Study of Growing Ni Nanoparticles Loaded on Layered Inorganic-Imidazoline Covalently Bonded Hybrids Under a Transmission
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Study of Growing Ni Nanoparticles Loaded on Layered Inorganic‑Imidazoline Covalently Bonded Hybrids Under a Transmission Electron Microscope Kazuko Fujii1 · Keiji Kurashima1 · Hideo Hashizume1 · Shuichi Shimomura1 · Takatsugu Wakahara1 · Toshihiro Ando1 Received: 26 July 2020 / Accepted: 9 September 2020 © Springer Science+Business Media, LLC, part of Springer Nature 2020
Abstract This study investigates nanoclusters loaded on layered inorganic-imidazoline covalently bonded hybrids. To reveal the existence of nanoclusters, transmission electron microscopy (TEM) and selected-area diffraction (SAD) analyses were g2+) as an performed. An imidazolyl group bonded covalently with an inorganic layer, which contained N i2+ (and not M octahedral cation, in the layered hybrids. In this study, the layered hybrids synthesized at 170 and 150 °C are referred to as Ni-Im170 and Ni-Im150, respectively. The TEM observations confirmed the presence of nanoclusters of 1–2 nm in diameter on thin sheets of Ni-Im170 and Ni-Im150. The nanoclusters appeared as dark dots in the bright-field images and were brighter than the thin sheets in dark-field images. The SAD analyses exhibited halo patterns similar to those of phyllosilicates at the beginning of the TEM observations. The TEM analyses further revealed that the nanoclusters in both Ni-Im170 and Ni-Im150 grew into Ni nanoparticles (3–5 nm diameter) under TEM. The SAD analyses demonstrated diffraction patterns with a weak ring with a d-value of 0.20 nm and/or diffraction patterns attributed to Ni exhibiting rings with d-values of 0.20, 0.18, 0.12, and 0.11 nm after the nanocluster growth. Furthermore, in the case of Ni-Im150, drastic growth was observed under TEM, i.e., the diameters increased to approximately 30 nm. Keywords Layered inorganic–organic hybrid · Nanocluster · Ni nanoparticle · Phyllosilicate
1 Introduction Layered inorganic/organic complexes have been extensively investigated as potential candidates for novel solid-state materials with various functionalities and properties (optical, electrical, magnetic properties, etc.). Many layered inorganic/organic complexes have been prepared by intercalating organic species into the interlayer spaces of inorganic materials, such as 2:1 phyllosilicates and layered double hydroxides. The synthesis of layered inorganic–organic hybrids consisting of inorganic layers covalently bonded with Electronic supplementary material The online version of this article (https://doi.org/10.1007/s10904-020-01753-w) contains supplementary material, which is available to authorized users. * Kazuko Fujii [email protected] 1
National Institute for Materials Science (NIMS), 1‑1 Namiki, Tsukuba, Ibaraki 305‑0044, Japan
organic groups has been reported using one-pot synthesis [1–15] and post-grafting [16, 17]. In the present study, such hybrids have been referred to as ‘layered inorganic–organic covalently bonded hybrids’. We have previously reported the synthesis of layered inorganic-imidazoline covalently bonded hybrids [18].
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