Apexes of commercial pyramidal silicon scanning microscopy tips were magnetically functionalized by means of local focused electron beam induced deposition. High aspect ratio supertips and local tip coatings with varying apex diameters can be produced by varying exposure time, beam current, and scan mode. The carbonyl precursor Co2(CO)8 was used as source of magnetic metal. Tip performance was tested with magnetic force microscopy (tapping / lift-retrace mode) and magnetically actuated cantilever atomic force microscopy. The deposit contains 34±2 at.% Co, dispersed as 2-5 nm metal nanocrystals in a carbonaceous matrix. Specific surface reactions and Boudouard reactions are proposed to explain the resulting deposit composition measured by Auger spectroscopy. The electrical resistivity is 104 higher than bulk Co resistivity.

Ni/Ti multilayers were prepared by argon sputtering. We observe changes of latticeparameter, strain, grain size and texture depending on the single layer thickness and thepressure of the sputter gas. Moreover the quality of the layers can be improved by including impurities during the growth of the Ni and the Ti layers. Generally the results show that such additions lead to more planar layers and to structural changes within the individual layers. Although we observe hexagonal Titanium in the as-deposited films, some of the specimens which were prepared for TEM observation reveal an fcc-Ti structure.The chemical composition of the layers has been investigated in a field emission microscope using a probe diameter of nmmC. omposition profiles were determined by evaluating EELS spectra taken at each point in an automated scan, In this way it was possible to determine residual concentrations of Ni in Ti layers lower than 0.5%. In the samples studied the interface width appears to be of the order of 4-5nm and the concentration profiles of Ni—Ti interfaces appear to be different from those of the Ti—Ni interfaces.

Methods were investigated for the rapid preparation of cross-sectional TEM samples from electroplated copper. Electropolishing and ultramicrotomy were used. The electropolished samples were sandwiched in a copper/nickel alloy and electropolished using a nitric acid/methanol mixture. Large transparent areas were obtained and it was possible to position the area of interest at the point where the hole would appear. Ultramicrotomed samples cut with 45° diamond knives were electron transparent but the crystalline structure of the sample was severely damaged. However, it was possible to identify the conditions by which good ultramicrotomed samples might be produced in the future.

The use of two methods for preparation of TEM samples has been investigated. It has been possible to show the practical details of the wedge cleaving method and illustrate it with original results on III-V semiconductors and on metallic thin layers on Silicon. Chemical etching of AlGaAs in heterostructures was clearly observed and can further be quantified. Preferred oxidation of AlAs was shown to be important this can be a problem to a faithful interpretation of images from cross section samples prepared in more conventional ways. Efficient microtomy for use in materials science is still in the development stage, however we think to have found the best conditions for sectioning very soft metals like copper. We hope to decrease the compression in these materials by using lower angle diamond knives

The observation of III–V multilayered semiconductors on 900 cleaved wedges is an interesting alternative to the conventional TEM observation on cross-sectioned samples. It offers a fast specimen preparation, the absence of ion irradiation damage or preferential etching, and a well controlled thickness across the sample. HREM observations are used to derive the layer thickness down to the atomic level. Image simulations were calculated with EMS programs on wedges described by a supercell.

A structural investigation of the Ru-RuOx/TiO2 catalyst was carried out in order to determine the role played by the support, the size of the particles, their dispersion, structural relationship with the support and the preparation conditions on the activity. In the ideal catalyst the metallic particles are 10–15Å in size. Moreover they are selectively dispersed on the TiO2 crystallites with the rutile structure. This uneven distribution is not found for other metals ( Rh, Pt, Co, Ni, etc...) on P25 though the preparation procedure was similar.