Search results for: electron tomography

Authors: Mostafa Elbaba

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Because childhood renal diseases are grossly different compared to adult diseases, pediatric nephrology was founded as a specialty in 1965. Renal pathology specialty was introduced at the London Ciba Symposium in 1961. The history of renal pathology can be divided into two eras: one starting in the 1650s with the invention of the microscope, the second in the 1950s with the implementation of renal biopsy, and the presence of electron microscopy and immunofluorescence study. Prior to the 1950s, the study of diseased human kidneys was restricted to postmortem examination by gross pathology. In 1827, Richard Bright first described his triad of kidney disease, which was confirmed by morbid kidney changes at autopsy. In 1905 Friedrich Mueller coined the term “nephrosis” describing the inflammatory form of “degenerative” diseases, and later F. Munk added the term “lipoid nephrosis”. The most profound influence on renal diseases’ classification came from the publication of Volhard and Fahr in 1914. In 1899, Carl Max Wilhelm Wilms described Wilms' tumor of the kidneys in children. Chronic pyelonephritis was a popular renal diagnosis and the most common cause of uremia until the 1960s. Although kidney biopsy had been used early in the 1930s for renal tumors, the earliest reports of its use in the diagnosis of medical kidney disease were by Iversen and Brun in 1951, followed by Alwall in 1952, then by Pardo in 1953. The earliest intentional renal biopsies were done in 1944 by Nils Alwall, while the procedure was abandoned after the death of one of his 13 patients who biopsied. In 1950, Antonino Perez-Ara attempted renal biopsies, but his results were missed because of an unpopular journal publication. In the year 1951, Claus Brun and Poul Iverson developed the biopsy procedure using an aspiration technique. Popularizing renal biopsy practice is accredited to Robert Kark, who published his distinct work in 1954. He perfected the technique of renal biopsy in the prone position using the Vim-Silverman needle and used intravenous pyelography to improve the localization of the kidney.

Keywords: history, medicine, nephrology, pediatrics, pathology

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Authors: Lucja Rodzik, Joanna Lewandowska-Lancucka, Michal Szuwarzynski, Krzysztof Szczubialka, Maria Nowakowska

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The analysis of nucleobases is of great importance for bioscience since their abnormal concentration in body fluids suggests the deficiency and mutation of the immune system, and it is considered to be an important parameter for diagnosis of various diseases. The presented conjugate meets the need for development of the effective, selective and highly sensitive sensor for nucleobase/nucleoside detection. The novel, highly fluorescent cadmium telluride quantum dots (CdTe QDs) functionalized with thymine and stabilized with thioglycolic acid (TGA) conjugates has been developed and thoroughly characterized. Successful formation of the material was confirmed by elemental analysis, and UV–Vis fluorescence and FTIR spectroscopies. The crystalline structure of the obtained product was characterized with X-ray diffraction (XRD) method. The composition of CdTe QDs and their thymine conjugate was also examined using X-ray photoelectron spectroscopy (XPS). The size of the CdTe-thymine was 3-6 nm as demonstrated using atomic force microscopy (AFM) and high resolution transmission electron microscopy (HRTEM) imaging. The plasmon resonance fluorescence band at 540 nm on excitation at 351 nm was observed for these nanoparticles. The intensity of this band increased with the increase in the amount of conjugated thymine with no shift in its position. Based on the fluorescence measurements, it was found that the CdTe-thymine conjugate interacted efficiently and selectively not only with adenine, a nucleobase complementary to thymine, but also with nucleosides and adenine-containing modified nucleosides, i.e., 5′-deoxy-5′-(methylthio)adenosine (MTA) and 2’-O-methyladenosine, the urinary tumor markers which allow monitoring of the disease progression. The applicability of the CdTe-thymine sensor for the real sample analysis was also investigated in simulated urine conditions. High sensitivity and selectivity of CdTe-thymine fluorescence towards adenine, adenosine and modified adenosine suggest that obtained conjugate can be potentially useful for development of the biosensor for complementary nucleobase/nucleoside detection.

Keywords: CdTe quantum dots, conjugate, sensor, thymine

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Authors: Mohanapriya Subramanian, V. Raj

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Direct methanol fuel cells (DMFCs) are considered to be one of the most promising candidates for portable and stationary applications in the view of their advantages such as high energy density, easy manipulation, high efficiency and they operate with liquid fuel which could be used without requiring any fuel-processing units. Electrolyte membrane of DMFC plays a key role as a proton conductor as well as a separator between electrodes. Increasing concern over environmental protection, biopolymers gain tremendous interest owing to their eco-friendly bio-degradable nature. Pectin is a natural anionic polysaccharide which plays an essential part in regulating mechanical behavior of plant cell wall and it is extracted from outer cells of most of the plants. The aim of this study is to develop and demonstrate pectin based polymer composite membranes as methanol impermeable polymer electrolyte membranes for DMFCs. Pectin based nanocomposites membranes are prepared by solution-casting technique wherein pectin is blended with chitosan followed by the addition of optimal amount of sulphonic acid modified Titanium dioxide nanoparticle (S-TiO2). Nanocomposite membranes are characterized by Fourier Transform-Infra Red spectroscopy, Scanning electron microscopy, and Energy dispersive spectroscopy analyses. Proton conductivity and methanol permeability are determined into order to evaluate their suitability for DMFC application. Pectin-chitosan blends endow with a flexible polymeric network which is appropriate to disperse rigid S-TiO2 nanoparticles. Resulting nanocomposite membranes possess adequate thermo-mechanical stabilities as well as high charge-density per unit volume. Pectin-chitosan natural polymeric nanocomposite comprising optimal S-TiO2 exhibits good electrochemical selectivity and therefore desirable for DMFC application.

Keywords: biopolymers, fuel cells, nanocomposite, methanol crossover

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Authors: Noura El-Ahmady El-Naggar

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Among the antitumour drugs, bacterial enzyme L-asparaginase has been employed as the most effective chemotherapeutic agent in pediatric oncotherapy especially for acute lymphoblastic leukemia. Glutaminase free L-asparaginase producing actinomycetes were isolated from soil samples collected from Egypt. Among them, a potential culture, strain NEAE-119, was selected and identified on the basis of morphological, cultural, physiological and biochemical properties, together with 16S rDNA sequence as Streptomyces olivaceus NEAE-119 and sequencing product(1509 bp) was deposited in the GenBank database under accession number KJ200342. The optimization of different process parameters for L-asparaginase production by Streptomyces olivaceus NEAE-119 using Plackett–Burman experimental design and response surface methodology was carried out. Fifteen nutritional variables (temperature, pH, incubation time, inoculum size, inoculum age, agitation speed, dextrose, starch, L-asparagine, KNO3, yeast extract, K2HPO4, MgSO4.7H2O, NaCl and FeSO4. 7H2O) were screened using Plackett–Burman experimental design. The most positive significant independent variables affecting enzyme production (temperature, inoculum age and agitation speed) were further optimized by the central composite face-centered design -response surface methodology. As a result, a medium of the following formula is the optimum for producing an extracellular L-asparaginase in the culture filtrate of Streptomyces olivaceus NEAE-119: Dextrose 3g, starch 20g, L-asparagine 10g, KNO3 1g, K2HPO4 1g, MgSO4.7H2O 0.1g, NaCl 0.1g, pH 7, temperature 37°C, agitation speed 200 rpm/min, inoculum size 4%, v/v, inoculum age 72 h and fermentation period 5 days.

Keywords: Streptomyces olivaceus NEAE-119, glutaminase free L-asparaginase, production, Plackett-Burman design, central composite face-centered design, 16S rRNA, scanning electron microscope

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Authors: Mehrnaz Mostafavi

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Lung cancer is one of the most harmful forms of cancer. The long-term survival rate of lung cancer patients treated by conventional modalities such as surgical resection, radiation, and chemotherapy remains far from satisfactory. Systemic drug delivery is rarely successful because only a limited amount of the chemotherapeutic drug targets lung tumor sites, even when administered at a high dose. Targeted delivery of drug molecules to organs or special sites is one of the most challenging research areas in pharmaceutical sciences. By developing colloidal delivery systems such as liposomes, micelles and nanoparticles a new frontier was opened for improving drug delivery. Nanoparticles with their special characteristics such as small particle size, large surface area and the capability of changing their surface properties have numerous advantages compared with other delivery systems. Targeted nanoparticle delivery to the lungs is an emerging area of interest.Multimodal or combination therapy represents a promising new method to fight disease. Therefore, a combination of different therapeutic strategies may be the best alternative to improve treatment outcomes for lung cancer. Photothermal therapy was proposed as a novel approach to treatment. In this work, photothermal therapy with gold nanoparticles and near infrared laser (NIR) irradiation was investigated.Four types of small (<100nm), NIR absorbing gold nanoparticles (nanospheres, nanorods) were synthesized using wet chemical methods and characterized by transmission electron microscopy, dynamic light scattering and UV-vis spectroscopy. Their synthesis and properties were evaluated, to determine their feasibility as a photothermal agent for clinical applications. In vitro cellular uptake studies of the nanoparticles into lung cancer cell lines was measured using light scattering microscopy.Small gold nanorods had good photothermal properties and the greatest cellular uptake, and were used in photothermal studies. Under 4W laser irradiation, an increase in temperature of 10°C and decrease in cell viability of up to 80% were obtained.

Keywords: photothermal, therapy, cancer, gold nanorods

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Authors: I. C. Cho, W. H. Wen, H. Y. Tsai, T. C. Chao, C. J. Tung

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Tissue-equivalent proportional counter (TEPC) is a useful instrument used to measure radiation single-event energy depositions in a subcellular target volume. The quantity of measurements is the microdosimetric lineal energy, which determines the relative biological effectiveness, RBE, for radiation therapy or the radiation-weighting factor, WR, for radiation protection. TEPC is generally used in a mixed radiation field, where each component radiation has its own RBE or WR value. To reduce the pile-up effect during radiotherapy measurements, a miniature TEPC (mini TEPC) with cavity size in the order of 1 mm may be required. In the present work, a homemade mini TEPC with a cylindrical cavity of 1 mm in both the diameter and the height was constructed to measure the lineal energy spectrum of a mixed radiation field with high- and low-LET radiations. Instead of using external radiation beams to penetrate the detector wall, mixed radiation fields were produced by the interactions of neutrons with TEPC walls that contained small plugs of different materials, i.e. Li, B, A150, Cd and N. In all measurements, mini TEPC was placed at the beam port of the Tsing Hua Open-pool Reactor (THOR). Measurements were performed using the propane-based tissue-equivalent gas mixture, i.e. 55% C3H8, 39.6% CO2 and 5.4% N2 by partial pressures. The gas pressure of 422 torr was applied for the simulation of a 1 m diameter biological site. The calibration of mini TEPC was performed using two marking points in the lineal energy spectrum, i.e. proton edge and electron edge. Measured spectra revealed high lineal energy (> 100 keV/m) peaks due to neutron-capture products, medium lineal energy (10 – 100 keV/m) peaks from hydrogen-recoil protons, and low lineal energy (< 10 keV/m) peaks of reactor photons. For cases of Li and B plugs, the high lineal energy peaks were quite prominent. The medium lineal energy peaks were in the decreasing order of Li, Cd, N, A150, and B. The low lineal energy peaks were smaller compared to other peaks. This study demonstrated that internally produced mixed radiations from the interactions of neutrons with different plugs in the TEPC wall provided a useful approach for TEPC measurements of lineal energies.

Keywords: TEPC, lineal energy, microdosimetry, radiation quality

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Authors: Chanchal Biswas, Anrin Bhattacharyya, Gopes Chandra Das, Mahua Ghosh Chaudhuri, Rajib Dey

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Boiler coals with low fixed carbon and higher ash content have always challenged the metallurgists to develop a suitable method for their utilization. In the present study, an attempt is made to establish an energy effective method for the reduction of iron ore fines in the form of nuggets by using ‘Syngas’. By devolatisation (expulsion of volatile matter by applying heat) of boiler coal, gaseous product (enriched with reducing agents like CO, CO2, H2, and CH4 gases) is generated. Iron ore nuggets are reduced by this syngas. For that reason, there is no direct contact between iron ore nuggets and coal ash. It helps to control the minimization of the sulphur intake of the reduced nuggets. A laboratory scale devolatisation furnace designed with reduction facility is evaluated after in-depth studies and exhaustive experimentations including thermo-gravimetric (TG-DTA) analysis to find out the volatile fraction present in boiler grade coal, gas chromatography (GC) to find out syngas composition in different temperature and furnace temperature gradient measurements to minimize the furnace cost by applying one heating coil. The nuggets are reduced in the devolatisation furnace at three different temperatures and three different times. The pre-reduced nuggets are subjected to analytical weight loss calculations to evaluate the extent of reduction. The phase and surface morphology analysis of pre-reduced samples are characterized using X-ray diffractometry (XRD), energy dispersive x-ray spectrometry (EDX), scanning electron microscopy (SEM), carbon sulphur analyzer and chemical analysis method. Degree of metallization of the reduced nuggets is 78.9% by using boiler grade coal. The pre-reduced nuggets with lesser sulphur content could be used in the blast furnace as raw materials or coolant which would reduce the high quality of coke rate of the furnace due to its pre-reduced character. These can be used in Basic Oxygen Furnace (BOF) as coolant also.

Keywords: alternative ironmaking, coal gasification, extent of reduction, nugget making, syngas based DRI, solid state reduction

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Authors: T. Abbas, J. McEvoy, E. Khan

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Pesticide contamination in water supply is a common environmental problem in rural agricultural communities. Advanced water treatment processes such as membrane filtration and adsorption on activated carbon only remove pesticides from water without degrading them into less toxic/easily degradable compounds leaving behind contaminated brine and activated carbon that need to be managed. Rural communities which normally cannot afford expensive water treatment technologies need an economical and sustainable filter which not only treats pesticides from water but also degrades them into benign products. In this study, iron turning waste experimented as potential point-of-use filtration media for the removal/degradation of a mixture of six chlorinated pesticides (lindane, heptachlor, endosulfan, dieldrin, endrin, and DDT) in water. As a common and traditional medium for water filtration, sand was also tested along with iron turning waste. Iron turning waste was characterized using scanning electron microscopy and energy dispersive X-Ray analyzer. Four glass columns with different filter media layer configurations were set up: (1) only sand, (2) only iron turning, (3) sand and iron turning (two separate layers), and (4) sand, iron turning and sand (three separate layers). The initial pesticide concentration and flow rate were 2 μg/L and 10 mL/min. Results indicate that sand filtration was effective only for the removal of DDT (100%) and endosulfan (94-96%). Iron turning filtration column effectively removed endosulfan, endrin, and dieldrin (85-95%) whereas the lindane and DDT removal were 79-85% and 39-56%, respectively. The removal efficiencies for heptachlor, endosulfan, endrin, dieldrin, and DDT were 90-100% when sand and iron turning waste (two separate layers) were used. However, better removal efficiencies (93-100%) for five out of six pesticides were achieved, when sand, iron turning and sand (three separate layers) were used as filtration media. Moreover, the effects of water pH, amounts of media, and minerals present in water such as magnesium, sodium, calcium, and nitrate on the removal of pesticides were examined. Results demonstrate that iron turning waste efficiently removed all the pesticides under studied parameters. Also, it completely de-chlorinated all the pesticides studied and based on the detection of by-products, the degradation mechanisms for all six pesticides were proposed.

Keywords: pesticide contamination, rural communities, iron turning waste, filtration

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Authors: Venkataraman Sivasankar, Kiyoshi Omine, Hideaki Sano

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The leaching of fluoride from Plaster Board Waste (PBW) is quite feasible in soil and water environments. The Ministry of Environment, Japan recommended the standard limit of 0.8 mgL⁻¹ or less for fluoride. Although the utilization of PBW as a substitute for cement is rather meritorious, its fluoride leaching behavior deteriorates the quality of soil and water and therefore envisaged as a demerit. In view of this fluoride leaching problem, the present research is focused on immobilizing fluoride in PBW. The immobilization experiments were conducted with four chemical systems operated by DAHP (diammonium hydrogen phosphate) and phosphoric acid carbonization of bamboo mass coupled with certain inorganic reactions using reagents such as calcium hydroxide, sodium hydroxide, and aqueous ammonia. The fluoride immobilization was determined after shaking the reactor contents including the plaster board waste for 24 h at 25˚C. In the DAHP system, the immobilization of fluoride was evident from the leaching of fluoride in the range 0.071-0.12 mgL⁻¹, 0.026-0.14 mgL⁻¹ and 0.068-0.12 mgL⁻¹ for the reaction temperatures at 30˚C, 50˚C, and 90˚C, respectively, with final pH of 6.8. The other chemical systems designated as PACCa, PACAm, and PACNa could immobilize fluoride in PBW, and the resulting solution was analyzed with the fluoride less than the Japanese environmental standard of 0.8 mgL⁻¹. In the case of PACAm and PACCa systems, the calcium concentration was found undetectable and witnessed the formation of phosphate compounds. The immobilization of fluoride was found inversely proportional to the increase in the volume of leaching solvent and dose of PBW. Characterization studies of PBW and the solid after fluoride immobilization was done using FTIR (Fourier transform infrared spectroscopy), Raman spectroscopy, FE-SEM ( Field Emission Scanning Electron Microscopy) with EDAX (Energy Dispersive Spectroscopy), XRD (X-ray diffraction), and XPS (X-ray photoelectron spectroscopy). The results revealed the formation of new calcium phosphate compounds such as apatite, monetite, and hydroxylapatite. The participation of such new compounds in fluoride immobilization seems indispensable through the exchange mechanism of hydroxyl and fluoride groups. Acknowledgment: First author thanks to Japanese Society for the Promotion of Science (JSPS) for the award of the fellowship (ID No. 16544).

Keywords: characterization, fluoride, immobilization, plaster board waste

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Authors: Manisha Choudhary, Sudarsan Neogi

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Malachite green (MG), an organic basic dye, has been widely used for the dyeing purpose, as well as a fungicide and antiseptic in aquaculture industry to control fish parasites and disease. However, MG has now turned out to be an extremely controversial compound due to its adverse impact on living beings. Due to high toxicity, proper treatment of wastewater containing MG is utmost important. Among different available technologies, adsorption process is one of the most efficient and cost-effective treatment method due to its simplicity of design, ease of operation and regeneration of used materials. Nonetheless, commercial activated carbon is expensive leading the researchers to focus on utilizing natural resources. In the present work, a species of cactus, Opuntia ficus-indica (OFI), was used to develop a highly efficient, low-cost powdered activated carbon by chemical activation using NaOH. The biosorbent was characterized by Fourier-transform infrared spectroscopy, field emission scanning electron microscope, energy-dispersive X-ray spectroscopy, Brunauer–Emmett–Teller (BET) and X-ray diffraction analysis. Batch adsorption studies were performed to remove MG from an aqueous solution as a function of contact time, initial solution pH, initial dye concentration, biosorbent dosages, the presence of salt and temperature. By increasing the initial dye concentration from 100 to 500 mg/l, adsorption capacity increased from 165.45 to 831.58 mg/g. The adsorption kinetics followed the pseudo-second-order model and the chemisorption mechanisms were revealed. The electrostatic attractions and chemical interactions were observed between amino and hydroxyl groups of the biosorbent and amine groups of the dye. The adsorption was solely controlled by film diffusion. Different isotherm models were used to fit the adsorption data. The excellent recovery of adsorption efficiency after the regeneration of biosorbent indicated the high potential of this adsorbent to remove MG from aqueous solution and an excellent cost-effective biosorbent for wide application in wastewater treatment.

Keywords: adsorption, biosorbent, cactus, malachite green

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Authors: Abidullah, Basharat Hussain, Jong Seok Kim

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Polymer electrolyte membrane fuel cell (PEMFC) is an electrochemical cell, which undergoes an oxygen reduction reaction to produce electrical energy. Platinum (Pt) metal has been used as a catalyst since its inception, but expensiveness is the major obstacle in the commercialization of fuel cells. Herein a non-precious group metal (NPGM) is employed instead of Pt to reduce the cost of PEMFCs. Manganese dioxide impregnated carbon nanotubes (MnO₂-CNTs composite) is a catalyst having excellent electrochemical properties and offers a better alternative to the Platinum-based PEMFC. The catalyst is synthesized by impregnating the transition metal on large surface carbonaceous CNTs by hydrothermal synthesis techniques. To enhance the catalytic activity and increase the volumetric current density, the sample was pyrolyzed at 800ᵒC under a nitrogen atmosphere. During pyrolysis, the nitrogen was doped in the framework of CNTs. Then the material was treated with acid for removing the unreacted metals and adding oxygen functional group to the CNT framework. This process ameliorates the catalytic activity of the manganese-based catalyst. The catalyst has been characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and the catalyst activity has been examined by rotating disc electrode (RDE) experiment. The catalyst was strong enough to withstand an austere alkaline environment in experimental conditions and had a high electrocatalytic activity for oxygen reduction reaction (ORR). Linear Sweep Voltammetry (LSV) depicts an excellent current density of -4.0 mA/cm² and an overpotential of -0.3V vs. standard calomel electrode (SCE) in 0.1M KOH electrolyte. Rotating disk electrode (RDE) was conducted at 400, 800, 1200, and 1600 rpm. The catalyst exhibited a higher methanol tolerance and long term durability with respect to commercial Pt/C. The results for MnO₂-CNT show that the low-cost catalyst will supplant the expensive Pt/C catalyst in the fuel cell.

Keywords: carbon nanotubes, methanol fuel cell, oxygen reduction reaction, MnO₂-CNTs

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Authors: A. Sezai Sarac

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Acrylonitrile (AN) copolymers with typical comonomers of vinyl acetate (VAc) or methyl acrylate (MA) exhibit better mechanical behaviors than its homopolymer. To increase processability of conjugated polymer, and to obtain a hybrid nano-structure multi-stepped emulsion polymerization was applied. Such products could be used in, i.e., drug-delivery systems, biosensors, gas-sensors, electronic compounds, etc. Incorporation of a number of flexible comonomers weakens the dipolar interactions among CN and thereby decreases melting point or increases decomposition temperatures of the PAN based copolymers. Hence, it is important to consider the effect of comonomer on the properties of PAN-based copolymers. Acrylonitrile vinylacetate (AN–VAc ) copolymers have the significant effect to their thermal behavior and are also of interest as precursors in the production of high strength carbon fibers. AN is copolymerized with one or two comonomers, particularly with vinyl acetate The copolymer of AN and VAc can be used either as a plastic (VAc > 15 wt %) or as microfibers (VAc < 15 wt %). AN provides the copolymer with good processability, electrochemical and thermal stability; VAc provides the mechanical stability. The free radical copolymerization of AN and VAc copolymer and core Shell structure of polyprrole composites,and nanofibers of poly(m-anthranilic acid)/polyacrylonitrile blends were recently studied. Free radical copolymerization of acrylonitrile (AN) – with different comonomers, i.e. acrylates, and styrene was realized using ammonium persulfate (APS) in the presence of a surfactant and in-situ polymerization of conjugated polymers was performed in this reaction medium to obtain core-shell nano particles. Nanofibers of such nanoparticles were obtained by electrospinning. Morphological properties of nanofibers are investigated by scanning electron microscopy (SEM) and atomic force spectroscopy (AFM). Nanofibers are characterized using Fourier Transform Infrared - Attenuated Total Reflectance spectrometer (FTIR-ATR), Nuclear Magnetic Resonance Spectroscopy (1H-NMR), differential scanning calorimeter (DSC), thermal gravimetric analysis (TGA), and Electrochemical Impedance Spectroscopy. The electrochemical Impedance results of the nanofibers were fitted to an equivalent curcuit by modelling (ECM).

Keywords: core shell nanoparticles, nanofibers, ascrylonitile copolymers, hybrid nanostructures

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Authors: Farha Mizana Shamsudin, Shahidan Radiman, Yusof Abdullah, Nasri Abdul Hamid

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Oxide dispersion strengthened (ODS) ferritic steels are amongst the most promising candidates for large scale structural materials to be applied in next generation fission and fusion nuclear power reactors. This kind of material is relatively stable at high temperature, possess remarkable mechanical properties and comparatively good resistance from neutron radiation damage. The superior performance of ODS ferritic steels over their conventional properties is attributed to the high number density of nano-sized dispersoids that act as nucleation sites and stable sinks for many small helium bubbles resulting from irradiation, and also as pinning points to dislocation movement and grain growth. ODS ferritic steels are usually produced by powder metallurgical routes involving mechanical alloying (MA) process of Y2O3 and pre-alloyed or elemental metallic powders, and then consolidated by hot isostatic pressing (HIP) or hot extrusion (HE) techniques. In this study, Fe-14Cr-3W-0.5Ti-0.3Y₂O₃ (designated as 14YWT) was produced by mechanical alloying process and followed by hot isostatic pressing (HIP) technique. Crystal structure and morphology of this sample were identified and characterized by using X-ray Diffraction (XRD) and field emission scanning electron microscope (FESEM) respectively. The magnetic measurement of this sample at room temperature was carried out by using a vibrating sample magnetometer (VSM). FESEM micrograph revealed a homogeneous microstructure constituted by fine grains of less than 650 nm in size. The ultra-fine dispersoids of size between 5 nm to 19 nm were observed homogeneously distributed within the BCC matrix. The EDS mapping reveals that the dispersoids contain Y-Ti-O nanoclusters and from the magnetization curve plotted by VSM, this sample approaches the behavior of soft ferromagnetic materials. In conclusion, ODS Fe-14Cr-3W-0.5Ti-0.3Y₂O₃ (14YWT) ferritic steel was successfully produced by HIP technique in this present study.

Keywords: hot isostatic pressing, magnetization, microstructure, ODS ferritic steel

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Authors: Laura Bravo-García, Gotzone Barandika, Begoña Bazán, M. Karmele Urtiaga, Luis M. Lezama, María I. Arriortua

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Solid coordination networks (SCNs) are materials consisting of metal ions or clusters that are linked by polyfunctional organic ligands and can be designed to form tridimensional frameworks. Their structural features, as for example high surface areas, thermal stability, and in other cases large cavities, have opened a wide range of applications in fields like drug delivery, host-guest chemistry, biomedical imaging, chemical sensing, heterogeneous catalysis and others referred to greenhouse gases storage or even separation. In this sense, the use of polycarboxylate anions and dipyridyl ligands is an effective strategy to produce extended structures with the needed characteristics for these applications. In this context, a novel compound, [Cu4(m-BDC)4(bpa)2DMF]•DMF has been obtained by microwave synthesis, where m-BDC is 1,3-benzenedicarboxylate and bpa 1,2-bis(4-pyridyl)ethane. The crystal structure can be described as a three dimensional framework formed by two equal, interpenetrated networks. Each network consists of two different CuII dimers. Dimer 1 have two coppers with a square pyramidal coordination, and dimer 2 have one with a square pyramidal coordination and other with octahedral one, the last dimer is unique in literature. Therefore, the combination of both type of dimers is unprecedented. Thus, benzenedicarboxylate ligands form sinusoidal chains between the same type of dimers, and also connect both chains forming these layers in the (100) plane. These layers are connected along the [100] direction through the bpa ligand, giving rise to a 3D network with 10 Å2 voids in average. However, the fact that there are two interpenetrated networks results in a significant reduction of the available volume. Structural analysis was carried out by means of single crystal X-ray diffraction and IR spectroscopy. Thermal and magnetic properties have been measured by means of thermogravimetry (TG), X-ray thermodiffractometry (TDX), and electron paramagnetic resonance (EPR). Additionally, CO2 and CH4 high pressure adsorption measurements have been carried out for this compound.

Keywords: gas adsorption, interpenetrated networks, magnetic measurements, solid coordination network (SCN), thermal stability

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Authors: Yulistiani, Muhammad Amin, Fasich

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A surface charge of the nanoparticle is a very important consideration in pulmonal drug delivery system. The zeta potential (ZP) is related to the surface charge which can predict stability of nanoparticles as nebules of liposomal amikacin. Anionic lipid such as 1,2-dipalmitoyl-sn-glycero-3-phosphatidylglycerol (DPPG) is expected to contribute to the physical stability of liposomal amikacin and the optimal ZP value. Suitable ZP can improve drug release profiles at specific sites in alveoli as well as their stability in dosage form. This study aimed to analyze the effect of DPPG on ZP values and physical stability of liposomal amikacin. Liposomes were prepared by using the reserved phase evaporation method. Liposomes consisting of DPPG, 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC), cholesterol and amikacin were formulated in five different compositions 0/150/5/100, 10//150/5/100, 20/150/5/100, 30/150/5/100 and 40/150/5/100 (w/v) respectively. A chloroform/methanol mixture in the ratio of 1 : 1 (v/v) was used as solvent to dissolve lipids. These systems were adjusted in the phosphate buffer at pH 7.4. Nebules of liposomal amikacin were produced by using the vibrating nebulizer and then characterized by the X-ray diffraction, differential scanning calorimetry, particle size and zeta potential analyzer, and scanning electron microscope. Amikacin concentration from liposome leakage was determined by the immunoassay method. The study revealed that presence of DPPG could increase the ZP value. The addition of 10 mg DPPG in the composition resulted in increasing of ZP value to 3.70 mV (negatively charged). The optimum ZP value was reached at -28.780 ± 0.70 mV and particle size of nebules 461.70 ± 21.79 nm. Nebulizing process altered parameters such as particle size, conformation of lipid components and the amount of surface charges of nanoparticles which could influence the ZP value. These parameters might have profound effects on the application of nebules in the alveoli; however, negatively charge nanoparticles were unexpected to have a high ZP value in this system due to increased macrophage uptake and pulmonal clearance. Therefore, the ratio of liposome 20/150/5/100 (w/v) resulted in the most stable colloidal system and might be applicable to pulmonal drug delivery system.

Keywords: anionic lipid, dipalmitoylphosphatidylglycerol, liposomal amikacin, stability, zeta potential

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Authors: L. Ebralidze, A. Tsertsvadze, D. Berashvili, A. Bakuridze

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Current cancer therapy strategies are based on surgery, radiotherapy and chemotherapy. The problems associated with chemotherapy are one of the biggest challenges for clinical medicine. These include: low specificity, broad spectrum of side effects, toxicity and development of cellular resistance. Therefore, anti-cance drugs need to be develop urgently. Particularly, in order to increase efficiency of anti-cancer drugs and reduce their side effects, scientists work on formulation of nano-drugs. The objective of this study was to develop composition and technology of vincristine nanoparticles using high-molecular carbohydrates of plant origin. Plant polysacharides, particularly, soy bean seed polysaccharides, flaxseed polysaccharides, citrus pectin, gum arabic, sodium alginate were used as objects. Based on biopharmaceutical research, vincristine containing nanoparticle formulations were prepared. High-energy emulsification and solvent evaporation methods were used for preparation of nanosystems. Polysorbat 80, polysorbat 60, sodium dodecyl sulfate, glycerol, polyvinyl alcohol were used in formulation as emulsifying agent and stabilizer of the system. The ratio of API and polysacharides, also the type of the stabilizing and emulsifying agents are very effective on the particle size of the final product. The influence of preparation technology, type and concentration of stabilizing agents on the properties of nanoparticles were evaluated. For the next stage of research, nanosystems were characterized. Physiochemical characterization of nanoparticles: their size, shape, distribution was performed using Atomic force microscope and Scanning electron microscope. The present study explored the possibility of production of NPs using plant polysaccharides. Optimal ratio of active pharmaceutical ingredient and plant polysacharids, the best stabilizer and emulsifying agent was determined. The average range of nanoparticles size and shape was visualized by SEM.

Keywords: nanoparticles, target delivery, natural high molecule carbohydrates, surfactants

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Authors: Seyedeh Mozhgan Seyed-Talebi, Javad Beheshtian

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The toxicity of lead associated with the lifecycle of perovskite solar cells (PSCs( is a serious concern which may prove to be a major hurdle in the path toward their commercialization. The current proposed lead-free PSCs including Ag(I), Bi(III), Sb(III), Ti(IV), Ge(II), and Sn(II) low-toxicity cations are still plagued with the critical issues of poor stability and low efficiency. This is mainly because of their chemical stability. In the present research, utilization of all inorganic CsSnGeI₃ based materials offers the advantages to enhance resistance of device to degradation, reduce the cost of cells, and minimize the carrier recombination. The presence of inorganic halide perovskite improves the photovoltaic parameters of PCSs via improved surface coverage and stability. The inverted structure of simulated devices using a 1D simulator like solar cell capacitance simulator (SCAPS) version 3308 involves TCOHTL/Perovskite/ETL/Au contact layer. PEDOT:PSS, PCBM, and CsSnGeI₃ used as hole transporting layer (HTL), electron transporting layer (ETL), and perovskite absorber layer in the inverted structure for the first time. The holes are injected from highly stable and air tolerant Sn_0.5Ge_0.5I₃ perovskite composition to HTM and electrons from the perovskite to ETL. Simulation results revealed a great dependence of power conversion efficiency (PCE) on the thickness and defect density of perovskite layer. Here the effect of an increase in operating temperature from 300 K to 400 K on the performance of CsSnGeI₃ based perovskite devices is investigated. Comparison between simulated CsSnGeI₃ based PCSs and similar real testified devices with spiro-OMeTAD as HTL showed that the extraction of carriers at the interfaces of perovskite absorber depends on the energy level mismatches between perovskite and HTL/ETL. We believe that optimization results reported here represent a critical avenue for fabricating the stable, low-cost, efficient, and eco-friendly all-inorganic Cs-Sn-Ge based lead-free perovskite devices.

Keywords: hole transporting layer, lead-free, perovskite solar cell, SCAPS-1D, Sn-Ge based

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Authors: J. Tirano, H. Zea, C. Luhrs

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Photocatalysis has established as viable option in the development of processes for the treatment of pollutants and clean energy production. This option is based on the ability of semiconductors to generate an electron flow by means of the interaction with solar radiation. Owing to its electronic structure, TiO₂ is the most frequently used semiconductors in photocatalysis, although it has a high recombination of photogenerated charges and low solar energy absorption. An alternative to reduce these limitations is the use of nanostructured morphologies which can be produced during the synthesis of TiO₂ nanotubes (TNTs). Therefore, if possible to produce vertically oriented nanostructures it will be possible to generate a greater contact area with electrolyte and better charge transfer. At present, however, the development of these innovative structures still presents an important challenge for the development of competitive photoelectrochemical devices. This research focuses on established correlations between synthesis variables and 1D nanostructure morphology which has a direct effect on the photocatalytic performance. TNTs with controlled morphology were synthesized by two-step potentiostatic anodization of titanium foil. The anodization was carried out at room temperature in an electrolyte composed of ammonium fluoride, deionized water and ethylene glycol. Consequent thermal annealing of as-prepared TNTs was conducted in the air between 450 °C-550 °C. Morphology and crystalline phase of the TNTs were carried out by SEM, EDS and XRD analysis. As results, the synthesis conditions were established to produce nanostructures with specific morphological characteristics. Anatase was the predominant phase of TNTs after thermal treatment. Nanotubes with 10 μm in length, 40 nm in pore diameter and a surface-volume ratio of 50 are important in photoelectrochemical applications based on TiO₂ due to their 1D characteristics, high surface-volume ratio, reduced radial dimensions and high oxide/electrolyte interface. Finally, this knowledge can be used to improve the photocatalytic activity of TNTs by making additional surface modifications with dopants that improve their efficiency.

Keywords: electrochemical anodization, morphology, self-organized nanotubes, TiO₂ nanotubes

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Authors: John Olorunfemi Abe, Olawale Muhammed Popoola, Abimbola Patricia Idowu Popoola

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Hydrogen is an appealing alternative to fossil fuels because of its abundance, low weight, high energy density, and relative lack of contaminants. However, its low density presents a number of storage challenges. Therefore, this work studies the influence of refractory nitride additives consisting of 5 wt. % each of hexagonal boron nitride (h-BN), titanium nitride (TiN), and aluminum nitride (AlN) on hydrogen storage and electrochemical characteristics of Ti6Al4V-based materials produced by spark plasma sintering. The microstructure and phase constituents of the sintered materials were characterized using scanning electron microscopy (in conjunction with energy-dispersive spectroscopy) and X-ray diffraction, respectively. Pressure-composition-temperature (PCT) measurements were used to assess the hydrogen absorption/desorption behavior, kinetics, and storage capacities of the sintered materials, respectively. The pure Ti6Al4V alloy displayed a two-phase (α+β) microstructure, while the modified composites exhibited apparent microstructural modifications with the appearance of nitride-rich secondary phases. It is found that the diffusion process controls the kinetics of the hydrogen absorption. Thus, a faster rate of hydrogen absorption at elevated temperatures ensued. The additives acted as catalysts, lowered the activation energy and accelerated the rate of hydrogen sorption in the composites relative to the monolithic alloy. Ti6Al4V-5 wt. % h-BN appears to be the most promising candidate for hydrogen storage (2.28 wt. %), followed by Ti6Al4V-5 wt. % TiN (2.09 wt. %), whereas Ti6Al4V-5 wt. % AlN shows the least hydrogen storage performance (1.35 wt. %). Accordingly, the developed hydride system (Ti6Al4V-5h-BN) may be competitive for use in applications involving short-range continuous vehicles (~50-100km) as well as stationary applications such as electrochemical devices, large-scale storage cylinders in hydrogen production locations, and hydrogen filling stations.

Keywords: hydrogen storage, Ti6Al4V hydride system, pressure-composition-temperature measurements, refractory nitride additives, spark plasma sintering, Ti6Al4V-based materials

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Authors: Abd El Rahman Mohamed

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Canopic jars made by the ancient Egyptians from different materials were used to preserve the viscera during the mummification process. The canopic jar studied here dates back to the Late Period (712-332 BC). It is found in the Grand Egyptian Museum (GEM), Giza, Egypt. This jar was carved from limestone and covered with a monkey head lid with painted eyes and ears with red pigment and surrounded with black pigment. The jar contains bandages of textile containing mummy viscera with resin and black resin blocks. The canopic jars were made using the sculpting tools that were used by the ancient Egyptians, such as metal chisels (made of copper) and hammers and emptying the mass of the jar from the inside using a tool invented by the ancient Egyptians, which called the emptying drill. This study also aims to use analytical techniques to identify the components of the jar, its contents, pigments, and previous restoration materials and to understand its deterioration aspects. Visual assessment, isolation and identification of fungi, optical microscopy (OM), scanning electron microscopy (SEM), X-ray fluorescence spectroscopy (XRF), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR) were used in our study. The jar showed different signs of deterioration, such as dust, dirt, stains, scratches, classifications, missing parts, and breaks; previous conservation materials include using iron wire, completion mortar and an adhesive for assembly. The results revealed that the jar was carved from Dolomite Limestone, red Hematite pigment, Mastic resin, and Linen textile bandages. The previous adhesive was Animal Glue and used Gypsum for the previous completion. The most dominant Microbial infection on the jar was found in the fungi of (Penicillium waksmanii), (Nigrospora sphaerica), (Actinomycetes sp) and (Spore-Forming Gram-Positive Bacilli). Conservation procedures have been applied with high accuracy to conserve the jar, including mechanical and chemical cleaning, re-assembling, completion and consolidation.

Keywords: Canopic jar, Consolidation, Mummification, Resin, Viscera.

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Authors: Aidan Battison, Neliswa Mama

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Environmental pollution by ionic species has been identified as one of the biggest challenges to the sustainable development of communities. The widespread use of organic and inorganic chemical products and the release of toxic chemical species from industrial waste have resulted in a need for advanced monitoring technologies for environment protection, remediation and restoration. Some of the disadvantages of conventional sensing methods include expensive instrumentation, well-controlled experimental conditions, time-consuming procedures and sometimes complicated sample preparation. On the contrary, the development of fluorescent chemosensors for biological and environmental detection of metal ions has attracted a great deal of attention due to their simplicity, high selectivity, eidetic recognition, rapid response and real-life monitoring. Coumarin derivatives S1 and S2 (Scheme 1) containing 1,2,3-triazole moieties at position -3- have been designed and synthesized from azide and alkyne derivatives by CuAAC “click” reactions for the detection of metal ions. These compounds displayed a strong preference for Fe3+ ions with complexation resulting in fluorescent quenching through photo-induced electron transfer (PET) by the “sphere of action” static quenching model. The tested metal ions included Cd2+, Pb2+, Ag+, Na+, Ca2+, Cr3+, Fe3+, Al3+, Cd2+, Ba2+, Cu2+, Co2+, Hg2+, Zn2+ and Ni2+. The detection limits of S1 and S2 were determined to be 4.1 and 5.1 uM, respectively. Compound S1 displayed the greatest selectivity towards Fe3+ in the presence of competing for metal cations. S1 could also be used for the detection of Fe3+ in a mixture of CH3CN/H¬2¬O. Binding stoichiometry between S1 and Fe3+ was determined by using both Jobs-plot and Benesi-Hildebrand analysis. The binding was shown to occur in a 1:1 ratio between the sensor and a metal cation. Reversibility studies between S1 and Fe3+ were conducted by using EDTA. The binding site of Fe3+ to S1 was determined by using 13 C NMR and Molecular Modelling studies. Complexation was suggested to occur between the lone-pair of electrons from the coumarin-carbonyl and the triazole-carbon double bond.

Keywords: chemosensor, "click" chemistry, coumarin, fluorescence, static quenching, triazole

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Authors: Vadim V. Zefirov, Victor E. Sizov, Marina A. Pigaleva, Igor V. Elmanovich, Mikhail S. Kondratenko, Marat O. Gallyamov

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This work presents a novel method for treating porous hydrophobic polyolefin membranes using supercritical carbon dioxide that allows usage of the modified membrane in redox flow batteries with an aqueous electrolyte. Polyolefin membranes are well known and widely used, however, they cannot be used as separators in redox flow batteries with an aqueous electrolyte since they have insufficient wettability, and therefore do not provide sufficient proton conductivity. The main aim of the presented work was the development of hydrophilic composites based on cheap membranes and precursors. Supercritical fluid was used as a medium for the deposition of the hydrophilic phase on the hydrophobic surface of the membrane. Due to the absence of negative capillary effects in a supercritical medium, a homogeneous composite is obtained as a result of synthesis. The in-situ synthesized silicon oxide nanoparticles and the chitosan polymer layer act as the hydrophilic phase and not only increase the affinity of the membrane towards the electrolyte, but also reduce the pore size of the polymer matrix, which positively affects the ion selectivity of the membrane. The composite material obtained as a result of synthesis has enhanced hydrophilic properties and is capable of providing proton conductivity in redox flow batteries. The morphology of the obtained composites was characterized by electron microscopy. To analyze the phase composition, infrared spectroscopy was used. The hydrophilic properties were studied by water contact angle measurements. In addition, the proton conductivity and ion selectivity of the obtained samples were studied, and tests in real redox flow batteries were performed. As a result, modified membrane was characterised in detail and moreover it was shown that modified cheap polyolefin membranes have pronounced proton conductivity and high ion selectivity, so their performance in a real redox flow battery approaches expensive commercial analogues, reaching 70% of energy efficiency.

Keywords: carbon dioxide, chitosan, polymer membrane, redox flow batteries, silica nanoparticles, supercritical fluid

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Authors: Siming Wang, Qing Ni, Yu Wu, Ruihai Xu, Hong Ye

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Porous electric heaters, compared to conventional electric heaters, exhibit excellent heating performance due to their large specific surface area. Porous electric heaters employ porous metallic materials or conductive porous ceramics as the heating element. The former attains a low heating power with a fixed current due to the low electrical resistivity of metal. Although the latter can bypass the inherent challenges of porous metallic materials, the fabrication process of the conductive porous ceramics is complicated and high cost. This work proposed a porous ceramic electric heater with dielectric honeycomb ceramic as a substrate and surface conductive coating as a heating element. The conductive coating was prepared by the sol-gel method using silica sol and methyl trimethoxysilane as raw materials and graphite powder as conductive fillers. The conductive mechanism and degradation reason of the conductive coating was studied by electrical resistivity and thermal stability analysis. The heating performance of the proposed heater was experimentally investigated by heating air and deionized water. The results indicate that the electron transfer is achieved by forming the conductive network through the contact of the graphite flakes. With 30 wt% of graphite, the electrical resistivity of the conductive coating can be as low as 0.88 Ω∙cm. The conductive coating exhibits good electrical stability up to 500°C but degrades beyond 600°C due to the formation of many cracks in the coating caused by the weight loss and thermal expansion. The results also show that the working medium has a great influence on the volume power density of the heater. With air under natural convection as the working medium, the volume power density attains 640.85 kW/m3, which can be increased by 5 times when using deionized water as the working medium. The proposed honeycomb ceramic electric heater has the advantages of the simple fabrication method, low cost, and high volume power density, demonstrating great potential in the fluid heating field.

Keywords: conductive coating, honeycomb ceramic electric heater, high specific surface area, high volume power density

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Authors: Lucija Pustahija, Christine Bandl, Wolfgang Kern, Christian Mitterer

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Concerning today´s ecological demands, producing reliable materials from sustainable resources is a continuously developing topic. Such an example is the production of carbon materials via pyrolysis of natural gases or biomass. The amazing properties of pyrolytic carbon are utilized in various fields, where in particular the application in building industry is a promising way towards the utilization of pyrolytic carbon and composites based on pyrolytic carbon. For many applications, surface modification of carbon is an important step in tailoring its properties. Therefore, in this paper, an investigation of different oxidation methods was performed to prepare the carbon surface before functionalizing it with organosilanes, which act as coupling agents for epoxy and polyurethane resins. Made in such a way, a building material based on carbon composites could be used as a lightweight, durable material that can be applied where water or air filtration / purification is needed. In this work, both wet and dry oxidation were investigated. Wet oxidation was first performed in solutions of nitric acid (at 120 °C and 150 °C) followed by oxidation in hydrogen peroxide (80 °C) for 3 and 6 h. Moreover, a hydrothermal method (under oxygen gas) in autoclaves was investigated. Dry oxidation was performed under plasma and corona discharges, using different power values to elaborate optimum conditions. Selected samples were then (in preliminary experiments) subjected to a silanization of the surface with amino and glycidoxy organosilanes. The functionalized surfaces were examined by X-ray photon spectroscopy and Fourier transform infrared spectroscopy spectroscopy, and by scanning electron microscopy. The results of wet and dry oxidation methods indicated that the creation of functionalities was influenced by temperature, the concentration of the reagents (and gases) and the duration of the treatment. Sequential oxidation in aq. HNO₃ and H₂O₂ results in a higher content of oxygen functionalities at lower concentrations of oxidizing agents, when compared to oxidizing the carbon with concentrated nitric acid. Plasma oxidation results in non-permanent functionalization on the carbon surface, by which it´s necessary to find adequate parameters of oxidation treatments that could enable longer stability of functionalities. Results of the functionalization of the carbon surfaces with organosilanes will be presented as well.

Keywords: building materials, dry oxidation, organosilanes, pyrolytic carbon, resins, surface functionalization, wet oxidation

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Authors: Kausar Harun, Ahmad Azmin Mohamad

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Zinc oxide (ZnO) has been extensively used in optoelectronic devices, with recent interest as photoanode material in dye-sensitize solar cell. Numerous methods employed to experimentally synthesized ZnO, while some are theoretically-modeled. Both approaches provide information on ZnO properties, but theoretical calculation proved to be more accurate and timely effective. Thus, integration between these two methods is essential to intimately resemble the properties of synthesized ZnO. In this study, experimentally-grown ZnO nanoparticles were prepared by sol-gel storage method with zinc acetate dihydrate and methanol as precursor and solvent. A 1 M sodium hydroxide (NaOH) solution was used as stabilizer. The optimum time to produce ZnO nanoparticles were recorded as 12 hours. Phase and structural analysis showed that single phase ZnO produced with wurtzite hexagonal structure. Further work on quantitative analysis was done via Rietveld-refinement method to obtain structural and crystallite parameter such as lattice dimensions, space group, and atomic coordination. The lattice dimensions were a=b=3.2498Å and c=5.2068Å which were later used as main input in first-principles calculations. By applying density-functional theory (DFT) embedded in CASTEP computer code, the structure of synthesized ZnO was built and optimized using several exchange-correlation functionals. The generalized-gradient approximation functional with Perdew-Burke-Ernzerhof and Hubbard U corrections (GGA-PBE+U) showed the structure with lowest energy and lattice deviations. In this study, emphasize also given to the modification of valence electron energy level to overcome the underestimation in DFT calculation. Both Zn and O valance energy were fixed at Ud=8.3 eV and Up=7.3 eV, respectively. Hence, the following electronic and optical properties of synthesized ZnO were calculated based on GGA-PBE+U functional within ultrasoft-pseudopotential method. In conclusion, the incorporation of Rietveld analysis into first-principles calculation was valid as the resulting properties were comparable with those reported in literature. The time taken to evaluate certain properties via physical testing was then eliminated as the simulation could be done through computational method.

Keywords: density functional theory, first-principles, Rietveld-refinement, ZnO nanoparticles

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Authors: S. Varnagiris, M. Urbonavicius, S. Tuckute, M. Lelis, K. Bockute

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Amongst many water purification techniques, TiO₂ photocatalysis is recognized as one of the most promising sustainable methods. It is known that for photocatalytical applications anatase is the most suitable TiO₂ phase, however heterojunction of anatase/rutile phases could improve the photocatalytical activity of TiO₂ even further. Despite the relative simplicity of TiO₂ different synthesis methods lead to the highly dispersed crystal phases and photocatalytic activity of the corresponding samples. Accordingly, suggestions and investigations of various innovative methods of TiO₂ synthesis are still needed. In this work structural and photocatalytical properties of TiO₂ films deposited by the unconventional method of simultaneous co-sputtering from two magnetrons powered by pulsed-Direct Current (pDC) and Radio Frequency (RF) power sources with negative bias voltage have been studied. More specifically, TiO₂ film thickness, microstructure, surface roughness, crystal structure, optical transmittance and photocatalytical properties were investigated by profilometer, scanning electron microscope, atomic force microscope, X-ray diffractometer and UV-Vis spectrophotometer respectively. The proposed unconventional two magnetron co-sputtering based TiO₂ film formation method showed very promising results for crystalline TiO₂ film formation while keeping process temperatures below 100 °C. XRD analysis revealed that by using proper combination of power source type and bias voltage various TiO₂ phases (amorphous, anatase, rutile or their mixture) can be synthesized selectively. Moreover, strong dependency between power source type and surface roughness, as well as between the bias voltage and band gap value of TiO₂ films was observed. Interestingly, TiO₂ films deposited by two magnetron co-sputtering without bias voltage had one of the highest band gap values between the investigated films but its photocatalytic activity was superior compared to all other samples. It is suggested that this is due to the dominating nanocrystalline anatase phase with various exposed surfaces including photocatalytically the most active {001}.

Keywords: films, magnetron co-sputtering, photocatalysis, TiO₂

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Authors: Muhammad Naeem, Juho Lee, Jin-Wook Yoo

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In this study, we hypothesized that prolonged gastrointestinal transit at the inflamed colon conferred by a pH-triggered mucoadhesive smart nanoparticulate drug delivery system aids in achieving selective and sustained levels of the drug within the inflamed colon for the treatment of ulcerative colitis. We developed budesonide-loaded pH-sensitive charge-reversal solid lipid nanoparticles (SLNs) using a hot homogenization method. Polyetylenimine (PEI) was used to render SLNs cationic (PEI-SLNs). Eudragit S100 (ES) was coated on PEI-SLNs for pH-trigger charge-reversal SLNs (ES-PEI-SLNs). Therapeutic potential of the prepared SNLs formulation was evaluated in ulcerative colitis in mice. The transmission electron microscopy, zeta size and zeta potential data showed the successful formation of SLNs formulations. SLNs and PEI-SLNs showed burst drug release in acidic pH condition mimicking stomach and early small intestine environment which limiting their application as oral delivery systems. However, ES-PEI-SLNs prevented a burst drug release in acidic pH conditions and showed sustained release at a colonic pH. Most importantly, the surface charge of ES-PEI-SLNs switched from negative to positive in colonic conditions by pH-triggered removal of ES coating and accumulated selectively in inflamed colon. Furthermore, a charge reversal ES-PEI-SLNs showed a superior mitigation of dextran sulfate sodium (DSS)-induced acute colitis in mice as compared to SLNs and PEI-SLNs treated groups. Moreover, histopathological analysis of distal colon sections stained with hematoxylin/eosin and E-cadherin immunostaining revealed attenuated inflammation in an ES-PEI-SLNs-treated group. We also found that ES-PEI-SLNs markedly reduced the myeloperoxidase level and expression of TNF-alpha in colon tissue. Our results suggest that the pH-triggered charge reversal SLNs presented in this study would be a promising approach for ulcerative colitis therapy.

Keywords: solid lipid nanoparticles, stimuli-triggered charge-reversal, ulcerative colitis, methacrylate copolymer, budesonide

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Authors: Caspar S. Carson, Gabriel W. Prather, Nicholas E. Wong, Jeffery R. Anton, William H. McCoy

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Cutibacterium acnes is a commensal bacterium found on human skin that has been linked to acne. C. acnes can also be an opportunistic pathogen when it infiltrates the body during surgery. This pathogen can cause dangerous infections of medical implants, such as shoulder replacements, leading to life-threatening blood infections. Compounding this issue, C. acnes resistance to many antibiotics has become an increasing problem worldwide, creating a need for special forms of treatment. C. acnes expresses the protein RoxP, and it requires this protein to colonize human skin. Though this protein is required for C. acnes skin colonization, its function is not yet understood. Inhibition of RoxP function might be an effective treatment for C. acnes infections. To develop such reagents, the McCoy Laboratory generated four unique anti-RoxP antibodies. Preliminary studies in the McCoy Lab have established that each antibody binds a distinct site on RoxP. To assess the potential of these antibodies as therapeutics, it is necessary to specifically characterize these antibody epitopes and evaluate them in assays that assess their ability to inhibit RoxP-dependent C. acnes growth. To provide material for these studies, an antibody expression construct, Fv-clasp(v2), was adapted to encode anti-RoxP antibody sequences. The author hypothesizes that this expression strategy can produce sufficient amounts of >95% pure antibody fragments for further characterization of these antibodies. Four anti-RoxP Fv-clasp(v2) expression constructs (pET vector-based) were transformed into E. coli BL21-Gold(DE3) cells and a small-scale expression and purification trial was performed for each construct to evaluate anti-RoxP Fv-clasp(v2) yield and purity. Successful expression and purification of these antibody constructs will allow for their use in structural studies, such as protein crystallography and cryogenic electron microscopy. Such studies would help to define the antibody binding sites on RoxP, which could then be leveraged in the development of certain methods to treat C. acnes infection through RoxP inhibition.

Keywords: structural biology, protein expression, infectious disease, antibody, therapeutics, E. coli

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Authors: Gerrit Ter Haar, Thorsten Becker, Deborah Blaine

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The Additive Manufacturing (AM) process of Selective Laser Melting (SLM) has seen an exponential growth in sales and development in the past fifteen years. Whereas the capability of SLM was initially limited to rapid prototyping, progress in research and development (R&D) has allowed SLM to be capable of fully functional parts. This technology is still at a primitive stage and technical knowledge of the vast number of variables influencing final part quality is limited. Ongoing research and development of the sensitive printing process and post processes is of utmost importance in order to qualify SLM parts to meet international standards. Quality concerns in Ti-6Al-4V manufactured through SLM has been identified, which include: high residual stresses, part porosity, low ductility and anisotropic mechanical properties. Whereas significant quality improvements have been made through optimising printing parameters, research indicates as-produced part ductility to be a major limiting factor when compared to its wrought counterpart. This study aims at achieving an in-depth understanding of the underlining links between SLM produced Ti-6Al-4V microstructure and its mechanical properties. Knowledge of microstructural transformation kinetics of Ti-6Al-4V allows for the optimisation of post-process heat treatments thereby achieving the required process route to manufacture high quality SLM produced Ti-6Al-4V parts. Experimental methods used to evaluate the kinematics of microstructural transformation of SLM Ti-6Al-4V are: optical microscopy and electron backscatter diffraction. Results show that a low-temperature heat treatment is capable of transforming the as-produced, martensitic microstructure into a duel-phase microstructure exhibiting both a high strength and improved ductility. Furthermore, isotropy of mechanical properties can be achieved through certain annealing routes. Mechanical properties identical to that of wrought Ti-6Al-4V can, therefore, be achieved through an optimised process route.

Keywords: EBSD analysis, heat treatments, microstructural characterisation, selective laser melting, tensile behaviour, Ti-6Al-4V

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Authors: Asselah Amel, Affif Chaouche M'yassa, Toudji Amira, Tazerouti Amel

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This study covers two aspects ; the biodegradability and the performances in corrosion inhibition of a series of synthetized surfactants namely Φ- sodium methyl ester sulfonates (Φ-MES: C₁₂-MES, C₁₄-MES and C₁₆-MES. The biodegradability of these organic compounds was studied using the respirometric method, ‘the standard ISO 9408’. Degradation was followed by analysis of dissolved oxygen using the dissolved oxygen meter over 28 days and the results were compared with that of sodium dodecyl sulphate (SDS). The inoculum used consists of activated sludge taken from the aeration basin of the biological wastewater treatment plant in the city of Boumerdes-Algeria. In addition, the anticorrosive performances of Φ-MES surfactants on a carbon steel "X70" were evaluated in an injection water from a well of Hassi R'mel region- Algeria, known as Baremian water, and are compared to sodium dodecyl sulphate. Two technics, the weight loss and the linear polarization resistance corrosion rate (LPR) are used allowing to investigate the relationships between the concentrations of these synthetized surfactants and their surface properties, surface coverage and inhibition efficiency. Various adsorption isotherm models were used to characterize the nature of adsorption and explain their mechanism. The results show that the MES anionic surfactants was readily biodegradable, degrading faster than SDS, about 88% for C₁₂-MES compared to 66% for the SDS. The length of their carbon chain affects their biodegradability; the longer the chain, the lower the biodegradability. The inhibition efficiency of these surfactants is around 78.4% for C₁₂-MES, 76.60% for C₁₄-MES and 98.19% for C₁₆-MES and increases with their concentration and reaches a maximum value around their critical micelle concentrations ( CMCs). Scanning electron microscopy coupled to energy dispersive X-ray spectroscopy allowed to the visualization of a good adhesion of the protective film formed by the surfactants to the surface of the steel. The studied surfactants show the Langmuirian behavior from which the thermodynamic parameters as adsorption constant (Kads), standard free energy of adsorption (〖∆G〗_ads^0 ) are determined. Interaction of the surfactants with steel surface have involved physisorptions.

Keywords: corrosion, surfactants, adsorption, adsorption isotherems

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