Corrosion mechanisms take place at the extreme surface of materials before spreading in the bulk. In this way, in situ surface characterization techniques as scanning probe microscopy (Scanning Tunneling Microscopy (STM) and Atomic Force Microscopy (AFM)) allow the observations of the very initial reaction steps.

To achieve that goal, an environmental cell has been designed ; it is able to integrate either an atomic force microscope (AFM) or a scanning tunneling microscope (STM). This cell can resist to internal pressures ranging from 10-5 to 20 atm. Heterogeneous “solid – gas” reactions that only occur with pressures above several atmospheres, can then be studied. This could be achieved by following the topographical evolution of samples reacting with gaseous species. Identification of the surface defects at the origin of corrosive attacks as well as proposition of reaction mechanisms will be describe in future works.

The present work shows first in situ measurements that validate this new and unique experimental “HP-AFM” (High Pressure Atomic Force Microscope). The impact of the atmosphere’s composition as well as the pressure values on the topographical measurements recorded by the AFM system is especially studied.

In this way, a calibration standard is used to detect a potential working drift of the AFM system (scanner head displacements, optical detection …) that could lead to eventual distortions of pictures recorded and misinterpretation of observations. This sample has been studied under several experimental conditions and the results have shown an identical behaviour of the AFM used ex situ and in situ under Ar or He up to 1.5 atm as well as a good stability during long recording acquisitions (up to 90 min) necessary for kinetic studies.

An experimental set up has been designed to suppress electron currents generated during energetic ion irradiation to obtain accurate current integration for Heavy Ion Rutherford Backscattering Spectroscopy (HIRBS) measurements of heavy element concentrations and target depth profiles. A combination of an electron trap to suppress any electrons ejected from beam collimators and slits, and a biased aluminum mesh to suppress any secondary electrons ejected from the target was used. Two samples that produce cleanly interpreted spectra have been used as targets to check the accuracy of the system for 3.0 and 4.5 MeV O+2 projectile ions. Details of the experimental set up and data are presented.

Electrical properties of grain boundaries grown by Czochralski process were studied by microwave phase shift (μW-PS) and electron beam induced current (EBIC), before and after gold diffusion at 700°C. As-grown samples had similar doping levels determined by four-point probe measurements but somewhat different oxygen concentrations, obtained by Fourier transform infrared spectroscopy (FTIR). It is shown that the increase of the grain boundary activity due to Au gathering at this planar defect can be hindered by native impurities (likely oxygen). EBIC and μW-PS techniques gave respectively electron diffusion lengths and lifetime values, both in good agreement. EBIC images on deformed Σ =9 showed that extrinsic dislocations do not activate the grain boundary at 300K.

We measure the mechanical response of optical multilayer dielectric (MLD) diffraction gratings, geometries which are constrained in only one transverse direction but free in the other, using nanoindentation. The results are explained using a stress-strain model, which reveals a uniaxial yield stress of 4.1- 4.6 GPa and predicts a similar dependence of yield stress on loads for both fully-elastic and fully-plastic solutions. Following R. Hill’s model of an expanding cavity under internal pressure, we show that the indentation response of the high-aspect ratio “pillar” geometry can be expressed in terms of uniaxial yield stress rather than material hardness.

We obtained interestingly-shaped ZnS nanocrystals in oleylamine solution and characterized their structures using HR-TEM and HAADF tomography. These interesting nanocrystals had a conical head rather than the frequently-reported pyramidal one. The cone consisted of not only low-energy planes but high Miller-index planes. In addition, we three-dimensionally and crystallographically investigated the particle growth of these nanocrystals by the same method.

In this work, an Atomic Force Microscope in the so-called Piezoresponse mode and Kelvin mode is used to image the grains, ferroelectric domains and surface potential in lithium niobate thin films. A RF magnetron sputter system was used to deposit LiNbO3 thin films on (100)-oriented Si substrates with SiO2 layer. The surface of the sample shows small grains which diameter ranges from 70 nm to 150 nm and roughness is less than 13 nm. Using the electric field from a biased conducting AFM tip, we show that possible to form and subsequently to visualize ferroelectric state. Also, we report surface charge retention on ferroelectric thin films by Kelvin probe microscope in comparison with the piezoresponse signal.

Single layer regions of MoS2 on SiO2 and SrTiO3 were identified by Raman spectroscopy and μ-photoluminescence before Kelvin probe force microscopy was performed. For the already known system MoS2/SiO2 we find 1.839 eV for the direct bandgap, in good agreement with earlier results. On MoS2/SrTiO3 the direct bandgap was determined to be 1.829 eV. From our Kelvin probe data we infer that the SrTiO3 substrate leads to a dipole layer at the interface of the MoS2 single layer. The corresponding μ-PL measurements however show no significant decrease of the bandgap. This shows, that in the case of MoS2 the carrier type as well as concentration is not significantly influenced by the choice of SrTiO3 as the substrate compared to SiO2.