基于FIB加工技术研究Ag@SiO_x自组织颗粒的内部结构
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摘要
本文采用FIB辐照样品表面和FIB提取样品截面两种方法,尝试获取Ag@SiO_x自组织结构的内部结构信息,分别得到柱状结构和核壳结构两种完全不同的结果。其中提取截面的方法可以在保留样品初始形貌的同时获取真实内部结构信息,结合EDS能谱,可以确定,半球状SiO_x颗粒包覆在实心银椭球体上表面,Ag@SiO_x自组织结构是一种粒子包覆型核壳结构。有序柱状结构并不反映样品真实内部结构,其产生与离子束的选择性刻蚀有关。
In this paper, two methods are used to investigate the microstructure of self-assembly Ag@SiO_x by focused ion beam(FIB). Ordered columnar arrays are achieved by FIB surface irradiation. Core-shell structure is observed by FIB cross-section lift-out. It is revealed that the microsphere is a kind of particle coated core-shell structure. In detail, separated hemi-spherical SiO_x particles distributed in hexagon are coated on the top surface of ellipsoidal silver. Ordered columnar arrays are believed to form under different etching rates related with material species on the surface. SiO_x with slower etching rate acts as a mask so that the columns arrange regurlarly just as the hemi-spherical SiO_x particles and the columnar direction is in accordance with the incident direction of ion beam.
In this paper, two methods are used to investigate the microstructure of self-assembly Ag@SiO_x by focused ion beam(FIB). Ordered columnar arrays are achieved by FIB surface irradiation. Core-shell structure is observed by FIB cross-section lift-out. It is revealed that the microsphere is a kind of particle coated core-shell structure. In detail, separated hemi-spherical SiO_x particles distributed in hexagon are coated on the top surface of ellipsoidal silver. Ordered columnar arrays are believed to form under different etching rates related with material species on the surface. SiO_x with slower etching rate acts as a mask so that the columns arrange regurlarly just as the hemi-spherical SiO_x particles and the columnar direction is in accordance with the incident direction of ion beam.
引文
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[14 ] MELNGAILIS J. Focused ion beam technology and applications[J]. Journal of Vacuum Science & Technology B, 1987, 5(2):469-495.
[15] 谢进,江素华,王家楫,等. 聚焦离子束刻蚀性能的研究[J]. 半导体学报,2001,22(2):151-155.
[2] 贾佳琦,邢远,史为,等. 聚焦离子束技术制备超薄TEM样品—X2样品台的应用[J]. 电子显微学报, 2016, 35(1):70-74.
[3] 王雪丽, 张伟, 贾志宏,等. 聚焦离子束技术制备与样品表面平行的TEM样品[J]. 电子显微学报, 2013, 32(5):420-425.
[4] CHEN L, HABLER G, BALDWIN L C, et al. An improved FIB sample preparation technique for site-specific plan-view specimens: a new cutting geometry[J]. Ultramicroscopy, 2018, 184(Pt A):310-317.
[5] GARG V, MOTE R G, FU J. FIB fabrication of highly ordered vertical Gaussian pillar nanostructures on silicon[C]. IEEE International Conference on Nanotechnology,2017:707-712.
[6] 彭开武. FIB/SEM双束系统在微纳米材料电学性能测试中的应用[J]. 电子显微学报, 2016, 35(1):75-80.
[7] OI T, ENOMOTO S, NAKAO T, et al. Three-dimensional intracellular structure of a whole rice mesophyll cell observed with FIB-SEM[J]. Ann Bot, 2017, 120(1):21.
[8] 马勇, 钟宁宁, 黄小艳,等. 聚集离子束扫描电镜(FIB-SEM)在页岩纳米级孔隙结构研究中的应用[J]. 电子显微学报, 2014, 33(3):251-256.
[9] MBAREK S, DHERBÉCOURT P, LATRY O, et al. Short-circuit robustness test and in depth microstructural analysis study of SiC MOSFET[J]. Microelectronics Reliability, 2017,76:527-531.
[10] SEKITANI T, YOKOTA T, ZSCHIESCHANG U, et al. Organic nonvolatile memory transistors for flexible sensor arrays[J]. Science,2009,326(5959):1516-1519.
[11] 吴宇虎, PAO Y H. 一种有效的铝材料内部微结构观察分析方法[J]. 固体电子学研究与进展,2000,20(3):318-323.
[12] 韩伟, 肖思群. 聚焦离子束(FIB)及其应用[J]. 中国材料进展, 2013(12):716-727.
[13] ZHANG X N,ZHANG C R,LI Z,et al. Self-assembly of Ag/SiOx spherules in triangular pattern on strained surface of primary particles[J]. Applied Physics Letters, 2004,85 (16): 3570-3571.
[14 ] MELNGAILIS J. Focused ion beam technology and applications[J]. Journal of Vacuum Science & Technology B, 1987, 5(2):469-495.
[15] 谢进,江素华,王家楫,等. 聚焦离子束刻蚀性能的研究[J]. 半导体学报,2001,22(2):151-155.