激光剥蚀电感耦合等离子体质谱分析硫化铅量子点光电器件多层薄膜厚度  

Laser Ablation Inductively Coupled Plasma Mass Spectrometry Analysis of Multilayer Thin Film Thickness of PbS Quantum Dot Photovoltaic Devices

作　　者：张鼎文 李会来 李凡 郭伟[2] 靳兰兰[2] 胡圣虹[1] ZHANG Ding-Wen;LI Hui-Lai;LI Fan;GUO Wei;JIN Lan-Lan;HU Sheng-Hong(School of Earth Sciences,China University of Geosciences(Wuhan),Wuhan 430074,China;State Key Laboratory of Biogeology and Environmental Geology,China University of Geosciences(Wuhan),Wuhan 430074,China)

机构地区：[1]中国地质大学(武汉)地球科学学院,武汉430074 [2]中国地质大学(武汉)生物地质与环境地质国家重点实验室,武汉430074

出　　处：《分析化学》2024年第10期1609-1618,共10页Chinese Journal of Analytical Chemistry

基　　金：国家重点研发计划项目(No.2021YFC2903003)资助。

摘　　要：随着薄膜沉积工艺技术的进步以及对光伏材料的质量要求不断提高,准确获得多层纳米薄膜材料各薄层的厚度已成为必要条件。激光剥蚀电感耦合等离子体质谱(LA-ICP-MS)已成功应用于金属镀层等薄膜材料的深度剖析,但元素信号的混合效应严重影响层界面的判别和薄层厚度测定的准确性。本研究采用具有高深度分辨率的LA-ICP-MS方法测定了PbS胶体量子点(Colloidal quantum dot,CQD)光电器件薄膜的厚度,对比了不同激光参数对剥蚀过程中元素信号混合效应的影响。结果表明,通过优化激光能量密度和斑径等参数,可改善激光与多层纳米薄膜材料的剥蚀行为,减少元素信号的混合。采用自行研制的气溶胶快速洗出小体积管式剥蚀池可有效地提高气溶胶的传输效率,洗出时间低至(1.60±0.6)s,与商用圆柱形剥蚀池相比,多层薄膜样品的深度剖面轮廓更清晰。层交界面的深度剖析轮廓表明,PbS量子点层剥蚀时呈现明显的热熔蚀现象,PbS/ZnO的层界面元素信号混合严重。在激光能量2.5 J/cm^(2)、斑径32μm和剥蚀频率1 Hz的条件下,PbS CQD光电器件中Au、PbS和ZnO层的平均剥蚀速率分别为(60±2)、(69±5)和(22±2)nm/pulse,深度分辨率分别为(26±2)、(213±11)和(68±6)nm。利用本方法对同一批次的PbS CQD光电器件薄膜厚度进行测定,测定结果与扫描电子显微镜(SEM)测量值具有良好的一致性,相对偏差小于6%。本方法可准确测定纳米级多层薄膜样品的厚度,为提高光伏器件性能和监控产品质量提供了新方法。Accurate determination of the thickness of multi-layered nanofilm materials is of great importance to advance the development of thin film deposition technology and ensure the quality assurance of photovoltaic materials.Laser ablation inductively coupled plasma mass spectrometry(LA-ICP-MS)has been successfully employed for depth profiling of thin film materials,such as metal coatings.However,the accuracy of interface discrimination and thin layer thickness measurement is limited by the mixing effects of elemental signals.In this work,a high-depth resolution method for measuring the thin film thickness of lead sulfide(PbS)colloidal quantum dot(CQD)photovoltaic devices by LA-ICP-MS was introduced.The influence of different laser parameters on the mixing effects of element signals during the ablation process was compared,and the results showed that the laser ablation behavior of multi-layered nanofilm materials were improved and the mixing of element signals were reduced by optimizing parameters such as laser energy density and spot diameter.Meanwhile,a self-developed aerosol rapid wash-out small volume tubular ablation cell was used to effectively improve the aerosol transport efficiency,and the wash-out time of aerosol was(1.60±0.6)s.Compared with commercial cylindrical ablation cells,the depth profile of multi-layer thin film samples was clearer.The depth profile of the interlayer interface showed a significant melting phenomenon during the ablation of the PbS CQD layer,leading to severe mixing of elemental signals at the PbS/ZnO layer interface.Under the conditions such as 2.5 J/cm^(2)laser energy,32μm spot diameter,and 1 Hz repetition rate,the average ablation rates of Au,PbS and ZnO layers in PbS CQD photovoltaic devices were(60±2)nm/pulse,(69±5)nm/pulse,and(22±2)nm/pulse,with depth resolution of(26±2)nm,(213±11)nm,and(68±6)nm,respectively.The thickness of PbS CQD photovoltaic device films from the same batch was determined,and the test results exhibited good consistency with scanning electron microsco

关 键 词：激光剥蚀电感耦合等离子体质谱 深度剖析 薄膜厚度 剥蚀池 光伏薄膜材料 硫化铅 

分 类 号：O657.63[理学—分析化学] TB383.2[理学—化学]