The Polyol Process and the Synthesis of ζ Intermetallic Compound Ag5Sn0.9.

The present work concerns the intermetallic compound (IMC) existing in the Ag-Sn system and its potential use in electronics as attachment materials allowing the adhesion of the chip to the substrate forming the power module. First, we present the synthesis protocol in polyol medium of a compound with the chemical formula Ag5Sn0.9 belonging to the solid solution of composition located between 9 and 16 at.% Sn, known as solid solution ζ (or ζ-Ag4Sn). This phase corresponds to the peritectic invariant point at 724 °C. Differential thermal analysis and X-ray dispersive analysis confirm the single-phased (monocrystalline) nature of the Ag5Sn0.9 powder issued after synthesis. Scanning electron microscopy shows that Ag5Sn0.9 particles are spherical, and range in submicronic size of around 0.18 µm. X-ray diffraction analysis reveals that the ζ phase mostly exists under the two allotropic varieties (orthorhombic symmetry and hexagonal symmetry) with however a slight excess of the hexagonal variety (60% for the hexagonal variety and 40% for the orthorhombic variety). The lattice parameters resulting from this study for the two allotropic varieties are in good agreement with the Hume-Rothery rules.

Introducing cobalt as a potential plasmonic candidate combining optical and magnetic functionalities within the same nanostructure.

The control of magnetic properties at the nanoscale is a current topic of intense research. It was shown that combining both magnetic and plasmonic nanoparticles (NPs) led to the improvement of their magneto-optical signal. In this context, common strategies consist of the design of bimetallic NPs. However, the understanding of the physics leading to the coupling between magnetic and plasmonic NPs is lacking, preventing any significant progress for the development of future photonic devices. In this article, we propose to focus our attention on an efficient and commonly used magnetic metal, cobalt, and evaluate its plasmonic properties at the nanoscale through the use of NP regular arrays, as a potential candidate combining both optical and magnetic functionalities within the same metal. We show that such NPs display plasmonic properties within a large spectral range from the UV to the NIR spectral range, with efficient quality factors, when the inter-particle distance is properly selected. These as-fabricated simple materials could find applications in integrated photonic devices for telecommunications.

Spin Coating and Micro-Patterning Optimization of Composite Thin Films Based on PVDF.

We optimize the elaboration of very thin film of poly(vinylidene fluoride) (PVDF) polymer presenting a well-controlled thickness, roughness, and nano-inclusions amount. We focused our effort on the spin coating elaboration technique which is easy to transfer to an industrial process. We show that it is possible to obtain continuous and smooth thin films with mean thicknesses of 90 nm by properly adjusting the concentration and the viscosity of the PVDF solution as well as the spin rate and the substrate temperature of the elaboration process. The electro-active phase content versus the magnetic and structural properties of the composite films is reported and fully discussed. Last but not least, micro-patterning optical lithography combined with plasma etching has been used to obtain well-defined one-dimensional micro-stripes as well as squared-rings, demonstrating the easy-to-transfer silicon technology to polymer-based devices.

Enhanced Magnetic Behavior of Cobalt Nano-Rods Elaborated by the Polyol Process Assisted with an External Magnetic Field.

Cobalt nano-rods with the hexagonal close-packed (hcp) structure were prepared by reduction of the long-chain carboxylate Co (II) precursor in polyol. The application of an external magnetic field (µ0H = 1.25 T) during the nucleation and growth steps resulted in a noticeable modification of the mean aspect ratio (length/diameter) of the particles. The particle morphology was also modified as the nano-rods did not exhibit conical heads at their extremities anymore, which are observed for particles prepared without application of an external magnetic field. Besides, the stacking faults density along the c axis of the hcp structure in the cobalt nano-rods has been found to decrease with the increase in the applied magnetic field. The coercive field of randomly oriented nano-rods increased with the aspect ratio, showing the highest value (i.e., 5.8 kOe at 300 K) for the cobalt nano-rods obtained under the highest applied magnetic field. For partially oriented Co nano-rods in toluene solution, the magnetic properties were significantly enhanced with a coercive field of 7.2 kOe at 140 K, while the magnetization saturation reached 92% of the bulk. The MR/MS value was about 0.8, indicating a good orientation of the anisotropic particles relative to each other, making them suitable for the preparation of permanent magnets via a bottom-up approach.

Tailoring the magnetic properties of cobalt ferrite nanoparticles using the polyol process.

Background: In extrinsically magnetoelectric materials made of two components, the direct magnetoelectric coupling arises from a mechanical strain transmission at the interface due to the shape change of the magnetostrictive component under an external magnetic field. Here, the size of the interface between the two components plays a crucial role. Therefore, the development of nanomaterials exhibiting large surface-to-volume ratios can help to respond to such a requirement. However, the magnetic nanoparticles (NPs) must be highly magnetostrictive and magnetically blocked at room temperature despite their nanometer-size. We describe here the use of the polyol process to synthesize cobalt ferrite (Co x Fe3- x O4) nanoparticles with controlled size and composition and the study of the relationship between size and composition and the magnetic behavior. Methods: We used an improved synthesis of magnetostrictive Co x Fe3- x O4 NPs based on the forced hydrolysis of metallic salts in a polyol solvent, varying the fraction x. Stoichiometric NPs (x = 1) are expected to be highly magnetostrictive while the sub-stoichiometric NPs (particularly for x ≈ 0.7) are expected to be less magnetostrictive but to present a higher magnetocrystalline anisotropy constant, as previously observed in bulk cobalt ferrites. To control the size of the NPs, in order to overcome the superparamagnetic limit, as well as their chemical composition, in order to get the desired magnetomechanic properties, we carried out the reactions for two nominal precursor contents (x = 1 and 0.67), using two different solvents, i.e., triethylene glycol (TriEG) and tetraethylene glycol (TetEG), and three different durations of refluxing (3, 6 and 15 h). The structure, microstructure and composition of the resulting NPs were then investigated by using X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray fluorescence spectroscopy (XRF), respectively. The magnetic properties were also evaluated using standard magnetometry. To measure the magnetostrictive response of the particles, the particles were sintered to dense pellets on which strain gauges were bonded, measuring the size variation radially, as a function of a dc magnetic field. Findings: We found two samples, the first one being stoichiometric and magnetostrictive, and the second one being sub-stoichiometric and presenting a higher magnetization, that are appropriate to be used as ferromagnetic building blocks in nanostructured magnetoelectric materials, particularly materials based on polymers. We show that the polyol solvent and the reaction time are two key parameters to control the size and the magnetic properties of the resulting nanoparticles. We believe that these results provide relevant insights to the design of efficient magnetic and magnetostrictive nanoparticles that can be further functionalized by coupling agents, to be contacted with piezoelectric polymers.

Synthesis and characterisation of the vibrational and electrical properties of antiferromagnetic 6L-Ba2CoTeO6 ceramics.

Optimal processing conditions for fabrication of dense single-phase 6L-Ba2CoTeO6 ceramics via the solid-state reaction method were determined. These ceramics possess a room-temperature crystal structure described by the centrosymmetric P3[combining macron]m1 space group. Polarized Raman spectroscopy enabled the observation of all the 25 predicted Raman modes and assignment of their symmetries. On cooling, BCTO ceramics exhibit two antiferromagnetic transitions at 3 K and 12.5 K, in broad agreement with a recent single-crystal study [P. Chanlert, N. Kurita, H. Tanaka, D. Goto, A. Matsuo and K. Kindo, Phys. Rev. B: Condens. Matter Mater. Phys., 2016, 93, 094420]. Low temperature Fourier-transform infrared reflectivity analyses suggest the antiferromagnetic phase transitions to be driven by small distortions of the CoO6 octahedra, lowering locally their C3v symmetry. This causes splitting of the associated vibrational modes, but without a long-range structural change. AC impedance spectroscopy revealed BCTO ceramics to be leaky insulators with an activation energy for conduction of ∼0.15-0.25 eV, which suggests electron hopping between mixed oxidation states of Co.

Real-time sensing of enteropathogenic E. coli-induced effects on epithelial host cell height, cell-substrate interactions, and endocytic processes by infrared surface plasmon spectroscopy.

Enteropathogenic Escherichia coli (EPEC) is an important, generally non-invasive, bacterial pathogen that causes diarrhea in humans. The microbe infects mainly the enterocytes of the small intestine. Here we have applied our newly developed infrared surface plasmon resonance (IR-SPR) spectroscopy approach to study how EPEC infection affects epithelial host cells. The IR-SPR experiments showed that EPEC infection results in a robust reduction in the refractive index of the infected cells. Assisted by confocal and total internal reflection microscopy, we discovered that the microbe dilates the intercellular gaps and induces the appearance of fluid-phase-filled pinocytic vesicles in the lower basolateral regions of the host epithelial cells. Partial cell detachment from the underlying substratum was also observed. Finally, the waveguide mode observed by our IR-SPR analyses showed that EPEC infection decreases the host cell's height to some extent. Together, these observations reveal novel impacts of the pathogen on the host cell architecture and endocytic functions. We suggest that these changes may induce the infiltration of a watery environment into the host cell, and potentially lead to failure of the epithelium barrier functions. Our findings also indicate the great potential of the label-free IR-SPR approach to study the dynamics of host-pathogen interactions with high spatiotemporal sensitivity.