的非辐射复合位点，从而提高其荧光量子效率并延长荧光发射寿命。"
}
]
},
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"label": [
{
"name": "text",
"data": "表4"
}
],
"title": [
{
"name": "text",
"data": "不同DMSO与PS+NaCl前驱液用量条件下制备的NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜的荧光寿命值"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Tab.4"
}
],
"title": [
{
"name": "text",
"data": "Fluorescence lifetime values of NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": " per‐ovskite composite films prepared with different volume ratios of DMSO and PS+NaCl precursor solution"
}
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"data": "7.5"
}
]
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{
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"data": "41.59"
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{
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{
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"data": "58.41"
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{
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"data": "31.2"
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"data": "1∶3"
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"data": "6.4"
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},
{
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"data": "28.31"
}
]
},
{
"align": "center",
"data": [
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"data": "40.16"
}
]
},
{
"align": "center",
"data": [
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"name": "text",
"data": "71.69"
}
]
},
{
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"data": "38.2"
}
]
}
],
[
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"data": "1∶2"
}
]
},
{
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"data": "7.1"
}
]
},
{
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"data": "28.19"
}
]
},
{
"align": "center",
"data": [
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"data": "42.8"
}
]
},
{
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"data": [
{
"name": "text",
"data": "71.81"
}
]
},
{
"align": "center",
"data": [
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"data": "40.6"
}
]
}
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"data": "1∶1"
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"data": "4.2"
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"data": [
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"data": "53.42"
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"data": [
{
"name": "text",
"data": "28.3"
}
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"data": [
{
"name": "text",
"data": "46.58"
}
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"style": "border-bottom:solid;",
"data": [
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"name": "text",
"data": "24.8"
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"title": [
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"data": "3.3 温度对NaCl/CsPbBr"
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"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜形貌的影响"
}
],
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}
},
{
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"data": [
{
"name": "text",
"data": "为了探究温度对NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜的影响，在DMSO与PS+NaCl两种溶液的体积比为 1∶2条件下，分别对其进行50，60，70，80，90，100 ℃的热处理，所制备复合薄膜的光学显微镜照片如"
},
{
"name": "xref",
"data": {
"text": "图7",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图7"
}
]
}
},
{
"name": "text",
"data": "所示。从图中可以观察到，所有的晶粒都呈现出良好的分散性，而其形貌随着温度的改变具有明显的变化。当热处理温度为50 ℃和60 ℃时，复合薄膜中分布着形貌不规则的立方和三角体晶粒（"
},
{
"name": "xref",
"data": {
"text": "图7",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图7"
}
]
}
},
{
"name": "text",
"data": "（a）~（b））；当温度提高到70 ℃时，复合薄膜中晶粒的形貌开始由三角体向“花状”转变（"
},
{
"name": "xref",
"data": {
"text": "图7",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图7"
}
]
}
},
{
"name": "text",
"data": "（c））；当温度超过80 ℃时，晶粒的形貌完全转变为“花状”，且随着温度升高，晶粒的体积逐渐增大，如"
},
{
"name": "xref",
"data": {
"text": "图7",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图7"
}
]
}
},
{
"name": "text",
"data": "（d）～（f）所示。不同热处理温度下，复合薄膜中晶粒形貌的改变与溶液的过饱和度和晶面生长速度相关。当温度较低时，溶剂的挥发速度较为缓慢，溶液的过饱和度较低，导致晶体的成核及生长速率较慢，晶粒尺寸普遍较小；而随着温度升高，溶剂的挥发速度加快，此时溶液的过饱和度相对增加，晶体的生长速率增大，晶粒的尺寸逐渐增大"
},
{
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"data": [
{
"name": "text",
"data": "["
},
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"name": "xref",
"data": {
"text": "27",
"type": "bibr",
"rid": "R27",
"data": [
{
"name": "text",
"data": "27"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。溶液过饱和度的改变也会导致溶质供应的不均匀，进而影响晶体中不同晶面间的生长速率，使得晶体的形貌发生改变"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
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"data": {
"text": "28",
"type": "bibr",
"rid": "R28",
"data": [
{
"name": "text",
"data": "28"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。"
}
]
},
{
"name": "fig",
"data": {
"id": "F7",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图7"
}
],
"title": [
{
"name": "text",
"data": "不同合成温度下制备的NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜的荧光显微镜照片"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.7"
}
],
"title": [
{
"name": "text",
"data": "Fluorescence microscope images of NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3 "
}
]
},
{
"name": "text",
"data": "perovskite composite films prepared at different temperatures"
}
]
}
],
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"note": [],
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"data": "3.4 NaCl/CsPbBr"
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"data": "钙钛矿复合薄膜稳定性探究"
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{
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"data": [
{
"name": "text",
"data": "为了评估NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜的稳定性，我们对S1、S2和S3薄膜进行热稳定性及环境稳定性的比较研究。"
},
{
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"data": {
"text": "图8",
"type": "fig",
"rid": "F8",
"data": [
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"data": "图8"
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{
"name": "text",
"data": "（a）为薄膜样品在100 ℃下持续加热21 h后的荧光发射强度变化。从图中可以看出，S1薄膜在持续加热条件下具有较快的荧光衰减速率，21 h后，其荧光发射峰强度较原始相比降低到了38%。与之相比，S2和S3薄膜表现出较高的稳定性。S2薄膜在持续加热21 h后，荧光发射峰强度降低到了65%，而S3薄膜的发射峰强度仍保留了原始的73%。这一结果表明DMSO和NaCl的协同作用更有利于提高NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜的热稳定性。同时，S3薄膜也呈现出更优异的环境稳定性，如"
},
{
"name": "xref",
"data": {
"text": "图8",
"type": "fig",
"rid": "F8",
"data": [
{
"name": "text",
"data": "图8"
}
]
}
},
{
"name": "text",
"data": "（b）所示。在温度为25 ℃，湿度为38%RH的室内环境条件下放置60 h之后，S3薄膜仍能保持原始荧光强度的79%，而S1和S2薄膜呈现出相对较快的荧光衰减性能。"
}
]
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"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图8"
}
],
"title": [
{
"name": "text",
"data": "S1、S2和S3钙钛矿薄膜在100 ℃下持续加热21 h（a）以及25 ℃、38%RH室内条件下放置60 h（b）的荧光发射强度变化。"
}
]
},
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"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.8"
}
],
"title": [
{
"name": "text",
"data": "Relative emission intensity of S1， S2 and S3 perovskite films after continuous heating for 21 h at 100 ℃（a） and placing for 60 h at the indoor conditions（25 ℃， 38%RH）（b）."
}
]
}
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"data": [
{
"name": "text",
"data": "本文通过一步法成功制备了原位生长的NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜。在制备过程中，选取水溶液作为溶剂来获得含有NaCl修饰剂的钙钛矿前驱体溶液。随后进一步引入DMSO溶液来改善NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜的结构和性能。通过改变原料配比、DMSO用量及热处理温度，制备的NaCl/CsPbBr"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "钙钛矿复合薄膜在形貌、晶体结构和荧光性能方面发生了明显的改变。研究结果表明NaCl和DMSO的协同作用能够有效钝化复合薄膜中的缺陷，进而提高其荧光发射性能。在DMSO和前驱液体积比达到1∶2、热处理温度为90 ℃时，薄膜具有最佳的绿光荧光发射，此时薄膜的荧光量子效率为48.2%。此外，持续热处理以及环境稳定性实验结果表明NaCl/钙钛矿复合薄膜的稳定性与未复合NaCl钙钛矿薄膜的相比具有极大的提升。在此基础上，后期也将针对当前制备薄膜的均匀性问题，通过对原材料筛选、组分配比、制备工艺等条件进行优化以期获得具有高均匀性、高荧光性能薄膜，进而为柔性、大面积和高稳定性的显示用荧光转换薄膜提供产业化可能。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "本文专家审稿意见及作者回复内容的下载地址： "
},
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"data": {
"text": [
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"data": [
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"data": "戴克城,翟玥,吴娜等.氯化钠/铯铅溴钙钛矿复合薄膜的原位制备及性能[J].发光学报,2022,43(08):1188-1197."
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"text": "戴克城,翟玥,吴娜等.氯化钠/铯铅溴钙钛矿复合薄膜的原位制备及性能[J].发光学报,2022,43(08):1188-1197."
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"data": " Synthesis and Performance of Sodium Chloride/ Cesium Lead Bromide Perovskite Composite Film[J].Chinese Journal of Luminescence,2022,43(08):1188-1197."
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"text": "DAI Ke-cheng,ZHAI Yue,WU Na,et al.In-situ Synthesis and Performance of Sodium Chloride/ Cesium Lead Bromide Perovskite Composite Film[J].Chinese Journal of Luminescence,2022,43(08):1188-1197."
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"fundinggroup": [
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"text": [
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"data": "国家自然科学基金（62075203，51832005，12104431，51702339）； 浙江省省杰出青年基金（LR19F050001）； 浙江省重点研发计划（2021C05005）； 浙江省普通高校基本科研业务费（2022YW02）资助项目"
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"data": "Supported by National Natural Science Foundation of China（62075203，51832005，12104431，51702339）； Preeminence Youth Science Fund Project of Zhejiang Province（LR19F050001）； Key Research and Development Program of Zhejiang Province （2021C05005）； The Fundamental Research Funds for The Provincial Universities of Zhejiang Province（2022YW02）"
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"history": {
"received": "2022-04-10",
"revised": "2022-04-25",
"ppub": "2022-08-05",
"opub": "2022-10-19"
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"supplementary": [],
"journalTitle": "发光学报",
"issue": "8",
"volume": "43",
"originalSource": []
}
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