Size and morphology control of ultrafine refractory complex oxide crystals

High-temperature complex oxides are of considerable interest as their applications cover a broad spectrum from catalytic to optical technology. Indeed, new exciting opportunities might emerge if these high-temperature complex oxides, in which structure crystallization is achieved at temperatures T > 1000 °C, could be synthesized as nonaggregated, ultrafine building blocks. In general, such refractory complex oxide particles are difficult to synthesize as ultrafine crystals because of the strong driving force available for sintering and coarsening in this high-temperature range. This paper reports a new synthetic process for the preparation of nonaggregated, ultrafine barium hexa-aluminate, BaO, 6Al2O3, (BHA), and Ba0.9Eu0.1MgAl10O17, (BAM) crystals in which structure crystallization occurs around 1300 °C. Our process is based on the Ba2+ and Al3+ ions high-temperature controlled diffusion from carbon−inorganic hybrid compounds prepared from soft chemistry routes. Control of morphology of these refractory complex aluminates displaying nanoplatelets morphology was achieved via the tailoring of high-temperature diffusion lengths of the various cations involved in the formation of these ultrafine refractory crystals

Surface characterization and properties of ordered arrays of CeO2 nanoparticles embedded in thin layers of SiO2

We demonstrated the surface composite character down to the nanometer scale of SiO2-CeO2 composite high surface area materials, prepared using 5 nm colloidal CeO2 nanoparticle building blocks. These materials are made of a homogeneous distribution of CeO2 nanoparticles in thin layers of SiO2, arranged in a hexagonal symmetry as shown by small-angle X-ray scattering and transmission electron microscopy. Since the preparation route of these composite materials was selected in order to produce SiO2 wall thickness in the range of the CeO2 nanoparticle diameter, these materials display surface nanorugosity as shown by inverse chromatography. Accessibility through the porous volume to the functional CeO2 nanoparticle surfaceswasevidenced throughanorganic acid chemisorption technique allowing quantitative determination of CeO2 surface ratio. This surface composite nanostructure down to the nanometer scale does not affect the fundamental properties of the functional CeO2 nanodomains, such as their oxygen storage capacity, but modifies the acid-base properties of the CeO2 surface nanodomains as evidenced by Fourier transform IR technique. These arrays of accessible CeO2 nanoparticles displaying high surface area and high thermal stability, along with the possibility of tuning their acid base properties, will exhibit potentialities for catalysis, sensors, etc

Characterization of Copolymer Latexes by Capillary Electrophoresis

Latexes are widely used for industrial applications, including decorative paints, binders for the papermaking industry, and drilling fluids for oil-field applications. In this work, the interest of capillary zone electrophoresis (CE) for the characterization of hydrophobic block copolymer latexes obtained by the conventional emulsion polymerization technique consisting of a core of polystyrene (PS) surrounded by a layer of poly(ethyl acrylate) (PEA) has been investigated. The PEA part of the copolymer can be partially hydrolyzed in poly(acrylic acid) (PAA) leading to PS−PEA-AA water-soluble amphiphilic copolymer having high viscosifying properties. The main purpose of this work was to evaluate the potential of CE for the characterization of the latexes at the different stages of the synthesis (PS core, PS−PEA diblock latex, and hydrolyzed PS−PEA-AA gel). The main analytical issues were to state (i) if there was free PS or PEA homopolymer latexes in the PS−PEA latex sample and (ii) if there was free PS, PEA, PS−PEA latexes, or free PAA chains in the PS−PEA-AA gel. Within this scope, this work describes the optimization of the selectivity of the separation between the different species (PS, PEA particles in the not hydrolyzed diblock latex and PS, PEA, PS−PEA particles as well as the polymer PAA chains in the PS−PEA-AA diblock gel sample obtained by latter latex hydrolysis). For that purpose, several experimental parameters were investigated such as pH and ionic strength of the background electrolyte (BGE) or the concentration of neutral surfactant added in the BGE. A challenging issue was to overcome the high viscosity of the PS−PEA-AA gel. This was resolved by the addition of 10 mM neutral surfactant in the gel sample and in the BGE. Finally, it is demonstrated that, within the detection limits, CE is a suitable analytical tool for controlling and monitoring the syntheses of these latexes and for intrinsically characterizing the distribution in charge density of the final PS−PEA-AA gel at different hydrolysis rates

Characterization of cationic copolymers by capillary electrophoresis using indirect UV detection and contactless conductivity detection

International audienceFor many industrial applications, the combination of two different monomers in statistical or diblock copolymers enhances the properties of the corresponding polymer. However, during the polymerization reaction, homopolymers might be formed and can influence the properties for the applications. Consequently, the separation and the quantification of the homopolymers contained in copolymer samples are crucial. In addition, the charge density distribution of the statistical copolymer is an important characteristic for the applications. The purpose of this work was to study the characterization of a statistical copolymer of acrylic acid (AA) and diallyldimethyl ammonium chloride (DADMAC) by capillary electrophoresis (CE) in acidic conditions (cationic copolymers). For that purpose, a free solution electrophoretic separation was carried out according to the charge rate (chemical composition) independently of the molar mass. The second objective was to compare contactless conductivity detection and indirect UV absorbance modes for the quantification of DADMAC homopolymers present in copolymer samples. Different coated capillaries based on neutral or positively charged modification were also compared. The comparison of indirect absorbance UV and contactless conductimetric detection demonstrated that both detection modes can be used for a complete CE characterization of non-UV absorbing PAA-DADMAC copolymers

Revealing the pulmonary surfactant corona on silica nanoparticles by cryo-transmission electron microscopy

When inhaled, nanoparticles (NPs) deposit in alveoli and transit through the pulmonary surfactant (PS), a biofluid made of proteins and phospholipid vesicles. They form a corona reflecting the PS–nanomaterial interaction. Since the corona determines directly the NPs' biological fate, the question of its nature and structure is central. Here, we report on the corona architecture formed after incubation of positive or negative silica particles with Curosurf®, a biomimetic pulmonary surfactant of porcine origin. Using optical, electron and cryo-electron microscopy (cryo-TEM), we determine the pulmonary surfactant corona structure at different scales of observation. Contrary to common belief, the PS corona is not only constituted by phospholipid bilayers surrounding NPs but also by multiple hybrid structures derived from NP–vesicle interaction. Statistical analysis of cryo-TEM images provides interesting highlights about the nature of the corona depending on the particle charge. The influence of Curosurf® pre- or post-treatment is also investigated and demonstrates the need for protocol standardization.Interactions des nanoparticules avec des surfaces mimétiques des poumons et du liquide pulmonair

Cyclopamine cooperates with EGFR inhibition to deplete stem-like cancer cells in glioblastoma-derived spheroid cultures

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