Abstract: The aim of this study is to moderate the dependence of counter frictional coefficient on temperature between counter surfaces and to reduce the wear of C/C composites at low temperature. To modify the C/C composites, Silica (SiO2) powders were added into phenolic resin for carbon precursor. The preform plate of the precursor of C/C composites was prepared by conventional filament winding method. The C/C composites plates were obtained by carbonizing preform plate at 2200 °C under an argon atmosphere. At that time, the silicon carbides (SiC) were synthesized around the surfaces and the internal vacancies of the C/C composites. The frictional coefficient on the counter surfaces and specific wear volumes of the C/C composites were measured by our developed frictional test machine like pin-on disk type. The XRD indicated that SiC was synthesized in the body of C/C composite fabricated by current method. The results of friction test showed that coefficient of friction of unmodified C/C composites have temperature dependence when the test condition was changed. In contrast, frictional coefficient of the C/C composite modified with SiO2 powders was almost constant at about 0.27 when the temperature condition was changed from Room Temperature (RT) to 300 °C. The specific wear rate decreased from 25×10-6 mm2/N to 0.1×10-6 mm2/N. The observations of the surfaces after friction tests showed that the frictional surface of the modified C/C composites was covered with a film produced by the friction. This study found that synthesizing SiC around surface and internal vacancies of C/C composites was effective to moderate the dependence on the frictional coefficient and reduce to the abrasion of C/C composites.
Abstract: This work investigated the use of Beijerinckia indica extracellular extract for the synthesis of silver nanoparticles using AgNO3. The formation of nanoparticles was confirmed by different methods, such as UV-Vis absorption spectroscopy, XRD, FTIR, EDX, and TEM analysis. The formation of silver nanoparticles (AgNPs) was confirmed by the change in color from light yellow to dark brown. The absorbance peak obtained at 430 nm confirmed the presence of silver nanoparticles. The XRD analysis showed the cubic crystalline phase of the synthesized nanoparticles. FTIR revealed the presence of groups that acts as stabilizing and reducing agents for silver nanoparticles formation. The synthesized silver nanoparticles were generally found to be spherical in shape with size ranging from 5 to 20 nm, as evident by TEM analysis. These nanoparticles were found to inhibit pathogenic bacterial strains. This work proved that the bacterial extract is a potential eco-friendly candidate for the synthesis of silver nanoparticles with promising antibacterial and antioxidant properties.
Abstract: The cadmium sulfide nanoparticles were synthesized from the nickel-cadmium cake of a hydrometallurgical zinc producing plant and sodium sulfide as Cd2+ and S-2 sources, respectively. Also, the synthesis process was performed by using the secretions of Bacillus licheniformis as bio-surfactant. Initially, in order to obtain a cadmium rich solution, two following steps were carried out: 1) Alkaline leaching for the removal of zinc oxide from the cake, and 2) acidic leaching to dissolve cadmium from the remained solid residue. Afterward, the obtained CdSO4 solution was used for the nanoparticle biosynthesis. Nanoparticles were characterized by the energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) to confirm the formation of CdS crystals with cubic structure. Also, transmission electron microscopy (TEM) was applied to determine the particle sizes which were in 2-10 nm range. Moreover, the presence of the protein containing bio-surfactants was approved by using infrared analysis (FTIR). In addition, the absorbance below 400 nm confirms quantum particles’ size. Finally, it was shown that valuable CdS quantum dots could be obtained from the industrial waste products via environment-friendly biological approaches.
Abstract: A nano-alumina-zirconia composite catalyst was synthesized by a simple aqueous sol-gel method using AlCl3.6H2O and ZrCl4 as precursors. Thermal decomposition of the precursor and subsequent formation of γ-Al2O3 and t-Zr were investigated by thermal analysis. XRD analysis showed that γ-Al2O3 and t-ZrO2 phases were formed at 700 °C. FT-IR analysis also indicated that the phase transition to γ-Al2O3 occurred in corroboration with X-ray studies. TEM analysis of the calcined powder revealed that spherical particles were in the range of 8-12 nm. The nano-alumina-zirconia composite particles were mesoporous and uniformly distributed in their crystalline phase. In order to measure the catalytic activity, esterification reaction was carried out. Biodiesel, as a renewable fuel, was formed in a continuous packed column reactor. Free fatty acid (FFA) was esterified with ethanol in a heterogeneous catalytic reactor. It was found that the synthesized γ-Al2O3/ZrO2 composite had the potential to be used as a heterogeneous base catalyst for biodiesel production processes.
Abstract: Well-defined 2D Eu+3 co-doped ZrO2: Gd+3 nanoparticles were successfully synthesized by microwave assisted solution combustion technique for luminescent applications. The present investigation reports the rapid and effective method for the synthesis of the Eu+3 co-doped ZrO2:Gd+3 nanoparticles and study of the luminescence behavior of Eu+3 ion in ZrO2:Gd+3 nanostructures. The optical properties of the prepared nanostructures were investigated by using UV-visible spectroscopy and photoluminescence spectra. The phase formation and the morphology of the nanoplatelets were studied by XRD, FESEM and HRTEM. The average grain size was found to be 45-50 nm. The presence of Gd3+ ion increases the crystallinity of the material and hence acts as a good nucleating agent. The ZrO2:Gd3+ co-doped with Eu+3 nanoplatelets gives an emission at 607 nm, a strong red emission under the excitation wavelength of 255 nm.
Abstract: Calcined kaolinite clay (CKC) is a pozzolanic material that is current drawing research attention. This work investigates the conditions for the best performance of a CKC from a kaolinite clay source in Ajebo, Abeokuta (southwest Nigeria) known for its commercial availability. Samples from this source were subjected to X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). XRD shows that kaolinite is the main mineral in the clay source. This mineral is responsible for the pozzolanic behavior of CKC. DSC indicates that the transformation from the clay to CKC occurred between 550 and 750 oC. Using this temperature range, clay samples were milled and different CKC samples were produced in an electric muffle furnace using temperatures of 550, 600, 650, 700, 750 and 800 oC respectively for 1 hour each. This was also repeated for 2 hours. The degree of de-hydroxylation (dtg) and strength activity index (SAI) were also determined for each of the CKC samples. The dtg and SAI tests were repeated two more times for each sample and averages were taken. Results showed that peak dtg occurred at 750 oC for 1 hour calcining combination (94.27%) whereas marginal differences were recorded at some lower temperatures (90.97% for 650 oC for 2 hours; 91.05% for 700 oC for 1 hour and 92.77% for 700 oC for 2 hours). Optimum SAI was reported at 700 oC for 1 hour (99.05%). Rating SAI as a better parameter than dtg, 700 oC for 1 hour combination was adopted as the best calcining condition. The paper recommends the adoption of this clay source for pozzolan production by adopting the calcining conditions established in this work.
Abstract: Silver ions (Ag+) and their compounds are consequentially toxic to microorganisms, showing biocidal effects on many species of bacteria. Silver-phosphate (or silver orthophosphate) is one of these compounds, which is famous for its antimicrobial effect and catalysis application. In the present study, a green method was presented to synthesis silver-phosphate nanoparticles using Sporosarcina pasteurii. The composition of the biosynthesized nanoparticles was identified as Ag3PO4 using X-ray Diffraction (XRD) and Energy Dispersive Spectroscopy (EDS). Also, Fourier Transform Infrared (FTIR) spectroscopy showed that Ag3PO4 nanoparticles was synthesized in the presence of biosurfactants, enzymes, and proteins. In addition, UV-Vis adsorption of the produced colloidal suspension approved the results of XRD and FTIR analyses. Finally, Transmission Electron Microscope (TEM) images indicated that the size of the nanoparticles was about 20 nm.
Abstract: Thermal insulating composites help to reduce the total power consumption in a building by creating a barrier between external and internal environment. Such composites can be used in the roofing tiles or wall panels for exterior surfaces. This study purposes to develop lightweight cement-based composites for thermal insulating applications. Waste materials like silica fume (an industrial by-product) and fly ash cenosphere (FAC) (hollow micro-spherical shells obtained as a waste residue from coal fired power plants) were used as partial replacement of cement and lightweight filler, respectively. Moreover, aerogel, a nano-porous material made of silica, was also used in different dosages for improved thermal insulating behavior, while poly vinyl alcohol (PVA) fibers were added for enhanced toughness. The raw materials including binders and fillers were characterized by X-Ray Diffraction (XRD), X-Ray Fluorescence spectroscopy (XRF), and Brunauer–Emmett–Teller (BET) analysis techniques in which various physical and chemical properties of the raw materials were evaluated like specific surface area, chemical composition (oxide form), and pore size distribution (if any). Ultra-lightweight cementitious composites were developed by varying the amounts of FAC and aerogel with 28-day unit weight ranging from 1551.28 kg/m3 to 1027.85 kg/m3. Excellent mechanical and thermal insulating properties of the resulting composites were obtained ranging from 53.62 MPa to 8.66 MPa compressive strength, 9.77 MPa to 3.98 MPa flexural strength, and 0.3025 W/m-K to 0.2009 W/m-K as thermal conductivity coefficient (QTM-500). The composites were also tested for peak temperature difference between outer and inner surfaces when subjected to heating (in a specially designed experimental set-up) by a 275W infrared lamp. The temperature difference up to 16.78 oC was achieved, which indicated outstanding properties of the developed composites to act as a thermal barrier for building envelopes. Microstructural studies were carried out by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDS) for characterizing the inner structure of the composite specimen. Also, the hydration products were quantified using the surface area mapping and line scale technique in EDS. The microstructural analyses indicated excellent bonding of FAC and aerogel in the cementitious system. Also, selective reactivity of FAC was ascertained from the SEM imagery where the partially consumed FAC shells were observed. All in all, the lightweight fillers, FAC, and aerogel helped to produce the lightweight composites due to their physical characteristics, while exceptional mechanical properties, owing to FAC partial reactivity, were achieved.
Abstract: The four-stroke single cylinder diesel engine has been used in this study, the pistons and valves of the engine have been stabilized, the aluminum oxide (Al2O3) in different ratios has been added in the power of zirconium (ZrO2) magnesium oxide (MgO), and has been coated with the plasma spray method. The pistons and valves of the combustion chamber of the engine are coated with 5 different (ZrO2 + MgO), (ZrO2 + MgO + 25% Al2O3), (ZrO2 + MgO + 50% Al2O3), (ZrO2 + MgO + 75% Al2O3), (Al2O3) sample. The material tests have been made for each of the coated engine parts with the scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) using Cu Kα radiation surface analysis methods. The engine tests have been repeated for each sample in any electric dynamometer in full power 1600 rpm, 2000 rpm, 2400 rpm and 2800 rpm engine speeds. The material analysis and engine tests have shown that the best performance has been performed with (ZrO2 + MgO + 50% Al2O3). Thus, there is no significant change in HC and Smoke emissions, but NOx emission is increased, as the engine improves power, torque, specific fuel consumption and CO emissions in the tests made with sample A3.
Abstract: Rare earths containing complex metal oxides have drawn much attention due to physical, chemical and optical properties which make them feasible in so many areas such as non-linear optical materials and ion exchanger. We have researched a systematic study to obtain rare earth containing zirconium molybdate compound, characterization, investigation of crystal system and calculation of unit cell parameters. After a successful synthesis of Nd2Zr3(MoO4)9 which is a member of rare earth metal containing complex oxides family, X-ray diffraction (XRD), High Score Plus/Rietveld refinement analysis, and Fourier Transform Infrared Spectroscopy (FTIR) were completed to determine the crystal structure. Morphological properties and elemental composition were determined by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. Thermal properties were observed via Thermogravimetric-differential thermal analysis (TG/DTA).
Abstract: Colemanite is the most common borate mineral, and the main source of the boron required by plants, human, and earth. Transition metals exhibit optical and physical properties such as; non-linear optical character, structural diversity, thermal stability, long cycle life and luminescent radiation. The doping of colemanite with a transition metal, bring it very interesting and attractive properties which make them applicable in industry. Iron doped calcium borate was synthesized by conventional solid state method at 1200 °C for 12 h with a systematic pathway. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS) were used to characterize structural and morphological properties. Also, thermal properties were recorded by thermogravimetric-differential thermal analysis (TG/DTA).
Abstract: CuAlO2 thin films are prepared on Si or sapphire substrate by sol-gel method using two kinds of sols. One is combination of Cu acetate and Al acetate basic, and the other is Cu nitrate and Al nitrate. In the case of acetate sol, XRD peaks of CuAlO2 observed at annealing temperature of 800-950 ºC on both Si and sapphire substrates. In contrast, in the case of the films prepared using nitrate on Si substrate, XRD peaks of CuAlO2 have been observed only at the annealing temperature of 800-850 ºC. At annealing temperature of 850ºC, peaks of other species have been observed beside the CuAlO2 peaks, then, the CuAlO2 peaks disappeared at annealing temperature of 900 °C with increasing in intensity of the other peaks. Intensity of the other peaks decreased at annealing temperature of 950 ºC with appearance of broad SiO2 peak. In the present, we ascribe these peaks as metal silicide.
Abstract: Natural sodium montmorillonite (NaMMT), Cloisite Na+ and two organophilic montmorillonites (OMMTs), Cloisites 20A and 15A were used. Polycaprolactone (PCL)/MMT composites containing 1, 3, 5, and 10 wt% of Cloisite Na+ and PCL/OMMT nanocomposites containing 5 and 10 wt% of Cloisites 20A and 15A were prepared via solution intercalation technique to study the influence of organic modifier loading on particle dispersion of PCL/ NaMMT composites. Thermal stabilities of the obtained composites were characterized by thermal analysis using the thermogravimetric analyzer (TGA) which showed that in the presence of nitrogen flow the incorporation of 5 and 10 wt% of filler brings some decrease in PCL thermal stability in the sequence: Cloisite Na+>Cloisite 15A > Cloisite 20A, while in the presence of air flow these fillers scarcely influenced the thermoxidative stability of PCL by slightly accelerating the process. The interaction between PCL and silicate layers was studied by Fourier transform infrared (FTIR) spectroscopy which confirmed moderate interactions between nanometric silicate layers and PCL segments. The electrical conductivity (σ) which describes the ionic mobility of the systems was studied as a function of temperature and showed that σ of PCL was enhanced on increasing the modifier loading at filler content of 5 wt%, especially at higher temperatures in the sequence: Cloisite Na+
Abstract: One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO3 (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La0.8Sr0.2MnO3/Zr0.92Y0.08O2 (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10-1 S/cm at 600 oC with 0.22 eV activation energy.
Abstract: Sorghum byproducts, namely bran, stalk, and panicle are examples of lignocellulosic biomass. These raw materials contain large amounts of polysaccharides, in particular hemicelluloses, celluloses, and lignins, which if efficiently extracted, can be utilised for the development of a range of added value products with potential applications in agriculture and food packaging sectors. The aim of this study was to characterise fractions extracted from sorghum bran and stalk with regards to their physicochemical properties that could determine their applicability as food-packaging materials. A sequential alkaline extraction was applied for the isolation of cellulosic, hemicellulosic and lignin fractions from sorghum stalk and bran. Lignin content, phenolic content and antioxidant capacity were also investigated in the case of the lignin fraction. Thermal analysis using differential scanning calorimetry (DSC) and X-Ray Diffraction (XRD) revealed that the glass transition temperature (Tg) of cellulose fraction of the stalk was ~78.33 oC at amorphous state (~65%) and water content of ~5%. In terms of hemicellulose, the Tg value of stalk was slightly lower compared to bran at amorphous state (~54%) and had less water content (~2%). It is evident that hemicelluloses generally showed a lower thermal stability compared to cellulose, probably due to their lack of crystallinity. Additionally, bran had higher arabinose-to-xylose ratio (0.82) than the stalk, a fact that indicated its low crystallinity. Furthermore, lignin fraction had Tg value of ~93 oC at amorphous state (~11%). Stalk-derived lignin fraction contained more phenolic compounds (mainly consisting of p-coumaric and ferulic acid) and had higher lignin content and antioxidant capacity compared to bran-derived lignin fraction.
Abstract: Organic compounds in wastewaters coming from textile and pharmaceutical industry generated multiple harmful effects on the environment and the human health. One of them is the methyl orange (MeO), an azoic dye considered to be a recalcitrant compound. The heterogeneous photocatalysis emerges as an alternative for treating this type of hazardous compounds, through the generation of OH radicals using radiation and a semiconductor oxide. According to the author’s knowledge, catalysts such as TiO2 doped with metals show high efficiency in degrading MeO; however, this presents economic limitations on industrial scale. Black sand can be considered as a naturally doped catalyst because in its structure is common to find compounds such as titanium, iron and aluminum oxides, also elements such as zircon, cadmium, manganese, etc. This study reports the photocatalytic activity of the mineral black sand used as semiconductor in the discoloration of MeO by oxidation and reduction photocatalytic techniques. For this, magnetic composites from the mineral were prepared (RM, M1, M2 and NM) and their activity were tested through MeO discoloration while TiO2 was used as reference. For the fractions, chemical, morphological and structural characterizations were performed using Scanning Electron Microscopy with Energy Dispersive X-Ray (SEM-EDX), X-Ray Diffraction (XRD) and X-Ray Fluorescence (XRF) analysis. M2 fraction showed higher MeO discoloration (93%) in oxidation conditions at pH 2 and it could be due to the presence of ferric oxides. However, the best result to reduction process was using M1 fraction (20%) at pH 2, which contains a higher titanium percentage. In the first process, hydrogen peroxide (H2O2) was used as electron donor agent. According to the results, black sand mineral can be used as natural semiconductor in photocatalytic process. It could be considered as a photocatalyst precursor in such processes, due to its low cost and easy access.
Abstract: Cylindrical alumina microfiltration membrane (GMITM Corporation, inside diameter=9 mm, outside diameter=13 mm, length= 50 mm) with an average pore size of 0.5 micrometer and porosity of about 0.35 was used as the support for membrane reactor. This support was soaked in boehmite sols, and the mean particle size was adjusted in the range of 50 to 500 nm by carefully controlling hydrolysis time, and calcined at 650 °C for two hours. This process was repeated with different boehmite solutions in order to achieve an intermediate layer with an average pore size of about 50 nm. The resulting substrate was then coated with a thin and dense layer of silica by counter current chemical vapour deposition (CVD) method. A boehmite sol with 10 wt.% of nickel which was prepared by a standard procedure was used to make the catalytic layer. BET, SEM, and XRD analysis were used to characterize this layer. The catalytic membrane reactor was placed in an experimental setup to evaluate the permeation and hydrogen separation performance for a steam reforming reaction. The setup consisted of a tubular module in which the membrane was fixed, and the reforming reaction occurred at the inner side of the membrane. Methane stream, diluted with nitrogen, and deionized water with a steam to carbon (S/C) ratio of 3.0 entered the reactor after the reactor was heated up to 500 °C with a specified rate of 2 °C/ min and the catalytic layer was reduced at presence of hydrogen for 2.5 hours. Nitrogen flow was used as sweep gas through the outer side of the reactor. Any liquid produced was trapped and separated at reactor exit by a cold trap, and the produced gases were analyzed by an on-line gas chromatograph (Agilent 7890A) to measure total CH4 conversion and H2 permeation. BET analysis indicated uniform size distribution for catalyst with average pore size of 280 nm and average surface area of 275 m2.g-1. Single-component permeation tests were carried out for hydrogen, methane, and carbon dioxide at temperature range of 500-800 °C, and the results showed almost the same permeance and hydrogen selectivity values for hydrogen as the composite membrane without catalytic layer. Performance of the catalytic membrane was evaluated by applying membranes as a membrane reactor for methane steam reforming reaction at gas hourly space velocity (GHSV) of 10,000 h−1 and 2 bar. CH4 conversion increased from 50% to 85% with increasing reaction temperature from 600 °C to 750 °C, which is sufficiently above equilibrium curve at reaction conditions, but slightly lower than membrane reactor with packed nickel catalytic bed because of its higher surface area compared to the catalytic layer.
Abstract: Perovskite-type membrane Ba0.5Sr0.5Ce0.9Y0.1O3-δ (BSCY) was successfully synthesized by liquid citrate method. The hydrogen permeation and stability of BSCY perovskite-type membranes were studied at high temperatures. The phase structure of the powder was characterized by X-ray diffraction (XRD). Scanning electron microscopy (SEM) was used to characterize microstructures of the membrane sintered under various conditions. SEM results showed that increasing in sintering temperature, formed dense membrane with clear grains. XRD results for BSCY membrane that sintered in 1150 °C indicated single phase perovskite structure with orthorhombic configuration, and SEM results showed dense structure with clear grain size which is suitable for permeation tests. Partial substitution of Sr with Ba in SCY structure improved the hydrogen permeation flux through the membrane due to the larger ionic radius of Ba2+. BSCY membrane shows high hydrogen permeation flux of 1.6 ml/min.cm2 at 900 °C and partial pressure of 0.6.
Abstract: Zinc oxide particles were synthesized using the sol-gel method and dip coated on polyester fabric. X-ray diffraction (XRD) analysis revealed a single crystal phase of ZnO particles. Chemical characteristics of the polyester fabric surface were investigated using attenuated total reflection-Fourier transform infrared (ATR-FTIR) measurements. Morphology of ZnO coated fabric was analyzed using field emission scanning electron microscopy (FESEM). After particle analysis, the aqueous ZnO solution resulted in a narrow size distribution at submicron levels. The deposit of ZnO on polyester fabrics yielded a homogeneous spread of spherical particles. Energy dispersive X-ray spectroscopy (EDX) results also affirmed the presence of ZnO particles on the polyester fabrics.
Abstract: Synthesizing supercritical carbon dioxide (scCO2) soluble precursors would be helpful for many processes of material syntheses based on scCO2. Ligand (amphi-(1Z, 2Z)-N-(2-fluoro-3-(trifluoromethyl) phenyl)-N'-hydroxy-2-(hydroxyimino) were synthesized from chloro glyoxime and flourus aniline and Pd(II) complex (precursor) prepared. For scCO2 deposition method, organometallic precursor was dissolved in scCO2 and impregnated onto the SBA-15 at 90 °C and 3000 psi. Then the organometallic precursor was reduced with H2 in the CO2 mixture (150 psi H2 + 2850 psi CO2). Pd deposited support material was characterized by ICP-OES, XRD, FE-SEM, TEM and EDX analyses. The Pd loading of the prepared catalyst, measured by ICP-OES showed a value of about 1.64% mol/g Pd of catalyst. Average particle size was found 5.3 nm. The catalytic activity of prepared catalyst was investigated over Suzuki-Miyaura C-C coupling reaction in different solvent with K2CO3 at 50 oC. The conversion ratio was determined by gas chromatography.