燃料电池FIB-SEM连续切片中Ni–YSZ的成分衬度研究

高  尚^#*，黄梦诗，冉  朋，范光涛，张天宇^#，徐心海，孙  千，陈涵铭^*

（1. 哈尔滨工业大学（深圳） 材料科学与工程学院，广东 深圳 518055；2. 广东省半导体光电材料与智能光子系统重点实验室  广东  深圳 518055；3. 哈尔滨工业大学（深圳） 机电工程与自动化学院，广东 深圳 518055；4. 华南理工大学 材料科学与工程学院，广东 广州 510640）

摘   要   固体氧化物燃料电池Ni-YSZ界面的三维表征对理解其性能演化具有重要意义，而FIB-SEM连续切片技术中的成分衬度优化是实现精确表征的关键。针对Ni-YSZ的成分衬度表征难题，系统优化了FIB-SEM连续切片技术的成像参数。通过对比分析背散射电子与二次电子信号的成像机制，揭示了背散射电子因YSZ与Ni的平均原子序数相近而难以区分两相的本质原因。进一步实验表明，低加速电压(1.5 kV)下二次电子信号可有效利用两相功函数差异提升成分衬度，但需解决荷电效应与取向衬度干扰的双重影响：Inlens探测器虽在短时照射下呈现清晰的Ni-YSZ相界，但其衬度易因荷电积累发生反转；SE2探测器虽在连续切片中稳定性更佳，但受取向衬度干扰严重。基于此，建立了以1.5 kV加速电压下Inlens与SE2探测器协同采集为核心的优化方案，在抑制荷电效应与取向衬度干扰的同时，实现了高质量的相分割。该方案在实际的FIB-SEM连续切片中表现出良好的适用性，为燃料电池电极微观结构的精确表征提供了新的技术途径，对多相复合材料的FIB-SEM表征具有普适性参考价值。

关键词   固体氧化物燃料电池；Ni-YSZ界面；FIB-SEM；成分衬度；探测器

中图分类号：TG115.21⁺5.5；TG115.21⁺5.3；TM911.4   文献标识码：B

Study on the compositional contrast of Ni–YSZ in FIB-SEM serial sectioning of fuel cells

GAO Shang^1，2*, HUANG Mengshi^1，2, RAN Peng³, FAN Guangtao³, ZHANG Tianyu¹^#, XU Xinhai³, SUN Qian⁴, CHEN Hanming^3*

(1. Harbin Institute of Technology (Shenzhen)，School of Materials Science and Engineering, Shenzhen Guangdong 518055; 2. Guangdong Provincial Key Laboratory of Semiconductor Optoelectronic Materials and Intelligent Photonic Systems, Shenzhen Guangdong 518055; 3. Harbin Institute of Technology (Shenzhen)，School of Mechanical Engineering and Automation, Shenzhen Guangdong 518055; 4. Harbin Institute of Technology (Shenzhen) ，South China University of Technology, School of Materials Science and Engineering, Guangzhou Guangdong 510640，China)

Abstract    Three-dimensional characterization of the Ni-YSZ interface in solid oxide fuel cells is critical for understanding its performance evolution, with compositional contrast optimization in FIB-SEM serial sectioning being key to achieving precise characterization. To address the challenges in compositional contrast characterization of Ni-YSZ, the imaging parameters of FIB-SEM serial sectioning were systematically optimized. By comparatively analyzing the imaging mechanisms of backscattered electrons (BSE) and secondary electrons (SE), the inherent difficulty of distinguishing the two phases using BSE due to the similar average atomic numbers of YSZ and Ni was revealed. Further experiments demonstrated that secondary electron signals at low accelerating voltage (1.5 kV) could effectively leverage the work function differences between the two phases to enhance compositional contrast, yet issues with charging effects and orientation contrast interference needed to be addressed. The Inlens detector provided clear Ni-YSZ phase boundaries under short illumination but exhibited contrast reversal due to charge accumulation. Conversely, the SE2 detector showed greater stability during serial sectioning but suffered significant interference from orientation contrast. Based on these findings, an optimized imaging protocol was developed, centered on the synergistic acquisition using Inlens and SE2 detectors at an accelerating voltage of 1.5 kV. This approach suppressed charging effects and orientation contrast interference while achieving high-quality phase segmentation. The method demonstrated excellent applicability in actual FIB-SEM serial sectioning and offers a novel technical pathway for precise characterization of electrode microstructures in fuel cells. Furthermore, it provides a broadly applicable reference for FIB-SEM characterization of multiphase composite materials.

Keywords   solid oxide fuel cell；Ni-YSZ interface；FIB-SEM；compositional contrast；detector

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