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Gas hydrates of argon and methane synthesized at high pressures: composition, thermal expansion, and self-preservation.

For the first time, the compositions of argon and methane high-pressure gas hydrates have been directly determined. The studied samples of the gas hydrates were prepared under high-pressure conditions and quenched at 77 K. The composition of the argon hydrate (structure H, stable at 460-770 MPa) was found to be Ar.(3.27 +/- 0.17)H(2)O. This result shows a good agreement with the refinement of the argon hydrate structure using neutron powder diffraction data and helps to rationalize the evolution of hydrate structures in the Ar-H(2)O system at high pressures. The quenched argon hydrate was found to dissociate in two steps. The first step (170-190 K) corresponds to a partial dissociation of the hydrate and the self-preservation of a residual part of the hydrate with an ice cover. Presumably, significant amounts of ice Ic form at this stage. The second step (210-230 K) corresponds to the dissociation of the residual part of the hydrate. The composition of the methane hydrate (cubic structure I, stable up to 620 MPa) was found to be CH(4).5.76H(2)O. Temperature dependence of the unit cell parameters for both hydrates has been also studied. Calculated from these results, the thermal expansivities for the structure H argon hydrate are alpha(a) = 76.6 K(-1) and alpha(c) = 77.4 K(-1) (in the 100-250 K temperature range) and for the cubic structure I methane hydrate are alpha(a) = 32.2 K(-1), alpha(a) = 53.0 K(-1), and alpha(a) = 73.5 K(-1) at 100, 150, and 200 K, respectively.

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Structural and spectroscopic investigations of blue, vanadium-doped ZrSiO4 pigments prepared by a sol-gel route.

A sol-gel reaction starting from silicon and zirconium alkoxides, in water-ethanol mixtures, was employed to obtain vanadium-doped zirconium silicate powders (zircon). The reactions were performed by modulating both (a) the amount of the vanadium salt in the starting mixture and also (b) the amount of mineralizer (NaF). The products of the sol-gel reaction were calcined at 600, 800, 1000, and 1200 degrees C. The samples were characterized by X-ray powder diffraction (XRPD), electron paramagnetic resonance spectroscopy (EPR), scanning electron microscopy (SEM), X-ray absorption near-edge spectroscopy (XANES), and diffuse UV-vis-near-IR reflectance spectroscopy. Results from the structural, morphological, and optical characterization are examined and cross-compared to produce a consistent picture of the key factors leading to the formation, growth, and optical properties of the reaction products.

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Preparation by high-energy milling, characterization, and catalytic properties of nanocrystalline TiO2.

Titanium dioxide (TiO2) is widely used for applications in heterogeneous photocatalysis. We prepared nanocrystalline powders of the anatase as well as the rutile modification by high-energy ball milling of the coarse grained source materials for up to 4 h. The resulting average grain size was about 20 nm. The morphology of the powders was investigated with transmission electron microscopy, X-ray powder diffraction, and BET surface area determination. Measurements of the catalytic activity reveal a maximum as a function of the milling time at about 40 min. This maximum could be explained by a superposition of two counteracting effects. The first one is the increase of the specific surface area resulting in an increase of the catalytic activity, and the second one is a change of the electronic structure at the surface of the TiO2 particles corresponding to a reduction of the surface. The latter one was confirmed by light absorption experiments, X-ray photoelectron spectroscopy, and electron paramagnetic resonance spectroscopy.

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Liquid crystalline metal-free phthalocyanines designed for charge and exciton transport.

A joint theoretical and experimental study of the electronic and structural properties of liquid crystalline metal-free phthalocyanines bearing a strong potential for charge and exciton transport has been performed. The synthesis of such compounds has been triggered by quantum chemical calculations showing that: (i) hole transport is favored in metal-free phthalocyanines by their extremely low reorganization energy (0.045 eV) and large electronic splittings; and (ii) the efficiency of energy transfer along the one-dimensional discotic stacks is weakly affected by rotational disorder due to the two-dimensional character of the molecules. We have synthesized two metal-free phthalocyanines with different branched aliphatic chains on the gram scale to allow for a full characterization of their solid-state properties. The two compounds self-organize in liquid crystalline mesophases, as evidenced by optical microscopy, differential scanning calorimetry, X-ray powder diffraction, and molecular dynamics simulations. They exhibit a columnar rectangular mesophase at room temperature and a columnar hexagonal mesophase at elevated temperature.

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Straight and thin ZnO nanorods: hectogram-scale synthesis at low temperature and cathodoluminescence.

A novel seed-assisted chemical reaction at 95 degrees C has been employed to synthesize uniform, straight, thin, and single-crystalline ZnO nanorods on a hectogram scale. The molar ratio of ZnO seed and zinc source plays a critical role in the preparation of thin ZnO nanorods. At a low molar ratio of ZnO seed and zinc source, javelin-like ZnO nanorods consisting of thin ZnO nanorods with a diameter of 100 nm and thick ZnO nanorods with a diameter of 200 nm have been obtained. In contrast, straight ZnO nanorods with a diameter of about 20 nm have been prepared. Dispersants such as poly(vinyl alcohol) act spatial obstructors to control the length of ZnO nanorods. The morphology, structure, and optical property of the ZnO nanostructures prepared under different conditions have been characterized by transmission electron microscopy, field emission scanning electron microscopy, X-ray powder diffraction, high-resolution transmission electron microscopy, and cathodoluminescence. The formation mechanisms for the synthesized nanostructures with different morphologies have been phenomenologically presented.

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Enhanced electrorheological activity of mesoporous Cr-doped TiO2 from activated pore wall and high surface area.

To enhance electrorheological (ER) activity by improving interfacial polarization, we prepared a new mesoporous Cr-doped TiO2 ER material by a copolymer-templated sol-gel method. The material was characterized by differential scanning calorimeter and thermogravimetric (DSC-TG) analysis, Fourier transform infrared (FT-IR), X-ray powder diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption, and X-ray photoelectron spectroscopy (XPS) techniques. The ER activity was studied by the rheological curve and yield stress under an electric field. The results showed that the mesoporous Cr-doped TiO2 ER material possessed a high surface area over 200 m2/g and a crystalline anatase pore wall doped by different valent Cr ions. The ER activity of mesoporous Cr-doped TiO2 was higher than that of nonporous Cr-doped TiO2. The yield stress and ER efficiency of the mesoporous Cr-doped TiO2 ER suspension was 3 times as high as that of the nonporous Cr-doped TiO2 ER suspension, 7 times as high as that of the mesoporous undoped TiO2 ER suspension, and 20 times as high as that of the nonporous pure TiO2 ER suspension. Furthermore, the ER activity of mesoporous Cr-doped TiO2 showed a dependence on surface area, and the high porosity or surface area samples showed higher ER activity. The dielectric spectra analysis showed that the mesoporous Cr-doped TiO2 ER suspension possessed a significantly larger interfacial polarizability compared with the nonporous Cr-doped TiO2 ER suspension, and the regular change of polarizability with surface area or porosity was in accordance with the change of ER activity with surface area or porosity. The improvement of dielectric properties or polarization could well explain the enhancement of the ER activity of mesoporous Cr-doped TiO2.

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Structural and vibrational characterization of tetracyanoethylene-hexamethylbenzene as a function of pressure.

The neutron powder diffraction and inelastic neutron scattering (INS) spectra of the electron donor-acceptor complex, tetracyanoethylene-hexamethylbenzene have been studied as a function of pressure to 0.414 GPa. Using the PW91 and PBE density functional theories, the unit cell vectors were calculated as a function of pressure and are compared to those experimentally obtained from the diffraction data. The calculated lattice vectors display large errors at low pressures but were found to be in close agreement with the experimental vectors at 0.414 GPa. Comparison of the experimental INS spectra of the TCNE-HMB enabled assignment of specific vibrational modes while providing a direct measurement of the effect of pressure on the complex. The PW91 vibrational frequency calculations reproduced both the vibrational intensities and frequencies with relative accuracy.

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Examination of spinel and nonspinel structural models for gamma-Al2O3 by DFT and rietveld refinement simulations.

Despite the widespread use of gamma-Al2O3, there is still considerable disagreement over the nature of its structure due to both its poor crystallinity and differing preparation techniques during experimentation. Using density-functional theory (DFT) calculations and Rietveld simulations and refinement, the structure of three spinel-related models and a recently proposed nonspinel model were studied in reference to synchrotron X-ray powder diffraction (SXPD) patterns. The spinel-based structural models represent the structural features of gamma-Al2O3 better than the nonspinel model. The major failure of the nonspinel model is that the model cannot reproduce the SXPD reflection originating from tetrahedral aluminum. The Rietveld-refined spinel model can accurately reproduce the lattice parameters and other structural features of gamma-Al2O3, and it can generate a consistent diffraction peak at 2theta which lies between the splitting peaks of the experimental pattern that are originated from the disordered tetrahedral aluminum cations.

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Crystal structure of zeolite MCM-68: a new three-dimensional framework with large pores.

The crystal structure of the aluminosilicate MCM-68 was solved from synchrotron powder diffraction data by the program FOCUS. The unit cell framework contains Si100.6Al11.4O224. This material crystallizes in space group P42/mnm, where, after Rietveld refinement, a=18.286(1) A and c=20.208(2) A. A three-dimensional framework is found that contains continuous 12-ring channels and two orthogonal, intersecting, undulating 10-ring channels. Rietveld refinement of the model coordinates optimizes the framework geometry, to match the observed intensity profile by Rwp=0.1371, R(F2)=0.1411. It is not possible to determine the location of approximately 0.84 K+ cations remaining in the unit cell after the material is steamed and then dehydrated. The framework model also successfully predicts observed electron diffraction data in two projections, and the tetragonal projection can be determined independently from these data by direct methods. The calculated density of the framework structure is 1.66 g/cm3, and the T-site framework density is 16.6 T/1000 A3.

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Pt and Ru X-ray absorption spectroscopy of PtRu anode catalysts in operating direct methanol fuel cells.

In situ X-ray absorption spectroscopy, ex situ X-ray fluorescence, and X-ray powder diffraction enabled detailed core analysis of phase segregated nanostructured PtRu anode catalysts in an operating direct methanol fuel cell (DMFC). No change in the core structures of the phase segregated catalyst was observed as the potential traversed the current onset potential of the DMFC. The methodology was exemplified using a Johnson Matthey unsupported PtRu (1:1) anode catalyst incorporated into a DMFC membrane electrode assembly. During DMFC operation the catalyst is essentially metallic with half of the Ru incorporated into a face-centered cubic (FCC) Pt alloy lattice and the remaining half in an amorphous phase. The extended X-ray absorption fine structure (EXAFS) analysis suggests that the FCC lattice is not fully disordered. The EXAFS indicates that the Ru-O bond lengths were significantly shorter than those reported for Ru-O of ruthenium oxides, suggesting that the phases in which the Ru resides in the catalysts are not similar to oxides.

Catalysis↗

Cation distribution in LiMgVO4 and LiZnVO4: structural and spectroscopic study.

The room temperature cation occupancy in LiMgVO(4) and LiZnVO(4) crystallographic sites is obtained by means of the combined use of X-ray powder diffraction (XRPD), (7)Li and (51)V magic angle spinning nuclear magnetic resonance (MAS NMR), and micro-Raman measurements. In the LiMgVO(4) Cmcm orthorhombic structure, the 4c (C(2)(v) symmetry) tetrahedral vanadium site is fully ordered; on the contrary, the Li 4c tetrahedral site and the 4b (C(2)(h) symmetry) Mg octahedral site display about 22% of reciprocal cationic exchange. Higher cationic disorder is observed in LiZnVO(4): the three cations can distribute on the three tetrahedral and distinct sites of the R-3 structure. XRPD and MAS NMR analysis results highly agree for what concerns vanadium ion distribution on the three cationic sites (about 25, 26, and 47%). From the full profile fitting of XRPD patterns with the Rietveld method, it is also obtained that Li(+) displays a slightly preferred occupation of the T1 position (approximately 55%) and Zn(2+) of the T2 position (approximately 46%). The vibrational spectra of the two compounds are characterized by different peak positions and broadening of the Raman modes, reflecting the cation distribution and the local vibrational unit distortion. A comparison is also made with recent Raman results on Li(3)VO(4). High temperature XRPD measurements rule out possible structural transitions up to 673 K for both compounds.

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Comparison of decanethiolate gold nanoparticles synthesized by one-phase and two-phase methods.

We investigated the differences between the decanethiolate gold nanoparticles synthesized by two different routes: one-phase and two-phase methods. Their properties were compared in bulk and at the air-water interface by transmission electron microscopy (TEM), X-ray reflectivity (XR), extended X-ray absorption fine structure (EXAFS) spectroscopy, X-ray powder diffraction (XRD), thermal gravimetric analysis (TGA), time-of-flight secondary-ion mass spectrometry (TOF-SIMS), electron paramagnetic resonance (EPR), and Langmuir-Blodgett technique. The mean nanoparticles sizes obtained by EXAFS and XRD were found to be smaller than those by the TEM measurements. We explained these differences by the structural disorder and multiple twinning in the nanoparticles. The one-phase particles were found by EXAFS to be smaller and had a higher grafting density of thiol chains than the two-phase particles. We attributed these differences to the enhanced disorder of the one-phase particles. At the air-water interface, the one-phase particles did not spread, while the two-phase particles spread and formed Langmuir films. TEM and XR results revealed that the close-packed monolayer of the two-phase particles collapsed and folded into multilayer films upon further compression.

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Microwave-assisted one-step synthesis of polyacrylamide-metal (M = Ag, Pt, Cu) nanocomposites in ethylene glycol.

Polyacrylamide-metal (M = Pt, Ag, Cu) nanocomposites with metal nanoparticles homogeneously dispersed in the polymer matrix have been successfully prepared with the corresponding metal salt and acrylamide monomer in ethylene glycol by microwave heating. This method is based on the single-step simultaneous formation of metal nanoparticles and polymerization of the acrylamide monomer, leading to a homogeneous distribution of metal nanoparticles in the polyacrylamide matrix. Ethylene glycol acts as both a reducing reagent and a solvent, thus no additional reductant is needed. Another advantage is that no initiator for AM polymerization and no surfactant for stabilization of metal nanoparticles are necessary. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR), ultraviolet visible (UV-vis) absorption spectra, and thermogravimetric (TG) and differential scanning calorimetric analysis (DSC).

Acrylic Resins↗

Precipitation of nanostructured copper oxalate: substructure and growth mechanism.

The possibility of controlling materials properties by tailoring their substructure at the nanometer scale is a current topic of great interest. To do so, a fundamental understanding of the growth mechanism is of key importance and an analytical challenge as nanostructured materials are often produced by precipitation methods at high supersaturations where formation kinetics are fast. The current study focuses on the precipitation of copper oxalate, which has been previously shown to produce self-assembled ordered nanostructured particles with the promise of being able to tailor this nanometer substructure. In the current study we investigate in detail the growth mechanism and kinetics of precipitation by using in-situ particle size measurement or by stopping the reaction at various stages and using ex-situ methods. Combining the ex-situ methods of high-resolution scanning electron microscopy, transmission electron microscopy, and X-ray powder diffraction along with the in-situ methods, we were able to follow the growth process from 2 min to 2 weeks. The results in the 2-30 min period lead to the proposal of a core-shell growth model with a poorly ordered core and a well-structured shell of nanosized crystallites (50-70 nm), adding support to the brick-by-brick model previously proposed for this phase of particle growth. Particle evolution over long periods up to 2 weeks show a ripening which produces lens-shaped particles that eliminate the "high" surface energy faces observed in the earlier stages of growth. A more complete growth mechanism for copper oxalate precipitation at moderate supersaturations is proposed similar to recent findings for other self-assembled nanostructured particles.

Chemical Precipitation↗

Microwave-assisted synthesis of calcium carbonate (vaterite) of various morphologies in water-ethylene glycol mixed solvents.

A fast microwave-assisted method is reported for the synthesis of CaCO3 (vaterite) with various morphologies in the water/ethylene glycol (EG) system with surfactants. Our experiments show that microwave heating, reaction time, surfactant, and the water-EG mixed solvents play important roles in the morphology of vaterite. Vaterite with dagger-like, bicone-like, shuttle-like morphology and microspheres self-assembled from nanoparticles have been obtained by adjusting the experimental parameters. The products were characterized by X-ray powder diffraction, transmission electron microscopy, and scanning electron microscopy.

Calcium Carbonate↗

Two-component system CCl4 + (CH3)3CBr: extrema in equilibria involving orientationally disordered phases.

Phase equilibria involving orientationally disordered (OD) and liquid phases of the two-component system between carbon tetrachloride (CCl4) and 2-methyl-2-bromomethane ((CH3)3CBr) have been determined by means of X-ray powder diffraction and thermal analysis techniques from 210 K up to the liquid state. The isomorphism relation between the OD stable face-centered cubic (FCC) phase of (CH3)3CBr and the metastable FCC phase of CCl4 has been demonstrated throughout the continuous evolution of the lattice parameters and the existence of the two-phase equilibrium [FCC + L] for the whole range of composition, despite the monotropy of the FCC phase for the CCl4 component with respect to its OD rhombohedral (R) stable phase. A continuous series of OD R mixed crystals is found, which confirms the R lattice symmetry of the OD phase II of (CH3)3CBr, for which the crystallographic results have been long-time misinterpreted. X-ray patterns of such a phase were indexed according to the recent single-crystal results obtained by Rudman (Rudman, R. J. Mol. Struct. 2001, 569, 157). In addition, some experimental evidences are given to confirm the number of molecules per unit cell (Z = 21). The thermodynamic assessment reproduces coherently the phase diagram for the stable [R + L] and [R + FCC] two-phase equilibria as well as for the partially metastable [FCC + L] two-phase equilibrium and provides a set of data for the thermodynamic properties of nonexperimentally available phase transitions of pure components. Surprisingly, the phase equilibrium involving R and FCC OD phases appears as one of the very few showing a solid-solid equilibrium with two extremes.

Journal Article↗

Preparation, characterization, and optical, electrochemical property research of CdS/PAM nanocomposites.

CdS/PAM nanocomposites have been successfully synthesized in situ via a ultrasound-assisted route under ambient condition, employing CdCl(2) and Na(2)S(2)O(3) as Cd(2+) and S(2-) ion sources and acrylamide (AM) and (NH(4))(2)S(2)O(8) as organic monomers and initiating reagents, respectively. The results from X-ray powder diffraction (XRD) analysis and the IR spectrum of the final product showed the formation of CdS nanoparticles and the polymerization of AM monomers. SEM observations showed that the CdS/PAM nanocomposites could film on the quartz substrate and some holes in which many nanorods regularly arranged distributed on the film. The UV-vis absorption and PL spectra of CdS/PAM nanocomposites obviously differed from those of CdS nanoparticles prepared under the same conditions due to the presence of PAM. The electrochemical research showed that CdS/PAM nanocomposites had a stronger ability to promote electron transfers between Hb and the Au electrode than CdS nanoparticles prepared under the same conditions. A possible formation mechanism was also suggested based on the results of experiments.

Journal Article↗

Facile synthesis and catalytic property of porous tin dioxide nanostructures.

Porous tin dioxide (SnO(2)) nanostructures consisting of nanoplates are prepared through thermal decomposition of the mixed solution composed of dibutyltin dilaurate and acetic acid. The aggregations of the nanoplates give rise to large macropores with the size of about 100-300 nm. These nanoplates have a wormhole-like porous structure with the size of about 4 nm and possess high surface area. X-ray powder diffraction, transmission electron microscopy, scanning electron microscopy, infrared spectroscopy, and nitrogen sorption have been employed to characterize the obtained porous structures. It is found that the obtained nanostructures exhibit excellent catalytic activity toward methanol decomposition. Such porous structures with high surface area have promising industrial applications as catalysts.

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