Search results for: relativistic runaway electron avalanches

Authors: Neha Batra Bali, Monika Tomar, Vinay Gupta

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A reagentless biosensor for detection of urea based on ZnO-CuO composite thin film is presented in following work. Biosensors have immense potential for varied applications ranging from environmental to clinical testing, health care, and cell analysis. Immense growth in the field of biosensors is due to the huge requirement in today’s world to develop techniques which are both cost effective and accurate for prevention of disease manifestation. The human body comprises of numerous biomolecules which in their optimum levels are essential for functioning. However mismanaged levels of these biomolecules result in major health issues. Urea is one of the key biomolecules of interest. Its estimation is of paramount significance not only for healthcare sector but also from environmental perspectives. If level of urea in human blood/serum is abnormal, i.e., above or below physiological range (15-40mg/dl)), it may lead to diseases like renal failure, hepatic failure, nephritic syndrome, cachexia, urinary tract obstruction, dehydration, shock, burns and gastrointestinal, etc. Various metal nanoparticles, conducting polymer, metal oxide thin films, etc. have been exploited to act as matrix to immobilize urease to fabricate urea biosensor. Amongst them, Zinc Oxide (ZnO), a semiconductor metal oxide with a wide band gap is of immense interest as an efficient matrix in biosensors by virtue of its natural abundance, biocompatibility, good electron communication feature and high isoelectric point (9.5). In spite of being such an attractive candidate, ZnO does not possess a redox couple of its own which necessitates the use of electroactive mediators for electron transfer between the enzyme and the electrode, thereby causing hindrance in realization of integrated and implantable biosensor. In the present work, an effort has been made to fabricate a matrix based on ZnO-CuO composite prepared by pulsed laser deposition (PLD) technique in order to incorporate redox properties in ZnO matrix and to utilize the same for reagentless biosensing applications. The prepared bioelectrode Urs/(ZnO-CuO)/ITO/glass exhibits high sensitivity (70µAmM⁻¹cm⁻²) for detection of urea (5-200 mg/dl) with high stability (shelf life ˃ 10 weeks) and good selectivity (interference ˂ 4%). The enhanced sensing response obtained for composite matrix is attributed to the efficient electron exchange between ZnO-CuO matrix and immobilized enzymes, and subsequently fast transfer of generated electrons to the electrode via matrix. The response is encouraging for fabricating reagentless urea biosensor based on ZnO-CuO matrix.

Keywords: biosensor, reagentless, urea, ZnO-CuO composite

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Authors: Bouanati Sidi Mohammed, N. E. Chabane Sari, Mostefa Kara Selma

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It is well-known that Organic light emitting diodes (OLEDs) are attracting great interest in the display technology industry due to their many advantages, such as low price of manufacturing, large-area of electroluminescent display, various colors of emission included white light. Recently, there has been much progress in understanding the device physics of OLEDs and their basic operating principles. In OLEDs, Light emitting is the result of the recombination of electron and hole in light emitting layer, which are injected from cathode and anode. For improve luminescence efficiency, it is needed that hole and electron pairs exist affluently and equally and recombine swiftly in the emitting layer. The aim of this paper is to modeling polymer LED and OLED made with small molecules for studying the electrical and optical characteristics. The first simulation structures used in this paper is a mono layer device; typically consisting of the poly (2-methoxy-5(2’-ethyl) hexoxy-phenylenevinylene) (MEH-PPV) polymer sandwiched between an anode usually an indium tin oxide (ITO) substrate, and a cathode, such as Al. In the second structure we replace MEH-PPV by tris (8-hydroxyquinolinato) aluminum (Alq3). We choose MEH-PPV because of it's solubility in common organic solvents, in conjunction with a low operating voltage for light emission and relatively high conversion efficiency and Alq3 because it is one of the most important host materials used in OLEDs. In this simulation, the Poole-Frenkel- like mobility model and the Langevin bimolecular recombination model have been used as the transport and recombination mechanism. These models are enabled in ATLAS -SILVACO software. The influence of doping and thickness on I(V) characteristics and luminescence, are reported.

Keywords: organic light emitting diode, polymer lignt emitting diode, organic materials, hexoxy-phenylenevinylene

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Authors: Bertilia L. Bartley, Ledjane S. Barreto

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As a preliminary investigation on the control of microcracking in composite cement pastes, this study explores and compares the compatibility of Tetraethyl Orthosilicate (TEOS), Ethylene Glycol (EG) and Silicone Resin (SIL) in cement pastes cured at high temperature. Pastes were prepared by incorporating ordinary Portland cement (OPC) into an additive solution, using a solution/cement ratio of 0.45. Specimens were molded for 24h at 21 ± 2°C, then cured in deionized water for another 24h at 74 ± 1°C. TEOS and EG influence on fresh paste properties were similar to the reference OPC paste yet disintegration was observed in EG and SIL specimens after the first 12h of curing. X-Ray Diffraction analysis (XRD) coupled with thermogravimetric analysis (TGA/DTG) verified that SIL addition impedes portlandite formation significantly. Backscatter Scanning Electron Microscopy (SEM) techniques were therefore performed on selected areas of each sample to investigate the morphology of the hydration products detected. Various morphologies of portlandite crystals were observed in pastes with EG and TEOS addition, as well as dense morphologies of calcium silicate hydrate (C-S-H) gel and fibers, and ettringite needles. However, the formation of portlandite aggregate and clusters of C-S-H was highly favored by TEOS addition. Furthermore, the microstructural details of composite pastes were clearly visible at low magnifications i.e. 500x, as compared to the OPC paste. The results demonstrate accelerated hydration within composite pastes, a uniform distribution of hydration products, as well as an adhesive interaction with the products and polymer additive. Overall, TEOS demonstrated the most favorable influence, which indicates the potential of TEOS as a compatible polymer additive within the cement system at high temperature.

Keywords: accelerated curing, cement/polymer composite, hydration, microstructural properties, morphology, portlandite, scanning electron microscopy (sem)

Procedia PDF Downloads 182

Authors: Fatai O. Oladoyinbo, Felix O. Sanni, Akinwunmi Fatai, Kamoli A. Amusa, Saheed A. Ganiyu, Wasiu B. Ayinde, Tajudeen A. Afolabi, Enock O. Dare

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Silver (Ag) and silica (SiO2) nanoparticles were synthesized using the chemical reduction method from silver nitrate and sodium silicate, respectively. X-ray Diffraction (XRD), High-Resolution Transmission Electron Microscopy (HRTEM), Scanning Electron Microscopy (SEM), Uv-Visible spectroscopy, Energy Dispersive X-ray (EDX) spectroscopy and N2 adsorption-desorption techniques were utilized to characterize the composition and structure of the samples. The crystallinity pattern of Ag nanoparticles was indexed as (111), (200), (220) and (311), which allowed reflections from face-centered cubic silver. XRD of SiO2 showed good porosity with a broad-spectrum band at Bragg’s angle 2θ of 22° while that of Ag-SiO2 showed distinct peaks at 2θ values of 39°, 43°, 66° and 79°. The XRD result agreed perfectly with the SEM and HRTEM images which showed Ag-SiO2 isotropic and anisotropic under the varying concentration of reactants. The elemental composition of Ag-SiO2, as displayed by EDX, confirmed Ag enrichment in the Ag-SiO2 heterostructure. The Uv-Visible peak at 421 nm confirmed the Surface Plasmon Resonance absorption peak of silver nanoparticles. N2 adsorption-desorption result showed a broad band of Ag-SiO2 from 3 to 8 nm, which indicated relatively narrow pore size distributions. Humidity sensing measurements performed in a controlled humidity chamber showed very high sensitivity with a sensitivity factor (SF) of 4.63 and high linearity with a steady decrease in resistance to humidity from 880 Ω at 10% RH to 190 Ω at 100% RH, indicating that Ag-SiO2 nanocomposite is a good sensing material with high sensitivity and linearity.

Keywords: silver, silica, nanocomposite, synthesis, heterostructure, core shell

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Authors: Songyan Yin, Ravindra Rajarao, Veena Sahajwalla

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Automotive plastics waste (widely known as auto-fluff or ASR) is a complicated mixture of various plastics incorporated with a wide range of additives and fillers like titanium dioxide, magnesium oxide, and silicon dioxide. Automotive plastics waste is difficult to recycle and its landfilling poses the significant threat to the environment. In this study, a sustainable technology to fabricate protective nanoscale TiN thin film on a steel substrate surface by using automotive waste plastics as titanium and carbon resources is suggested. When heated automotive plastics waste with steel at elevated temperature in a nitrogen atmosphere, titanium dioxide contented in ASR undergo carbothermal reduction and nitridation reactions on the surface of the steel substrate forming a nanoscale thin film of titanium nitride on the steel surface. The synthesis of TiN film on steel substrate under this technology was confirmed by X-ray photoelectron spectrometer, high resolution X-ray diffraction, field emission scanning electron microscope, a high resolution transmission electron microscope fitted with energy dispersive X-ray spectroscopy, and inductively coupled plasma mass spectrometry techniques. This sustainably fabricated TiN film was verified of dense, well crystallized and could provide good oxidation resistance to the steel substrate. This sustainable fabrication technology is maneuverable, reproducible and of great economic and environmental benefit. It not only reduces the fabrication cost of TiN coating on steel surface, but also provides a sustainable environmental solution to recycling automotive plastics waste. Moreover, high value copper droplets and char residues were also extracted from this unique fabrication process.

Keywords: automotive plastics waste, carbonthermal reduction and nitirdation, sustainable, TiN film

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Authors: M. Kowalik, J. Masternak, K. Kazimierczuk, O. V. Khavryuchenko, B. Kupcewicz, B. Barszcz

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Recently, the growing interest of chemists in metal-organic coordination polymers (MOCPs) is primarily derived from their intriguing structures and potential applications in catalysis, gas storage, molecular sensing, ion exchanges, nonlinear optics, luminescence, etc. Currently, we are devoting considerable effort to finding the proper method of synthesizing new coordination polymers containing S- or N-heteroaromatic carboxylates as linkers and characterizing the obtained Pb(II) compounds according to their structural diversity, luminescence, and thermal properties. The choice of Pb(II) as the central ion of MOCPs was motivated by several reasons mentioned in the literature: i) a large ionic radius allowing for a wide range of coordination numbers, ii) the stereoactivity of the 6s2 lone electron pair leading to a hemidirected or holodirected geometry, iii) a flexible coordination environment, and iv) the possibility to form secondary bonds and unusual non-covalent interactions, such as classic hydrogen bonds and π···π stacking interactions, as well as nonconventional hydrogen bonds and rarely reported tetrel bonds, Pb(lone pair)···π interactions, C–H···Pb agostic-type interactions or hydrogen bonds, and chelate ring stacking interactions. Moreover, the construction of coordination polymers requires the selection of proper ligands acting as linkers, because we are looking for materials exhibiting different network topologies and fluorescence properties, which point to potential applications. The reaction of Pb(NO₃)₂ with 1H-pyrrole-2-carboxylic acid (2prCOOH) leads to the formation of a new four-nuclear Pb(II) polymer, [Pb4(2prCOO)₈(H₂O)]ₙ, which has been characterized by CHN, FT-IR, TG, PL and single-crystal X-ray diffraction methods. In view of the primary Pb–O bonds, Pb1 and Pb2 show hemidirected pentagonal pyramidal geometries, while Pb2 and Pb4 display hemidirected octahedral geometries. The topology of the strongest Pb–O bonds was determined as the (4·8²) fes topology. Taking the secondary Pb–O bonds into account, the coordination number of Pb centres increased, Pb1 exhibited a hemidirected monocapped pentagonal pyramidal geometry, Pb2 and Pb4 exhibited a holodirected tricapped trigonal prismatic geometry, and Pb3 exhibited a holodirected bicapped trigonal prismatic geometry. Moreover, the Pb(II) lone pair stereoactivity was confirmed by DFT calculations. The 2D structure was expanded into 3D by the existence of non-covalent O/C–H···π and Pb···π interactions, which was confirmed by the Hirshfeld surface analysis. The above mentioned interactions improve the rigidity of the structure and facilitate the charge and energy transfer between metal centres, making the polymer a promising luminescent compound.

Keywords: coordination polymers, fluorescence properties, lead(II), lone electron pair stereoactivity, non-covalent interactions

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Authors: Zheng Wang, Zhenhong Li, Jon Mills

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Ground-based synthetic aperture radar (GBSAR) represents a powerful remote sensing tool for deformation monitoring towards various geohazards, e.g. landslides, mudflows, avalanches, infrastructure failures, and the subsidence of residential areas. Unlike spaceborne SAR with a fixed revisit period, GBSAR data can be acquired with an adjustable temporal resolution through either continuous or discontinuous operation. However, challenges arise from processing high temporal-resolution continuous GBSAR data, including the extreme cost of computational random-access-memory (RAM), the delay of displacement maps, and the loss of temporal evolution. Moreover, repositioning errors between discontinuous campaigns impede the accurate measurement of surface displacements. Therefore, a versatile package with two complete chains is developed in this study in order to process both continuous and discontinuous GBSAR data and address the aforementioned issues. The first chain is based on a small-baseline subset concept and it processes continuous GBSAR images unit by unit. Images within a window form a basic unit. By taking this strategy, the RAM requirement is reduced to only one unit of images and the chain can theoretically process an infinite number of images. The evolution of surface displacements can be detected as it keeps temporarily-coherent pixels which are present only in some certain units but not in the whole observation period. The chain supports real-time processing of the continuous data and the delay of creating displacement maps can be shortened without waiting for the entire dataset. The other chain aims to measure deformation between discontinuous campaigns. Temporal averaging is carried out on a stack of images in a single campaign in order to improve the signal-to-noise ratio of discontinuous data and minimise the loss of coherence. The temporal-averaged images are then processed by a particular interferometry procedure integrated with advanced interferometric SAR algorithms such as robust coherence estimation, non-local filtering, and selection of partially-coherent pixels. Experiments are conducted using both synthetic and real-world GBSAR data. Displacement time series at the level of a few sub-millimetres are achieved in several applications (e.g. a coastal cliff, a sand dune, a bridge, and a residential area), indicating the feasibility of the developed GBSAR data processing package for deformation monitoring of a wide range of scientific and practical applications.

Keywords: ground-based synthetic aperture radar, interferometry, small baseline subset algorithm, deformation monitoring

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Authors: Mojtaba Barzegar, Alireza Shirazi, Saied Rabi Mahdavi

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Intraoperative radiation therapy (IORT) is an innovative treatment modality that the delivery of a large single dose of radiation to the tumor bed during the surgery. The radiotherapy success depends on the absorbed dose delivered to the tumor. The achievement better accuracy in patient treatment depends upon the measured dose by standard dosimeter such as ionization chamber, but because of the high density of electric charge/pulse produced by the accelerator in the ionization chamber volume, the standard correction factor for ion recombination Ksat calculated with the classic two-voltage method is overestimated so the use of dose/pulse independent dosimeters such as chemical Fricke and ethanol chlorobenzene (ECB) dosimeters have been suggested. Dose measurement is usually calculated and calibrated in the Zmax. Ksat calculated by comparison of ion chamber response and ECB dosimeter at each applicator degree, size, and dose. The relative output factors for IORT applicators have been calculated and compared with experimentally determined values and the results simulated by Monte Carlo software. The absorbed doses have been calculated and measured with statistical uncertainties less than 0.7% and 2.5% consecutively. The relative differences between calculated and measured OF’s were up to 2.5%, for major OF’s the agreement was better. In these conditions, together with the relative absorbed dose calculations, the OF’s could be considered as an indication that the IORT electron beams have been well simulated. These investigations demonstrate the utility of the full Monte Carlo simulation of accelerator head with ECB dosimeter allow us to obtain detailed information of clinical IORT beams.

Keywords: intra operative radiotherapy, ethanol chlorobenzene, ksat, output factor, monte carlo simulation

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Authors: Jung-Hwan Oh, Rajesh Kumar, Il-Kwon Oh

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Porous graphene has extensive potential applications in variety of fields such as hydrogen storage, CO oxidation, gas separation, supercapacitors, fuel cells, nanoelectronics, oil adsorption, and so on. However, the generation of some carbon atoms vacancies for precise small holes have been not extensively studied to prevent the agglomerates of graphene sheets and to obtain porous graphene with high surface area. Recently, many research efforts have been presented to develop physical and chemical synthetic approaches for porous graphene. But physical method has very high cost of manufacture and chemical method consumes so many hours for porous graphene. Herein, we propose a porous graphene contained holes with atomic scale precision by embedding metal nano-particles through microwave irradiation for hydrogen storage and CO oxidation multi- functionalities. This proposed synthetic method is appropriate for fast and convenient production of three dimensional nanostructures, which have nanoholes on the graphene surface in consequence of microwave irradiation. The metal nanoparticles are dispersed quickly on the graphene surface and generated uniform nanoholes on the graphene nanosheets. The morphological and structural characterization of the porous graphene were examined by scanning electron microscopy (SEM), transmission scanning electron microscopy (TEM) and RAMAN spectroscopy, respectively. The metal nanoparticle-embedded porous graphene exhibits a microporous volume of 2.586cm3g-1 with an average pore radius of 0.75 nm. HR-TEM analysis was carried out to further characterize the microstructures. By investigating the RAMAN spectra, we can understand the structural changes of graphene. The results of this work demonstrate a possibility to produce a new class of porous graphene. Furthermore, the newly acquired knowledge for the diffusion into graphene can provide useful guidance for the development of the growth of nanostructure.

Keywords: CO oxidation, hydrogen storage, nanocomposites, porous graphene

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Authors: Thais Cardoso Franco, Caio Nahuel Sousa Fagonde, Willer Gomes dos Santos

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Aurora Borealis is an optical phenomenon composed of luminous events observed in the night skies in the polar regions resulting from disturbances in the magnetosphere due to the impact of solar wind particles with the Earth's upper atmosphere, channeled by the Earth's magnetic field, which causes atmospheric molecules to become excited and emit electromagnetic spectrum, leading to the display of lights in the sky. However, there are still different implications of this phenomenon under study: high intensity auroras are often accompanied by geomagnetic storms that cause blackouts on Earth and impair the transmission of signals from the Global Navigation Satellite Systems (GNSS). Auroras are also known to occur on other planets and exoplanets, so the activity is an indication of active space weather conditions that can aid in learning about the planetary environment. In order to improve understanding of the phenomenon, this research aims to design a satellite formation flying solution for collecting and transmitting data for monitoring aurora borealis in northern hemisphere, an approach that allows studying the event with multipoint data collection in a reduced time interval, in order to allow analysis from the beginning of the phenomenon until its decline. To this end, the ideal number of satellites, the spacing between them, as well as the ideal topology to be used will be analyzed. From an orbital study, approaches from different altitudes, eccentricities and inclinations will also be considered. Given that at large relative distances between satellites in formation, controllers tend to fail, a study on the efficiency of nonlinear adaptive control methods from the point of view of position maintenance and propellant consumption will be carried out. The main orbital perturbations considered in the simulation: non-homogeneity terrestrial, atmospheric drag, gravitational action of the Sun and the Moon, accelerations due to solar radiation pressure and relativistic effects.

Keywords: formation flying, nonlinear adaptive control method, aurora borealis, adaptive SDRE method

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Authors: A. Abdelnasser, M. Kumral, B. Zoheir, P. Weihed, M. Budakoglu, L. Gumus

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Atud gold deposits located at the central part of the Egyptian Eastern Desert of Egypt. It represents the vein-type gold mineralization at the Arabian-Nubian Shield in North Africa. Furthermore, this Au mineralization was closely associated with intense hydrothermal alteration haloes along the NW-SE brittle-ductile shear zone at the mined area. This study reports new data about the mineral chemistry of the hydrothermal and metamorphic minerals as well as the geothermobarometry of the metamorphism and determines the paragenetic interrelationship between Au-bearing sulfides and gangue minerals in Atud gold mine by using the electron microprobe analyses (EMPA). These analyses revealed that the ore minerals associated with gold mineralization are arsenopyrite, pyrite, chalcopyrite, sphalerite, pyrrhotite, tetrahedrite and gersdorffite-cobaltite. Also, the gold is highly associated with arsenopyrite and As-bearing pyrite as well as sphalerite with an average ~70 wt.% Au (+26 wt.% Ag) whereas it occurred either as disseminated grains or along microfractures of arsenopyrite and pyrite in altered wallrocks and mineralized quartz veins. Arsenopyrite occurs as individual rhombic or prismatic zoned grains disseminated in the quartz veins and wallrock and is intergrown with euhedral arsenian pyrite (with ~2 atom % As). Pyrite is As-bearing pyrite that occurs as disseminated subhedral or anhedral zoned grains replacing by chalcopyrite in some samples. Inclusions of sphalerite and pyrrhotite are common in the large pyrite grains. Secondary minerals such as sericite, calcite, chlorite and albite are disseminated either in altered wallrocks or in quartz veins. Sericite is the main secondary and alteration mineral associated with Au-bearing sulfides and calcite. Electron microprobe data of the sericite show that its muscovite component is high in all analyzed flakes (XMs= an average 0.89) and the phengite content (Mg+Fe a.p.f.u.) varies from 0.10 to 0.55 and from 0.13 to 0.29 in wallrocks and mineralized veins respectively. Carbonate occurs either as thin veinlets or disseminated grains in the mineralized quartz vein and/or the wallrocks. It has higher amount of calcite (CaCO3) and low amount of MgCO3 as well as FeCO3 in the wallrocks relative to the quartz veins. Chlorite flakes are associated with arsenopyrite and their electron probe data revealed that they are generally Fe-rich composition (FeOt 20.64–20.10 wt.%) and their composition is clinochlore either pycnochlorite or ripidolite with Al (iv) = 2.30-2.36 pfu and 2.41-2.51 pfu and with narrow range of estimated formation temperatures are (289–295°C) and (301-312°C) for pycnochlorite and ripidolite respectively. Albite is accompanied with chlorite with an Ab content is high in all analyzed samples (Ab= 95.08-99.20).

Keywords: micro-analytical data, mineral chemistry, EMPA, Atud gold deposit, Egypt

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Authors: Kamrun N. Keya, Nasrin A. Kona, Ruhul A. Khan

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Pineapple leaf fiber (PALF) reinforced polypropylene (PP) based composites were fabricated by a conventional compression molding technique. In this investigation, PALF composites were manufactured using different percentages of fiber, which were varying from 25-50% on the total weight of the composites. To fabricate the PALF/PP composites, untreated and treated fibers were selected. A systematic study was done to observe the physical, mechanical and interfacial behavior of the composites. In this study, mechanical properties of the composites such as tensile, impact and bending properties were observed precisely. It was found that 45wt% of fiber composites showed better mechanical properties than others. Maximum tensile strength (TS) and bending strength (BS) was observed, 65 MPa and 50 MPa respectively, whereas the highest tensile modulus (TM) and bending modulus (BM) was examined, 1.7 GPa and 0.85 GPa respectively. The PALF/PP based composites were treated with irradiated under gamma radiation (the source strength 50 kCi Cobalt-60) of various doses (2.5 kGy to 10 kGy). The effect of gamma radiation on the composites was also investigated, and it found that the effect of 5.0 kGy (i.e. units for radiation measurement is 'gray', kGy=kilogray ) gamma dose showed better mechanical properties than other doses. The values of TS, BS, TM, and BM of the irradiated (5.0 kGy) composites were found to improve by 19%, 23%, 17% and 25 % over non-irradiated composites. After flexural testing, fracture sides of the untreated and treated both composites were studied by scanning electron microscope (SEM). SEM results of the treated PALF/PP based composites showed better fiber-matrix adhesion and interfacial bonding than untreated PALF/PP based composites. Water uptake and soil degradation tests of untreated and treated composites were also investigated.

Keywords: PALF, polypropylene, compression molding technique, gamma radiation, mechanical properties, scanning electron microscope

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Authors: Okafor E. Ijeoma, Isimi C. Yetunde, Okoh E. Judith, Kunle O. Olobayo, Emeje O. Martins

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Starch has gained interest as a renewable and environmentally compatible polymer due to the increase in its use. However, starch by itself could not be satisfactorily applied in industrial processes due to some inherent disadvantages such as its hydrophilic character, poor mechanical properties, its inability to withstand processing conditions such as extreme temperatures, diverse pH, high shear rate, freeze-thaw variation and dimensional stability. The range of physical properties of parent starch can be enlarged by chemical modification which invariably enhances their use in a number of applications found in industrial processes and food manufacture. In this study, Manihot esculentus starch was subjected to modification by oxidation. Fourier Transmittance Infra- Red (FTIR) and Raman spectroscopies were used to confirm the synthesis while Scanning Electron Microscopy (SEM) and X- Ray Diffraction (XRD) were used to characterize the new polymer. DPPH (2, 2-diphenyl-1-picryl-hydrazyl-hydrate) free radical assay was used to determine the antioxidant property of the oxidized starch. Our results show that the modification had no significant effect on the foaming capacity as well as on the emulsion capacity. Scanning electron microscopy revealed that oxidation did not alter the predominantly circular-shaped starch granules, while the X-ray pattern of both starch, native and modified were similar. FTIR results revealed a new band at 3007 and 3283cm-1. Differential scanning calorimetry returned two new endothermic peaks in the oxidized starch with an improved gelation capacity and increased enthalpy of gelatinization. The IC50 of oxidized starch was notably higher than that of the reference standard, ascorbic acid.

Keywords: antioxidant activity, DPPH, M. esculentus, oxidation, starch

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Authors: Alexey Yu. Postnikov, Nikolay T. Kazakovskiy, Valery V. Mokrushin, Irina A. Tsareva, Andrey A. Potekhin, Valentina N. Golubeva, Yuliya V. Potekhina, Maxim V. Tsarev

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The development of tritium and deuterium targets for neutron tubes and generators is a part of the activities in All-Russia Research Institute of Experimental Physics (RFNC-VNIIEF). These items contain a metal substrate (for example, copper) with a titanium film with a few microns thickness deposited on it. Then these metal films are saturated with tritium, deuterium or their mixtures. The significant problem in neutron tubes and neutron generators is the characterization of substrate surface before a deposition of titanium film on it, and analysis of the deposited titanium film’s surface before hydrogenation and after a saturation of the film with hydrogen isotopes. The performance effectiveness of neutron tube and generator also depends on upon the quality parameters of the surface of the initial substrate, deposited metal film and hydrogenated target. The objective of our work is to study the target prototype samples, that have differ by various approaches to the preliminary chemical processing of a copper substrate, and to analyze the integrity of titanium film after its saturation with deuterium. The research results of copper substrate and the surface of deposited titanium film with the use of electron microscopy, X-ray spectral microanalysis and laser-spark methods of analyses are presented. The causes of surface defects appearance have been identified. The distribution of deuterium and some impurities (oxygen and nitrogen) along the surface and across the height of the hydrogenated film in the target has been established. This allows us to evaluate the composition homogeneity of the samples and consequently to estimate the quality of hydrogenated samples. As the result of this work the propositions on the advancement of production technology and characterization of target’s surface have been presented.

Keywords: tritium and deuterium targets, titanium film, laser-spark methods, electron microscopy

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Authors: Satam Alotibi, Osama A. Hussein, Aziz H. Al-Shaibani, Nawaf A. Al-Aqeel, Abdellah Kaiba, Fatehia S. Alhakami, Mohammed Alyami, Talal F. Qahtan

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The demand for sustainable and efficient energy conversion using solar energy has grown rapidly in recent years. In this pursuit, solar-to-chemical conversion has emerged as a promising approach, with oxygen vacancies-rich tungsten trioxide (WO₃) playing a crucial role. This study presents a method for synthesizing oxygen vacancies-rich WO3, resulting in a significant enhancement of its photocatalytic activity, representing a significant step towards sustainable energy solutions. Experimental results underscore the importance of oxygen vacancies in modifying the properties of WO₃. These vacancies introduce additional energy states within the material, leading to a reduction in the bandgap, increased light absorption, and acting as electron traps, thereby reducing emissions. Our focus lies in developing oxygen vacancies-rich WO₃, which demonstrates unparalleled potential for improved photocatalytic applications. The effectiveness of oxygen vacancies-rich WO₃ in solar-to-chemical conversion was showcased through rigorous assessments of its photocatalytic degradation performance. Sunlight irradiation was employed to evaluate the material's effectiveness in degrading organic pollutants in wastewater. The results unequivocally demonstrate the superior photocatalytic performance of oxygen vacancies-rich WO₃ compared to conventional WO₃ nanomaterials, establishing its efficacy in sustainable and efficient energy conversion. Furthermore, the synthesized material is utilized to fabricate films, which are subsequently employed in immobilized WO₃ and oxygen vacancies-rich WO₃ reactors for water purification under natural sunlight irradiation. This application offers a sustainable and efficient solution for water treatment, harnessing solar energy for effective decontamination. In addition to investigating the photocatalytic capabilities, we extensively analyze the structural and chemical properties of the synthesized material. The synthesis process involves in situ thermal reduction of WO₃ nano-powder in a nitrogen environment, meticulously monitored using thermogravimetric analysis (TGA) to ensure precise control over the synthesis of oxygen vacancies-rich WO₃. Comprehensive characterization techniques such as UV-Vis spectroscopy, X-ray photoelectron spectroscopy (XPS), FTIR, Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) provide deep insights into the material's optical properties, chemical composition, elemental states, structure, surface properties, and crystalline structure. This study represents a significant advancement in sustainable energy conversion through solar-to-chemical processes and water purification. By harnessing the unique properties of oxygen vacancies-rich WO₃, we not only enhance our understanding of energy conversion mechanisms but also pave the way for the development of highly efficient and environmentally friendly photocatalytic materials. The application of this material in water purification demonstrates its versatility and potential to address critical environmental challenges. These findings bring us closer to a sustainable energy future and cleaner water resources, laying a solid foundation for a more sustainable planet.

Keywords: sustainable energy conversion, solar-to-chemical conversion, oxygen vacancies-rich tungsten trioxide (WO₃), photocatalytic activity enhancement, water purification

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Authors: Ontima Yamchuti, Waruntorn Kanitpanyacharoen, Chakkaphan Sutthirat, Wantana Klysuban, Penphitcha Amonpattarakit

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Natural corundum occurs in various colors due to impurities or trace elements in its structure. Sapphire and ruby are essentially the same mineral, corundum, but valued differently due to their red and blue varieties, respectively. Color is one of the critical factors used to determine the value of natural and synthetic corundum. Despite the abundance of research on impurities in natural corundum, little is known about trace elements in synthetic corundum. This project thus aims to quantify trace elements and identify their oxidation states in synthetic corundum. A total of 15 corundum samples in red, blue, and yellow, synthesized by melt growth process, were first investigated by X-ray diffraction (XRD) analysis to determine the composition. Electron probe micro-analyzer (EPMA) was used to identify the types of trace elements. Results confirm that all synthetic corundums contain crystalline Al₂O₃ and a wide variety type of trace element, particularly Cr, Fe, and Ti. In red, yellow, and blue corundums respectively. To further determine their oxidation states, synchrotron X-ray absorption near edge structure spectrometry (XANES) was used to observe absorbing energy of each element. XANES results show that red synthetic corundum has Cr³⁺ as a major trace element (62%). The pre-edge absorption energy of Cr³⁺ is at 6001 eV. In addition, Fe²⁺ and Fe³⁺ are dominant oxidation states of yellow synthetic corundum while Ti³⁺and Ti⁴⁺ are dominant oxidation states of blue synthetic corundum. the average absorption energy of Fe and Ti is 4980 eV and 7113 eV respectively. The presence of Fe²⁺, Fe³⁺, Cr³⁺, Ti³⁺, and Ti⁴⁺ in synthetic corundums in this study is governed by comparison absorption energy edge with standard transition. The results of oxidation states in this study conform with natural corundum. However yellow synthetic corundums show difference oxidation state of trace element compared with synthetic in electron spin resonance spectrometer method which found that Ni³⁺ is a dominant oxidation state.

Keywords: corundum, trace element, oxidation state, XANES technique

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Authors: Yogita Patil-Sen

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Magnetic nanoparticles such as those made of iron oxide have been widely explored as biocatalysts, contrast agents, and drug delivery systems. However, some of the challenges associated with these particles are agglomeration and biocompatibility, which lead to concern of toxicity of the particles, especially for drug delivery applications. Coating the particles with biocompatible materials such as lipids and peptides have shown to improve the mentioned issues. Thus, these core-shell type nanoparticles are emerging as the new class of nanomaterials for targeted drug delivery applications. In this study, various types of core-shell magnetic nanoparticles are prepared and characterized using techniques, such as Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Vibrating Sample Magnetometer (VSM) and Thermogravimetric Analysis (TGA). The heating ability of nanoparticles is tested under oscillating magnetic field. The efficacy of the nanoparticles as drug carrier is also investigated. The loading of an anticancer drug, Doxorubicin at 18 °C is measured up to 48 hours using UV-visible spectrophotometer. The drug release profile is obtained under thermal incubation condition at 37 °C and compared with that under the influence of oscillating field. The results suggest that the core-shell nanoparticles exhibit superparamagnetic behaviour, although, coating reduces the magnetic properties of the particles. Both the uncoated and coated particles show good heating ability, again it is observed that coating decreases the heating behaviour of the particles. However, coated particles show higher drug loading efficiency than the uncoated particles and the drug release is much more controlled under the oscillating magnetic field. Thus, the results strongly indicate the suitability of the prepared core-shell type nanoparticles as drug delivery vehicles and their potential in magnetic hyperthermia applications and for hyperthermia cancer therapy.

Keywords: core-shell, hyperthermia, magnetic nanoparticles, targeted drug delivery

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Authors: Disha Gupta

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The aim of this research is to conduct X-ray and e-beam characterization techniques on lithium-ion battery materials for the improvement of battery performance. The key characterization techniques employed are the synchrotron X-ray Absorption Spectroscopy (XAS) combined with X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to obtain a more holistic approach to understanding material properties. This research effort provides additional battery characterization knowledge that promotes the development of new cathodes, anodes, electrolyte and separator materials for batteries, hence, leading to better and more efficient battery performance. Both ex-situ and in-situ synchrotron experiments were performed on LiFePO₄, one of the most common cathode material, from different commercial sources and their structural analysis, were conducted using Athena/Artemis software. This analysis technique was then further extended to study other cathode materials like LiMnxFe(₁₋ₓ)PO₄ and even some sulphate systems like Li₂Mn(SO₄)₂ and Li₂Co0.5Mn₀.₅ (SO₄)₂. XAS data were collected for Fe and P K-edge for LiFePO4, and Fe, Mn and P-K-edge for LiMnxFe(₁₋ₓ)PO₄ to conduct an exhaustive study of the structure. For the sulphate system, Li₂Mn(SO₄)₂, XAS data was collected at both Mn and S K-edge. Finite Difference Method for Near Edge Structure (FDMNES) simulations were also conducted for various iron, manganese and phosphate model compounds and compared with the experimental XANES data to understand mainly the pre-edge structural information of the absorbing atoms. The Fe K-edge XAS results showed a charge compensation occurring on the Fe atom for all the differently synthesized LiFePO₄ materials as well as the LiMnxFe(₁₋ₓ)PO₄ systems. However, the Mn K-edge showed a difference in results as the Mn concentration changed in the materials. For the sulphate-based system Li₂Mn(SO₄)₂, however, no change in the Mn K-edge was observed, even though electrochemical studies showed Mn redox reactions.

Keywords: li-ion batteries, electrochemistry, X-ray absorption spectroscopy, XRD

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Authors: Nneka Augustina Akwu, Yougasphree Naidoo

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Molecular advancement in technology has created a means whereby the atoms and molecules (solid forms) of certain materials such as plants, can now be reduced to a range of 1-100 nanometres. Green synthesis of silver nanoparticles (AgNPs) was carried out at room temperature (RT) 25 ± 2°C and 80°C, using the metabolites in the aqueous extracts of the leaves and stem bark of Grewia lasiocarpa as reductants and stabilizing agents. The biosynthesized AgNPs were characterized by UV-Vis spectrophotometry, attenuated total reflectance - Fourier transforms infrared (ATR-FTIR) spectroscopy, nanoparticle tracking analysis (NTA), Energy Dispersive X-ray fluorescence scanning electron microscope (SEM-EDXRF) and high-resolution transmission electron microscopy (HRTEM). The AgNPs were biologically evaluated for antioxidant, antibacterial and cytotoxicity activities. The phytochemical and FTIR analyses revealed the presence of metabolites that act as reducing and capping agents, while the UV-Vis spectroscopy of the biosynthesized NPs showed absorption between 380-460 nm, confirming AgNP synthesis. The Zeta potential values were between -9.1 and -20.6 mV with a hydrodynamics diameter ranging from 38.3 to 46.7 nm. SEM and HRTEM analyses revealed that AgNPs were predominately spherical with an average particle size of 2- 31 nm for the leaves and 5-27 nm for the stem bark. The cytotoxicity IC50 values of the AgNPs against HeLa, Caco-2 and MCF-7 were >1 mg/mL. The AgNPs were sensitive to all strains of bacteria used, with methicillin-resistant Staphylococcus aureus (MRSA), Staphylococcus aureus (ATCC 25923) and Escherichia coli (ATCC 25922) being more sensitive to the AgNPs. Our findings propose that antibacterial and anticancer agents could be derived from these AgNPs of G. lasiocarpa, and warrant their further investigation.

Keywords: antioxidant, cytotoxicity, Grewia lasiocarpa, silver nanoparticles, Zeta potentials

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Authors: Anastasia Beketova, Emmanouil-George C. Tzanakakis, Ioannis G. Tzoutzas, Eleana Kontonasaki

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In restorative dentistry, yttria-stabilized zirconia (YSZ) nanoparticles can be applied as fillers to improve the mechanical properties of various resin-based materials. Using sol-gel based synthesis as simple and cost-effective method, nano-sized YSZ particles with high purity can be produced. The aim of this study was to synthesize YSZ nanoparticles by the Pechini sol-gel method at different temperatures and to investigate their composition, structure, and morphology. YSZ nanopowders were synthesized by the sol-gel method using zirconium oxychloride octahydrate (ZrOCl₂.8H₂O) and yttrium nitrate hexahydrate (Y(NO₃)₃.6H₂O) as precursors with the addition of acid chelating agents to control hydrolysis and gelation reactions. The obtained powders underwent TG_DTA analysis and were sintered at three different temperatures: 800, 1000, and 1200°C for 2 hours. Their composition and morphology were investigated by Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction Analysis (XRD), Scanning Electron Microscopy with associated with Energy Dispersive X-ray analyzer (SEM-EDX), Transmission Electron Microscopy (TEM) methods, and Dynamic Light Scattering (DLS). FTIR and XRD analysis showed the presence of pure tetragonal phase in the composition of nanopowders. By increasing the calcination temperature, the crystallinity of materials increased, reaching 47.2 nm for the YSZ1200 specimens. SEM analysis at high magnifications and DLS analysis showed submicron-sized particles with good dispersion and low agglomeration, which increased in size as the sintering temperature was elevated. From the TEM images of the YSZ1000 specimen, it can be seen that zirconia nanoparticles are uniform in size and shape and attain an average particle size of about 50 nm. The electron diffraction patterns clearly revealed ring patterns of polycrystalline tetragonal zirconia phase. Pure YSZ nanopowders have been successfully synthesized by the sol-gel method at different temperatures. Their size is small, and uniform, allowing their incorporation of dental luting resin cements to improve their mechanical properties and possibly enhance the bond strength of demanding dental ceramics such as zirconia to the tooth structure. This research is co-financed by Greece and the European Union (European Social Fund- ESF) through the Operational Programme 'Human Resources Development, Education and Lifelong Learning 2014- 2020' in the context of the project 'Development of zirconia adhesion cements with stabilized zirconia nanoparticles: physicochemical properties and bond strength under aging conditions' (MIS 5047876).

Keywords: dental cements, nanoparticles, sol-gel, yttria-stabilized zirconia, YSZ

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Authors: Anna Jastrzebska, K. S. Suresh, T. Kitashima, Y. Yamabe-Mitarai, Z. Pakiela

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Near α titanium alloys are important materials for aerospace applications, especially in high temperature applications such as jet engine. Mechanical properties of Ti alloys strongly depends on their processing route, then it is very important to understand micro-structure change by different processing. In our previous study, Nb was found to improve oxidation resistance of Ti alloys. In this study, micro-structure evolution of Ti-6Al-4Nb (wt %) alloy was investigated after plain strain compression test in hot working temperatures in the α and β phase region. High-resolution EBSD was successfully used for precise phase and texture characterization of this alloy. 1.1 kg of Ti-6Al-4Nb ingot was prepared using cold crucible levitation melting. The ingot was subsequently homogenized in 1050 deg.C for 1h followed by cooling in the air. Plate like specimens measuring 10×20×50 mm3 were cut from an ingot by electrical discharge machining (EDM). The plain strain compression test using an anvil with 10 x 35 mm in size was performed with 3 different strain rates: 0.1s-1, 1s-1and 10s-1 in 700 deg.C and 1050 deg.C to obtain 75% of deformation. The micro-structure was investigated by scanning electron microscopy (SEM) equipped with electron backscatter diffraction (EBSD) detector. The α/β phase ratio and phase morphology as well as the crystallographic texture, subgrain size, misorientation angles and misorientation gradients corresponding to each phase were determined over the middle and the edge of sample areas. The deformation mechanism in each working temperature was discussed. The evolution of texture changes with strain rate was investigated. The micro-structure obtained by plain strain compression test was heterogeneous with a wide range of grain sizes. This is because deformation and dynamic recrystallization occurred during deformation at temperature in the α and β phase. It was strongly influenced by strain rate.

Keywords: EBSD, plain strain compression test, Ti alloys

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Authors: Wei-Jing Li, Ren-Xuan Yang, Kui-Hao Chuang, Ming-Yen Wey

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Nowadays, plastic product and utilization are extensive and have greatly improved our life. Yet, plastic wastes are stable and non-biodegradable challenging issues to the environment. Waste-to-energy strategies emerge a promising way for waste management. This work investigated the co-production of hydrogen and carbon nanotubes from the syngas which was from the gasification of polypropylene. A nickel-silica core-shell catalyst was applied for syngas reaction from plastic waste gasification in a fixed-bed reactor. SiO2 were prepared through various synthesis solvents by Stöber process. Ni plays a role as modified SiO2 support, which were synthesized by deposition-precipitation method. Core-shell catalysts have strong interaction between active phase and support, in order to avoid catalyst sintering. Moreover, Fe or Co metal acts as promoter to enhance catalytic activity. The effects of calcined atmosphere, second metal addition, and reaction temperature on hydrogen production and carbon yield were examined. In this study, the catalytic activity and carbon yield results revealed that the Ni/SiO2 catalyst calcined under H2 atmosphere exhibited the best performance. Furthermore, Co promoted Ni/SiO2 catalyst produced 3 times more than Ni/SiO2 on carbon yield at long-term operation. The structure and morphological nature of the calcined and spent catalysts were examined using different characterization techniques including scanning electron microscopy, transmission electron microscopy, X-ray diffraction. In addition, the quality and thermal stability of the nano-carbon materials were also evaluated by Raman spectroscopy and thermogravimetric analysis.

Keywords: plastic wastes, hydrogen, carbon nanotube, core-shell catalysts

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Authors: M. N. Baig, F. N. Khan, M. Junaid

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Titanium alloys are widely employed in aerospace, medical, chemical, and marine applications. These alloys offer many advantages such as low specific weight, high strength to weight ratio, excellent corrosion resistance, high melting point and good fatigue behavior. These attractive properties make titanium alloys very unique and therefore they require special attention in all areas of processing, especially welding. In this work, 1.6 mm thick sheets of Ti-5Al-2,5Sn, an alpha titanium (α-Ti) alloy, were welded using electron beam (EBW) and laser beam (LBW) welding processes to achieve a full penetration Bead-on Plate (BoP) configuration. The weldments were studied using polarized optical microscope, SEM, EDS and XRD. Microhardness distribution across the weld zone and smooth and notch tensile strengths of the weldments were also recorded. Residual stresses using Hole-drill Strain Measurement (HDSM) method and deformation patterns of the weldments were measured for the purpose of comparison of the two welding processes. Fusion zone widths of both EBW and LBW weldments were found to be approximately equivalent owing to fairly similar high power densities of both the processes. Relatively less oxide content and consequently high joint quality were achieved in EBW weldment as compared to LBW due to vacuum environment and absence of any shielding gas. However, an increase in heat-affected zone width and partial ά-martensitic transformation infusion zone of EBW weldment were observed because of lesser cooling rates associated with EBW as compared with LBW. The microstructure infusion zone of EBW weldment comprised both acicular α and ά martensite within the prior β grains whereas complete ά martensitic transformation was observed within the fusion zone of LBW weldment. Hardness of the fusion zone in EBW weldment was found to be lower than the fusion zone of LBW weldment due to the observed microstructural differences. Notch tensile specimen of LBW exhibited higher load capacity, ductility, and absorbed energy as compared with EBW specimen due to the presence of high strength ά martensitic phase. It was observed that the sheet deformation and deformation angle in EBW weldment were more than LBW weldment due to relatively more heat retention in EBW which led to more thermal strains and hence higher deformations and deformation angle. The lowest residual stresses were found in LBW weldments which were tensile in nature. This was owing to high power density and higher cooling rates associated with LBW process. EBW weldment exhibited highest compressive residual stresses due to which the service life of EBW weldment is expected to improve.

Keywords: Laser and electron beam welding, Microstructure and mechanical properties, Residual stress and distortions, Titanium alloys

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Authors: Sudeshna Chandra, Christian Gäbler, Christian Schliebe, Heinrich Lang

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Highly branched dendrimers provide structural homogeneity, controlled composition, comparable size to biomolecules, internal porosity and multiple functional groups for conjugating reactions. Electro-active dendrimers containing multiple redox units have generated great interest in their use as electrode modifiers for development of biosensors. The electron transfer between the redox-active dendrimers and the biomolecules play a key role in developing a biosensor. Ferrocenes have multiple and electrochemically equivalent redox units that can act as electron “pool” in a system. The ferrocenyl-terminated polyamidoamine dendrimer is capable of transferring multiple numbers of electrons under the same applied potential. Therefore, they can be used for dual purposes: one in building a film over the electrode for immunosensors and the other for immobilizing biomolecules for sensing. Electrochemical immunosensor, thus developed, exhibit fast and sensitive analysis, inexpensive and involve no prior sample pre-treatment. Electrochemical amperometric immunosensors are even more promising because they can achieve a very low detection limit with high sensitivity. Detection of the cancer biomarkers at an early stage can provide crucial information for foundational research of life science, clinical diagnosis and prevention of disease. Elevated concentration of biomarkers in body fluid is an early indication of some type of cancerous disease and among all the biomarkers, IgG is the most common and extensively used clinical cancer biomarkers. We present an IgG (=immunoglobulin) electrochemical immunosensor using a newly synthesized redox-active ferrocenyl dendrimer of generation 2 (G2Fc) as glassy carbon electrode material for immobilizing the antibody. The electrochemical performance of the modified electrodes was assessed in both aqueous and non-aqueous media using varying scan rates to elucidate the reaction mechanism. The potential shift was found to be higher in an aqueous electrolyte due to presence of more H-bond which reduced the electrostatic attraction within the amido groups of the dendrimers. The cyclic voltammetric studies of the G2Fc-modified GCE in 0.1 M PBS solution of pH 7.2 showed a pair of well-defined redox peaks. The peak current decreased significantly with the immobilization of the anti-goat IgG. After the immunosensor is blocked with BSA, a further decrease in the peak current was observed due to the attachment of the protein BSA to the immunosensor. A significant decrease in the current signal of the BSA/anti-IgG/G2Fc/GCE was observed upon immobilizing IgG which may be due to the formation of immune-conjugates that blocks the tunneling of mass and electron transfer. The current signal was found to be directly related to the amount of IgG captured on the electrode surface. With increase in the concentration of IgG, there is a formation of an increasing amount of immune-conjugates that decreased the peak current. The incubation time and concentration of the antibody was optimized for better analytical performance of the immunosensor. The developed amperometric immunosensor is sensitive to IgG concentration as low as 2 ng/mL. Tailoring of redox-active dendrimers provides enhanced electroactivity to the system and enlarges the sensor surface for binding the antibodies. It may be assumed that both electron transfer and diffusion contribute to the signal transformation between the dendrimers and the antibody.

Keywords: ferrocenyl dendrimers, electrochemical immunosensors, immunoglobulin, amperometry

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Authors: Mirijam Vrabec, Marian Janak, Bojan Ambrozic, Angelja K. Surca, Nastja Rogan Smuc, Nina Zupancic, Saso Sturm

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Natural microdiamonds and moissanite (SiC) can form during the orogenic events under ultrahigh-pressure metamorphic conditions (UHP), when parts of Earth’s crust are subducted to extreme depths. So far, such processes were identified only in few places on the Earth, and therefore, represent unique opportunity to study the evolution of the Earth’s deep interior. An important discovery of microdiamonds and moissanite was reported from Pohorje, (Slovenia), where they occurred as single or polyphase inclusions in garnets. Metasedimentary rocks from Pohorje are predominantly gneisses representing parts of the Austroalpine metamorphic units of the Eastern Alps. During Cretaceous orogeny, (ca. 95–92 Ma) continental crustal rocks were deeply subducted to the mantle depths (below 100 km) and metamorphosed at pressures exceeding 3.5 GPa and temperatures between 800–850 °C. Microstructural and phase analysis of the inclusions as well as detailed elemental analysis of host garnets were carried out combining several analytical techniques: optical microscope in plane polarized transmitted light, electron probe microanalysis (EPMA) with wavelength-dispersive x-ray spectrometry (WDS) and field-emission scanning microscope (FEG-SEM) with energy-dispersive x-ray spectroscopy (EDS). Micro-Raman analysis revealed sharp, first order diamond bands sometimes accompanied by graphite bands implying that transformation of diamond back to graphite occurred. To study the chemical and crystallographic relationship between microdiamonds and co-inclusions, advanced techniques of transmission electron microscopy (TEM) were applied, which included high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), combined with EDS and electron energy-loss spectroscopy (EELS). To prepare electron transparent TEM lamellae selectively a dual-beam Focused Ion Beam/SEM (FIB/SEM) was employed. Detailed study of TEM lamellae, which was cross-sectioned from the highly faceted inclusion body located within the host garnet crystal matrix, revealed rich and rather complex internal structure. Namely, the negative crystal facets of the main inclusion body were typically decorated with up to 1 μm thick amorphous layer, reflecting the general garnet composition with slight variations in Fe/Ca content. Within these layers, ELNES analysis revealed the presence of a 28–30 nm thick layer of amorphous carbon. The very last section of this layer corresponds to composition of SiO2. Within the inclusion, besides diamond and moissanite alumosilicate mineral with pronounced layered structure, iron sulfides and chlorine were identified under TEM and CO2 and CH4 using Raman. Moissanite is found as single crystal or composed from numerous highly textured nano-crystals with the average size of 10 nm. Moissanite inclusions were found embedded inside the amorphous crust implying that moissanite crystalized well before the deposition of the amorphous layer. From the microstructural, crystallographic and chemical observations so far we can deduce, that polyphase inclusions in diamond bearing garnets from Pohorje most probably crystallized from reduced supercritical fluids. Based on layered interface structure of the host mineral multiphase process of crystallization is possible. The presence of microdiamonds and moissanite in rocks from Pohorje demonstrates that these parts of the Eastern Alps were subducted to extreme depths, and were subsequently exhumed back to the Earth's surface without complete breakdown of UHP mineral phases, allowing a rear and exceptional opportunity to study them in-situ.

Keywords: diamond, fluid inclusions, moissanite, TEM, UHP metamorphism.

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Authors: E. Gandomkar, S. Sabbaghi

Abstract:

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: Fanyuan Shao, Wei Liu, Deli Gao

Abstract:

Polycrystalline diamond composite (PDC) cutter is made of diamond powder as raw material, cobalt metal or non-metallic elements as a binder, mixed with WC cemented carbide matrix assembly, through high temperature and high-pressure sintering. PDC bits with PDC cutters are widely used in oil and gas drilling because of their high hardness, good wear resistance and excellent impact toughness. And PDC cutter is the main cutting tool of bit, which seriously affects the service of the PDC bit. The wear resistance of the PDC cutter is measured by cutting granite with a vertical turret lathe (VTL). This experiment can achieve long-distance cutting to obtain the relationship between the wear resistance of the PDC cutter and cutting distance, which is more closely to the real drilling situation. Load cell and 3D optical profiler were used to obtain the value of cutting forces and wear area, respectively, which can also characterize the damage and wear of the PDC cutter. PDC cutters were cut via electrical discharge machining (EDM) and then flattened and polished. A scanning electron microscope (SEM) was used to observe the distribution of binder cobalt and the size of diamond particles in a diamond PDC cutter. The cutting experimental results show that the wear area of the PDC cutter has a good linear relationship with the cutting distance. Simultaneously, the larger the wear area is and the greater the cutting forces are required to maintain the same cutting state. The size and distribution of diamond particles in the polycrystalline diamond layer have a great influence on the wear resistance of the diamond layer. And PDC cutter with fine diamond grains shows more wear resistance than that with coarse grains. The deep leaching process is helpful to reduce the effect of binder cobalt on the wear resistance of the polycrystalline diamond layer. The experimental study can provide an important basis for the application of PDC cutters in oil and gas drilling.

Keywords: polycrystalline diamond compact, scanning electron microscope, wear resistance, cutting distance

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Authors: Diptiman Dinda, Shyamal Kumar Saha

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In the 21st century, sensitive and selective detection of trace amounts of explosives has become a serious problem. Generally, nitro compound and its derivatives are being used worldwide to prepare different explosives. Recently, TNP (2, 4, 6 trinitrophenol) is the most commonly used constituent to prepare powerful explosives all over the world. It is even powerful than TNT or RDX. As explosives are electron deficient in nature, it is very difficult to detect one separately from a mixture. Again, due to its tremendous water solubility, detection of TNP in presence of other explosives from water is very challenging. Simple instrumentation, cost-effective, fast and high sensitivity make fluorescence based optical sensing a grand success compared to other techniques. Graphene oxide (GO), with large no of epoxy grps, incorporate localized nonradiative electron-hole centres on its surface to give very weak fluorescence. In this work, GO is functionalized with 2, 6-diamino pyridine to remove those epoxy grps. through SN2 reaction. This makes GO into a bright blue luminescent fluorophore (DAP/rGO) which shows an intense PL spectrum at ∼384 nm when excited at 309 nm wavelength. We have also characterized the material by FTIR, XPS, UV, XRD and Raman measurements. Using this as fluorophore, a large fluorescence quenching (96%) is observed after addition of only 200 µL of 1 mM TNP in water solution. Other nitro explosives give very moderate PL quenching compared to TNP. Such high selectivity is related to the operation of FRET mechanism from fluorophore to TNP during this PL quenching experiment. TCSPC measurement also reveals that the lifetime of DAP/rGO drastically decreases from 3.7 to 1.9 ns after addition of TNP. Our material is also quite sensitive to 125 ppb level of TNP. Finally, we believe that this graphene based luminescent material will emerge a new class of sensing materials to detect trace amounts of explosives from aqueous solution.

Keywords: graphene, functionalization, fluorescence quenching, FRET, nitroexplosive detection

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Authors: Gaurav Bhanjana, Ganga Ram Chaudhary, Sandeep Kumar, Neeraj Dilbaghi

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Main sources of endocrine disrupting compounds in the ecosystem are hormones, pesticides, phthalates, flame retardants, dioxins, personal-care products, coplanar polychlorinated biphenyls (PCBs), bisphenol A, and parabens. These endocrine disrupting compounds are responsible for learning disabilities, brain development problems, deformations of the body, cancer, reproductive abnormalities in females and decreased sperm count in human males. Although discharge of these chemical compounds into the environment cannot be stopped, yet their amount can be retarded through proper evaluation and detection techniques. The available techniques for determination of these endocrine disrupting compounds mainly include high performance liquid chromatography (HPLC), mass spectroscopy (MS) and gas chromatography-mass spectrometry (GC–MS). These techniques are accurate and reliable but have certain limitations like need of skilled personnel, time consuming, interference and requirement of pretreatment steps. Moreover, these techniques are laboratory bound and sample is required in large amount for analysis. In view of above facts, new methods for detection of endocrine disrupting compounds should be devised that promise high specificity, ultra sensitivity, cost effective, efficient and easy-to-operate procedure. Nowadays, electrochemical sensors/biosensors modified with nanomaterials are gaining high attention among researchers. Bioelement present in this system makes the developed sensors selective towards analyte of interest. Nanomaterials provide large surface area, high electron communication feature, enhanced catalytic activity and possibilities of chemical modifications. In most of the cases, nanomaterials also serve as an electron mediator or electrocatalyst for some analytes.

Keywords: electrochemical, endocrine disruptors, microscopy, nanoparticles, sensors

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Authors: Khadijat O. Abdulwahab, Mohammad A. Malik, Paul O’Brien, Grigore A. Timco, Floriana Tuna

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The synthesis of spinel ferrite nanoparticles with a narrow size distribution is very crucial in their numerous applications including information storage, hyperthermia treatment, drug delivery, contrast agent in magnetic resonance imaging, catalysis, sensors, and environmental remediation. Ferrites have the general formula MFe2O4 (M = Fe, Co, Mn, Ni, Zn etc.) and possess remarkable electrical and magnetic properties which depend on the cations, method of preparation, size and their site occupancies. To the best of our knowledge, there are no reports on the use of a single source precursor to synthesise quaternary ferrite nanoparticles. Herein, we demonstrated the use of trimetallic iron pivalate cluster [CrCoFeO(O2CtBu)6(HO2CtBu)3] as a single source precursor to synthesise monodisperse cobalt chromium ferrite (FeCoCrO4) nanoparticles by the hot injection thermolysis method. The precursor was thermolysed in oleylamine, oleic acid, with diphenyl ether as solvent at its boiling point (260°C). The effect of concentration on the stoichiometry, phases or morphology of the nanoparticles was studied. The p-XRD patterns of the nanoparticles obtained at both concentrations were matched with cubic iron cobalt chromium ferrite (FeCoCrO4). TEM showed that a more monodispersed spherical ferrite nanoparticles of average diameter 4.0 ± 0.4 nm were obtained at higher precursor concentration. Magnetic measurements revealed that all the ferrite particles are superparamagnetic at room temperature. The nanoparticles were characterised by Powder X-ray Diffraction (p-XRD), Transmission Electron Microscopy (TEM), Inductively Coupled Plasma (ICP), Electron Probe Microanalysis (EPMA), Energy Dispersive Spectroscopy (EDS) and Super Conducting Quantum Interference Device (SQUID).

Keywords: quaternary ferrite nanoparticles, single source precursor, monodisperse, cobalt chromium ferrite, colloidal, hot injection thermolysis

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