J. Osuna et al., SYNTHESIS, CHARACTERIZATION, AND MAGNETIC-PROPERTIES OF COBALT NANOPARTICLES FROM AN ORGANOMETALLIC PRECURSOR, Journal of physical chemistry, 100(35), 1996, pp. 14571-14574
THF solutions of the new organometallic precursor Co(eta(3)-C8H13)(eta
(4)-C8H12) react with 3 bar dihydrogen in the presence of polyvinylpyr
rolidone (PVP) at three different temperatures, namely, 0, 20, and 60
degrees C to give colloidal solutions containing fee cobalt particles
of respectively less than or equal to 1 nm (Cell, 1) and ca. 1.5 nm (C
ell, 2 and Cell, 3) mean sizes, as evidenced by HREM analysis. All col
loids react with carbon monoxide to give new colloids (Cell, 1'-3') di
splaying broad CO stretches near 2000 and 1890 cm(-1) on their infrare
d spectra recorded in KBr disks. The magnetic behavior of the colloids
was studied by SQUID techniques. Cell, 1-3 display a typical superpar
amagnetic behavior with blocking temperatures in the range 9-10 K. Fro
m magnetization studies above and below the blocking temperature, it w
as possible to determine that Cell, 3 shows a mean size of 1.6 nm and
a very narrow size distribution. Because of a magnetic surface effect,
the magnetic moment per atom (nu(Co) = 1.94 +/- 0.04 mu(B)) appears s
ignificantly larger than the value admitted for bulk cobalt. In contra
st, Cell, 2' shows a weak magnetization and disappearance of the block
ing temperature as a result of CO coordination.