In Situ Transmission Electron Microscopy Observations of the Growth Process of Fe3O4-Ag Nanoparticles

doi:10.1007/s40195-020-01053-9

Abstract

Abstract:

The properties of nanocrystals are highly dependent on their morphology, composition and structure. To obtain full control over their properties, the behavior of nanocrystals under external stimuli, such as heat treatment, needs to be understood. Herein, to in situ observe their microstructure and morphology changes, Fe₃O₄-Ag heterodimers were selected as a model system. Their structural changes after heat treatment were investigated by in situ transmission electron microscopy. A combination of real-time imaging with elemental analysis enabled observation of the transformation of Fe₃O₄-Ag heterodimers having a loose interface configuration to those with a Janus structure at the atomic scale after heating from room temperature to 600 °C. After incubation at 600 °C for 32 min, two kinds of Janus structures could be seen, including a clear linear interface in the Fe₃O₄-Ag heterodimers and a semi-crescent-shaped interface between the Ag and Fe₃O₄ nanoparticles (NPs). These dynamic observations provide unique insights into NP growth mechanisms, which are essential for understanding and controlling the structure and morphology of nanoparticles.

Key words: In situ TEM, Fe₃O₄-Ag heterodimer, Nanoparticle, Janus structure, Interface

Jing-Hua Liu, Jin-Jun Liu, Qiang Zheng, Bao-Ru Bian, Juan Du. In Situ Transmission Electron Microscopy Observations of the Growth Process of Fe₃O₄-Ag Nanoparticles[J]. Acta Metallurgica Sinica (English Letters), 2020, 33(9): 1283-1288.

Figures/Tables 5

Fig. 1 a TEM images of the as-synthesized Fe3O4-Ag heterodimers, b HRTEM images of Fe3O4-Ag heterodimers. The insets in a and b are the SAED patterns for the Fe3O4-Ag heterodimers and Fast FFT images for the Ag and Fe3O4 nanoparticles, respectively

Fig. 2 Selected bright-field TEM images of Fe3O4-Ag heterodimers with free Ag nanoparticles at room temperature (a), at temperatures ranging from 300 to 600 °C (b-f)

Table 1 Statistical particle size of the Ag and Fe3O4 NPs from room temperature (25 °C) to 600 °C

	25 °C	300 °C (0 s)	500 °C (0 s)	600 °C (2 min 59 s)
Fe₃O₄ size (nm)	11.3 ± 2.0	11.5 ± 2.3	12.0 ± 2.3	12.1 ± 1.7
Ag size (nm)	3.5 ± 0.5	4.7 ± 0.6	5.3 ± 1.20	6.0 ± 1.0

Fig. 3 HAADF-TEM image (a) and HAADF-TEM EDS mapping images of Fe, Ag, and O elements (b), and the corresponding elemental maps for Ag (c), Fe (d) and O (e), respectively

Fig. 4 SAED patterns from a large area of the Fe3O4-Ag nanoparticles after heating at 600 °C for 32 min (a), HRTEM images of a Fe3O4-Ag Janus structure with a clear interface (b) and a Fe3O4-Ag Janus structure with a semi-crescent-shaped interface (c). The insets in b and c are FFT images of the Ag and Fe3O4 nanoparticles

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In Situ Transmission Electron Microscopy Observations of the Growth Process of Fe₃O₄-Ag Nanoparticles

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