Search results for: iron doping
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 1218

Search results for: iron doping

738 Composite Electrodes Containing Ni-Fe-Cr as an Activatable Oxygen Evolution Catalyst

Authors: Olga A. Krysiak, Grzegorz Cichowicz, Wojciech Hyk, Michal Cyranski, Jan Augustynski

Abstract:

Metal oxides are known electrocatalyst in water oxidation reaction. Due to the fact that it is desirable for efficient oxygen evolution catalyst to contain numerous redox-active metal ions to guard four electron water oxidation reaction, mixed metal oxides exhibit enhanced catalytic activity towards oxygen evolution reaction compared to single metal oxide systems. On the surface of fluorine doped tin oxide coated glass slide (FTO) deposited (doctor blade technique) mixed metal oxide layer composed of nickel, iron, and chromium. Oxide coating was acquired by heat treatment of the aqueous precursors' solutions of the corresponding salts. As-prepared electrodes were photosensitive and acted as an efficient oxygen evolution catalyst. Our results showed that obtained by this method electrodes can be activated which leads to achieving of higher current densities. The recorded current and photocurrent associated with oxygen evolution process were at least two orders of magnitude higher in the presence of oxide layer compared to bare FTO electrode. The overpotential of the process is low (ca. 0,2 V). We have also checked the activity of the catalyst at different known photoanodes used in sun-driven water splitting. Herein, we demonstrate that we were able to achieve efficient oxygen evolution catalysts using relatively cheap precursor consisting of earth abundant metals and simple method of preparation.

Keywords: chromium, electrocatalysis, iron, metal oxides, nickel, oxygen evolution

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737 Structural and Morphological Study of Europium Doped ZnO

Authors: Abdelhak Nouri

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Europium doped zinc oxide nanocolumns (ZnO:Eu) were deposited on indium tin oxide (ITO) substrate from an aqueous solution of 10⁻³M Zn(NO₃)₂ and 0.5M KNO₃ with different concentration of europium ions. The deposition was performed in a classical three-electrode electrochemical cell. The structural, morphology and optical properties have been characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM). The XRD results show high quality of crystallite with preferential orientation along c-axis. SEM images speculate ZnO: Eu has nanocolumnar form with hexagonal shape. The diameter of nanocolumns is around 230 nm. Furthermore, it was found that tail of crystallite, roughness, and band gap energy is highly influenced with increasing Eu ions concentration. The average grain size is about 102 nm to 125 nm.

Keywords: deterioration lattice, doping, nanostructures, Eu:ZnO

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736 Preparation of Chromium Nanoparticles on Carbon Substrate from Tannery Waste Solution by Chemical Method Compared to Electrokinetic Process

Authors: Mahmoud A. Rabah, Said El Sheikh

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This work shows the preparation of chromium nanoparticles from tannery waste solution on glassy carbon by chemical method compared to electrokinetic process. The waste solution contains free and soluble fats, calcium, iron, magnesium and high sodium in addition to the chromium ions. Filtration helps removal of insoluble matters. Diethyl ether successfully extracted soluble fats. The method started by removing calcium as insoluble oxalate salts at hot conditions in a faint acidic medium. The filtrate contains iron, magnesium, chromium ions and sodium chloride in excess. Chromium was separated selectively as insoluble hydroxide sol-gel at pH 6.5, filtered and washed with distilled water. Part of the gel reacted with sulfuric acid to produce chromium sulfate solution having 15-25 g/L concentration. Electrokinetic deposition of chromium nanoparticles on a carbon cathode was carried out using platinum anode under different galvanostatic conditions. The chemical method involved impregnating the carbon specimens with chromium hydroxide gel followed by reduction using hydrazine hydrate or by thermal reduction using hydrogen gas at 1250°C. Chromium grain size was characterized by TEM, FT-IR and SEM. Properties of the Cr grains were correlated to the conditions of the preparation process. Electrodeposition was found to control chromium particles to be more identical in size and shape as compared to the chemical method.

Keywords: chromium, electrodeposition, nanoparticles, tannery waste solution

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735 Modification of Li-Rich Layered Li1.2Mn0.54Ni0.13Co0.13O2 Cathode Material

Authors: Liu Li, Kim Seng Lee, Li Lu

Abstract:

The high-energy-density Li-rich layered materials are promising cathode materials for the next-generation high-performance lithium-ion batteries. The relatively low rate capability is one of the major problems that limit their practical application. In this work, Li-rich layered Li1.2Mn0.54Ni0.13Co0.13O2 cathode material synthesized by coprecipitation method is further modified by F doping or surface treatment to enhance its cycling stability as well as rate capability.

Keywords: Li-ion battery, Li-rich layered cathode material, phase transformation, cycling stability, rate capacility

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734 Assessment of the Physical and Chemical Characteristics of Ugbogui River, Edo State, Nigeria

Authors: Iyagbaye O. Rich, Omoigberale O. Michael, Iyagbaye A. Louis

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The physical, chemical parameters and some trace contents of Ugbogui in Edo State, Nigeria were investigated from August 2015 to April 2016. Four stations were studied from upstream to downstream using standard methods. A total of thirty-three (33) physical and chemical characteristics and trace metal contents were examined; Air and water temperatures, depth, transparency, colour, turbidity, flow velocity, pH, total alkalinity, conductivity and dissolved solids etc. Other includes dissolved oxygen, oxygen saturation, biochemical oxygen demand, chloride, phosphate, sodium, nitrate, sulphate, potassium, calcium, magnesium, iron, lead, copper, zinc, nickel, cadmium, vanadium and chromium. Eleven (11) parameters exhibited clear seasonal variations. However, there were high significant differences (p < 0.01) in the values of depth, colour, total suspended solid, biochemical oxygen demand, chemical oxygen demand, chloride, bicarbonate, phosphate, sulphate, iron, manganese, zinc, copper, chromium and cadmium among the stations. The anthropogenic activities had negatively impacted at station 3 of the river, although most of the recorded values were still within permissible limits.

Keywords: anthropogenic activities, Nigeria, permissible limits, physical and chemical parameters, trace metal, water quality

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733 Elaboration and Investigation of the New Ecologically Clean Friction Composite Materials on the Basis of Nanoporous Raw Materials

Authors: Lia Gventsadze, Elguja Kutelia, David Gventsadze

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The purpose of the article is to show the possibility for the development of a new generation, eco-friendly (asbestos free) nano-porous friction materials on the basis of Georgian raw materials, along with the determination of technological parameters for their production, as well as the optimization of tribological properties and the investigation of structural aspects of wear peculiarities of elaborated materials using the scanning electron microscopy (SEM) and Auger electron spectroscopy (AES) methods. The study investigated the tribological properties of the polymer friction materials on the basis of the phenol-formaldehyde resin using the porous diatomite filler modified by silane with the aim to improve the thermal stability, while the composition was modified by iron phosphate, technical carbon and basalt fibre. As a result of testing the stable values of friction factor (0.3-0,45) were reached, both in dry and wet friction conditions, the friction working parameters (friction factor and wear stability) remained stable up to 500 OC temperatures, the wear stability of gray cast-iron disk increased 3-4 times, the soundless operation of materials without squeaking were achieved. Herewith it was proved that small amount of ingredients (5-6) are enough to compose the nano-porous friction materials. The study explains the mechanism of the action of nano-porous composition base brake lining materials and its tribological efficiency on the basis of the triple phase model of the tribo-pair.

Keywords: brake lining, friction coefficient, wear, nanoporous composite, phenolic resin

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732 First Earth Size

Authors: Ibrahim M. Metwally

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Have you ever thought that earth was not the same earth we live on? Was it bigger or smaller? Was it a great continent surrounded by huge ocean as Alfred Wegener (1912) claimed? Earth is the most amazing planet in our Milky Way galaxy and may be in the universe. It is the only deformed planet that has a variable orbit around the sun and the only planet that has water on its surface. How did earth deformation take place? What does cause earth to deform? What are the results of earth deformation? How does its orbit around the sun change? First earth size computation can be achieved only considering the quantum of iron and nickel rested into earth core. This paper introduces a new theory “Earth expansion Theory”. The principles of “Earth Expansion Theory” are leading to new approaches and concepts to interpret whole earth dynamics and its geological and environmental changes. This theory is not an attempt to unify the two divergent dominant theories of continental drift, plate tectonic theory and earth expansion theory. The new theory is unique since it has a mathematical derivation, explains all the change to and around earth in terms of geological and environmental changes, and answers all unanswered questions in other theories. This paper presents the basic of the introduced theory and discusses the mechanism of earth expansion and how it took place, the forces that made the expansion. The mechanisms of earth size change from its spherical shape with radius about 3447.6 km to an elliptic shape of major radius about 6378.1 km and minor radius of about 6356.8 km and how it took place, are introduced and discussed. This article also introduces, in a more realistic explanation the formation of oceans and seas, the preparation of river formation. It also addresses the role of iron in earth size enlargement process within the continuum mechanics framework.

Keywords: earth size, earth expansion, continuum mechanics, continental and ocean formation

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731 Consequential Effects of Coal Utilization on Urban Water Supply Sources – a Study of Ajali River in Enugu State Nigeria

Authors: Enebe Christian Chukwudi

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Water bodies around the world notably underground water, ground water, rivers, streams, and seas, face degradation of their water quality as a result of activities associated with coal utilization including coal mining, coal processing, coal burning, waste storage and thermal pollution from coal plants which tend to contaminate these water bodies. This contamination results from heavy metals, presence of sulphate and iron, dissolved solids, mercury and other toxins contained in coal ash, sludge, and coal waste. These wastes sometimes find their way to sources of urban water supply and contaminate them. A major problem encountered in the supply of potable water to Enugu municipality is the contamination of Ajali River, the source of water supply to Enugu municipal by coal waste. Hydro geochemical analysis of Ajali water samples indicate high sulphate and iron content, high total dissolved solids(TDS), low pH (acidity values) and significant hardness in addition to presence of heavy metals, mercury, and other toxins. This is indicative of the following remedial measures: I. Proper disposal of mine wastes at designated disposal sites that are suitably prepared. II. Proper water treatment and III. Reduction of coal related contaminants taking advantage of clean coal technology.

Keywords: effects, coal, utilization, water quality, sources, waste, contamination, treatment

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730 Sources of Water Supply and Water Quality for Local Consumption: The Case Study of Eco-Tourism Village, Suan Luang Sub- District Municipality, Ampawa District, Samut Songkram Province, Thailand

Authors: Paiboon Jeamponk, Tasanee Ponglaa, Patchapon Srisanguan

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The aim of this research paper was based on an examination of sources of water supply and water quality for local consumption, conducted at eco-tourism villages of Suan Luang Sub- District Municipality of Amphawa District, Samut Songkram Province. The study incorporated both questionnaire and field work of water testing as the research tool and method. The sample size of 288 households was based on the population of the district, whereas the selected sample water sources were from 60 households: 30 samples were ground water and another 30 were surface water. Degree of heavy metal contamination in the water including copper, iron, manganese, zinc, cadmium and lead was investigated utilizing the Atomic Absorption- Direct Aspiration method. The findings unveiled that 96.0 percent of household water consumption was based on water supply, while the rest on canal, river and rain water. The household behaviour of consumption revealed that 47.2 percent of people routinely consumed water without boiling or filtering prior to consumption. The investigation of water supply quality found that the degree of heavy metal contamination including metal, lead, iron, copper, manganese and cadmium met the standards of the Department of Health.

Keywords: sources of water supply, water quality, water supply, Thailand

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729 Increase in the Shelf Life Anchovy (Engraulis ringens) from Flaying then Bleeding in a Sodium Citrate Solution

Authors: Santos Maza, Enzo Aldoradin, Carlos Pariona, Eliud Arpi, Maria Rosales

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The objective of this study was to investigate the effect of flaying then bleeding anchovy (Engraulis ringens) immersed within a sodium citrate solution. Anchovy is a pelagic fish that readily deteriorates due to its high content of polyunsaturated fatty acids. As such, within the Peruvian food industry, the shelf life of frozen anchovy is explicitly 6 months, this short duration imparts a barrier to use for direct consumption human. Thus, almost all capture of anchovy by the fishing industry is eventually used in the production of fishmeal. We offer this an alternative to its typical production process in order to increase shelf life. In the present study, 100 kg of anchovies were captured and immediately mixed with ice on ship, maintaining a high quality sensory metric (e.g., with color blue in back) while still arriving for processing less than 2 h after capture. Anchovies with fat content of 3% were immediately flayed (i.e., reducing subcutaneous fat), beheaded, gutted and bled (i.e., removing hemoglobin) by immersion in water (Control) or in a solution of 2.5% sodium citrate (treatment), then subsequently frozen at -30 °C for 8 h in 2 kg batches. Subsequent glazing and storage at -25 °C for 14 months completed the experiments parameters. The peroxide value (PV), acidity (A), fatty acid profile (FAP), thiobarbituric acid reactive substances (TBARS), heme iron (HI), pH and sensory attributes of the samples were evaluated monthly. The results of the PV, TBARS, A, pH and sensory analyses displayed significant differences (p<0.05) between treatment and control sample; where the sodium citrate treated samples showed increased preservation features. Specifically, at the beginning of the study, flayed, beheaded, gutted and bled anchovies displayed low content of fat (1.5%) with moderate amount of PV, A and TBARS, and were not rejected by sensory analysis. HI values and FAP displayed varying behavior, however, results of HI did not reveal a decreasing trend. This result is indicative of the fact that levels of iron were maintained as HI and did not convert into no heme iron, which is known to be the primary catalyst of lipid oxidation in fish. According to the FAP results, the major quantity of fatty acid was of polyunsaturated fatty acid (PFA) followed by saturated fatty acid (SFA) and then monounsaturated fatty acid (MFA). According to sensory analysis, the shelf life of flayed, beheaded and gutted anchovy (control and treatment) was 14 months. This shelf life was reached at laboratory level because high quality anchovies were used and immediately flayed, beheaded, gutted, bled and frozen. Therefore, it is possible to maintain the shelf life of anchovies for a long time. Overall, this method displayed a large increase in shelf life relative to that commonly seen for anchovies in this industry. However, these results should be extrapolated at industrial scales to propose better processing conditions and improve the quality of anchovy for direct human consumption.

Keywords: citrate sodium solution, heme iron, polyunsaturated fatty acids, shelf life of frozen anchovy

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728 Diversification of Sweet Potato Blends and Utilization for Malnutrition and Poverty Alleviation

Authors: Ladele Ademola A., Nkiru T. Meludu, Olufunke Ezekiel, Olaoye Taye F., Okanlowan Oluwatoyin M.

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Value addition to agricultural produce is of possible potential in reducing poverty, improving food security and malnutrition, therefore the need to develop small and micro-enterprises of sweet potato production. The study was carried out in Nigeria to determine the acceptability of blends sweet potato (Ipomea batatas) and commodities yellow maize (Zea mays), millet (Pennisetum glaucum), soybean (Glycine max), bambara groundnut (Vigna subterranean), guinea corn (Sorghum vulgare), wheat (Triticum aestivum), and roselle (Hibiscus sabdariffa) through sensory evaluation. Sweet potato (Ipomea batatas) roots were processed using two methods. The first method involved the use of a fabricated gas powered cabinet dryer to dry sulphited chips and the second method was the use of traditional sun drying method without the addition of the chemical. The blends were also assessed in terms of functional, chemical and color properties. Most acceptable blends include BAW (80:20 of sweet potato/wheat), BBC (80:20 of sweet potato/guinea corn), AAB (60:40 of sweet potato/guinea corn), YTE (100% soybean), TYG (100% sweet potato), KTN (100% wheat flour), XGP (80:20 of sweet potato/soybean), XAX (60:40 of sweet potato/wheat), LSS (100% Roselle), CHK (100% Guinea corn), and ABC (60:40% of sweet potato/ yellow maize). In addition, chemical analysis carried out revealed that sweet potato has high percentage of vitamins A and C, potassium (K), manganese (Mn), calcium (Ca), magnesium (Mg) and iron (Fe) and fibre content. There is also an increase of vitamin A and Iron in the blended products.

Keywords: blends, diversification, sensory evaluation, sweet potato, utilization

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727 Determination of Nutritional Value and Steroidal Saponin of Fenugreek Genotypes

Authors: Anita Singh, Richa Naula, Manoj Raghav

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Nutrient rich and high-yielding varieties of fenugreek can be developed by using genotypes which are naturally high in nutrients. Gene banks harbour scanty germplasm collection of Trigonella spp. and a very little background information about its genetic diversity. The extent of genetic diversity in a specific breeding population depends upon the genotype included in it. The present investigation aims at the estimation of macronutrient (phosphorus by spectrophotometer and potassium by flame photometer), micronutrients, namely, iron, zinc, manganese, and copper from seeds of fenugreek genotypes using atomic absorption spectrophotometer, protein by Rapid N Cube Analyser and Steroidal Saponins. Twenty-eight genotypes of fenugreek along with two standard checks, namely, Pant Ragini and Pusa Early Bunching were collected from different parts of India, and nutrient contents of each genotype were determined at G. B. P. U. A. & T. Laboratory, Pantnagar. Highest potassium content was observed in PFG-35 (1207 mg/100g). PFG-37 and PFG-20 were richest in phosphorus, iron and manganese content among all the genotypes. The lowest zinc content was found in PFG-26 (1.19 mg/100g), while the maximum zinc content was found in PFG- 28 (4.43 mg/100g). The highest content of copper was found in PFG-26 (1.97 mg/100g). PFG-39 has the highest protein content (29.60 %). Significant differences were observed in the steroidal saponin among the genotypes. Saponin content ranged from 0.38 g/100g to 1.31 g/100g. Steroidal Saponins content was found the maximum in PFG-36 (1.31 g/100g) followed by PFG-17 (1.28 g/100g). Therefore, the genotypes which are rich in nutrient and oil content can be used for plant biofortification, dietary supplements, and herbal products.

Keywords: genotypes, macronutrients, micronutrient, protein, seeds

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726 Structural and Magnetic Properties of Undoped and Ni Doped CdZnS

Authors: Sabit Horoz, Ahmet Ekicibil, Omer Sahin, M. Akyol

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In this study, CdZnS and Ni-doped CdZnS quantum dots(QDs) were prepared by the wet-chemical method at room temperature using mercaptoethanol as a capping agent. The structural and magnetic properties of the CdZnS and CdZnS doped with different concentrations of Ni QDs were examined by XRD and magnetic susceptibility measurements, respectively. The average particles size of cubic QDs obtained by full-width half maxima (FWHM) analysis, increases with increasing doping concentrations. The investigation of the magnetic properties showed that the Ni-doped samples exhibit signs of ferromagnetism, on the other hand, un-doped CdZnS is diamagnetic.

Keywords: un-doped and Ni doped CdZnS Quantum Dots (QDs), co-precipitation method, structural and optical properties of QDs, diluted magnetic semiconductor materials (DMSMs)

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725 Highly Efficient Iron Oxide-Sulfonated Graphene Oxide Catalyst for Esterification and Trans-Esterification Reactions

Authors: Reena D. Souza, Tripti Vats, Prem F. Siril

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Esterification of free fatty acid (oleic acid) and transesterification of waste cooking oil (WCO) with ethanol over graphene oxide (GO), GO-Fe2O3, sulfonated GO (GO-SO3H), and Fe2O3/GO-SO3H catalysts were examined in the present study. Iron oxide supported graphene-based acid catalyst (Fe2O3/GO-SO3H) exhibited highest catalytic activity. GO was prepared by modified Hummer’s process. The GO-Fe2O3 nanocomposites were prepared by the addition of NaOH to a solution containing GO and FeCl3. Sulfonation was done using concentrated sulfuric acid. Transmissionelectron microscopy (TEM) and atomic force microscopy (AFM) imaging revealed the presence of Fe2O3 particles having size in the range of 50-200 nm. Crystal structure was analyzed by XRD and defect states of graphene were characterized using Raman spectroscopy. The effects of the reaction variables such as catalyst loading, ethanol to acid ratio, reaction time and temperature on the conversion of fatty acids were studied. The optimum conditions for the esterification process were molar ratio of alcohol to oleic acid at 12:1 with 5 wt% of Fe2O3/GO-SO3H at 1000C with a reaction time of 4h yielding 99% of ethyl oleate. This is because metal oxide supported solid acid catalysts have advantages of having both strong Brønsted as well as Lewis acid properties. The biodiesel obtained by transesterification of WCO was characterized by 1H NMR and Gas Chromatography techniques. XRD patterns of the recycled catalyst evidenced that the catalyst structure was unchanged up to the 5th cycle, which indicated the long life of the catalyst.

Keywords: Fe₂O₃/GO-SO₃H, Graphene Oxide, GO-Fe₂O₃, GO-SO₃H, WCO

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724 Monitoring the Pollution Status of the Goan Coast Using Genotoxicity Biomarkers in the Bivalve, Meretrix ovum

Authors: Avelyno D'Costa, S. K. Shyama, M. K. Praveen Kumar

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The coast of Goa, India receives constant anthropogenic stress through its major rivers which carry mining rejects of iron and manganese ores from upstream mining sites and petroleum hydrocarbons from shipping and harbor-related activities which put the aquatic fauna such as bivalves at risk. The present study reports the pollution status of the Goan coast by the above xenobiotics employing genotoxicity studies. This is further supplemented by the quantification of total petroleum hydrocarbons (TPHs) and various trace metals (iron, manganese, copper, cadmium, and lead) in gills of the estuarine clam, Meretrix ovum as well as from the surrounding water and sediment, over a two-year sampling period, from January 2013 to December 2014. Bivalves were collected from a probable unpolluted site at Palolem and a probable polluted site at Vasco, based upon the anthropogenic activities at these sites. Genotoxicity was assessed in the gill cells using the comet assay and micronucleus test. The quantity of TPHs and trace metals present in gill tissue, water and sediments were analyzed using spectrofluorometry and atomic absorption spectrophotometry (AAS), respectively. The statistical significance of data was analyzed employing Student’s t-test. The relationship between DNA damage and pollutant concentrations was evaluated using multiple regression analysis. Significant DNA damage was observed in the bivalves collected from Vasco which is a region of high industrial activity. Concentrations of TPHs and trace metals (iron, manganese, and cadmium) were also found to be significantly high in gills of the bivalves collected from Vasco compared to those collected from Palolem. Further, the concentrations of these pollutants were also found to be significantly high in the water and sediments at Vasco compared to that of Palolem. This may be due to the lack of industrial activity at Palolem. A high positive correlation was observed between the pollutant levels and DNA damage in the bivalves collected from Vasco suggesting the genotoxic nature of these pollutants. Further, M. ovum can be used as a bioindicator species for monitoring the level of pollution of the estuarine/coastal regions by TPHs and trace metals.

Keywords: comet assay, metals, micronucleus test, total petroleum Hydrocarbons

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723 Identification of Associated-Virulence Genes in Quinolone-Resistant Escherichia coli Strains Recovered from an Urban Wastewater Treatment Plant

Authors: Alouache Souhila, Messai Yamina, Torres Carmen, Bakour Rabah

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Objective: It has often been reported an association between antibiotic resistance and virulence. However, resistance to quinolones seems to be an exception, it tends instead to be associated with an attenuation of virulence, particularly in clinical strains. The purpose of this study was to evaluate the potential virulence of 28 quinolone-resistant E. coli strains recovered from water at the inflow (n=16) and outflow (n=12) of an urban wastewater treatment plant (WWTP). Methods: E. coli isolates were selected on Tergitol-7 agar supplemented with 2µg/ml of ciprofloxacin, they were screened by PCR for 11 virulence genes related to Extraintestinal pathogenic E. coli (ExPEC): papC, papG, afa/draBC, sfa/foc, kpsMTII, iutA, iroN, hlyF, ompT, iss and traT. The phylogenetic groups were determined by PCR and clonal relationship was evaluated by ERIC-PCR. Results: Genotyping by ERIC-PCR showed 7 and 12 DNA profiles among strains of wastewater (inflow) and treated water (outflow), respectively. Strains were assigned to the following phylogenetic groups: B2 (n = 1, 3.5%), D (n = 3, 10.7%), B1 (n = 10, 35.7%.) and A (n = 14, 50%). A total of 8 virulence-associated genes were detected, traT (n=19, 67.8%), iroN (n= 16, 57 .1%), hlyF (n=15, 53 .5%), ompT (n=15, 53 .5%), iss (n=14, 50%), iutA (n=9, 32.1%) , sfa/foc (n=7, 25%) and kpsMTII (n=2, 7.1%). Combination of virulence factors allowed to define 16 virulence profiles. The pathotype APEC was observed in 17.8% (D=1, B1=4) and human ExPEC in 7% (B2=1, D=1) of strains. Conclusion: The study showed that quinolone-resistant E. coli strains isolated from wastewater and treated water in WWTP harbored virulence genes with the presence of APEC and human ExPEC strains.

Keywords: E. coli, quinolone-resistance, virulence, WWTP

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722 Iron Catalyst for Decomposition of Methane: Influence of Al/Si Ratio Support

Authors: A. S. Al-Fatesh, A. A. Ibrahim, A. M. AlSharekh, F. S. Alqahtani, S. O. Kasim, A. H. Fakeeha

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Hydrogen is the expected future fuel since it produces energy without any pollution. It can be used as a fuel directly or through the fuel cell. It is also used in chemical and petrochemical industry as reducing agent or in hydrogenation processes. It is produced by different methods such as reforming of hydrocarbon, electrolytic method and methane decomposition. The objective of the present paper is to study the decomposition of methane reaction at 700°C and 800°C. The catalysts were prepared via impregnation method using 20%Fe and different proportions of combined alumina and silica support using the following ratios [100%, 90%, 80%, and 0% Al₂O₃/SiO₂]. The prepared catalysts were calcined and activated at 600 OC and 500 OC respectively. The reaction was carried out in fixed bed reactor at atmospheric pressure using 0.3g of catalyst and feed gas ratio of 1.5/1 CH₄/N₂ with a total flow rate 25 mL/min. Catalyst characterizations (TPR, TGA, BET, XRD, etc.) have been employed to study the behavior of catalysts before and after the reaction. Moreover, a brief description of the weight loss and the CH₄ conversions versus time on stream relating the different support ratios over 20%Fe/Al₂O₃/SiO₂ catalysts has been added as well. The results of TGA analysis provided higher weights losses for catalysts operated at 700°C than 800°C. For the 90% Al₂O₃/SiO₂, the activity decreases with the time on stream using 800°C reaction temperature from 73.9% initial CH₄ conversion to 46.3% for a period of 300min, whereas the activity for the same catalyst increases from 47.1% to 64.8% when 700°C reaction temperature is employed. Likewise, for 80% Al₂O₃/SiO₂ the trend of activity is similar to that of 90% Al₂O₃/SiO₂ but with a different rate of activity variation. It can be inferred from the activity results that the ratio of Al₂O₃ to SiO₂ is crucial and it is directly proportional with the activity. Whenever the Al/Si ratio decreases the activity declines. Indeed, the CH₄ conversion of 100% SiO₂ support was less than 5%.

Keywords: Al₂O₃, SiO₂, CH₄ decomposition, hydrogen, iron

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721 Iron Doping Enhanced Photocatalytic Nitrogen Fixation Performance of WO₃ with Three-Dimensionally Orderd Macroporous Structure

Authors: Xiaoling Ren, Guidong Yang

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Ammonia, as one of the largest-volume industrial chemicals, is mostly produced by century-old Haber-Bosch process with extreme conditionsand high-cost. Under the circumstance, researchersarededicated in finding new ways to replace the Haber-Bosch process. Photocatalytic nitrogen fixation is a promising sustainable, clear and green strategy for ammonia synthesis, butit is still a big challenge due to the high activation energy for nitrogen. It is essential to develop an efficient photocatalyst for making this approach industrial application. Constructing chemisorption active sites through defect engineering can be defined as an effective and reliable means to improve nitrogen activation by forming the extraordinary coordination environment and electronic structure. Besides, the construction of three-dimensionally orderdmacroporous (3DOM) structured photocatalyst is considered to be one of effectivestrategiesto improve the activity due to it canincrease the diffusion rate of reactants in the interior, which isbeneficial to the mass transfer process of nitrogen molecules in photocatalytic nitrogen reduction. Herein, Fe doped 3DOM WO₃(Fe-3DOM WO₃) without noble metal cocatalysts is synthesized by a polystyrene-template strategy, which is firstly used for photocatalytic nitrogen fixation. To elucidate the chemical nature of the dopant, the X-ray diffraction (XRD) analysiswas conducted. The pure 3DOM WO₃ has a monoclinic type crystal structure. And no additional peak is observed in Fe doped 3DOM WO₃, indicating that the incorporation of Fe atoms did not result in a secondary phase formation. In order to confirm the morphologies of Fe-3DOM WO₃and 3DOM WO₃, scanning electron microscopy (SEM) was employed. The synthesized Fe-3DOM WO₃and 3DOM WO₃ both exhibit a highly ordered three dimensional inverse opal structure with interconnected pores. From high-resolution TEM image of Fe-3DOM WO₃, the ordered lattice fringes with a spacing of 3.84 Å can be assigned to the (001) plane of WO₃, which is consistent with the XRD results. Finally, the photocatalytic nitrogen reduction performance of 3DOM WO₃ and Fe doped 3DOM WO₃with various Fe contents were examined. As a result, both Fe-3DOM WO₃ samples achieve higher ammonia production rate than that of pure 3DOM WO₃, indicating that the doped Fe plays a critical role in the photocatalytic nitrogen fixation performance. To verify the reaction process upon N2 reduction on the Fe-3DOM WO₃, in-situ diffuse reflectance infrared Fourier-transform spectroscopy was employed to monitor the intermediates. The in-situ DRIFTS spectra of Fe-3DOM WO₃ exhibit the increased signals with the irradiation time from 0–60min in the N2 atmosphere. The above results prove that nitrogen is gradually hydrogenated to produce ammonia over Fe-3DOM WO₃. Thiswork would enrich our knowledge in designing efficient photocatalystsfor photocatalytic nitrogen reduction.

Keywords: ammonia, photocatalytic, nitrogen fixation, Fe doped 3DOM WO₃

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720 Bioremediation Potentials of Some Indigenous Microorganisms Isolated from Auto Mechanic Workshops on Irrigation Water Used in Lokoja Kogi State of Nigeria

Authors: Emmanuel Ekpa, Adaji Andrew, Queen Opaluwa, Isreal Daraobong

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Three (3) indigenous bacteria species (Bacillus spp, Acinectobacter spp and Moraxella spp) previously isolated from contaminated soil of some auto mechanic workshops were used for bioremediation studies on some irrigation water used at Sarkin-noma Fadama farms located in Lokoja Kogi State, Nigeria. This was done in order to investigate their bioremediation potentials using a simple pour plate method. The physicochemical parameters and heavy metal analysis (using AAS iCE 3000) of the irrigation water were performed before and after inoculation of the isolated organisms. Nitrate and phosphate concentration were found to be 10.56mg/L and 12.63mg/L prior to inoculation while iron and zinc were 0.9569mg/L and 0.2245mg/L respectively. Other physicochemical parameters were also observed to be high prior to inoculation. After the bioremediation test (inoculation with the isolated organisms), a nitrate and phosphate content of 2.53mg/L and 2.61mg/L were recorded respectively, iron and zinc gave 0.1694mg/L and 0.0174mg/L concentrations while other physicochemical parameters measured were also found to be lower in their respective values. The implication of this present study is that a number of carefully isolated indigenous bacteria species are capable of reducing the amount of heavy metal concentrations in water. Also, non-metallic contaminants like nitrate and phosphate are susceptible to bioremediation in the presence of such efficient system.

Keywords: bioremediation, heavy metals, physicochemical parameters, Bacillus spp, Acinectobacter spp and Moraxella spp, AAS, spectrometer 3000

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719 The Effect of Mechanical Stress on the Magnetic Structure and Properties of Ferromagnetic Microwires in Glass Insulation

Authors: N. N. Orlova, A. S. Aronin, Yu. P. Kabanov, S. I. Bozhko, V. S. Gornakov

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We have investigated the change of the magnetic structure and the hysteresis properties of iron-based microwires after decreasing levels of internal mechanical stresses. The magnetic structure was investigated by the method of magneto-optical indicator film and the method of magnetic force microscopy. The hysteresis properties were studied by the vibrating sample magnetometer. The stresses were decreased by removing the glass coat and/or by low-temperature isothermal annealing. Previously, the authors carried out experimentally investigation of the magnetic structure of Fe-based microwire using these methods. According to the obtained results the domain structure of a microwire with a positive magnetostriction is composed of the inner cylindrical domains with the magnetization along the wire axis and the surface layer of the ring shape domains with the radial direction of magnetization. Surface ring domains with opposite magnetization direction (i.e., to the axis or from the axis) alternate with each other. For the first time the size of magnetic domains was determined experimentally. In this study it was found that in the iron-based microwires the value of the coercive force can be reduce more than twice by decreasing levels of internal mechanical stresses. Decrease of the internal stress value by the relaxation annealing influence on the magnetic structure. So in the as-prepared microwires observed local deviations of the magnetization of the magnetic core domains from the axis of the wire. After low-temperature annealing the local deviations of magnetization is not observed.

Keywords: amorphous microwire, magnetic structure, internal stress, hysteresis properties, ferromagnetic

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718 Nutritional Status of Morbidly Obese Patients Prior to Bariatric Surgery

Authors: Azadeh Mottaghi, Reyhaneh Yousefi, Saeed Safari

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Background: Bariatric surgery is widely proposed as the most effective approach to mitigate the growing pace of morbid obesity. As bariatric surgery candidates suffer from pre-existing nutritional deficiencies, it is of great importance to assess nutritional status of candidates before surgery in order to establish appropriate nutritional interventions. Objectives: The present study assessed and represented baseline data according to the nutritional status among candidates for bariatric surgery. Methods: A cross-sectional analysis of pre-surgery data was collected on 170 morbidly obese patients undergoing bariatric surgery between October 2017 and February 2018. Dietary intake data (evaluated through 147-item food frequency questionnaire), anthropometric measures and biochemical parameters were assessed. Results: Participants included 145 females (25 males) with average age of 37.3 ± 10.2 years, BMI of 45.7 ± 6.4 kg/m² and reported to have a total of 72.3 ± 22.2 kg excess body weight. The most common nutritional deficiencies referred to iron, ferritin, transferrin, albumin, vitamin B12, and vitamin D, the prevalence of which in the study population were as followed; 6.5, 6.5, 3, 2, 17.6 and 66%, respectively. Mean energy, protein, fat, and carbohydrate intake were 3887.3 ± 1748.32 kcal/day, 121.6 ± 57.1, 144.1 ± 83.05, and 552.4 ± 240.5 gr/day, respectively. The study population consumed lower levels of iron, calcium, folic acid, and vitamin B12 compared to the Dietary Reference Intake (DRI) recommendations (2, 26, 2.5, and 13%, respectively). Conclusion: According to the poor dietary quality of bariatric surgery candidates, leading to nutritional deficiencies pre-operatively, close monitoring and tailored supplementation pre- and post-bariatric surgery are required.

Keywords: bariatric surgery, food frequency questionnaire, obesity, nutritional status

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717 Resonant Tunnelling Diode Output Characteristics Dependence on Structural Parameters: Simulations Based on Non-Equilibrium Green Functions

Authors: Saif Alomari

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The paper aims at giving physical and mathematical descriptions of how the structural parameters of a resonant tunnelling diode (RTD) affect its output characteristics. Specifically, the value of the peak voltage, peak current, peak to valley current ratio (PVCR), and the difference between peak and valley voltages and currents ΔV and ΔI. A simulation-based approach using the Non-Equilibrium Green Function (NEGF) formalism based on the Silvaco ATLAS simulator is employed to conduct a series of designed experiments. These experiments show how the doping concentration in the emitter and collector layers, their thicknesses, and the width of the barriers and the quantum well influence the above-mentioned output characteristics. Each of these parameters was systematically changed while holding others fixed in each set of experiments. Factorial experiments are outside the scope of this work and will be investigated in future. The physics involved in the operation of the device is thoroughly explained and mathematical models based on curve fitting and underlaying physical principles are deduced. The models can be used to design devices with predictable output characteristics. These models were found absent in the literature that the author acanned. Results show that the doping concentration in each region has an effect on the value of the peak voltage. It is found that increasing the carrier concentration in the collector region shifts the peak to lower values, whereas increasing it in the emitter shifts the peak to higher values. In the collector’s case, the shift is either controlled by the built-in potential resulting from the concentration gradient or the conductivity enhancement in the collector. The shift to higher voltages is found to be also related to the location of the Fermi-level. The thicknesses of these layers play a role in the location of the peak as well. It was found that increasing the thickness of each region shifts the peak to higher values until a specific characteristic length, afterwards the peak becomes independent of the thickness. Finally, it is shown that the thickness of the barriers can be optimized for a particular well width to produce the highest PVCR or the highest ΔV and ΔI. The location of the peak voltage is important in optoelectronic applications of RTDs where the operating point of the device is usually the peak voltage point. Furthermore, the PVCR, ΔV, and ΔI are of great importance for building RTD-based oscillators as they affect the frequency response and output power of the oscillator.

Keywords: peak to valley ratio, peak voltage shift, resonant tunneling diodes, structural parameters

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716 Methyl Red Adsorption and Photodegradation on TiO₂ Modified Mesoporous Carbon Photocatalyst

Authors: Seyyed Ershad Moradi, Javad Khodaveisi, Atefeh Nasrollahpour

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In this study, the highly ordered mesoporous carbon molecular sieve with high surface area and pore volume have been synthesized and modified by TiO₂ doping. The titanium oxide modified mesoporous carbon (Ti-OMC) was characterized by scanning electron microscope (SEM), BET surface area, DRS also XRD analysis (low and wide angle). Degradation experiments were conducted in batch mode with the variables such as amount of contact time, initial solution concentration, and solution pH. The optimal conditions for the degradation of methyl red (MR) were 100 mg/L dye concentration, pH of 7, and 0.12 mg/L of TiO₂ modified mesoporous carbon photocatalyst dosage.

Keywords: mesoporous carbon, photodegradation, surface modification, titanium oxide

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715 Antioxidant and Antimicrobial Activities of Matricaria pubscens Extracts: A Wild Space of North African Pharmacopeia

Authors: Abdelouahab Dehimati, Fatiha Bedjou

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This study focused on the antioxidant and antimicrobial activity of four extracts from the plant Matricaria pubscens (Asteraceae) harvest in the region of Ghardaia, the northern Sahara of Algeria. The different extracts were analyzed for their content of phenolic compounds and their biological activities. The ethanol extract expresses a better extraction yield (44.22%). We have first performed the quantitative colorimetric methods for total polyphenols. Wherein the aqueous extract shows the highest total polyphenol content and total flavonoid (216.66±2.58 mg Eq GA/g and 111.04±0.49 mg Eq Q/g E, respectively) and ethanol extract 50% total tannins content (68.88±2.72 mg Eq AT/g E). The evaluation of the antioxidant activity of extracts of Matricaria pubscens by the arbitrary value IC50. The ethanol 50% extract is expressed strong activity with an IC50 14.19±1.25 mg/m against the DPPH radical and 11.66±0.53 mg/ml against the ABTS radical). In addition, the aqueous extract showed strong reducing power with an IC50 (48.61±1.14 mg/ml). However, the results obtained by the reducing power of phosphomolybdat the test are calculated by the iron maximum absorbance where ethanol extract 50% gives an absorbance of about 1.641 ± 0.01nm. Otherwise, methanol 70% and butanol 80% extracts gave a very large chelating effect of iron with an IC50 (38.38±0.01 μg/ml and 38.58±0.04 μg/ml respectively). By the method of disc Diffuson, the results of the antimicrobial activity are achieved butanolic extract 80% shows high activity towards MRSA (MIC: 3.51mg/ml; BMC>100 mg/ml). Their shares, the extracts were the most active for the antifungal test, the butanol 80% extract was the most active against A. niger (MIC: 12.5 mg/ml; FMC>100 mg/ml). These preliminary results could be used to justify the traditional use of this plant and their phenolic compounds could be exploited for therapeutic purposes, such as antioxidants and antimicrobial effects.

Keywords: Matricaria pubscens, phenolic compounds, antioxidant activity, antimicrobial activity, IC50, MIC

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714 The Synthesis, Structure and Catalytic Activity of Iron(II) Complex with New N2O2 Donor Schiff Base Ligand

Authors: Neslihan Beyazit, Sahin Bayraktar, Cahit Demetgul

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Transition metal ions have an important role in biochemistry and biomimetic systems and may provide the basis of models for active sites of biological targets. The presence of copper(II), iron(II) and zinc(II) is crucial in many biological processes. Tetradentate N2O2 donor Schiff base ligands are well known to form stable transition metal complexes and these complexes have also applications in clinical and analytical fields. In this study, we present salient structural features and the details of cathecholase activity of Fe(II) complex of a new Schiff Base ligand. A new asymmetrical N2O2 donor Schiff base ligand and its Fe(II) complex were synthesized by condensation of 4-nitro-1,2 phenylenediamine with 6-formyl-7-hydroxy-5-methoxy-2-methylbenzopyran-4-one and by using an appropriate Fe(II) salt, respectively. Schiff base ligand and its metal complex were characterized by using FT-IR, 1H NMR, 13C NMR, UV-Vis, elemental analysis and magnetic susceptibility. In order to determine the kinetics parameters of catechol oxidase-like activity of Schiff base Fe(II) complex, the oxidation of the 3,5-di-tert-butylcatechol (3,5-DTBC) was measured at 25°C by monitoring the increase of the absorption band at 390-400 nm of the product 3,5-di-tert-butylcatequinone (3,5-DTBQ). The compatibility of catalytic reaction with Michaelis-Menten kinetics also investigated by the method of initial rates by monitoring the growth of the 390–400 nm band of 3,5-DTBQ as a function of time. Kinetic studies showed that Fe(II) complex of the new N2O2 donor Schiff base ligand was capable of acting as a model compound for simulating the catecholase properties of type-3 copper proteins.

Keywords: catecholase activity, Michaelis-Menten kinetics, Schiff base, transition metals

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713 Antiulcer Potential of Heme Oxygenase-1 Inducers

Authors: Gaweł Magdalena, Lipkowska Anna, Olbert Magdalena, Frąckiewicz Ewelina, Librowski Tadeusz, Nowak Gabriel, Pilc Andrzej

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Heme oxygenase-1 (HO-1), also known as heat shock protein 32 (HSP32), has been shown to be implicated in cytoprotection in various organs. Its activation plays a significant role in acute and chronic inflammation, protecting cells from oxidative injury and apoptosis. This inducible isoform of HO catalyzes the first and rate-limiting step in heme degradation to produce equimolar quantities of biologically active products: carbon monoxide (CO), free iron and biliverdin. CO has been reported to possess anti-apoptotic properties. Moreover, it inhibits the production of proinflammatory cytokines and stimulates the synthesis of the anti-inflammatory interleukin-10 (IL-10), as well as promotes vasodilatation at sites of inflammation. The second product of catalytic HO-1 activity, free cytotoxic iron, is promptly sequestered into the iron storage protein ferritin, which lowers the pro-oxidant state of the cell. The third product, biliverdin, is subsequently converted by biliverdin reductase into the bile pigment bilirubin, the most potent endogenous antioxidant among the constituents of human serum, which modulates immune effector functions and suppresses inflammatory response. Furthermore, being one of the so-called stress proteins, HO-1 adaptively responds to different stressors, such as reactive oxygen species (ROS), inflammatory cytokines and heavy metals and thus protects cells against such conditions as ischemia, hemorrhagic shock, heat shock or hypoxia. It is suggested that pharmacologic modulation of HO-1 may represent an effective strategy for prevention of stress and drug-induced gastrointestinal toxicity. HO-1 is constitutively expressed in normal gastric, intestinal and colonic mucosa and up-regulated during inflammation. It has been proven that HO-1 up-regulated by hemin, heme and cobalt-protoporphyrin ameliorates experimental colitis. In addition, the up-regulation of HO-1 partially explains the mechanism of action of 5-aminosalicylic acid (5-ASA), which is used clinically as an anti-colitis agent. In 2009 Ueda et al. has reported for the first time that mucosal protection by Polaprezinc, a chelate compound of zinc and L-carnosine used as an anti-ulcer drug in Japan, is also attributed to induction of HO-1 in the stomach. Since then, inducers of HO-1 are desired subject of research, as they may constitute therapeutically effective anti-ulcer drugs.

Keywords: heme oxygenase-1, gastric lesions, gastroprotection, Polaprezinc

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712 Polar Nanoregions in Lead-Free Relaxor Ceramics: Unveiling through Impedance Spectroscopy

Authors: Mohammed Mesrar, Hamza El Malki, Hamza Mesrar

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In this study, ceramics of (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3 were synthesized through a conventional calcination process (solid-state method) at 1000°C for 4 hours, with x(%) values ranging from 0.0 to 100. Room temperature XRD patterns confirmed the phase formation of the samples. The Rietveld refinement method was employed to verify the morphotropic phase boundary (MPB) at x(%)=16-20. We investigated the average crystallite size and lattice strain using Scherrer's formula and Williamson-Hall (W-H) analysis. SEM image analyses provided additional evidence of the impact of doping on structural growth under low temperatures. Relaxation time extracted from Z″(f) and M″(f) spectra for x(%) = 0.0, 12, 16, 20, and 30 followed the Arrhenius law, revealing the presence of three distinct relaxation mechanisms with varying activation energies. The shoulder response in M″(f) indirectly indicated the existence of highly polarizable entities in the samples, serving as a signature of polar nanoregions (PNRs) within the grains.In this study, ceramics of (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3 were synthesized through a conventional calcination process (solid-state method) at 1000°C for 4 hours, with x(%) values ranging from 0.0 to 100. Room temperature XRD patterns confirmed the phase formation of the samples. The Rietveld refinement method was employed to verify the morphotropic phase boundary (MPB) at x(%)=16-20. We investigated the average crystallite size and lattice strain using Scherrer's formula and Williamson-Hall (W-H) analysis. SEM image analyses provided additional evidence of the impact of doping on structural growth under low temperatures. Relaxation time extracted from Z″(f) and M″(f) spectra for x(%) = 0.0, 12, 16, 20, and 30 followed the Arrhenius law, revealing the presence of three distinct relaxation mechanisms with varying activation energies. The shoulder response in M″(f) indirectly indicated the existence of highly polarizable entities in the samples, serving as a signature of polar nanoregions (PNRs) within the grains.

Keywords: (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3, Rietveld refinement, Scanning electron microscopy (SEM), Williamson-Hall plots, charge density distribution, dielectric properties

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711 Effect of Boric Acid Content on the Structural and Optical Properties of In2O3 Films Prepared by Spray Pyrolysis Technique

Authors: Mustafa Öztas, Metin Bedir, Yahya Özdemir

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Boron doped of In2O3 films were prepared by spray pyrolysis technique at 350 °C substrate temperature, which is a low cost and large area technique to be well-suited for the manufacture of solar cells, using boric acid (H3BO3) as dopant source, and their properties were investigated as a function of doping concentration. X-ray analysis showed that the films were polycrystalline fitting well with a hexagonal structure and have preferred orientation in (220) direction. The changes observed in the energy band gap and structural properties of the films related to the boric acid concentration are discussed in detail.

Keywords: spray pyrolysis, In2O3, boron, optical properties, boric acid

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710 Ferrites of the MeFe2O4 System (Me – Zn, Cu, Cd) and Their Two Faces

Authors: B. S. Boyanov, A. B. Peltekov, K. I. Ivanov

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The ferrites of Zn, Cd, Cu, and mixed ferrites with NiO, MnO, MgO, CoO, ZnO, BaO combine the properties of dielectrics, semiconductors, ferro-magnets, catalysts, etc. The ferrites are used in an impressive range of applications due to their remarkable properties. A specific disadvantage of ferrites is that they are undesirably obtained in a lot of processes connected with metal production. They are very stable and poorly soluble compounds. The obtained ZnFe2O4 in zinc production connecting about 15% of the total zinc remains practically insoluble in dilute solutions of sulfuric acid. This decreases the degree of recovery of zinc and necessitates to further process the zinc-containing cake. In this context, the ferrites; ZnFe2O4, CdFe2O4, and CuFe2O4 are synthesized in laboratory conditions using ceramic technology. Their homogeneity and structure are proven by X-Ray diffraction analysis and Mössbauer spectroscopy. The synthesized ferrites are subjected to strong acid and high temperature leaching with solutions of H2SO4, HCl, and HNO3 (7, 10 and 15 %). The results indicate that the highest degree of leaching of Zn, Cd, and Cu from the ferrites is achieved by use of HCl. The resulting values for the degree of leaching of metals using H2SO4 are lower, but still remain significantly higher for all of the experimental conditions compared to the values obtained using HNO3. Five zinc sulfide concentrates are characterized for iron content by chemical analysis, Web-based Information System, and iron phases by Mössbauer spectroscopy. The charging was optimized using the criterion of minimal amount of zinc ferrite produced when roasting the concentrates in a fluidized bed. The results obtained are interpreted in terms of the hydrometallurgical zinc production and maximum recovery of zinc, copper and cadmium from initial zinc sulfide concentrates after their roasting.

Keywords: hydrometallurgy, inorganic acids, solubility, zinc ferrite

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709 Carbon Nanotube-Based Catalyst Modification to Improve Proton Exchange Membrane Fuel Cell Interlayer Interactions

Authors: Ling Ai, Ziyu Zhao, Zeyu Zhou, Xiaochen Yang, Heng Zhai, Stuart Holmes

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Optimizing the catalyst layer structure is crucial for enhancing the performance of proton exchange membrane fuel cells (PEMFCs) with low Platinum (Pt) loading. Current works focused on the utilization, durability, and site activity of Pt particles on support, and performance enhancement has been achieved by loading Pt onto porous support with different morphology, such as graphene, carbon fiber, and carbon black. Some schemes have also incorporated cost considerations to achieve lower Pt loading. However, the design of the catalyst layer (CL) structure in the membrane electrode assembly (MEA) must consider the interactions between the layers. Addressing the crucial aspects of water management, low contact resistance, and the establishment of effective three-phase boundary for MEA, multi-walled carbon nanotubes (MWCNTs) are promising CL support due to their intrinsically high hydrophobicity, high axial electrical conductivity, and potential for ordered alignment. However, the drawbacks of MWCNTs, such as strong agglomeration, wall surface chemical inertness, and unopened ends, are unfavorable for Pt nanoparticle loading, which is detrimental to MEA processing and leads to inhomogeneous CL surfaces. This further deteriorates the utilization of Pt and increases the contact resistance. Robust chemical oxidation or nitrogen doping can introduce polar functional groups onto the surface of MWCNTs, facilitating the creation of open tube ends and inducing defects in tube walls. This improves dispersibility and load capacity but reduces length and conductivity. Consequently, a trade-off exists between maintaining the intrinsic properties and the degree of functionalization of MWCNTs. In this work, MWCNTs were modified based on the operational requirements of the MEA from the viewpoint of interlayer interactions, including the search for the optimal degree of oxidation, N-doping, and micro-arrangement. MWCNT were functionalized by oxidizing, N-doping, as well as micro-alignment to achieve lower contact resistance between CL and proton exchange membrane (PEM), better hydrophobicity, and enhanced performance. Furthermore, this work expects to construct a more continuously distributed three-phase boundary by aligning MWCNT to form a locally ordered structure, which is essential for the efficient utilization of Pt active sites. Different from other chemical oxidation schemes that used HNO3:H2SO4 (1:3) mixed acid to strongly oxidize MWCNT, this scheme adopted pure HNO3 to partially oxidize MWCNT at a lower reflux temperature (80 ℃) and a shorter treatment time (0 to 10 h) to preserve the morphology and intrinsic conductivity of MWCNT. The maximum power density of 979.81 mw cm-2 was achieved by Pt loading on 6h MWCNT oxidation time (Pt-MWCNT6h). This represented a 59.53% improvement over the commercial Pt/C catalyst of 614.17 (mw cm-2). In addition, due to the stronger electrical conductivity, the charge transfer resistance of Pt-MWCNT6h in the electrochemical impedance spectroscopy (EIS) test was 0.09 Ohm cm-2, which was 48.86% lower than that of Pt/C. This study will discuss the developed catalysts and their efficacy in a working fuel cell system. This research will validate the impact of low-functionalization modification of MWCNTs on the performance of PEMFC, which simplifies the preparation challenges of CL and contributing for the widespread commercial application of PEMFCs on a larger scale.

Keywords: carbon nanotubes, electrocatalyst, membrane electrode assembly, proton exchange membrane fuel cell

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