Extrinsic Measurement of Carbon Black Aggregate Distribution within a Fluoroelastomer Matrix from Nanoindentation Experiments.

A novel extrinsic method for the measurement of particle surface distribution in a carbon black-filled elastomer via nanoindentation is developed. This method is based on the measurement of the contact stiffness obtained from the continuous stiffness measurement mode. The proposed tip-particle model is held by two main hypotheses: the particles do not deform significantly during indentation so that only the elastomer matrix elastically deforms; particles are physically bounded with the surrounding matrix. Therefore, when the tip comes in contact with a particle, the latter becomes a hard extension of the tip, able to deform the elastomer matrix. Finally, the evolution of the measured contact stiffness is directly related to the increase of the contact area between the tip-particles set and the elastomer matrix. The proposed model is validated through a numerical and an experimental study. Moreover, an evaluation of the measurements bias allows to correct the particle surface distribution. A good agreement is found between the distribution measured from transmission electron microscopy observations and nanoindentation measurements.

Locally measuring the adhesion of InP directly bonded on sub-100 nm patterned Si.

A nano-scale analogue to the double cantilever experiment that combines instrumented nano-indentation and atomic force microscopy is used to precisely and locally measure the adhesion of InP bonded on sub-100 nm patterned Si using oxide-free or oxide-mediated bonding. Surface-bonding energies of 0.548 and 0.628 J m(-2), respectively, are reported. These energies correspond in turn to 51% and 57% of the surface bonding energy measured in unpatterned regions on the same samples, i.e. the proportion of unetched Si surface in the patterned areas. The results show that bonding on patterned surfaces can be as robust as on unpatterned surfaces, provided care is taken with the post-patterning surface preparation process and, therefore, open the path towards innovative designs that include patterns embedded in the Si guiding layer of hybrid III-V/Si photonic integrated circuits.

Dynamics of colloids in single solid-state nanopores.

We use solid-state nanopores to study the dynamics of single electrically charged colloids through nanopores as a function of applied voltage. We show that the presence of a single colloid inside of the pore changes the pore resistance, in agreement with theory. The normalized ionic current blockade increases with the applied voltage and remains constant when the electrical force increases even more. We observe short and long events of current blockades. Their durations are associated, respectively, with low and high current variation. The ratio of long events increases with the electrical force. The events frequency increases exponentially as a function of applied voltage and saturates at high voltage. The dwelling time decreases exponentially at low and medium voltages when the electrical force increases. At large voltages, this time decreases inversely proportionally to the applied voltage. The long events are associated with translocation events. We show that the dynamics of colloids through the nanopore is governed mainly by two mechanisms, by the free-energy barrier at relatively low and medium voltages and by the electrophoresis mechanism at high voltage.

Development of a synchrotron biaxial tensile device for in situ characterization of thin films mechanical response.

We have developed on the DIFFABS-SOLEIL beamline a biaxial tensile machine working in the synchrotron environment for in situ diffraction characterization of thin polycrystalline films mechanical response. The machine has been designed to test compliant substrates coated by the studied films under controlled, applied strain field. Technological challenges comprise the sample design including fixation of the substrate ends, the related generation of a uniform strain field in the studied (central) volume, and the operations from the beamline pilot. Preliminary tests on 150 nm thick W films deposited onto polyimide cruciform substrates are presented. The obtained results for applied strains using x-ray diffraction and digital image correlation methods clearly show the full potentialities of this new setup.

Magnetization reversal in Pt/Co(0.5 nm)/Pt nano-platelets patterned by focused ion beam lithography.

Arrays of ultrathin Pt/Co(0.5 nm)/Pt nano-platelets with lateral sizes ranging from 30 nm to 1 µm have been patterned by focused ion beam (FIB) lithography under a weak Ga(+) ion fluence. From polar magneto-optical Kerr microscopy it is demonstrated that nano-platelets are ferromagnetic with perpendicular anisotropy down to a size of 50 nm. The irradiation process creates a magnetically soft ring at the nano-platelet periphery in which domain nucleation is initiated at a low field. The magnetization reversal in nano-platelets can be interpreted using a confined droplet model. All of the results prove that ultimate FIB patterning is suitable for preparing discrete magnetic recording media or small magnetic memory elements and nano-devices.

Ti-Si-C thin films produced by magnetron sputtering: correlation between physical properties, mechanical properties and tribological behavior.

Ti-Si-C thin films were deposited onto silicon, stainless steel and high-speed steel substrates by magnetron sputtering, using different chamber configurations. The composition of the produced films was obtained by Electron Probe Micro-Analysis (EPMA) and the structure by X-ray diffraction (XRD). The hardness and residual stresses were obtained by depth-sensing indentation and substrate deflection measurements (using Stoney's equation), respectively. The tribological behavior of the produced films was studied by pin-on-disc. The increase of the concentration of non-metallic elements (carbon and silicon) caused significant changes in their properties. Structural analysis revealed the possibility of the coexistence of different phases in the prepared films, namely Ti metallic phase (alpha-Ti or beta-Ti) in the films with higher Ti content. The coatings with highest carbon contents, exhibited mainly a sub-stoichiometric fcc NaCI TiC-type structure. These structural changes were also confirmed by resistivity measurements, whose values ranged from 10(3) omega/sq for low non-metal concentration, up to 10(6) omega/sq for the highest metalloid concentration. A strong increase of hardness and residual stresses was observed with the increase of the non-metal concentration in the films. The hardness (H) values ranged between 11 and 27 GPa, with a clear dependence on both crystalline structure and composition features. Following the mechanical behavior, the tribological results showed similar trends, with both friction coefficients and wear revealing also a straight correlation with the composition and crystalline structure of the coatings.

Local tuning of CoPt nanoparticle size and density with a focused ion beam nanowriter.

Ultra-small CoPt nanoparticles (NPs) with a mean diameter of 1.3 nm (around 100 atoms) were deposited on a thin 5 nm self-supported amorphous carbon membrane. The effects of focused irradiation with a newly developed Ga(+) ion source were studied by transmission electron microscopy. While the overall coverage of the NPs remained constant, the mean diameter and the density of the NPs evolve in the dose range from 5 x 10(13) to 1 x 10(15) ions cm(-2). The local tuning of the size and density of CoPt NPs by means of ion irradiation could be used in magnetic data storage applications.

Single-shot diffractive imaging with a table-top femtosecond soft x-ray laser-harmonics source.

Coherent x-ray diffractive imaging is a powerful method for studies on nonperiodic structures on the nanoscale. Access to femtosecond dynamics in major physical, chemical, and biological processes requires single-shot diffraction data. Up to now, this has been limited to intense coherent pulses from a free electron laser. Here we show that laser-driven ultrashort x-ray sources offer a comparatively inexpensive alternative. We present measurements of single-shot diffraction patterns from isolated nano-objects with a single 20 fs pulse from a table-top high-harmonic x-ray laser. Images were reconstructed with a resolution of 119 nm from the single shot and 62 nm from multiple shots.

Exploration of the ultimate patterning potential achievable with focused ion beams.

Decisive advances in the field of nanosciences and nanotechnologies are intimately related to the development of new instruments and of related writing schemes and methodologies. Therefore we have recently proposed the exploitation of the nano-structuring potential of a highly focused ion beam (FIB) as a tool, to overcome intrinsic limitations of current nano-fabrication techniques and to allow innovative patterning schemes that are urgently needed in many nanoscience challenges. In this work, we will first detail a very high-resolution FIB instrument we have developed specifically to meet these nano-fabrication requirements. Then we will introduce and illustrate an advanced FIB processing scheme that is the fabrication of artificial nanopores.

Ion beam nanopatterning in graphite: characterization of single extended defects.

The morphology and the electronic structure of a single focused ion-beam-induced artificial extended defect is probed by several methods including micro-Raman spectroscopy, atomic force and scanning tunneling microscopies and Monte Carlo and/or semi-analytical simulation within standard codes. The efficiency of the artificial defect for deposited metallic cluster pinning is also investigated. We show a correlation between the ion dose, morphology, electronic structure and cluster trapping efficiency. At room temperature, cluster pinning is efficient when the displacement per atom is one or more. Well-ordered patterned cluster networks are considered for potential applications.

TEM-nanoindentation studies of semiconducting structures.

This paper reviews the application of nanoindentation coupled with transmission electron microscopy (TEM) to investigations of the plastic behaviour of semiconducting structures and its implication for device design. Instrumented nanoindentation has been developed to extract the mechanical behaviour of small volumes scaled to those encountered in semiconductor heterostructures. We illustrate that TEM is a powerful complementary tool for the study of local plasticity induced by nanoindentation. TEM-nanoindentation allows for detailed understanding of the plastic deformation in semiconducting structures and opens practical routes for improvement of devices. Performances of heterostructures are deteriously affected by dislocations that relax the lattice mismatched layers. Different ways to obtain compliant substructures are being developed in order to concentrate the plastic relaxation underneath the heterostructure. Such approaches allow for mechanical design of micro- and opto-electronic devices to be considered throughout the fabrication process.

Detecting enteropathogenic strains of Escherichia coli of porcine origin. 2. Relationship between O and K antigens and the production of enterotoxin in strains isolated from the piglet after weaning.

The production of enterotoxin by biological tests (Yl adrenal cells and the suckling mouse) has been examined in 96 strains of Escherichia coli, isolated from sick piglets after weaning. There is a good correlation between the presence of the capsular antigen K88 and that of the thermolabile fraction (LT) of the enterotoxin (69.2 per cent of the enteropathogenic strains studied). However, the presence of the thermostable fraction (ST) of the enterotoxin of strains which, according to their serological grouping, possess in theory the two fractions LT + ST or only the ST fraction is only confirmed in a small number of strains (16 per cent) by the biological test.

Detecting enteropathogenic Escherichia coli strains of porcine origin. 1. Correlations between O and K antigens and the enterotoxin production in strains isolated from the newborn piglet.

A study of enterotoxin production by means of biological tests (Y1 adrenal cells and suckling mice) using 67 Escherichia coli strains responsible for diarrhea in newborn piglets, confirmed the advantages of these methods and demonstrated the correlation between antigenic specificity and enterotoxin production. In particular the presence of capsular antigen K 88 is related to the thermolabile (LT) fraction of the enterotoxin in 73.9 % of the enteropathogenic strains studied.