Search results for: electron backscatter diffraction

Authors: Hubert Beisch, Janik Marx, Svenja Garlof, Roman Shvets, Ivan Grygorchak, Andriy Kityk, Bodo Fiedler

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Three-dimensional carbon materials can be used as electrode materials for energy storage systems such as batteries and supercapacitors. Fast charging and discharging times are realizable without reducing the performance due to aging processes. Furthermore high specific surface area (SSA) of three-dimensional carbon structures leads to high specific capacities. One newly developed carbon foam is Globugraphite. This interconnected globular carbon morphology with statistically distributed hierarchical pores is manufactured by a chemical vapor deposition (CVD) process from ceramic templates resulting from a sintering process. Via scanning electron (SEM) and transmission electron microscopy (TEM), the morphology is characterized. Moreover, the SSA was measured by the Brunauer–Emmett–Teller (BET) theory. Measurements of Globugraphite in an organic and inorganic electrolyte show high energy densities and power densities resulting from ion absorption by forming an electrochemical double layer. A comparison of the specific values is summarized in a Ragone diagram. Energy densities up to 48 Wh/kg and power densities to 833 W/kg could be achieved for an SSA from 376 m²/g to 859 m²/g. For organic electrolyte, a specific capacity of 100 F/g at a density of 20 mg/cm³ was achieved.

Keywords: BET, carbon foam, CVD process, electrochemical cell, Ragone diagram, SEM, TEM

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Authors: Marius Sebastian Secula, Mihaela Darie, Gabriela Carja

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Persistent organic pollutant discharged by various industries or urban regions into the aquatic ecosystems represent a serious threat to fauna and human health. The endocrine disrupting compounds are known to have toxic effects even at very low values of concentration. The anti-inflammatory agent Ibuprofen is an endocrine disrupting compound and is considered as model pollutant in the present study. The use of light energy to accomplish the latest requirements concerning wastewater discharge demands highly-performant and robust photo-catalysts. Many efforts have been paid to obtain efficient photo-responsive materials. Among the promising photo-catalysts, layered double hydroxides (LDHs) attracted significant consideration especially due to their composition flexibility, high surface area and tailored redox features. This work presents Fe(II) self-supported on ZnMeLDHs (Me =Al3+, Fe3+) as novel efficient photo-catalysts for Fenton-like catalysis. The co-precipitation method was used to prepare ZnAlLDH, ZnFeAlLDH and ZnCrLDH (Zn2+/Me3+ = 2 molar ratio). Fe(II) was self-supported on the LDHs matrices by using the reconstruction method, at two different values of weight concentration. X-ray diffraction (XRD), thermogravimetric analysis (TG/DTG), Fourier transform infrared (FTIR) and transmission electron microscopy (TEM) were used to investigate the structural, textural, and micromorphology of the catalysts. The Fe(II)/ZnMeLDHs nano-hybrids were tested for the degradation of a model pharmaceutical agent, the anti-inflammatory agent ibuprofen, by photocatalysis and photo-Fenton catalysis, respectively. The results point out that the embedment Fe(II) into ZnFeAlLDH and ZnCrLDH lead to a slight enhancement of ibuprofen degradation by light irradiation, whereas in case of ZnAlLDH, the degradation process is relatively low. A remarkable enhancement of ibuprofen degradation was found in the case of Fe(II)/ZnMeLDHs by photo-Fenton process. Acknowledgements: This work was supported by a grant of the Romanian National Authority for Scientific Research and Innovation, CNCS - UEFISCDI, project number PN-II-RU-TE-2014-4-0405.

Keywords: layered double hydroxide, heterogeneous Fenton, micropollutant, photocatalysis

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Authors: Sijie Chen, Xiaofang Chen, Juan Wang, Yingying Zhang, Yu Hong, Wanyu Zhuang, Xinxin Huang, Ping Ou, Longsheng Huang

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Purpose: Autistic symptom improvement can be observed in children treated with acupuncture, but the mechanism is still being explored. In the present study, we used scalp acupuncture to treat autism rat model, and then their improvement in the abnormal behaviors and specific mechanisms behind were revealed by detecting animal behaviors, analyzing the RNA sequencing of the prefrontal cortex(PFC), and observing the ultrastructure of PFC neurons under the transmission electron microscope. Methods: On gestational day 12.5, Wistar rats were given valproic acid (VPA) by intraperitoneal injection, and their offspring were considered to be reliable rat models of autism. They were randomized to VPA or VPA-acupuncture group (n=8). Offspring of Wistar pregnant rats that were simultaneously injected with saline were randomly selected as the wild-type group (WT). VPA_acupuncture group rats received acupuncture intervention at 23 days of age for 4 weeks, and the other two groups followed without intervention. After the intervention, all experimental rats underwent behavioral tests. Immediately afterward, they were euthanized by cervical dislocation, and their prefrontal cortex was isolated for RNA sequencing and transmission electron microscopy. Results: The main results are as follows: 1. Animal behavioural tests: VPA group rats showed more anxiety-like behaviour and repetitive, stereotyped behaviour than WT group rats. While VPA group rats showed less spatial exploration ability, activity level, social interaction, and social novelty preference than WT group rats. It was gratifying to observe that acupuncture indeed improved these abnormal behaviors of autism rat model. 2. RNA-sequencing: The three groups of rats differed in the expression and enrichment pathways of multiple genes related to synaptic function, neural signal transduction, and circadian rhythm regulation. Our experiments indicated that acupuncture can alleviate the major symptoms of ASD by improving these neurological abnormalities. 3. Under the transmission electron microscopy, several lysosomes and mitochondrial structural abnormalities were observed in the prefrontal neurons of VPA group rats, which were manifested as atrophy of the mitochondrial membran, blurring or disappearance of the mitochondrial cristae, and even vacuolization. Moreover, the number of synapses and synaptic vesicles was relatively small. Conversely, the mitochondrial structure of rats in the WT group and VPA_acupuncture was normal, and the number of synapses and synaptic vesicles was relatively large. Conclusion: Acupuncture effectively improved the abnormal behaviors of autism rat model and the ultrastructure of the PFC neurons, which might worked by improving their abnormal synaptic function, synaptic plasticity and promoting neuronal signal transduction.

Keywords: autism spectrum disorder, acupuncture, animal behavior, RNA sequencing, transmission electron microscope

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Authors: S. Kerakra, S. Bouhelal, M. Poncot

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The aim of this study is to give a comprehensive overview of the effect of short hollow and solid recycled polyethylene terephthalate (PET) fibers in different breaking tenacities reinforced isotactic polypropylene (iPP) composites on the mechanical and morphological properties. Composites of iPP/3, 7and 10 wt% of solid and hollow recycled PET fibers were prepared by batched melt mixing in a Brabender. The incorporation of solid recycled-PET fibers in isotactic polypropylene increase Young’s modulus of iPP relatively, meanwhile it increased proportionally with hollow fibers content. An improvement of the storage modulus, and a shift up in glass transition temperatures of hollow fibers/iPP composites was determined by DMA results. The morphology of composites was determined by scanning electron microscope (SEM) and optical polarized microscopy (OM) showing a good dispersion of the hollow fibers. Also, their flexible aspect (folding, bending) was observed. But, one weak interaction between the polymer/fibers phases was shown. Polymers can be effectively reinforced with short hollow recycled PET fibers due to their characteristics like recyclability, lightweight and the flexible aspect, which allows the absorbance of the energy of a striker with a minimum damage of the matrix. Aiming to improve the affinity matrix–recycled hollow PET fibers, it is suggested the addition of compatibilizers, as maleic anhydride.

Keywords: isotactic polypropylene, hollow recycled PET fibers, solid recycled-PET fibers, composites, short fiber, scanning electron microscope

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Authors: Eun-Soo Lim, Young-Min Kang

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M-type Sr-hexaferrite (SrFe₁₂O₁₉) have been studied during the past decades because it is the most utilized materials in permanent magnets due to their low price, outstanding chemical stability, and appropriate hard magnetic properties. Many attempts have been made to improve the intrinsic magnetic properties of M-type Sr-hexaferrites (SrM), such as by improving the saturation magnetization (MS) and crystalline anisotropy by cation substitution. It is well proved that the Ca-La-Co substitutions are one of the most successful approaches, which lead to a significant enhancement in the crystalline anisotropy without reducing MS, and thus the Ca-La-Co-doped SrM have been commercialized in high-grade magnet products. In this research, the effect of respective doping of Ca and La into the SrM lattices were studied with assumptions that these elements could substitute both of Fe and Sr sites. The hexaferrite samples of stoichiometric SrFe₁₂O₁₉ (SrM) and the Ca substituted SrM with formulae of Sr₁₋ₓCaₓFe₁₂Oₐ (x = 0.1, 0.2, 0.3, 0.4) and SrFe₁₂₋ₓCaₓOₐ (x = 0.1, 0.2, 0.3, 0.4), and also La substituted SrM of Sr₁₋ₓLaₓFe₁₂Oₐ (x = 0.1, 0.2, 0.3, 0.4) and SrFe₁₂₋ₓLaₓOₐ (x = 0.1, 0.2, 0.3, 0.4) were prepared by conventional solid state reaction processes. X-ray diffraction (XRD) with a Cu Kα radiation source (λ=0.154056 nm) was used for phase analysis. Microstructural observation was conducted with a field emission scanning electron microscopy (FE-SEM). M-H measurements were performed using a vibrating sample magnetometer (VSM) at 300 K. Almost pure M-type phase could be obtained in the all series of hexaferrites calcined at > 1250 ºC. Small amount of Fe₂O₃ phases were detected in the XRD patterns of Sr₁₋ₓCaₓFe₁₂Oₐ (x = 0.2, 0.3, 0.4) and Sr₁₋ₓLaₓFe₁₂Oₐ (x = 0.1, 0.2, 0.3, 0.4) samples. Also, small amount of unidentified secondary phases without the Fe₂O₃ phase were found in the samples of SrFe₁₂₋ₓCaₓOₐ (x = 0.4) and SrFe₁₂₋ₓLaₓOₐ (x = 0.3, 0.4). Although the Ca substitution (x) into SrM structure did not exhibit a clear tendency in the cell parameter change in both series of samples, Sr₁₋ₓCaₓFe₁₂Oₐ and SrFe₁₂₋ₓCaₓOₐ , the cell volume slightly decreased with doping of Ca in the Sr₁₋ₓCaₓFe₁₂Oₐ samples and increased in the SrFe₁₂₋ₓCaₓOₐ samples. Considering relative ion sizes between Sr²⁺ (0.113 nm), Ca²⁺ (0.099 nm), Fe³⁺ (0.064 nm), these results imply that the Ca substitutes both of Sr and Fe in the SrM. A clear tendency of cell parameter change was observed in case of La substitution into Sr site of SrM ( Sr₁₋ₓLaₓFe₁₂Oₐ); the cell volume decreased with increase of x. It is owing to the similar but smaller ion size of La³⁺ (0.106 nm) than that of Sr²⁺. In case of SrFe₁₂₋ₓLaₓOₐ, the cell volume first decreased at x = 0.1 and then remained almost constant with increase of x from 0.2 to 0.4. These results mean that La only substitutes Sr site in the SrM structure. Besides, the microstructure and magnetic properties of these samples, and correlation between them will be revealed.

Keywords: M-type hexaferrite, substitution, cell parameter, magnetic properties

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Authors: Prabu Duplex

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Due to stringent emission regulation targets, large-scale transition to renewable energy sources is a global challenge, and wind power plays a significant role in the solution vector. This scenario has led to the construction of offshore wind farms, and several wind farms are planned in the shallow waters where the marine habitat exists. It raises concerns over impacts of underwater noise on marine species, for example bridge constructions in the ocean straits. Dangerous to aquatic life, the environmental organisations say, the bridge would be devastating, since ocean straits are important place of transit for marine mammals. One of the highest concentrations of biodiversity in the world is concentrated these areas. The investigation of ship noise and piling noise that may happen during bridge construction and in operation is therefore vital. Once the source levels are known the receiver levels can be modelled. With this objective this work investigates the key requirement of the software that can model transmission loss in high frequencies that may occur during construction or operation phases. Most propagation models are 2D solutions, calculating the propagation loss along a transect, which does not include horizontal refraction, reflection or diffraction. In many cases, such models provide sufficient accuracy and can provide three-dimensional maps by combining, through interpolation, several two-dimensional (distance and depth) transects. However, in some instances the use of 2D models may not be sufficient to accurately model the sound propagation. A possible example includes a scenario where an island or land mass is situated between the source and receiver. The 2D model will result in a shadow behind the land mass where the modelled transects intersect the land mass. Diffraction will occur causing bending of the sound around the land mass. In such cases, it may be necessary to use a 3D model, which accounts for horizontal diffraction to accurately represent the sound field. Other scenarios where 2D models may not provide sufficient accuracy may be environments characterised by a strong up-sloping or down sloping seabed, such as propagation around continental shelves. In line with these objectives by means of a case study, this work addresses the importance of 3D interactions in underwater acoustics. The methodology used in this study can also be used for other 3D underwater sound propagation studies. This work assumes special significance given the increasing interest in using underwater acoustic modeling for environmental impacts assessments. Future work also includes inter-model comparison in shallow water environments considering more physical processes known to influence sound propagation, such as scattering from the sea surface. Passive acoustic monitoring of the underwater soundscape with distributed hydrophone arrays is also suggested to investigate the 3D propagation effects as discussed in this article.

Keywords: underwater acoustics, naval, maritime, cetaceans

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Authors: Adeyemi Isaac Sanusi, Gueguim E. B. Kana

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Nanoparticles have received attention of the scientific community due to their biotechnological potentials. They exhibit advantageous size, shape and concentration-dependent catalytic, stabilizing, immunoassays and immobilization properties. This study investigates the impact of metallic oxide nanoparticles (NPs) on ethanol production by Saccharomyces cerevisiae BY4743. Nine different nanoparticles were synthesized using precipitation method and microwave treatment. The nanoparticles synthesized were characterized by Fourier Transform Infra-Red spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Fermentation processes were carried out at varied NPs concentrations (0 – 0.08 wt%). Highest ethanol concentrations were achieved after 24 h using Cobalt NPs (5.07 g/l), Copper NPs (4.86 g/l) and Manganese NPs (4.74 g/l) at 0.01 wt% NPs concentrations, which represent 13%, 8.7% and 5.4% increase respectively over the control (4.47 g/l). The lowest ethanol concentration (0.17 g/l) was obtained when 0.08 wt% of Silver NPs was used. And lower ethanol concentrations were observed at higher NPs concentration. Ethanol concentration decrease after 24 h for all the processes. In all set up with NPs, the pH was observed to be stable and the stability was directly proportional to nanoparticles concentrations. These findings suggest that the presence of some of the NPs in the bioprocesses has catalytic and pH stabilizing potential. Ethanol production by Saccharomyces cerevisiae BY4743 was enhanced in the presence of Cobalt NPs, Copper NPs and Manganese NPs. Optimization study using response surface methodology (RSM) will further elucidate the impact of these nanoparticles on bioethanol production.

Keywords: agitation, bioethanol, nanoparticles concentration, optimization, pH value

Procedia PDF Downloads 183

Authors: Ariadne C. Catto, Luis F. da Silva, Khalifa Aguir, Valmor Roberto Mastelaro

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Zinc oxide (ZnO) pure or doped are one of the most promising metal oxide semiconductors for gas sensing applications due to the well-known high surface-to-volume area and surface conductivity. It was shown that ZnO is an excellent gas-sensing material for different gases such as CO, O2, NO2 and ethanol. In this context, pure and doped ZnO exhibiting different morphologies and a high surface/volume ratio can be a good option regarding the limitations of the current commercial sensors. Different studies showed that the sensitivity of metal-doped ZnO (e.g. Co, Fe, Mn,) enhanced its gas sensing properties. Motivated by these considerations, the aim of this study consisted on the investigation of the role of Co ions on structural, morphological and the gas sensing properties of nanostructured ZnO samples. ZnO and Zn1-xCoxO (0 < x < 5 wt%) thin films were obtained via the polymeric precursor method. The sensitivity, selectivity, response time and long-term stability gas sensing properties were investigated when the sample was exposed to a different concentration range of ozone (O3) at different working temperatures. The gas sensing property was probed by electrical resistance measurements. The long and short-range order structure around Zn and Co atoms were investigated by X-ray diffraction and X-ray absorption spectroscopy. X-ray photoelectron spectroscopy measurement was performed in order to identify the elements present on the film surface as well as to determine the sample composition. Microstructural characteristics of the films were analyzed by a field-emission scanning electron microscope (FE-SEM). Zn1-xCoxO XRD patterns were indexed to the wurtzite ZnO structure and any second phase was observed even at a higher cobalt content. Co-K edge XANES spectra revealed the predominance of Co2+ ions. XPS characterization revealed that Co-doped ZnO samples possessed a higher percentage of oxygen vacancies than the ZnO samples, which also contributed to their excellent gas sensing performance. Gas sensor measurements pointed out that ZnO and Co-doped ZnO samples exhibit a good gas sensing performance concerning the reproducibility and a fast response time (around 10 s). Furthermore, the Co addition contributed to reduce the working temperature for ozone detection and improve the selective sensing properties.

Keywords: cobalt-doped ZnO, nanostructured, ozone gas sensor, polymeric precursor method

Procedia PDF Downloads 237

Authors: M.St. Węglowski, D. Miara, S. Błacha, J. Dworak, J. Rykała, K. Kwieciński, J. Pikuła, G. Ziobro, A. Szafron, P. Zimierska-Nowak, M. Richert, P. Noga

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In the paper the results of welding of car’s air-conditioning elements are presented. These systems based on, mainly, the environmental unfriendly refrigerants. Thus, the producers of cars will have to stop using traditional refrigerant and to change it to carbon dioxide (R744). This refrigerant is environmental friendly. However, it should be noted that the air condition system working with R744 refrigerant operates at high temperature (up to 150 °C) and high pressure (up to 130 bar). These two parameters are much higher than for other refrigerants. Thus new materials, design as well as joining technologies are strongly needed for these systems. AISI 304 and 316L steels as well as aluminium alloys 5xxx are ranked among the prospective materials. As a joining process laser welding, plasma welding, electron beam welding as well as high rotary friction welding can be applied. In the study, the metallographic examination based on light microscopy as well as SEM was applied to estimate the quality of welded joints. The analysis of welding was supported by numerical modelling based on Sysweld software. The results indicated that using laser, plasma and electron beam welding, it is possible to obtain proper quality of welds in stainless steel. Moreover, high rotary friction welding allows to guarantee the metallic continuity in the aluminium welded area. The metallographic examination revealed that the grain growth in the heat affected zone (HAZ) in laser and electron beam welded joints were not observed. It is due to low heat input and short welding time. The grain growth and subgrains can be observed at room temperature when the solidification mode is austenitic. This caused low microstructural changes during solidification. The columnar grain structure was found in the weld metal. Meanwhile, the equiaxed grains were detected in the interface. The numerical modelling of laser welding process allowed to estimate the temperature profile in the welded joint as well as predicts the dimensions of welds. The agreement between FEM analysis and experimental data was achieved.  

Keywords: car’s air–conditioning, microstructure, numerical modelling, welding

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Authors: H. Medjadji, A. Boulahouache, N. Salhi, A. Boudjemaa, M. Trari

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Hydrogen from renewable sources, such as solar, is referred to as green hydrogen. The splitting water process using semiconductors, such as photocatalysts, has attracted significant attention due to its potential application for solving the energy crisis and environmental pollution. Spinel ferrites of the MF₂O₄ type have shown broad interest in diverse energy conversion processes, including fuel cells and photo electrocatalytic water splitting. This work focuses on preparing nano-spinels based on iron AFe₂O₄ (A= Ca, Co, and Cu) as photocatalysts using the nitrate method. These materials were characterized both physically and optically and subsequently tested for hydrogen generation under visible light irradiation. Various techniques were used to investigate the properties of the materials, including TGA-DT, X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), UV-visible spectroscopy, Scanning Electron Microscopy with Energy Dispersive X-ray Spectroscopy (SEM-EDX) and X-ray Photoelectron Spectroscopy (XPS) was also undertaken. XRD analysis confirmed the formation of pure phases at 850°C, with crystalline sizes of 31 nm for CaFe₂O₄, 27 nm for CoFe₂O₄, and 40 nm for CuFe₂O₄. The energy gaps, calculated from recorded diffuse reflection data, are 1.85 eV for CaFe₂O₄, 1.27 eV for CoFe₂O₄, and 1.64 eV for CuFe₂O₄. SEM micrographs showed homogeneous grains with uniform shapes and medium porosity in all samples. EDX elemental analysis determined the absence of any contaminating elements, highlighting the high purity of the prepared materials via the nitrate route. XPS spectra revealed the presence of Fe3+ and O in all samples. Additionally, XPS analysis revealed the presence of Ca²⁺, Co²⁺, and Cu²⁺ on the surface of CaFe₂O₄ and CoFe₂O₄ spinels, respectively. The photocatalytic activity was successfully evaluated by measuring H₂ evolution through the water-splitting process. The best performance was achieved with CaFe₂O₄ in a neutral medium (pH ~ 7), yielding 189 µmol at an optimal temperature of ~50°C. The highest hydrogen production rates for CoFe₂O₄ and CuFe₂O₄ were obtained at pH ~ 12 with release rates of 65 and 85 µmol, respectively, under visible light irradiation at the same optimal temperature. Various conditions were investigated including the pH of the solution, the hole sensors utilization and recyclability.

Keywords: hydrogen, MFe₂O₄, nitrate route, spinel ferrite

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Authors: F. Kashanian, M. M. Masoudi, A. Akbari, A. Shamloo, M. R. Zand, S. S. Salehi

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Nano-sized materials present new opportunities in biology and medicine and they are used as biomedical tools for investigation, separation of molecules and cells. To achieve more effective cancer therapy, it is essential to select cancer cells exactly. This research suggests that using the antibody-functionalized nontoxic Arginine-doped magnetic nanoparticles (A-MNPs), has been prosperous in detection, capture, and magnetic separation of circulating tumor cells (CTCs) in tumor tissue. In this study, A-MNPs were synthesized via a simple precipitation reaction and directly immobilized Ep-CAM EBA-1 antibodies over superparamagnetic A-MNPs for Mucin BCA-225 in breast cancer cell. The samples were characterized by vibrating sample magnetometer (VSM), FT-IR spectroscopy, Tunneling Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). These antibody-functionalized nontoxic A-MNPs were used to capture breast cancer cell. Through employing a strong permanent magnet, the magnetic separation was achieved within a few seconds. Antibody-Conjugated nontoxic Arginine-doped Fe₃O₄ nanoparticles have the potential for the future study to capture CTCs which are released from tumor tissue and for drug delivery, and these results demonstrate that the antibody-conjugated A-MNPs can be used in magnetic hyperthermia techniques for cancer treatment.

Keywords: tumor tissue, antibody, magnetic nanoparticle, CTCs capturing

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Authors: Yik Ling Chew, Adlina Maisarah Mahadi, Joo Kheng Goh

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Bauhinia kockiana originates from Peninsular Malaysia, and it is grown as a garden ornamental plant. However, it is used as medicinal plant by Malaysia ‘Kelabit’ ethic group in treating various diseases and illnesses. This study focused on the assessment of the antibacterial activity of B. kockiana towards MRSA, to purify and identify the antibacterial compounds, and to determine the mechanism of antibacterial activity. Antibacterial activity of B. kockiana flower is evaluated qualitatively and quantitatively using disc diffusion assay and microbroth dilution method to determine the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of extracts. Phytochemical analysis is performed to determine the classes of phytochemicals in the extracts. Bioactivity-guided isolation is performed to purify the antibacterial agents and identified the chemical structures via various spectroscopy methods. Scanning electron microscopy (SEM) technique is adopted to evaluate the antibacterial mechanism of extract and compounds isolated. B. kockiana flower is found to exhibit fairly strong antibacterial activity towards both strains of MRSA bacteria. Gallic acid and its ester derivatives are purified from ethyl acetate extract and the antibacterial activity is evaluated. SEM has revealed the mechanism of the extracts and compounds isolated.

Keywords: alkyl gallates, Bauhinia kockiana, MRSA, scanning electron microscopy

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Authors: Seyfullah Madakbaş, Ferhat Şen, Memet Vezir Kahraman

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The aim of this study was to improve thermal stability, mechanical and surface properties of thermoplastic polyurethane (TPU) with the addition of BaTiO3. The TPU/ BaTiO3 composites having various ratios of TPU and BaTiO3 were prepared. The chemical structure of the prepared composites was investigated by FT-IR. FT-IR spectra of TPU/ barium titanate composites show that they successfully were prepared. Thermal stability of the samples was evaluated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The prepared composites showed high thermal stability, and the char yield increased as barium titanate content increased. The glass transition temperatures of the composites rise with the addition of barium titanate. Mechanical properties of the samples were characterized with stress-strain test. The mechanical properties of the TPU were increased with the contribution of the contribution of the barium titanate it increased. Hydrophobicity of the samples was determined by the contact angle measurements. The contact angles have the tendency to increase the hydrophobic behavior on the surface, when barium titanate was added into TPU. Moreover, the surface morphology of the samples was investigated by a scanning electron microscopy (SEM). SEM-EDS mapping images showed that barium titanate particles were dispersed homogeneously. Finally, the obtained results prove that the prepared composites have good thermal, mechanical and surface properties and that they can be used in many applications such as the electronic devices, materials engineering and other emergent.

Keywords: barium titanate, composites, thermoplastic polyurethane, scanning electron microscopy

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Authors: Saheli Mitra, Ramesh Karri, Praveen K. Mylapalli, Arka. B. Dey, Gourav Bhattacharya, Gouriprasanna Roy, Syed M. Kamil, Surajit Dhara, Sunil K. Sinha, Sajal K. Ghosh

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The most well-known structures of lyotropic liquid crystalline systems are the two dimensional hexagonal phase of cylindrical micelles with a positive interfacial curvature and the lamellar phase of flat bilayers with zero interfacial curvature. In aqueous solution of surfactants, the concentration dependent phase transitions have been investigated extensively. However, instead of changing the surfactant concentrations, the local curvature of an aggregate can be altered by tuning the electrostatic interactions among the constituent molecules. Intermediate phases with non-uniform interfacial curvature are still unexplored steps to understand the route of phase transition from hexagonal to lamellar. Understanding such structural evolution in lyotropic liquid crystalline systems is important as it decides the complex rheological behavior of the system, which is one of the main interests of the soft matter industry. Sodium dodecyl sulfate (SDS) is an anionic surfactant and can be considered as a unique system to tune the electrostatics by cationic additives. In present study, imidazolium-based ionic liquids (ILs) with different number of carbon atoms in their single hydrocarbon chain were used as the additive in the aqueous solution of SDS. At a fixed concentration of total non-aqueous components (SDS and IL), the molar ratio of these components was changed, which effectively altered the electrostatic interactions between the SDS molecules. As a result, the local curvature is observed to modify, and correspondingly, the structure of the hexagonal liquid crystalline phases are transformed into other phases. Polarizing optical microscopy of SDS and imidazole-based-IL systems have exhibited different textures of the liquid crystalline phases as a function of increasing concentration of the ILs. The small angle synchrotron x-ray diffraction (SAXD) study has indicated the hexagonal phase of direct cylindrical micelles to transform to a rectangular phase at the presence of short (two hydrocarbons) chain IL. However, the hexagonal phase is transformed to a lamellar phase at the presence of long (ten hydrocarbons) chain IL. Interestingly, at the presence of a medium (four hydrocarbons) chain IL, the hexagonal phase is transformed to another hexagonal phase of direct cylindrical micelles through the lamellar phase. To the best of our knowledge, such a phase sequence has not been reported earlier. Even though the small angle x-ray diffraction study has revealed the lattice parameters of these phases to be similar to each other, their rheological behavior has been distinctly different. These rheological studies have shed lights on how these phases differ in their viscoelastic behavior. Finally, the packing parameters, calculated for these phases based on the geometry of the aggregates, have explained the formation of the self-assembled aggregates.

Keywords: lyotropic liquid crystals, polarizing optical microscopy, rheology, surfactants, small angle x-ray diffraction

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Authors: Anshuman Srivastava, Shiv Singh, Sheelendra Pratap Singh

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A simple, sensitive and effective gas chromatography tandem mass spectrometry (GC-MS/MS) method was developed for simultaneous analysis of multi pesticide residues (organophosphate, organochlorines, synthetic pyrethroids and herbicides) in food commodities using phenolic resin based activated carbon fibers (ACFs) as reversed-dispersive solid phase extraction (r-DSPE) sorbent in modified QuEChERS (Quick Easy Cheap Effective Rugged Safe) method. The acetonitrile-based QuEChERS technique was used for the extraction of the analytes from food matrices followed by sample cleanup with ACFs instead of traditionally used primary secondary amine (PSA). Different physico-chemical characterization techniques such as Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and Brunauer-Emmet-Teller surface area analysis were employed to investigate the engineering and structural properties of ACFs. The recovery of pesticides and herbicides was tested at concentration levels of 0.02 and 0.2 mg/kg in different commodities such as cauliflower, cucumber, banana, apple, wheat and black gram. The recoveries of all twenty-six pesticides and herbicides were found in acceptable limit (70-120%) according to SANCO guideline with relative standard deviation value < 15%. The limit of detection and limit of quantification of the method was in the range of 0.38-3.69 ng/mL and 1.26 -12.19 ng/mL, respectively. In traditional QuEChERS method, PSA used as r-DSPE sorbent plays a vital role in sample clean-up process and demonstrates good recoveries for multiclass pesticides. This study reports that ACFs are better in terms of removal of co-extractives in comparison of PSA without compromising the recoveries of multi pesticides from food matrices. Further, ACF replaces the need of charcoal in addition to the PSA from traditional QuEChERS method which is used to remove pigments. The developed method will be cost effective because the ACFs are significantly cheaper than the PSA. So the proposed modified QuEChERS method is more robust, effective and has better sample cleanup efficiency for multiclass multi pesticide residues analysis in different food matrices such as vegetables, grains and fruits.

Keywords: QuEChERS, activated carbon fibers, primary secondary amine, pesticides, sample preparation, carbon nanomaterials

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Authors: Krupali Mehta, Sandip Bhatt, Umesh Trivedi, Bhavesh Bharatiya, Mukesh Ranjan, Atindra D. Shukla

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Owing to the dominating surface forces and large-scale surface interactions, the nano-scale particles face difficulties in getting suspended in various media. Magnetic nanoparticles of iron oxide offer a great deal of promise due to their ease of preparation, reasonable magnetic properties, low cost and environmental compatibility. We intend to modify the surface of magnetic Fe₂O₃ nanoparticles with selected surface modifying agents using simple and effective single-step chemical reactions in order to enhance dispersibility of magnetic nanoparticles in non-polar media. Magnetic particles were prepared by hydrolysis of Fe²⁺/Fe³⁺ chlorides and their subsequent oxidation in aqueous medium. The dried particles were then treated with Octadecyl quaternary ammonium silane (Terrasil™), stearic acid and gallic acid ester of stearyl alcohol in ethanol separately to yield S-2 to S-4 respectively. The untreated Fe₂O₃ was designated as S-1. The surface modified nanoparticles were then analysed with Dynamic Light Scattering (DLS), Fourier Transform Infrared spectroscopy (FTIR), X-Ray Diffraction (XRD), Thermogravimetric Gravimetric Analysis (TGA) and Scanning Electron Microscopy and Energy dispersive X-Ray analysis (SEM-EDAX). Characterization reveals the particle size averaging 20-50 nm with and without modification. However, the crystallite size in all cases remained ~7.0 nm with the diffractogram matching to Fe₂O₃ crystal structure. FT-IR suggested the presence of surfactants on nanoparticles’ surface, also confirmed by SEM-EDAX where mapping of elements proved their presence. TGA indicated the weight losses in S-2 to S-4 at 300°C onwards suggesting the presence of organic moiety. Hydrophobic character of modified surfaces was confirmed with contact angle analysis, all modified nanoparticles showed super hydrophobic behaviour with average contact angles ~129° for S-2, ~139.5° for S-3 and ~151° for S-4. This indicated that surface modified particles are super hydrophobic and they are easily dispersible in non-polar media. These modified particles could be ideal candidates to be suspended in oil-based fluids, polymer matrices, etc. We are pursuing elaborate suspension/sedimentation studies of these particles in various oils to establish this conjecture.

Keywords: iron nanoparticles, modification, hydrophobic, dispersion

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Authors: Abdelghani May

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This paper reports on experimental investigations concerning the underlying reasons for the anisotropic behavior observed during the cyclic loading of AA2017 aluminum alloy. Initially, we quantified the evolution of fatigue damage resulting from controlled proportional cyclic loadings along the axial and shear directions. Our primary objective at this stage was to verify the anisotropic mechanical behavior recently observed. To accomplish this, we utilized various models of fatigue damage quantification and conducted a comparative study of the obtained results. Our analysis confirmed the anisotropic nature of the material under investigation. In the subsequent step, we performed microstructural investigations aimed at understanding the origins of the anisotropic mechanical behavior. To this end, we utilized scanning electron microscopy to examine the phases and precipitates in both the transversal and longitudinal sections. Our findings indicate that the structure and morphology of these entities are responsible for the anisotropic behavior observed in the aluminum alloy. Furthermore, results obtained from Kikuchi diagrams, pole figures, and inverse pole figures have corroborated these conclusions. These findings demonstrate significant differences in the crystallographic texture of the material.

Keywords: microstructural investigation, fatigue damage quantification, anisotropic behavior, AA2017 aluminum alloy, cyclic loading, crystallographic texture, scanning electron microscopy

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Authors: Hamza Ouachtouk, Amine Harbi, Said Azerblou, Youssef Naimi, El Mostafa Tace

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This study delves into the structural, vibrational, magnetic, and electronic properties of La₂MMnO₆ double perovskites, where M denotes Ni, Co, and Zn. Recognized for their versatile ionic configurations within the A and B sub-lattices, double perovskite oxides have attracted considerable interest due to their extensive array of physical properties, which include multiferroic behavior, colossal magnetoresistance, and ferroelectric/piezoelectric functionalities. These materials are pivotal for energy-related technologies like solid oxide fuel cells and water-splitting catalysis, attributed to their superior oxygen ion transport and storage capabilities. This research places particular emphasis on La₂NiMnO₆ and La₂CoMnO₆, known for their distinct magnetic, electric, and multiferroic properties, and extends the investigation to La₂ZnMnO₆, synthesized via high-temperature solid-state chemistry. This addition aims to ascertain the impact of zinc substitution on these properties. Structural analysis through X-ray diffraction has confirmed a monoclinic structure within the P2₁/n space group. Comprehensive vibrational studies utilizing infrared and Raman spectroscopy, alongside additional XRD assessments, provide a detailed examination of the dynamic and electronic behaviors of these compounds. The results underscore the significant role of chemical composition in modulating their functional properties. Comparatively, this study highlights that zinc substitution notably alters the electronic and magnetic responses, which could enhance the applicability of these materials in advanced energy technologies. This expanded analysis not only reinforces our understanding of La₂MMnO₆'s physical characteristics but also highlights its potential applications in the next generation of energy solutions.

Keywords: double perovskites, structural analysis, vibrational spectroscopy, magnetic properties, electronic properties, high-temperature solid-state chemistry, La₂MMnO₆, monoclinic structure, x-ray diffraction

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Authors: Elif Doğru, Bülent Kızılduman, Huriye İcil

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Throughout history, Cyprus has been involved in various commercial and cultural relationships with different civilizations, owing to its strategic location. Particularly during the Late Bronze Age, Cyprus emerged as a significant region engaged in interactions with the Mycenaeans and other Mediterranean civilizations. Presently, findings from archaeological excavations provide valuable insights into Cyprus' cultural history and its connections with other civilizations. Painted Mycenaean ceramics discovered during the excavations at Kaleburnu-Kral Tepesi (Galinaporni-Vasili), dated to the Late Bronze Age in Cyprus, are considered significant archaeological findings that carry traces of the art and culture of that era, reflecting the island's commercial and cultural connections. Considering these findings, there is a need for archaeometric studies to aid in the understanding of the commercial and cultural ties at Kaleburnu-Kral Tepesi. In line with this need, analytical studies have been initiated concerning the provenance and production techniques of the Mycenaean ceramics discovered in the excavations at Kaleburnu-Kral Tepesi, dated to the Late Bronze Age. In the context of origin analysis studies, it is advocated that understanding the techniques and materials used for the figures and designs applied on Mycenaean ceramics would significantly contribute to a better comprehension of historical contexts. Hence, the adopted approach involves not only the analysis of the ceramic raw material but also the characterization of the pigments on the ceramics as a whole. In light of this, in addition to the studies aimed at determining the provenance and production techniques of the Mycenaean ceramic bodies, the characterization of the pigments used in the decorations of the relevant ceramics has been included in the research scope. Accordingly, this study aims to characterize the pigments used in the decorations of Mycenaean ceramics discovered at Kaleburnu-Kral Tepesi, dated to the Late Bronze Age. The X-Ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Scanning Electron Microscopy with Energy Dispersive X-ray Spectroscopy (SEM-EDX) methods have been employed to determine the surface morphology and chemical properties of the Mycenaean pigments. The characterization has been conducted through the combination of multiple analytical methods. The characterization of the pigments of Mycenaean ceramics aims to enhance the scientific perspective adopted for understanding the contributions of Mycenaean ceramics found in Cyprus to the island's culture, by providing scientific data on the types and origins of pigments used during the Late Bronze Age.

Keywords: mycenaean, ceramic, provenance, pigment

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Authors: Prasanna Kumar Acharya, Mausam Kumari Yadav

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Cement concrete has emerged as the most consumed construction material. It has also dominated all other construction materials because of its versatility. Apart from numerous advantages it has a disadvantage concerning durability. The large structures constructed with cement concrete involving the consumption of huge natural materials remain in serviceable condition for 5 – 7 decades only while structures made with stones stand for many centuries. The short life span of structures not only affects the economy but also affects the ecology greatly. As such, the improvement of durability of cement concrete is a global concern and scientists around the globe are trying for this purpose. Functionally graded concrete (FGC) is an exciting development. In contrast to conventional concrete, FGC demonstrates different characteristics depending on its thickness, which enables it to conform to particular structural specifications. The purpose of FGC is to improve the performance and longevity of conventional concrete structures with cutting-edge building materials. By carefully distributing various kinds and amounts of reinforcements, additives, mix designs and/or aggregates throughout the concrete matrix, this variety is produced. A key component of functionally graded concrete's performance is its durability, which affects the material's capacity to tolerate aggressive environmental influences and load-bearing circumstances. This paper reports the durability of FGC made using Portland slag cement (PSC). For this purpose, control concretes (CC) of M20, M30 and M40 grades were designed. Single-layered samples were prepared using each grade of concrete. Further using combinations of M20 + M30, M30 + M40 and M40 + M20, doubled layered concrete samples in a depth ratio of 1:1 was prepared those are herein called FGC samples. The efficiency of FGC samples was compared with that of the higher-grade concrete of parent materials in terms of compressive strength, water absorption, sorptivity, acid resistance, sulphate resistance, chloride resistance and abrasion resistance. The properties were checked at the age of 28 and 91 days. Apart from strength and durability parameters, the microstructure of CC and FGC were studied in terms of X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray. The result of the study revealed that there is an increase in the efficiency of concrete evaluated in terms of strength and durability when it is made functionally graded using a layered technology having different grades of concrete in layers. The results may help to enhance the efficiency of structural concrete and its durability.

Keywords: fresh on compacted, functionally graded concrete, acid, chloride, sulphate test, sorptivity, abrasion, water absorption test

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Authors: Sabir Hussain, Mujtaba Hassan, Kashif Rasool, Asif Shahzad

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Fine particulate matter with an aerodynamic diameter of less than 2.5 μm (PM2.5) was collected in Islamabad from November 2022 to January 2023, at urban sites. The average mass concentrations of PM2.5 varied, ranging from 90.5 to 133 μg m−3 in urban areas. Environmental scanning electron microscopy (ESEM) analysis revealed that Islamabad's PM2.5 comprised soot aggregates, ashes, minerals, bio-particles, and unidentified particles. Results from inductively coupled plasma atomic emission spectroscopy (ICP-OES) indicated a gradual increase in total elemental concentrations in Islamabad PM2.5 in winter, with relatively high levels in December. Significantly different elemental compositions were observed in urban PM2.5. Enrichment factor (EF) analysis suggested that elements such as K, Na, Ca, Mg, Al, Fe, Ba, and Sr were of natural origin, while As, Cu, Zn, Pb, Cd, Mn, Ni, and Se originated from anthropogenic sources. Plasmid DNA assays demonstrated varying levels of potential toxicity in Islamabad PM2.5 collected from urban sites, as well as across different seasons. Notably, the urban winter PM2.5 sample exhibited much stronger toxicity compared to other samples. The presence of heavy metals in Islamabad PM2.5, including Cu, Zn, Pb, Cd, Cr, Mn, and Ni, may have synergistic effects on human health.

Keywords: islamabad particulate matter pm2.5, scanning electron microscopy with energy-dispersive x-ray spectroscopy(sem-eds), fourier transform infrared spectroscopy(ftir), inductively coupled plasma optical emission spectroscopy(icp-oes)

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Authors: Ayomide A Sijuade, Nafiza Anjum

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The rising demand to meet the need for clean and sustainable energy solutions has led the market to create effective energy storage technologies. In this study, we look at the possibility of using a heterostructure made of polyaniline (PANI), titanium carbide (Ti₃C₂), and vanadium carbide (V₂C) for energy storage devices. V₂C is a two-dimensional transition metal carbide with remarkable mechanical and electrical conductivity. Ti₃C2 has solid thermal conductivity and mechanical strength. PANI, on the other hand, is a conducting polymer with customizable electrical characteristics and environmental stability. Layer-by-layer assembly creates the heterostructure of V₂C, Ti₃C₂, and PANI, allowing for precise film thickness and interface quality control. Structural and morphological characterization is carried out using X-ray diffraction, scanning electron microscopy, and atomic force microscopy. For energy storage applications, the heterostructure’s electrochemical performance is assessed. Electrochemical experiments, such as cyclic voltammetry and galvanostatic charge-discharge tests, examine the heterostructure’s charge storage capacity, cycle stability, and rate performance. Comparing the heterostructure to the individual components reveals better energy storage capabilities. V₂C, Ti₃C₂, and PANI synergize to increase specific capacitance, boost charge storage, and prolong cycling stability. The heterostructure’s unique arrangement of 2D materials and conducting polymers promotes effective ion diffusion and charge transfer processes, improving the effectiveness of energy storage. The heterostructure also exhibits remarkable electrochemical stability, which minimizes capacity loss after repeated cycling. The longevity and long-term dependability of energy storage systems depend on this quality. By examining the potential of V₂C, Ti₃C₂, and PANI heterostructures, the results of this study expand energy storage technology. These materials’ specialized integration and design show potential for use in hybrid energy storage systems, lithium-ion batteries, and supercapacitors. Overall, the development of high-performance energy storage devices utilizing V₂C, Ti₃C₂, and PANI heterostructures is clarified by this research, opening the door to the realization of effective, long-lasting, and eco-friendly energy storage solutions to satisfy the demands of the modern world.

Keywords: MXenes, energy storage materials, conductive polymers, composites

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

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

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

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

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

Keywords: tissue, laser, ultrasound, effect, imaging

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Authors: Manuel Salado, Mikel Rincón, Arkaitz Fidalgo, Roberto Fernandez, Senentxu Lanceros-Méndez

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Lithium-ion batteries (LIBs) are a promising technology for energy storage, but they suffer from safety concerns due to the use of flammable organic solvents in their liquid electrolytes. Solid-state electrolytes (SSEs) offer a potential solution to this problem, but they have their own limitations, such as poor ionic conductivity and high interfacial resistance. The aim of this research was to develop a new type of SSE based on metal-organic frameworks (MOFs) and ionic liquids (ILs). MOFs are porous materials with high surface area and tunable electronic properties, making them ideal for use in SSEs. ILs are liquid electrolytes that are non-flammable and have high ionic conductivity. A series of MOFs were synthesized, and their electrochemical properties were evaluated. The MOFs were then infiltrated with ILs to form a quasi-solid gel and solid xerogel SSEs. The ionic conductivity, interfacial resistance, and electrochemical performance of the SSEs were characterized. The results showed that the MOF-IL SSEs had significantly higher ionic conductivity and lower interfacial resistance than conventional SSEs. The SSEs also exhibited excellent electrochemical performance, with high discharge capacity and long cycle life. The development of MOF-IL SSEs represents a significant advance in the field of solid-state electrolytes. The high ionic conductivity and low interfacial resistance of the SSEs make them promising candidates for use in next-generation LIBs. The data for this research was collected using a variety of methods, including X-ray diffraction, scanning electron microscopy, and electrochemical impedance spectroscopy. The data was analyzed using a variety of statistical and computational methods, including principal component analysis, density functional theory, and molecular dynamics simulations. The main question addressed by this research was whether MOF-IL SSEs could be developed that have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. The results of this research demonstrate that MOF-IL SSEs are a promising new type of solid-state electrolyte for use in LIBs. The SSEs have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. These properties make them promising candidates for use in next-generation LIBs that are safer and have higher energy densities.

Keywords: energy storage, solid-electrolyte, ionic liquid, metal-organic-framework, electrochemistry, organic inorganic plastic crystal

Procedia PDF Downloads 79

Authors: Marinela Miclau, Melinda Vajda, Nicolae Miclau, Daniel Ursu

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Characterized by a simple structure, easy and low cost fabrication, the dye-sensitized solar cell (DSSC) attracted the interest of the scientific community as an attractive alternative of conventional Si-based solar cells and thin-film solar cells. Over the past 20 years, the main efforts have attempted to enhance the efficiency of n-type DSSCs, the highest efficiency record of 14.30% was achieved using the co-sensitization of two metal-free organic dyes and Co (II/III) tris(phenanthroline)-based redox electrolyte. In the last years, the development of the efficient p-type DSSC has become a research focus owing to the fact that the concept of tandem solar cell was proposed as the solution to increase the power conversion efficiency. A promising alternative for the photocathodes of p-type DSSC, cuprous (Cu2O) and cupric (CuO) oxides have been investigated because of its nontoxic nature, low cost, high natural abundance, a good absorption coefficient for visible light and a higher dielectric constant than NiO. In case of p-type DSSC based on copper oxides with I3-/I- as redox mediator, the highest conversion efficiency of 0.42% (Cu2O) and 0.03% (CuO) has achieved. Towards the increase in the performance, we have fabricated and analyzed the performance of p-type DSSC prepared with the binder-free porous Cu2O photocathodes. Porous thin film could be an attractive alternative for DSSC because of their large surface areas which enable the efficient absorption of the dyes and light. We propose a simple and one-step hydrothermal method for the preparation of porous Cu2O thin film using copper substrate, cupric acetate and ethyl cellulose. The cubic structure of Cu2O has been determined by X-ray diffraction (XRD) and porous morphology of thin film was emphasized by Scanning Electron Microscope Inspect S (SEM). Optical and Mott-Schottky measurements attest of the high quality of the Cu2O thin film. The binder-free porous Cu2O photocathode has confirmed the excellent photovoltaic properties, the best value reported for p-type DSSC (1%) in similar conditions being reached.

Keywords: cuprous oxide, dye-sensitized solar cell, hydrothermal method, porous photocathode

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Authors: Sandra Tapin-Lingua, Katia Ruel, Jean-Paul Joseleau, Daouia Messaoudi, Olivier Fahy, Michel Petit-Conil

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The preservative efficacy of organic biocides is strongly related to their capacity of penetration and retention within wood tissues. The specific detection of the pyrethroid insecticide is currently obtained after extraction followed by chemical analysis by chromatography techniques. However visualizing the insecticide molecule within the wood structure requires specific probes together with microscopy techniques. Therefore, the aim of the present work was to apply a new methodology based on antibody-antigen recognition and electronic microscopy to visualize directly pyrethroids in the wood material. A polyclonal antibody directed against cypermethrin was developed and implement it on Pinus sylvestris wood samples coated with technical cypermethrin. The antibody was tested on impregnated wood and the specific recognition of the insecticide was visualized in transmission electron microscopy (TEM). The immunogold-TEM assay evidenced the capacity of the synthetic biocide to penetrate in the wood. The depth of penetration was measured on sections taken at increasing distances from the coated surface of the wood. Such results correlated with chemical analyzes carried out by GC-ECD after extraction. In addition, the immuno-TEM investigation allowed visualizing, for the first time at the ultrastructure scale of resolution, that cypermethrin was able to diffuse within the secondary wood cell walls.

Keywords: cypermethrin, insecticide, wood penetration, wood retention, immuno-transmission electron microscopy, polyclonal antibody

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Authors: Vimal Kumar Dewangan, T. S. Sampath Kumar, Mukesh Doble, Viju Daniel Varghese

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The apatite-based, i.e., calcium-deficient hydroxyapatite (CDHAp) bone cement is well-known potential bone graft/substitute in orthopaedics due to its similar chemical composition with natural bone minerals. Therefore, an easy approach was attempted to fabricate the apatite-based (CDHAp) bone cement with improved injectability, bioresorbability, and macroporosity. In this study, the desired bone cement was developed by mixing the solid phase (consisting of wet chemically synthesized nanocrystalline hydroxyapatite and commercially available (synthetic) tricalcium phosphate) and the liquid phase (consisting of cement binding accelerator with few biopolymers in a dilute acidic solution) along with a liquid porogen as polysorbate or a solid porogen as mannitol (for comparison) in an optimized liquid-to-powder ratio. The fabricated cement sets within clinically preferred setting time (≤20 minutes) are better injectable (>70%) and also stable at ~7.3-7.4 (physiological pH). The CDHAp phased bone cement was resulted by immersing the fabricated after-set cement in phosphate buffer solution and other similar artificial body fluids and incubated at physiological conditions for seven days, confirmed through the X-ray diffraction and Fourier transform-infrared spectroscopy analyses. The so-formed synthetic apatite-based bone cement holds the acceptable compressive strength (within the range of trabecular bone) with average interconnected pores size falls in a macropores range (~50-200μm) inside the cement, verified by scanning electron microscopy (SEM), mercury intrusion porosimetry and micro-CT analysis techniques. Also, it is biodegradable (degrades ~19-22% within 10-12 weeks) when incubated in artificial body fluids under physiological conditions. The biocompatibility study of the bone cement, when incubated with MG63 cells, shows a significant increase in the cell viability after 3rd day of incubation compared with the control, and the cells were well-attached and spread completely on the surface of the bone cement, confirmed through SEM and fluorescence microscopy analyses. With this all, we can conclude that the developed synthetic macroporous apatite-based bone cement may have the potential to become promising material used as a trabecular bone substitute.

Keywords: calcium deficient hydroxyapatite, synthetic apatite-based bone cement, injectability, macroporosity, trabecular bone substitute

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Authors: O. M. Lemine

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The effect of milling parameters on the structural and magnetic properties of nickel powder was investigated. The samples were characterized by X-ray powder diffraction and vibrating sample magnetometer (VSM). The results did not reveal any phase change of nickel during the milling. The average crystallite size decreases with a prolongation of milling times, whereas the lattice parameters increase. The hysteresis loop reveals the intrinsic magnetic behaviour. It was observed an increase in the magnetization which can be correlated to the volume expansion showed by XRD results.

Keywords: nickel powders, nanocrystallines, XRD, VSM

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Authors: Ajay Mandal, Jitendar Kumar Tiwari, N. Sathish, A. K. Srivastava

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A fundamental investigation is performed on the development of graphene (Gr) reinforced stainless steel 316L (SS 316L) metal matrix composite via selective laser melting (SLM) in order to improve specific strength and wear resistance property of SS 316L. Firstly, SS 316L powder and graphene were mixed in a fixed ratio using low energy planetary ball milling. The milled powder is then subjected to the SLM process to fabricate composite samples at a laser power of 320 W and exposure time of 100 µs. The prepared composite was mechanically tested (hardness and tensile test) at ambient temperature, and obtained results indicate that the properties of the composite increased significantly with the addition of 0.2 wt. % Gr. Increment of about 25% (from 194 to 242 HV) and 70% (from 502 to 850 MPa) is obtained in hardness and yield strength of composite, respectively. Raman mapping and XRD were performed to see the distribution of Gr in the matrix and its effect on the formation of carbide, respectively. Results of Raman mapping show the uniform distribution of graphene inside the matrix. Electron back scatter diffraction (EBSD) map of the prepared composite was analyzed under FESEM in order to understand the microstructure and grain orientation. Due to thermal gradient, elongated grains were observed along the building direction, and grains get finer with the addition of Gr. Most of the mechanical components are subjected to several types of wear conditions. Therefore, it is very necessary to improve the wear property of the component, and hence apart from strength and hardness, a tribological property of composite was also measured under dry sliding condition. Solid lubrication property of Gr plays an important role during the sliding process due to which the wear rate of composite reduces up to 58%. Also, the surface roughness of worn surface reduces up to 70% as measured by 3D surface profilometry. Finally, it can be concluded that SLM is an efficient method of fabricating cutting edge metal matrix nano-composite having Gr like reinforcement, which was very difficult to fabricate through conventional manufacturing techniques. Prepared composite has superior mechanical and tribological properties and can be used for a wide variety of engineering applications. However, due to the unavailability of a considerable amount of literature in a similar domain, more experimental works need to perform, such as thermal property analysis, and is a part of ongoing study.

Keywords: selective laser melting, graphene, composite, mechanical property, tribological property

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