M. Texier

Sample preparation by focused ion beam micromachining for transmission electron microscopy imaging in front-view

This article deals with the development of an original sample preparation method for transmission electron microscopy (TEM) using focused ion beam (FIB) micromachining. The described method rests on the use of a removable protective shield to prevent the damaging of the sample surface during the FIB lamellae micromachining. It enables the production of thin TEM specimens that are suitable for plan view TEM imaging and analysis of the sample surface, without the deposition of a capping layer. This method is applied to an indented silicon carbide sample for which TEM analyses are presented to illustrate the potentiality of this sample preparation method.

Tungsten diffusion in silicon

Two doses (1013 and 1015 cm−2) of tungsten (W) atoms were implanted in different Si(001) wafers in order to study W diffusion in Si. The samples were annealed or oxidized at temperatures between 776 and 960 °C. The diffusion profiles were measured by secondary ion mass spectrometry, and defect formation was studied by transmission electron microscopy and atom probe tomography. W is shown to reduce Si recrystallization after implantation and to exhibit, in the temperature range investigated, a solubility limit close to 0.15%–0.2%, which is higher than the solubility limit of usual metallic impurities in Si. W diffusion exhibits unusual linear diffusion profiles with a maximum concentration always located at the Si surface, slower kinetics than other metals in Si, and promotes vacancy accumulation close to the Si surface, with the formation of hollow cavities in the case of the higher W dose. In addition, Si self-interstitial injection during oxidation is shown to promote W-Si clustering. Taking into account these observations, a diffusion model based on the simultaneous diffusion of interstitial W atoms and W-Si atomic pairs is proposed since usual models used to model diffusion of metallic impurities and dopants in Si cannot reproduce experimental observations.

Al–Pd–Mn icosahedral quasicrystal: deformation mechanisms in the brittle domain

The extreme brittleness of Al–Pd–Mn quasi-crystalline alloys over a wide range of temperatures drastically restricts investigation of their plastic deformation mechanisms over a small high-temperature regime. Recently, plastic deformation of Al–Pd–Mn quasicrystal has been achieved in the brittle domain (20 ≤ T ≤ 690°C) using specific deformation devices, which combined a uniaxial compression deformation or a shear deformation with a hydrostatic pressure confinement (0.35–5 GPa). Results of these experimental techniques, which provide various deformation conditions giving rise to a range of Al–Pd–Mn plastic features in the brittle domain, are discussed. On this basis, we propose that low and intermediate temperature plastic properties of Al–Pd–Mn are controlled by non-planar dislocation core extensions specific to the non-periodic structure.

LACBED study of extended defects in 4H-SiC

Large-angle convergent-beam electron diffraction analysis was successfully performed on pairs of partial dislocations so close that their effect on Bragg lines overlap. These pairs, dragging 3C layers, were nucleated by mechanical deformation of 4H-SiC. Splitting of Bragg lines on crossing a dislocation pair can be interpreted as resulting from a single dislocation having a Burgers vector equal to the sum of the two partial dislocation ones. Splitting rules using phase-shifted reflections ( ) are also given depending on the phase shift produced by 3C lamellae. These results give a direction in agreement with weak-beam dark-field studies and suggest that Si core dislocations have highest mobilities for low-temperature (<700○C) plastic deformation.

Mechanism of β-FeSi2 precipitates growth-and-dissolution and pyramidal defects' formation during oxidation of Fe-contaminated silicon wafers

Fe-implanted Si-wafers have been oxidized at 900 °C and 1100 °C in order to investigate the behaviour of Fe atoms at the growing SiO2/Si interface and the impact on the integrity of microelectronic devices of an involuntary Fe contamination before or during the oxidation process. As-implanted and oxidized wafers have been characterized using secondary ion mass spectroscopy, atom probe tomography, and high-resolution transmission electron microscopy. Experimental results were compared to calculated implantation profiles and simulated images. Successive steps of iron disilicide precipitation and oxidation were evidenced during the silicon oxidation process. The formation of characteristic pyramidal-shaped defects, at the SiO2/Si interface, was notably found to correlate with the presence of β-FeSi2 precipitates. Taking into account the competitive oxidation of these precipitates and of the surrounding silicon matrix, dynamic mechanisms are proposed to model the observed microstructural evolution of the SiO2...

Dislocation distribution across ultrathin silicon-on-insulator with epitaxial SiGe stressor

We studied the plastic deformation of an ultrathin silicon-on-insulator with epitaxial Si1−xGex by transmission electron microscopy, Raman spectroscopy, and finite-element method. We analyzed a top Si layer of 10 nm (testing also a 2 nm layer) with epitaxial Si0.64Ge0.36 stressors of 50 and 100 nm. SiGe plastically deforms the top Si layer, and this strain remains even when Si1−xGex is removed. For low dislocation densities, dislocations are gettered close to the Si/SiO2 interface, while the SiGe/Si interface is coherent. Beyond a threshold dislocation density, interactions between dislocations force additional dislocations to position at the Si1−xGex/Si interface.

Nanoporous Ge thin film production combining Ge sputtering and dopant implantation.

Summary In this work a novel process allowing for the production of nanoporous Ge thin films is presented. This process uses the combination of two techniques: Ge sputtering on SiO2 and dopant ion implantation. The process entails four successive steps: (i) Ge sputtering on SiO2, (ii) implantation preannealing, (iii) high-dose dopant implantation, and (iv) implantation postannealing. Scanning electron microscopy and transmission electron microscopy were used to characterize the morphology of the Ge film at different process steps under different postannealing conditions. For the same postannealing conditions, the Ge film topology was shown to be similar for different implantation doses and different dopants. However, the film topology can be controlled by adjusting the postannealing conditions.

Dynamic segregation of metallic impurities at SiO2/Si interfaces

The behaviour of two metallic impurities, iron and tungsten, during oxidation of silicon wafers has been investigated using transmission electron microscopy and atom probe tomography. Metallic contamination has been introduced by implantation of 54Fe at 65 keV and 186W at 150 keV, with a dose of 1015 at/cm2. Oxidation of Fe-contaminated Si wafer results in the precipitation of iron as β-FeSi2 at the SiO2/Si interface. The presence of these precipitates hinders the oxidation front which forms silicon pyramidal defects. Further oxidation of the precipitates leads to iron-rich cluster formation in the SiO2 layer, surrounding the pyramids. Dry oxidation of a tungsten-contaminated Si wafer is characterised by the formation of nanometric spherical precipitates in the Si layer. The size and density of these precipitates versus depth follow the as-implanted W concentration profile.

Piezoelectric response and electrical properties of Pb(Zr1-xTix)O3 thin films: The role of imprint and composition

The compositional dependence of the piezoelectric properties of self-polarized PbZr1-xTixO3 (PZT) thin films deposited on Pt/TiO2/SiO2/Si substrates (x = 0.47, 0.49 and 0.50) was investigated by in situ synchrotron X-ray diffraction and electrical measurements. The latter evidenced an imprint effect in the studied PZT films, which is pronounced for films with the composition of x = 0.50 and tends to disappear for x = 0.47. These findings were confirmed by in situ X-ray diffraction along the crystalline [100] and [110] directions of the films with different compositions revealing asymmetric butterfly loops of the piezoelectric strain as a function of the electric field; the asymmetry is more pronounced for the PZT film with a composition of x = 0.50, thus indicating a higher built-in electric field. The enhancement of the dielectric permittivity and the effective piezoelectric coefficient at compositions around the morphotropic phase boundary were interpreted in terms of the polarization rotation mechanism...

Te homogeneous precipitation in Ge dislocation loop vicinity

High resolution microscopies were used to study the interactions of Te atoms with Ge dislocation loops, after a standard n-type doping process in Ge. Te atoms neither segregate nor precipitate on dislocation loops, but form Te-Ge clusters at the same depth as dislocation loops, in contradiction with usual dopant behavior and thermodynamic expectations. Atomistic kinetic Monte Carlo simulations show that Te atoms are repulsed from dislocation loops due to elastic interactions, promoting homogeneous Te-Ge nucleation between dislocation loops. This phenomenon is enhanced by coulombic interactions between activated Te2+ or Te1+ ions.