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Our work reports the hydrothermal synthesis of a bimetallic composite CoMoS, followed by the addition of cellulose fibers and its subsequent carbonization under Ar atmosphere (CoMoS@C). For comparison, CoMoS was heat-treated under the same conditions and referred as bare-CoMoS. X-ray diffraction analysis indicates that CoMoS@C composite matches with the CoMoS 4 phase with additional peaks corresponding to MoO 3 and CoMoO 4 phases, which probably arise from air exposure during the carbonization process. Scanning electron microscopy images of CoMoS@C exhibit how the CoMoS material is anchored to the surface of carbonized cellulose fibers. As anode material, CoMoS@C shows a superior performance than bare-CoMoS. The CoMoS@C composite presents an initial high discharge capacity of ∼1164 mA h/g and retains a high specific discharge capacity of ∼715 mA h/g after 200 cycles at a current density of 500 mA/g compared to that of bare-CoMoS of 102 mA h/g. The high specific capacity and good cycling stability could be attributed to the synergistic effects of CoMoS and carbonized cellulose fibers. The use of biomass in the anode material represents a very easy and cost-effective way to improve the electrochemical Li-ion battery performance., Competing Interests: The authors declare no competing financial interest.

Hydrotreatment catalytic operations are commonly performed industrially by layered molybdenum sulfide promoted by cobalt or nickel in order to remove heteroelements (S, N, O) from fossil fuels and biofuels. Indeed, these heteroelements are responsible of the emission of pollutants when these fuels are used in vehicles. In this respect, previous studies made by our research group have shown that the active phase under steady state conditions is partially carbided while strong bending effects of MoS2 slabs were also observed. However, up to now, the morphology of the resulting Co/MoSxCy carbided catalyst has not been fully characterized. In the present study, for the first time, a chemical reaction between the carbon content of a TEM Cu/C grid and a freshly sulfide Co/MoS2 catalyst was in situ observed at 300 °C and 450 °C by HRTEM experimental techniques at ~10 nm of resolution. Results indicate that bending of MoS2 layers occurred due to carbon addition on MoS2 edge sites, as observed in stabilized catalysts after HDS reaction. Using a silicon grid, only cracks of MoS2 slabs were observed without bending effect confirming the role of structural-carbon in this change of morphology., (Copyright © 2012 Elsevier B.V. All rights reserved.)

The chemical synthesis of gold nanoparticles (NP) by using gold (III) chloride trihydrate (HAuCl∙3H₂O) and sodium citrate as a reducing agent in aqueous conditions at 100 °C is presented here. Gold nanoparticles areformed by a galvanic replacement mechanism as described by Lee and Messiel. Morphology of gold-NP was analyzed by way of high-resolution transmission electron microscopy; results indicate a six-fold icosahedral symmetry with an average size distribution of 22 nm. In order to understand the mechanical behaviors, like hardness and elastic moduli, gold-NP were subjected to nanoindentation measurements-obtaining a hardness value of 1.72 GPa and elastic modulus of 100 GPa in a 3-5 nm of displacement at the nanoparticle's surface.

We have used laboratory and synchrotron x-ray diffraction to investigate the structural and chemical changes undergone by polycrystalline RbH(2)PO(4) upon heating within the 30-250 °C temperature interval. Our data show no evidence of the previously reported onset of partial polymerization at T = 96 °C (Park et al 2001 J. Phys.: Condens. Matter 13 9411) which was proposed as an explanation for the high-temperature proton conductivity enhancement in phosphate-based solid acids. Instead, we found that a tetragonal [Formula: see text] monoclinic polymorphic transition initiates at T≈90 °C. The transition is complete at T≈130 °C, and the new monoclinic RbH(2)PO(4) polymorph is stable upon further heating to T = 200 °C. Moreover, its crystal structure is isomorphic to that of monoclinic CsH(2)PO(4). This remarkable similarity suggests that the microscopic structures and dynamics responsible for the high-temperature superprotonic behavior of RbH(2)PO(4) could be the same as those of its Cs-based counterpart.

To clarify the microscopic origin of the temperature-induced three-order-of-magnitude jump in the proton conductivity of CsH(2)PO(4) (superprotonic behavior), we have investigated its crystal structure modifications within the 25-300 degrees C temperature range under both ambient- and high-pressure conditions using synchrotron x-ray diffraction. Our high-pressure data show no indication of the thermal decomposition/polymerization at the crystal surface recently proposed as the origin of the enhanced proton conductivity [Phys. Rev. B 69, 054104 (2004)]. Instead, we found direct evidence that the superprotonic behavior of the title material is associated with a polymorphic structural transition to a high-temperature cubic phase. Our results are in excellent agreement with previous high-pressure ac impedance measurements.

Maya Blue is an ancient blue pigment composed of palygorskite clay and indigo. It was used by the ancient Maya and provides a dramatic background for some of the most impressive murals throughout Mesoamerica. Despite exposure to acids, alkalis, and chemical solvents, the color of the Maya Blue pigment remains unaltered. The chemical interaction between palygorskite and indigo form an organic/inorganic complex with the carbonyl oxygen of the indigo bound to a surface Al(3+) in the Si-O lattice. In addition indigo will undergo an oxidation to dehydroindigo during preparation. The dehydro-indigo molecule forms a similar but stronger complex with the Al(3+). Thus, Maya Blue varies in color due to the mixed indigo/dehydroindigo complex. The above conclusions are the result of application of multiple techniques (X-ray diffraction, differential thermal analysis/thermal gravimetric analysis, high resolution transmission electron microscopy, scanning electron microscopy, infrared and Raman spectroscopy) to the characterization of the organic/inorganic complex. A picture of the bonding of the organic molecule to the palygorskite surface forming a surface complex is developed and supported by the results of density functional theory calculations. We also report that other organic molecules such as thioindigo form similar organic/inorganic complexes thus, opening an entirely new class of complex materials for future applications.

Development of synchrotron techniques for the determination of the structure of disordered, amorphous and surface materials has exploded over the past 20 years owing to the increasing availability of high-flux synchrotron radiation and the continuing development of increasingly powerful synchrotron techniques. These techniques are available to materials scientists who are not necessarily synchrotron scientists through interaction with effective user communities that exist at synchrotrons such as the Stanford Synchrotron Radiation Laboratory. In this article the application of multiple synchrotron characterization techniques to two classes of materials defined as 'surface compounds' is reviewed. One class of surface compounds are materials like MoS(2-x)C(x) that are widely used petroleum catalysts, used to improve the environmental properties of transportation fuels. These compounds may be viewed as 'sulfide-supported carbides' in their catalytically active states. The second class of 'surface compounds' are the 'Maya blue' pigments that are based on technology created by the ancient Maya. These compounds are organic/inorganic 'surface complexes' consisting of the dye indigo and palygorskite, common clay. The identification of both surface compounds relies on the application of synchrotron techniques as described here.

Chromium contamination of the environment has become an important issue due to the potential health threat it poses. Conventional technologies to clean up heavy metal ions from contaminated waters have been utilized, but these technologies are not cost-effective. However, the use of agricultural waste byproducts for the removal of Cr(VI) from contaminated waters may be a new cost-effective alternative. Oat byproducts from the Juarez Valley in Mexico were studied for the ability to bind Cr(VI) under different temperature and time conditions. The metal binding ability of oat byproducts was calculated from experimental data collected at temperatures of 8, 26, and 54 degrees C, and time exposures of 1, 6, 24, 48, and 72 h at each temperature. These results showed that the binding of Cr(VI) to oat biomass increased as time and temperature increased. The bound chromium was recovered from the oat biomass by treatment with 0.2M HCl. Through the use of X-ray absorption spectroscopy, the reduction of Cr(VI) to Cr(III) was determined to occur by the oat byproducts. These results indicate that the use of agricultural waste byproducts could be a better alternative for the removal and subsequent reduction of Cr(VI) to Cr(III) from contaminated waters.

Lithographic techniques were used to expose edge surfaces in layered molybdenum disulfide single crystals. This microstructuring produced ideal samples for the study of the surface morphology and electronic structure of this catalytically important material. The optical absorption that was measured at mid-gap increased by two orders of magnitude after texturing. This increase resulted from reduced molybdenum at surface defects that are located on edge planes, as shown by photoemission spectroscopy. This information cannot easily be obtained on conventional crystals with predominantly basal plane surfaces.

Fibrous apatite has been grown by the enzymatic hydrolysis of calcium beta-glycerophosphate on reconstituted calfskin collagen tapes which had been modified by the addition of a phosphoprotein, phosvitin, in the presence of a cross-linking agent, dimethylsuberimidate. The deposits were identified as a carbonate-bearing hydroxyapatite by x-ray diffraction, and scanning electron micrographs confirmed their fibrous character.

Molybdenum disulfide has been prepared in an unusual poorly crystalline form, termed the "rag" structure, consisting of several stacked but highly folded and disordered S-Mo-S layers. This previously unknown structure demonstrates the flexible and macromolecular nature of the layered transition metal dichalcogenides. The determination of this structure provides a basis for understanding its highly broadened x-ray diffraction pattern and relatively low surface area, and is a starting point for optimizing the catalytic and surface properties of molybdenum disulfide.