Search results for: optimum block size

Authors: Preeti Makkar, R. C. Agarwala, Vijaya Agarwala

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The present study focuses on the preparation of Al2O3 nanoparticles by top down approach i.e. mechanical milling using high energy planetary ball mill at 250 rpm for 40h. The milled Al2O3 nanoparticles are then used as the second phase to develop electroless (EL) Ni-P- Al2O3 nanocomposite coatings on mild steel substrate. An alkaline bath was used with a suspension of Al2O3 particles (4 g/L) for the synthesis of Ni-P-Al2O3 nanocomposite coating. The surface morphology, size range and phase analysis of as-prepared Al2O3 particles and the coatings were characterized using X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The coatings were heat treated at 400°C for 1h in argon atmosphere and the hardness of the nanocomposite coatings was investigated with respect to Ni-P before and after heat treatment. The results showed that as milled Al2O3 nanoparticles exhibit irregular shaped and size ranges around 40-45 nm. The Al2O3 particles are uniformly distributed in Ni-P matrix. The microhardness of the coatings is found to be significantly improved after heat treatment (1126 VHN).

Keywords: Electroless (EL), Ni-P-Al2O3, nanocomposite, mechanical milling, microhardness

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Authors: Nasruddin Junus

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CFTR column is one of the improvements CFT columns by inserting reinforcing steel bars into infill concrete. The presence of inserting reinforcing steel bars is increasing the excellent structural performance of the CFT column, especially on the fire-resisting performance. Investigation on the mechanical behavior of CFTR column connection is summarized in the three parts; column to column joint, column to beam connection, and column base. Experiment that reported in this paper is concerned on the mechanical behavior of CFTR column joint under pull out testing, especially on its stress transfer mechanism. A number series of the pull out test on the CFT with inserting reinforcing steel bar are conducted. Ten test specimens are designed, constructed, and tested to examine experimentally the effect of the size of square steel tube, size of the bearing plate, length of embedment steel bars, kind of steel bars, and the numbers of rib plate.

Keywords: CFTR column, pull out, stress, transfer mechanism

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Authors: Aarti Agarwal, Ajmal Khan

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Background and Objective: Breathing difficulty is most distressing symptom for the patient and their caregivers providing palliative care to individuals with advanced malignancy. It needs to be tackled effectively and sometimes preemptively to provide relief from respiratory obstruction. Interventional procedures like tracheal stenting are becoming increasingly popular as a part of palliation for respiratory symptoms. We present a case of esophageal tumor earlier stented by Gastroenterologist to maintain esophageal patency, but the tumor outgrew to produce tracheal infiltration and thereby causing airway obstruction. Method and Result: 62-year-old man presented with unresectable Carcinoma oesophagus with inability to swallow. A metallic stent was placed by the gastroenterologist, to maintain esophageal patency and enable patient to swallow. Two months later, the patient returned to hospital in emergency with respiratory distress. CT neck and thorax revealed tumor infiltration through posterior tracheal wall. Lower extent of the tumor was till 1 cm above the carina. Airway stenting with Tracheo bronchial stent with Y configuration was planned under general anaesthesia with airway blocks. Superior Laryngeal Nerve Block, Glossopharyngeal block and Trans tracheal infiltration of local anaesthetics were performed. The patient was sedated with Fentanyl, Midazolam and propofol infusion but was breathing spontaneously. Once the rigid bronchoscope was placed inside trachea, breathing was supported with oxygen and sevoflurane. Initially, the trachea was cleared of tumor by coring. After creating space, tracheal stent was positioned and deployed. After stent placement patient was awakened, suctioned and nebulized. His respiratory stridor relieved instantaneously and was shifted to recovery. Conclusion: Airway blocks help in decreasing the incidence and severity of coughing during airway instrumentation thereby help in proper stent placement. They also reduce the requirement of general anaesthetics and hasten the post stenting recovery. Airway stent provided immediate relief to patient from symptoms of respiratory difficulty. Decision for early tracheal stenting may be taken for a select group of patients with high propensity for local spread, thereby avoiding respiratory complications and providing better quality of life in patients with inoperable malignancy.

Keywords: tracheal stent, respiratory difficulty, esophageal tumor, anaesthetic management

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Authors: Pimpak Phumat, Sakornrat Khongkhunthian, Thomas Rades, Anette Müllertz, Siriporn Okonogi

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Self-nanoemulsifying drug delivery systems (SNEDDS) containing 4-allylpyrocatechol (AP) extracted from Piper betle were developed to enhance water solubility of AP by using modeling and design (MODDE) program. The amount of AP in each SNEDDS formulation was determined by using high-performance liquid chromatography. The formulation consisted of 20% Miglyol®812N, 40 % Kolliphor®RH40, 30 % Maisine®35-1 and 10 % ethanol was found to be the best SNEDDS that provided the highest loading capacity of AP. (141.48±15.64 mg/g SNEDDS). The system also showed miscibility with water. The particle shape and size of the AP-SNEDDS after dispersing in water was investigated by using a transmission electron microscope and photon correlation spectrophotometer, respectively. The results showed that they were a spherical shape, having a particle size of 34.27 ± 1.14 nm with a narrow size distribution of 0.17 ± 0.04. The particles showed negative zeta potential with a value of -21.66 ± 2.09 mV. Antibacterial activity of AP-SNEDDS containing 1.5 mg/mL of AP was investigated against Streptococcus intermedius. The effect of this system on S. intermedius cells was observed by a scanning electron microscope (SEM). The results from SEM revealed that the bacterial cells were obviously destroyed. Killing kinetic study of AP-SNEDDS was carried out. It was found that the killing rate of AP-SNEDDS against S. intermedius was dose-dependent and the bacterial reduction was 79.86 ± 0.45 % within 30 min. In comparison with chlorhexidine (CHX), AP-SNEDDS showed similar antibacterial effects against S. intermedius. It is concluded that SNEDDS is a potential system for enhancing water solubility of AP. The antibacterial study reveals that AP-SNEDDS can be a promising system to treat bacterial infection caused by S. intermedius.

Keywords: SNEDDS, 4-allylpyrocathecol, solubility, antibacterial activity, Streptococcus intermedius

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Authors: Noor F. Ilias, Mazlifah Omar, Hashbullah Ismail

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Exercise training has been shown to improve functional capacity and is recommended as a therapy for management of blood pressure. Our purpose was to establish whether different exercise capacity produces different effect size for Cardiorespiratory Fitness (CRF), systolic (SBP) and diastolic (DBP) blood pressure in patients with hypertension. Exercise characteristic is required in order to have optimal benefit from the training, but optimal exercise capacity is still unwarranted. A MEDLINE search (1985 to 2015) was conducted for exercise based rehabilitation trials in hypertensive patients. Thirty-seven studies met the selection criteria. Of these, 31 (83.7%) were aerobic exercise and 6 (16.3%) aerobic with additional resistance exercise, providing a total of 1318 exercise subjects and 819 control, the total of subjects was 2137. We calculated exercise volume and energy expenditure through the description of exercise characteristics. 4 studies (18.2%) were 451kcal - 900 kcal, 12 (54.5%) were 900 kcal – 1350 kcal and 6 (27.3%) >1351kcal per week. Peak oxygen consumption (peak VO2) increased by mean difference of 1.44 ml/kg/min (95% confidence interval [CI]: 1.08 to 1.79 ml/kg/min; p = 0.00001) with weighted mean 21.2% for aerobic exercise compare to aerobic with additional resistance exercise 4.50 ml/kg/min (95% confidence interval [CI]: 3.57 to 5.42 ml/kg/min; p = 0.00001) with weighted mean 14.5%. SBP was clinically reduce for both aerobic and aerobic with resistance training by mean difference of -4.66 mmHg (95% confidence interval [CI]: -5.68 to -3.63 mmHg; p = 0.00001) weighted mean 6% reduction and -5.06 mmHg (95% confidence interval [CI]: -7.32 to -2.8 mmHg; p = 0.0001) weighted mean 5% reduction respectively. Result for DBP was clinically reduce for aerobic by mean difference of -1.62 mmHg (95% confidence interval [CI]: -2.09 to -1.15 mmHg; p = 0.00001) weighted mean 4% reduction and aerobic with resistance training reduce by mean difference of -3.26 mmHg (95% confidence interval [CI]: -4.87 to -1.65 mmHg; p = 0.0001) weighted mean 6% reduction. Optimum exercise capacity for 451 kcal – 900 kcal showed greater improvement in peak VO2 and SBP by 2.76 ml/kg/min (95% confidence interval [CI]: 1.47 to 4.05 ml/kg/min; p = 0.0001) with weighted mean 40.6% and -16.66 mmHg (95% confidence interval [CI]: -21.72 to -11.60 mmHg; p = 0.00001) weighted mean 9.8% respectively. Our data demonstrated that aerobic exercise with total volume of 451 kcal – 900 kcal/ week energy expenditure may elicit greater changes in cardiorespiratory fitness and blood pressure in hypertensive patients. Higher exercise capacity weekly does not seem better result in management hypertensive patients.

Keywords: blood Pressure, exercise, hypertension, peak VO2

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Authors: Fayad Ghawbar

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The significance of the Multiple Input Multiple Output (MIMO) system in the 5G wireless communication system is essential to enhance channel capacity and provide a high data rate resulting in a need for dual-polarization in vertical and horizontal. Furthermore, size reduction is critical in a MIMO system to deploy more antenna elements requiring a compact, low-profile design. A compact dual-band 4-MIMO antenna system has been presented in this paper with pattern and polarization diversity. The proposed single antenna structure has been designed using two antenna layers with a C shape in the front layer and a partial slot with a U-shaped cut in the ground to enhance isolation. The single antenna is printed on an FR4 dielectric substrate with an overall size of 18 mm×18 mm×1.6 mm. The 4-MIMO antenna elements were printed orthogonally on an FR4 substrate with a size dimension of 36 × 36 × 1.6 mm3 with zero edge-to-edge separation distance. The proposed compact 4-MIMO antenna elements resonate at 3.4-3.6 GHz and 4.8-5 GHz. The s-parameters measurement and simulation results agree, especially in the lower band with a slight frequency shift of the measurement results at the upper band due to fabrication imperfection. The proposed design shows isolation above -15 dB and -22 dB across the 4-MIMO elements. The MIMO diversity performance has been evaluated in terms of efficiency, ECC, DG, TARC, and CCL. The total and radiation efficiency were above 50 % across all parameters in both frequency bands. The ECC values were lower than 0.10, and the DG results were about 9.95 dB in all antenna elements. TARC results exhibited values lower than 0 dB with values lower than -25 dB in all MIMO elements at the dual-bands. Moreover, the channel capacity losses in the MIMO system were depicted using CCL with values lower than 0.4 Bits/s/Hz.

Keywords: compact antennas, MIMO antenna system, 5G communication, dual band, ECC, DG, TARC

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Authors: S. Siddharth, Saravana Kumar

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All Metros across the world tend to have a large number of bridges and there have been concerns about the safety of these bridges. As the traffic in most cities in India is heterogeneous, Trucks and Heavy vehicles traverse on our roads on an everyday basis this will lead to structural damage on the long run. All bridges are designed with a maximum Load limit and this limit is seldom checked. We have hence come up with an idea to check the load of all the vehicles entering the bridge and block the bridge with barricades if the vehicle surpasses the maximum load , this is done to catch hold of the perpetrators. By doing this we can avoid further structural damage and also provide an effective way to enforce the law. If our solution is put in place structural damage and accidents would be reduced to a great deal and it would also make the law enforcement job easier.

Keywords: heterogeneous, structural, load, law, heavy, vehicles

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Authors: Benbellil-Tafoughalt Saida, Tababouchet Meriem

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Sexual selection is the most supported explanation for genital extravagance occurring in animals. In promiscuous species, population density, as well as climate conditions, may act on the sperm competition intensity, one of the most important mechanism of post-copulatory sexual selection. The present study is empirical testing of sexual selection's potential role on genitalia variation in the simultanuously hermaphroditic land snail Helixaperta (Pulmonata, Stylommatophora). The purpose was to detect the patterns as well as the origin of the distal genitalia variability and especially to test the potential effect of sexual selection. The study was performed on four populations, H. aperta, different in habitat humidity regimes and presenting variable densities, which were mostly low. The organs of interest were those involved in spermatophore production, reception, and manipulation. We examined whether the evolution of those organs is connected to sperm competition intensity which is traduced by both population density and microclimate humidity. We also tested the hypothesis that those organs evolve in response to shell size. The results revealed remarkable differences in both snails’ size and organs lengths between populations. In most cases, the length of genitalia correlated positively to snails’ body size. Interestingly, snails from the more humid microclimate presented the highest mean weight and shell dimensions comparing to those from the less humid microclimate. However, we failed to establish any relation between snail densities and any of the measured genitalia traits.

Keywords: fertilization pouch, helix aperta, land snails, reproduction, sperm storage, spermatheca

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Authors: Phalaunnaphat Siriwongs

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The classroom of the 21st century is an ever-changing forum for new and innovative thoughts and ideas. With increasing technology and opportunity, students have rapid access to information that only decades ago would have taken weeks to obtain. Unfortunately, new techniques and technology are not a cure for the fundamental problems that have plagued the classroom ever since education was established. Class size has been an issue long debated in academia. While it is difficult to pinpoint an exact number, it is clear that in this case, more does not mean better. By looking into the success and pitfalls of classroom size, the true advantages of smaller classes becomes clear. Previously, one class was comprised of 50 students. Since they were seventeen- and eighteen-year-old students, it was sometimes quite difficult for them to stay focused. To help students understand and gain much knowledge, a researcher introduced “The Theory of Multiple Intelligence” and this, in fact, enabled students to learn according to their own learning preferences no matter how they were being taught. In this lesson, the researcher designed a cycle of learning activities involving all intelligences so that everyone had equal opportunities to learn.

Keywords: multiple intelligences, role play, performance assessment, formative assessment

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Authors: Endris Yibru Hanurry, Wei-Hsin Hsu, Hsieh-Chih Tsai

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In recent years, the discovery of small interfering RNAs (siRNAs) has got great attention for the treatment of cancer and other diseases. However, the therapeutic efficacy of siRNAs has been faced with many drawbacks because of short half-life in blood circulation, poor membrane penetration, weak endosomal escape and inadequate release into the cytosol. To overcome these drawbacks, we designed a non-viral vector by conjugating polyamidoamine generation 4.5 dendrimer (PDG4.5) with diethylenetriamine (DETA)- and tetraethylenepentamine (TEPA) followed by binding with siRNA to form polyplexes through electrostatic interaction. The result of 1H nuclear magnetic resonance (NMR), 13C NMR, correlation spectroscopy, heteronuclear single–quantum correlation spectroscopy, and Fourier transform infrared spectroscopy confirmed the successful conjugation of DETA and TEPA with PDG4.5. Then, the size, surface charge, morphology, binding ability, stability, release assay, toxicity and cellular internalization were analyzed to explore the physicochemical and biological properties of PDG4.5-DETA and PDG4.5-TEPA polyplexes at specific N/P ratios. The polyplexes (N/P = 8) exhibited spherical nanosized (125 and 85 nm) particles with optimum surface charge (13 and 26 mV), showed strong siRNA binding ability, protected the siRNA against enzyme digestion and accepted biocompatibility to the HeLa cells. Qualitatively, the fluorescence microscopy image revealed the delocalization (Manders’ coefficient 0.63 and 0.53 for PDG4.5-DETA and PDG4.5-TEPA, respectively) of polyplexes and the translocation of the siRNA throughout the cytosol to show a decent cellular internalization and intracellular biodistribution of polyplexes in HeLa cells. Quantitatively, the flow cytometry result indicated that a significant (P < 0.05) amount of siRNA was internalized by cells treated with PDG4.5-DETA (68.5%) and PDG4.5-TEPA (73%) polyplexes. Generally, PDG4.5-DETA and PDG4.5-TEPA were ideal nanocarriers of siRNA in vitro and might be used as promising candidates for in vivo study and future pharmaceutical applications.

Keywords: non-viral carrier, oligoalkylamine, poly(amidoamine) dendrimer, polyplexes, siRNA

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Authors: Edmund Gyimah

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Using data from 146 annual reports of listed firms in Ghana for the period 2013-2020, this study presents indicative findings which inspire practical actions and future research. Firms which prepared and presented sustainability reports were excluded from this study for a coverage of corporate sustainability disclosures centred on annual reports. Also, corporate sustainability disclosures of the firms on corporate websites were not included in the study considering the tendency of updates which cannot easily be traced. The corporate sustainability disclosures in the annual reports since the commencement of the G4 Guidelines in 2013 have been below average for all the dimensions of sustainability and the general sustainability disclosures. Few traditional elements of the board composition such as board size and board independence could affect the corporate sustainability disclosures in the annual reports as well as the age of the firm, firm size, and industry classification of the firm. Sustainability disclosures are greater in sustainability reports than in annual reports, however, firms without sustainability reports should have a considerable amount of sustainability disclosures in their annual reports. Also, because of the essence of sustainability, this study suggests to firms to have sustainability committee perhaps, they could make a difference in disclosing the enough sustainability information even when they do not present sustainability information in stand-alone reports.

Keywords: disclosures, sustainability, board, reports

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Authors: Maja Benkovic, Dubravka Novotni, Bojana Voucko, Duska Curic, Damir Jezek, Nikolina Cukelj

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Cryo-grinding is an ultra-fine grinding method used in the pharmaceutical industry, production of herbs and spices and in the production and handling of cereals, due to its ability to produce powders with small particle sizes which maintain their favorable bioactive profile. The aim of this study was to determine the particle size distributions of the proso millet (Panicum miliaceum) bran fraction grinded at cryogenic temperature (using liquid nitrogen (LN₂) cooling, T = - 196 °C), in comparison to non-cooled grinding. Proso millet bran is primarily used as an animal feed, but has a potential in food applications, either as a substrate for extraction of bioactive compounds or raw material in the bakery industry. For both applications finer particle sizes of the bran could be beneficial. Thus, millet bran was ground for 2, 4, 8 and 12 minutes using the ball mill (CryoMill, Retsch GmbH, Haan, Germany) at three grinding modes: (I) without cooling, (II) at cryo-temperature, and (III) at cryo-temperature with included 1 minute of intermediate cryo-cooling step after every 2 minutes of grinding, which is usually applied when samples require longer grinding times. The sample was placed in a 50 mL stainless steel jar containing one grinding ball (Ø 25 mm). The oscillation frequency in all three modes was 30 Hz. Particle size distributions of the bran were determined by a laser diffraction particle sizing method (Mastersizer 2000) using the Scirocco 2000 dry dispersion unit (Malvern Instruments, Malvern, UK). Three main effects of the grinding set-up were visible from the results. Firstly, grinding time at all three modes had a significant effect on all particle size parameters: d(0.1), d(0.5), d(0.9), D[3,2], D[4,3], span and specific surface area. Longer grinding times resulted in lower values of the above-listed parameters, e.g. the averaged d(0.5) of the sample (229.57±1.46 µm) dropped to 51.29±1.28 µm after 2 minutes grinding without LN₂, and additionally to 43.00±1.33 µm after 4 minutes of grinding without LN₂. The only exception was the sample ground for 12 minutes without cooling, where an increase in particle diameters occurred (d(0.5)=62.85±2.20 µm), probably due to particles adhering to one another and forming larger particle clusters. Secondly, samples with LN₂ cooling exhibited lower diameters in comparison to non-cooled. For example, after 8 minutes of non-cooled grinding d(0.5)=46.97±1.05 µm was achieved, while the LN₂ cooling enabled collection of particles with average sizes of d(0.5)=18.57±0.18 µm. Thirdly, the application of intermediate cryo-cooling step resulted in similar particle diameters (d(0.5)=15.83±0.36 µm, 12 min of grinding) as cryo-milling without this step (d(0.5)=16.33±2.09 µm, 12 min of grinding). This indicates that intermediate cooling is not necessary for the current application, which consequently reduces the consumption of LN₂. These results point out the potential beneficial effects of millet bran grinding at cryo-temperatures. Further research will show if the lower particle size achieved in comparison to non-cooled grinding could result in increased bioavailability of bioactive compounds, as well as protein digestibility and solubility of dietary fibers of the proso millet bran fraction.

Keywords: ball mill, cryo-milling, particle size distribution, proso millet (Panicum miliaceum) bran

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Authors: H. Barati, M. Wu, A. Kharicha, A. Ludwig

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A transient model for nozzle clogging has been developed and successfully validated against a laboratory experiment. Key steps of clogging are considered: transport of particles by turbulent flow towards the nozzle wall; interactions between fluid flow and nozzle wall, and the adhesion of the particle on the wall; the growth of the clog layer and its interaction with the flow. The current paper is to investigate the mesh (size and type) sensitivity of the model in both two and three dimensions. It is found that the algorithm for clog growth alone excluding the flow effect is insensitive to the mesh type and size, but the calculation including flow becomes sensitive to the mesh quality. The use of 2D meshes leads to overestimation of the clog growth because the 3D nature of flow in the boundary layer cannot be properly solved by 2D calculation. 3D simulation with tetrahedron mesh can also lead to an error estimation of the clog growth. A mesh-independent result can be achieved with hexahedral mesh, or at least with triangular prism (inflation layer) for near-wall regions.

Keywords: clogging, continuous casting, inclusion, simulation, submerged entry nozzle

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Authors: Nititorn Ounpipat

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The objective of this study was to find the relationship between internal communication and job satisfaction, and to find out the best communication channel to contact employees for a quality working within the operation or organizational rules. The sample size of 100% who were working as a shop floor level employee in the company. The study used the quantitative research method by distributing a structured questionnaire to collect data from 150 employees as the sample size. Inferential statistics and forward multiple regression analysis were used to analyze the results of this research. The result shows that communication channel correlated with job satisfaction. Each channel has a correlation with the satisfaction of working with the Department Board Information and All Employee / Weekly Meeting Relevance high. Since there is a correlation coefficient equal. 851 and. 840, respectively. Company Board Information, Memo, Letter, Leader, Supervisor, Friends and Email Relevance moderate as well.

Keywords: internal communication channels, job satisfaction, personal feedback, Rayong province

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Authors: Zehra Aybike Kılıç, Alpin Köknel Yener

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Daylight is a powerful driver in terms of improving human health, enhancing productivity and creating sustainable solutions by minimizing energy demand. A proper daylighting system allows not only a pleasant and attractive visual and thermal environment, but also reduces lighting energy consumption and heating/cooling energy load with the optimization of aperture size, glazing type and solar control strategy, which are the major design parameters of daylighting system design. Particularly, in high-rise buildings where large openings that allow maximum daylight and view out are preferred, evaluation of daylight performance by considering the major parameters of the building envelope design becomes crucial in terms of ensuring occupants’ comfort and improving energy efficiency. Moreover, it is increasingly necessary to examine the daylighting design of high-rise residential buildings, considering the share of residential buildings in the construction sector, the duration of occupation and the changing space requirements. This study aims to identify a proper daylighting design solution considering window area, glazing type and solar control strategy for a high-residential building in terms of visual comfort and lighting energy efficiency. The dynamic simulations are carried out/conducted by DIVA for Rhino version 4.1.0.12. The results are evaluated with Daylight Autonomy (DA) to demonstrate daylight availability in the space and Daylight Glare Probability (DGP) to describe the visual comfort conditions related to glare. Furthermore, it is also analyzed that the lighting energy consumption occurred in each scenario to determine the optimum solution reducing lighting energy consumption by optimizing daylight performance. The results revealed that it is only possible that reduction in lighting energy consumption as well as providing visual comfort conditions in buildings with the proper daylighting design decision regarding glazing type, transparency ratio and solar control device.

Keywords: daylighting , glazing type, lighting energy efficiency, residential building, solar control strategy, visual comfort

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Authors: A. Lovascio, A. D’Orazio, V. Centonze

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From several years till now the aerospace industry is developing more and more small satellites for Low-Earth Orbit (LEO) missions. Such satellites have a low cost of making and launching since they have a size and weight smaller than other types of satellites. However, because of size limitations, small satellites need integrated electronic equipment based on digital logic. Moreover, the LEOs require telecommunication modules with high throughput to transmit to earth a big amount of data in a short time. In order to meet such requirements, in this paper we propose a Telemetry, Tracking & Command module optimized through the use of the Commercial Off-The-Shelf components. The proposed approach exploits the major flexibility offered by these components in reducing costs and optimizing the performance. The method has been applied in detail for the design of the front-end receiver, which has a low noise figure (1.5 dB) and DC power consumption (smaller than 2 W). Such a performance is particularly attractive since it allows fulfilling the energy budget stringent constraints that are typical for LEO small platforms.

Keywords: COTS, LEO, small-satellite, TT&C

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Authors: S. Paszkiewicz, A. Zubkiewicz, A. Szymczyk, D. Pawlikowska, I. Irska, E. Piesowicz, A. Linares, T. A. Ezquerra

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Over the last century, the world has become increasingly dependent on oil as its main source of chemicals and energy. Driven largely by the strong economic growth of India and China, demand for oil is expected to increase significantly in the coming years. This growth in demand, combined with diminishing reserves, will require the development of new, sustainable sources for fuels and bulk chemicals. Biomass is an attractive alternative feedstock, as it is widely available carbon source apart from oil and coal. Nowadays, academic and industrial research in the field of polymer materials is strongly oriented towards bio-based alternatives to petroleum-derived plastics with enhanced properties for advanced applications. In this context, 2,5-furandicarboxylic acid (FDCA), a biomass-based chemical product derived from lignocellulose, is one of the most high-potential biobased building blocks for polymers and the first candidate to replace the petro-derived terephthalic acid. FDCA has been identified as one of the top 12 chemicals in the future, which may be used as a platform chemical for the synthesis of biomass-based polyester. The aim of this study is to synthesize and characterize the multiblock copolymers containing rigid segments of poly(trimethylene 2,5-furanoate) (PTF) and soft segments of poly(tetramethylene oxide) (PTMO) with excellent elastic properties or aliphatic polyesters of polycaprolactone (PCL). Two series of PTF based copolymers, i.e., PTF-block-PTMO-T and PTF-block-PCL-T, with different content of flexible segments were synthesized by means of a two-step melt polycondensation process and characterized by various methods. The rigid segments of PTF, as well as the flexible PTMO/or PCL ones, were randomly distributed along the chain. On the basis of 1H NMR, SAXS and WAXS, DSC an DMTA results, one can conclude that both phases were thermodynamically immiscible and the values of phase transition temperatures varied with the composition of the copolymer. The copolymers containing 25, 35 and 45wt.% of flexible segments (PTMO) exhibited elastomeric property characteristics. Moreover, with respect to the flexible segments content, the temperatures corresponding to 5%, 25%, 50% and 90% mass loss as well as the values of tensile modulus decrease with the increasing content of aliphatic polyether or aliphatic polyester in the composition.

Keywords: furan based polymers, multiblock copolymers, supramolecular structure, functional properties

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Authors: Ankit Patil, Tushar D. Deshpande, Yogesh M. Nimdeo

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Pickering emulsions (PE) were developed in response to increased demand for organic, eco-friendly, and biocompatible products. These emulsions are usually stabilized by solid particles. In this research, we created chitosan-based sunflower oil-in-water (O/W) PE without the need for a surfactant. In our work, we employed chitosan, a biopolymer derived from chitin, as a stabilizer. This decision was influenced by chitosan's biocompatibility and biodegradability, as well as its anti-inflammatory and antibacterial capabilities. It also has other functional properties, such as antioxidant activity, a probiotic delivery mechanism, and the ability to encapsulate bioactive compounds. The purpose of this study was to govern key parameters that can be changed to obtain stable PE, such as the concentration of chitosan (0.3-0.5 wt.%), the concentration of oil (0.8-1 vol%), the pH of the emulsion (3-7) manipulated by the addition of 1M HCl/ 4M NaOH, and the amount of electrolyte (NaCl-0-300mM) added to increase or decrease ionic strength. A careful combination of these properties resulted in the production of the most stable and optimal PE. Particle size study found that emulsions with pH 6, 0.4% chitosan, and 300 mM salts were exceptionally stable, with droplet size 886 nm, PI of 0.1702, and zeta potential of 32.753.83 mV. It is fair to infer that when ionic strength rises, particle size, zeta potential, and PI value decrease. A lower PI value suggests that emulsion nanoparticles are more homogeneous. The addition of sodium chloride increases the ionic strength of the emulsion, facilitating the formation of more compact and ordered particle layers. These findings provide light on the creation of stimulus-responsive chitosan-based PE capable of encapsulating bioactive materials, functioning as antioxidants, and serving as food-grade emulsifiers.

Keywords: pickering emulsion, biocompatibility, eco-friendly, chitosan

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Authors: Anna Cameron, Chunxia Zhao, Haofei Wang, Yun Liu, Guang Ze Yang

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Since the first publication in 1775, cancer research has built a comprehensive understanding of how cellular components of the tumor niche promote disease development. However, only within the last decade has research begun to establish the impact of non-cellular components of the niche, particularly the extracellular matrix (ECM). The ECM, a three-dimensional scaffold that sustains the tumor microenvironment, plays a crucial role in disease progression. Cancer cells actively deregulate and remodel the ECM to establish a tumor-promoting environment. Recent work has highlighted the need to further our understanding of the complexity of this cancer-ECM relationship. In vitro models use hydrogels to mimic the ECM, as hydrogel matrices offer biological compatibility and stability needed for long term cell culture. However, natural hydrogels are being used in these models verbatim, without tuning their biophysical characteristics to achieve pathophysiological relevance, thus limiting their broad use within cancer research. The biophysical attributes of these gels dictate cancer cell proliferation, invasion, metastasis, and therapeutic response. Evaluating the three most widely used natural hydrogels, Matrigel, collagen, and agarose gel, the permeability, stiffness, and pore-size of each gel were measured and compared to the in vivo environment. The pore size of all three gels fell between 0.5-6 µm, which coincides with the 0.1-5 µm in vivo pore size found in the literature. However, the stiffness for hydrogels able to support cell culture ranged between 0.05 and 0.3 kPa, which falls outside the range of 0.3-20,000 kPa reported in the literature for an in vivo ECM. Permeability was ~100x greater than in vivo measurements, due in large part to the lack of cellular components which impede permeation. Though, these measurements prove important when assessing therapeutic particle delivery, as the ECM permeability decreased with increasing particle size, with 100 nm particles exhibiting a fifth of the permeability of 10 nm particles. This work explores ways of adjusting the biophysical characteristics of hydrogels by changing protein concentration and the trade-off, which occurs due to the interdependence of these factors. The global aim of this work is to produce a more pathophysiologically relevant model for each tumor type.

Keywords: cancer, extracellular matrix, hydrogel, microfluidic

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Authors: Darren A. Whitaker, Dan Palmer, Jens Wesholowski, James Flaherty, John Mack, Ahmad B. Albadarin, Gavin Walker

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Traditional mechanosynthesis has been performed by either ball milling or manual grinding. However, neither of these techniques allow the easy application of process control. The temperature may change unpredictably due to friction in the process. Hence the amount of energy transferred to the reactants is intrinsically non-uniform. Recently, it has been shown that the use of Twin-Screw extrusion (TSE) can overcome these limitations. Additionally, TSE enables a platform for continuous synthesis or manufacturing as it is an open-ended process, with feedstocks at one end and product at the other. Several materials including metal-organic frameworks (MOFs), co-crystals and small organic molecules have been produced mechanochemically using TSE. The described advantages of TSE are offset by drawbacks such as increased process complexity (a large number of process parameters) and variation in feedstock flow impacting on product quality. To handle the above-mentioned drawbacks, this study utilizes UV-Vis spectrophotometry (InSpectroX, ColVisTec) as an online tool to gain real-time information about the quality of the product. Additionally, this is combined with real-time process information in an Advanced Process Control system (PharmaMV, Perceptive Engineering) allowing full supervision and control of the TSE process. Further, by characterizing the dynamic behavior of the TSE, a model predictive controller (MPC) can be employed to ensure the process remains under control when perturbed by external disturbances. Two reactions were studied; a Knoevenagel condensation reaction of barbituric acid and vanillin and, the direct amidation of hydroquinone by ammonium acetate to form N-Acetyl-para-aminophenol (APAP) commonly known as paracetamol. Both reactions could be carried out continuously using TSE, nuclear magnetic resonance (NMR) spectroscopy was used to confirm the percentage conversion of starting materials to product. This information was used to construct partial least squares (PLS) calibration models within the PharmaMV development system, which relates the percent conversion to product to the acquired UV-Vis spectrum. Once this was complete, the model was deployed within the PharmaMV Real-Time System to carry out automated optimization experiments to maximize the percentage conversion based on a set of process parameters in a design of experiments (DoE) style methodology. With the optimum set of process parameters established, a series of PRBS process response tests (i.e. Pseudo-Random Binary Sequences) around the optimum were conducted. The resultant dataset was used to build a statistical model and associated MPC. The controller maximizes product quality whilst ensuring the process remains at the optimum even as disturbances such as raw material variability are introduced into the system. To summarize, a combination of online spectral monitoring and advanced process control was used to develop a robust system for optimization and control of two TSE based mechanosynthetic processes.

Keywords: continuous synthesis, pharmaceutical, spectroscopy, advanced process control

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Authors: Junkal Gutierrez, Hernane S. Barud, Sidney J. L. Ribeiro, Agnieszka Tercjak

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Nowadays the interest on green nanocomposites and on the development of more environmental friendly products has been increased. Bacterial cellulose has been recently investigated as an attractive environmentally friendly material for the preparation of low-cost nanocomposites. The formation of cellulose by laboratory bacterial cultures is an interesting and attractive biomimetic access to obtain pure cellulose with excellent properties. Additionally, properties as molar mass, molar mass distribution, and the supramolecular structure could be control using different bacterial strain, culture mediums and conditions, including the incorporation of different additives. This kind of cellulose is a natural nanomaterial, and therefore, it has a high surface-to-volume ratio which is highly advantageous in composites production. Such property combined with good biocompatibility, high tensile strength, and high crystallinity makes bacterial cellulose a potential material for applications in different fields. The aim of this investigation work was the fabrication of novel hybrid inorganic-organic composites based on bacterial cellulose, cultivated in our laboratory, as a template. This kind of biohybrid nanocomposites gathers together excellent properties of bacterial cellulose with the ones displayed by typical inorganic nanoparticles like optical, magnetic and electrical properties, luminescence, ionic conductivity and selectivity, as well as chemical or biochemical activity. In addition, the functionalization of cellulose with inorganic materials opens new pathways for the fabrication of novel multifunctional hybrid materials with promising properties for a wide range of applications namely electronic paper, flexible displays, solar cells, sensors, among others. In this work, different pathways for fabrication of multifunctional biohybrid nanopapers with tunable properties based on BC modified with amphiphilic poly(ethylene oxide-b-propylene oxide-b-ethylene oxide) (EPE) block copolymer, sol-gel synthesized nanoparticles (titanium, vanadium and a mixture of both oxides) and functionalized iron oxide nanoparticles will be presented. In situ (biosynthesized) and ex situ (at post-production level) approaches were successfully used to modify BC membranes. Bacterial cellulose based biocomposites modified with different EPE block copolymer contents were developed by in situ technique. Thus, BC growth conditions were manipulated to fabricate EPE/BC nanocomposite during the biosynthesis. Additionally, hybrid inorganic/organic nanocomposites based on BC membranes and inorganic nanoparticles were designed via ex-situ method, by immersion of never-dried BC membranes into different nanoparticle solutions. On the one hand, sol-gel synthesized nanoparticles (titanium, vanadium and a mixture of both oxides) and on the other hand superparamagnetic iron oxide nanoparticles (SPION), Fe2O3-PEO solution. The morphology of designed novel bionanocomposites hybrid materials was investigated by atomic force microscopy (AFM) and scanning electron microscopy (SEM). In order to characterized obtained materials from the point of view of future applications different techniques were employed. On the one hand, optical properties were analyzed by UV-vis spectroscopy and spectrofluorimetry and on the other hand electrical properties were studied at nano and macroscale using electric force microscopy (EFM), tunneling atomic force microscopy (TUNA) and Keithley semiconductor analyzer, respectively. Magnetic properties were measured by means of magnetic force microscopy (MFM). Additionally, mechanical properties were also analyzed.

Keywords: bacterial cellulose, block copolymer, advanced characterization techniques, nanoparticles

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Authors: MD Mashiur Rahman, Muhammad Arshadul Haque

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Emerging conservation agriculture (CA) is an option for improving soil health and maintaining environmental sustainability for intensive agriculture, especially in the tropical climate. Three years lengthy research experiment was performed in arid climate from 2018 to 2020 at research field of Bangladesh Agricultural Research Station (RARS)F, Jamalpur (soil texture belongs to Agro-Ecological Zone (AEZ)-8/9, 24˚56'11''N latitude and 89˚55'54''E longitude and an altitude of 16.46m) to evaluate the effect of CA approaches on energy use efficiency and a streamlined life cycle greenhouse gas (GHG) emission of wheat production. For this, the conservation tillage practices (strip tillage (ST) and minimum tillage (MT)) were adopted in comparison to the conventional farmers' tillage (CT), with retained a fixed level (30 cm) of residue retention. This study examined the relationship between energy consumption and life cycle greenhouse gas (GHG) emission of wheat cultivation in Jamalpur region of Bangladesh. Standard energy equivalents megajoules (MJ) were used to measure energy from different inputs and output, similarly, the global warming potential values for the 100-year timescale and a standard unit kilogram of carbon dioxide equivalent (kg CO₂eq) was used to estimate direct and indirect GHG emissions from the use of on-farm and off-farm inputs. Farm efficiency analysis tool (FEAT) was used to analyze GHG emission and its intensity. A non-parametric data envelopment (DEA) analysis was used to estimate the optimum energy requirement of wheat production. The results showed that the treatment combination having MT with optimum energy inputs is the best suit for cost-effective, sustainable CA practice in wheat cultivation without compromising with the yield during the dry season. A total of 22045.86 MJ ha⁻¹, 22158.82 MJ ha⁻¹, and 23656.63 MJ ha⁻¹ input energy for the practice of ST, MT, and CT was used in wheat production, and output energy was calculated as 158657.40 MJ ha⁻¹, 162070.55 MJ ha⁻¹, and 149501.58 MJ ha⁻¹, respectively; where energy use efficiency/net energy ratio was found to be 7.20, 7.31 and 6.32. Among these, MT is the most effective practice option taken into account in the wheat production process. The optimum energy requirement was found to be 18236.71 MJ ha⁻¹ demonstrating for the practice of MT that if recommendations are followed, 18.7% of input energy can be saved. The total greenhouse gas (GHG) emission was calculated to be 2288 kgCO₂eq ha⁻¹, 2293 kgCO₂eq ha⁻¹ and 2331 kgCO₂eq ha⁻¹, where GHG intensity is the ratio of kg CO₂eq emission per MJ of output energy produced was estimated to be 0.014 kg CO₂/MJ, 0.014 kg CO₂/MJ and 0.015 kg CO₂/MJ in wheat production. Therefore, CA approaches ST practice with 30 cm residue retention was the most effective GHG mitigation option when the net life cycle GHG emission was considered in wheat production in the silt clay loam soil of Bangladesh. In conclusion, the CA approaches being implemented for wheat production involving MT practice have the potential to mitigate global warming potential in Bangladesh to achieve soil carbon footprint, where the life cycle assessment approach needs to be applied to a more diverse range of wheat-based cropping systems.

Keywords: conservation agriculture and tillage, energy use efficiency, life cycle GHG, Bangladesh

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Authors: Laura Kocsor, Laszlo Peter, Laszlo Kovacs, Zsolt Kis

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The aim of our research is to prepare rare-earth-doped lithium niobate (LiNbO3) nanocrystals, having only a few dopant ions in the focal point of an exciting laser beam. These samples will be used to achieve individual addressing of the dopant ions by light beams in a confocal microscope setup. One method for the preparation of nanocrystalline materials is to reduce the particle size by mechanical grinding. High-energy ball-milling was used in several works to produce nano lithium niobate. Previously, it was reported that dry high-energy ball-milling of lithium niobate in a shaker mill results in the partial reduction of the material, which leads to a balanced formation of bipolarons and polarons yielding gray color together with oxygen release and Li2O segregation on the open surfaces. In the present work we focus on preparing LiNbO3 nanocrystals by high-energy ball-milling using a Fritsch Pulverisette 7 planetary mill. Every ball-milling process was carried out in zirconia vial with zirconia balls of different sizes (from 3 mm to 0.1 mm), wet grinding with water, and the grinding time being less than an hour. Gradually decreasing the ball size to 0.1 mm, an average particle size of about 10 nm could be obtained determined by dynamic light scattering and verified by scanning electron microscopy. High-energy ball-milling resulted in sample darkening evidenced by optical absorption spectroscopy measurements indicating that the material underwent partial reduction. The unwanted lithium oxide loss decreases the Li/Nb ratio in the crystal, strongly influencing the spectroscopic properties of lithium niobate. Zirconia contamination was found in ground samples proved by energy-dispersive X-ray spectroscopy measurements; however, it cannot be explained based on the hardness properties of the materials involved in the ball-milling process. It can be understood taking into account the presence of lithium hydroxide formed the segregated lithium oxide and water during the ball-milling process, through chemically induced abrasion. The quantity of the segregated Li2O was measured by coulometric titration. During the wet milling process in the planetary mill, it was found that the lithium oxide loss increases linearly in the early phase of the milling process, then a saturation of the Li2O loss can be seen. This change goes along with the disappearance of the relatively large particles until a relatively narrow size distribution is achieved in accord with the dynamic light scattering measurements. With the 3 mm ball size and 1100 rpm rotation rate, the mean particle size achieved is 100 nm, and the total Li2O loss is about 1.2 wt.% of the original LiNbO3. Further investigations have been done to minimize the Li2O segregation during the ball-milling process. Since the Li2O loss was observed to increase with the growing total surface of the particles, the influence of ball-milling parameters on its quantity has also been studied.

Keywords: high-energy ball-milling, lithium niobate, mechanochemical reaction, nanocrystals

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Authors: Hicham Idriss

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Hydrogen production from water is one of the most promising methods to secure renewable sources or vectors of energy for societies in general and for chemical industries in particular. At present over 90% of the total amount of hydrogen produced in the world is made from non-renewable fossil fuels (via methane reforming). There are many methods for producing hydrogen from water and these include reducible oxide materials (solar thermal production), combined PV/electrolysis, artificial photosynthesis and photocatalysis. The most promising of these processes is the one relying on photocatalysis; yet serious challenges are hindering its success so far. In order to make this process viable considerable improvement of the photon conversion is needed. Among the key studies that our group has been conducting in the last few years are those focusing on synergism between the semiconductor phases, photonic band gap materials, pn junctions, plasmonic resonance responses, charge transfer to metal cations, in addition to metal dispersion and band gap engineering. In this work results related to phase transformation of the anatase to rutile in the case of TiO2 (synergism), of Au and Ag dispersion (electron trapping and hydrogen-hydrogen recombination centers) as well as their plasmon resonance response (visible light conversion) are presented and discussed. It is found for example that synergism between the two common phases of TiO2 (anatase and rutile) is sensitive to the initial particle size. It is also found, in agreement with previous results, that the rate is very sensitive to the amount of metals (with similar particle size) on the surface unlike the case of thermal heterogeneous catalysis.

Keywords: photo-catalysis, hydrogen production, water splitting, plasmonic

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Authors: Adnan I. O. Zaid

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As aluminum solidifies in columnar structure with large grain size which reduces its surface quality and mechanical strength; therefore it is normally grain refined either by titanium or titanium + boron (Ti or Ti + B). In this paper, the effect of addition of either Ti or Ti + B to commercially pure aluminum on its grain size, Vickers hardness, mechanical strength and fatigue strength and life is presented and discussed. Similarly, the effect of vanadium addition to Al grain refined by Ti or Ti+ B is presented and discussed. Two binary master alloys Al-Ti and Al-Vi were laboratory prepared from which five different micro-alloys in addition to the commercially pure aluminum namely Al-Ti, Al-Ti-B, Al-V, Al-Ti-V and Al-Ti-B-V were prepared for the investigation. Finally, the effect of their addition on the fatigue cracks initiation and propagation, using scanning electron microscope, SEM, is also presented and discussed. Photomirographs and photoscans are included in the paper.

Keywords: aluminum, fatigue, grain refinement, titanium, titanium+boron, vanadium

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Authors: Deeksha Arora

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The study aims to explore the applicability of the widely used asset pricing models, namely, Capital Asset Pricing Model (CAPM) and the Fama-French Four Factor Model in the Indian equity market. The study will be based on the companies that form part of the Nifty Fifty Index for a period of five years: 2011 to 2016. The asset pricing model is examined by forming portfolios on the basis of three variables – market capitalization (size effect), book-to-market equity ratio (value effect) and profitability. The study provides a basis to test the presence of the Fama-French Four factor model in Indian stock market. This study may provide a basis for future research in the generalized asset pricing model comprising of multiple risk factors.

Keywords: book to market equity, Fama French four factor model, market capitalization, profitability, size effect, value effect

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Authors: T. Pathinathan, M. Peter

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Fuzzy graphs incorporate concepts from graph theory with fuzzy principles. In this paper, we make a study on the properties of fuzzy graphs which are non-cyclic and are of two-dimensional in structure. In particular, this paper presents 2D structure or the structure of double layer for a non-cyclic fuzzy graph whose underlying crisp graph is non-cyclic. In any graph structure, introducing 2D structure may lead to an inherent cycle. We propose relevant conditions for 2D structured non-cyclic fuzzy graphs. These conditions are extended even to fuzzy graphs of the 3D structure. General theoretical properties that are studied for any fuzzy graph are verified to 2D structured or double layered fuzzy graphs. Concepts like Order, Degree, Strong and Size for a fuzzy graph are studied for 2D structured or double layered non-cyclic fuzzy graphs. Using different types of fuzzy graphs, the proposed concepts relating to 2D structured fuzzy graphs are verified.

Keywords: double layered fuzzy graph, double layered non–cyclic fuzzy graph, order, degree and size

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Authors: O. Anwar Beg, Armghan Zubair, Sireetorn Kuharat, Meisam Babaie

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In this work, motivated by rocket channel cooling applications, we describe recent CFD simulations of turbulent convective heat transfer in mini-channels at different aspect ratios. ANSYS FLUENT software has been employed with a mean average error of 5.97% relative to Forrest’s MIT cooling channel study (2014) at a Reynolds number of 50,443 with a Prandtl number of 3.01. This suggests that the simulation model created for turbulent flow was suitable to set as a foundation for the study of different aspect ratios in the channel. Multiple aspect ratios were also considered to understand the influence of high aspect ratios to analyse the best performing cooling channel, which was determined to be the highest aspect ratio channels. Hence, the approximate 28:1 aspect ratio provided the best characteristics to ensure effective cooling. A mesh convergence study was performed to assess the optimum mesh density to collect accurate results. Hence, for this study an element size of 0.05mm was used to generate 579,120 for proper turbulent flow simulation. Deploying a greater bias factor would increase the mesh density to the furthest edges of the channel which would prove to be useful if the focus of the study was just on a single side of the wall. Since a bulk temperature is involved with the calculations, it is essential to ensure a suitable bias factor is used to ensure the reliability of the results. Hence, in this study we have opted to use a bias factor of 5 to allow greater mesh density at both edges of the channel. However, the limitations on mesh density and hardware have curtailed the sophistication achievable for the turbulence characteristics. Also only linear rectangular channels were considered, i.e. curvature was ignored. Furthermore, we only considered conventional water coolant. From this CFD study the variation of aspect ratio provided a deeper appreciation of the effect of small to high aspect ratios with regard to cooling channels. Hence, when considering an application for the channel, the geometry of the aspect ratio must play a crucial role in optimizing cooling performance.

Keywords: rocket channel cooling, ANSYS FLUENT CFD, turbulence, convection heat transfer

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Authors: Ece A. Irmak, Amdulla O. Mekhrabov, M. Vedat Akdeniz

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There is a growing interest on the synthesis and characterization of nanoalloys since the unique chemical, and physical properties of nanoalloys can be tuned and, consequently, new structural motifs can be created by varying the type of constituent elements, atomic and magnetic ordering, as well as size and shape of the nanoparticles. Due to the fine size effects, magnetic nanoalloys have considerable attention with their enhanced mechanical, electrical, optical and magnetic behavior. As an important magnetic nanoalloy, the novel application area of Fe-Ni based nanoalloys is expected to be widened in the chemical, aerospace industry and magnetic biomedical applications. Noble metals have been using in biomedical applications for several years because of their surface plasmon properties. In this respect, iron-nickel nanoalloys are promising materials for magnetic biomedical applications because they show novel properties such as superparamagnetism and surface plasmon resonance property. Also, there is great attention for the usage Fe-Ni based nanoalloys as radar absorbing materials in aerospace and stealth industry due to having high Curie temperature, high permeability and high saturation magnetization with good thermal stability. In this study, FeNi₃ bimetallic nanoalloys were synthesized by mechanical alloying in a planetary high energy ball mill. In mechanical alloying, micron size powders are placed into the mill with milling media. The powders are repeatedly deformed, fractured and alloyed by high energy collision under the impact of balls until the desired composition and particle size is achieved. The experimental studies were carried out in two parts. Firstly, dry mechanical alloying with high energy dry planetary ball milling was applied to obtain FeNi₃ nanoparticles. Secondly, dry milling was followed by surfactant-assisted ball milling to observe the surfactant and solvent effect on the structure, size, and properties of the FeNi₃ nanoalloys. In the first part, the powder sample of iron-nickel was prepared according to the 1:3 iron to nickel ratio to produce FeNi₃ nanoparticles and the 1:10 powder to ball weight ratio. To avoid oxidation during milling, the vials had been filled with Ar inert gas before milling started. The powders were milled for 80 hours in total and the synthesis of the FeNi₃ intermetallic nanoparticles was succeeded by mechanical alloying in 40 hours. Also, regarding the particle size, it was found that the amount of nano-sized particles raised with increasing milling time. In the second part of the study, dry milling of the Fe and Ni powders with the same stoichiometric ratio was repeated. Then, to prevent agglomeration and to obtain smaller sized nanoparticles with superparamagnetic behavior, surfactants and solvent are added to the system, after 40-hour milling time, with the completion of the mechanical alloying. During surfactant-assisted ball milling, heptane was used as milling medium, and as surfactants, oleic acid and oleylamine were used in the high energy ball milling processes. The characterization of the alloyed particles in terms of microstructure, morphology, particle size, thermal and magnetic properties with respect to milling time was done by X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, vibrating-sample magnetometer, and differential scanning calorimetry.

Keywords: iron-nickel systems, magnetic nanoalloys, mechanical alloying, nanoalloy characterization, surfactant-assisted ball milling

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Authors: Jing-Yang Chung, Chi-Wei Liao, Jing Li, Bor Kae Chang, Cheng-Yu Wang

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Chemical hydride ammonia borane (AB, NH3BH3) draws attentions to hydrogen energy researches for its high theoretical gravimetrical capacity (19.6 wt%). Nevertheless, the elevated AB decomposition temperatures (Td) and unwanted byproducts are main hurdles in practical application. It was reported that the byproducts and Td can be reduced with nanoconfinement technique, in which AB molecules are confined in porous materials, such as porous carbon, zeolite, metal-organic frameworks (MOFs), etc. Although nanoconfinement empirically shows effectiveness on hydrogen generation temperature reduction in AB, the theoretical mechanism is debatable. Low Td was reported in AB@IRMOF-1 (Zn4O(BDC)3, BDC = benzenedicarboxylate), where Zn atoms form closed metal clusters secondary building unit (SBU) with no exposed active sites. Other than nanosized hydride, it was also observed that catalyst addition facilitates AB decomposition in the composite of Li-catalyzed carbon CMK-3, MOF JUC-32-Y with exposed Y3+, etc. It is believed that nanosized AB is critical for lowering Td, while active sites eliminate byproducts. Nonetheless, some researchers claimed that it is the catalytic sites that are the critical factor to reduce Td, instead of the hydride size. The group physically ground AB with ZIF-8 (zeolitic imidazolate frameworks, (Zn(2-methylimidazolate)2)), and found similar reduced Td phenomenon, even though AB molecules were not ‘confined’ or forming nanoparticles by physical hand grinding. It shows the catalytic reaction, not nanoconfinement, leads to AB dehydrogenation promotion. In this research, we explored the possible criteria of hydrogen production temperature from nanoconfined AB in MOFs with different pore sizes and active sites. MOFs with metal SBU such as Zn (IRMOF), Zr (UiO), and Al (MIL-53), accompanying with various organic ligands (BDC and BPDC; BPDC = biphenyldicarboxylate) were modified with AB. Excess MOFs were used for AB size constrained in micropores estimated by revisiting Horvath-Kawazoe model. AB dissolved in methanol was added to MOFs crystalline with MOF pore volume to AB ratio 4:1, and the slurry was dried under vacuum to collect AB@MOF powders. With TPD-MS (temperature programmed desorption with mass spectroscopy), we observed Td was reduced with smaller MOF pores. For example, it was reduced from 100°C to 64°C when MOF micropore ~1 nm, while ~90°C with pore size up to 5 nm. The behavior of Td as a function of AB crystalline radius obeys thermodynamics when the Gibbs free energy of AB decomposition is zero, and no obvious correlation with metal type was observed. In conclusion, we discovered Td of AB is proportional to the reciprocal of MOF pore size, possibly stronger than the effect of active sites.

Keywords: ammonia borane, chemical hydride, metal-organic framework, nanoconfinement

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