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无机材料学报

• 研究论文 •    

电子能量损失谱在BaTiO3基多层陶瓷电容器中的应用研究

吴鲁康1, 傅正钱1, 于子怡1, 杨俊2, 周斌1, 陈学锋1, 许钫钫1   

  1. 1.中国科学院上海硅酸盐研究所,上海 200050;
    2.深圳市宇阳科技发展有限公司,深圳 523686
  • 收稿日期:2025-01-15 修回日期:2025-03-05
  • 作者简介:吴鲁康(2000-), 男, 博士研究生. E-mail: wulukang23@mails.ucas.ac.cn
  • 基金资助:
    国家重点研发计划(2023YFB3508200); 上海市无机材料测试与表征技术平台(19DZ2290700)

Application of Electron Energy Loss Spectroscopy to BaTiO3 Multi-Layer Ceramic Capacitors

WU Lukang1, FU Zhengqian1, YU Ziyi1, YANG Jun2, ZHOU Bin1, CHENG Xuefeng1, XU Fangfang1   

  1. 1. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China;
    2. Shenzhen Yuyang Technology Development Co., Shenzhen 523686, China
  • Received:2025-01-15 Revised:2025-03-05
  • About author:WU Lukang (2000-), male, PhD candidate. E-mail: wulukang23@mails.ucas.ac.cn
  • Supported by:
    National Key R&D Program of China(2023YFB3508200);Shanghai Technical Platform for Testing and Charac-terization on Inorganic Materials (19DZ2290700) 作者简介：吴鲁康(2000-), 男, 博士研究生. E-mail: wulukang23@mails.ucas.ac.cn;WU Lukang (2000-), male, PhD candidate. E-mail: wulukang23@mails.ucas.ac.cn

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摘要： 消费电子、航空航天和国防科研等领域对BaTiO3基多层片式陶瓷电容器(Multi-Layer Ceramic Capacitors, MLCC)的性能要求日益提高。在MLCC复杂制作工艺过程中,元素的分布和偏析会显著影响其相组成、微结构和性能,亟需一个有效的分析手段在微观尺度上对MLCC进行元素的精确解析。基于先进透射电镜的元素分析技术因其亚埃尺度的超高空间分辨率而展现出独特优势。其中,X射线能谱(Energy Dispersive X-ray Spectroscopy, EDS)可快速进行金属元素的定性分析,但其对轻元素O的检测灵敏度较低,且因能量分辨率较低(~130 eV),致使Ba和Ti元素存在谱峰重叠,无法进行准确的定量分析。相比之下,电子能量损失谱(Electron Energy-Loss Spectroscopy, EELS)不仅具有超高能量分辨率(<1.0 eV),而且能够给出化学价态等信息,在MLCC微观尺度元素分析中具有较大的潜力与优势。本工作一方面利用EELS解决了EDS因为谱峰重叠而不能区分Ba和Ti元素的问题;另一方面通过EELS揭示了在较小晶粒中Ti3+离子占比更多,且单晶粒的EELS线扫分析发现烧结过程中Ba的扩散比Ti更容易。基于高空间分辨率的EELS可以提供更为准确和丰富的元素和价态信息,为MLCC的工艺改良和性能优化提供重要支撑。

关键词: 多层陶瓷电容器, 元素分析, 电子能量损失谱, BaTiO3

Abstract: The BaTiO3 multi-layer ceramic capacitors are meeting the growing performance demands in consumer electronics, aerospace and defense research. Distribution and segregation of elements during the complex fabrication process of MLCCs significantly effect on the phase composition, microstructures and hence the performance, which necessitates an effective analytical means capable of accurately resolving the elements of MLCCs at microscopic scales. Elemental analysis techniques integrated with modern transmission electron microscopes (TEM) have unique advantages due to their ultra-high spatial resolution, reaching the sub-Ångström scale. Among them, energy dispersive X-ray spectroscopy (EDS) provides a simple and fast way for qualitative analysis of metallic elements. However, limitations such as its low sensitivity for detecting the light element O, and more critically, its low energy resolution (~130 eV) results in the severe overlap of spectral peaks of Ba and Ti elements, thereby hindering the accurate quantitative analysis of BaTiO3. In contrast, electron energy-loss spectroscopy (EELS) possesses ultra-high energy resolution (<1.0 eV), and can provide additional information regarding chemical valence, etc, thus demonstrating enhanced potentials and advantages in the micro-scale elemental analysis of MLCC. In this work, EELS is employed to address the limitation of EDS in distinguish between Ba and Ti elements due to spectral peaks overlap. In addition, EELS reveals that the proportion of Ti3+ ions is higher in smaller BaTiO3 grains. Meanwhile, EELS line-scan analysis of individual grains indicates that Ba element diffuses more easily than Ti during the sintering process of ceramics. Given its high spatial resolution, EELS offers more accurate and comprehensive information on the elements and valence states, thereby providing potential supports for the process improvement and performance optimization of MLCC.

Key words: multi-layer ceramic capacitors, elemental analysis, electron energy-loss spectroscopy, BaTiO3

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