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Diffractometry
Kinds of Diffractometry Selected AbstractsEffect of the substrate temperature on the properties of the RF sputtered TiO2 thin filmsPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 9 2010I. Ben Mbarek Abstract Titanium dioxide (TiO2) thin films were deposited by RF magnetron sputtering on glass and silicon substrates at different substrate temperatures (20, 100, 200 and 300 °C). The structural and morphological characteristics of the films were investigated by X ray Diffractometry (XRD) and Atomic Force Microscopy (AFM) while the optical properties of the films were studied by optical spectroscopy. It was shown that at room temperature, TiO2 films grown on glass were amorphous following the substrate structure. At higher temperatures, XRD detected only a nanocrystalline rutile TiO2 structure. This indicated that the transition temperature toward the most stable TiO2 phase was obtained from 100 °C and the crystallinity was enhanced at higher growth temperature. For TiO2 films grown on Si substrates, only a nanocrystalline anatase TiO2 structure was obtained at room temperature. At higher temperatures, we noticed the appearance of other secondary phases related to rutile, anatase and brookite structures. From AFM images, we noticed that at room temperature, the films were porous. With increasing the temperature, the structure of the films became crystallized showing a columnar structure. Film growth and structural properties were discussed in terms of the Thornton model. From optical analysis, the films were transparent with an indirect band gap and a refraction index which reached 3.09 eV and 2.7, respectively. The reflectance and transmittance spectra showed, not only that there was a little translation from UVB to UVA and near-visible range, but also a decrease of reflection with a temperature increase indicating that the films could be used as anti-reflection coatings. (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Examination of an unusual grain boundary in CaF2PHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 11 2004M.E. Msall Abstract We have examined a grain boundary in CaF2 using Phonon Imaging and Electron Backscatter Diffractometry (EBSD). Unlike the <111> twin boundary typically found in CaF2, the crystal grains on either side of the boundary are not simply related to any principle symmetry directions, and are not related to one another by symmetry operations of the cubic group. In spite of the high degree of misalignment of the crystalline lattices, phonons can pass this grain boundary without excessive energy loss. Phonon images of samples taken from different sections of the grain boundary show that the structural properties of the grain boundary are constant over a large area. Computer simulations of phonon scattering at the interface based on acoustic mismatch models demonstrate that the caustic positions are sensitive to small changes in the relative orientation of the two pieces and to the projection of the grain boundary on the image plane. EBSD gives the needed high precision measurement of the relative orientation, resulting in a superior model of phonon transmission through this very asymmetric interface. (© 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Synthesis, Crystal Structure Determination from X-Ray Powder Diffractometry and Vibrational Spectroscopic Properties of Mg[N(CN)2]2×4H2O.CHEMINFORM, Issue 36 2005Elisabeth Irran Abstract For Abstract see ChemInform Abstract in Full Text. [source] Synthesis of rhombohedral strontium carbonate aggregates at the water/hexamethylene interface with cetyltrimethylammonium bromideCRYSTAL RESEARCH AND TECHNOLOGY, Issue 8 2008Long Chen Abstract Unusual rhombohedral strontium carbonate (SrCO3) aggregates have been synthesized in situ from strontium nitrate by the slow release of carbon dioxide by alkaline hydrolysis of diethyl carbonate at the water/hexamethylene interface in the presence of cetyltrimethylammonium bromide (CTAB). Transmission electron microscopy, Fourier transform infrared spectroscopy and X-ray powder diffractometry were used to characterize the products. The results indicate that rhombohedral SrCO3 aggregates are obtained with weaker crystallinity and sizes of several micrometers. The possible formation mechanism of the SrCO3 aggregates at the interface is discussed, which can be interpreted by particle-aggregation based non-classical crystallization laws. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Studies on the structural, thermal and optical behaviour of solution grown organic NLO material: 8-hydroxyquinolineCRYSTAL RESEARCH AND TECHNOLOGY, Issue 2 2007N. Vijayan Abstract Single crystal of 8-hydroxyquinoline (8HQ) having chemical formula C9H7NO, an organic nonlinear optical (NLO) material has been successfully grown by slow evaporation solution growth technique at room temperature. The crystal system has been confirmed from the powder X-ray diffraction (PXRD) analysis. The crystalline perfection was evaluated by high resolution X-ray diffractometry (HRXRD). From this analysis we found that the quality of the crystal is quite good. However, a very low angle (tilt angle 14 arc sec) boundary was observed which might be due to entrapping of solvent molecules in the crystal during growth. Its optical behavior has been examined by UV-Vis. analysis, which shows the absence of absorbance between the wavelengths ranging from 400 to 1200 nm. From the thermal analysis it was observed that the material exhibits single sharp weight loss starting at 113°C without any degradation. The laser damage threshold was measured at single shot mode and the SHG behavior has been tested using Nd:YAG laser as a source. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Influence of the starting powders on the synthesis of nickel ferriteCRYSTAL RESEARCH AND TECHNOLOGY, Issue 8 2006F. Kenfack Abstract The thermal decomposition of freeze-dried nickel(II)-iron(III) formate was investigated by means of DTA, TG, mass spectrometry and X-ray powder diffractometry. For the preparation of homogeneous freeze-dried nickel(II)-iron(III) formate precursors, a rigorous control of nickel ion concentration in the precursor solution was required. The decomposition of the reactive nickel(II)-iron(III) formate does not only reflect aspects of single formates, but also an interaction between components which lowers the decomposition temperature. Crystalline nickel ferrite powders were obtained at 600-800°C. This temperature is quite lower than 1100°C employed for the ceramic method. In the presence of air, the regeneration of nickel ferrite from the taenite phase (,Ni,Fe) is accomplished at 800°C. This temperature is also 300°C below the temperature employed when the mixtures NiO:,-Fe2O3 or Ni:2Fe are the starting powders. The main reason for the high reactivity of the freeze-dried formates and the taenite alloy is the large homogeneity of these precursors. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Bis(fluoromesityl) Palladium Complexes, Archetypes of Steric Crowding and Axial Protection by ortho Effect , Evidence for Dissociative Substitution Processes , Observation of 19F,19F Through-Space CouplingsEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 11 2004Camino Bartolomé Abstract Bisarylated complexes trans -[Pd(Fmes)2(SR2)2] [Fmes = 2,4,6-tris(trifluoromethyl)phenyl (fluoromesityl); SR2 = SMe2, tht; tht = tetrahydrothiophene] are precursors for various bisarylated fluoromesityl palladium(II) complexes by ligand-substitution reactions. Boiling under reflux in acetonitrile gives the mixed complexes trans -[Pd(Fmes)2(NCMe)(SR2)], whereas boiling under reflux in toluene leads to trans -[PdCl2L2] (L = PMe3, tBuNC, pTol-NC, 4-MePy), in the presence of neutral monodentate ligands, or to (NnBu4)[trans -Pd(Fmes)2I(SR2)] when treated with (NnBu4)I. trans -[Pd(Fmes)2(SMe2)2] reacts with bidentate ligands, also boiling under reflux in toluene, to give [Pd(Fmes)2(L,L)] [L,L = Me2bipy, 2,2, - biquinolyl, ,2N,N, -OCPy2, dppm (Ph2PCH2PPh2), dppe (Ph2PCH2CH2PPh2), pte (PhSCH2CH2SPh), ,2S,N -SPPh2Py, ,2O,N -OPPhPy2], or the bimetallic complex [Pd(Fmes)2(,-1,N:1,2,O:2,N -Py2MeCO)Pd(Fmes)(SMe2)] (characterized by X-ray diffractometry) when treated with (OH)(CH3)CPy2. The crowding associated with two Fmes groups produces several interesting features: (1) trans complexes are preferred over cis complexes, against the expected electronic preferences; (2) the low-temperature NMR spectra of several complexes, or the X-ray diffraction structure of [Pd(Fmes)2(2,2, - biquinolyl)], reveal significant structural distortions associated with steric crowding; (3) the need for boiling under reflux in the synthesis suggests a dissociative substitution mechanism, which is unknown so far for Pd; (4) some of the complexes show 19F,19F through-space couplings. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004) [source] Structural Characterization of N -Methylpyridoxine (MePN; PN = Vitamin B6) and Its Diorganotin Complexes [SnR2(MePN-H)]I (R = Me, Et, Bu and Ph)EUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 15 2003José S. Casas Abstract For comparison with the corresponding pyridoxine complexes we have prepared dimethyl-, diethyl-, dibutyl- and diphenyltin(IV) complexes of N -methylpyridoxine (MePN). The compounds [SnMe2(MePN,H)]I (1), [SnEt2(MePN,H)]I (2), [SnBu2(MePN,H)]I (3) and [SnPh2(MePN,H)]I·H2O (4) were isolated and characterized by IR, Raman, Mössbauer, 1H, 13C and 119Sn NMR spectroscopy, and by EI and FAB mass spectrometry. The crystal structures of [HMePN]I and of compounds 1, 2·2H2O and 3 were determined by X-ray diffractometry. Their lattices contain dimeric [SnR2(MePN,H)]22+ units (R = Me, Et, Bu) in which two bridging-chelating methylpyridoxinato anions link pentacoordinate Sn atoms with coordination polyhedra closer to square pyramids than to trigonal bipyramids. NMR results show that the dimeric cations persist in (CD3)2SO. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003) [source] Petrography and provenance of Laecanius Amphorae from Istria, northern Adriatic region, CroatiaGEOARCHAEOLOGY: AN INTERNATIONAL JOURNAL, Issue 5 2006Maria A. Mange Amphorae sherds from the Laecanius workshop of Roman Istria (10,5 B.C. and 78 A.D.), Croatia, were studied by integrating archaeological and geological techniques including fabric analysis, thin-section petrography, X-ray diffractometry (XRD), and heavy mineral analysis. The fabric of the sherds showed distinctive characteristics, permitting their classification and allocation into nine fabric groupss. Petrography revealed that quartz is the dominant clastic component, whereas carbonate is common as temper; XRD provided information on firing temperatures that ranged between 750 and 900°C. The sherds contain diverse heavy mineral suites with generally high epidote and garnet proportions; zircon is occasionally important. Garnet/epidote ratios and the presence of diagnostic species (pyroxene, hornblende) showed systematic variations that coincided with similar variations in fabric characteristics. Heavy mineral signatures of amphorae produced in other workshops proved essential in differentiating them from Laecanius sherds. A comparative heavy mineral analysis of terra rossa samples from the vicinity of the workshop indicated that terra rossa was the major source for the paste. Differences observed in the heavy mineral composition of the sherds and terra rossa were interpreted by the spatial heterogeneity of the latter and the mixing of the paste with sandy temper. Fresh Adriatic sponge spicules in the majority of Laecanius sherds and the temper-derived, generally immature heavy mineral assemblages suggest that sandy deposits from the Adriatic were used for the clastic temper. © 2006 Wiley Periodicals, Inc. [source] Fabrication and Optical Characteristics of Position-Controlled ZnO Nanotubes and ZnO/Zn0.8Mg0.2O Coaxial Nanotube Quantum Structure ArraysADVANCED FUNCTIONAL MATERIALS, Issue 10 2009Jinkyoung Yoo Abstract The position-controlled growth and structural and optical characteristics of ZnO nanotubes and their coaxial heterostructures are reported. To control both the shape and position of ZnO nanotubes, hole-patterned SiO2 growth-mask layers on Si(111) substrates with GaN/AlN intermediate layers using conventional lithography are prepared. ZnO nanotubes are grown only on the hole patterns at 600,°C by catalyst-free metal,organic vapor-phase epitaxy. Furthermore, the position-controlled nanotube growth method allows the fabrication of artificial arrays of ZnO-based coaxial nanotube single-quantum-well structures (SQWs) on Si substrates. In situ heteroepitaxial growth of ZnO and Zn0.8Mg0.2O layers along the circumference of the ZnO nanotube enable an artificial formation of quantum-well arrays in a designed fashion. The structural and optical characteristics of the ZnO nanotubes and SQW arrays are also investigated using synchrotron radiation X-ray diffractometry and photoluminescence and cathodoluminescence spectroscopy. [source] Synthesis and Dielectric Properties of Niobia Coating on BaTiO3INTERNATIONAL JOURNAL OF APPLIED CERAMIC TECHNOLOGY, Issue 6 2009Jia-Jia Gan Different from conventional powder mixing, this study demonstrates a method of homogeneous coating for niobia (Nb2O5) on ferroelectric barium titanate (BaTiO3) powders. The precipitation of Nb coating with pH has been determined quantitatively by the inductance-coupled plasma method. Crystalline phases were determined by X-ray diffractometry, and the formation of a "core-shell" structure with a Nb concentration gradient was observed by a transmission electron microscope with X-ray energy-dispersive spectroscopy. The dielectric constant (K) of the samples prepared by the nanocoating method showed a more stable temperature coefficient of capacitance and well satisfied the requirements of X7R. [source] Phase Transformation and Densification Behavior of Microwave-Sintered Si3N4,Y2O3,MgO,ZrO2 SystemINTERNATIONAL JOURNAL OF APPLIED CERAMIC TECHNOLOGY, Issue 1 2009Sreekumar Chockalingam A 2.45 GHz microwave-sintered Si3N4,Y2O3,MgO system containing various amounts of ZrO2 secondary additives have been studied with respect to phase transformation and densification behavior. The temperature dependent dielectric properties were measured from 25°C to 1400°C using a conventional cavity perturbation technique. Phase transformation behavior was studied using X-ray diffractometry. Microwave sintered results were compared with those of conventional sintered results. It has been found that , to , phase transformation was completed at a lower temperature in microwave-sintered samples than those of the conventionally sintered samples. Density of the microwave-sintered samples increased up to 2.5 wt% of ZrO2 addition and thereafter it showed a tendency to decrease or remain constant. The decrease in density is attributed to the pore generation caused by decomposition due to the localized over heating. [source] Determination of average carbon number of petroleum waxes by X-ray diffractionJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 5 2008Sanat Kumar Eight petroleum waxes, both paraffin as well as microcrystalline, have been analysed by X-ray diffraction. The average carbon number has been estimated by the long-range ordering observed in the diffractograms of these waxes. The average carbon number has also been determined following the standard gas chromatographic (GC) method. The results obtained by X-ray diffractometry compare well with those obtained by the GC method. The former method also permits determination of the average carbon number of high melting point waxes, which is otherwise difficult using GC. [source] Enhancement of crystalline perfection by organic dopants in ZTS, ADP and KHP crystals as investigated by high-resolution XRD and SEMJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 6 2006S. Parthiban To reveal the influence of complexing agents on crystalline perfection, tristhiourea zinc(II) sulfate (ZTS), ammonium dihydrogen phosphate (ADP) and potassium hydrogen phthalate (KHP) crystals grown by slow-evaporation solution growth technique using low concentrations (5 × 10,3M) of dopants like ethylenediamminetetraacetic acid (EDTA) and 1,10-phenanthroline (phen) were characterized by high-resolution X-ray diffractometry (XRD) and scanning electron microscopy (SEM). High-resolution diffraction curves (DCs) recorded for ZTS and ADP crystals doped with EDTA show that the specimen contains an epilayer, as observed by the additional peak in the DC, whereas undoped specimens do not have such additional peaks. On etching the surface layer, the additional peak due to the epilayer disappears and a very sharp DC is obtained, with full width at half-maximum (FWHM) of less than 10,arcsec, as expected from the plane wave dynamical theory of X-ray diffraction for an ideally perfect crystal. SEM micrographs also confirm the existence of an epilayer in doped specimens. The ZTS specimen has a layer with a rough surface morphology, having randomly oriented needles, whereas the ADP specimen contains a layer with dendric structure. In contrast to ADP and ZTS crystals, the DC of phen-doped KHP shows no additional peak, but it is quite broad (FWHM = 28,arcsec) with a high value of integrated intensity, , (area under the DC). The broadness of the DC and the high value of , indicate the formation of a mosaic layer on the surface of the crystal. However, similar to ADP and ZTS, the DC recorded after etching the surface layer of the KHP specimen shows a very sharp peak with an FWHM of 8 arcsec. An SEM photograph of phen-doped KHP shows deep cracks on the surface, confirming the mosaicity. After removing the surface layer, the SEM pictures reveal a smooth surface. A similar trend is observed with other complexing agents, like oxalic acid, bipy and picolinic acid. However, only typical examples are described in the present article where the effects were observed prominently. The investigations on ZTS, ADP and KHP crystals, employing high-resolution XRD and SEM studies, revealed that some organic dopants added to the solution during the growth lead to the formation of a surface layer, due to complexation of these dopants with the trace metal ion impurities present in the solution, which prevents the entry of impurities, including the solvent, into the crystal, thereby assisting crystal growth with high crystalline perfection. The influence of organic dopants on the second harmonic generation efficiency is also investigated. [source] Deconvolution of instrumental aberrations for synchrotron powder X-ray diffractometryJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 2 2003T. Ida A method to remove the effects of instrumental aberrations from the whole powder diffraction pattern measured with a high-resolution synchrotron powder diffractometer is presented. Two types of asymmetry in the peak profiles caused by (i) the axial-divergence aberration of the diffractometer (diffractometer aberration) and (ii) the aberration of the monochromator and focusing optics on the beamline (beamline aberration) are both taken into account. The method is based on the whole-pattern deconvolution by Fourier technique combined with the abscissa-scale transformation appropriate for each instrumental aberration. The experimental powder diffraction data of LaB6 (NIST SRM660) measured on beamline BL-4B2 at the Photon Factory in Tsukuba have been analysed by the method. The formula of the scale transformation for the diffractometer aberration has a priori been derived from the instrumental function with geometric parameters of the optics. The strongly deformed experimental peak profiles at low diffraction angles have been transformed to sharp peak profiles with less asymmetry by the deconvolution of the diffractometer aberration. The peak profiles obtained by the deconvolution of the diffractometer aberration were modelled by an asymmetric model profile function synthesized by the convolution of the extended pseudo-Voigt function and an asymmetric component function with an empirical asymmetry parameter, which were linearly dependent on the diffraction angle. Fairly symmetric peak profiles have been obtained by further deconvolution of the empirically determined asymmetric component of the beamline aberration. [source] A comparative study of single-line and Rietveld strain,size evaluation procedures using MgO ceramicsJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 2 2002Suminar Pratapa Strain,size evaluations from diffraction line broadening for MgO ceramic materials have been compared using single-line integral-breadth and Rietveld procedures with the Voigt function. Diffraction data were measured by Bragg,Brentano X-ray diffractometry (XRD), without incident beam monochromatization, and neutron diffractometry (ND) to encompass near-surface and bulk effects, respectively. The specimens consisted of sets of MgO ceramics and MgO,Y2O3 ceramic composites sintered over a range of temperatures. An MgO ceramic sintered at 1723,K for 2,h exhibited slightly less XRD broadening than the standard LaB6 NIST 660 SRM, and was therefore selected to make instrument profile corrections for both XRD and ND data. It was found for both data types that: (a) sintering initially relieves residual strain present in the MgO powder used to sinter the ceramics and also promotes grain growth; (b) residual strain of the MgO ceramic minimizes as the sintering temperature increases, and then increases with further rise in the sintering temperature, presumably as a result of intragranular interactions associated with grain growth; and (c) introduction of the second phase (Y2O3) increases strain and inhibits crystal growth. The single-line and Rietveld methods gave similar strain values from both the XRD and ND data within the limits of experimental error, but there were substantial differences between the single-line and Rietveld size estimates determined with the XRD and ND data. [source] Simultaneous determination of specimen temperature and specimen displacement in high-temperature X-ray diffractometry applying Bragg,Brentano geometryJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 1 2002M. Beck Temperature uncertainty and unknown specimen displacement are the most severe errors in high-temperature X-ray diffractometry, in particular when using a strip heater mounted on a Bragg,Brentano goniometer. A method is presented that enables the simultaneous determination of the specimen displacement and the temperature of the sample. The method splits the determination of the aberrations into two steps: at room temperature and at elevated temperature. It is based on the use of a reference material as an internal standard. An experimental example applying the method to a specific material is given, and shows that the method provides correct data. [source] Parallel-beam X-ray diffractometry using X-ray guide tubesJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 2 2000Toyoko Yamanoi A parallel-beam X-ray diffraction geometry using X-ray guide tubes is proposed to eliminate preferred-orientation effects in powder X-ray diffraction (XRD) patterns and for new applications of XRD. A bundle of X-ray guide tubes (polycapillaries) is used to provide an intense quasi-parallel (approximately 0.2° divergence) and large-diameter (approximately 20,mm) beam of X-rays needed for parallel-beam diffractometry. Mica and silicon particles were agitated inside a cylindrical chamber by a steady flow of N2 gas so that they were randomly oriented. The quasi-parallel incident X-ray beam passed through the cloud of floating particles. The diffracted X-rays were detected using a standard 2, diffractometer. The integrated intensities observed agree well with those calculated from the known model of the crystal structure. This result demonstrates that this type of diffractometry is capable of avoiding preferred-orientation effects and of collecting XRD data for moving powder samples. [source] The microencapsulation of terbinafine via in situ polymerization of melamine-formaldehyde and their application to cotton fabricJOURNAL OF APPLIED POLYMER SCIENCE, Issue 6 2010Gökhan Erkan Abstract In this study an antifungal pharmaceutical agent, terbinafine, was microencapsulated by using in situ polymerization. The polymerization was carried out at four mole ratio level and preparations were applied to the 100% cotton fabric. X-ray diffractometry, DSC, FTIR, BET, contact angle measurements, particle size distribution and imaging techniques were performed. Best results were obtained in the case of 8 : 1 mole ratio. Strength of microcapsule applied fabrics to washing and fungus were also determined. After 25 washing cycle, microcapsules were still in the fabric and had antifungal properties against A. niger. Antifungal strength against T. rubrum was observed up to 15 washing cycles. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 [source] Preparation and characterization of polyalginate,glutaraldehyde membranes,Swelling analysis by microcalorimetry and adsorption kinetics of cationic dyeJOURNAL OF APPLIED POLYMER SCIENCE, Issue 2 2010Eunice F. S. Vieira Abstract Thin crosslinked polyalginate,glutaraldehyde membranes were prepared and characterized by Fourier-transformed infrared spectroscopy, thermal analysis (TG/DTG), and X-ray diffractometry. Microcalorimetric analyses have pointed out that water swellings of the membranes are slightly exothermic, and the swelling energies decrease with increasing temperature. The membranes were tested for the adsorption of methylene blue (MB) dye from aqueous solutions. The adsorption capacity of the membranes increased with increasing initial MB concentration and decreased with increasing temperature. It was observed that the MB adsorption kinetic data were best fitted by the Avrami model. Intraparticle diffusion of MB into the interior of the membranes was detected after 60 min of contact time. The MB adsorption on the membranes was also evaluated by three new 22 full factorial designs (36 experiments). It was found that binary interactions between initial dye concentration and temperature are statistically important for MB adsorption on the membranes. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 [source] Physicochemical characterization and antioxidant activity of quercetin-loaded chitosan nanoparticlesJOURNAL OF APPLIED POLYMER SCIENCE, Issue 2 2008Yuying Zhang Abstract Quercetin is an abundant flavonoid in food plants with numerous biological activities and widely used as a potent antioxidant. Being sparingly soluble in water and subject to degradation in aqueous intestinal fluids, the absorption of quercetin is limited upon oral administration. In the present study, chitosan nanoparticles and quercetin-loaded nanoparticles were prepared based on the ionic gelation of chitosan with tripolyphosphate anions. The encapsulation of quercetin in the chitosan nanoparticles were confirmed by differential scanning calorimetry, X-ray powder diffractometry, Fourier transformed infrared spectroscopy, ultraviolet-visible spectrum, and fluorescence spectrum. The morphology of the nanoparticles was characterized by atomic force microscopy. The antioxidant activity of the quercetin-nanoparticles was also evaluated in vitro by two different methods (free radical scavenging activity test and reducing power test), which indicates that inclusion of quercetin in chitosan nanopaticles may be useful in improving the bioavailabilty of quercetin. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008 [source] Unexpected fluorescence emission of poly(,,,- L -malic acid) in aqueous mediumJOURNAL OF APPLIED POLYMER SCIENCE, Issue 3 2007Yaofeng Fan Abstract Unexpected fluorescence of poly(,,,- L -malic acid) (,,,-PMA) without traditional fluorophore was observed firstly. This fluorescent polymer was synthesized via melt polycondensation of L -malic acid. The polymer was characterized by gel permeation chromatography (GPC), nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), thermogravimetry (TG), Fourier transform infrared spectroscopy (IR), Fourier transform Raman spectroscopy (Raman), and X-ray powder diffractometry (XRD). The high molecular weight ,,,-PMA was synthesized by the optimum polycondensation at 130°C for 15 h, followed by fractional precipitation with diethyl ether and petroleum ether. The degree of branching of ,,,-PMA was from 10% to 20% according to the reaction condition. Terminal group of ,,,-PMA was mainly hydroxycarboxylic group companied with a few CHCHCOOH groups owing to dehydration of a normal terminal during the melt polycondensation. A fluorescence emission maximum of ,,,-PMA in water appeared at 420 nm when it was excited at 340 nm. Further study indicated that the fluorescence intensity was concentration-dependent, pH-dependent, and molecular-weight-dependent. The fluorescence formation may result from multichain aggregations, which was formed readily in aqueous solution due to intermolecular hydrogen bonds between branched ,,,-PMA. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007 [source] Development of flame retardancy properties of new halogen-free phosphorous doped SiO2 thin films on fabricsJOURNAL OF APPLIED POLYMER SCIENCE, Issue 6 2007Aysun Cireli Abstract In this study, flame retardancy properties of fabrics treated with phosphorous (P) doped and undoped SiO2 thin films were developed by sol,gel technique. As to this aim, P-doped and undoped SiO2 film were coated on cotton fabric from the solutions prepared from P, Si-based precursors, solvent, and chelating agent at low temperature in air using sol,gel technique. To determine solution characteristics, which affect thin film structure, turbidity, pH values, and rheological properties of the prepared solutions were measured using a turbidimeter, a pH meter, and a rheometer machines before coating process. The thermal, structural, and microstructural characterization of the coating were done using differential thermal analysis/thermograviometry, fourier transform infrared spectroscopy, X-ray diffractometry, and scanning electron microscopy. In addition, tensile strength, wash fastness, flame retandancy, and lightness properties of the coated fabrics were determined. To compensate the slight loss of tensile strength of samples, which occurred at the treated fabrics with P-doped Si-based solutions, the cotton fabrics were coated with polyurethane films during second step. In conclusion, the flame retardant cotton fabric with durability of washing as halogen-free without requiring after treatment with formaldehyde was fabricated using sol,gel processing for the first time. Moreover the cotton fabrics, which were treated with P-doped Si-based solutions and then coated with polyurethane at second step, still has got nonflammable property. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007 [source] Effect of monomer composition on crystal growth by resin containing bioglassJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 1 2010Masanori Hashimoto Abstract This study evaluated the effect of resin monomer composition on crystal growth at the interface between the resin/bioglass composites and water. Light-cured resin that contained 2-bis[4(2-hydroxy-3-methacryloyloxy-propyloxy)-phenyl], 2-hydroxyethyl methacrylate, and triethylene glycol dimethacrylate with different compositions were used. Resin/bioglass composites were prepared with 40 mass% bioglass and 60 mass% resin. The resin/bioglass composites were stored in deionized distilled water for 24 h (control group) or 3,12 months (experimental groups). After water storage, the disk surfaces were examined by light- and scanning electron microscopy. Chemical states of the crystals were analyzed by laser-Raman spectroscopy and micro-X-ray diffractometry. The microscopic analysis showed crystal on the resin disks surface after six months of water storage for hydrophilic resins. However, there was no crystal formation in the control and the experimental groups of specimens of hydrophobic resins. Raman analysis showed the chemical states of the crystals formed on the resin matrix and bioglass to be different. The micro-X-ray analysis of crystals on resin disks identified them to be calcium carbonate. This crystal formation occurred in water instead of simulated body fluid. In conclusion, the resin monomer compositions affected the ability to induce crystal growth on the surfaces of disks containing bioglass. © 2010 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2010 [source] Preparation and characterization of novel biphasic calcium phosphate powders (,-TCP/HA) derived from carbonated amorphous calcium phosphatesJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 2 2009Yanbao Li Abstract Novel biphasic calcium phosphate (BCP) powders composed of ,-tricalcium phosphate (,-TCP) and hydroxyapatite (HA) were prepared by thermal decomposition of carbonated amorphous calcium phosphates (CACP). At first, the CACP precipitates were synthesized by adding ammonium carbonate in the presence of poly(ethylene glycol) at pH 10 with an initial Ca/P molar ratio of 1.60 at 5°C. The Ca/P molar ratios of the CACP precursors are between 1.50 and 1.67 investigated by ICP. Then BCP (,-TCP/HA) powders were obtained after heating the CACP precursors at relatively low temperature (800°C) for 3 h. ,-TCP/HA powders were characterized by X-ray diffractometry, Fourier transform infrared spectra, transmission electron microscopy/scanning electron microscopy, and sedimentation experiment. The results show that ,-TCP and HA phases form in one powder, ,-TCP/HA powders are sphere with the diameter of 300 nm to less than 100 nm varied with their chemical compositions and the ratio of ,-TCP and HA in the powders can be adjusted by the adding amount of carbonates. The possible formation process of biphasic ,-TCP/HA powders was proposed. © 2008 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2009 [source] ,-Carotene-Loaded Nanostructured Lipid CarriersJOURNAL OF FOOD SCIENCE, Issue 2 2008A. Hentschel ABSTRACT:, Nanostructured lipid carriers (NLC) technology was used to disperse hydrophobic ,-carotene in an aqueous phase. NLC are lipid nanoparticles with a particle matrix consisting of a blend of a liquid and solid lipid. They were produced by melting the lipid blend at 80 °C and dispersing it into a hot emulsifier solution. The aim of this study was to extend the limited knowledge of melt-emulsified lipidic colloids in food systems and to evaluate the feasibility for further applications as functional ingredient in beverages. Physical stability of the NLC suspension was examined at 2 different storage temperatures by measuring the particle size with photon correlation spectroscopy (PCS) and laser diffractometry (LD). All particles containing sufficient amounts of emulsifier were smaller than 1 ,m (LD diameter 100%) at a mean particle size of around 0.3 ,m (LD) for 9 wk at 20 °C and at least 30 wk at 4 to 8 ° C. Differential scanning calorimetry (DSC) was used to study the solid state of the lipids both in the ,-carotene loaded PGMS and in the NLC particles. Propylene glycol monostearate (PGMS) when dispersed as NLC recrystallized up to 98% during storage time. Within the regarded period of 7 mo no polymorph transitions were observed. Furthermore, stability of the ,-carotene in water dependent on NLC concentration and tocopherol content was measured photospectrometrically to get an estimation of the behavior of NLC in beverages. [source] The Death of Countess Agusta in Portofino (Northern Italy) and the Soil from Two Mismatched SlippersJOURNAL OF FORENSIC SCIENCES, Issue 2 2009Gianni Lombardi Ph.D. Abstract:, Accident, suicide, or homicide might have caused the death of Countess Agusta who fell from the 80-m tall cliff of her villa. Two mismatched slippers were recovered along the cliff. Use was made of microscope, X-ray diffractometry, scanning electron microscopy, and microprobe techniques to compare 40 mg of soil collected from the slipper soles with samples from the villa garden. Structural details of the slipper soles were consistent with the lady wearing them during the fall. Analysis of the soil residues confirmed that they originated from the garden only. The features of a few, minute glass chips adhering to the slipper soles reasonably matched those of other fragments that were found on a small ledge on the cliff beyond the garden parapet. Based on this and other evidence, the case was closed with a verdict of accidental fall. [source] Characterization of the Triacylglycerol Crystal Formation in Adipose Tissue During a Vehicle CollisionJOURNAL OF FORENSIC SCIENCES, Issue 4 2007Barbara H. Stuart Ph.D. Abstract:, The unusual appearance of crystalline fat structures was observed during the postmortem examination of a motor vehicle accident victim. The crystal structures were characterized using Fourier transform infrared spectroscopy and x-ray diffractometry. The structures were found to be made of triacylglycerols, a dominant lipid structure found in human adipose tissue, capable of forming various polymorphic structures. The morphology of the crystalline material was found using both techniques to be predominantly the ,, form of triacylglycerols. The accelerated growth of such triacylglycerol morphology has been observed as a result of shear stresses in other studies involving edible fats. As a result of the findings of this study, it is proposed that increased shear forces may be responsible for the formation of the unusual fat structure found in the victim. An understanding of the effect of forces on the structure of body fat in high-impact collisions can potentially assist in verifying a high-velocity impact. [source] Characterization and use of acid-activated montmorillonite-illite type of clay for lead(II) removalAICHE JOURNAL, Issue 9 2010John U. Kennedy Oubagaranadin Abstract The natural local deposits of montmorillonite-illite type of clay (MIC) were susceptible for acid activation. Raw clay was taken for experimentation, disintegrated on acid activation with sulfuric acid, which showed a particle size distribution. The montmorillonite and illite phases in the raw clay disappeared on acid activation and the activated clay, MIC(AA), showed with sodium-aluminum-silicate and beidellite phases apart from quartz (low) phase. The raw and acid-activated clays were characterized using X-ray powder diffractometry, X-ray fluorescence, Fourier transform infrared spectrometry, and energy dispersive X-ray, and their adsorption capacities were compared. When tested for adsorption of Pb(II) in aqueous solutions, the acid-activated clay showed about 50% increased adsorption than raw clay. Sips adsorption isotherm and pseudo-second-order kinetic models were found to be best for the batch adsorption data. Kinetic studies showed the existence of film diffusion and intraparticle diffusion. A two-stage batch adsorber was designed for the removal of Pb(II) from aqueous solutions. © 2010 American Institute of Chemical Engineers AIChE J, 2010 [source] Influence of Ca content and oxygen partial pressure on microstructural evolution of (Co,Ca)O at elevated temperaturesJOURNAL OF MICROSCOPY, Issue 1 2006J. KUSINSKI Summary Ca-doped (1, 1.7, 5 and 10 mol% CaO) cobalt oxide single-crystal samples, with an [001] orientation, were annealed at elevated temperatures of 1000,1200 °C for different times and at different oxygen partial pressures. The microstructure was examined by means of transmission light and electron microscopy. High-temperature X-ray diffractometry was used, with the aim of determining the temperature of the CoO , Co3O4 transition in these materials. Extensive precipitation of Ca-free Co3O4 spinel crystals was observed with increasing Ca content and oxygen activity. It is suggested that the electrical conductivity changes in this material may be related to this precipitation, because it changes the electronic state of cobalt cations. [source] | |||||||||||||||||||||||||||||||||||||