This work illustrates that a variety of nanowire microstructures can be obtained either by controlling the nanowire formation kinetics or by suitable thermal processing of as-deposited nanowires with nonequilibrium metastable microstructure. In the present work, 200-nm diameter Ag–Ni nanowires with similar compositions, but with significantly different microstructures, were electrodeposited. A 15 mA deposition current produced nanowires in which Ag-rich crystalline nanoparticles were embedded in a Ni-rich amorphous matrix. A 3 mA deposition current produced nanowires in which an Ag-rich crystalline phase formed a backbone-like configuration in the axial region of the nanowire, whereas the peripheral region contained Ni-rich nanocrystalline and amorphous phases. Isothermal annealing of the nanowires illustrated a phase evolution pathway that was extremely sensitive to the initial nanowire microstructure.

In the present work, Pt nanoparticles were produced from a reaction mixture containing a trace amount of cobalt carbonyl salt acting as a shape inducer. Nanoparticle shape evolution during reaction mixture reflux was monitored by characterizing particles extracted from the reaction mixture at different times. It was observed that 5 min of reflux produced spherical nanoparticles, 30 min of reflux produced cube shaped nanoparticles, and 60 min of reflux produced truncated octahedron morphology nanoparticles. It is illustrated that during nanoparticle synthesis the reflux process can provide energy needed for shape transformation from a metastable cube morphology to a truncated octahedron morphology which is thermodynamically the most stable geometry for fcc crystals. An optimization of the reaction reflux is thus needed for isolating metastable shapes.

A series of atom probe and transmission electron microscopy (TEM) studies have been performed to quantify minute compositional fluctuations in Fe55Pt45 thin films during the A1 to L10 phase transformation. The atom probe specimens were analyzed in an Imago Local Electrode Atom Probe (LEAP®) at a target evaporation of 0.5%, a pulse fraction of 20% and a temperature of 120K. We noted a propensity of fracture failures in the LEAP with this material at lower temperatures. The atom probe reconstruction showed small levels of Pt segregation at grain boundaries in the as-deposited films. Fresnel-contrast TEM imaging confirmed high density fluctuations in these boundaries. Upon annealing at 600°C for 10 minutes, the film transformed from A1 to L10 and the grain boundaries become Fe enriched as compared to the as-deposited film.

Self-assembled FePt nanoparticle arrays are candidate structures for ultrahigh density magnetic storage media. One of the factors limiting their application to this technology is particle-to-particle compositional variation. In the present study, an analysis is provided for the formation mechanism of FePt nanoparticles synthesized from the thermal decomposition of Fe(CO)5 and the reduction of FeCl2 by superhydride. In both processes, Pt rich seeds initially form from the reduction of Pt acetylacetonate. The particle formation mechanism has been studied by extracting particles at different stages of the synthesis and individually determining particle-to-particle composition by STEM-XEDS. In the case Fe(CO)5, the Fe is gradually incorporated into the Pt seeds and produces a wide variation in compositional distribution about the mean value. In contrast, the FeCl2 has a nearly instantaneous shift in composition to the average value with the introduction of the superhydride reducing agent. The discrepancies in compositional uniformity between the two processes will be discussed in terms of the intrinsic differences between the different precursors.