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4-Dimethylaminopyridine (DMAP)-stabilized palladium nanoparticles with a mean diameter of 3.4 +/- 0.5 nm are prepared from the aqueous phase reduction of Na2PdCl4 using NaBH4 in the presence of DMAP. TEM and UV-vis spectroscopy characterization of the nanoparticle dispersion shows no obvious change in the nanoparticles several months after preparation. 1H NMR spectroscopy of the nanoparticles shows that the nanoparticle dispersion also contains a boron/DMAP complex and two palladium/DMAP complexes. One of the palladium complexes crystallizes out of the dispersion and is identified as Pd(DMAP)4(OH)2 by X-ray crystallography. Following extensive analysis, it is believed that the palladium/DMAP complexes are formed following the oxidation of the palladium nanoparticles. The prepared nanoparticle dispersion promotes selective hydrogen/deuterium (H/D) exchange on the carbon atoms alpha to the endocyclic nitrogen atom on the DMAP-stabilizing ligands through reaction with D2O. This activity is attributed to the presence of the nanoparticles rather than to the presence of the oxidized palladium/DMAP complexes.
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PMID:Preparation and characterization of 4-dimethylaminopyridine-stabilized palladium nanoparticles. 1798 37

The incorporation of organic moieties into siliceous frameworks leads to a wide variety of adsorbate-adsorbent interactions including weak van-der-Waal attractions as well as strong interactions such as Coulomb forces. Depending on the desired properties of such substituted highly porous matrix materials, optimized synthesis routes can be established to enhance the desired internal pore surface-affinity toward certain volatile compounds. On the basis of a fundamental knowledge of the host-guest system, sorption-related applications may benefit from individually fine-tuned and modified sample materials. The sorption isotherms of vaporized toluene on nonmodified and phenyl-functionalized mesoporous silica samples were determined on an acoustic wave device at different temperatures. The mesoporous silica was modified by in situ co-condensation and postsynthesis grafting approaches, respectively. All samples were thoroughly characterized by nitrogen sorption, thermogravimetric analysis (TGA), scanning and transmission electron microscopy (SEM, TEM), solid-state nuclear magnetic resonance (29Si NMR), dynamic light scattering (DLS), Raman spectroscopy, and toluene adsorption on a quartz crystal microbalance (QCM). The different heats of adsorption of toluene on the various modified silica surfaces obtained by the sorption data make it possible to gain additional information about the degree and type of surface functionalization. It is thus demonstrated that QCM studies can be a powerful and convenient tool for efficient investigations of functionalized mesoporous silica particles that yield valuable quantitative information on molecule-surface interactions.
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PMID:Probing the intrapore surface of phenyl-substituted nanoscale mesoporous silica-piezoelectric sorption measurements in thin films. 1800 Oct 67

We present a detailed study of the growth mechanism of single-walled boron nitride nanotubes synthesized by laser vaporization, which is the unique route known to the synthesis of this kind of tube in high quantities. We have performed a nanometric chemical and structural characterization by transmission electron microscopy (high-resolution mode (HRTEM) and electron energy loss spectroscopy) of the synthesis products. Different boron-based compounds and other impurities were identified in the raw synthesis products. The results obtained by the TEM analysis and from the synthesis parameters (temperature, boron, and nitrogen sources) combined with phase diagram analysis to provide identification of the fundamental factors determining the nanotube growth mechanism. Our experiments strongly support a root-growth model that involves the presence of a droplet of boron. This phenomenological model considers the solubility, solidification, and segregation phenomena of the elements present in this boron droplet. In this model, we distinguish three different steps as a function of the temperature: (1) formation of the liquid boron droplet from the decomposition of different boron compounds existing in the hexagonal boron nitride target, (2) reaction of these boron droplets with nitrogen gas present in the vaporization chamber and recombination of these elements to form boron nitride, and (3) incorporation of the nitrogen atoms at the root of the boron particle at active reacting sites that achieves the growth of the tube.
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PMID:Root-growth mechanism for single-walled boron nitride nanotubes in laser vaporization technique. 1805 51

This study aims to evaluate the in vivo performance of ordered mesoporous silica (OMS) as a carrier for poorly water soluble drugs. Itraconazole was selected as model compound. Physicochemical characterization was carried out by SEM, TEM, nitrogen adsorption, DSC, TGA and in vitro dissolution. After loading itraconazole into OMS, its oral bioavailability was compared with the crystalline drug and the marketed product Sporanox in rabbits and dogs. Plasma concentrations of itraconazole and OH-itraconazole were determined by HPLC-UV. After administration of crystalline itraconazole in dogs (20mg), no systemic itraconazole could be detected. Using OMS as a carrier, the AUC0-8 was boosted to 681+/-566 nM h. In rabbits, the AUC0-24 increased significantly from 521+/-159 nM h after oral administration of crystalline itraconazole (8 mg) to 1069+/-278 nM h when this dose was loaded into OMS. Tmax decreased from 9.8+/-1.8 to 4.2+/-1.8h. No significant differences (AUC, Cmax, and Tmax) could be determined when comparing OMS with Sporanox in both species. The oral bioavailability of itraconazole formulated with OMS as a carrier compares well with the marketed product Sporanox, in rabbits as well as in dogs. OMS can therefore be considered as a promising carrier to achieve enhanced oral bioavailability for drugs with extremely low water solubility.
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PMID:Increasing the oral bioavailability of the poorly water soluble drug itraconazole with ordered mesoporous silica. 1816 30

Swollen polymer networks exhibit multiscale pores filled with solvent. Such porosity, inherent to cross-linked polymers, determines some of their most relevant physical properties and applications. In this research, several samples of chemically crosslinked poly(N-vinylimidazole) were synthesized with the same permanent crosslinking density at two different conversions, and their inherent porosity was characterized on freeze-dried specimens by SEM, TEM and nitrogen physisorption. It was thus found that all of the samples showed pores, both on the nanometer and the micrometer scales, whose dimensions were mostly equal to or larger than the mesh size of the primary polymer network (22 nm) and whose volume and specific surface decreased with increasing conversion. Micropores have, in all cases, a very minor contribution. Samples synthesized with the largest comonomer concentrations show quasi-spherical mesopores (90 nm average diameter at any conversion) and macropores (from 5 to 10 microm with increasing conversion), whereas the mesopores of samples synthesized with the largest crosslinker ratios were channel-like (150 nm) and the macropores were interconnected contiguous voids (3 microm). Samples with intermediate compositions exhibit the lowest porosity due, mostly, to interconnected mesopores. The differences in shape were ascribed to the mechanism of phase separation, taking place during polymerization, even for samples that are transparent following polymerization. The inherent porosity is a significant source of spatial inhomogeneity, which contributes to the increase in turbidity. Light scattering decreases with increasing ionization when the degree of protonation is greater than 10%. An important consequence of the inherent porosity is that the degrees of swelling determined either gravimetrically or through size measurements are not equivalent.
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PMID:Porosity inherent to chemically crosslinked polymers. Poly(N-vinylimidazole) hydrogels. 1828 79

The facile synthesis of highly ordered mesoporous aluminas with high thermal stability and tunable pore sizes is systematically investigated. The general synthesis strategy is based on a sol-gel process associated with nonionic block copolymer as templates in ethanol solvent. Small-angle XRD, TEM, and nitrogen adsorption and desorption results show that these mesoporous aluminas possess a highly ordered 2D hexagonal mesostructure, which is resistant to high temperature up to 1000 degrees C. Ordered mesoporous structures with tunable pore sizes are obtained with various precursors, different acids as pH adjustors, and different block copolymers as templates. These mesoporous aluminas have large surface areas (ca. 400 m2/g), pore volumes (ca. 0.70 cm3/g), and narrow pore-size distributions. The influence of the complexation ability of anions and hydro-carboxylic acid, acid volatility, and other important synthesis conditions are discussed in detail. Utilizing this simple strategy, we also obtained partly ordered mesoporous alumina with hydrous aluminum nitrate as the precursor. FTIR pyridine adsorption measurements indicate that a large amount of Lewis acid sites exist in these mesoporous aluminas. These materials are expected to be good candidates in catalysis due to the uniform pore structures, large surface areas, tunable pore sizes, and large amounts of surface Lewis acid sites. Loaded with ruthenium, the representative mesoporous alumina exhibits reactant size selectivity in hydrogenation of acetone, D-glucose, and D-(+)-cellobiose as a test reaction, indicating the potential applications in shape-selective catalysis.
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PMID:Facile synthesis for ordered mesoporous gamma-aluminas with high thermal stability. 1828 38

We report the first formation of arrays of InN nanorods inside the nanoscale channels of mesoporous silica SBA-15. In(NO3)3 dissolved in methanol was incorporated into SBA-15 powder without prior pore surface functionalization. Formation of InN nanorod arrays was carried out by ammonolysis at 700 degrees C for 8 h. The final products have been characterized by FT-IR spectra, (29)Si MAS NMR spectra, Raman spectra, XRD patterns, TEM images, nitrogen adsorption-desorption isotherm measurements, and optical spectroscopy. The freestanding InN nanorods observed after silica framework removal with HF solution show diameters of 6-7.5 nm and lengths of 25-50 nm. Formation of a trace amount of In2O3 was also verified. The InN nanorods exhibit a broad band centered at around 550-600 nm, and a band gap energy of 1.5 eV was determined. No light absorption in the near-IR region was measured. The nanorods give a weak emission band centered at around 600 nm. These optical properties are believed to be related to the possible incorporation of oxygen during InN nanorod synthesis.
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PMID:Formation of indium nitride nanorods within mesoporous silica SBA-15. 1831 14

Efficient operation of a diode-pumped Nd:YAlO(3) laser on low-gain 1378- and 1385-nm transitions is reported for the first time, to our knowledge. A three-mirror folded cavity with a prism yielded a cw laser output power of 800 mW for an absorbed pump power of 11 W. The laser beam was TEM(00). We managed to eliminate the instabilities in the output power by purging the cavity of water vapor with nitrogen.
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PMID:High-Power Continuous-Wave Diode-Pumped Nd:YAlO(3) Laser that Emits on Low-Gain 1378- and 1385-nm Transitions. 1835 20

The straightforward, efficient, solventless, RAPET (reactions under autogenic pressure at elevated temperature) approach was explored for the fabrication of core-shell nanomaterials. Carbon-encapsulated SnS and SnSe nanorods were synthesized by a one-step thermal decomposition of tetramethyltin in the presence of either S or Se powder in a closed reactor at 700 degrees C for 40 min, under their autogenic pressure in an inert atmosphere. The powder X-ray diffraction measurements provided structural evidence for the formation of pure orthorhombic phases of SnS or SnSe particles. The Raman spectroscopy measurements ensured that the nature of the coated carbon was semigraphitic. The scanning electron micrographs verified the 1D morphology of the formed SnS and SnSe chalcogenides, and their stoichiometry was confirmed by EDAX measurements. The HR-TEM micrographs distinguished between core and shell morphologies. The nitrogen gas adsorption on the surface of core-shell nanostructures was determined by BET surface area analysis. The plausible mechanism for the creation of chalcogenide cores (SnS or SnSe) with a carbon shell was elucidated.
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PMID:Core-shell nanorods of SnS-C and SnSe-C: synthesis and characterization. 1836 19

In this study, nitrogen-doped titanium dioxide (TiO2) powders were synthesized in two ways: by heating of titanium hydroxide with urea and by direct hydrolysis of titanium tetraisopropoxide (TTIP) with ammonium hydroxide. The samples were characterized by structural (XRD), analytical (XPS), optical (UV/Vis absorption/reflection and Raman spectroscopy) and morphological (SEM, TEM) techniques. The characterization suggested that the doped materials have anatase crystalline form without any detectable peaks that correspond to dopants. The absorption threshold of titanium dioxide was moved in the visible range of optical spectrum from 3.2 eV to 2.20 eV. Particle sizes of synthesized powders were obtained from XRD measurements and from TEM data ranging from 6-20 nm. XPS and Raman spectroscopy were used for detection of nitrogen in doped samples.
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PMID:TiO2 doped with nitrogen: synthesis and characterization. 1846 79


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