The reduction of TiBr4·2THF using
K[BEt3H] yields the hydrogen-free organosol Ti·0.5THF.
According
to the HRTEM (high-resolution transmission electron microscopy), EDX
(energy-dispersive X-ray) fluorescence,
XPS (X-ray photoelectron spectroscopy), XANES (X-ray absorption near
edge structure), and EXAFS (extended
X-ray absorption fine structure) data, this nanoparticulate metal
colloid consists of very small Ti particles in the
zerovalent state, stabilized by intact THF molecules.
Transition metal colloids are potential precursors of heterogeneous catalysts with application to selective chemical reactions. Sample preparation techniques are described. Experimental details are given of the characterization of these often air-sensitive particles by X-ray photoelectron and X-ray absorption spectroscopy. First results obtained with both techniques for a Rh-colloid show that the metal is mainly present in the zerovalent chemical state. But the spectra indicate further chemical states of Rh which can be assigned to the outermost metal atoms of the colloid interacting with organic ligands or to the educt Rh-halides.
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