HOLZ lines splitting on SiGe/Si relaxed samples: analytical solutions for the kinematical equation.

Sample thinning for TEM observation introduces large changes with respect to the initial strain state of the bulk sample and particularly relaxation via the free surfaces which leads to HOLZ lines splitting in the CBED pattern. This phenomenon has been simulated owing to extensive calculations either in the kinematical or the dynamical framework of electron diffraction mainly using displacement fields resulting from finite element modelling of the sample relaxation. HOLZ line splitting is well reproduced and numerical fits can be used to compare experimental and calculated curves. This paper proposes new analytical solutions for the kinematical equation of electron diffraction. Simple mathematical functions are used to approximate the deformation profiles. We showed that, under certain conditions, the rocking curve profile can be analytically calculated, thus providing some clue to separate different contributions to the rocking curves against deformation profile. These simplified analytical expressions are used to extract the maximum amplitude displacement within the sample with about 10% accuracy. This accuracy can even be improved to 1% with a short adjustment routine. The influence of the shape of the displacement profile on the rocking curves is demonstrated.

Optimized FIB silicon samples suitable for lattice parameters measurements by convergent beam electron diffraction.

The aim of this paper is to check the effect of artefacts introduced by focused ion beam (FIB) milling on the strain measurement by convergent beam electron diffraction (CBED). We show that on optimized silicon FIB samples, the strain measurement can be performed with a sensitivity of about 2.5 x 10(-4) which is very close to the theoretical one and we conclude that FIB preparation can be suitable for such measurements in microelectronic devices. To achieve this, we first used CBED and electron energy loss spectroscopy (EELS) which provide a procedure permitting an exact knowledge of the sample geometry, i.e. the thickness of both amorphous and crystalline layers. This procedure was used in order to measure the FIB-amorphized sidewall layer. It was found that if the FIB preparation is optimized one can reduce this amorphous layer down to around 7 nm on each side. Secondly different preparation techniques (cleavage, Tripodtrade mark and FIB) permit to check if the surface damaged layer introduced by FIB influences the strain state of the sample. Finally, it was found that the damaged layer does not introduce measurable strain in pure silicon but reduces appreciably the quality of the CBED patterns.

Evolution of ELNES spectra as a function of experimental settings for any uniaxial specimen: a fully relativistic study.

We perform calculations of the fully relativistic, corrected geometrical weighting of the pi* and sigma* transitions measured from the 1s core loss electron energy loss spectroscopy (EELS) spectrum in any uniaxial specimen. We present a complete calculation of the differential scattering cross-section (DSCS), taking into account the collection angle, the illumination angle and the tilt of the sample over the optical axis. Owing to high electron velocity in an EELS experiment, the relativistic correction has to be considered. We thus, present a relativistic, corrected DSCS by using the theory recently developed by Jouffrey et al. [Ultramicroscopy 102 (2004) 61] and P. Schattschneider et al. [Phys. Rev. B 72 (2005) 045142]. The relativistic correction is first performed in the natural coordinate system of the scattering event. We then point out a straightforward method to introduce this correction in the microscopic coordinate system, where all calculations have to be done to be experimentally useful. Using the fully corrected DSCS, we present an expression predicting the evolution of the R=pi*/(pi*+sigma*) ratio (related to the ratio of sp2 and sp3 bondings) as a function of experimental settings. We show how the R-evolution can be predicted, for any experimental setting, by the knowledge of one unique reference value. We verify on graphite specimens, the validity of the R-calculation by comparing theoretical predictions presented in this work with experimental data published elsewhere [Daniels et al., Ultramicroscopy 96 (2003) 523 and Menon et al., Ultramicroscopy 74 (1998) 83].

Morphology and microstructure at different scales of porous silicon prepared by a nonconventional technique.

In this work we present first results concerning the detailed structure of porous silicon (PS) layers prepared by a new method using a vapour-etching (VE)-based technique. Studies of the photoluminescence properties of VE-based PS show that the visible emission occurs at high energies as compared with PS prepared by conventional techniques. To understand the VE-based PS features, we need to point out the PS microstructure throughout its general morphology. For this purpose a microscopy multiscale study was done. Scanning, conventional transmission, and high-resolution transmission electron microscopes were employed. The investigations were made on PS films prepared from moderately and heavily doped n- and p-type silicon. SEM images show that VE-based PS layers are essentially formed of clusters like interconnected structures. TEM studies show that these clusters are composed of nanocrystallites with different shapes. The effect of the doping type of the starting Si substrate on the characteristics of the PS layers was examined (thickness, porosity, behavior). Pore propagation was found to depend on doping type. The crystallinity of the PS layers was also locally studied in depth.