Search results for: different nighttime temperatures

Authors: Rachmat Mauludin, Novita R. Kusuma, Diky Mudhakir

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Famotidine (FMT) is one of used substances in the treatment of hiperacidity and peptic ulcer, administered orally and parenterally via intravenous injection. Oral administration, which is more favorable, has been reported to have many obstacles in the process of the treatment, includes decreasing the bioavailability of FMT. This research was aimed to prepare FMT in form of solid lipid nanoparticles (SLN) with size ranging between 100-200 nm. The research was carried out also by optimizing factors that may affect physical stability of SLN. Formulation of Famotidine SLN was carried out by optimizing factors, such as duration of homogenization and sonication, lipid concentration, stabilizer composition and stabilizer concentration. SLN physical stability was evaluated (particle size distribution) for 42 days in 3 diferent temperatures. Entrapment efficiency and drug loading was determined indirectly and directly. The morphology of SLN was visualized by transmission electron microscope (TEM). In vitro release study of FMT was conducted in 2 mediums, at pH of 1.2 and 7.4. Chemical stability of FMT was determined by quantifying the concentration of FMT within 42 days. Famotidin SLN consisted of GMS as lipid and poloxamer 188, lecithin, and polysorbate 80 as stabilizers. Homogenization and sonication was performed for 5 minutes and 10 minutes. Physyical stability of nanoparticles at 3 different temperatures was no significant difference. The best formula was physically stable until 42 days with mean particle size below 200 nm. Nanoparticles produced was able to entrap FMT until 86.6%. Evaluation by TEM showed that nanoparticles was spherical and solid. In medium pH of 1.2, FMT was released only 30% during 4 hour. On the other hand, within 4 hours SLN could release FMT completely in medium pH of 7.4. The FMT concentration in nanoparticles dispersion was maintained until 95% in 42 days (40oC, RH 75%). Famotidine SLN was able to be produced with mean particle size ranging between 100-200 nm and physically stable for 42 days. SLN could be loaded by 86,6% of FMT. Morphologically, obtained SLN was spheric and solid. During 4 hours in medium pH of 1.2 and 7.4, FMT was released until 30% and 100%, respectively.

Keywords: solid lipid nanoparticle (SLN), famotidine (FMT), physicochemical properties, release study

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Authors: Fazil Hasan, M. Shafiq Ansari, Mohammad Muslim

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Zygogramma bicolorata Pallister (Coleoptera: Chrysomelidae) is an exotic insect and effective biocontrol agent of Parthenium hysterophorus L. (Asteraceae). Our study aimed to determine the induction and termination of diapause, in response to abiotic (temperature and moisture) and biotic factors (age and reproductive status) and the effect of diapause on adult longevity and female fecundity. The adults burrowed into the soil about 1–6 cm below the surface for diapause at any time from July to December with a peak of 70% in the 2nd week of December at Aligarh region, India. The termination of diapause took place in May and June with the commencement of monsoon rains. Non-diapausing adults were also capable of breeding during winter under laboratory conditions. There was a significantly increased in the percentage of diapaused adults in subsequent generation i.e. 4% in F1 generation and 90% in F7 generation. The percentage of diapause was also significantly increased with age of adults. It has a positive effect on female fecundity as compared to the fecundity in pre-diapaused duration. Experiments proved that soil moisture played an important role in providing the conditions for initiation and termination of diapause. The adults which undergone diapause in January and February were continuously exposed to 35º, 40º and 45º C for one week and a daily dose of 10 and 8 hours for 6 and 5 days, respectively resulting in termination of diapause. This method may be used to initiate mass multiplication for carrying out releases early in the season. Exposure of adults to extremely low temperatures i.e. 5º and 10º C induced 94.3% and 92.5% diapause, respectively with no adult mortality. Therefore, low temperatures can also be used as a medium for the storage of mass reared beetles for a long time without having negative effect on their longevity and fecundity. Thus, our findings are of great utility in the biological suppression of P. hysterophorus as it will enhance the effectiveness of this beetle through manipulation of diapause.

Keywords: Zygogramma bicolorata, environmental factors, age, sex, diapause, Parthenium hysterophorus, biocontrol

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Authors: Himali N. Balasooriya, Kithsiri B. Dassanayake, Saman Seneweera, Said Ajlouni

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Increase in atmospheric CO₂ concentration [CO₂] and ambient temperature associated with changing climatic conditions will have significant impacts on agriculture crop productivity and quality. Independent effects of the above two environmental variables on the growth, yield and quality of strawberry were well documented. Higher temperatures over the optimum range (20-25ºC) lead to crop failures, while elevated [CO₂] stimulated plant growth and yield but compromised the physical quality of fruits. However, there is very limited understanding of the interaction between these variables on the plant growth, yield and quality. Therefore, this study was designed to investigate the interactive effect of high temperature and elevated [CO₂] on growth, yield and quality of strawberries. Strawberry cultivars ‘Albion’ and ‘San Andreas’ were grown under six different combinations of two temperatures (25 and 30ºC) and three [CO₂] (400, 650 and 950 µmol mol^-1) in controlled-environmental growth chambers. Plant growth measurements such as plant height, canopy area, number of flowers, and fruit yield were measured during phonological development. Photosynthesis and transpiration, the ratio of intercellular to atmospheric [CO₂] (Ci/Ca) were measured to estimate the physiological adjustment to climate stress. The impact of temperature and [CO₂] interaction on growth and yield of strawberry was significant (p < 0.05). Across both cultivars, highest fruit yields were observed at 650 µmol mol^-1 [CO₂], which was particularly clear at 25°C. The fruit yield gradually decreased at 30°C under all the treatment combinations. However, photosynthesis rates were highest at 650 µmol mol^-1 [CO₂] but no increment was found at 900 µmol mol^-1 [CO₂]. Interestingly, Ci/Ca ratio increased with increasing atmospheric [CO₂] which was predominant at high temperature. Similarly, fruit yield was substantially reduced at high [CO₂] under high temperature. Our findings suggest that increased Ci/Ca ratio at high temperature is likely reduces the photosynthesis and thus yield response to elevated [CO₂].

Keywords: atmospheric CO₂ concentration, fruit yield, strawberry, temperature

Procedia PDF Downloads 244

Authors: T. Srinivasa Krishna, K. Narendra, K. Thomas, S. S. Raju, B. Munibhadrayya

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The densities, speeds of sound and refractive index of the binary mixture of ionic liquid (IL) 1-Butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([BMIM][Imide]) and Pyrrolidin-2-one(PY) was measured at atmospheric pressure, and over the range of temperatures T= (298.15 -323.15)K. The excess molar volume, excess isentropic compressibility, excess speed of sound, partial molar volumes, and isentropic partial molar compressibility were calculated from the values of the experimental density and speed of sound. From the experimental data excess thermal expansion coefficients and isothermal pressure coefficient of excess molar enthalpy at 298.15K were calculated. The results were analyzed and were discussed from the point of view of structural changes. Excess properties were calculated and correlated by the Redlich–Kister and the Legendre polynomial equation and binary coefficients were obtained. Values of excess partial volumes at infinite dilution for the binary system at different temperatures were calculated from the adjustable parameters obtained from Legendre polynomial and Redlich–Kister smoothing equation. Deviation in refractive indices ΔnD and deviation in molar refraction, ΔRm were calculated from the measured refractive index values. Equations of state and several mixing rules were used to predict refractive indices of the binary mixtures and compared with the experimental values by means of the standard deviation and found to be in excellent agreement. By using Prigogine–Flory–Patterson (PFP) theory, the above thermodynamic mixing functions have been calculated and the results obtained from this theory were compared with experimental results.

Keywords: density, refractive index, speeds of sound, Prigogine-Flory-Patterson theory

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Authors: Surini Duthika Fernandopulle, Kalamba Arachchige Pramodya Wijesinghe

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Macrocapsules containing phase change material (PCM) PEG4000 as core and Calcium Alginate as the shell was synthesized by in-situ polymerization process, and their suitability for textile applications was studied. PCM macro-capsules were sandwiched between two polyurethane foams at regular intervals, and the sandwiched foams were subsequently covered with 100% cotton woven fabrics. According to the mathematical modelling and calculations 46 capsules were required to provide cooling for a period of 2 hours at 56ºC, so a panel of 10 cm x 10 cm area with 25 parts (having 5 capsules in each for 9 parts are 16 parts spaced for air permeability) were effectively merged into one textile material without changing the textile's original properties. First, the available cooling techniques related to textiles were considered and the best cooling techniques suiting the Sri Lankan climatic conditions were selected using a survey conducted for Sri Lankan Public based on ASHRAE-55-2010 standard and it consisted of 19 questions under 3 sections categorized as general information, thermal comfort sensation and requirement of Personal Cooling Garments (PCG). The results indicated that during daytime, majority of respondents feel warm and during nighttime also majority have responded as slightly warm. The survey also revealed that around 85% of the respondents are willing to accept a PCG. The developed panels were characterized using Fourier-transform infrared spectroscopy (FTIR) and Thermogravimetric Analysis (TGA) tests and the findings from FTIR showed that the macrocapsules consisted of PEG 4000 as the core material and Calcium Alginate as the shell material and findings from TGA showed that the capsules had the average weight percentage for core with 61,9% and shell with 34,7%. After heating both control samples and samples incorporating PCM panels, it was discovered that only the temperature of the control sample increased after 56ºC, whereas the temperature of the sample incorporating PCM panels began to regulate the temperature at 56ºC, preventing a temperature increase beyond 56ºC.

Keywords: phase change materials, thermal regulation, textiles, macrocapsules

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Authors: Martin Botz, Michael Kraus, Geralt Siebert

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The use of laminated glass gains increasing importance in structural engineering. For safety reasons, at least two glass panes are laminated together with a polymeric interlayer. In case of breakage of one or all of the glass panes, the glass fragments are still connected to the interlayer due to adhesion forces and a certain residual load-bearing capacity is left in the system. Polymer interlayers used in the laminated glass show a viscoelastic material behavior, e.g. stresses and strains in the interlayer are dependent on load duration and temperature. In the intact stage only small strains appear in the interlayer, thus the material can be described in a linear way. In the broken stage, large strains can appear and a non-linear viscoelasticity material theory is necessary. Relaxation tests on two different types of polymeric interlayers are performed at different temperatures and strain amplitudes to determine the border to the non-linear material regime. Based on the small-scale specimen results further tests on broken laminated glass panes are conducted. So-called ‘through-crack-bending’ (TCB) tests are performed, in which the laminated glass has a defined crack pattern. The test set-up is realized in a way that one glass layer is still able to transfer compressive stresses but tensile stresses have to be transferred by the interlayer solely. The TCB-tests are also conducted under different temperatures but constant force (creep test). Aims of these experiments are to elaborate if the results of small-scale tests on the interlayer are transferable to a laminated glass system in the broken stage. In this study, limits of the applicability of linear-viscoelasticity are established in the context of two commercially available polymer-interlayers. Furthermore, it is shown that the results of small-scale tests agree to a certain degree to the results of the TCB large-scale experiments. In a future step, the results can be used to develop material models for the post breakage performance of laminated glass.

Keywords: glass breakage, laminated glass, relaxation test, viscoelasticity

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Authors: Tatiana L. Avalos-Rendon, Elias A. Pasten Chelala, Carlos J. Mendoza EScobedo, Ignacio A. Figueroa, Victor H. Lara, Luis M. Palacios-Romero

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The cement industry is facing cost increments in energy supply, requirements for reduction of CO₂, and insufficient supply of raw materials of good quality. According to all these environmental issues, cement industry must change its consumption patterns and reduce CO₂ emissions to the atmosphere. This can be achieved by generating environmental consciousness, which encourages the use of industrial by-products and/or recycling for the production of cement, as well as alternate, environment-friendly methods of synthesis which reduce CO₂. Calcination is the conventional method for the obtainment of Portland cement clinker. This method consists of grinding and mixing of raw materials (limestone, clay, etc.) in an adequate dosage. Resulting mix has a clinkerization temperature of 1450 °C so that the formation of the main component occur: alite (Ca₃SiO₅, C₃S). Considering that the energy required to produce C₃S is 1810 kJ kg -1, calcination method for the obtainment of clinker represents two major disadvantages: long thermal treatment and elevated temperatures of synthesis, both of which cause high emissions of carbon dioxide (CO₂) to the atmosphere. Belite Portland clinker is characterized by having a low content of calcium oxide (CaO), causing the presence of alite to diminish and favoring the formation of belite (β-Ca₂SiO₄, C₂S), so production of clinker requires a reduced energy consumption (1350 kJ kg-1), releasing less CO₂ to the atmosphere. Conventionally, β-Ca₂SiO₄ is synthetized by the calcination of calcium carbonate (CaCO₃) and silicon dioxide (SiO₂) through the reaction in solid state at temperatures greater than 1300 °C. Resulting belite shows low hydraulic reactivity. Therefore, this study concerns a new simple modified combustion method for the synthesis of two belite cements at low temperatures (1000 °C). Silica fume, as subproduct of metallurgic industry and commercial natural zeolite were utilized as raw materials. These are considered low-cost materials and were utilized with no additional purification process. Belite cements properties were characterized by XRD, SEM, EDS and BET techniques. Hydration capacity of belite cements was calculated while the mechanical strength was determined in ordinary Portland cement specimens (PC) with a 10% partial replacement of the belite cements obtained. Results showed belite cements presented relatively high surface áreas, at early ages mechanical strengths similar to those of alite cement and comparable to strengths of belite cements obtained by different synthesis methods. Cements obtained in this work present good hydraulic reactivity properties.

Keywords: belite, silica fume, zeolite, hydraulic reactivity

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Authors: Jessica Morales Perdomo, Daniel Rodriguez Caicedo, Fernando Cantor Rincon

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Tuta absoluta known as the tomato leaf miner, is one of the main pests in tomato crops in South America and the main pest in many European countries. Apanteles gelechiidivoris is a parasitoid of third instar Tuta absoluta larvae. Our studies have demonstrated that this parasitoid can cause up to 80% mortality of T. absoluta larvae in the field. We investigated cold storage of A. gelechiidivoris pupae as a method of mass production of this parasitoid. This storage method does not interfere with biological characteristics of the parasitoid. In this study, we evaluated the effect of different temperatures (4, 8 and 12°C) and different time duration (7, 14, 21 or 28 days) of cold storage on biological parameters of A. gelechiidivoris pupae and adults. The biological parameters of the parasitoid evaluated were: adult emergence time, lifespan, parasitism percentage and sex ratio. We found that the adult emergence time was delayed when the parasitoid pupae were stored at 4°C and 8°C. The shortest adult emergence was recorded when pupae were stored for seven days. The lowest adult emergence was found for pupae stored at 4°C and decreased significantly as the days of storage increased. We found high percentages of adult emergence when pupae were stored at 8°C and 12°C for seven days. Adult lifespan decreased with increasing days of cold storage. Adults emerging from pupae stored at 8°C during seven and 14 days showed the longest lifespan (nine days). The lowest parasitism rate was recorded at 4°C at every time point. The highest percentage of parasitism (80%) was found at 8°C during seven days of storage. The treatments had no effect on adults the sex ratio. The results suggest that A. gelechiidivoris pupae can be stored for up to 14 days at 8°C without affecting the efficacy of the parasitoid in the field.

Keywords: biological control, cold storage, massive rearing, quality control

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Authors: Deginet Aklilu, Tianqi Wang, Endwoke Amsalu, Wei Feng, Zhiwei Li, Xia Li, Lixin Tao, Yanxia Luo, Moning Guo, Xiangtong Liu, Xiuhua Guo

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Extreme temperature-related cardiovascular diseases (CVDs) have become a growing public health concern. However, the impact of temperature on the cause of specific CVDs has not been well studied in the study area. The objective of this study was to assess the impact of temperature on cause-specific cardiovascular hospital admissions in Beijing, China. We obtained data from 172 large general hospitals from the Beijing Public Health Information Center Cardiovascular Case Database and China. Meteorological Administration covering 16 districts in Beijing from 2013 to 2017. We used a time-stratified case crossover design with a distributed lag nonlinear model (DLNM) to derive the impact of temperature on CVD in hospitals back to 27 days on CVD admissions. The temperature data were stratified as cold (extreme and moderate ) and hot (moderate and extreme ). Within five years (January 2013-December 2017), a total of 460,938 (male 54.9% and female 45.1%) CVD admission cases were reported. The exposure-response relationship for hospitalization was described by a "J" shape for the total and cause-specific. An increase in the six-day moving average temperature from moderate hot (30.2 °C) to extreme hot (36.9 °C) resulted in a significant increase in CVD admissions of 16.1%(95% CI = 12.8%-28.9%). However, the effect of cold temperature exposure on CVD admissions over a lag time of 0-27 days was found to be non significant, with a relative risk of 0.45 (95% CI = 0.378-0.55) for extreme cold (-8.5 °C)and 0.53 (95% CI = 0.47-0.60) for moderate cold (-5.6 °C). The results of this study indicate that exposure to extremely high temperatures is highly associated with an increase in cause-specific CVD admissions. These finding may guide to create and raise awareness of the general population, government and private sectors regarding on the effects of current weather conditions on CVD.

Keywords: admission, Beijing, cardiovascular diseases, distributed lag non linear model, temperature

Procedia PDF Downloads 67

Authors: L. Gyansah, Yanfang Shen, Jiqiang Wang, Tianying Xiong

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SiCₚ/ pure Al composites with different SiC fractions (20 wt %, 30 wt %, and 40 wt %) were precisely cold sprayed, followed by hot axial-compression tests at deformation temperatures of 473 K to 673 K, leading to failure of specimens through routine crack propagation in their multiphase. The plastic deformation behaviour with respect to the SiCₚ contents and the deformation temperatures were studied at strain rate 1s-1.As-sprayed and post-failure specimens were analyzed by X-ray computed tomography (XCT), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Quasi-static thermomechanical testing results revealed that compressive strength (UTS = 228 MPa and 30.4 %) was the highest in the composites that was thermomechanically compressed at 473 K compared to those of the as-sprayed, while the as-sprayed exhibited a compressive strength of 182.8 MPa related to the increment in SiC fraction. Strength—plasticity synergy was promoted by dynamic recrystallization (DRX) through strengthening and refinement of the grains. The DRX degree depends relevantly on retainment of the uniformly ultrafine SiCₚ particulates, the pinning effects of the interfaces promoted by the ultrafine grain structures (UFG), and the higher deformation temperature. Reconstructed X-ray computed tomography data revealed different crack propagation mechanisms. A single-plane shear crack with multi-laminates fracture morphology yields relatively through the as-sprayed and as-deformed at 473 K deposits, while a multiphase plane shear cracks preeminently existed in high temperature deformed deposits resulting in multiphase-interface delaminations. Three pertinent strengthening mechanisms, videlicet, SiCp dispersed strengthening, refined grain strengthening, and dislocation strengthening, existed in the gradient microstructure, and their detailed contributions to the thermomechanical properties were discussed.

Keywords: cold spraying, hot deformation, deformation temperature, thermomechancal properties, SiC/Al composite

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Authors: Helan Gethse J., Dhanya K., Muthuselvi G., Diana Hyden N., Samuel Pakianathan P.

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Transformer oil is mostly used to keep the transformer cool. It functions as a cooling agent. Mineral oil has long been used in transformers. Mineral oil has a high dielectric strength, which allows it to withstand high temperatures. Mineral oil's main disadvantage is that it is not environmentally friendly and can be dangerous to the environment. The features of breakdown voltage (BDV), viscosity, flash point, and fire point are measured and reported in this study, and the characteristics of olive oil are compared to the characteristics of mineral oil.

Keywords: antioxidants, transformer oil, mineral oil, olive oil

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Authors: Dmytro Zubov, Francesco Volponi

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In this paper, D-Wave quantum computing Ising model is used for the forecasting of positive extremes of daily mean air temperature. Forecast models are designed with two to five qubits, which represent 2-, 3-, 4-, and 5-day historical data respectively. Ising model’s real-valued weights and dimensionless coefficients are calculated using daily mean air temperatures from 119 places around the world, as well as sea level (Aburatsu, Japan). In comparison with current methods, this approach is better suited to predict heat wave values because it does not require the estimation of a probability distribution from scarce observations. Proposed forecast quantum computing algorithm is simulated based on traditional computer architecture and combinatorial optimization of Ising model parameters for the Ronald Reagan Washington National Airport dataset with 1-day lead-time on learning sample (1975-2010 yr). Analysis of the forecast accuracy (ratio of successful predictions to total number of predictions) on the validation sample (2011-2014 yr) shows that Ising model with three qubits has 100 % accuracy, which is quite significant as compared to other methods. However, number of identified heat waves is small (only one out of nineteen in this case). Other models with 2, 4, and 5 qubits have 20 %, 3.8 %, and 3.8 % accuracy respectively. Presented three-qubit forecast model is applied for prediction of heat waves at other five locations: Aurel Vlaicu, Romania – accuracy is 28.6 %; Bratislava, Slovakia – accuracy is 21.7 %; Brussels, Belgium – accuracy is 33.3 %; Sofia, Bulgaria – accuracy is 50 %; Akhisar, Turkey – accuracy is 21.4 %. These predictions are not ideal, but not zeros. They can be used independently or together with other predictions generated by different method(s). The loss of human life, as well as environmental, economic, and material damage, from extreme air temperatures could be reduced if some of heat waves are predicted. Even a small success rate implies a large socio-economic benefit.

Keywords: heat wave, D-wave, forecast, Ising model, quantum computing

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Authors: Risdiana, D. Suhendar, S. Pratiwi, W. A. Somantri, T. Saragi

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Superconductor is a promising material for future applications especially for energy saving because of their advantages properties such as zero electrical resistivity when they are cooled down to sufficiently low temperatures. However, the mechanism describing the role of physical properties in superconductor is far from being understood clearly, so that the application of this material for wider benefit in various industries is very limited. Most of superconductors are cuprate compounds, which has CuO2 as a conducting plane in their crystal structures. The study of physical properties through the partially substitution of impurity for Cu in superconducting cuprates has been one of great interests in relation to the mechanism of superconductivity. Different behaviors between the substitution of nonmagnetic impurity and magnetic impurity for Cu are observed. For examples, the superconductivity and Cu-spin fluctuations in the electron-doped system are suppressed through the substitution of magnetic Ni for Cu more markedly than through the substitution of nonmagnetic Zn for Cu, which is contrary to the result in the hole-doped system. Here, we reported the effect of partially substitution of magnetic impurity Fe for Cu to the magnetic and transport properties in electron-doped superconducting cuprates of Eu1.85+yCe0.15-yCu1-yFeyO4+α-δ (ECCFO) with y = 0.01, 0.02, and 0.05, in order to investigate the mechanism of magnetic and transport properties of ECCFO in normal-state. Magnetic properties are investigated by DC magnetic-susceptibility measurements that carried out at low temperatures down to 2 K using a standard SQUID magnetometer in a magnetic field of 5 Oe on field cooling. Transport properties addressed to electron mobility, are extracted from radius of electron localization calculated from temperature dependence of resistivity. For y = 0, temperature dependence of dc magnetic-susceptibility indicated the change of magnetic behavior from paramagnetic to diamagnetic below 15 K. Above 15 K, all samples show paramagnetic behavior with the values of magnetic moment in every volume unit increased with increasing y. Electron mobility decreased with increasing y. Some reasons for these results will be discussed.

Keywords: DC magnetic-susceptibility, electron mobility, Eu1.85+yCe0.15-yCu1-yFeyO4+α-δ, normal state

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Authors: Sahin Yakut, H. Kemal Ulutas, Deniz Deger

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Plasma Assisted Physical Vapor Deposition (PAPVD) method used to produce Poly(ethylene oxide) (pPEO) thin films. Depositions were progressed at various plasma discharge powers as 0, 2, 5 and 30 W for pPEO at 500nm film thicknesses. The capacitance and dielectric dissipation of the thin films were measured at 0,1-107 Hz frequency range and 173-353 K temperature range by an impedance analyzer. Then, alternative conductivity (σac) and activation energies were derived from capacitance and dielectric dissipation. σac of conventional PEO (PEO precursor) was measured to determine the effect of plasma discharge. Differences were observed between the alternative conductivity of PEO’s and pPEO’s depending on plasma discharge power. By this purpose, structural characterization techniques such as Differential Scanning Calorimetry (DSC) and Fourier Transform Infrared Spectroscopy (FT-IR) were applied on pPEO thin films. Structural analysis showed that density of crosslinking is plasma power dependent. The crosslinking density increases with increasing plasma discharge power and this increase is displayed as increasing dynamic glass transition temperatures at DSC results. Also, shifting of frequencies of some type of bond vibrations, belonging to bond vibrations produced after fragmentation because of plasma discharge, were observed at FTIR results. The dynamic glass transition temperatures obtained from alternative conductivity results for pPEO consistent with the results of DSC. Activation energies exhibit Arrhenius behavior. Activation energies decrease with increasing plasma discharge power. This behavior supports the suggestion expressing that long polymer chains and long oligomers are fragmented into smaller oligomers or radicals.

Keywords: activation energy, dielectric spectroscopy, organic thin films, plasma polymer

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Authors: Reshan Perera, Sarith Munasinghe, Himali Lakshika, Yasith Perera, Hasitha Walakadawattage, Udayanga Hemapala

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This research presents a reconfigurable architecture for residential microgrid systems utilizing Z-Source Inverter (ZSI) to optimize solar photovoltaic (SPV) system utilization and enhance grid resilience. The proposed system addresses challenges associated with high solar power penetration through various modes, including current control, voltage-frequency control, and reactive power control. It ensures uninterrupted power supply during grid faults, providing flexibility and reliability for grid-connected SPV customers. Challenges and opportunities in reactive power control for microgrids are explored, with simulation results and case studies validating proposed strategies. From a control and power perspective, the ZSI-based inverter enhances safety, reduces failures, and improves power quality compared to traditional inverters. Operating seamlessly in grid-connected and islanded modes guarantees continuous power supply during grid disturbances. Moreover, the research addresses power quality issues in long distribution feeders during off-peak and night-peak hours or fault conditions. Using the Distributed Static Synchronous Compensator (DSTATCOM) for voltage stability, the control objective is nighttime voltage regulation at the Point of Common Coupling (PCC). In this mode, disconnection of PV panels, batteries, and the battery controller allows the ZSI to operate in voltage-regulating mode, with critical loads remaining connected. The study introduces a structured controller for Reactive Power Controlling mode, contributing to a comprehensive and adaptable solution for residential microgrid systems. Mathematical modeling and simulations confirm successful maximum power extraction, controlled voltage, and smooth voltage-frequency regulation.

Keywords: reconfigurable architecture, solar photovoltaic, microgrids, z-source inverter, STATCOM, power quality, battery storage system

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Authors: Shihab Ibrahim

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Geopolymer binders as an alternative binder system to ordinary Portland cement are the focus of the past 2 decades of researches. In order to eliminate CO2 emission by cement manufacturing and utilizing construction waste as a source material, clean waste clay bricks which are the waste from Levent Brick factory was activated with a mixture of sodium hydroxide and sodium silicate solution. 12 molarity of sodium hydroxide solution was used and the ratio of sodium silicate to sodium hydroxide was 2.5. Alkaline solution to clay brick powder ratio of 0.35, 0.4, 0.45, and 0.5 was studied. Alkaline solution to powder ratio of 0.4 was found to be optimum ratio to have the same workability as ordinary Portland cement paste. Compressive strength of the clay brick based geopolymer paste samples was evaluated under different curing temperatures and curing durations. One day compressive strength of 57.3 MPa after curing at 85C for 24 hours was obtained which was higher than 7 days compressive strength of ordinary Portland cement paste. The highest compressive strength 71.4 MPa was achieved at seventh day age for the geopolymer paste samples cured at 85C for 24 hours. It was found that 8 hour curing at elevated temperature 85C, is sufficient to get 96% of total strength. 37.4 MPa strength at seventh day of clay brick based geopolymer sample cured at room temperature was achieved. Water absorption around 10% was found for clay brick based geopolymer samples cured at different temperatures with compare to 9.14% water absorption of ordinary Portland cement paste. The clay brick based geopolymer binder can have the potentiality to be used as an alternative binder to Portland cement in a case that the heat treatment provided. Further studies are needed in order to produce the binder in a way that can harden and gain strength without any elevated curing.

Keywords: construction and demolition waste, geopolymer, clay brick, compressive strength.

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Authors: Antonina Semakova, Karim Mynbaev, Nikolai Bazhenov, Anton Chernyaev, Sergei Kizhaev, Nikolai Stoyanov

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At present, heterostructures are used for fabrication of almost all types of optoelectronic devices. Our research focuses on the optoelectronic properties of InAs(Sb) solid solutions that are widely used in fabrication of light emitting diodes (LEDs) operating in middle wavelength infrared range (MWIR). This spectral range (2-6 μm) is relevant for laser diode spectroscopy of gases and molecules, for systems for the detection of explosive substances, medical applications, and for environmental monitoring. The fabrication of MWIR LEDs that operate efficiently at room temperature is mainly hindered by the predominance of non-radiative Auger recombination of charge carriers over the process of radiative recombination, which makes practical application of LEDs difficult. However, non-radiative recombination can be partly suppressed in quantum-well structures. In this regard, studies of such structures are quite topical. In this work, electroluminescence (EL) of LED heterostructures based on InAs(Sb) epitaxial films with the molar fraction of InSb ranging from 0 to 0.09 and multi quantum-well (MQW) structures was studied in the temperature range 4.2-300 K. The growth of the heterostructures was performed by metal-organic chemical vapour deposition on InAs substrates. On top of the active layer, a wide-bandgap InAsSb(Ga,P) barrier was formed. At low temperatures (4.2-100 K) stimulated emission was observed. As the temperature increased, the emission became spontaneous. The transition from stimulated emission to spontaneous one occurred at different temperatures for structures with different InSb contents in the active region. The temperature-dependent carrier lifetime, limited by radiative recombination and the most probable Auger processes (for the materials under consideration, CHHS and CHCC), were calculated within the framework of the Kane model. The effect of various recombination processes on the carrier lifetime was studied, and the dominant role of Auger processes was established. For MQW structures quantization energies for electrons, light and heavy holes were calculated. A characteristic feature of the experimental EL spectra of these structures was the presence of peaks with energy different from that of calculated optical transitions between the first quantization levels for electrons and heavy holes. The obtained results showed strong effect of the specific electronic structure of InAsSb on the energy and intensity of optical transitions in nanostructures based on this material. For the structure with MQWs in the active layer, a very weak temperature dependence of EL peak was observed at high temperatures (>150 K), which makes it attractive for fabricating temperature-resistant gas sensors operating in the middle-infrared range.

Keywords: Electroluminescence, InAsSb, light emitting diode, quantum wells

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Authors: Adriana Duarte, Sandra Sampaio, Catia Ferreira, Jaime I. N. R. Gomes

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With the fashion of faded worn garments the textile industry has moved from indigo and pigments to dyes that are fixed by cationization, with products that can be toxic, and that can show this effect after washing down the dye with friction and/or treating with enzymes in a subsequent operation. Increasingly they are treated with bleaches, such as hypochlorite and permanganate, both toxic substances. An alternative process is presented in this work for both garment and jet dyeing processes, without the use of pre-cationization and the alternative use of “particle-dyes”. These are hybrid products, made up by an inorganic particle and an organic dye. With standard soluble dyes, it is not possible to avoid diffusion into the inside of the fiber unless using previous cationization. Only in this way can diffusion be avoided keeping the centre of the fibres undyed so as to produce the faded effect by removing the surface dye and showing the white fiber beneath. With “particle-dyes”, previous cationization is avoided. By applying low temperatures, the dye does not diffuse completely into the inside of the fiber, since it is a particle and not a soluble dye, being then able to give the faded effect. Even though bleaching can be used it can also be avoided, by the use of friction and enzymes they can be used just as for other dyes. This fashion brought about new ways of applying reactive dyes by the use of previous cationization of cotton, lowering the salt, and temperatures that reactive dyes usually need for reacting and as a side effect the application of a more environmental process. However, cationization is a process that can be problematic in applying it outside garment dyeing, such as jet dyeing, being difficult to obtain level dyeings. It also should be applied by a pad-fix or Pad-batch process due to the low affinity of the pre-cationization products making it a more expensive process, and the risk of unlevelness in processes such as jet dyeing. Wit particle-dyes, since no pre-cationizartion is necessary, they can be applied in jet dyeing. The excess dye is fixed by a fixing agent, fixing the insoluble dye onto the surface of the fibers. By applying the fixing agent only one to 1-3 rinses in water at room temperature are necessary, saving water and improving the washfastness.

Keywords: denim, garment dyeing, worn look, eco-fashion

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Authors: Ioana Stanciu

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This article presents the study of the rheological behavior of oxidized and non-oxidized vegetable oils at high temperatures and increasing shear rates. The largest increases in the dynamic viscosity of oxidized oils, in relation to the values that characterize non-oxidized oils, are recorded for soybean oil, followed by corn oil. Oxidized olive and rapeseed oils do not register significant increases in dynamic viscosity compared to non-oxidized oils.

Keywords: oil, oxidized, viscosity, vegetable

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Authors: Morteza Khashehchi, Kamel Hooman

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Thermal effects on the dynamics and stability of the flow past a circular cylinder operating in the mixed convection regime is studied experimentally for Reynolds number (ReD) between 1000 and 4000, and different cylinder wall temperatures (Tw) between 25 and 75°C by means of Particle Image Velocimetry (PIV). The experiments were conducted in a horizontal wind tunnel with the heated cylinder placed horizontally. With such assumptions, the direction of the thermally induced buoyancy force acting on the fluid surrounding the heated cylinder would be perpendicular to the flow direction. In each experiment, to acquire 3000 PIV image pairs, the temperature and Reynolds number of the approach flow were held constant. By adjusting different temperatures in different Reynolds numbers, the corresponding Richardson number (RiD = Gr/Re^2) was varied between 0:0 (unheated) and 10, resulting in a change in the heat transfer process from forced convection to mixed convection. With increasing temperature of the wall cylinder, significant modifications of the wake flow pattern and wake vortex shedding process were clearly revealed. For cylinder at low wall temperature, the size of the wake and the vortex shedding process are found to be quite similar to those of an unheated cylinder. With high wall temperature, however, the high temperature gradient in the wake shear layer creates a type of vorticity with opposite sign to that of the shear layer vorticity. This temperature gradient vorticity weakens the strength of the shear layer vorticity, causing delay in reaching the recreation point. In addition to the wake characteristics, the shedding frequency for the heated cylinder is determined for all aforementioned cases. It is found that, as the cylinder wall is heated, the organization of the vortex shedding is altered and the relative position of the first detached vortices with respect to the second one is changed. This movement of the first detached vortex toward the second one increases the frequency of the shedding process. It is also found that the wake closure length decreases with increasing the Richardson number.

Keywords: heated cylinder, PIV, wake, Reynolds number

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Authors: Neha Thakur, Pravin S. More

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The interaction of CO, H2 and LPG with Cu-dosed SnO2 catalysts was studied by means of Fourier transform infrared spectroscopy (FTIR). With increasing Cu loading, pronounced and progressive red shifts of the C–O stretching frequency associated with molecular CO adsorbed on the Cu/SnO2 component were observed. This decrease in n(CO) correlates with enhancement of CO dissociation at higher temperatures on Cu promoted SnO2 catalysts under conditions, where clean Cu is almost ineffective. In the conclusion, the capability of our technique is discussed, and a technique for enhancing the sensitivity in our technique is proposed.

Keywords: FTIR, spectroscopic, dissociation, n(CO)

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Authors: Quentin C.P. Bourgogne, Vanessa Bouchart, Pierre Chevrier, Emmanuel Dattoli

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This study presents an experimental and theoretical work conducted on a PolyPhenylene Sulfide reinforced with 40%wt of short glass fibers (PPS GF40) and its matrix. Thermoplastics are widely used in the automotive industry to lightweight automotive parts. The replacement of metallic parts by thermoplastics is reaching under-the-hood parts, near the engine. In this area, the parts are subjected to high temperatures and are immersed in cooling liquid. This liquid is composed of water and glycol and can affect the mechanical properties of the composite. The aim of this work was thus to quantify the evolution of mechanical properties of the thermoplastic composite, as a function of temperature and liquid aging effects, in order to develop a reliable design of parts. An experimental campaign in the tensile mode was carried out at different temperatures and for various glycol proportions in the cooling liquid, for monotonic and cyclic loadings on a neat and a reinforced PPS. The results of these tests allowed to highlight some of the main physical phenomena occurring during these solicitations under tough hydro-thermal conditions. Indeed, the performed tests showed that temperature and liquid cooling aging can affect the mechanical behavior of the material in several ways. The more the cooling liquid contains water, the more the mechanical behavior is affected. It was observed that PPS showed a higher sensitivity to absorption than to chemical aggressiveness of the cooling liquid, explaining this dominant sensitivity. Two kinds of behaviors were noted: an elasto-plastic type under the glass transition temperature and a visco-pseudo-plastic one above it. It was also shown that viscosity is the leading phenomenon above the glass transition temperature for the PPS and could also be important under this temperature, mostly under cyclic conditions and when the stress rate is low. Finally, it was observed that soliciting this composite at high temperatures is decreasing the advantages of the presence of fibers. A new phenomenological model was then built to take into account these experimental observations. This new model allowed the prediction of the evolution of mechanical properties as a function of the loading environment, with a reduced number of parameters compared to precedent studies. It was also shown that the presented approach enables the description and the prediction of the mechanical response with very good accuracy (2% of average error at worst), over a wide range of hydrothermal conditions. A temperature-humidity equivalence principle was underlined for the PPS, allowing the consideration of aging effects within the proposed model. Then, a limit of improvement of the reachable accuracy was determinate for all models using this set of data by the application of an artificial intelligence-based model allowing a comparison between artificial intelligence-based models and phenomenological based ones.

Keywords: aging, analytical modeling, mechanical testing, polymer matrix composites, sequential model, thermomechanical

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Authors: Selim Kara, Ertan Arda, Fahrettin Dolastir, Önder Pekcan

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Biomaterials and thin film coatings play a fundamental role in medical, food and pharmaceutical industries. Carrageenan is a linear sulfated polysaccharide extracted from algae and seaweeds. To date, such biomaterials have been used in many smart drug delivery systems due to their biocompatibility and antimicrobial activity properties. Poly (N-isopropylacrylamide) (PNIPAm) gels and copolymers have also been used in medical applications. PNIPAm shows lower critical solution temperature (LCST) property at about 32-34 °C which is very close to the human body temperature. Below and above the LCST point, PNIPAm gels exhibit distinct phase transitions between swollen and collapsed states. A special class of gels are microgels which can react to environmental changes significantly faster than microgels due to their small sizes. Quartz crystal microbalance (QCM) measurement technique is one of the attractive techniques which has been used for monitoring the thin-film formation process. A sensitive QCM system was designed as to detect 0.1 Hz difference in resonance frequency and 10-7 change in energy dissipation values, which are the measures of the deposited mass and the film rigidity, respectively. PNIPAm microgels with the diameter around few hundred nanometers in water were produced via precipitation polymerization process. 5 MHz quartz crystals with functionalized gold surfaces were used for the deposition of the carrageenan molecules and microgels in the solutions which were slowly pumped through a flow cell. Interactions between charged carrageenan and microgel particles were monitored during the formation of the film layers, and the Sauerbrey masses of the deposited films were calculated. The critical phase transition temperatures around the LCST were detected during the heating and cooling cycles. It was shown that it is possible to monitor the interactions between PNIPAm microgels and biopolymer molecules, and it is also possible to specify the critical phase transition temperatures by using a QCM system.

Keywords: carrageenan, phase transitions, PNIPAm microgels, quartz crystal microbalance (QCM)

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Authors: Adedapo Jepson Olumide, Kurowska Ewa, K. Schoeneich, Ikpokonte A. Enoch

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In this paper, subsurface temperature measured from continuous temperature logs were used to determine the geothermal gradient of NigerDelta sedimentary basin. The measured temperatures were corrected to the true subsurface temperatures by applying the American Association of Petroleum Resources (AAPG) correction factor, borehole temperature correction factor with La Max’s correction factor and Zeta Utilities borehole correction factor. Geothermal gradient in this basin ranges from 1.20C to 7.560C/100m. Six geothermal anomalies centres were observed at depth in the southern parts of the Abakaliki anticlinorium around Onitsha, Ihiala, Umuaha area and named A1 to A6 while two more centre appeared at depth of 3500m and 4000m named A7 and A8 respectively. Anomaly A1 describes the southern end of the Abakaliki anticlinorium and extends southwards, anomaly A2 to A5 were found associated with a NW-SE structural alignment of the Calabar hinge line with structures describing the edge of the Niger Delta basin with the basement block of the Oban massif. Anomaly A6 locates in the south-eastern part of the basin offshore while A7 and A8 are located in the south western part of the basin offshore. At the average exploratory depth of 3500m, the geothermal gradient values for these anomalies A1, A2, A3, A4, A5, A6, A7, and A8 are 6.50C/100m, 1.750C/100m, 7.50C/100m, 1.250C/100m, 6.50C/100m, 5.50C/100m, 60C/100m, and 2.250C/100m respectively. Anomaly A8 area may yield higher thermal value at greater depth than 3500m. These results show that anomalies areas of A1, A3, A5, A6 and A7 are potentially prospective and explorable for geothermal energy using abandoned oil wells in the study area. Anomalies A1, A3.A5, A6 occur at areas where drilled boreholes were not exploitable for oil and gas but for the remaining areas where wells are so exploitable there appears no geothermal anomaly. Geothermal energy is environmentally friendly, clean and reversible.

Keywords: temperature logs, geothermal gradient anomalies, alternative energy, Niger delta basin

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Authors: B. J. Babalola, M. B. Shongwe

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Spark Plasma Sintering technique is a novel processing method that produces limited grain growth and highly dense variety of materials; alloys, superalloys, and carbides just to mention a few. However, initial particle size and spark plasma sintering parameters are factors which influence the grain growth and mechanical properties of sintered materials. Ni-Cr alloys are regarded as the most promising alloys for aerospace turbine blades, owing to the fact that they meet the basic requirements of desirable mechanical strength at high temperatures and good resistance to oxidation. The conventional method of producing this alloy often results in excessive grain growth and porosity levels that are detrimental to its mechanical properties. The effect of sintering temperature was evaluated on the microstructure and mechanical properties of the nanostructured Ni-17Cr alloy. Nickel and chromium powder were milled using high energy ball milling independently for 30 hours, milling speed of 400 revs/min and ball to powder ratio (BPR) of 10:1. The milled powders were mixed in the composition of Nickel having 83 wt % and chromium, 17 wt %. This was sintered at varied temperatures from 800°C, 900°C, 1000°C, 1100°C and 1200°C. The structural characteristics such as porosity, grain size, fracture surface and hardness were analyzed by scan electron microscopy and X-ray diffraction, Archimedes densitometry, micro-hardness tester. The corresponding results indicated an increase in the densification and hardness property of the alloy as the temperature increases. The residual porosity of the alloy reduces with respect to the sintering temperature and in contrast, the grain size was enhanced. The study of the mechanical properties, including hardness, densification shows that optimum properties were obtained for the sintering temperature of 1100°C. The advantages of high sinterability of Ni-17Cr alloy using milled powders and microstructural details were discussed.

Keywords: densification, grain growth, milling, nanostructured materials, sintering temperature

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Authors: T. Kuchukhidze, N. Jalagonia, Z. Phachulia, R. Chedia

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Ceramic obtained on the base of aluminum oxide has wide application range, because it has unique properties, for example, wear-resistance, dielectric characteristics, exploitation ability at high temperatures and in corrosive atmosphere. Low temperature synthesis of α-Al2O3 is energo-economical process and it is actual for developing technologies of corundum ceramics fabrication. In the present work possibilities of low temperature transformation of oxyhydroxides in α-Al2O3, during a presence of small amount of rare–earth elements compounds (also Th, Re), have been discussed. Aluminium unstable oxyhydroxides have been obtained by hydrolysis of aluminium isopropoxide, nitrates, sulphate, chloride in alkaline environment at 80-90ºC tempertures. β-Al(OH)3 has been received from aluminium powder by ultrasonic development. Drying of oxyhydroxide sol has been conducted with presence of various types seeds, which amount reaches 0,1-0,2% (mas). Neodymium, holmium, thorium, lanthanum, cerium, gadolinium, disprosium nitrates and rhenium carbonyls have been used as seeds and they have been added to the sol specimens in amount of 0.1-0.2% (mas) calculated on metals. Annealing of obtained gels is carried out at 70 – 1100ºC for 2 hrs. The same specimen transforms in α-Al2O3 at 1100ºC. At this temperature in case of presence of lanthanum and gadolinium transformation takes place by 70-85%. In case of presence of thorium stabilization of γ-and θ-phases takes place. It is established, that thorium causes inhibition of α-phase generation at 1100ºC, at the time in all other doped specimens α-phase is generated at lower temperatures (1000-1050ºC). During the work the following devices have been used: X-ray difractometer DRON-3M (Cu-Kα, Ni filter, 2º/min), High temperature vacuum furnace OXY-GON, electronic scanning microscopes Nikon ECLIPSE LV 150, NMM-800TRF, planetary mill Pulverisette 7 premium line, SHIMADZU Dynamic Ultra Micro Hardness Tester, DUH-211S, Analysette 12 Dyna sizer.

Keywords: α-Alumina, combustion, phase transformation, seeding

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Authors: Yasin Polat, Yılmaz Dağdemir, Mehmet Arı

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Samarium (III) oxide and Ytterbium (III) oxide doped Bismuth trioxide solid solutions, the nano ceramic (Bi2O3)1-x-y(Sm2O3)x(Yb2O3)y ternary system were obtained with x=5, 20 mol %, and y=5, 20 mol % dopant concentrations have been synthesized in air atmosphere with solid state reaction. Temperature dependent electrical conductivity of the samples have been investigated by 4-point probe technique by heating and cooling process. Doped-Bi2O3 materials of solid electrolyte systems are good oxygen anions O2-conductors which have collected much attention as potential solid ceramic electrolytes for solid oxide fuel cells (SOFCs) because of their relatively high oxygen ionic conductivity at lower temperatures.(Bi2O3)-based electrolytes have also wide other technological applications in devices with high economical interest such as oxygen sensors, ceramic membranes for oxygen separation, oxygen pumps, catalyzing of some heterogeneous reactions, partial oxidation of the hydrocarbons, and additive material in paints. In recent years, many experimental researches have mostly focused on improving of the Bi-based electrolytes which have high oxide ionic conductivity at low temperatures and better performance as alternatives to traditional stabilized zirconia has taken place. Generally, these systems are much better solid electrolytes than well-known stabilized zirconia, because some of the bismuth trioxide phases exhibit higher ion conductivity than other oxide ionic conductors. Crystal structure of the Nano ceramic (Bi2O3)1-x-y(Sm2O3)x(Yb2O3)y has been determined by X-Ray powder diffractions (XRD) measurements before and after electrical conductivity measurements of the samples. Surface and grain structure properties of the samples were determined by SEM analysis. The samples which synthesized in this study can be used in industrial applications such as electrolytes of the solid oxide fuel cells (SOFC).

Keywords: 4-point probe technique, bismuth trioxide, solid state reaction, solid oxide fuel cell

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Authors: K. A. Weidenmann, M. Grigo, B. Brylka, P. Elsner, T. Böhlke

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In order to reduce fuel consumption, the weight of automobiles has to be reduced. Fiber reinforced polymers offer the potential to reach this aim because of their high stiffness to weight ratio. Additionally, the use of fiber reinforced polymers in automotive applications has to allow for an economic large-scale production. In this regard, long fiber reinforced thermoplastics made by direct processing offer both mechanical performance and processability in injection moulding and compression moulding. The work presented in this contribution deals with long glass fiber reinforced polypropylene directly processed in compression moulding (D-LFT). For the use in automotive applications both the temperature and the time dependency of the materials properties have to be investigated to fulfill performance requirements during crash or the demands of service temperatures ranging from -40 °C to 80 °C. To consider both the influence of temperature and time, quasistatic tensile tests have been carried out at different temperatures. These tests have been complemented by high speed tensile tests at different strain rates. As expected, the increase in strain rate results in an increase of the elastic modulus which correlates to an increase of the stiffness with decreasing service temperature. The results are in good accordance with results determined by dynamic mechanical analysis within the range of 0.1 to 100 Hz. The experimental results from different testing methods were grouped and interpreted by using different time temperature shift approaches. In this regard, Williams-Landel-Ferry and Arrhenius approach based on kinetics have been used. As the theoretical shift factor follows an arctan function, an empirical approach was also taken into consideration. It could be shown that this approach describes best the time and temperature superposition for glass fiber reinforced polypropylene manufactured by D-LFT processing.

Keywords: composite, dynamic mechanical analysis, long fibre reinforced thermoplastics, mechanical properties, time temperature superposition

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Authors: Houssam Hijazi, Laurent Cantrel, Jean-François Paul

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Periodic DFT calculations were performed to study the chemistry of CsI particles and the possible release of volatile iodine from CsI surfaces for nuclear safety interest. The results show that water adsorbs at low temperature associatively on the (011) surface of CsI, while water desorbs at higher temperatures. On the other hand, removing iodine species from the surface requires oxidizing the surface one time for each removed iodide atom. The activation energy of removing I₂ from the surface in the presence of two OH is 1,2 eV.

Keywords: aerosols, CSI, reactivity, DFT, water adsorption

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Authors: Emma Castiglioni, Nigel Scrutton, Derren Heyes, Alistair Fielding

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By using light as trigger, it is possible to study many biological processes, such as the activity of genes, proteins, and other molecules, with precise spatiotemporal control. Caged compounds, where biologically active molecules are generated from an inert precursor upon laser photolysis, offer the potential to initiate such biological reactions with high temporal resolution. As light acts as the trigger for cleaving the protecting group, the ‘caging’ technique provides a number of advantages as it can be intracellular, rapid and controlled in a quantitative manner. We are developing caging strategies to study the catalytic cycle of a number of enzyme systems, such as nitric oxide synthase and ethanolamine ammonia lyase. These include the use of caged substrates, caged electrons and the possibility of caging the enzyme itself. In addition, we are developing a novel freeze-quench instrument to study these reactions, which combines rapid mixing and flashing capabilities. Reaction intermediates will be trapped at low temperatures and will be analysed by using electron paramagnetic resonance (EPR) spectroscopy to identify the involvement of any radical species during catalysis. EPR techniques typically require relatively long measurement times and very often, low temperatures to fully characterise these short-lived species. Therefore, common rapid mixing techniques, such as stopped-flow or quench-flow are not directly suitable. However, the combination of rapid freeze-quench (RFQ) followed by EPR analysis provides the ideal approach to kinetically trap and spectroscopically characterise these transient radical species. In a typical RFQ experiment, two reagent solutions are delivered to the mixer via two syringes driven by a pneumatic actuator or stepper motor. The new mixed solution is then sprayed into a cryogenic liquid or surface, and the frozen sample is then collected and packed into an EPR tube for analysis. The earliest RFQ instrument consisted of a hydraulic ram unit as a drive unit with direct spraying of the sample into a cryogenic liquid (nitrogen, isopentane or petroleum). Improvements to the RFQ technique have arisen from the design of new mixers in order to reduce both the volume and the mixing time. In addition, the cryogenic isopentane bath has been coupled to a filtering system or replaced by spraying the solution onto a surface that is frozen via thermal conductivity with a cryogenic liquid. In our work, we are developing a novel RFQ instrument which combines the freeze-quench technology with flashing capabilities to enable the studies of both thermally-activated and light-activated biological reactions. This instrument also uses a new rotating plate design based on magnetic couplings and removes the need for mechanical motorised rotation, which can otherwise be problematic at cryogenic temperatures.

Keywords: caged compounds, freeze-quench apparatus, photolysis, radicals

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