Atom Probe Analysis of Nanoparticles Through Pick and Coat Sample Preparation

Atom Probe Analysis of Nanoparticles Through Pick and Coat Sample Preparation
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通过拾取和涂覆样品制备对纳米粒子进行原子探针分析

DOI:
10.1017/s1431927621000465
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发表时间:
--
影响因子:
2.8
通讯作者:
P.J. Felfer
P.J. Felfer
中科院分区:
工程技术4区
文献类型:
--
作者:
J.P. Josten;P.J. Felfer

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在原子探针中分析纳米颗粒的能力常常受到样品制备复杂性的限制。在这项工作中,我们提出了一种方法,在扫描电子显微镜提升出单个纳米粒子。首先,将纳米颗粒分散在花边碳网格上,然后定位在尖锐的基底尖端上,并通过物理气相沉积在所有侧面上涂覆金属基质。组成和结构的见解提供了球形金纳米粒子和银和铜的偏析在银氧化铜纳米棒中显示在3D原子图。使用标准的原子探针重建算法,数据质量受到典型的标准重建工件的异质标本(轨迹畸变)和选择合适的涂层的颗粒。这种方法可以应用于各种无支撑的独立纳米粒子,通过相关技术实现粒子的预选,并可靠地产生定义明确的结构化样品。唯一的先决条件是纳米颗粒必须足够大以进行操作,这是针对尺寸低至约50 nm的纳米颗粒进行的。
The ability to analyze nanoparticles in the atom probe has often been limited by the complexity of the sample preparation. In this work, we present a method to lift–out single nanoparticles in the scanning electron microscope. First, nanoparticles are dispersed on a lacey carbon grid, then positioned on a sharp substrate tip and coated on all sides with a metallic matrix by physical vapor deposition. Compositional and structural insights are provided for spherical gold nanoparticles and a segregation of silver and copper in silver copper oxide nanorods is shown in 3D atom maps. Using the standard atom probe reconstruction algorithm, data quality is limited by typical standard reconstruction artifacts for heterogeneous specimens (trajectory aberrations) and the choice of suitable coatings for the particles. This approach can be applied to various unsupported free-standing nanoparticles, enables preselection of particles via correlative techniques, and reliably produces well-defined structured samples. The only prerequisite is that the nanoparticles must be large enough to be manipulated, which was done for sizes down to ~50 nm.
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