Klaus Weiss

HRTEM observation of the monoclinic-to-tetragonal (m-t) phase transition in nanocrystalline ZrO2

The orientation relations m(100) || t(001), m[001] || t[110]; m(011) || t(100), m[100] || t[001]; m(100) || t(110), m[001] || t[001]; m(013) || t(116), m[001] || t[001] (indices for the primitive tetragonal cell) have been found between the tetragonal (t) and monoclinic (m) domains during the electron irradiation-induced m-t phase transition observed in-situ with HREM within isolated zirconia nanoparticles. Geometric models of the m-t interfaces are proposed.

Study of partial oxidation of Cu clusters by HRTEM

Cu clusters of diameters less than 10 nm were selected as models to study oxidation as a function of size, chemical composition, and structure. The investigations were performed with high-resolution electron microscopy. It was shown that beginning with multiply twinned particles as stable structures for particles with diameters less than 5 nm and of cuboctahedra for larger particles, in the transitional state between pure metal and oxide both states can coexist within the same particle; this latter can be proved by HRTEM. It was also demonstrated that this is due to incorporating distortions as step dislocations within grain boundaries which can be shown in electron micrographs of high resolution better than 0.18 nm after image processing. The creation of sub-oxides with less reactivity than the pure metal clusters could also be demonstrated leading to morphologies which are different from those of the pure metal.

Structures of clusters

With regard to different preparation techniques of inert gas aggregation for Cu and of aqueous chemical methods for ligand stabilised particles of CdS and Cu the structure of nanoparticles is discussed. In the latter case, long needles of micrometer lengths and nanometer diameters are prepared which have the structure of multiply twinned particles like truncated decahedra. For interpretation purposes high resolution electron microscopy was performed together simultaneously with computer simulations by phase grating approximation or multi-slice technique in combination with image processing.

Preparation of vanadium and vanadium oxide clusters by means of inert gas aggregation

Vanadium clusters were prepared by the inert gas aggregation technique by evaporating V of high purity. Structural characterization was performed by high-resolution transmission electron microscopy. Apart from vanadium clusters of bcc structures in different orientations, crystalline VO clusters of NaCl structures were observed, which was attributed to the reaction with free oxygen present on the amorphous carbon substrates. The latter could be detected by electron energy-loss spectroscopy. The exposure of the samples to air caused a change to amorphous structures, which re-crystallized under the electron beam. This effect was interpreted as a reaction with water present in the air.