The scientific careers of Robert Sinclair and Nestor Zaluzec - A brief sketch.

Robert (Bob) Sinclair and Nestor Zaluzec have been working for many years at the leading edge of developments in electron microscopy techniques and applications. Their distinguished careers and some of their notable scientific achievements are briefly highlighted.

In situ investigation of ordering phase transformations in FePt magnetic nanoparticles.

In situ high-resolution electron microscopy was used to reveal information at the atomic level for the disordered-to-ordered phase transformation of equiatomic FePt nanoparticles that can exhibit outstanding magnetic properties after transforming from disordered face-centered-cubic into the tetragonal L10 ordered structure. High-angle annular dark-field imaging in the scanning transmission electron microscope provided sufficient contrast between the Fe and Pt atoms to readily monitor the ordering of the atoms during in situ heating experiments. However, during continuous high-magnification imaging the electron beam influenced the kinetics of the transformation so annealing had to be performed with the electron beam blanked. At 500°C where the reaction rate was relatively slow, observation of the transformation mechanisms using this sequential imaging protocol revealed that ordering proceeded from (002) surface facets but was incomplete and multiple-domain particles were formed that contained anti-phase domain boundaries and anti-site defects. At 600 and 700°C, the limitations of sequential imaging were revealed as a consequence of increased transformation kinetics. Annealing for only 5min at 700°C produced complete single-domain L10 order; such single-domain particles were more spherical in shape with (002) facets. The in situ experiments also provided information concerning nanoparticle sintering, coalescence, and consolidation. Although there was resistance to complete sintering due to the crystallography of L10 order, the driving force from the large surface-area-to-volume ratio resulted in considerable nanoparticle coalescence, which would render such FePt nanoparticles unsuitable for use as magnetic recording media. Comparison of the in situ data acquired using the protocol described above with parallel ex situ annealing experiments showed that identical behavior resulted in all cases.

Formation of FePt nanoparticles having high coercivity.

Ultrasonication of toluene solutions of the heteropolynuclear cluster complex, Pt3Fe3(CO)15, in the presence of oleic acid and oleylamine affords surface-capped fcc FePt nanoparticles having an average diameter of ca. 2 nm. Self-assembled arrays of these nanoparticles on oxidized Si wafers undergo a fcc-to-fct phase transition at 775 degrees C to form ferromagnetic FePt nanocrystals ca. 5.8 nm in diameter well dispersed on the Si wafer surface. Room-temperature coercivity measurements of these annealed FePt nanoparticles confirm a high coercivity of ca. 22.3 kOe. Such high coercivity for fct FePt nanoparticles might result from use of a heterpolynuclear complex as a single-source precursor of Fe and Pt neutral atoms or from use of ultrasonication to form fcc FePt nanoparticles under conditions of exceptionally rapid heating. Experiments to determine the critical experimental conditions required to achieve such high room-temperature coercivities in ferromagnetic nanoparticles are underway.