Search results for: in-situ synchrotron X-ray diffraction

Authors: A. Fernandez Zuvich, I. Gana Watkins, H. Zolotucho, H. Troiani, A. Caneiro, M. Prado, A. L. Soldati

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The study of actinide nanoparticles (NPs) has attracted the attention of the scientific community not only because the lack of information about their ecotoxicological effects but also because the use of NPs could open a new way in the production of nuclear energy. Indeed, it was recently demonstrated that UO2 NPs sintered pellets exhibit closed porosity with improved fission gas retention and radiation-tolerance , ameliorated mechanical properties, and less detriment of the thermal conductivity upon use, making them an interesting option for new nuclear fuels. In this work, we used a combination of diffraction and microscopy tools to characterize the morphology, the crystalline structure and the composition of UO2 nanoparticles doped with 10%wt Gd2O3. The particles were synthesized by a modified sol-gel method at low temperatures. X-ray Diffraction (XRD) studies determined the presence of a unique phase with the cubic structure and Fm3m spatial group, supporting that Gd atoms substitute U atoms in the fluorite structure of UO2. In addition, Field Emission Gun Scanning (FEG-SEM) and Transmission (FEG-TEM) Electron Microscopy images revealed the presence of micrometric agglomerates of nanoparticles, with rounded morphology and an average crystallite size < 50 nm. Energy Dispersive Spectroscopy (EDS) coupled to TEM determined the presence of Gd in all the analyzed crystallites. Besides, FEG-SEM-EDS showed a homogeneous concentration distribution at the micrometer scale indicating that the small size of the crystallites compensates the variation in composition by averaging a large number of crystallites. These techniques, as combined tools resulted thus essential to find out details of morphology and composition distribution at the sub-micrometer scale, and set a standard for developing and analyzing nanoparticulated nuclear fuels.

Keywords: actinide nanoparticles, burnable poison, nuclear fuel, sol-gel

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Authors: N. Boudinar, A. Djekoun, A. Otmani, B. Bouzabata, J. M. Greneche

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High-energy ball milling is a solid-state powder processing technique that allows synthesizing a variety of equilibrium and non-equilibrium alloy phases starting from elemental powders. The advantage of this process technology is that the powder can be produced in large quantities and the processing parameters can be easily controlled, thus it is a suitable method for commercial applications. It can also be used to produce amorphous and nanocrystalline materials in commercially relevant amounts and is also amenable to the production of a variety of alloy compositions. Mechanical alloying (high-energy ball milling) provides an inter-dispersion of elements through a repeated cold welding and fracture of free powder particles; the grain size decreases to nano metric scale and the element mix together. Progressively, the concentration gradients disappear and eventually the elements are mixed at the atomic scale. The end products depend on many parameters such as the milling conditions and the thermodynamic properties of the milled system. Here, the mechanical alloying technique has been used to prepare nano crystalline Fe_50 and Fe_64 wt.% Ni alloys from powder mixtures. Scanning electron microscopy (SEM) with energy-dispersive, X-ray analyses and Mössbauer spectroscopy were used to study the mixing at nanometric scale. The Mössbauer Spectroscopy confirmed the ferromagnetic ordering and was use to calculate the distribution of hyperfin field. The Mössbauer spectrum for both alloys shows the existence of a ferromagnetic phase attributed to γ-Fe-Ni solid solution.

Keywords: nanocrystalline, mechanical alloying, X-ray diffraction, Mössbauer spectroscopy, phase transformations

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Authors: Arturo Reyes Roman, Daniza Castillo Godoy, Francisca Balarezo Olivares, Francisco Arriagada Castro, Miguel Maulen Tapia

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Mining waste–based geopolymers are a sustainable alternative to conventional cement materials due to their contribution to the valorization of mining wastes as well as to the new construction materials with reduced fingerprints. The objective of this study was to determine the potential of leaching gravel (LG) from hydrometallurgical copper processing to be used as a raw material in the manufacture of geopolymer. NaOH, Na2SiO3 (modulus 1.5), and LG were mixed and then wetted with an appropriate amount of tap water, then stirred until a homogenous paste was obtained. A liquid/solid ratio of 0.3 was used for preparing mixtures. The paste was then cast in cubic moulds of 50 mm for the determination of compressive strengths. The samples were left to dry for 24h at room temperature, then unmoulded before analysis after 28 days of curing time. The compressive test was conducted in a compression machine (15/300 kN). According to the laser diffraction spectroscopy (LDS) analysis, 90% of LG particles were below 500 μm. The X-ray diffraction (XRD) analysis identified crystalline phases of albite (30 %), Quartz (16%), Anorthite (16 %), and Phillipsite (14%). The X-ray fluorescence (XRF) determinations showed mainly 55% of SiO2, 13 % of Al2O3, and 9% of CaO. ICP (OES) concentrations of Fe, Ca, Cu, Al, As, V, Zn, Mo, and Ni were 49.545; 24.735; 6.172; 14.152, 239,5; 129,6; 41,1;15,1, and 13,1 mg kg-1, respectively. The geopolymer samples showed resistance ranging between 2 and 10 MPa. In comparison with the raw material composition, the amorphous percentage of materials in the geopolymer was 35 %, whereas the crystalline percentage of main mineral phases decreased. Further studies are needed to find the optimal combinations of materials to produce a more resistant and environmentally safe geopolymer. Particularly are necessary compressive resistance higher than 15 MPa are necessary to be used as construction unit such as bricks.

Keywords: mining waste, geopolymer, construction material, alkaline activation

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Authors: P. Mirahmadpour, M. H. Banitaba, D. Nematollahi

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The chemistry of coordination polymers in recent years has grown exponentially not only because of their interesting architectures but also due to their various technical applications in many fields including ion exchange, chemical catalysis, small molecule separations, and drug release. The use of bridging ligands for the controlled self-assembly of one, two or three dimensional metallo-supramolecular species is the subject of serious study in last decade. Numerous different synthetic methods have been offered for the preparation of coordination polymers such as (a) diffusion from the gas phase, (b) slow diffusion of the reactants into a polymeric matrix, (c) evaporation of the solvent at ambient or reduced temperatures, (d) temperature controlled cooling, (e) precipitation or recrystallisation from a mixture of solvents and (f) hydrothermal synthesis. The electrosynthetic process suggested several advantages over conventional approaches. A general advantage of electrochemical synthesis is that it allows synthesis under milder conditions than typical solvothermal or microwave synthesis. In this work we have introduced a simple electrochemical method for growing metal coordination polymers based on copper with a flexible 2,2’-thiodiacetic acid (TDA) and rigid 1,2,4,5-benzenetetracarboxylate (BTC) ligands. The structure of coordination polymers were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), elemental analysis, thermal gravimetric (TG) and differential thermal analyses (DTA). The single-crystal X-ray diffraction analysis revealed that different conformations of the ligands and different coordination modes of the carboxylate group as well as different coordination geometries of the copper atoms. Electrochemical synthesis of coordination polymers has different advantages such as faster synthesis at lower temperature in compare with conventional chemical methods and crystallization of desired materials in a single synthetic step.

Keywords: 1, 2, 4, 5-benzenetetracarboxylate, coordination polymer, copper, 2, 2’-thiodiacetic acid

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Authors: A. E. Yakshin, D. Ijpes, J. M. Sturm, I. A. Makhotkin, M. D. Ackermann

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Applications like synchrotron optics, soft X-ray microscopy, X-ray astronomy, and wavelength dispersive X-ray fluorescence (WD-XRF) rely heavily on short- and ultra-short-period multilayer (ML) structures. In WD-XRF, ML serves as an analyzer crystal to disperse emission lines of light elements. The key requirement for the ML is to be highly reflective while also providing sufficient angular dispersion to resolve specific XRF lines. For these reasons, MLs with periods ranging from 1.0 to 2.5 nm are of great interest in this field. Due to the short period, the reflectance of such MLs is extremely sensitive to interface imperfections such as roughness and interdiffusion. Moreover, the thickness of the individual layers is only a few angstroms, which is close to the limit of materials to grow a continuous film. MLs with a period between 2.5 nm and 1.0 nm, combining tungsten (W) reflector with B₄C, Si, and Al spacers, were created and examined. These combinations show high theoretical reflectance in the full range from C-Kα (4.48nm) down to S-Kα (0.54nm). However, the formation of optically unfavorable compounds, intermixing, and interface roughness result in limited reflectance. A variety of techniques, including diffusion barriers, seed layers, and ion polishing for sputter-deposited MLs, were used to address these issues. Diffuse scattering measurements, photo-electron spectroscopy analysis, and X-ray reflectivity measurements showed a noticeable reduction of compound formation, intermixing, and interface roughness. This also resulted in a substantial increase in soft X-ray reflectance for W/Si, W/B4C, and W/Al MLs. In particular, the reflectivity of 1 nm period W/Si multilayers at the wavelength of 0.84 nm increased more than 3-fold – propelling forward the applicability of such multilayers for shorter wavelengths.

Keywords: interface engineering, reflectance, short period multilayer structures, x-ray optics

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Authors: Andile Mkhohlakali, Tien-Chien Jen, James Tshilongo, Happy Mabowa

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Among different parameters, oxygen is one of the most important analytes of interest, dissolved oxygen (DO) concentration is very crucial and significant for various areas of physical, chemical, and environmental monitoring. Herein we report oxygen-sensitive luminophores -based lanthanum(III) trifluoromethanesulfonate), [La]³⁺ was encapsulated into SiO₂-based xerogel matrix. The nanosensor is composed of organically modified silica nanoparticles, doped with the luminescent oxygen–sensitive lanthanum(III) trifluoromethanesulfonate complex. The precursor materials used for sensing film were triethyl ethoxy silane (TEOS) and (3-Mercaptopropyltriethoxysilane) (MPTMS- TEOS) used for SiO2-baed matrices. Brunauer–Emmett–Teller (BET), and BJH indicate that the SiO₂ transformed from microporous to mesoporous upon the addition of La³⁺ luminophore with increased surface area (SBET). The typical amorphous SiO₂ based xerogels were revealed with X-Ray diffraction (XRD) and Selected Area Electron Diffraction (SAED) analysis. Scanning electron microscope- (SEM) and transmission electron microscope (TEM) showed the porous morphology and reduced particle for SiO₂ and La-SiO₂ xerogels respectively. The existence of elements, siloxane networks, and thermal stability of xerogel was confirmed by energy dispersive spectroscopy (EDS), Fourier-transform infrared spectroscopy (FTIR), and Thermographic analysis (TGA). UV-Vis spectroscopy and photoluminescence (PL) have been used to characterize the optical properties of xerogels. La-SiO₂ demonstrates promising characteristic features of an active sensing film for dissolved oxygen in the water. Keywords: Sol-gel, ORMOSILs, encapsulation, Luminophores quenching, O₂-sensing

Keywords: sol-gel, ORMOSILs, luminophores quenching, O₂-sensing

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Authors: S. S. Sravanthi, Swati Ghosh Acharyya

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Automotive light weighting is of major prominence in the current times due to its contribution in improved fuel economy and reduced environmental pollution. Various arc welding technologies are being employed in the production of automobile components with reduced weight. The present study is of practical importance since it involves preferential substitution of Zinc coated mild steel with a light weight alloy such as 6061 Aluminium by means of Gas Metal Arc Welding (GMAW) – Brazing technique at different processing parameters. However, the fabricated joints have shown the generation of Al – Fe layer at the interfacial regions which was confirmed by the Scanning Electron Microscope and Energy Dispersion Spectroscopy. These Al-Fe compounds not only affect the mechanical strength, but also predominantly deteriorate the corrosion resistance of the joints. Hence, it is essential to understand the phases formed in this layer and their crystal structure. Micro area X - ray diffraction technique has been exclusively used for this study. Moreover, the crevice corrosion analysis at the joint interfaces was done by exposing the joints to 5 wt.% FeCl₃ solution at regular time intervals as per ASTM G 48-03. The joints have shown a decreased crevice corrosion resistance with increased heat intensity. Inner surfaces of welds have shown severe oxide cracking and a remarkable weight loss when exposed to concentrated FeCl₃. The weight loss was enhanced with decreased filler wire feed rate and increased heat intensity. 

Keywords: automobiles, welding, corrosion, lap joints, Micro XRD

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Authors: Navneet Kaur, S. D. Tiwari

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Magnetic nanoparticles possess fascinating properties which make their behavior unique in comparison to corresponding bulk materials. Superparamagnetism is one such interesting phenomenon exhibited only by small particles of magnetic materials. In this state, the thermal energy of particles become more than their magnetic anisotropy energy, and so particle magnetic moment vectors fluctuate between states of minimum energy. This situation is similar to paramagnetism of non-interacting ions and termed as superparamagnetism. The magnetization of such systems has been described by Langevin function. But, the estimated fit parameters, in this case, are found to be unphysical. It is due to non-consideration of particle size distribution. In this work, analysis of magnetization data on NiO nanoparticles is presented considering the effect of particle size distribution. Nanoparticles of NiO of two different sizes are prepared by heating freshly synthesized Ni(OH)₂ at different temperatures. Room temperature X-ray diffraction patterns confirm the formation of single phase of NiO. The diffraction lines are seen to be quite broad indicating the nanocrystalline nature of the samples. The average crystallite size are estimated to be about 6 and 8 nm. The samples are also characterized by transmission electron microscope. Magnetization of both sample is measured as function of temperature and applied magnetic field. Zero field cooled and field cooled magnetization are measured as a function of temperature to determine the bifurcation temperature. The magnetization is also measured at several temperatures in superparamagnetic region. The data are fitted to an appropriate expression considering a distribution in particle size following a least square fit procedure. The computer codes are written in PYTHON. The presented analysis is found to be very useful for estimating the particle size distribution present in the samples. The estimated distributions are compared with those determined from transmission electron micrographs.

Keywords: anisotropy, magnetization, nanoparticles, superparamagnetism

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Authors: Amal A. Al-Kahlawy, Heba H. El-Maghrabi

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Due to the increasing need to environment protection in real time need to energize new materials are under extensive investigations. Between others, TiO2 nanotubes (TNTs) nanocomposite with iron oxide and silver carbonate, are promising alternatives as high-efficiency visible light photocatalyst due to their unique properties and their superior charge transport properties. Our efforts in this domain aim the construction of novel nanocomposite of TiO2NT/Fe2O3@Ag2CO3. The structure, surface morphology, chemical composition and optical properties were characterized by X-ray diffraction (XRD), Raman, Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and UV–vis diffuse reflectance spectroscopy (DRS). XRD results confirm the interaction of TiO2-NT with iron oxide. This novel nanocomposite shows remarkably enhanced performance for phenol compounds photodegradation. The experimental data shows a promising photocatalytic activity. In particular, a maximum value of 450 mg/g was removed within 60 min at solar light irradiation with degradation efficiency of 99.5%. The high photocatalytic activity of the nanocomposite is found to be related to the increased adsorption toward chemical species, enhanced light absorption and efficient charge separation and transfer. Finally, the designed TiO2NT/Fe2O3@Ag2CO3 nanocomposite has a great degree of sustainability and could has a potential application for the industrial treatment of wastewater containing toxic organic materials.

Keywords: nanocomposite, photocatalyst, solar energy, titanium dioxide nanotubes

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Authors: Reza Ziaie Moayed, Saeideh Mohammadi

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Soft soil is used in many of civil engineering projects like coastal, marine and road projects. Because of low shear strength and stiffness of soft soils, large settlement and low bearing capacity will occur under superstructure loads. This will make the civil engineering activities more difficult and costlier. In the case of soft soils, improvement is a suitable method to increase the shear strength and stiffness for engineering purposes. In recent years, the artificial cementation of soil by cement and lime has been extensively used for soft soil improvement. Cement stabilization is a well-established technique for improving soft soils. Artificial cementation increases the shear strength and hardness of the natural soils. On the other hand, in soft soils, the use of piles to transfer loads to the depths of ground is usual. By using cement treated soil around the piles, high bearing capacity and low settlement in piles can be achieved. In the present study, lateral bearing capacity of short piles in cemented soils is investigated by numerical approach. For this purpose, three dimensional (3D) finite difference software, FLAC 3D is used. Cement treated soil has a strain hardening-softening behavior, because of breaking of bonds between cement agent and soil particle. To simulate such behavior, strain hardening-softening soil constitutive model is used for cement treated soft soil. Additionally, conventional elastic-plastic Mohr Coulomb constitutive model and linear elastic model are used for stress-strain behavior of natural soils and pile. To determine the parameters of constitutive models and also for verification of numerical model, the results of available triaxial laboratory tests on and insitu loading of piles in cement treated soft soil are used. Different parameters are considered in parametric study to determine the effective parameters on the bearing of the piles on cemented treated soils. In the present paper, the effect of various length and height of the artificial cemented area, different diameter and length of the pile and the properties of the materials are studied. Also, the effect of choosing a constitutive model for cemented treated soils in the bearing capacity of the pile is investigated.

Keywords: bearing capacity, cement-treated soils, FLAC 3D, pile

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Authors: Pramod Jagtap, Kisan Jadhav, Neha Dand

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Risperidone (RISP) is an antipsychotic agent and has low water solubility and nontargeted delivery results in numerous side effects. Hence, an attempt was made to develop SLNs hydrogel for intranasal delivery of RISP to achieve maximum bioavailability and reduction of side effects. RISP loaded SLNs composed of 1.65% (w/v) lipid mass were produced by high shear homogenization (HSH) coupled ultrasound (US) method using glyceryl monostearate (GMS) or Imwitor 900K (solid lipid). The particles were loaded with 0.2% (w/v) of the RISP & surface-tailored with a 2.02% (w/v) non-ionic surfactant Tween® 80. Optimization was done using 32 factorial design using Design Expert® software. The prepared SLNs dispersion incorporated into Polycarbophil AA1 hydrogel (0.5% w/v). The final gel formulation was evaluated for entrapment efficiency, particle size, rheological properties, X ray diffraction, in vitro diffusion, ex vivo permeation using sheep nasal mucosa and histopathological studies for nasocilliary toxicity. The entrapment efficiency of optimized SLNs was found to be 76 ± 2 %, polydispersity index <0.3., particle size 278 ± 5 nm. This optimized batch was incorporated into hydrogel. The pH was found to be 6.4 ± 0.14. The rheological behaviour of hydrogel formulation revealed no thixotropic behaviour. In histopathology study, there was no nasocilliary toxicity observed in nasal mucosa after ex vivo permeation. X-ray diffraction data shows drug was in amorphous form. Ex vivo permeation study shows controlled release profile of drug.

Keywords: ex vivo, particle size, risperidone, solid lipid nanoparticles

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Authors: Salvana P. M. Costa, Tarcyla A. Gomes, Giovanna C. R. M. Schver, Leslie R. M. Ferraz, Cristovão R. Silva, Magaly A. M. Lyra, Danilo A. F. Fonte, Larissa A. Rolim, Amanda C. Q. M. Vieira, Miracy M. Albuquerque, Pedro J. Rolim-neto

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Efavirenz (EFV) is considered one of the most widely used anti-HIV drugs. However, it is classified as a drug class II (poorly soluble, highly permeable) according to the biopharmaceutical classification system, presenting problems of absorption in the gastrointestinal tract and thereby inadequate bioavailability for its therapeutic action. This study aimed to overcome these barriers by developing and obtaining solid dispersions (SD) in order to increase the EFZ bioavailability. For the development of SD with EFV, theoretical and practical studies were initially performed. Thus, there was a choice of a carrier to be used. For this, it was analyzed the various criteria such as glass transition temperature of the polymer, intra- and intermolecular interactions of hydrogen bonds between drug and polymer, the miscibility between the polymer and EFV. The choice of the obtainment method of the SD came from the analysis of which method is the most consolidated in both industry and literature. Subsequently, the choice of drug and carrier concentrations in the dispersions was carried out. In order to obtain DS to present the drug in its amorphous form, as the DS were obtained, they were analyzed by X-ray diffraction (XRD). SD are more stable the higher the amount of polymer present in the formulation. With this assumption, a SD containing 10% of drug was initially prepared and then this proportion was increased until the XRD showed the presence of EFV in its crystalline form. From this point, it was not produced SD with a higher concentration of drug. Thus, it was allowed to select PVP-K30, PVPVA 64 and the SOLUPLUS formulation as carriers, once it was possible the formation of hydrogen bond between EFV and polymers since these have hydrogen acceptor groups capable of interacting with the donor group of the drug hydrogen. It is worth mentioning also that the films obtained, independent of concentration used, were presented homogeneous and transparent. Thus, it can be said that the EFV is miscible in the three polymers used in the study. The SD and Physical Mixtures (PM) with these polymers were prepared by the solvent method. The EFV diffraction profile showed main peaks at around 2θ of 6,24°, in addition to other minor peaks at 14,34°, 17,08°, 20,3°, 21,36° and 25,06°, evidencing its crystalline character. Furthermore, the polymers showed amorphous nature, as evidenced by the absence of peaks in their XRD patterns. The XRD patterns showed the PM overlapping profile of the drug with the polymer, indicating the presence of EFV in its crystalline form. Regardless the proportion of drug used in SD, all the samples showed the same characteristics with no diffraction peaks EFV, demonstrating the behavior amorphous products. Thus, the polymers enabled, effectively, the formation of amorphous SD, probably due to the potential hydrogen bonds between them and the drug. Moreover, the XRD analysis showed that the polymers were able to maintain its amorphous form in a concentration of up to 80% drug.

Keywords: amorphous form, Efavirenz, solid dispersions, solubility

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Authors: Michella Alnajjar, Frederic Christien, Krzysztof Wolski, Cedric Bosch

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Additive manufacturing (AM) has gained more interest in the past few years because it allows 3D parts often having a complex geometry to be directly fabricated, layer by layer according to a CAD model. One of the AM techniques is the selective laser melting (SLM) which is based on powder bed fusion. In this work, the corrosion resistance of 17-4 PH steel obtained by SLM is investigated. Wrought 17-4 PH steel is a martensitic precipitation hardenable stainless steel. It is widely used in a variety of applications such as aerospace, medical and food industries, due to its high strength and relatively good corrosion resistance. However, the combined findings of X-Ray diffraction and electron backscatter diffraction (EBSD) proved that SLM-ed 17-4 PH steel has a fully ferritic microstructure, more specifically δ ferrite. The microstructure consists of coarse ferritic grains elongated along the build direction, with a pronounced solidification crystallographic texture. These results were associated with the high cooling and heating rates experienced throughout the SLM process (10⁵-10⁶ K/s) that suppressed the austenite formation and produced a 'by-passing' phenomenon of this phase during the numerous thermal cycles. Furthermore, EDS measurements revealed a uniform distribution of elements without any dendritic structure. The extremely high cooling kinetics induced a diffusionless solidification, resulting in a homogeneous elemental composition. Consequently, the corrosion properties of this steel are altered from that of conventional ones. By using electrochemical means, it was found that SLM-ed 17-4 PH is more resistant to general corrosion than the wrought steel. However, the SLM-ed material exhibits metastable pitting due to its high porosity density. In addition, the hydrogen embrittlement of SLM-ed 17-4 PH steel is investigated, and a correlation between its behavior and the observed microstructure is made.

Keywords: corrosion resistance, 17-4 PH stainless steel, selective laser melting, hydrogen embrittlement

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Authors: Osman Adiguzel

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Shape-memory alloys are a new class of functional materials with a peculiar property known as shape memory effect. These alloys return to a previously defined shape on heating after deformation in low temperature product phase region and take place in a class of functional materials due to this property. The origin of this phenomenon lies in the fact that the material changes its internal crystalline structure with changing temperature. Shape memory effect is based on martensitic transitions, which govern the remarkable changes in internal crystalline structure of materials. Martensitic transformation, which is a solid state phase transformation, occurs in thermal manner in material on cooling from high temperature parent phase region. This transformation is governed by changes in the crystalline structure of the material. Shape memory alloys cycle between original and deformed shapes in bulk level on heating and cooling, and can be used as a thermal actuator or temperature-sensitive elements due to this property. Martensitic transformations usually occur with the cooperative movement of atoms by means of lattice invariant shears. The ordered parent phase structures turn into twinned structures with this movement in crystallographic manner in thermal induced case. The twinned martensites turn into the twinned or oriented martensite by stressing the material at low temperature martensitic phase condition. The detwinned martensite turns into the parent phase structure on first heating, first cycle, and parent phase structures turn into the twinned and detwinned structures respectively in irreversible and reversible memory cases. On the other hand, shape memory materials are very important and useful in many interdisciplinary fields such as medicine, pharmacy, bioengineering, metallurgy and many engineering fields. The choice of material as well as actuator and sensor to combine it with the host structure is very essential to develop main materials and structures. Copper based alloys exhibit this property in metastable beta-phase region, which has bcc-based structures at high temperature parent phase field, and these structures martensitically turn into layered complex structures with lattice twinning following two ordered reactions on cooling. Martensitic transition occurs as self-accommodated martensite with inhomogeneous shears, lattice invariant shears which occur in two opposite directions, <110 > -type directions on the {110}-type plane of austenite matrix which is basal plane of martensite. This kind of shear can be called as {110}<110> -type mode and gives rise to the formation of layered structures, like 3R, 9R or 18R depending on the stacking sequences on the close-packed planes of the ordered lattice. In the present contribution, x-ray diffraction and transmission electron microscopy (TEM) studies were carried out on two copper based alloys which have the chemical compositions in weight; Cu-26.1%Zn 4%Al and Cu-11%Al-6%Mn. X-ray diffraction profiles and electron diffraction patterns reveal that both alloys exhibit super lattice reflections inherited from parent phase due to the displacive character of martensitic transformation. X-ray diffractograms taken in a long time interval show that locations and intensities of diffraction peaks change with the aging time at room temperature. In particular, some of the successive peak pairs providing a special relation between Miller indices come close each other.

Keywords: Shape memory effect, martensite, twinning, detwinning, self-accommodation, layered structures

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Authors: C. Busuioc, S. I. Jinga, E. Pavel

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The continuous need of more non-volatile memories with a higher storage capacity, smaller dimensions and weight, as well as lower costs, has led to the exploration of optical lithography on active media, as well as patterned magnetic composites. In this context, optical lithography is a technique that can provide a significant decrease of the information bit size to the nanometric scale. However, there are some restrictions that arise from the need of breaking the optical diffraction limit. Major achievements have been obtained by employing a vitoceramic material as active medium and a laser beam operated at low power for the direct writing procedure. Thus, optical discs with ultra-high density were fabricated by a conventional melt-quenching method starting from analytical purity reagents. They were subsequently used for 3D recording based on their photosensitive features. Naturally, the next step consists in the elucidation of the composition and structure of the active centers, in correlation with the use of silver and rare-earth compounds for the synthesis of the optical supports. This has been accomplished by modern characterization methods, namely transmission electron microscopy coupled with selected area electron diffraction, scanning transmission electron microscopy and electron energy loss spectroscopy. The influence of laser diode parameters, silver concentration and fluorescent compounds formation on the writing process and final material properties was investigated. The results indicate performances in terms of capacity with two order of magnitude higher than other reported information storage systems. Moreover, the fluorescent photosensitive vitroceramics may be integrated in other applications which appeal to nanofabrication as the driving force in electronics and photonics fields.

Keywords: data storage, fluorescent compounds, laser writing, vitroceramics

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Authors: Opeyemi Atiba-Oyewo, Maurice S. Onya, Christian Wolkersdorfer

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Nanostructure formation and characterization of eco-friendly banana peels nanosorbent are thoroughly described in this paper. The transformation of material during mechanical milling to enhance certain properties such as changes in microstructure and surface area to solve the current problems involving water pollution and water quality were studied. The mechanical milling was employed using planetary continuous milling machine and ethanol as process control agent, the sample were taken at time interval between 10 h to 30 h to examine the structural changes. The samples were characterised by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infra-red (FTIR), Transmission electron microscopy (TEM) and Brunauer Emmett and teller (BET). Results revealed that the three typical structures with different grain-size, lattice strain and shapes were observed, and the deformation mechanisms in these structures were found to be different, further particles fracturing results to surface area increment which was confirmed by Brunauer Emmett and teller (BET) analysis. X-ray diffraction (XRD) shows high densities of dislocations in large crystallites, implying that dislocation slip is the dominant deformation mechanism. Scanning electron microscopy revealed the morphological properties of the materials at different milling time, nanostructure of the particles and fibres were confirmed by Transmission electron microscopy and FT-IR identified the functional groups responsible for its capacity to coordinate and remove metal ions, such as the carboxylic and amine groups at absorption bands of 1730 and 889 cm-1, respectively. However, the choice of this sorbent material for the sorption of any contaminants will depend on the composition of the effluent to be treated.

Keywords: banana peels, eco-friendly, mechanical milling, nanosorbent, nanostructure water quality

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Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

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We are reporting a simple and low-cost chemical precipitation method adopted to prepare zinc oxide nanoparticles (ZnO) using polyvinyl pyrrolidone (PVP) as a capping agent. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) was applied on the dried gel sample to record the phase transformation temperature of zinc hydroxide Zn(OH)2 to zinc oxide (ZnO) to obtain the annealing temperature of 800C. The thermal, structure, morphology and optical properties have been employed by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM). X-ray diffraction results confirmed the wurtzite hexagonal structure of ZnO nanoparticles. The two intensive peaks at 160 and 432 cm-1 in the Raman Spectrum are mainly attributed to the first order modes of the wurtzite ZnO nanoparticles. The energy band gap obtained from the UV-Vis absorption spectra, shows a blue shift, which is attributed to increase in carrier concentration (Burstein Moss Effect). Photoluminescence studies of the single crystalline ZnO nanoparticles, show a strong peak centered at 385 nm, corresponding to the near band edge emission in ultraviolet range. The mixed shape of grapes, sphere, hexagonal and rock like structure has been noticed in FESEM. The results showed that PVP is a suitable capping agent for the preparation of ZnO nanoparticles by simple chemical precipitation method.

Keywords: ZnO nanoparticles, simple chemical precipitation route, mixed shape morphology, UV-visible absorption, photoluminescence, Fourier transform infra-Red spectroscopy

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Authors: J. Alvarez, J. Pimienta, R. Sarmiento

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Diode lasers working in free mode present different shifting and broadening determined by external factors such as temperature, current or mechanical vibrations, and they are not more useful in applications such as spectroscopy, metrology, and cooling of atoms, among others. Different configurations can reduce the spectral width of a laser; one of the most effective is to extend the optical resonator of the laser diode and use optical feedback either with the help of a partially reflective mirror or with a diffraction grating; this latter configuration is not only allowed to reduce the spectral width of the laser line but also to coarsely adjust its working wavelength, within a wide range typically ~ 10nm by slightly varying the angle of the diffraction grating. Two settings are commonly used for this purpose, the Littrow configuration and the Littmann Metcalf. In this paper, we present the design, construction, and characterization of a compact extended laser cavity in Littrow configuration. The designed cavity is compact and was machined on an aluminum block using computer numerical control (CNC); it has a mass of only 380 g. The design was tested on laser diodes with different wavelengths, 650nm, 780nm, and 795 nm, but can be equally efficient at other wavelengths. This report details the results obtained from the extended cavity working at a wavelength of 780 nm, with an output power of around 35mW and a line width of less than 1Mhz. The cavity was used to observe the spectrum of the corresponding Rubidium D2 line. By modulating the current and with the help of phase detection techniques, a dispersion signal with an excellent signal-to-noise ratio was generated that allowed the stabilization of the laser to a transition of the hyperfine structure of Rubidium with an integral proportional controller (PI) circuit made with precision operational amplifiers.

Keywords: Littrow, Littman-Metcalf, line width, laser stabilization, hyperfine structure

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Authors: Matthew Ferguson, Tatyana Konkova, Ioannis Violatos

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Microstructure analysis of additively manufactured (AM) materials is an important step in understanding the interrelationship between mechanical properties and materials performance. Literature on the effect of laser-based AM process parameters on the microstructure in the substrate-deposit interface is limited. The interface region, the adjoining area of substrate and deposit, is characterized by the presence of the fusion zone (FZ) and heat-affected zone (HAZ), experiencing rapid thermal gyrations resulting in thermal-induced transformations. Inconel 718 was utilized as work material for both the substrate and deposit. Three blocks of Inconel 718 material were deposited by Direct Energy Deposition (DED) using three different laser powers, 550W, 750W and 950W, respectively. A coupled thermo-mechanical transient approach was utilized to correlate temperature history to the evolution of microstructure. The thermal history of the deposition process was monitored with the thermocouples installed inside the substrate material. The interface region of the blocks was analyzed with Optical Microscopy (OM) and Scanning Electron Microscopy (SEM), including the electron back-scattered diffraction (EBSD) technique. Laser power was found to influence the dissolution of intermetallic precipitated phases in the substrate and grain growth in the interface region. Microstructure and thermal history data were utilized to draw conclusive comparisons between the investigated process parameters.

Keywords: additive manufacturing, direct energy deposition, electron back-scattered diffraction, finite element analysis, inconel 718, microstructure, optical microscopy, scanning electron microscopy, substrate-deposit interface region

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Authors: Vaibhav Budhiraja, Chandra Mouli Pandey

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The ultrasonic synthesis of nanostructured conducting copolymer is an effective technique to synthesize polymer with desired chemical properties. This tailored nanostructure, shows tremendous improvement in sensitivity and stability to detect a variety of analytes. The present work reports ultrasonically synthesized nanostructured conducting poly(o-phenylenediamine)-co-poly(1-naphthylamine) (POPD-co-PNA). The synthesized material has been characterized using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy, transmission electron microscopy, X-ray diffraction and cyclic voltammetry. FTIR spectroscopy confirmed random copolymerization, while UV-visible studies reveal the variation in polaronic states upon copolymerization. High crystallinity was achieved via ultrasonic synthesis which was confirmed by X-ray diffraction, and the controlled morphology of the nanostructures was confirmed by transmission electron microscopy analysis. Cyclic voltammetry shows that POPD-co-PNA has rather high electrochemical activity. This behavior was explained on the basis of variable orientations adopted by the conducting polymer chains. The synthesized material was electrophoretically deposited at onto indium tin oxide coated glass substrate which is used as cathode and parallel platinum plate as the counter electrode. The fabricated bioelectrode was further used for detection of glucose by crosslinking of glucose oxidase in the PODP-co-PNA film. The bioelectrode shows a surface-controlled electrode reaction with the electron transfer coefficient (α) of 0.72, charge transfer rate constant (ks) of 21.77 s⁻¹ and diffusion coefficient 7.354 × 10⁻¹⁵ cm²s⁻¹.

Keywords: conducting, electrophoretic, glucose, poly (o-phenylenediamine), poly (1-naphthylamine), ultrasonic

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Authors: E. Gandomkar, S. Sabbaghi

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In this paper, the effects of variation synthesized methods on morphology and size of silica nanostructure via modifying sol-gel and precipitation method have been investigated. Meanwhile, resulting products have been characterized by particle size analyzer, scanning electron microscopy (SEM), X-ray Diffraction (XRD) and Fourier transform infrared (FT-IR) spectra. As result, the shape of SiO2 with sol-gel and precipitation methods was spherical but with modifying sol-gel method we have been had nanolayer structure.

Keywords: modified sol-gel, precipitation, nanolayer, Na2SiO3, nanoparticle

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Authors: Atef Y. Shenouda, Anton A. Momchilov

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Graphene and CdO with different stoichiometric ratios of Cd(CH₃COO)₂ and graphene samples were prepared by hydrothermal reaction. The crystalline phases of pure CdO and 3CdO:1graphene were identified by X-ray diffraction (XRD). The particle morphology was studied with SEM. Furthermore, impedance measurements were applied. Galvanostatic measurements for the cells were carried out using potential limits between 0.01 and 3 V vs. Li/Li⁺. The current cycling intensity was 10⁻⁴ A. The specific discharge capacity of 3CdO-1G cell was about 450 Ah.Kg⁻¹ up to more than 100 cycles.

Keywords: CdO, graphene, negative electrode, lithium battery

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Authors: Adya H. Uluwita, Fernando B. D. S. Pedrosa, Georgi M. Georgiev, Raoul Masterson

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CERN is an international organisation funded by 23 countries which provides the particle physics community with excellence in particle accelerators and other related facilities. Founded in 1954, CERN has a wide range of accelerators that allow groundbreaking science to be conducted. Accelerators bring particles to high levels of energy and make them collide with each other or with fixed targets, creating specific conditions that are of high interest to physicists. A chain of accelerators is used to ramp up the energy of particles and eventually inject them into the largest and most recent one of them: the Large Hadron Collider (LHC). Among this chain of machines is, for instance, the Proton Synchrotron, which was started in 1959 and is still in operation. These machines, called "injectors”, keep evolving over time, as well as the related infrastructure. Massive decommissioning of obsolete cables started in 2015 at CERN in the frame of the so-called "injectors de-cabling project phase 1". Its goal was to replace aging cables and remove unused ones, freeing space for new cables necessary for upgrades and consolidation campaigns. To proceed with the de-cabling, a project coordination team was assembled. The start of this project phase led to the investigation of legacy cables throughout the organisation. The identification of cables stacked during half a century proved to be arduous. Phase 1 of the injectors de-cabling was implemented for three years with success after overcoming some difficulties. Phase 2, which started 3 years later, focused on improving safety and structure with the introduction of a quality assurance procedure. This paper discusses the implementation of this quality assurance procedure throughout phase 2 of the project and the transition between the two phases. Over hundreds of kilometres of cable were removed in the injectors complex at CERN from 2015 to 2023.

Keywords: CERN, de-cabling, injectors, quality assurance procedure

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Authors: Madeleine Cox

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Objective: discussion of diagnosis of vernix caseosa peritonitis, recovery and subsequent caesarean seciton Case: 30 year old G4P1 presented in labour at 40 weeks, planning a vaginal birth afterprevious caesarean section. She underwent an emergency caesarean section due to concerns for fetal wellbeing on CTG. She was found to have a thin lower segment with a very small area of dehiscence centrally. The operation was uncomplicated, and she recovered and went home 2 days later. She then represented to the emergency department day 6 post partum feeling very unwell, with significant abdominal pain, tachycardia as well as urinary retention. Raised white cell count of 13.7 with neutrophils of 11.64, CRP of 153. An abdominal ultrasound was poorly tolerated by the patient and did not aide in the diagnosis. Chest and abdominal xray were normal. She underwent a CT chest and abdomen, which found a small volume of free fluid with no apparent collection. Given no obvious cause of her symptoms were found and the patient did not improve, she had a repeat CT 2 days later, which showed progression of free fluid. A diagnostic laparoscopy was performed with general surgeons, which reveled turbid fluid, an inflamed appendix which was removed. The patient improved remarkably post operatively. The histology showed periappendicitis with acute appendicitis with marked serosal inflammatory reaction to vernix caseosa. Following this, the patient went on to recover well. 4 years later, the patient was booked for an elective caesarean section, on entry into the abdomen, there were very minimal adhesions, and the surgery and her subsequent recovery was uncomplicated. Discussion: this case represents the diagnostic dilemma of a patient who presents unwell without a clear cause. In this circumstance, multiple modes of imaging did not aide in her diagnosis, and so she underwent diagnostic surgery. It is important to evaluate if a patient is or is not responding to the typical causes of post operative pain and adjust management accordingly. A multiteam approach can help to provide a diagnosis for these patients. Conclusion: Vernix caseosa peritonitis is a rare cause of acute abdomen post partum. There are few reports in the literature of the initial presentation and no reports on the possible effects on future pregnancies. This patient did not have any complications in her following pregnancy or delivery secondary to her diagnosis of vernix caseosa peritonitis. This may assist in counselling other women who have had this uncommon diagnosis.

Keywords: peritonitis, obstetrics, caesarean section, pain

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Authors: A. Feliczak Guzik, I. Nowak

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Zeolites, classified as microporous materials, are a large group of crystalline aluminosilicate materials commonly used in the chemical industry. These materials are characterized by large specific surface area, high adsorption capacity, hydrothermal and thermal stability. However, the micropores present in them impose strong mass transfer limitations, resulting in low catalytic performance. Consequently, mesoporous (hierarchical) zeolites have attracted considerable attention from researchers. These materials possess additional porosity in the mesopore size region (2-50 nm according to IUPAC). Mesoporous zeolites, based on commercial MFI-type zeolites modified with silver, were synthesized as follows: 0.5 g of zeolite was dispersed in a mixture containing CTABr (template), water, ethanol, and ammonia under ultrasound for 30 min at 65°C. The silicon source, which was tetraethyl orthosilicate, was then added and stirred for 4 h. After this time, silver(I) nitrate was added. In a further step, the whole mixture was filtered and washed with water: ethanol mixture. The template was removed by calcination at 550°C for 5h. All the materials obtained were characterized by the following techniques: X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), nitrogen adsorption/desorption isotherms, FTIR spectroscopy. X-ray diffraction and low-temperature nitrogen adsorption/desorption isotherms revealed additional secondary porosity. Moreover, the structure of the commercial zeolite was preserved during most of the material syntheses. The aforementioned materials were used in the epoxidation reaction of cyclohexene using conventional heating and microwave radiation heating. The composition of the reaction mixture was analyzed every 1 h by gas chromatography. As a result, about 60% conversion of cyclohexene and high selectivity to the desired reaction products i.e., 1,2-epoxy cyclohexane and 1,2-cyclohexane diol, were obtained.

Keywords: catalytic application, characterization, epoxidation, hierarchical zeolites, synthesis

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Authors: Hasan Türe, Kader Terzioglu, Evren Tunca

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Contamination of aqueous environment by heavy metal ions is a serious and complex problem, owing to their hazards to human being and ecological systems. The treatment methods utilized for removing metal ions from aqueous solution include membrane separation, ion exchange and chemical precipitation. However, these methods are limited by high operational cost. Recently, biobased beads are considered as promising biosorbent to remove heavy metal ions from water. The aim of present study was to characterize the alginate/perlite composite beads and to investigate the adsorption performance of obtained beads for removing Pb (II) from aqueous solution. Alginate beads were synthesized by ionic gelation methods and different amount of perlite (aljinate:perlite=1, 2, 3, 4, 5 wt./wt.) was incorporated into alginate beads. Samples were characterized by means of X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM). The effects of perlite level, the initial concentration of Pb (II), initial pH value of Pb(II) solution and effect of contact time on the adsorption capacity of beads were investigated by using batch method. XRD analysis indicated that perlite includes silicon or silicon and aluminum bearing crystalline phase. The diffraction pattern of perlite containing beads is similar to that of that perlite powder with reduced intensity. SEM analysis revealed that perlite was embedded into alginate polymer and SEM-EDX (Energy-Dispersive X-ray) showed that composite beads (aljinate:perlite=1) composed of C (41.93 wt.%,), O (43.64 wt.%), Na (10.20 wt.%), Al (0.74 wt.%), Si (2.72 wt.%) ve K (0.77 wt.%). According to TGA analysis, incorporation of perlite into beads significantly improved the thermal stability of the samples. Batch experiment indicated that optimum pH value for Pb (II) adsorption was found at pH=7 with 1 hour contact time. It was also found that the adsorption capacity of beads decreased with increases in perlite concentration. The results implied that alginate/perlite composite beads could be used as promising adsorbents for the removal of Pb (II) from wastewater. Acknowledgement: This study was supported by TUBITAK (Project No: 214Z146).

Keywords: alginate, adsorption, beads, perlite

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Authors: Atef Y. Shenouda, Fei Xu

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Cu₃SbS₃ (CAS) was synthesized by direct solid-state reaction from elementary Cu, Sb, & S and hydrothermal reaction using thioacetamide (TAM). Crystal structure and morphology for the prepared phases of Cu₃SbS₃ were studied via X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM). The band gap energies are 2 and 2.2 eV for the prepared samples. The two samples are as anode for Na ion storage. They show high initial capacity to 490 mAh/g. Na cell prepared from TAM sample shows 280 mAh/g after 25 cycles vs. 60 mAh/g for elemental sample.

Keywords: Cu3SbS3, sodium batteries, thioacetamide, sulphur sources

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Authors: Jin Lin, Shouxiang Lu, Kim Meow Liew

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In a fire accident, fire smoke often poses a serious threat to human safety especially in the enclosed space such as submarine and space-crafts environment. Efficient removal of the hazardous gas products particularly a large amount of CO and CO₂ gases from these confined space is critical for the security of the staff and necessary for the post-fire environment recovery. In this work, Cu-Mn-Ce composite oxide catalysts coupled with CO₂ sorbents were prepared using wet impregnation method, solid-state impregnation method and wet/solid-state impregnation method. The as-prepared samples were tested dynamically and isothermally for CO oxidation and CO₂ sorption and further characterized by the X-ray diffraction (XRD), nitrogen adsorption and desorption, and field emission scanning electron microscopy (FE-SEM). The results showed that all the samples were able to catalyze CO into CO₂ and capture CO₂ in situ by chemisorption. Among all the samples, the sample synthesized by the wet/solid-state impregnation method showed the highest catalytic activity toward CO oxidation and the fine ability of CO₂ sorption. The sample prepared by the solid-state impregnation method showed the second CO oxidation performance, while the coupled sample using the wet impregnation method exhibited much poor CO oxidation activity. The various CO oxidation and CO₂ sorption properties of the samples might arise from the different dispersed states of the CO₂ sorbent in the CO catalyst, owing to the different preparation methods. XRD results confirmed the high-dispersed sorbent phase in the samples prepared by the wet and solid impregnation method, while that of the sample prepared by wet/solid-state impregnation method showed the larger bulk phase as indicated by the high-intensity diffraction peaks. Nitrogen adsorption and desorption results further revealed that the latter sample had a higher surface area and pore volume, which were beneficial for the CO oxidation over the catalyst. Hence, the Cu-Mn-Ce oxide catalyst coupled with CO₂ sorbent using wet/solid-state impregnation method could be a good choice for fire smoke removal in the enclosed space.

Keywords: CO oxidation, CO₂ sorption, preparation methods, smoke removal

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Authors: Pandiyarajan Thangaraj, Mangalaraja Ramalinga Viswanathan, Karthikeyan Balasubramanian, Héctor D. Mansilla, José Ruiz

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Rare earth ions doped semiconductor nanostructures gained much attention due to their novel physical and chemical properties which lead to potential applications in laser technology as inexpensive luminescent materials. Doping of rare earth ions into ZnO semiconductor alter its electronic structure and emission properties. Surface modification (polymer covering) is one of the simplest techniques to modify the emission characteristics of host materials. The present work reports the synthesis and structural properties of PVA:Zn97Pr3O polymer nanocomposite free standing films. To prepare Pr3+ doped ZnO nanostructures and PVA:Zn97Pr3O polymer nanocomposite free standing films, the colloidal chemical and solution casting techniques were adopted, respectively. The formation of PVA:Zn97Pr3O films were confirmed through X-ray diffraction (XRD), absorption and Fourier transform infrared (FTIR) spectroscopy analyses. XRD measurements confirm the prepared materials are crystalline having hexagonal wurtzite structure. Polymer composite film exhibits the diffraction peaks of both PVA and ZnO structures. TEM images reveal the pure and Pr3+ doped ZnO nanostructures exhibit sheet like morphology. Optical absorption spectra show free excitonic absorption band of ZnO at 370 nm and, the PVA:Zn97Pr3O polymer film shows absorption bands at ~282 and 368 nm and these arise due to the presence of carbonyl containing structures connected to the PVA polymeric chains, mainly at the ends and free excitonic absorption of ZnO nanostructures, respectively. Transmission spectrum of as prepared film shows 57 to 69% of transparency in the visible and near IR region. FTIR spectral studies confirm the presence of A1 (TO) and E1 (TO) modes of Zn-O bond vibration and the formation of polymer composite materials.

Keywords: rare earth doped ZnO, polymer composites, structural characterization, surface modification

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Authors: Hayder Raad Hafuze, Munqith Saleem Dawood, Jamal Abdul Jabbar

Abstract:

The effect of using both ultrasounds with laser in medical imaging of the biological tissue has been studied in this paper. Different wave lengths of incident laser light (405 nm, 532 nm, 650 nm, 808 nm and 1064 nm) were used with different ultrasound frequencies (1MHz and 3.3MHz). The results showed that, the change of acoustic intensity enhance the laser penetration of the tissue for different thickness. The existence of the ideal Raman-Nath diffraction pattern were investigated in terms of phase delay and incident angle.

Keywords: tissue, laser, ultrasound, effect, imaging

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