Search results for: X-ray diffraction

Authors: Fernando G. Torres, Donna M. Ebenstein, Monica Merino

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Most fish are covered by a protective external armour. The characteristics of these armours depend on the individual elements that form them, such as scales, scutes or dermal plates. In this work, we assess the properties of two different types of protective elements: scales from A. gigas and dermal plates from P. pardalis. A. Gigas and P. Pardalis are two Amazonian fish with a rather prehistoric aspect. They have large scales and dermal plates that form two different types of protective body armours. Although both scales and dermal plates are formed by collagen and hydroxyapatite, their structures display remarkable differences. The structure and composition of the samples were assessed by means of X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). Morphology studies were carried out using a Scanning Electron Microscopy (SEM). Nanoindentation tests were performed to measure the reduced moduli in A. gigas scales and P. pardalis plates. The similarities and differences between scales and dermal plates are discussed based on the experimental results. Both protective armours are designed to be lightweight, flexible and tough. A. Gigas scales are are light laminated composites, while P. pardalis dermal plates show a sandwich like structure with dense outer layers and a porous inner matrix. It seems that the armour of P. pardalis is more suited for a bottom-dwelling fish and allows for protection against predators. The scales from A. Gigas are more adapted to give protection to a swimming fish. The information obtained from these studies is also important for the development of bioinspired nanocomposites, with potential applications in the biomedical field.

Keywords: pterygoplichthys pardalis, dermal plates arapaima gigas, fish scales

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Authors: Shaila Bahl, S. P. Lochab, Pratik Kumar

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Nanotechnology and nanomaterials have attracted researchers from different fields, especially from the field of luminescence. Recent studies on various luminescent nanomaterials have shown their relevance in dosimetry of ionizing radiations for the measurements of high doses using the Thermoluminescence (TL) technique, where the conventional microcrystalline phosphors saturate. Ion beams have been used for diagnostic and therapeutic purposes due to their favorable profile of dose deposition at the end of the range known as the Bragg peak. While dealing with human beings, doses from these beams need to be measured with great precision and accuracy. Henceforth detailed investigations of suitable thermoluminescent dosimeters (TLD) for dose verification in ion beam irradiation are required. This paper investigates the TL response of nanocrystalline BaSO4 doped with Eu to 85 MeV carbon beam. The synthesis was done using Co-precipitation technique by mixing Barium chloride and ammonium sulphate solutions. To investigate the crystallinity and particle size, analytical techniques such as X-ray diffraction (XRD) and Transmission electron microscopy (TEM) were used which revealed the average particle sizes to 45 nm with orthorhombic structure. Samples in pellet form were irradiated by 85 MeV carbon beam in the fluence range of 1X1010-5X1013. TL glow curves of the irradiated samples show two prominent glow peaks at around 460 K and 495 K. The TL response is linear up to 1X1013 fluence after which saturation was observed. The wider linear TL response of nanocrystalline BaSO4: Eu and low fading make it a superior candidate as a dosimeter to be used for detecting the doses of carbon beam.

Keywords: radiation, dosimetry, carbon ions, thermoluminescence

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Authors: Ubeyd Toçoğlu, Miraç Alaf, Hatem Akbulut

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We present a work which was conducted in order to improve the cycle life of silicon based lithium ion battery anodes by utilizing novel composite structure. In this study, carbon coated nano sized (50-100 nm) silicon particles were embedded into Graphene/MWCNT silicon matrix to produce free standing silicon based electrodes. Also, conventional Si powder anodes were produced from Si powder slurry on copper current collectors in order to make comparison of composite and conventional anode structures. Free –standing composite anodes (binder-free) were produced via vacuum filtration from a well dispersion of Graphene, MWCNT and carbon coated silicon powders. Carbon coating process of silicon powders was carried out via microwave reaction system. The certain amount of silicon powder and glucose was mixed under ultrasonication and then coating was conducted at 200 °C for two hours in Teflon lined autoclave reaction chamber. Graphene which was used in this study was synthesized from well-known Hummers method and hydrazine reduction of graphene oxide. X-Ray diffraction analysis and RAMAN spectroscopy techniques were used for phase characterization of anodes. Scanning electron microscopy analyses were conducted for morphological characterization. The electrochemical performance tests were carried out by means of galvanostatic charge/discharge, cyclic voltammetry and electrochemical impedance spectroscopy.

Keywords: graphene, Li-Ion, MWCNT, silicon

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Authors: Kane Esien, Eadaoin McCourt, Peter Nockemann, Soveig Felton

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Magnetic ionic liquids (MILs) are a class of ionic liquid incorporating one or more magnetic atoms into the anion or cation of the ionic liquid, endowing the ionic liquid with magnetic properties alongside the existing properties of ionic liquids. MILs have applications in e.g. fluid-fluid separations, electrochemistry, and polymer chemistry. In this study three different types of Bis-Lanthanoates, that exist in different phases, have been synthesised and characterised (Ln = lanthanide): 1) imidazolium lanthanide acetate – [C4Mim]2[Ln2(OAc)8] – forms a crystalline solid at room temperature, 2) phosphonium lanthanide acetate – [P666 14]2[Ln2(OAc)8] – is in a solid glassy state, and 3) phosphonium lanthanide octanoate – [P666 14]2[Ln2(Oct)8] – is an ionic liquid. X-ray diffraction of the crystalline solid imidazolium lanthanide acetate – [C4Mim]2[Ln2(OAc)8] confirm that the Ln(III) ions form dimers, bridged by carboxyl groups, but cannot yield information about samples phosphonium lanthanide acetate – [P666 14]2[Ln2(OAc)8] (glass) and phosphonium lanthanide octanoate – [P666 14]2[Ln2(Oct)8] (ionic liquid) since these lack long-range order. SQUID magnetometry studies show that all three samples have effective magnetic moments consistent with non-interacting Ln(III) ions at room temperature but deviate from this behavior in the same way below 50 K. Through modeling the magnetic response, we are able to show that we have formed magnetic dimers, in all compounds, that are weakly antiferromagnetically interacting

Keywords: dimeric ionic liquids, interactions, SQUID, structure

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Authors: Eman A. Alghamdi, A. M. Aldhafiri

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It was found that the induce an isolated dopant close to the middle of the bandgap by occupying the Cd position in the CdTe lattice structure is an efficient factor in reducing the nonradiative recombination rate and increasing the solar efficiency. According to our laboratory results, this work has been carried out to obtain the effect of substrate temperature on the CdTe0.6Sn0.4 prepared by thermal evaporation technique for photovoltaic application. Various substrate temperature (25°C, 100°C, 150°C, 200°C, 250°C and 300°C) was applied. Sn-doped CdTe thin films on a glass substrate at a different substrate temperature were made using CdTe and SnTe powders by the thermal evaporation technique. The structural properties of the prepared samples were determined using Raman, x-Ray Diffraction. Spectroscopic ellipsometry and spectrophotometric measurements were conducted to extract the optical constants as a function of substrate temperature. The structural properties of the grown films show hexagonal and cubic mixed structures and phase change has been reported. Scanning electron microscopy (SEM) reviled that a homogenous with a bigger grain size was obtained at 250°C substrate temperature. The conductivity measurements were recorded as a function of substrate temperatures. The open-circuit voltage was improved by controlling the substrate temperature due to the improvement of the fundamental material issues such as recombination and low carrier concentration. All the result was explained and discussed on the biases of the influences of the Sn dopant and the substrate temperature on the structural, optical and photovoltaic characteristics.

Keywords: CdTe, conductivity, photovoltaic, ellipsometry

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Authors: Michael Regev, Shai Essel, Alexander Katz-Demyanetz

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Magnesium alloys are characterized by good physical properties: They exhibit high strength, are lightweight and have good damping absorption and good thermal and electrical conductivity. Amorphous magnesium alloys, moreover, exhibit higher strength, hardness and a large elastic domain in addition to having excellent corrosion resistance. These above-mentioned advantages make magnesium based metallic glasses attractive for industrial use. Among the various existing magnesium alloys, Mg₆₅Cu₂₅Y₁₀ alloy is known to be one of the best glass formers. In the current study, Mg₆₅Cu₂₅Y₁₀ ribbons were produced by melt spinning, their microstructure was investigated in its as-cast condition, after pressing under 0.5 GPa for 5 minutes under different temperatures - RT, 500C, 1000C, 1500C and 2000C - and after five minute exposure to the above temperatures without pressing. The microstructure was characterized by means of X-ray Diffraction (XRD), Differential Scanning Calorimetry (DSC), High Resolution Scanning Electron Microscope (HRSEM) and High Resolution Transmission Electron Microscopy (HRTEM). XRD and DSC studies showed that the as-cast material had an amorphous character and that the material crystallized during exposure to temperature with or without applying stress. HRTEM revealed that the as-cast Mg65Cu25Y10, although known to be one of the best glass formers, is nano-crystalline rather than amorphous. The current study casts light on the question what an amorphous alloy is and whether there is any clear borderline between amorphous and nano-crystalline alloys.

Keywords: metallic glass, magnesium, melt spinning, amorphous alloys

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Authors: Akshita Jindal, Renu Chadha, Maninder Karan

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Supramolecular chemistry has gained recent eminence in a flurry of research documents demonstrating the formation of new crystalline forms with potentially advantageous characteristics. Mesalamine (5-amino salicylic acid) belongs to anti-inflammatory class of drugs, is used to treat ulcerative colitis and Crohn’s disease. Unfortunately, mesalamine suffer from poor solubility and therefore very low bioavailability. This work is focused on preparation and characterization of cocrystal of mesalamine with nicotinamide (MNIC) a coformer of GRAS status. Cocrystallisation was achieved by solvent drop grinding in stoichiometric ratio of 1:1 using acetonitrile as solvent and was characterized by various techniques including DSC (Differential Scanning Calorimetry), PXRD (X-ray Powder Diffraction), and FTIR (Fourier Transform Infrared Spectrometer). The co-crystal depicted single endothermic transitions (254°C) which were different from the melting peaks of both drug (288°C) and coformer (128°C) indicating the formation of a new solid phase. Different XRPD patterns and FTIR spectrums for the co-crystals from those of individual components confirms the formation of new phase. Enhancement in apparent solubility study and intrinsic dissolution study showed effectiveness of this cocrystal. Further improvement in pharmacokinetic profile has also been observed with 2 folds increase in bioavailability. To conclude, our results show that application of nicotinamide as a coformer is a viable approach towards the preparation of cocrystals of potential drug molecule having limited solubility.

Keywords: cocrystal, mesalamine, nicotinamide, solvent drop grinding

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Authors: Khamael M. Abualnaja, Lidija Šiller, Ben R. Horrocks

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Surface enhanced Raman spectroscopy (SERS) of Silicon nano crystals (SiNCs) were obtained using two different laser excitations: 488 nm and 514.5 nm. Silver nano particles were used as plasmonics metal nano particles due to a robust SERS effect that observed when they mixed with SiNCs. SiNCs have been characterized by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). It is found that the SiNCs are crystalline with an average diameter of 65 nm and FCC lattice. Silver nano particles (AgNPs) of two different sizes were synthesized using photo chemical reduction of AgNO3 with sodium dodecyl sulfate (SDS). The synthesized AgNPs have a polycrystalline structure with an average particle diameter of 100 nm and 30 nm, respectively. A significant enhancement in the SERS intensity was observed for AgNPs100/SiNCs and AgNPs30/SiNCs mixtures increasing up to 9 and 3 times respectively using 488 nm intensity; whereas the intensity of the SERS signal increased up to 7 and 2 times respectively, using 514.5 nm excitation source. The enhancement in SERS intensities occurs as a result of the coupling between the excitation laser light and the plasmon bands of AgNPs; thus this intense field at AgNPs surface couples strongly to SiNCs. The results provide good consensus between the wavelength of the laser excitation source and surface plasmon resonance absorption band of silver nano particles consider to be an important requirement in SERS experiments.

Keywords: silicon nanocrystals (SiNCs), silver nanoparticles (AgNPs), surface enhanced raman spectroscopy (SERS)

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Authors: Lin Huang, Bo Wang, Armando Borgna

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Dehydration of glycerol to acrolein was conducted with solid acid catalysts in liquid phase in a batch reactor and in gas phase in a fix-bed reactor, respectively. In the liquid-phase reaction, ZSM-5, H3PO4-modified ZSM-5 and heteropolyacids including H3PW12O40•xH2O (HPW) and Cs2.5H0.5PW12O40 (CsPW) were studied as catalysts. High temperatures and high boiling point solvents such as sulfolane improved the selectivity to acrolein through suppressing the formation of polyglycerols and coke. Catalytic results and temperature-programmed desorption of ammonia showed that the yield of acrolein increased with increasing catalyst acidity within the range of weak acid strength. Weak acid sites favored the selectivity to acrolein whereas strong acid sites promoted the formation of coke. ZSM-5 possessing only acid sites led to a high acrolein yield, while heteropolyacid catalysts with strong acid sites produced a low acrolein yield. In the gas-phase reaction, HPW and CsPW supported on metal oxides such as SiO2, γ-Al2O3, SiO2-Al2O3, ZrO2 and silicate TUD-1 were studied as catalysts. HPW/TUD-1 was most active for the production of acrolein, followed by HPW/SiO2. An acrolein yield of 61 % was obtained over HPW/TUD-1. X-ray diffraction study suggested that HPW and CsPW were stable and more dispersed on SiO2, silicate TUD-1 and SiO2-Al2O3. It was found that the structures of HPW and CsPW were destroyed by interaction with γ-Al2O3 and ZrO2. Compared to CsPW/TUD-1, the higher acrolein yield with HPW/TUD-1 may be attributed to more Brønsted acid sites on HPW/TUD-1, based on preliminary pyridine adsorption IR study.

Keywords: dehydration, glycerol, acrolein, solid acid catalysts, gas-phase, liquid-phase

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Authors: Chongtham Jiten, Radhapiyari Laishram, K. Chandramani Singh

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Alkaline niobate (Na_0.5K_0.5)NbO₃ ceramic system has attracted major attention in view of its potential for replacing the highly toxic but superior lead zirconate titanate (PZT) system for piezoelectric applications. Recently, a more detailed study of this system reveals that the ferroelectric and piezoelectric properties are optimized in the Li- and V-modified system having the composition (K_0.485Na_0.5Li_0.015)(Nb_0.98V_0.02)O₃. In the present work, we further study the pyroelectric behaviour of this composition along with another doped with Mn⁴⁺. So, (K_0.485Na_0.5Li_0.015)(Nb_0.98V_0.02)O₃ + x MnO₂ (x = 0, and 0.01 wt. %) ceramic compositions were synthesized by conventional ceramic processing route. X-ray diffraction study reveals that both the undoped and Mn⁴⁺-doped ceramic samples prepared crystallize into a perovskite structure having orthorhombic symmetry. Dielectric study indicates that Mn⁴⁺ doping has little effect on both the Curie temperature (T_c) and tetragonal-orthorhombic phase transition temperature (T_ot). The bulk density, room-temperature dielectric constant (ε_RT), and room-c The room-temperature coercive field (E_c) is observed to be lower in Mn⁴⁺ doped sample. The detailed analysis of the P-E hysteresis loops over the range of temperature from about room temperature to T_ot points out that enhanced ferroelectric properties exist in this temperature range with better thermal stability for the Mn⁴⁺ doped ceramic. The study reveals that small traces of Mn⁴⁺ can modify (K_0.485Na_0.5Li_0.015)(Nb_0.98V_0.02)O₃ system so as to improve its ferroelectric properties with good thermal stability over a wide range of temperature.

Keywords: ceramics, dielectric properties, ferroelectric properties, lead-free, sintering, thermal stability

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Authors: Ki-Ho Nam, Haksoo Han

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Tetrapod zinc oxide whiskers (TZnO-Ws) were successfully synthesized by a thermal oxidation method. A series of transparent polyimide (PI)/TZnO-W composites were successfully synthesized via a solution-blending method. The structural and morphological features of TZnO-Ws and PI/TZnO-W composites were characterized by Fourier transform infrared spectroscopy (FT-IR), wide-angle X-Ray diffraction (WAXD), and field emission scanning electron microscope (FE-SEM). Dynamic stress behaviors were investigated in-situ during thermal imidization of the soft-baked PI/TZnO-W composite precursor and thermally cured composite films using a thin film stress analyzer (TFSA) by wafer bending technique. The PI/TZnO-W composite films exhibited an optical transparency greater than 80% at 550 nm (≤ 0.5 wt% TZnO-W content), a low coefficient of thermal expansion (CTE), and enhanced glass transition temperature. However, the thermal decomposition temperature decreased as the TZnO-W content increased. The water diffusion coefficient and water uptake of the PI/TZNO-W composite films were obtained by best fits to a Fickian diffusion model. The water resistance capacity of PI was greatly enhanced and moisture diffusion in the pure PI was retarded by incorporating the TZnO-W. The PI composite films based on TZNO-W resultantly may have potential applications in optoelectronic manufacturing processes as a flexible transparent substrate.

Keywords: polyimide (PI), tetrapod ZnO whisker (TZnO-W), transparent, dynamic stress behavior, water resistance

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Authors: H. K. G. K. D. K. Hapuhinna, R. D. Gunaratne, H. M. J. C. Pitawala

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Hydroxyapatite is a bioceramic which can be used for applications in orthopedics and dentistry due to its structural similarity with the mineral phase of mammalian bones and teeth. In this study, it was synthesized, chemically changing natural Eppawala chloroapatite mineral as a value-added product. Sol-gel approach and solid state sintering were used to synthesize products using diluted nitric acid, ethanol and calcium hydroxide under different conditions. Synthesized Eppawala hydroxyapatite powder was characterized using X-ray Fluorescence (XRF), X-ray Powder Diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) in order to find out its composition, crystallinity, presence of functional groups, bonding type, surface morphology, microstructural features, and thermal dependence and stability, respectively. The XRD results reflected the formation of a hexagonal crystal structure of hydroxyapatite. Elementary composition and microstructural features of products were discussed based on the XRF and SEM results of the synthesized hydroxyapatite powder. TGA and DSC results of synthesized products showed high thermal stability and good material stability in nature. Also, FTIR spectroscopy results confirmed the formation of hydroxyapatite from apatite via the presence of hydroxyl groups. Those results coincided with the FTIR results of mammalian bones including human bones. The study concludes that there is a possibility of producing hydroxyapatite using commercially available Eppawala chloroapatite in Sri Lanka.

Keywords: dentistry, Eppawala chlorapatite, hydroxyapatite, orthopedics

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Authors: Tal Remez, Or Litany, Alex Bronstein

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The pursuit of smaller pixel sizes at ever increasing resolution in digital image sensors is mainly driven by the stringent price and form-factor requirements of sensors and optics in the cellular phone market. Recently, Eric Fossum proposed a novel concept of an image sensor with dense sub-diffraction limit one-bit pixels (jots), which can be considered a digital emulation of silver halide photographic film. This idea has been recently embodied as the EPFL Gigavision camera. A major bottleneck in the design of such sensors is the image reconstruction process, producing a continuous high dynamic range image from oversampled binary measurements. The extreme quantization of the Poisson statistics is incompatible with the assumptions of most standard image processing and enhancement frameworks. The recently proposed maximum-likelihood (ML) approach addresses this difficulty, but suffers from image artifacts and has impractically high computational complexity. In this work, we study a variant of a sensor with binary threshold pixels and propose a reconstruction algorithm combining an ML data fitting term with a sparse synthesis prior. We also show an efficient hardware-friendly real-time approximation of this inverse operator. Promising results are shown on synthetic data as well as on HDR data emulated using multiple exposures of a regular CMOS sensor.

Keywords: binary pixels, maximum likelihood, neural networks, sparse coding

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Authors: Ayoub Bouazza, Ali Faddouli, Said Amal, Rachid Benhida, Khaoula Khaless

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Brine waste generated from reverse osmosis (RO) desalination plants contains various valuable compounds, mainly salts, trace elements, and organic matter. These wastes are up to two times saltier than standard seawater. Therefore, there is a strong economic interest in recovering these salts. The current practice in desalination plants is to reject the brine back to the sea, which affects the marine ecosystem and the environment. Our study aims to bring forth a reliable management solution for the valorisation of waste brines. Natural evaporation, isothermal evaporation at 25°C and 50°C, and evaporation using continuous heating were used to crystallize valuable salts from a reverse osmosis desalination plant brine located on the Moroccan Atlantic coast. The crystallization sequence of the brine was studied in comparison with standard seawater. The X-Ray Diffraction (XRD) of the precipitated solid phases showed similar results, where halite was the main solid phase precipitated from both the brine and seawater. However, Jänecke diagram prediction, along with FREZCHEM simulations, showed that Kainite should crystallize before Epsomite and Carnallite. As the absence of kainite formation in many experiments in the literature has been related to the metastability of kainite and the critical relative humidity conditions, and the precipitation of K–Mg salts is very sensitive to climatic conditions. An evaporation process is proposed as a solution to achieve the predicted crystallization path and to affirm the recovery of Kainite.

Keywords: salts crystallization, reverse osmosis, solar evaporation, frezchem, ZLD

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Authors: Christian C. Vaso, Rinlee Butch M. Cervera

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Solid oxide electrolysis cell (SOEC) is a promising technology for hydrogen production that will contribute to the sustainable energy of the future. An important component of this SOEC is the anode material and one of the promising anode material for such application is the Sr-doped LaMnO3 (LSM) and Yttrium-stabilized ZrO2 (YSZ) composite material. In this study, LSM/YSZ with different weight percent compositions of LSM and YSZ were synthesized using solid-state reaction method. The obtained samples, 60LSM/40YSZ, 50LSM/50YSZ, and 40LSM/60YSZ, were fully characterized for its microstructure using X-ray diffraction, FTIR, and SEM/EDS. EDS analysis confirmed the elemental composition and distribution of the synthesized samples. Surface morphology of the sample using SEM exhibited a well sintered and densified samples and revealed a beveled cube-like LSM morphology while the YSZ phase appeared to have a sphere-like microstructure. Density measurements using Archimedes principle showed relative densities greater than 90%. In addition, AC impedance measurement of the synthesized samples have been investigated at intermediate temperature range (400-700 °C) in an inert and oxygen gas flow environment. At pure states, LSM exhibited a high electronic conductivity while YSZ demonstrated an ionic conductivity of 3.25 x 10-4 S/cm at 700 °C under Oxygen gas environment with calculated activation energy of 0.85eV. The composite samples were also studied and revealed that as the YSZ content of the composite electrode increases, the total conductivity decreases.

Keywords: ceramic composites, fuel cells, strontium lanthanum manganite, yttria partially-stabilized zirconia

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Authors: Samadhan S. Nagane, Sachin S. Kuhire, Prakash P. Wadgaonkar

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Lignocellulose-derived chemicals such as furfural, furandicarboxylic acid, syringol, guaiacol, etc are highly attractive as sustainable alternatives to petrochemicals for the synthesis of monomers and polymers. We wish to report herein the facile synthesis of fully bio-based bisphenols containing pendant furyl group by base-catalyzed condensation of furfural with guaiacol. Bisphenols possessing pendant furyl group represent valuable monomers for the synthesis of a range of polymers which include epoxy resins, polyesters, polycarbonates, poly(aryl ether)s, etc. Several new homo/co-poly(arylene ether sulfone)s have been prepared by the reaction of 4,4(-fluorodiphenyl sulfone (FDS) with 4,4'-(furan-2-ylmethylene)bis(2-methoxyphenol) (BPF) and 4,4(-isopropylidenediphenol (BPA) using different molar ratios of bisphenols. Poly(arylene ether sulfone)s showed inherent viscosities in the range 0.92-1.47 dLg-1 and number average molecular weights (Mn), obtained from gel permeation chromatography (GPC), were in the range 91,300 – 1,31,000. Poly(arylene ether sulfone)s could be cast into tough, transparent and flexible films from chloroform solutions. X-Ray diffraction studies indicated amorphous nature of poly(arylene ether sulfone)s. Poly(arylene ether sulfone)s showed Tg values in the range 179-191 oC. Additionally, the pendant furyl groups in poly(arylene ether sulfone)s provide reactive sites for chemical modifications and cross-linking via Diels-Alder reaction with maleimides and bismaleimides, respectively.

Keywords: bio-based, bisphenols, Diels-Alder reaction, poly(arylene ether sulfone)s

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Authors: Surendra Kumar Gautam, Mahesh Dhungana

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Magnesium oxide nanoparticles (MgO NPs) are less toxic to humans and the environment as compared to other metal oxide nanoparticles. Various conventional chemical and physical methods are used for synthesis whose toxicity level is high and highly expensive. As the best alternative, phyto-assisted synthesis has emerged, which uses extracts from plant parts for the synthesis of nanoparticles. Here, we report the synthesis of MgO nanoparticles with the assistance of beetroot extract and leaf extract of P. guajava and A. adenophora. The synthesized MgO NPs were characterized by X-ray diffraction (XRD), Fourier transforms infrared spectroscopy (FTIR), and UV-visible spectroscopy. X-ray analysis for the broadening of peaks was used to evaluate the crystallite size and lattice strain using Debye-Scherer and Williamson–Hall method. The results of crystallite size obtained by both methods are in close proximity. The crystallite size obtained by the Williamson-Hall method seems more accurate, with values being 8.1 nm and 13.2 nm for beetroot MgO NPs and P. guajava MgO NPs, respectively. The FT-IR spectroscopy revealed the dominance of chemical bonds as well as functional groups on MgO NPs surfaces. The UV-visible absorption spectra of MgO NPs were found to be 310 nm, 315 nm, and 315 nm for beetroot, P. guajava, and A. adenophora leaf extract, respectively. Among the three samples, beetroot-mediated MgO NPs were effective antibacterial against both gram-positive and Gram-negative bacteria. In addition, synthesized MgO NPs also show significant antioxidant efficacy against 1,1-diphenyl-2-picrylhydrazyl radical. Further, beetroot MgO NPs showed the highest photocatalytic activity of about 91% in comparison with other samples.

Keywords: MgO NPs, XRD, FTIR, antibacterial, antioxidant and photocatalytic activity

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Authors: Shaya Mahmoudian, Mohammad Reza Sazegar, Nazanin Afshari

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Graphene, a single layer of carbon atoms in a hexagonal lattice, has recently attracted great attention due to its unique mechanical, thermal and electrical properties. The high aspect ratio and unique surface features of graphene resulted in significant improvements of the nano composites properties. In this study, nano composite fibres made of cellulose and graphene nano platelets were wet spun from solution by using ionic liquid, 1-ethyl-3-methylimidazolium acetate (EMIMAc) as solvent. The effect of graphene loading on the thermal and electrical properties of the nanocomposite fibres was investigated. The nano composite fibres characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis. XRD analysis revealed a cellulose II crystalline structure for regenerated cellulose and the nano composite fibres. SEM images showed a homogenous morphology and round cross section for the nano composite fibres along with well dispersion of graphene nano platelets in regenerated cellulose matrix. The incorporation of graphene into cellulose matrix generated electrical conductivity. At 6 wt. % of graphene, the electrical conductivity was 4.7 × 10-4 S/cm. The nano composite fibres also showed considerable improvements in thermal stability and char yield compared to pure regenerated cellulose fibres. This work provides a facile and environmentally friendly method of preparing nano composite fibres based on cellulose and graphene nano platelets that can find several applications in cellulose-based carbon fibres, conductive fibres, apparel, etc.

Keywords: nanocomposite, graphene nanoplatelets, regenerated cellulose, electrical properties

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Authors: Amit Kumar, Davide Lionetti, Victor Day, James Blakemore

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Capture and activation of the water-soluble uranyl dication (UO22+) remains a challenging problem, as few rational approaches are available for modulating the reactivity of this species. Here, we report the divergent synthesis of heterobimetallic complexes in which UO22+ is held in close proximity to a range of redox-inactive metals by tailored macrocyclic ligands. Crystallographic and spectroscopic studies confirm assembly of homologous UVI(μ-OAr)2Mn+ cores with a range of mono-, di-, and trivalent Lewis acids (Mn+). X-ray diffraction (XRD) and cyclic voltammetry (CV) data suggest preferential binding of K+ in an 18-crown-6-like cavity and Na+ in a 15-crown-5-like cavity, both appended to Schiff-base type sites that selectively bind UO22+. CV data demonstrate that the UVI/UV reduction potential in these complexes shifts positive and the rate of electron transfer decreases with increasing Lewis acidity of the incorporated redox-inactive metals. Moreover, spectroelectrochemical studies confirm the formation of [UV] species in the case of monometallic UO22+ complex, consistent with results from prior studies. However, unique features were observed during spectroelectrochemical studies in the presence of the K+ ion, suggesting new insights into electronic structure may be accessible with the heterobimetallic complexes. Overall, these findings suggest that interactions with Lewis acids could be effectively leveraged for rational tuning of the electronic and thermochemical properties of the 5f elements, reminiscent of strategies more commonly employed with 3d transition metals.

Keywords: electrochemistry, Lewis acid, macrocycle, uranyl

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Authors: N. G. Margiani, I. G. Kvartskhava, G. A. Mumladze, Z. A. Adamia

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Chemical doping with different elements and compounds at various amounts represents the most suitable approach to improve the superconducting properties of bismuth-based superconductors for technological applications. In this paper, the influence of partial substitution of Sr(BO₂)₂ for SrO on the phase formation kinetics and transport properties of (Bi,Pb)-2223 HTS has been studied for the first time. Samples with nominal composition Bi_1.7Pb_0.3Sr_2-xCa₂Cu₃O_y[Sr(BO₂)₂]_x, x=0, 0.0375, 0.075, 0.15, 0.25, were prepared by the standard solid state processing. The appropriate mixtures were calcined at 845 ^oC for 40 h. The resulting materials were pressed into pellets and annealed at 837 ^oC for 30 h in air. Superconducting properties of undoped (reference) and Sr(BO₂)₂-doped (Bi,Pb)-2223 compounds were investigated through X-ray diffraction (XRD), resistivity (ρ) and transport critical current density (J_c) measurements. The surface morphology changes in the prepared samples were examined by scanning electron microscope (SEM). XRD and J_c studies have shown that the low level Sr(BO₂)₂ doping (x=0.0375-0.075) to the Sr-site promotes the formation of high-T_c phase and leads to the enhancement of current carrying capacity in (Bi,Pb)-2223 HTS. The doped sample with x=0.0375 has the best performance compared to other prepared samples. The estimated volume fraction of (Bi,Pb)-2223 phase increases from ~25 % for reference specimen to ~70 % for x=0.0375. Moreover, strong increase in the self-field J_c value was observed for this dopant amount (J_c=340 A/cm²), compared to an undoped sample (J_c=110 A/cm²). Pronounced enhancement of superconducting properties of (Bi,Pb)-2223 superconductor can be attributed to the acceleration of high-T_c phase formation as well as the improvement of inter-grain connectivity by small amounts of Sr(BO₂)₂ dopant.

Keywords: bismuth-based superconductor, critical current density, phase formation, Sr(BO₂)₂ doping

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Authors: Padmalochan Panda, R. Ramaseshan

Abstract:

Aluminum nitride (AlN) is a potential candidate for semiconductor industry due to its wide band gap (6.2 eV), high thermal conductivity and low thermal coefficient of expansion. A-plane oriented AlN film finds an important role in deep UV-LED with higher isotropic light extraction efficiency. Also, Cr-doped AlN films exhibit dilute magnetic semiconductor property with high Curie temperature (300 K), and thus compatible with modern day microelectronics. In this work, highly a-axis oriented wurtzite AlN and Al1-xMxN (M = Cr, Ti) films have synthesized by reactive co-sputtering technique at different concentration. Crystal structure of these films is studied by Grazing incidence X-ray diffraction (GIXRD) and Transmission electron microscopy (TEM). Identification of binding energy and concentration (x) in these films is carried out by X-ray photoelectron spectroscopy (XPS). Local crystal structure around the Cr and Ti atom of these films are investigated by X-ray absorption spectroscopy (XAS). It is found that Cr and Ti replace the Al atom in AlN lattice and the bond lengths in first and second coordination sphere with N and Al, respectively, decrease concerning doping concentration due to strong p-d hybridization. The nano-indentation hardness of Cr and Ti-doped AlN films seems to increase from 17.5 GPa (AlN) to around 23 and 27.5 GPa, respectively. An-isotropic optical properties of these films are studied by the Spectroscopic Ellipsometry technique. Refractive index and extinction coefficient of these films are enhanced in normal dispersion region as compared to the parent AlN film. The optical band gap energies also seem to vary between deep UV to UV regions with the addition of Cr, thus by bringing out the usefulness of these films in the area of optoelectronic device applications.

Keywords: ellipsometry, GIXRD, hardness, XAS

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Authors: Sara Mercedes Barroso Pinzón, Antonio Javier Sanchéz Herencia, Begoña Ferrari, Álvaro Jesús Castro

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The current need for durable implants and bone substitutes characterised by biocompatibility, bioactivity and mechanical properties, without immunological rejection, is a major challenge for scientists. Hydroxyapatite (HAp) has been considered for decades as an ideal biomaterial for bone regeneration due to its chemical and crystallographic similarity to the mineral structure bioapatites. However, the lack of trace elements in the hydroxyapatite structure gives it very low mechanical and biological properties. In this sense, the objective of the research is to address the synthesis of hydroxyapatite with Mg from phosphate rock from sedimentary deposits in the central-eastern region of Colombia, taking advantage of the release of the species contained as natural precursors of Ca, P and Mg. The minerals present were studied, fluorapatite as the mineral of interest associated with mineralogical species of magnesium carbonates and quartz. The chemical and mineralogical composition was determined by X-ray fluorescence (XRF) and X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX); as well as the evaluation of the surface physicochemical properties of zeta potential (PZC), with the aim of studying the surface behaviour of the microconstituents present in the phosphate rock and to elucidate the synergistic mechanism between the minerals and establish the optimum conditions for the wet concentration process. From the products obtained and characterised by XRD, XRF, SEM, FTIR, RAMAN, HAp-Mg biocomposite scaffolds are fabricated and the influence of Mg on the morphometric parameters, mechanical and biological properties of the designed materials is evaluated.

Keywords: phosphate rock, hydroxyapatite, magnesium, biomaterials

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Authors: Sajad Haghanifar, Seyed-Farshid Kashani Bozorg

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Nano-crystalline Mg2Ni-based powder was produced by mechanical alloying technique using binary and ternary powder mixtures with stoichiometric compositions of Mg2Ni, Mg1.9C0.1Ni and Mg2C0.1Ni0.9. The structures and morphologies of the milled products were studied by XRD, SEM and HRTEM. Their electrochemical hydrogen storage characteristics were investigated in 6 M KOH solution. X-Ray diffraction, scanning and transmission electron microscopy of the milled products showed the formation of Mg2Ni-based nano-crystallites after 5, 15 and 30 h of milling using the initial powder mixtures of Mg1.9C0.1Ni, Mg2Ni and Mg2C0.1Ni0.9, respectively. It was found that partial substitution of C for Mg has beneficial effect on the formation kinetic of nano-crystalline Mg2Ni. Contrary to this, partial substitution of C for Ni was resulted in retardation of formation kinetic of nano-crystalline Mg2Ni. In addition, the negative electrode made from Mg1.9C0.1Ni ternary milled product after 30 hour of milling exhibited the highest initial discharge capacity and longest discharge life. Thus, partial substitution of C for Mg is beneficial to electrode properties of the Mg2Ni-based crystallites. The relation between the discharge capacity and cycling number of mechanically alloyed products was proposed on the basis of the fact that the degradation of discharge capacity was mainly caused by the oxidation of magnesium and nickel. The experimental data fitted the deduced equation well.

Keywords: Mg2Ni, hydrogen absorbing materials, electrochemical properties, nano-crystalline, amorphous, mechanical alloying, carbon

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Authors: Houria Rezala, Jose Luis Valverde, Amaya Romero, Alessandra Molinari, Andrea Maldotti

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A pillared montmorillonite containing iron doped titania (Fe/Ti-PILC) has been prepared from a natural clay. This material has been characterized by X-ray diffraction, nitrogen adsorption, temperature programmed desorption of ammonia, inductively coupled plasma atomic emission spectroscopy, atomic absorption, and diffuse reflectance UV-VIS spectroscopy. The layer structure of Fe/Ti-PILC resulted to be ordered with an insertion of pillars, which caused a slight increase in the basal spacing of the clay. Its specific surface area was about three times larger than that of the parent Na-montmorillonite due principally to the creation of a remarkable microporous network. The doped material was a robust photocatalyst able to oxidize liquid alkyl aromatics to the corresponding carbonylic derivatives, using O2 as the oxidizing species, at mild pressure and temperature conditions. Accumulation of valuable carbonylic derivatives was possible since their over-oxidation to carbon dioxide was negligible. Fe/Ti-PILC was able to discriminate between toluene and cyclohexane in favor of the aromatic compound with an efficiency that is about three times higher than that of titanium pillared clays (Ti-PILC). It is likely that the addition of iron favored the formation of new acid sites able to interact with the aromatic substrate. Iron doping caused a significant TiO2 visible light-induced activity (wavelength > 400 nm) with only minor negative effects on its performance under UV-light irradiation (wavelength > 290 nm).

Keywords: alkyl aromatics oxidation, heterogeneous photocatalysis, iron doping, pillared clays

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Authors: B. Białecka, Z. Adamczyk, M. Cempa

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The use of ultrasounds in zeolization of fly ash can increase the efficiency of this process. The molar ratios of the reagents, as well as the time and temperature of the synthesis, are the main parameters determining the type and properties of the zeolite formed. The aim of the work was to create hydrosodalite in a short time (8h), with low NaOH concentration (3 M) and in low temperature (80°C). A zeolite material contained in fly ash from hard coal combustion in one of Polish Power Plant was subjected to hydrothermal alkaline synthesis. The phase composition of the ash consisted mainly of glass, mullite, quartz, and hematite. The dominant chemical components of the ash were SiO₂ (over 50%mas.) and Al₂O₃ (more than 28%mas.), whereas the contents of the remaining components, except Fe₂O₃ (6.34%mas.), did not exceed 4% mas. The hydrothermal synthesis of the zeolite material was carried out in the following conditions: 3M-solution of NaOH, synthesis time – 8 hours, 40 kHz-frequency ultrasounds during the first two hours of synthesis. The mineral components of the input ash as well as product after synthesis were identified in microscopic observations, in transmitted light, using X-ray diffraction (XRD) and electron scanning microscopy (SEM/EDS). The chemical composition of the input ash was identified by the method of X-ray fluorescence (XRF). The obtained material apart from phases found in the initial fly ash sample, also contained new phases, i.e., hydrosodalite and NaP-type zeolite. The chemical composition in micro areas of grains indicated their diversity: i) SiO₂ content was in the range 30-59%mas., ii) Al₂O₃ content was in the range 24-35%mas., iii) Na₂O content was in the range 6-15%mas. This clearly indicates that hydrosodalite forms hypertrophies with NaP type zeolite as well as relict grains of fly ash. A small amount of potassium in the examined grains is noteworthy, which may indicate the substitution of sodium with potassium. This is confirmed by the high value of the correlation coefficient between these two components.

Keywords: fly ash, hydrosodalite, ultrasounds, zeolite

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Authors: Bright Kwakye-Awuah, Elizabeth Von-Kiti, Isaac Nkrumah, Baah Sefa-Ntiri, Craig D. Williams

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Bauxite and kaolin from Ghana Bauxite Company mine site were used to synthesize zeolites. Bauxite served as the alumina source and kaolin the silica source. Synthesis variations include variation of aging time at constant crystallization time and variation of crystallization times at constant aging time. Characterization techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive x-ray analysis (EDX) and Fourier transform infrared spectroscopy (FTIR) were employed in the characterization of the raw samples as well as the synthesized samples. The results obtained showed that the transformations that occurred and the phase of the resulting products were coordinated by the aging time, crystallization time, alkaline concentration and Si/Al ratio of the system. Zeolites A, X, Y, analcime, Sodalite, and ZK-14 were some of the phases achieved. Zeolite LTA was achieved with short crystallization times of 3, 5, 18 and 24 hours and a maximum aging of 24 hours. Zeolite LSX was synthesized with 24 hr aging followed with 24 hr hydrothermal treatment whilst zeolite Y crystallized after 48 hr of aging and 24 hr crystallization. Prolonged crystallization time produced a mixed phased product. Prolonged aging times, on the other hand, did not yield any zeolite as the sample was amorphous. Increasing the alkaline content of the reaction mixture above 5M introduced sodalite phase in the final product. The properties of the final products were comparable to zeolites synthesized from pure chemical reagents.

Keywords: bauxite, kaolin, aging, crystallization, zeolites

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Authors: Tumelo W. P. Seadira, Thabang Ntho, Cornelius M. Masuku, Michael S. Scurrell

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A ternary Cu/TiO2/rGO photocatalysts was prepared using solvothermal method. Firstly, pure anatase TiO2 hollow spheres were prepared with titanium butoxide, ethanol, ammonium sulphate, and urea via hydrothermal method; and Cu nanoparticles were subsequently loaded on the surface of the hollow spheres by wet impregnation. During the solvothermal process, the deposition and well dispersion of Cu-TiO2 hollow spheres composites onto the graphene oxide surface, as well as the reduction of graphene oxide to graphene were achieved. The morphological and structural properties of the prepared samples were characterized by Brunauer-Emmett-Tellet (BET), X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscopy (TEM), and UV-vis DRS, and photoelectrochemical. The activities of the prepared catalysts were tested for hydrogen production via simultaneous photocatalytic water-splitting and glycerol reforming under visible light irradiation. The excellent photocatalytic activity of the Cu-TiO2-hollow-spheres/rGO catalyst was attributed the rGO which acts as both storage and transferor of electrons generated at the Cu and TiO2 heterojunction, thus increasing the electron-hole pairs separation. This paper reports the preparation of photocatalyst which is highly active by coupling reduced graphene oxide with nano-structured TiO2 with high surface area that can efficiently harvest the visible light for effective water-splitting and glycerol photocatalytic reforming in order to achieve efficient hydrogen evolution.

Keywords: glycerol reforming, hydrogen evolution, graphene oxide, Cu/TiO2-hollow-spheres/rGO

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Authors: Sanghamitra Acharya, Suwarna Datar

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Extensive use of digital and smart communication createsprolong expose of unwanted electromagnetic (EM) radiations. This harmful radiation creates not only malfunctioning of nearby electronic gadgets but also severely affects a human being. So, a suitable microwave absorbing material (MAM) becomes a necessary urge in the field of stealth and radar technology. Initially, Aluminum based hexa ferrite was prepared by sol-gel technique and for carbon derived composite was prepared by the simple one port chemical reduction method. Finally, composite films of Poly (Vinylidene) Fluoride (PVDF) are prepared by simple gel casting technique. Present work demands that aluminum-based hexaferrite phase conjugated with graphene in PVDF matrix becomes a suitable candidate both in commercially important X and Ku band. The structural and morphological nature was characterized by X-Ray diffraction (XRD), Field emission-scanning electron microscope (FESEM) and Raman spectra which conforms that 30-40 nm particles are well decorated over graphene sheet. Magnetic force microscopy (MFM) and conducting force microscopy (CFM) study further conforms the magnetic and conducting nature of composite. Finally, shielding effectiveness (SE) of the composite film was studied by using Vector network analyzer (VNA) both in X band and Ku band frequency range and found to be more than 30 dB and 40 dB, respectively. As prepared composite films are excellent microwave absorbers.

Keywords: carbon nanocomposite, microwave absorbing material, electromagnetic shielding, hexaferrite

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Authors: Tefera Worku Mekonnen, Hiseh Chih Tsai

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Enhancement of drug efficacy is essential in cancer treatment. The immune stimulator ovalbumin (Ova)-coated citric acid (AC-)-stabilized iron oxide nanoparticles (AC-IO-Ova NPs) and enhanced permeability and retention (EPR) based tumor targeted 4.5 (4.5G) poly(amidoamine) dendrimer-cisplatin nanocomplex (4.5GDP-Cis-pt NC) were used for enhanced anticancer efficiency. The formations of 4.5GDP-Cis-pt NC, AC-IO, and AC-IO-Ova NPs have been examined by FTIR, X-ray diffraction, Raman, and X-ray photoelectron spectroscopy. The conjugation of cisplatin (Cis-pt) with 4.5GDP was confirmed using carbon NMR. The tumor-specific 4.5GDP-Cis-pt NC provided ~45% and 28% cumulative cisplatin release in 72 h at pH 6.5 and 7.4, respectively. A significant immune response with high TNF-α and IL-6 cytokine secretion was confirmed when the co-incubation of AC-IO-Ova with RAW 264.7 or HaCaT cells. AC-IO-Ova NP was biocompatible in different cell lines, even at a high concentration (200 µg mL−1). In contrast, AC-IO-Ova NPs mixed with 4.5GDP-Cis-pt NC (Cis-pt at 15 µg mL−1) significantly increased the cytotoxicity against the cancer cells, which is dose-dependent on the concentration of AC-IO-Ova NPs. The increased anticancer effects may be attributed to the generation of reactive oxygen species (ROS). Moreover, the efficiency of anticancer cells may be further assisted by induction of an innate immune response via M1 macrophage polarization due to the presence of AC-IO-Ova NPs. We provide a better synergestic chemoimmunotherapeutic strategy to enhance the efficiency of anticancer of cisplatin via chemotherapeutic agent 4.5GDP-Cis-pt NC and induction of proinflammatory cytokines to stimulate innate immunity through AC-IO-Ova NPs against tumors.

Keywords: cisplatin-release, iron oxide, ovalbumin, poly(amidoamine) dendrimer

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Authors: Shefaa Mansour, Hassan Arafat, Shadi Hasan

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Management of reverse osmosis (RO) brine has become a major area of research due to the environmental concerns associated with it. This study worked on studying the feasibility of the direct contact membrane distillation (DCMD) system in the treatment of this RO brine. The system displayed great potential in terms of its flux and salt rejection, where different operating conditions such as the feed temperature, feed salinity, feed and permeate flow rates were varied. The highest flux of 16.7 LMH was reported with a salt rejection of 99.5%. Although the DCMD has displayed potential of enhanced water recovery from highly saline solutions, one of the major drawbacks associated with the operation is the fouling of the membranes which impairs the system performance. An operational run of 77 hours for the treatment of RO brine of 56,500 ppm salinity was performed in order to investigate the impact of fouling of the membrane on the overall operation of the system over long time operations. Over this time period, the flux was observed to have reduced by four times its initial flux. The fouled membrane was characterized through different techniques for the identification of the organic and inorganic foulants that have deposited on the membrane surface. The Infrared Spectroscopy method (IR) was used to identify the organic foulants where SEM images displayed the surface characteristics of the membrane. As for the inorganic foulants, they were identified using X-ray Diffraction (XRD), Ion Chromatography (IC) and Energy Dispersive Spectroscopy (EDS). The major foulants found on the surface of the membrane were inorganic salts such as sodium chloride and calcium sulfate.

Keywords: brine treatment, membrane distillation, fouling, characterization

Procedia PDF Downloads 436