After about three decades of development, the polyol process is now widely recognized and practised as a unique soft chemical method for the preparation of a large variety of nanoparticles which can be used in important technological fields. It offers many advantages: low cost, ease of use and, very importantly, already proven scalability for industrial applications. Among the different classes of inorganic nanoparticles which can be prepared in liquid polyols, metals were the first reported. This review aims to give a comprehensive account of the strategies used to prepare monometallic nanoparticles and multimetallic materials with tailored size and shape. As regards monometallic materials, while the preparation of noble as well as ferromagnetic metals is now clearly established, the scope of the polyol process has been extended to the preparation of more electropositive metals, such as post-transition metals and semi-metals. The potential of this method is also clearly displayed for the preparation of alloys, intermetallics and core-shell nanostructures with a very large diversity of compositions and architectures.
In
this work, we propose an original strategy for the functionalization
of aluminum nanoparticles (Al NPs), based on a combination of aryl
diazonium salt chemistry and the photopolymerization iniferter method.
It consists in grafting coupling agents, derived from diazonium salts,
at the surface of Al NPs and in initiating the photopolymerization
of methacrylic acid (MAA) directly from the surface. The hybrid NPs
were fully characterized using XRD, TEM, TGA, and XPS. The results
show that the obtained hybrids exhibit a core-double shell structure,
the metallic core being preserved while a thin natural oxide layer
and a strongly anchored organic shell surround it. The controlled
and living character of the photopolymerization process allowed for
the control of the polymer shell thickness with the polymerization
time. Interestingly, the formation of compact aryl layers derived
from the diazonium salts at the surface of Al NPs appears to provide
an efficient protection against oxidation.
The full quantitative characterization of nanopowders using transmission electron microscopy scattering patterns is shown. This study demonstrates the feasibility of the application of so-called combined analysis, a global approach for phase identification, structure refinement, characterization of anisotropic crystallite sizes and shapes, texture analysis and texture variations with the probed scale, using electron diffraction patterns of TiO2 and Mn3O4 nanocrystal aggregates and platinum films. Electron diffraction pattern misalignments, positioning, and slight changes from pattern to pattern are directly integrated and refined within this approach. The use of a newly developed full-pattern search-match methodology for phase identification of nanopowders and the incorporation of the two-wave dynamical correction for diffraction patterns are also reported and proved to be efficient.
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