Search results for: diffraction

Authors: C. K. Ngaw

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Crystal facet engineering, which involves tuning and controlling a crystal surface and morphology, is a commonly employed strategy to optimize the performance of crystalline nanocrystals. The principle behind this strategy is that surface atomic rearrangement and coordination, which inherently determines their catalytic activity, can be easily tuned by morphological control. Because of this, the catalytic properties of a nanocrystal are closely related to the surface of an exposed facet, and it has provided great motivation for researchers to synthesize photocatalysts with high catalytic activity by maximizing reactive facets exposed through morphological control. In this contribution, octahedral NaInS₂ crystals have been successfully developed via solvothermal method. The formation of the octahedral NaInS₂ crystals was investigated using field emission scanning electron microscope (FESEM) and X-Ray diffraction (XRD), and results have shown that the concentration of sulphur precursor plays an important role in the growth process, leading to the formation of other NaInS₂ crystal structures in the form of hexagonal nanosheets and microspheres. Structural modeling analysis suggests that the octahedral NaInS₂ crystals were enclosed with {012} and {001} facets, while the nanosheets and microspheres are bounded with {001} facets only and without any specific facets, respectively. Visible-light photocatalytic H₂ evolution results revealed that the octahedral NaInS₂ crystals (~67 μmol/g/hr) exhibit ~6.1 and ~2.3 times enhancement as compared to the conventional NaInS₂ microspheres (~11 μmol/g/hr) and nanosheets (~29 μmol/g/hr), respectively. The H₂ enhancement of the NaInS₂ octahedral crystal is attributed to the presence of {012} facets on the surface. Detailed analysis of the octahedron model revealed obvious differences in the atomic arrangement between the {001} and {012} facets and this can affect the interaction between the water molecules and the surface facets before reducing into H₂ gas. These results highlight the importance of tailoring crystal morphology with highly reactive facets in improving photocatalytic properties.

Keywords: H₂ evolution, photocatalysis, octahedral, reactive facets

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Authors: Ganesh R. Bhand, N. B. Chaure

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Cadmium selenide (CdSe) quantum dots (QDs) were prepared by solvothermal route. Subsequently a inorganic QDs-organic semiconductor (copper phthalocyanine) nanocomposite (i.e CuPc:CdSe nanocomposites) were produced by different concentration of QDs varied in CuPc. The nanocomposite thin films have been prepared by means of spin coating technique. The optical, structural and morphological properties of nanocomposite films have been investigated. The transmission electron microscopy (TEM) confirmed the formation of QDs having average size of  4 nm. The X-ray diffraction pattern exhibits cubic crystal structure of CdSe with reflection to (111), (220) and (311) at 25.4ᵒ, 42.2ᵒ and 49.6ᵒ respectively. The additional peak observed at lower angle at 6.9ᵒ in nanocomposite thin films are associated to CuPc. The field emission scanning electron microscopy (FESEM) observed that surface morphology varied in increasing concentration of CdSe QDs. The obtained nanocomposite show significant improvement in the thermal stability as compared to the pure CuPc indicated by thermo-gravimetric analysis (TGA) in thermograph. The effect in the Raman spectra of composites samples gives a confirm evidence of homogenous dispersion of CdSe in the CuPc matrix and their strong interaction between them to promotes charge transfer property. The success of reaction between composite was confirmed by Fourier transform infrared spectroscopy (FTIR). The photo physical properties were studied using UV - visible spectroscopy. The enhancement of the optical absorption in visible region for nanocomposite layer was observed with increasing the concentration of CdSe in CuPc. This composite may obtain the maximized interface between QDs and polymer for efficient charge separation and enhance the charge transport. Such nanocomposite films for potential application in fabrication of hybrid solar cell with improved power conversion efficiency.

Keywords: CdSe QDs, cupper phthalocyanine, FTIR, optical absorption

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Authors: Weiwei Cao, Xiaodong Xing

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In order to effectively resolve the microbial pollution and contamination, synthetic nano-antibacterial materials are widely used in daily life. Among them, nanodiamonds (NDs) have recently been demonstrated to hold promise as useful materials in biomedical applications due to their high specific surface area and biocompatibility. In this work, the copolymer, poly(4-vinylpyridine-co-2-hydroxyethyl methacrylate) was applied for the surface functionalization of NDs to produce the quaternized poly(4-vinylpyridine-co-2-hydroxyethyl methacrylate)-functionalized NDs (QNDs). Then, QNDs were used as a substrate for silver nanoparticles (AgNPs) to produce a QND@Ag hybrid. The composition and morphology of the resultant nanostructures were confirmed by Fourier transform infrared spectra (FT-IR), transmission electron microscope (TEM), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). The mass fraction of AgNPs in the nanocomposites was about 35.7%. The antibacterial performances of the prepared nanocomposites were evaluated with Gram-negative Escherichia coli and Gram-positive Staphylococcus aureus by minimum inhibitory concentration (MIC), inhibition zone testing and time-kill study. As a result, due to the synergistic antibacterial activity of QND and AgNPs, this hybrid showed substantially higher antibacterial activity than QND and polyvinyl pyrrolidone (PVP)-stabilized AgNPs, and the AgNPs on QND@Ag were more stable than the Ag NPs on PVP, resulting in long-term antibacterial effects. More importantly, this hybrid showed excellent water solubility and low cytotoxicity, suggesting the great potential application in biomedical applications. The present work provided a simple strategy that successfully turned NDs into nanosized antibiotics with simultaneous superior stability and biocompatibility, which would broaden the applications of NDs and advance the development of novel antibacterial agents.

Keywords: cationic copolymer, nanodiamonds, silver nanoparticles, dual antibacterial activity, lower cytotoxicity

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Authors: Emineh Tsegahun Gedif

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Zinc oxide nanoparticles (ZnO NPs) have garnered significant attention due to their diverse applications encompassing catalytic, optical, photonic, and antibacterial properties. In this study, we successfully synthesized zinc oxide nanoparticles using a rapid, environmentally benign, and cost-effective method. Neem (Azadirachta indica) leaf extract served as the reducing agent for Zn (NO₃)₂.6H2O solution under optimized conditions (pH = 9). Qualitative screening techniques and FT-IR Spectroscopy confirmed the presence of active biomolecules such as flavonoids, phenolic groups, alkaloids, terpenoids, and tannins within the Neem leaf extract, both before and after reduction. The formation of ZnO NPs was visually evident through a distinct color change from colorless to light yellow. The biosynthesized nanoparticles underwent comprehensive characterization through UV-visible, FT-IR, and XRD spectroscopies. The reduction process proved to be straightforward and user-friendly, with UV-visible spectroscopy demonstrating a surface plasmon resonance (SPR) at 321 nm, unequivocally confirming the ZnO NP formation. X-ray diffraction analysis elucidated the crystal structure, revealing an average particle size of approximately 20 nm using Scherrer's equation based on the line width of the plane. Furthermore, the synthesized zinc oxide nanoparticles were evaluated for their antimicrobial properties against both Gram-positive and Gram-negative bacteria. The results showcased significant inhibitory activity, with the highest zone of inhibition observed against Escherichia coli (15 mm) and comparatively lower activity against Staphylococcus aureus. This research underscores the potential of Neem leaf extract-mediated synthesis of ZnO NPs as an eco-friendly and effective approach for various applications, including antibacterial agents.

Keywords: zinc oxide nanoparticles (ZnO NPs), bioreducing agent, green synthesis, antibacterial activity

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Authors: Reza Miresmaeili, Asghar Heydari Astaraee, Fereshteh Dolati

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In the present study, an analytical model based on dislocation density model was developed to simulate grain refinement in surface mechanical attrition treatment (SMAT). The correlation between SMAT time and development in plastic strain on one hand, and dislocation density evolution, on the other hand, was established to simulate the grain refinement in SMAT. A dislocation density-based constitutive material law was implemented using VUHARD subroutine. A random sequence of shots is taken into consideration for multiple impacts model using Python programming language by utilizing a random function. The simulation technique was to model each impact in a separate run and then transferring the results of each run as initial conditions for the next run (impact). The developed Finite Element (FE) model of multiple impacts describes the coverage evolution in SMAT. Simulations were run to coverage levels as high as 4500%. It is shown that the coverage implemented in the FE model is equal to the experimental coverage. It is depicted that numerical SMAT coverage parameter is adequately conforming to the well-known Avrami model. Comparison between numerical results and experimental measurements for residual stresses and depth of deformation layers confirms the performance of the established FE model for surface engineering evaluations in SMA treatment. X-ray diffraction (XRD) studies of grain refinement, including resultant grain size and dislocation density, were conducted to validate the established model. The full width at half-maximum in XRD profiles can be used to measure the grain size. Numerical results and experimental measurements of grain refinement illustrate good agreement and show the capability of established FE model to predict the gradient microstructure in SMA treatment.

Keywords: dislocation density, grain refinement, severe plastic deformation, simulation, surface mechanical attrition treatment

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Authors: Saba Didarataee, Abbas Ali Khodadadi, Yadollah Mortazavi, Fatemeh Mousavi

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Photocatalytic water splitting is one of the most attractive alternative methods for hydrogen evolution. A variety of nanoparticle engineering techniques were introduced to improve the activity of semiconductor photocatalysts. Among these methods, heterojunction formation is an appealing method due to its ability to effectively preventing electron-hole recombination and improving photocatalytic activity. Reaching an optimal ratio of the two target semiconductors for the formation of heterojunctions is still an open question. Considering environmental issues as well as the cost and availability, ZnS and ZnO are frequently studied as potential choices. In this study, first, the ZnS nanoparticle was synthesized in a hydrothermal process; the formation of ZnS nanorods with a diameter of 14-30 nm was confirmed by field emission scanning electron microscope (FESEM). Then two different methods, partial oxidation and chemical precipitation were employed to construct ZnS/ZnO core-shell heterojunction. X-ray diffraction (XRD), BET, and diffuse reflectance spectroscopy (DRS) analysis were carried out to determine crystallite phase, surface area, and bandgap of photocatalysts. Furthermore, the temperature of oxidation was specified by a temperature programmed oxidation (TPO) and was fixed at 510℃, at which mild oxidation occurred. The bandgap was calculated by the Kubelka-Munk method and decreased by increasing oxide content from 3.53 (pure ZnS) to 3.18 (pure ZnO). The optimal samples were determined by testing the photocatalytic activity of hydrogen evolution in a quartz photoreactor with side irradiation of UVC lamps with a wavelength of 254 nm. In both procedures, it was observed that the photocatalytic activity of the ZnS/ZnO composite was sensibly higher than the pure ZnS and ZnO, which is attributed to forming a type-II heterostructure. The best ratio of oxide to sulfide was 0.24 and 0.37 in partial oxidation and chemical precipitation, respectively. The highest hydrogen evolution was 1081 µmol/gr.h, gained from partial oxidizing of ZnS nanoparticles at 510℃ for 30 minutes.

Keywords: heterostructure, hydrogen, partial oxidation, photocatalyst, water splitting, ZnS

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Authors: Katarzyna Wal, Wojciech Stawiński, Piotr Rutkowski

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The scientific community is paying more and more attention to the problem of air pollution. Carbon dioxide is classified as one of the most harmful gases. Its emissions are generated during fossil fuel burning, waste management, and combustion and are responsible for global warming. Clay minerals constitute a group of promising materials for the role of adsorbents. They are composed of two types of phyllosilicate sheets: tetrahedral and octahedral, which form 1:1 or 2:1 structures. Vermiculite is one of their best-known representative, which can be used as an adsorbent from water and gaseous phase. The aim of the presented work was carbon dioxide adsorption on vermiculite. Acid-activated samples (W_NO3_x) were prepared by acid treatment with different concentrations of nitric acid (1, 2, 3, 4 mol L⁻¹). Vermiculite was subjected to modification in order to increase its porosity and adsorption properties. The prepared adsorbents were characterized using the BET-specific surface area analysis, thermogravimetry (TG), attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). Applied modifications significantly increase the specific surface area from 78,21 m² g⁻¹ for the unmodified sample (W_REF) to 536 m² g-1 for W_NO3_4. Obtained results showed that acid treatment tunes the material’s functional properties by increasing the contact surface and generating more active sites in its structure. The adsorption performance in terms carbon dioxide adsorption capacities follows the order of W_REF (25.91 mg g⁻¹) < W_NO3_1 (38.54 mg g⁻¹) < W_NO3_2 (44.03 mg g⁻¹) W_NO3_4 (67.51 mg g⁻¹) < W_NO3_3 (70.48 mg g⁻¹). Acid activation significantly improved the carbon dioxide adsorption properties of modified samples compared to raw material. These results demonstrate that vermiculite-based samples have the potential to be used as effective CO₂ adsorbents. Furthermore, acid treatment is a promising technique for improving the adsorption properties of clay minerals.

Keywords: adsorption, adsorbent, clay minerals, air pollution, environment

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Authors: Gustave Semugaza, Anne Zora Gierth, Tommy Mielke, Marianela Escobar Castillo, Nat Doru C. Lupascu

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The generation of Construction and Demolition Waste (CDW) has globally increased enormously due to the enhanced need in construction, renovation, and demolition of construction structures. Several studies investigated the use of CDW materials in the production of new concrete and indicated the lower mechanical properties of the resulting concrete. Many other researchers considered the possibility of using the Hydrated Cement Powder (HCP) to replace a part of Ordinary Portland Cement (OPC), but only very few investigated the use of Recycled Concrete Powder (RCP) from CDW. The partial replacement of OPC for making new concrete intends to decrease the CO₂ emissions associated with OPC production. However, the RCP and HCP need treatment to produce the new concrete of required mechanical properties. The thermal treatment method has proven to improve HCP properties before their use. Previous research has stated that for using HCP in concrete, the optimum results are achievable by heating HCP between 400°C and 800°C. The optimum heating temperature depends on the type of cement used to make the Hydrated Cement Specimens (HCS), the crushing and heating method of HCP, and the curing method of the Rehydrated Cement Specimens (RCS). This research assessed the quality of recycled materials by using different techniques such as X-ray Diffraction (XRD), Differential Scanning Calorimetry (DSC) and thermogravimetry (TG), Scanning electron Microscopy (SEM), and X-ray Fluorescence (XRF). These recycled materials were thermally pretreated at different temperatures from 200°C to 1000°C. Additionally, the research investigated to what extent the thermally treated recycled cement could partially replace the OPC and if the new concrete produced would achieve the required mechanical properties. The mechanical properties were evaluated on the RCS, obtained by mixing the Dehydrated Cement Powder and Recycled Powder (DCP and DRP) with water (w/c = 0.6 and w/c = 0.45). The research used the compressive testing machine for compressive strength testing, and the three-point bending test was used to assess the flexural strength.

Keywords: hydrated cement powder, dehydrated cement powder, recycled concrete powder, thermal treatment, reactivation, mechanical performance

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Authors: Noor Ul Huda, Mushtaq Ahmed, Nadia Mushtaq, Naila Sher, Rahmat Ali Khan

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Purpose: The green synthesis of AgNPs has been favored over chemical synthesis due to their distinctive properties such as high dispersion, surface-to-volume ratio, low toxicity, and easy preparation. In the present work, the biosynthesis of AgNPs (KE-AgNPs) was carried out in one step by using the traditionally used plant Kickxia elatine (KE) extract and then investigated its enzyme inhibiting activity against rat’s brain acetylcholinesterase (AChE) in vitro. Methods: KE-AgNPs were synthesized from 1mM AgNO₃ using KE extract and characterized by UV–spectroscopy, SEM, EDX, XRD, and FTIR analysis. Rat’s brain acetylcholinesterase (AChE) inhibition activity was evaluated by the standard protocol. Results: UV–spectrum at 416 nm confirmed the formation of KE-AgNPs. X-ray diffraction (XRD) pattern presented 2θ values corresponding to the crystalline nature of KE-AgNPs with an average size of 42.47nm. The scanning electron microscope (SEM) analysis confirmed the presence of spherical-shaped and huge density KE-AgNPs with a size of 50nm. Fourier transform infrared spectroscopy (FT-IR) suggested that the functional groups present in KE extract and on the surface of KE-AgNPs are responsible for the stability of biosynthesized NPs. Energy dispersive X-ray (EDX) displayed an intense sharp peak at 3.2 keV, presenting that Ag was the chief element with 61.67%. Both KE extract and KE-AgNPs showed good and potent anti-AChE activity, with higher inhibition potential at a concentration of 175 µg/ml. Statistical analysis showed that both KEE and AgNPs exhibited non-competitive type inhibition against AChE, i.e., Vmax decreased (34.17-68.64% and 22.29- 62.10%) in the concentration-dependent mode for KEE and KE-AgNPs respectively and while Km values remained constant. Conclusions: KEE and KE-AgNPs can be considered an inhibitor of rats’ brain AChE, and the synthesis of KE-AgNPs-based drugs can be used as a cheaper and alternative option against diseases such as Alzheimer’s disease.

Keywords: Kickxia elatine, AgNPs, brain homogenate, acetylcholinesterase, kinetics

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Authors: Ben Yahia Nouha, Sebei Abdelaziz, Boussen Slim, Chaabani Fredj

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The present work aims to determine mineralogical and geochemical characteristics of siliceous rock levels and to clarify the origin through geochemical arguments. This study was performed on the deposit of Tabarka-Babouch, which belongs to the northwestern of Tunisia; they spread out the later Miocene. Investigations were carried out to study mineralogical structure by XRD and chemical analysis by ICP-AES. The X-ray diffraction (XRD) patterns of the powdered natural rocks show that the Babouchite is composed mainly of quartz and clay minerals (smectite, illite, and kaolinite). Siliceous rocks contain quartz as a major silica mineral, which is characterized by two broad reflections at the vicinity of 4.26Å and 3.34 Å, respectively, with a total lack of opal-CT. That confirms that these siliceous rocks are quartz-rich (can reach 90%). Indeed, the amounts of all clay minerals (ACM), constituted essentially by smectite marked by a close association with illite and kaolinite, are relatively high, where their percentages vary from 7 to 46%. Chemical analyses show that the major oxide contents are consistent with mineralogical observations. It reveals that the siliceous rocks of the Babouchite formation are rich in SiO₂. The data of whole-rock chemical analyses indicate that the SiO₂ content is generally in the range 73-91 wt.%; (average: 80.43 wt.%). The concentration of Al₂O₃, which represent the detrital fractions in the studied samples, varies from 3.99 to 10.55 wt. % and Fe₂O₃ from 0.73 to 4.41wt. %. The low levels recorded in CaO (%) show that the carbonate is considered impurities. However, these rocks contain a low amount of some others oxides, such as the following: Na₂O, MgO, K₂O, and TiO₂. The trace elemental distributions also vary with high Sr (up to 84.55 ppm), Cu (5–127 ppm), and Zn (up to 124 ppm), with a relatively lower concentration of Co (2.43-25.54 ppm), Cr (10–61 ppm) and Pb (8-22ppm). The Babouchite siliceous rocks of northwestern of Tunisia have generally high Al/ (Al+Fe+Mn) values (0.63-0.83). The majority of Al/ (Al+Fe+Mn) values are nearly of 0.6, which is the biogenic end-member. Thus, Al/ (Al+Fe+Mn) values revealed the biogenic origin of silica.

Keywords: siliceous rocks, Babouchite formation, XRD, chemical analysis, biogenic silica, Northwestern of Tunisia

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Authors: Marco Naegele, Klaus Stoppel, Thomas Dekorsy

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Passively Q-switched microchip lasers enable the great potential for sophisticated LiDAR systems due to their compact overall system design, excellent beam quality, and scalable pulse energies. However, many near-infrared solid-state lasers show emitting wavelengths > 1000 nm, which are not compatible with state-of-the-art silicon detectors. Here we demonstrate a passively Q-switched microchip laser operating at 914 nm. The microchip laser consists of a 3 mm long Nd:YVO₄ crystal as a gain medium, while Cr⁴⁺:YAG with an initial transmission of 98% is used as a saturable absorber. Quasi-continuous pumping enables single pulse operation, and low duty cycles ensure low overall heat generation and power consumption. Thus, thermally induced instabilities are minimized, and operation without active cooling is possible while ambient temperature changes are compensated by adjustment of the pump laser current only. Single-emitter diode pumping at 808 nm leads to a compact overall system design and robust setup. Utilization of a microchip cavity approach ensures single-longitudinal mode operation with spectral bandwidths in the picometer regime and results in short laser pulses with pulse durations below 10 ns. Beam quality measurements reveal an almost diffraction-limited beam and enable conclusions concerning the thermal lens, which is essential to stabilize the plane-plane resonator. A 7% output coupler transmissivity is used to generate pulses with energies in the microjoule regime and peak powers of more than 600 W. Long-term pulse duration, pulse energy, central wavelength, and spectral bandwidth measurements emphasize the excellent system stability and facilitate the utilization of this laser in the context of a LiDAR system.

Keywords: diode-pumping, LiDAR system, microchip laser, Nd:YVO4 laser, passively Q-switched

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Authors: Malay K. Das, Bhanu P. Sahu

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Furosemide is a weakly acidic diuretic indicated for treatment of edema and hypertension. It has very poor solubility but high permeability through stomach and upper gastrointestinal tract (GIT). Due to its limited solubility it has poor and variable oral bioavailability of 10-90%. The aim of this study was to enhance the oral bioavailability of furosemide by preparation of nanosuspensions. The nanosuspensions were prepared by nanoprecipitation with sonication using DMSO (dimethyl sulfoxide) as a solvent and water as an antisolvent (NA). The prepared nanosuspensions were sterically stabilized with polyvinyl acetate (PVA).These were characterized for particle size, ζ potential, polydispersity index, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), X-ray diffraction (XRD) pattern and release behavior. The effect of nanoprecipitation on oral bioavailability of furosemide nanosuspension was studied by in vitro dissolution and in vivo absorption study in rats and compared to pure drug. The stable nanosuspension was obtained with average size range of the precipitated nanoparticles between 150-300 nm and was found to be homogenous showing a narrow polydispersity index of 0.3±0.1. DSC and XRD studies indicated that the crystalline furosemide drug was converted to amorphous form upon precipitation into nanoparticles. The release profiles of nanosuspension formulation showed up to 81.2% release in 4 h. The in vivo studies on rats revealed a significant increase in the oral absorption of furosemide in the nanosuspension compared to pure drug. The AUC0→24 and Cmax values of nanosuspension were approximately 1.38 and 1.68-fold greater than that of pure drug, respectively. Furosemide nanosuspension showed 20.06±0.02 % decrease in systolic blood pressure compared to 13.37±0.02 % in plain furosemide suspension, respectively. The improved oral bioavailability and pharmacodynamics effect of furosemide may be due to the improved dissolution of furosemide in simulated gastric fluid which results in enhanced oral systemic absorption of furosemide from stomach region where it has better permeability.

Keywords: furosemide, nanosuspension, bioavailability enhancement, nanoprecipitation, oral drug delivery

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Authors: Moses C. Siame, Kazutoshi Haga, Atsushi Shibayama

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This study investigates the removal of silica, alumina and phosphorus as impurities from Sanje iron ore using wet high-intensity magnetic separation (WHIMS). Sanje iron ore contains low-grade hematite ore found in Nampundwe area of Zambia from which iron is to be used as the feed in the steelmaking process. The chemical composition analysis using X-ray Florence spectrometer showed that Sanje low-grade ore contains 48.90 mass% of hematite (Fe₂O₃) with 34.18 mass% as an iron grade. The ore also contains silica (SiO₂) and alumina (Al₂O₃) of 31.10 mass% and 7.65 mass% respectively. The mineralogical analysis using X-ray diffraction spectrometer showed hematite and silica as the major mineral components of the ore while magnetite and alumina exist as minor mineral components. Mineral particle distribution analysis was done using scanning electron microscope with an X-ray energy dispersion spectrometry (SEM-EDS) and images showed that the average mineral size distribution of alumina-silicate gangue particles is in order of 100 μm and exists as iron-bearing interlocked particles. Magnetic separation was done using series L model 4 Magnetic Separator. The effect of various magnetic separation parameters such as magnetic flux density, particle size, and pulp density of the feed was studied during magnetic separation experiments. The ore with average particle size of 25 µm and pulp density of 2.5% was concentrated using pulp flow of 7 L/min. The results showed that 10 T was optimal magnetic flux density which enhanced the recovery of 93.08% of iron with 53.22 mass% grade. The gangue mineral particles containing 12 mass% silica and 3.94 mass% alumna remained in the concentrate, therefore the concentrate was further treated in the second stage WHIMS using the same parameters from the first stage. The second stage process recovered 83.41% of iron with 67.07 mass% grade. Silica was reduced to 2.14 mass% and alumina to 1.30 mass%. Accordingly, phosphorus was also reduced to 0.02 mass%. Therefore, the two stage magnetic separation process was established using these results.

Keywords: Sanje iron ore, magnetic separation, silica, alumina, recovery

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Authors: Saeedeh Imani Moqadam, Ilya Bobrov, Jérémy Epp, Nils Ellendt, Lutz Mädler

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High entropy alloys (HEAs), having adjustable properties and enhanced stability compared with intermetallic compounds, are solid solution alloys that contain more than five principal elements with almost equal atomic percentage. The concept of producing such alloys pave the way for developing advanced materials with unique properties. However, the synthesis of such alloys may require advanced processes with high cooling rates depending on which alloy elements are used. In this study, the micro spheres of different diameters of HEAs were generated via a drop-on-demand droplet generator and subsequently solidified during free-fall in an argon atmosphere. Such droplet generators can generate individual droplets with high reproducibility regarding droplet diameter, trajectory and cooling while avoiding any interparticle momentum or thermal coupling. Metallography as well as X-ray diffraction investigations for each diameter of the generated metallic droplets where then carried out to obtain information about the microstructural state. To calculate the cooling rate of the droplets, a droplet cooling model was developed and validated using model alloys such as CuSn%6 and AlCu%4.5 for which a correlation of secondary dendrite arm spacing (SDAS) and cooling rate is well-known. Droplets were generated from these alloys and their SDAS was determined using quantitative metallography. The cooling rate was then determined from the SDAS and used to validate the cooling rates obtained from the droplet cooling model. The application of that model on the HEA then leads to the cooling rate dependency and hence to the identification of process windows for the synthesis of these alloys. These process windows were then compared with cooling rates obtained in processes such as powder production, spray forming, selective laser melting and casting to predict if a synthesis is possible with these processes.

Keywords: cooling rate, drop-on-demand, high entropy alloys, microstructure, single droplet generation, X-ray Diffractometry

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Authors: Amirhossein Moghanian, Morteza Elsa, Mehrnaz Aminitabar

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Modified bioactive glass has been considered as a promising multifunctional candidate in bone repair and regeneration due to its attractive properties. The present study mainly aims to evaluate how the individual substitution of lithium (L-BG) and magnesium (M-BG) for calcium can affect the in vitro bioactivity of sol-gel derived substituted 58S bioactive glass (BG); and to present one composition in both of the 60SiO2–(36-x)CaO–4P₂O₅–(x)Li₂O and 60SiO₂ –(36-x)CaO–4P₂O₅–(x)MgO quaternary systems (where x= 0, 5, 10 mol.%) with improved biocompatibility, enhanced alkaline phosphatase (ALP) activity, and the most efficient antibacterial activity against methicillin-resistant staphylococcus aureus bacteria. To address these aims, and study the effect of CaO/Li₂O and CaO/MgO substitution up to 10 mol % in 58S-BGs, the samples were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, inductively coupled plasma atomic emission spectrometry and scanning electron microscopy after immersion in simulated body fluid up to 14 days. Results indicated that substitution of either CaO/ Li₂O and CaO/ MgO had a retarding effect on in vitro hydroxyapatite (HA) formation due to the lower supersaturation degree for nucleation of HA compared with 58s-BG. Meanwhile, magnesium had a more pronounced effect. The 3-(4,5dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) and alkaline phosphatase (ALP) assays showed that both substitutions of CaO/ Li₂O and CaO/ MgO up to 5mol % in 58s-BGs led to increased biocompatibility and stimulated proliferation of the pre-osteoblast MC3T3 cells with respect to the control. On the other hand, the substitution of either Li or Mg for Ca in the 58s BG composition resulted in improved bactericidal efficiency against MRSA bacteria. Taken together, sample 58s-BG with 5 mol % CaO/Li₂O substitution (BG-5L) was considered as a multifunctional biomaterial in bone repair/regeneration with improved biocompatibility, enhanced ALP activity as well as significant antibacterial activity against methicillin-resistant staphylococcus aureus (MRSA) bacteria.

Keywords: alkaline, alkaline earth, bioactivity, biomedical applications, sol-gel processes

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Authors: Sachin Pawar, Suman Patra, Goutam Mukhopadhyay

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The primary function of a shaft is to transfer power. The shaft can be cast or forged and then machined to the final shape. Manufacturing of ~5 m length and 0.6 m diameter shaft is very critical. More difficult is to maintain its straightness during heat treatment and machining operations, which involve thermal and mechanical loads, respectively. During the machining operation of a such forged mandrel shaft, a deflection of 3-4mm was observed. To remove this deflection shaft was pressed at both ends which led to the development of cracks in it. To investigate the root cause of the deflection and cracking, the sample was cut from the failed shaft. Possible causes were identified with the help of a cause and effect diagram. Chemical composition analysis, microstructural analysis, and hardness measurement were done to confirm whether the shaft meets the required specifications or not. Chemical composition analysis confirmed that the material grade was 42CrMo4. Microstructural analysis revealed the presence of untempered martensite, indicating improper heat treatment. Due to this, ductility and impact toughness values were considerably lower than the specification of the mentioned grade. Residual stress measurement of one more bent shaft manufactured by a similar route was done by portable X-ray diffraction(XRD) technique. For better understanding, measurements were done at twelve different locations along the length of the shaft. The occurrence of a high amount of undesirable tensile residual stresses close to the Ultimate Tensile Strength(UTS) of the material was observed. Untempered martensitic structure, lower ductility, lower impact strength, and presence of a high amount of residual stresses all confirmed the improper tempering heat treatment of the shaft. Tempering relieves the residual stresses. Based on the findings of this study, stress-relieving heat treatment was done to remove the residual stresses and deflection in the shaft successfully.

Keywords: residual stress, mandrel shaft, untempered martensite, portable XRD

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Authors: Muhammad Waheed Mushtaq, Shahid bashir, Atta Ur Rehman

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In the past decade, the growing demand for capital and the increased utilization of supercapacitors reflect advancements in energy-producing systems and energy storage devices. Metal oxides and ferrites have emerged as promising candidates for supercapacitors and batteries. In our current study, we synthesized Lithium manganese nanoferrite, denoted as LixMnxFe₂O₄, using the hydrothermal technique. Subsequently, we treated it with sodium dodecyl benzene sulphonate (SDBS) surfactant to create nanocomposites of Lithium manganese nano ferrite (LMFe) with poly pyrrole (LixMnxFe₂O₄-PPY). We employed Powder X-ray diffraction (XRD) to confirm the crystalline nature and spinel phase structure of LMFe nanoparticles, which exhibited a single-phase crystal structure, indicating sample purity. To assess the surface topography, morphology, and grain size of both synthesized LixMnxFe₂O₄ and LixMnxFe₂O₄-PPY, we used atomic force microscopy and scanning electron microscopy (SEM). The average particle size of pure ferrite was found to be 54 nm, while that of its nanocomposite was 71 nm. Energy dispersive X-ray (EDX) analysis confirmed the presence of all required elements, including Li, Mn, Fe, and O, in the appropriate proportions. Saturation magnetization (32.69 emu), remanence (Mr), and coercive force (Hc) were measured using a Vibrating Sample Magnetometer (VSM). To assess the electrochemical performance of the material, we conducted Cyclic Voltammetry (CV) measurements for both pure LMFe and LMFe-PPY. The CV results for LMFe-PPY demonstrated that specific capacitance decreased with increasing scan rate while the area of the current-voltage loop increased. These findings are promising for the development of supercapacitors and lithium-ion batteries (LIBs).

Keywords: lithium manganese ferrite, poly pyrrole, nanocomposites, cyclic voltammetry, cathode

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Authors: A. Kabir, D. Boulainine, I. Bouanane, N. Benslim, B. Boudjema, C. Sedrati

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SnO₂ is an n-type semiconductor with a direct gap of about 3.6 eV. It is largely used in several domains such as nanocrystalline photovoltaic cells. Due to its interesting physic-chemical properties, this material was elaborated in thin film forms using different deposition techniques. It was found that SnO₂ properties were directly affected by the deposition method parameters. In this work, the RGTO method (Rheotaxial Growth and Thermal Oxidation) was used to deposit elaborate SnO₂ thin films. This technique consists on thermal oxidation of the Sn films deposited onto a substrate heated to a temperature close to Sn melting point (232°C). Such process allows the preparation of high porosity tin oxide films which are very suitable for the gas sensing. The films structural, morphological and optical properties pre and post thermal oxidation were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-Visible spectroscopy and Fourier transform infrared spectroscopy (FTIR) respectively. XRD patterns showed a polycrystalline structure of the cassiterite phase of SnO₂. The grain growth was found affected by the oxidation temperature. This grain size evolution was confronted to existing grain growth models in order to understand the growth mechanism. From SEM images, the as deposited Sn film was formed of difference diameter spherical agglomerations. As a function of the oxidation temperature, these spherical agglomerations shape changed due to the introduction of oxygen ions. The deformed spheres started to interconnect by forming bridges between them. The volume porosity, determined from the UV-Visible reflexion spectra, Changes as a function of the oxidation temperature. The variation of the crystalline fraction, determined from FTIR spectra, correlated with the variation of both the grain size and the volume porosity.

Keywords: tin oxide, RGTO, grain growth, volume porosity, crystalline fraction

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Authors: Suresh Vanguri, Suresh Palla, Prasad G., Ramaswamy V., Kalyani K. V., Chaturvedi S. K., Mohapatra B. N., Sunder Rao TBVN

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The utilization of industrial waste materials and by-products in the cement industry helps in the conservation of natural resources besides avoiding the problems arising due to waste dumping. The use of non-carbonated materials as raw mix components in clinker manufacturing is identified as one of the key areas to reduce Green House Gas (GHG) emissions. Chrome sludge is a waste material generated from the manufacturing process of sodium dichromate. This paper aims to present studies on the use of chrome sludge in clinker manufacturing, its impact on the development of clinker mineral phases and on the cement properties. Chrome sludge was found to contain substantial amounts of CaO, Fe2O3 and Al2O3 and therefore was used to replace some conventional sources of alumina and iron in the raw mix. Different mixes were prepared by varying the chrome sludge content from 0 to 5 % and the mixes were evaluated for burnability. Laboratory prepared clinker samples were evaluated for qualitative and quantitative mineralogy using X-ray Diffraction Studies (XRD). Optical microscopy was employed to study the distribution of clinker phases, their granulometry and mineralogy. Since chrome sludge also contains considerable amounts of chromium, studies were conducted on the leachability of heavy elements in the chrome sludge as well as in the resultant cement samples. Estimation of heavy elements, including chromium was carried out using ICP-OES. Further, the state of chromium valence, Cr (III) & Cr (VI), was studied using conventional chemical analysis methods coupled with UV-VIS spectroscopy. Assimilation of chromium in the clinker phases was investigated using SEM-EDXA studies. Bulk cement was prepared from the clinker to study the effect of chromium sludge on the cement properties such as setting time, soundness, strength development against the control cement. Studies indicated that chrome sludge can be successfully utilized and its content needs to be optimized based on raw material characteristics.

Keywords: chrome sludge, leaching, mineralogy, non-carbonate materials

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Authors: Rabindranath Jana, Plabani Basu, Keka Rana

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Nucleating agents are widely used to modify the properties of various polymers. The rate of crystallization and the size of the crystals have a strong impact on mechanical and optical properties of a polymer. The addition of nucleating agents to the semi-crystalline polymers provides a surface on which the crystal growth can start easily. As a consequence, fast crystal formation will result in many small crystal domains so that the cycle times for injection molding may be reduced. Moreover, the mechanical properties e.g., modulus, tensile strength, heat distortion temperature and hardness may increase. In the present work, multi-walled carbon nanotubes (MWNTs) as nucleating agents for the crystallization of poly (e-caprolactone)diol (PCL). Thus nanocomposites of PCL filled with MWNTs were prepared by solution blending. Differential scanning calorimetry (DSC) tests were carried out to study the effect of CNTs on on-isothermal crystallization of PCL. The polarizing optical microscopy (POM), and wide-angle X-ray diffraction (WAXD) were used to study the morphology and crystal structure of PCL and its nanocomposites. It is found that MWNTs act as effective nucleating agents that significantly shorten the induction period of crystallization and however, decrease the crystallization rate of PCL, exhibiting a remarkable decrease in the Avrami exponent n, surface folding energy σe and crystallization activation energy ΔE. The carbon-based fillers act as templates for hard block chains of PCL to form an ordered structure on the surface of nanoparticles during the induction period, bringing about some increase in equilibrium temperature. The melting process of PCL and its nanocomposites are also studied; the nanocomposites exhibit two melting peaks at higher crystallization temperature which mainly refer to the melting of the crystals with different crystal sizes however, PCL shows only one melting temperature.

Keywords: poly(e-caprolactone)diol, multiwalled carbon nanotubes, composite materials, nonisothermal crystallization, crystal structure, nucleation

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Authors: H. Aripin, I. Made Joni, Edvin Priatna, Nundang Busaeri, Svilen Sabchevski

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In this investigation, manganese has been produced from medium grade manganese ore from Karangnunggal mine (West Java, Indonesia). The ores were grinded using a jar mill to pass through a 150 mesh sieve. The effects of keeping it at a temperature of 1200 °C in methane gas on the structural properties have been studied. The material’s properties have been characterized on the basis of the experimental data obtained using X-ray fluorescence (XRF), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), and Fourier transform infrared (FTIR) spectroscopy. It has been found that the ore contains MnO₂ as the main constituents at about 46.80 wt.%. It can be also observed that the ore particles are agglomerated forming dense grains with different texture and morphology. The irregular-shaped grains with dark contrast, the large brighter grains, and smaller grains with bright texture and smooth surfaces are associated with the presence of manganese, calcium, and quartz, respectively. From XRD patterns, MnO₂ is reduced to hausmannite (Mn₃O₄), manganosite (MnO) and manganese carbide (Mn₇C₃). At a temperature of 1200°C the keeping time does not have any effect on the formation of crystals and the crystalline phases remain almost unchanged in the time range from 15 to 90 minutes. An increase of the keeping time up to 45 minutes during the sintering process leads to an increase of the MnO concentration, while at 90 minutes, the concentration decreases. At longer keeping times the excess reaction of the methane gas and manganese oxide in the ore causes an increase of carbon deposition. As a result, it blocks the particle surface and then hinders the reduction process of manganese oxide. From FTIR spectrum allows one to explain that the appearance of C=O stretching mode arises from absorption of atmospheric methane and manganese oxide of the ore. The intensity of this band increases with increasing the keeping time, indicating an increase of carbon deposition on the surface of manganese oxide.

Keywords: manganese, medium grade manganese ore, structural properties, keeping the temperature, carbon deposition

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Authors: Steffen Illig, Alexander S. Eggeman, Alessandro Troisi, Stephen G. Yeates, John E. Anthony, Henning Sirringhaus

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Large-amplitude intermolecular vibrations in combination with complex shaped transfer integrals generate a thermally fluctuating energetic landscape. The resulting dynamic disorder and its intrinsic presence in organic semiconductors is one of the most fundamental differences to their inorganic counterparts. Dynamic disorder is believed to govern many of the unique electrical and optical properties of organic systems. However, the low energy nature of these vibrations makes it difficult to access them experimentally and because of this we still lack clear molecular design rules to control and reduce dynamic disorder. Applying a novel technique based on electron diffraction we encountered strong intermolecular, thermal vibrations in every single organic material we studied (14 up to date), indicating that a large degree of dynamic disorder is a universal phenomenon in organic crystals. In this paper a new molecular design strategy will be presented to avoid dynamic disorder. We found that small molecules that have their side chains attached to the long axis of their conjugated core have been found to be less likely to suffer from dynamic disorder effects. In particular, we demonstrate that 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothio-phene (C8-BTBT) and 2,9-di-decyl-dinaphtho-[2,3-b:20,30-f]-thieno-[3,2-b]-thiophene (C10DNTT) exhibit strongly reduced thermal vibrations in comparison to other molecules and relate their outstanding performance to their lower dynamic disorder. We rationalize the low degree of dynamic disorder in C8-BTBT and C10-DNTT with a better encapsulation of the conjugated cores in the crystal structure which helps reduce large amplitude thermal motions. The work presented in this paper provides a general strategy for the design of new classes of very high mobility organic semiconductors with low dynamic disorder.

Keywords: charge transport, C8-BTBT, C10-DNTT, dynamic disorder, organic semiconductors, thermal vibrations

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Authors: Yatimah Alias, Tilagam Marimuthu, M. R. Mahmoudian, Sharifah Mohamad

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The rapid growth of science and technology in energy and environmental fields has enlightened the substantial importance of the conducting polymer and metal composite materials engineered at nano-scale. In this study, polypyrrole-cobalt composites (PPy-Co Cs) and polypyrrole-nickel oxide composites (PPy-NiO Cs) were prepared by a simple and facile chemical polymerization method with an aqueous solution of pyrrole monomer in the presence of metal salt. These composites then fabricated into non-enzymatic hydrogen peroxide (H2O2) and glucose sensor. The morphology and composition of the composites are characterized by the Field Emission Scanning Electron Microscope, Fourier Transform Infrared Spectrum and X-ray Powder Diffraction. The obtained results were compared with the pure PPy and metal oxide particles. The structural and morphology properties of synthesized composites are different from those of pure PPy and metal oxide particles, which were attributed to the strong interaction between the PPy and the metal particles. Besides, a favorable micro-environment for the electrochemical oxidation of H2O2 and glucose was achieved on the modified glassy carbon electrode (GCE) coated with PPy-Co Cs and PPy-NiO Cs respectively, resulting in an enhanced amperometric response. Both PPy-Co/GCE and PPy-NiO/GCE give high response towards target analyte at optimum condition of 500 μl pyrrole monomer content. Furthermore, the presence of pyrrole monomer greatly increases the sensitivity of the respective modified electrode. The PPy-Co/GCE could detect H2O2 in a linear range of 20 μM to 80 mM with two linear segments (low and high concentration of H2O2) and the detection limit for both ranges is 2.05 μM and 19.64 μM, respectively. Besides, PPy-NiO/GCE exhibited good electrocatalytic behavior towards glucose oxidation in alkaline medium and could detect glucose in linear ranges of 0.01 mM to 0.50 mM and 1 mM to 20 mM with detection limit of 0.33 and 5.77 μM, respectively. The ease of modifying and the long-term stability of this sensor have made it superior to enzymatic sensors, which must kept in a critical environment.

Keywords: metal oxide, composite, non-enzymatic sensor, polypyrrole

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Authors: Sonia Barbouchi, Meriem Samcha

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Scale deposition during water injection into aquifer of oil reservoirs is a serious problem experienced in the oil production industry. One of the primary causes of scale formation and injection well plugging is mixing two waters which are incompatible. Considered individually, the waters may be quite stable at system conditions and present no scale problems. However, once they are mixed, reactions between ions dissolved in the individual waters may form insoluble products. The purpose of this study is to identify the causes of well plugging in a southern Tunisian oilfield, where fresh water has been injected into the producing wells to counteract the salinity of the formation waters and inhibit the deposition of halite. X-ray diffraction (XRD) mineralogical analysis has been carried out on scale samples collected from the blocked well. Two samples collected from both formation water and injected water were analysed using inductively coupled plasma atomic emission spectroscopy, ion chromatography and other standard laboratory techniques. The results of complete waters analysis were the typical input parameters, to determine scaling tendency. Saturation indices values related to CaCO3, CaSO4, BaSO4 and SrSO4 scales were calculated for the water mixtures at different share, under various conditions of temperature, using a computerized scale prediction model. The compatibility study results showed that mixing the two waters tends to increase the probability of barite deposition. XRD analysis confirmed the compatibility study results, since it proved that the analysed deposits consisted predominantly of barite with minor galena. At the studied temperatures conditions, the tendency for barite scale is significantly increasing with the increase of fresh water share in the mixture. The future scale inhibition and removal strategies to be implemented in the concerned oilfield are being derived in a large part from the results of the present study.

Keywords: compatibility study, produced water, scaling, water injection

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Authors: Suresh Vanguri, Suresh Palla, K. V. Kalyani, S. K. Chaturvedi, B. N. Mohapatra

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Enhancing the fly ash utilization in the manufacture of cement is identified as one of the key areas to mitigate the Green House Gas emissions from the cement industry. Though increasing the fly ash content in cement has economic and environmental benefits, it results in a decrease in the compressive strength values, particularly at early ages. Quality of clinker and fly ash were identified as predominant factors that govern the extent of absorption of fly ash in the manufacturing of cement. This paper presents systematic investigations on the effect of clinker and fly ash quality on the properties of resultant cement. Since mechanical activation alters the physicochemical properties such as particle size distribution, surface area, phase morphology, understanding the variation of these properties with activation is required for its applications. The effect of mechanical activation on fly ash surface area, specific gravity, flow properties, lime reactivity, comparative compressive strength (CCS), reactive silica and mineralogical properties were also studied. The fineness of fly ash was determined by Blaine’s method, specific gravity, lime reactivity, CCS were determined as per the method IS 1727-1967. The phase composition of fly ash was studied using the X-ray Diffraction technique. The changes in the microstructure and morphology with activation were examined using the scanning electron microscope. The studies presented in this paper also include evaluation of Portland Pozzolana Cement (PPC), prepared using high volume fly ash. Studies are being carried out using clinker from cement plants located in different regions/clusters in India. Blends of PPC containing higher contents of activated fly ash have been prepared and investigated for their chemical and physical properties, as per Indian Standard procedures. Changes in the microstructure of fly ash with activation and mechanical properties of resultant cement containing high volumes of fly ash indicated the significance of optimization of the quality of clinker and fly ash fineness for better techno-economical benefits.

Keywords: flow properties, fly ash enhancement, lime reactivity, microstructure, mineralogy

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Authors: Golam Saklayen, Sheikh Rashel al Ahmed, Ferdous Rahman, Ismail Abu Bakar

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Investigation on Lanthanum Fluoride LaF3 layer embedding Silicon Nanocrystals (Si-NCs) fabricated using a novel one-step chemical method has been reported in this presentation. Application of this material has been tested for low-voltage operating non-volatile memory and Schottkey-junction solar cell. Colloidal solution of Si-NCs in hydrofluoric acid (HF) was prepared from meso-porous silicon by ultrasonic vibration (sonication). This solution prevents the Si-NCs to be oxidized. On a silicon (Si) substrate, LaCl3 solution in HCl is allowed to react with the colloidal solution of prepared Si-NCs. Since this solution contains HF, LaCl3 reacts with HF and produces LaF3 crystals that deposits on the silicon substrate as a layer embedding Si-NCs. This a novel single step chemical way of depositing LaF3 insulating layer embedding Si-NCs. The X-Ray diffraction of the deposited layer shows a polycrystalline LaF3 deposition on silicon. A non-stoichiometric LaF3 layer embedding Si-NCs was found by EDX analysis. The presence of Si-NCs was confirmed by SEM. FTIR spectroscopy of the deposited LaF3 powder also confirmed the presence of Si-NCs. The size of Si-NCs was found to be inversely proportional to the ultrasonic power. After depositing proper contacts on the back of Si and LaF3, the devices have been tested as a non-volatile memory and solar cell. A memory window of 525 mV was obtained at a programming and erasing bias of 2V. The LaF3 films with Si NCs showed strong absorption and was also found to decrease optical transmittance than pure LaF3 film of same thickness. The I-V characteristics of the films showed a dependency on the incident light intensity where current changed under various light illumination. Experimental results show a lot of promise for Si-NCs-embedded LaF3 layer to be used as an insulating layer in MIS devices as well as an photoactive material in Schottkey junction solar cells.

Keywords: silicon nanocrystals (Si NCs), LaF3, colloidal solution, Schottky junction solar cell

Procedia PDF Downloads 392

Authors: Amir Khaleghipour, Amirhossein Moghanian, Elhamalsadat Ghaffari

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Modified bioactive glass has been considered as a promising multifunctional candidate in bone repair and regeneration due to its attractive properties. The present study mainly aims to evaluate how the individual substitution of lithium (L-BG) and magnesium (M-BG) for calcium can affect the in vitro bioactivity of sol-gel derived substituted 58S bioactive glass (BG); and to present one composition in both of the 60SiO₂–(36-x)CaO–4P₂O₅–(x)Li₂O and 60SiO₂–(36-x)CaO–4P₂O₅–(x)MgO quaternary systems (where x= 0, 5, 10 mol.%) with improved biocompatibility, enhanced alkaline phosphatase (ALP) activity, and the most efficient antibacterial activity against methicillin-resistant Staphylococcus aureus bacteria. To address these aims, and study the effect of CaO/Li₂O and CaO/MgO substitution up to 10 mol % in 58S-BGs, the samples were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, inductively coupled plasma atomic emission spectrometry and scanning electron microscopy after immersion in simulated body fluid up to 14 days. Results indicated that substitution of either CaO/ Li₂O and CaO/ MgO had a retarding effect on in vitro hydroxyapatite (HA) formation due to the lower supersaturation degree for nucleation of HA compared with 58s-BG. Meanwhile, magnesium had a more pronounced effect. The 3-(4, 5dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) and alkaline phosphatase (ALP) assays showed that both substitutions of CaO/ Li₂O and CaO/ MgO up to 5mol % in 58s-BGs led to increased biocompatibility and stimulated proliferation of the pre-osteoblast MC3T3 cells with respect to the control. On the other hand, substitution of either Li or Mg for Ca in the 58s BG composition resulted in improved bactericidal efficiency against MRSA bacteria. Taken together, sample 58s-BG with 5 mol % CaO/Li₂O substitution (BG-5L) was considered as a multifunctional biomaterial in bone repair/regeneration with improved biocompatibility, enhanced ALP activity as well enhanced antibacterial efficiency against methicillin-resistant Staphylococcus aureus (MRSA) bacteria among all of the synthesized L-BGs and M-BGs.

Keywords: alkaline, alkaline earth, bioactivity, biomedical applications, sol-gel processes

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Authors: Omkar Gaonkar, Indumathi Nambi, Suresh G. Kumar

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The functional and morphological aspects of soil structure determine the soil quality. The dispersion of colloidal soil particles, especially the clay fraction and rupture of soil aggregates, both of which play an important role in soil structure development, lead to degradation of soil quality. The main objective of this work was to determine the effect of the behaviour of soil colloids on the agricultural soil structure and quality. The effect of commercial humic acid and soil natural organic matter on the electrical and structural properties of the soil colloids was also studied. Agricultural soil, belonging to the sandy loam texture class from northern part of India was considered in this study. In order to understand the changes in the soil quality in the presence and absence of humic acids, the soil fabric and structure was analyzed by X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) Spectroscopy and Scanning Electron Microscopy (SEM). Electrical properties of natural soil colloids in aqueous suspensions were assessed by zeta potential measurements at varying pH values with and without the presence of humic acids. The influence of natural organic matter was analyzed by oxidizing the natural soil organic matter with hydrogen peroxide. The zeta potential of the soil colloids was found to be negative in the pH range studied. The results indicated that hydrogen peroxide treatment leads to deflocculation of colloidal soil particles. In addition, the humic acids undergoes effective adsorption onto the soil surface imparting more negative zeta potential to the colloidal soil particles. The soil hydrophilicity decreased in the presence of humic acids which was confirmed by surface free energy determination. Thus, it can be concluded that the presence of humic acids altered the soil fabric and structure, thereby affecting the soil quality. This study assumes significance in understanding soil aggregation and the interactions at soil solid-liquid interface.

Keywords: humic acids, natural organic matter, zeta potential, soil quality

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Authors: S. Mohajeri

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Electrocodeposition of Ni-TiO2 nanocomposite single layers and Ni-TiO2/TiO2 multilayers from Watts bath containing TiO2 sol was carried out on copper substrate. Pulse plating and pulse reverse plating techniques were applied to facilitate higher incorporations of TiO2 nanoparticles in Ni-TiO2 nanocomposite single layers, and the results revealed that by prolongation of the current-off durations and the anodic cycles, deposits containing 11.58 wt.% and 13.16 wt.% TiO2 were produced, respectively. Multilayer coatings which consisted of Ni-TiO2 and TiO2-rich layers were deposited by pulse potential deposition through limiting the nickel deposition by diffusion control mechanism. The TiO2-rich layers thickness and accordingly, the content of TiO2 reinforcement reached 104 nm and 18.47 wt.%, respectively in the optimum condition. The phase structure and surface morphology of the nanocomposite coatings were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The cross sectional morphology and line scans of the layers were studied by field emission scanning electron microscopy (FESEM). It was confirmed that the preferred orientations and the crystallite sizes of nickel matrix were influenced by the deposition technique parameters, and higher contents of codeposited TiO2 nanoparticles refined the microstructure. The corrosion behavior of the coatings in 1M NaCl and 0.5M H2SO4 electrolytes were compared by means of potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. Increase of corrosion resistance and the passivation tendency were favored by TiO2 incorporation, while the degree of passivation declined as embedded particles disturbed the continuity of passive layer. The role of TiO2 incorporation on the improvement of mechanical properties including hardness, elasticity, scratch resistance and friction coefficient was investigated by the means of atomic force microscopy (AFM). Hydrophilicity and wettability of the composite coatings were investigated under UV illumination, and the water contact angle of the multilayer was reduced to 7.23° after 1 hour of UV irradiation.

Keywords: electrodeposition, hydrophilicity, multilayer, pulse-plating

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Authors: Swati Sundararajan, , Asit B. Samui, Prashant S. Kulkarni

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The global energy crisis has led to extensive research on alternative sources of energy. The gap between energy supply and demand can be met by thermal energy storage techniques, of which latent heat storage is most effective in the form of phase change materials (PCMs). Phase change materials utilize latent heat absorbed or released over a narrow temperature range of the material undergoing phase transformation, to store energy. The latent heat can be utilized for heating or cooling purposes. It can also be used for converting to electricity. All these actions amount to minimizing the load on electricity demand. These materials retain this property over repeated number of cycles. Different PCMs differ in the phase change temperature and the heat storage capacities. Poly(ethylene glycol) (PEG) was cross-linked to hydroxyl-terminated poly(dimethyl siloxane) (PDMS) in the presence of cross-linker, tetraethyl orthosilicate (TEOS) and catalyst, dibutyltin dilaurate. Four different ratios of PEG and PDMS were reacted together, and the composition with the lowest PEG concentration resulted in the formation of a flexible solid-solid phase change membrane. The other compositions are obtained in powder form. The enthalpy values of the prepared PCMs were studied by using differential scanning calorimetry and the crystallization properties were analyzed by using X-ray diffraction and polarized optical microscopy. The incorporation of silicone moiety was expected to reduce the hydrophilic character of PEG, which was evaluated by measurement of contact angle. The membrane forming ability of this crosslinked polymer can be extended to several smart packaging, building and textile applications. The detailed synthesis, characterization and performance evaluation of the crosslinked polymer blend will be incorporated in the presentation.

Keywords: phase change materials, poly(ethylene glycol), poly(dimethyl siloxane), thermal energy storage

Procedia PDF Downloads 354