Energy Dispersive X-Ray Analysis

CdTe/CdS thin £lm solar cells have been grown by closed space sublimation and high vacuum evaporation at different temperatures. After the growth, a standard CdCl 2 treatment was applied for 30 min at 430 • C. The microstructure of the cells was studied by cross-sectional transmission electron microscopy. A recrystallization after the CdCl 2 treatment was observed not only for CdTe but also for CdS. For all cells, diffusion of S into CdTe and Te in CdS were studied. The presence and distribution of Cl at the interface and at grain boundaries was also investigated. The lattice parameter as an indicator for a compositional change in the CdTe absorber layer after the CdCl 2 treatment was determined from convergent beam electron diffraction. The results were cross-checked with X-ray diffraction and compared with results obtained for a Cd 50 S 5 Te 45 polycrystal. The chemical composition at the interface of the cells was studied directly with energy dispersive X-ray spectroscopy mapping.The diffusion of S is found to depend on the extent of CdCl 2 treatment. While a diffusion of Te at the interface was not observed, segregation of Cl and Te at the CdTe/CdS interface was clearly revealed. Based on these results, a formation of a Te-Cl compound is proposed to explain the catalytic role of Cl for the CdTe/CdS recrystallization.

SnS is of interest for use as an absorber layer and the wider energy bandgap phases e.g. SnS 2 , Sn 2 S 3 and Sn/S/ O alloys of interest as Cd-free buffer layers for use in thin film solar cells. In this work thin films of tin sulphide have been thermally evaporated onto soda-lime glass substrates with the aim of optimising the properties of the material for use in superstrate configuration device structures. The thin films were characterised using energy dispersive X-ray analysis (EDS) to determine the film composition, X-ray diffraction (XRD) to determine the phases present and structure of each phase, transmittance versus wavelength measurements to determine the energy bandgap and scanning electron microscopy (SEM) to observe the surface topology and topography. These properties were then correlated to the deposition parameters. Using the optimised conditions it is possible to produce thin films of tin sulphide that are pinhole free and conformal to the substrate that are suitable for use in thin film solar cell structures.

For the first time, Germanium (Ge) nanowires have been grown on a gold (Au) coated flexible aluminum (Al) foil substrate in high vacuum (1 9 10 -5 mbar) by electron-beam evaporation of germanium using the vaporliquid-solid mechanism at a substrate temperature of 380°C. The grown nanowires have been analyzed for their structural, morphological and chemical properties by employing standard techniques X-ray diffraction, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy, respectively. X-ray diffraction measurements revealed the formation of cubic Ge phase highly oriented in (111) reflection in plane with the Al foil substrate. The morphological observations by SEM have shown the randomly grown nanowires with an average length and diameter of 600 ± 50 and 100 ± 10 nm, respectively, for a deposition time of 30 min. TEM investigation revealed single crystalline nanowires with free of defects. The wettability studies by contact angle measurement have confirmed the hydrophobic nature of the Ge NWs film surface with contact angle for water 110°± 1°. The growth mechanism of Ge nanowires on Al foil substrate has also been discussed.

AgGaS 2 (AGS) thin films were deposited onto glass substrates by sequential thermal evaporation of AgGaS 2 single crystalline powder and excess silver (Ag) interlayer. Systematic optimization to obtain single phase AgGaS 2 thin films was carried out by changing the thickness of the excess silver layer. The structure and composition of as-grown and annealed films were studied by means of X-ray diffraction and energy dispersive X-ray analysis, respectively. The optical properties of AGS thin films determined by transmittance and reflection measurements showed that they had quite high absorption coefficient with the values around 10 4 (cm −1 ). The calculated band gap values were found to be between 2.30 and 2.75 eV depending on annealing temperature. The refractive index (n) and extinction coefficient (k) of the films were determined by the envelope method. Finally, photo-electrical measurements under different illumination intensities were carried out, and different sensitizing and recombination centers were defined.

Microstructural changes in a metallic oxidation protection coating (Ni-Co-Cr-Al-Y) applied on a nickel base superalloy were investigated by means of scanning and transmission electron microscopy. The changes are due either to thermal mechanical fatigue testing under high thermal gradients or to defined isothermal heat treatments. The coated specimens were quenched from temperatures between 840 and 1100 • C to ambient temperature. The resultant phases, their local distribution and compositions were determined by energy dispersive X-ray (EDX) spectroscopy and electron diffraction. Phase equilibria at respective temperatures were determined by thermodynamic calculations based on the CALPHAD method. The calculated and experimentally determined phase distributions were compared. A particular microstructural feature, namely the existence and spatial distribution of spherical ␥ Ni 3 Al precipitates in the coating and the diffusion zone between substrate and coating, was used as a postmortem indicator for the maximum temperature experienced by the specimen during testing. This paper gives a road map for developing a microstructural-based temperature calibration for complex metallic materials using thermodynamic simulations.

Iron oxide thin films have been obtained by spray pyrolysis using 100% methanolic and ethanolic solutions of iron trichloride. The films were deposited onto ITO-coated glass substrates. The preparative conditions have been optimized to obtain compact, pin-hole-free and smooth thin films which are adherent to the substrate. The structural, morphological and compositional characterizations have been carried out by X-ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis. The films deposited using ethanolic solution results into pure hematite; a-Fe 2 O 3 thin films, however, films deposited using methanolic solution consists of hematite and maghemite-c phases of iron oxide. The films are nanocrystalline with particle size of 30-40 nm. The optical absorbance of the film was of the order of 10 5 cm À1 . The optical band gap of films was found to be 2.26 and 2.20 eV for the films deposited using methanolic and ethanolic solutions, respectively.

A system to turn a potentially harmful stream of solid waste into a set of substreams with either commercial value or highly concentrated residual streams is presented. The waste which is considered is metal impregnated (in particular Chromated Copper Arsenate (CCA) treated) wood waste and timber, such as telephone poles, railway sleepers, timber from landscape and cooling towers, wooden silos, hop-poles, cable drums and wooden playground equipment. These waste streams sum up to several 100,000 tons of material per year currently to be dumped in every major country of the European Community (EC).

Simulated spent clinoptilolite was immobilised in a monolithic glass composite wasteform (GCM) produced by a pressureless sintering for 2 hours at relative low temperatures 750 deg. C. The GCM utilises the high durability of alkali borosilicate glass to encapsulate the Cs-impregnated clinoptilolite (Cs-Clino). With this approach mobile radionuclides are retained by a multi-barrier system, comprising the crystalline form of the clinoptilolite and the borosilicate glass Wastes loading ranging from 1:1 up to 1:10 glass to Cs-clino volume ratios corresponding to 37- 88 mass % were studied. Water durability of GCM was assessed in 7, 14 and 28 days leaching tests in deionised water at 40 deg. C based on ASTM C1220-98 standard. It was found that the normalised leaching rates of Cs remaining below 6.35 10 g/cm² day in a GCM with 73 mass % waste during a leaching test for 7 days. However, at higher waste loading of {>=}80 mass %, the normalised leaching rate of Cs was as high as 9.06 10 g...

This study focused on the characterization of fouling cake layer during operation of a membrane bioreactor system employed for the treatment of synthetic hypersaline oily wastewater. Also the effects of ultrasound and addition of four types of flocculants (aluminium sulfate, Chitosan, ferric chloride, polyaluminium chloride) on mitigation of membrane fouling were studied. The components of the foulants were examined by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-ray (EDX) analysis, inductively coupled plasma (ICP) and particle size analyzer (PSA). The FTIR demonstrated that membrane fouling layer is governed by the deposition of organic and inorganic substances composed of extracellular polymeric substances (EPS) (proteins, polysaccharides, etc.), hydrocarbon components and inorganic matters. The AFM images of the fouled membrane confirmed the idea of surface coverage as a fouling mechanism. The SEM analysis showed that rod-shape bacterial clusters were one of the contributors to membrane cake layer. The EDX and ICP results showed that Mg, Al, Ca, Na, K and Fe were the major metal elements in the fouling cake. The PSA results indicate that membrane foulants had a much smaller size than mixed liquor suspensions in the MSBR. Fouling mitigation experiments showed that the effect of organic flocculant was more than inorganic chemicals but the overall effects were not significant. Ultrasound could effectively remove the fouling cake from the membrane surface and thus recovered the membrane permeation flux for a long time.

Doped and undoped nanostructured titanium dioxide was synthesized via a sol-gel method under varying conditions to determine the effects of neodymium ion doping on the titania lattice. Specifically, the effects of doping on the anatase to rutile phase transformation were studied. Samples were analyzed by a variety of techniques, including X-ray diffraction, Rutherford back-scattering spectroscopy, scanning electron microscopy, and energy dispersive X-ray spectrometry to investigate the thermodynamic and structural effects of dopant addition. Analysis of the anatase to rutile phase transformation in TiO 2 showed a maximum increase in activation energy for 0.1 mol% Nd 3+ doped TiO 2 with no further response at higher dopant concentrations. This was supported by structural analyses, which showed distortion only along the c-axis of anatase TiO 2 with a maximal distortion at 0.1 mol% Nd 3+ and no further response at higher concentration. This is due to a combination of interstitial and substitutional accommodation of the dopant ions.

Soils from many industrial sites in southeastern USA are contaminated with As because of the application of herbicide containing As2O3. Among those contaminated sites, two industrial sites, FW and BH, which are currently active and of most serious environmental concerns, were selected to characterize the occurrence of As in the contaminated soils and to evaluate its environmental leachability. The soils are both sandy loams with varying mineralogical and organic matter contents. Microwave-assisted acid digestion (EPA method 3051) of the contaminated soils indicated As levels of up to 325 mg/kg and 900 mg/kg (dry weight basis) for FW and BH soils, respectively. However, bulk X-ray powder diffraction (XRD) analysis failed to find any detectable As-bearing phases in either of the studied soil samples. Most of the soil As was observed by scanning electron microscopy, coupled with energy dispersive X-ray spectroscopy (SEM/EDX), to be disseminated on the surfaces of fine-grained soil particles in close association with Al and Fe. A few As-bearing particles were detected in BH soil using electron microprobe analysis (EMPA). Synchrotron micro-XRD and X-ray absorption near-edge structure (XANES) analyses indicated that these As-rich particles were possibly phaunouxite, a mineral similar to calcium arsenate, which could have been formed by natural weathering after the application of As2O3. However, the scarcity of those particles eliminated them from playing any important role in Assequestration.Synthetic acid rain sequential batch leaching experiments showed distinct As leaching behaviors of the two studied soil samples: BH soil, which has the higher As content, showed a slow, steady release of As, while FW soil, with a lower As content, showed a much quicker release and lower overall retention of As upon leaching. Sequential chemical extraction experiments were carried out using a simplified 4-step sequential chemical extraction procedure (SCEP) previously developed to characterize the fractionation of As and better understand the different leaching behaviors of the two studied soils. It was shown that only about 50 percent of the total extractable As was removed by the first two extraction steps, which represented the most weakly bonded and readily available As for environmental leaching. Compared with eScholarship provides open access, scholarly publishing services to the University of California and delivers a dynamic research platform to scholars worldwide. the sequential leaching experiments, it was further indicated that only half of the As associated with phases extracted by the second SCEP step was mobilized by SPLP leaching. Although microwave-assisted acid digestion results showed similar Al and Fe contents in both soils, the sequential chemical extraction experiments indicated that BH soil has a much higher content of amorphous Al and Fe phases and that a comparably higher portion of soil As was associated with those materials. The experimental results suggest that remediation efforts for the contaminated sites can be directed towards enhancing the formation of more stable As-bearing compounds in the soils to reduce the environmental leachability of As.

The beneficial effect of vegetation on particle deposition is often stated in arboricultural literature but has rarely been researched in detail. To quantify these filtering effects of faç ade greening, it is necessary to study the accumulation properties of leaf surfaces on particle adsorption. In this paper attention will be given to a measure technique for particle adsorption on vegetation. The presented preliminary study aims to classify the total amount of particles by counting of particles on ESEM photographs. In the PhD research more attention will be given on the relation between particle reduction and the effect of vegetation on air quality improvements. Two locations were investigated, namely: leaves from near a traffic road and from a woodland. A difference in the particle amount was found at the underside and upper side of the leaves. For example, in a sampling at early autumn for the road location roughly 7000 particles (per 1275 × 950 m) were counted for the upper side, and, roughly 3200 particles for the underside. Also a difference in particle amount was found between the two different locations, respectively roughly 7000 particles for the upper side of the leaf at the road location and roughly 3300 for the woodland location. The comparison must give more insight into the sink capacity of vegetation, but also between the environments. In the paper, results of counting particles on leaves from both locations are provided via a factorial design approach with four independent factors at two levels (height, leaf, time and environment). The outcome of the factorial design shows that there is a difference between the collecting capacity of the leaf (upper side/underside) and between the environments (road/woodland). Fine and ultra-fine particles (i.e., the fractions that are potentially the most harmful to human health) were more abundantly found on the leaves than coarser particles. Also some energy dispersive X-ray analysis (EDS) of the adhered particles is provided. As the main conclusion of this research, it can be said that counting particles instead of weighing particles on a specific leaf area seems to be a proper way to classify aerosol deposition on vegetation.

The research presented in this paper is focused on the effect of silicon carbide (SiC) on friction-wear properties of semi-metallic friction composites (FC). Semi-metallic FC with increasing content of silicon carbide (SiC: 0, 3.4, 5.6, 9 and 14.6 vol.%) were prepared and slid against cast iron disc and their friction-wear properties were evaluated. The friction coefficient ( ) was observed to increase with SiC content, nonetheless the highest content (14.6 vol.% of SiC) did not significantly increase its value. The volume wear rate (V) of tested friction composites slightly increases with SiC content and temperature. The character of friction layer was analyzed using scanning electron microscopy (SEM) with energy dispersive X-ray microanalysis (EDX) and the topography of friction surface was studied using atomic force microscopy (AFM). Two types of films assigned as film I and film II appearing on the friction surfaces of samples after friction test were observed. Film I originate on the friction surface of sample without SiC and is composed of debris of iron, iron oxide, stibnite and carbon. Film II is formed on the friction surface of composites containing SiC and in contrast to film I contain additional debris of SiC.

In the present study, EPS secreted by the endophytic bacterium Bacillus licheniformis was isolated and characterized. The molecular masses of the EPS were 1540 and 44,565 kDa and 1 H NMR, FT-IR and UV-Vis spectral analyses revealed prevalence of characteristic primary amine-group, aromatic-compound, halide and aliphatic alkyl-group in addition to Na, P, Ca, C, O, Cl and S as inferred from EDX analysis. XRD and DSC analysis confirmed the amorphous nature of EPS, showing an average particle size of 24.977 m (d 0.5) with 191 nm average roughness. The positive ion reflector mode of MALDI TOF-TOF MS exhibited a series of low and high mass peaks corresponding to various oligosaccharides and polysaccharides respectively. Further, GC-MS analysis revealed its four monosaccharide constituents glucose, galactose, mannose and arabinose. The potential heterogeneous properties of EPS as revealed in the present study may be explored in various biotechnological and industrial applications.

In view of the wide interest in high refractive index polymers for microreplication, study was made of UV-curable high refractive index nanocomposite material for microreplication purposes. The refractive index of the nanocomposite was tailored through the addition of surface-modified ZnS nanoparticles to commercial ORMOCOMP Ò inorganic-organic hybrid polymer. The refractive index of ORMOCOMP Ò was increased linearly from 1.514 (620 nm) to 1.645 (620 nm) by embedding of the nanoparticles (18.6 V%). The nanocomposite showed excellent transparency (T = 89-92%), and increase in the nanoparticle loading shifted the absorption edge from 380 nm to 420 nm. Low scattering of transmitted light (determined by UV-VIS-NIR spectrophotometry) and high dispersion of ZnS (determined by scanning electron microscopy with energy dispersive X-ray spectrometry and transmission electron microscopy) indicated low aggregation of the ZnS nanoparticles. Finally, the nanocomposite was applied to micromolding in capillaries to replicate micrometer-size channels (8 lm  1.5 lm) with Bragg gratings (period 520 nm and depth 400 nm) on top of the channels. Based on the AFM results the MIMIC molding method was found to be suitable for the replication of microchannels into nanocomposite material.

In the present work microwave cladding was explored as a new processing method for enhancement of surface properties of austenitic stainless steel (SS-316). Cladding of nickel based powder (EWAC) was developed using microwave radiation as the heating source. This paper explains the possible mechanism of clad formation using microwave hybrid heating with the help of a schematic model. The developed clads were characterized using field emission scanning electron microscope (FE-SEM), energy dispersive X-ray spectroscope (EDS), X-ray diffraction (XRD) and measurement of Vicker's microhardness. Typical X-ray diffraction (XRD) pattern of the clad showed the presence of chromium carbide, nickel silicide and nickel iron phases that eventually contribute to enhancement in microhardness of the clads. Clads of approximately 1 mm thickness were developed without any visible interfacial cracking and had significantly less porosity (1.09%). Microstructure of clad transverse section revealed good metallurgical bond with SS-316 substrate by partial mutual diffusion of constituent elements. The microstructure of the clad was found dominantly cellular in nature. Chromium was observed segregated around the cell boundaries while iron and nickel were identified inside the cells. Chromium carbides (Cr 23 C 6 , Cr 3 C 2) were formed during the processing and appeared at the cell boundaries. Vicker's microhardness study revealed that the hardness profile varies within the clad zone and the average microhardness of the developed clad was observed to be 304 ± 48 H v .

Experimental studies on preparation of thin films of ternary compositions of Mn 3 O 4 , NiO and CoO using ion beam sputtering technique and electrical properties characterization have been carried out. The compatibility of thin films deposited on thermally grown silicon oxide on Si wafer of <1 0 0> orientation to produce thin film thermistors on a thermal isolation structure (TIS) by wet chemical micro-machining process has also been investigated. It is observed from energy dispersive X-ray (EDAX) analysis that the chemical compositions of thin films have close proximity to the target composition, with minor deviations in the individual oxide contents. While the films whose manganese oxide content is higher and nickel oxide lower, have higher thermistor constant 3600 K, and sheet resistance 4×10 7 /sq, the films which have lower manganese oxide and higher nickel oxide are found to have medium thermistor constant 2186 K, and lower sheet resistance 5×10 5 /sq. The micro-machined TIS, analyzed by scanning electron microscope, is observed to have an isolated bridge structure. The voltage-current relationship of the sensor element deposited on the TIS is linear up to an applied bias of 10 V, and the thermal conductivity and the thermal mass of the entire bridge structure are respectively 2.6×10 −6 W K −1 and 1.3 × 10 −9 J K −1 . The responsivity, and detectivity of the infrared detector fabricated, using thin film thermistor sensor deposited on a micro-machined TIS together with a suitable infrared absorber coating, are respectively equal to 3000 V W −1 and 4.4×10 8 cm Hz 1/2 W −1 at 10 Hz operating frequency, and the time constant is 0.53 ms.

An investigation undertaken on the Al-Ni-Re system using optical microscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction revealed that the largest liquidus surface was due to (Re). The Al Re composition was shown to be 5 24 the limit of solubility of (Re). No exclusively new ternary phases were found, and the solubilities of the binary phases were limited. Al Re and Al Re had solubilities of up to |5 at. % Ni, AlNi up to |2 at. % Re (maximum), and AlRe up to 2 at. % Ni. The AlNi , 3 6 2 3 Al Ni , Al Ni, Al Re and Al Re phases had negligible solubility, and Al Re was not observed. Eleven ternary invariant reactions were 3 2 3 2 3 4 12

The amorphous precursors of the ZrO 2 -CuO system at the ZrO 2 -rich side of the concentration range were prepared by co-precipitation from aqueous solutions of the corresponding salts. Thermal behavior of the amorphous precursors was monitored using X-ray powder diffraction, Raman spectroscopy, field emission scanning electron microscopy, energy dispersive X-ray spectrometry, differential scanning calorimetry and thermogravimetric analysis. The crystallization temperature of the amorphous precursors rose with an increase in the CuO content for ∼180 • C. Maximum solubility of Cu 2+ ions in the ZrO 2 lattice (∼23 mol%) occurs in the metastable products obtained upon crystallization of the amorphous precursors. The results of Raman spectroscopy indicate that the incorporation of Cu 2+ ions stabilize the tetragonal ZrO 2 polymorph. A precise determination of lattice parameters, using both Rietveld and Le Bail refinements of the powder diffraction patterns, showed that the axial ratio c/a in the ZrO 2 -type solid solutions with a Cu 2+ content ≥20 mol% approach 1 (formation of t -form of tetragonal phase). The terminal solid solubility limit of Cu 2+ ions in the ZrO 2 lattice rapidly drops with an increase in treatment temperature (up to 1000 • C) that is followed by the formation of and increase in phases structurally closely related to tenorite and monoclinic ZrO 2 . Low thermal stability of the t-ZrO 2 -type phase was attributed to the reduction of the sintering temperature in the presence of CuO and a significant difference in size and shape of zirconia and tenorite particles, which prevent surface interactions.

Cyclic voltammetry of the CuCl powder in a cavity microelectrode revealed direct electro-reduction in solid state in 1-butyl-3-methylimidazolium hexafluorophosphate. Potentiostatic electrolysis of the salt powder (attached to a current collector) in the ionic liquid produced Cu ...

mation is accompanied by a large increase in electrical conductivity; the low-temperature phase is a protonic con-Potassium hydrogen fluoride (KHF 2 ) crystallizes in the tetragonal system, space group I4/mcm, Z ‫؍‬ 4, a ‫؍‬ 5.668(2) Å , ductor, whereas Kϩ, F-, and [FHF]-groups are all very c ‫؍‬ 6.801(7) Å , under ambient conditions. Energy-dispersive mobile in the cubic phase (3-5). A high-pressure conduc-X-ray diffraction was used to study the compression behavior tivity study by Bradley et al. (6) traced the tetragonal-cubic of KHF 2 in a diamond anvil cell. Unit cell parameters were transition up to 5.7 GPa, where it occurred at 245ЊC. The determined at ten different static pressures between 1 atm and near-isothermal slope in P-T space for this transition is a 12.3 GPa, and the calculated cell volumes were found to fit consequence of the large entropy increase on formation a third-order Birch-Murnaghan equation of state with K 0 ‫؍‬ of the cubic phase (23.8 J/mol K; 7, 8) despite the large 25.1(15) GPa and K ‫؍‬ 10.0(19). The compressibility is greatest volume increase (ϩ12.7% at 1 bar). There is a possibility by a factor of two parallel to z despite the short K-K distances of ordered pyrite-like KHF 2 being stable at high pressure in this direction, implying that F-F repulsion controls the comand lower temperatures than the disordered structure or pressibility behavior. A reconnaissance study to much higher the tetragonal phase. Orientational ordering causes a 13% pressure showed that KHF 2 remains in this structure down to volume decrease in NaSH (9). Such a volume change com-67.6% of its ambient volume, at a pressure estimated as 50 bined with loss of configurational entropy might be suffi-

Polycrystalline AgGaSe 2 thin films were deposited by using single crystalline powder of AgGaSe 2 grown by vertical Bridgman-Stockbarger technique. Post-annealing effect on the structural and morphological properties of the deposited films were studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDXA) measurements. XRD analysis showed that as-grown films were in amorphous structure, whereas annealing between 300 and 600 8C resulted in polycrystalline structure. At low annealing temperature, they were composed of Ag, Ga 2 Se 3 , GaSe, and AgGaSe 2 phases but with increasing annealing temperature AgGaSe 2 was becoming the dominant phase. In the as-grown form, the film surface had large agglomerations of Ag as determined by EDXA analysis and they disappeared because of the triggered segregation of constituent elements with increasing annealing temperature. Detail analyses of chemical composition and bonding nature of the films were carried out by XPS survey. The phases of AgO, Ag, Ag 2 Se, AgGaSe 2 , Ga, Ga 2 O 3 , Ga 2 Se 3 , Se and SeO 2 were identified at the surface (or near the surface) of AgGaSe 2 thin films depending on the annealing temperature, and considerable changes in the phases were observed. ß

This study focuses on structural and photocatalytic degradation of olive mill wastewater (OMW) of TiO 2 supported sepiolite catalysts, prepared by a sol-gel method in aqueous solution. To get the TiO 2 /Sep nanoparticle, the nanocrystalline TiO 2 anatase phase on sepiolite was obtained using a sufficient thermal treatment by gradually increasing the temperature from 300, 400 and 500 • C with 1 h intervals for a total of 3 h. Then, the structural features of TiO 2 /Sep materials were investigated by using different spectral and technical structural analyses with scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray (EDX) analysis, Fourier transform infrared (FTIR), thermal gravimetric analysis (TGA), XRF and X-ray diffraction (XRD). The photocatalytic degradation of TiO 2 /Sep materials has been investigated in OMW by using ultraviolet (UV), hydrogen peroxide (H 2 O 2 ) and TiO 2 /Sep nanoparticles together. The influence of pH, catalyst amount and temperature was investigated in all the experiments and the degradation ratios were found to be strongly influenced by all investigated parameters. The photocatalytic degradation of lignin and phenol was favorable at pH 9-11.0. Optimum values of catalyst dose and temperature were found to be 0.25 and 0.50 g L −1 and 318 K, respectively. In addition, the pseudo-first order model was applied and r 2 values were noted from 0.90 to 0.99.

The structural characteristics of Ba-Fe double hydroxides were studied by various methods, such as scanning electron microscopy (SEM), energy dispersive X-ray (EDX) fluorescence and X-ray absorption spectroscopies (XAS). It was verified that under hyperalkaline conditions (using 10 M or 20 M NaOH solution for precipitating the substances) layered double hydroxides could be prepared and the structure collapsed on heat treatment at 523 K. Important structural parameters could also be obtained through the quantitative analysis of the XAS spectrum of Ba 3 Fe-LDH made using 20 M NaOH for precipitating the material.

A consolidating product based on nanoparticles of slaked lime (Ca(OH)2) dispersed in isopropyl alcohol was exposed under different relative humidities (RH), 33%, 54%, 75% and 90% during 7, 14, 21 and 28 days. The characterization of the calcium hydroxide nanoparticles and the formed calcium carbonate polymorphs have been performed by Micro Raman spectroscopy, Transmission Electron Microscopy (TEM), Environmental Scanning Electron Microscopy (ESEM) with Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Diffraction (XRD). Precipitation and transformation of calcium carbonate polymorphs strongly depend on the relative humidity (RH). Higher RH (75%–90% RH) gives rise to amorphous calcium carbonate and monohydrocalcite, calcite, aragonite and vaterite, faster carbonation and larger particles sizes with higher crystallinity compared to lower RH (33%–54% RH) that gives rise mainly to portlandite and vaterite, slower carbonation and smaller particle sizes with lower crystallinity.Ca(OH)2 nanoparticles dispersed in isopropyl alcohol exposed under different relative humidities (RH) 7, 14, 21 and 28 days. Higher RH (75%–90% RH): faster carbonation (amorphous CaCO3, CaCO3·H2O, calcite, aragonite and vaterite) and larger particles sizes with higher crystallinity. Lower RH (33%–54% RH): mainly portlandite (Ca(OH)2) and vaterite with smaller particle sizes and lower crystallinity.

Thermal barrier coating system comprised of 8 wt.% yttria stabilized zirconia (YSZ) top coat, glass-ceramic bond coat and nimonic alloy (AE 435) substrate was subjected to thermal shock test from 1000 8C to room temperature for 100 cycles. Two types of thermal shock testing were performed. In one test, specimens held at 1000 8C for 5 min were forced air quenched while in the other test specimens were water quenched from the same conditions. Microstructural changes were investigated by scanning electron microscopy (SEM) and phase analysis was conducted by XRD and energy dispersive X-ray (EDX) analysis. In the case of forced air quenched specimens, no deterioration was observed in the top coats after 100 cycles while the top coats were damaged in the water quenched ones. In both forced air quenched and water quenched specimens, interfacial crack was not observed at the top coat-bond coat and bond coat-substrate interfaces after thermal cycling experiments and the top coat maintained its phase stability. #

Effects of 2-amino-5-ethylthio-1,3,4-thiadiazole (AETD) on copper corrosion as a corrosion inhibitor in an aerated acidic pickling solution of 0.50 M HCl have been investigated using gravimetric and electrochemical techniques. Weight losses of copper coupons in 0.50 M HCl measured after varied exposure periods of 2-12 h indicate that the addition of AETD significantly decreases the dissolution rate and the effect increases upon increasing its concentration. Results of potentiodynamic polarization experiments show a large decrease in cathodic, anodic, and corrosion currents due to the presence of the organic molecules. Potentiostatic current-time measurements at 200 mV versus Ag/AgCl for 120 min, scanning electron microscope (SEM), and energy dispersive X-ray (EDX) investigations also indicate that AETD greatly lowers the dissolution currents as a result of its strong adsorption onto the copper surface preventing it from being corroded easily. EIS measurements confirmed that the charge transfer resistance increases and mass transport decreases in the presence of AETD upon increasing its concentration.

Single crystals of uranium intermetallic compound UCo 0:5 Sb 2 were grown by means of the antimony-flux technique. The characterization of the samples has been carried out utilizing single crystal X-ray diffraction and magnetization measurements. UCo 0:5 Sb 2 is found to crystallize in the tetragonal HfCuSi 2-type structure, space group P4=nmm with Z ¼ 2 formula units per cell, and the lattice parameters a ¼ 0:4300ð1Þ and c ¼ 0:8958ð2Þ nm: The refinement of the occupancy parameters and the energy dispersive X-ray analysis have indicated a distinct deficiency on the cobalt sites. The results of magnetization measurements showed that UCo 0:5 Sb 2 orders ferromagnetically below 65 K with a huge magnetocrystalline anisotropy with the c direction being the easy magnetization axis.

Cu 2 O nanopowders have been prepared by ultrasound-assisted electrochemistry with a potentiostatic set-up. Their composition has been determined by X-ray diffraction and energy dispersive X-ray spectroscopy. Transmission electron microscopy and centrifugation analyses indicate that the nanopowders consist of agglomerates of variable nanometric diameter grain. Most of particles have a diameter of 8 nm whatever the electrodeposition potential. The influence of the parameters of electrochemical and ultrasonic pulses on the particle diameter was also studied. The specific surface areas determined by Brunauer-Emmet-Teller (BET) model are very high with a value close to 2000 m 2 g À1 .

We studied the copper corrosion and product layers originating in a simulated uterine solution at pH values 6.3 and 8.0 for 15, 65, 180, and 360 days at 37°C. Absorbance measurements were performed. Corrosion product layers on the copper surface were characterized by scanning electron microscopy, energy dispersive x-ray, and x-ray photo-electron spectroscopy techniques. Copper release for pH 6.3 and 8.0 was 3.4 -4.5 g/day for 15 days and 0.1-0.3 g/day for 360 days. Of the order of 30%-40% of dissolved cupric ions were trapped in the product layers. The main compounds identified were cuprite (Cu 2 O), calcite (CaCO 3 ), and phosphates. CONTRACEPTION 2000;61: 395-399

Isotropic and anisotropic nanocrystalline Nd 14 Fe 80 B 6 and Nd 12 Dy 2 Fe 73.2 Co 6.6 Ga 0.6 B 5.6 magnets have been produced from melt-spun materials by hot pressing and subsequent die-upsetting. The microstructure has been characterized using XRD, scanning electron microscope and energy dispersive X-ray analysis. The corrosion behaviour of die-upset NdFeB-based magnets has been studied in 0.1 M H 2 SO 4 by inductively coupled plasma solution analysis and electrochemical polarization techniques and compared with their hot-pressed counterparts. Texturing of hot-pressed (isotropic) NdFeB-based magnets via die-upsetting significantly modifies their corrosion performance. Textured Nd 12 Dy 2 Fe 73.2 Co 6.6 Ga 0.6 B 5.6 magnets exhibit the highest corrosion resistance in this study. The low effective diffusivity of corrosion hydrogen inside the bulk magnet and the reduction in the strength of galvanic coupling between magnet phases are the main reasons for the observed improvement in the corrosion resistance. The corrosion behaviour of the magnets in relation to their phase composition and phase distribution is discussed in terms of dissolution, hydrogenation and pulverization. Pulverization trends are correlated with hydrides formation and hydrogen-trapping sites using thermal desorption analysis. r

This work applies established analytical techniques of physical sciences to Irish brick in order to gather evidence of ceramic technologies, provenance and sources of raw materials. Petrographic microscopy, X-ray diffractometry and scanning electron microscopy with an energy dispersive Xray diffraction attachment were used to study the brick of Rathfarham Castle, Dublin, built c.1618, where clay brick was introduced in 1771. Local clay was fired in the laboratory and analysed in a similar manner. The petrography of the pointing mortar was studied in order to gather evidence of ceramic provenance. This paper concludes that the brick was hand-moulded with a silica-based, predominantly non-calcareous clay of glacial origin gathered locally, including fluxes and a high percentage of non-plastic material. The mineralogy and petrography of the brick together with the presence of pebbles and a coarse-matrix suggest that the raw clay was probably gathered from a glacial deposit. The presence of abundant pebbles and colour inhomogeneities suggests a lack of processing of the raw clay. The brick was probably fired in clamps at top firing temperatures of 750 to above 900 ºC. Transformation of limestone temper involving breakdown of calcite and generation of calcium silicates, new-formation of plagioclase, high-temperature quartz, hematite and spinel were evidenced. The presence of spinel in 'hot spots' indicates that fuel was added to the raw clay in order to assist firing.

Reactively sputtered Mo 2 N/MoS 2 /Ag nanocomposite coatings were deposited from three individual Mo, MoS 2 , and Ag targets in a nitrogen environment onto Si (111), 440C grade stainless steel, and inconel 600 substrates. The power to the Mo target was kept constant, while power to the MoS 2 and Ag targets was varied to obtain different coating compositions. The coatings consisted of Mo 2 N, with silver and/or sulfur additions of up to approximately 24 at%. Coating chemistry and crystal structure were evaluated using X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD), which showed the presence of tetragonal Mo 2 N and cubic Ag phases. The MoS 2 phase was detected from XPS analysis and was likely present as an amorphous inclusion based on the absence of characteristic XRD peaks. The tribological properties of the coatings were investigated in dry sliding at room temperature against Si 3 N 4 , 440C stainless steel, and Al 2 O 3 . Tribological testing was also conducted at 350 and 600°C against Si 3 N 4 . The coatings and respective wear tracks were examined using scanning electron microscopy (SEM), optical microscopy, profilometry, energy dispersive X-ray spectroscopy (EDX), and micro-Raman spectroscopy. During room temperature tests, the coefficients of friction (CoF) were relatively high (0.5-1.0) for all coating compositions, and particularly high against Si 3 N 4 counterfaces. During high-temperature tests, the CoF of single-phase Mo 2 N coatings remained high, but much lower CoFs were observed for composite coatings with both Ag and S additions. CoF values were maintained as low as 0.1 over 10,000 cycles for samples with Ag content in excess of 16 at% and with sulfur content in the 5-14 at% range. The chemistry and phase analysis of coating contact surfaces showed temperature-adaptive behavior with the formation of metallic silver at 350°C and silver molybdate compounds at 600°C tests. These adaptive Mo 2 N/MoS 2 /Ag coatings exhibited wear rates that were two orders of magnitude lower compared to Mo 2 N and Mo 2 N/Ag coatings, hence providing a high potential for lubrication and wear prevention of hightemperature sliding contacts.

Phosphomolybdate nanorods were synthesized using dodecyl pyridinium cations as structure directing agent. Composition and morphology of the nanorods were established by powder X-ray diffraction, energy dispersive X-ray analysis, fourier transform infrared spectroscopy, thermogravimetric analysis, transmission electron microscopy and scanning electron microscopy. Effect of synthetic variables such as pH and nature of templating agent on structure and morphology of the nanorods under ambient condition is discussed.

The potential toxicity of stannum dioxide (SnO 2 ), cerium dioxide (CeO 2 ) and iron oxide (Fe 3 O 4 ) nanoparticles (NPs) in the marine environment was investigated using the sea urchin, Paracentrotus lividus, as an in vivo model. We found that 5 days after force-feeding of NPs in aqueous solutions, the three NPs presented different toxicity degrees, depending on the considered biomarkers. We examined: 1) the presence of the NPs in the coelomic fluid and the uptake into the immune cells (coelomocytes); 2) the cholinesterase activity and the expression of the stress-related proteins HSC70 and GRP78; 3) the morphological changes affecting cellular compartments, such as the endoplasmic reticulum (ER) and lysosomes. By Environmental Scanning Electron Microscope (ESEM) analysis, coupled with Energy Dispersive X-ray Spectroscopy (EDS) we found that NPs were uptaken inside coelomocytes. The cholinesterases activity, a well known marker of blood intoxication in vertebrates, was greatly reduced in specimens exposed to NPs. We found that levels of stress proteins were down-regulated, matching the observed ER and lysosomes morphological alterations. In conclusion, this is the first study which utilizes the sea urchin as a model organism for biomonitoring the biological impact of NPs and supports the efficacy of the selected biomarkers.

The development of production processes that can reduce the environmental impact, offer waste reduction and increase energy efficiency is an important step in the field of application of nanotechnology. In this work the filamentous fungus Neurospora crassa was screened and found to be successful for the production of mono and bimetallic Au/Ag nanoparticles (NPs). Analysis by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM) confirmed the biosynthesis of NPs by the fungus. The shape of NPs was found to be mainly spherical with average diameter of 11 nm for silver and 32 nm for gold, when the fungus was exposed to the aqueous solutions of 10 −3 M of AgNO 3 and HAuCl 4 , respectively. EDS analysis also confirmed the formation of alloy-type Au/Ag bimetallic NPs when three different ratios of AgNO 3 /HAuCl 4 were used. TEM images of thin sections of N. crassa cells confirmed the intracellular formation of silver and gold NPs. The results obtained indicate that N. crassa can be a potential "nanofactory" for the synthesis of metallic NPs. The use of this organism will offer several advantages since it is considered as a non-pathogenic organism, has a fast growth rate, rapid capacity of metallic ions reduction, NPs stabilization and facile and economical biomass handling.

Sn-Bi alloys were electroplated from sulphuric acid based plating baths containing tin sulfate (SnSO4) and bismuth nitrate (Bi(NO 3)3). The electrochemical behavior of the plating bath was investigated by electrochemical studies. Potentiodynamic polarization curves of the plating bath revealed the large potential gap between the two elements. The effects of SnSO4 concentration and current density on the composition and morphology of the Sn-Bi electrodeposition were investigated. The surface morphology and composition of the Sn-Bi electrodeposited were investigated by scanning electron microscopic (SEM) coupled with energy dispersive X-ray (EDS) spectroscopic. The Sn content in the deposits increased with increasing of Sn content in the bath. Bi content was found to decrease with increasing current density because of the more noble deposition potential of Bi. The microstructure and surface morphology of the Sn-Bi electrodeposits become finer and smoother with increasing Sn content in bath but rougher and less compact when current density is increased. Sn-36.47 wt.% Bi alloy was fabricated from this additive free plating bath.

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Ba 1Àx Sr x TiO 3 solid solutions were prepared by solid-state reaction from raw materials. Four compositions with x ¼ 0.25, 0.50, 0.75 and 0.90 have been investigated. The perovskite type and polycrystalline structure of the BST samples were revealed by X-ray diffraction data. The morphology, grain size distribution, porous structure and elemental composition of the sintered ceramics were analyzed by using scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) microanalysis. The temperature dependence of permittivity and of dielectric loss tangent at low frequency (1 kHz) showed decrease of Curie temperature with increase of Sr content. Microwave measurements (1 GHz) showed substantial decrease of the dielectric constant from about 1600 to 200 and also of the losses from 12% to less than 2% with the Sr concentration increase from x ¼ 0.25 to x ¼ 0.90. Moreover, the addition of MgO and MnO 2 1 wt.% each, improved sintering process and lowered the microwave losses up to 0.2%.