Scholarly

Monitoring the Drying and Grinding Process during Production of Celitement through a NIR-Spectroscopy Based Approach

Year: 2016 Volume: 10 Issue: 1 1 - 10 Pages

Abstract: Online measurement of the product quality is a challenging task in cement production, especially in the production of Celitement, a novel environmentally friendly hydraulic binder. The mineralogy and chemical composition of clinker in ordinary Portland cement production is measured by X-ray diffraction (XRD) and X-ray fluorescence (XRF), where only crystalline constituents can be detected. But only a small part of the Celitement components can be measured via XRD, because most constituents have an amorphous structure. This paper describes the development of algorithms suitable for an on-line monitoring of the final processing step of Celitement based on NIR-data. For calibration intermediate products were dried at different temperatures and ground for variable durations. The products were analyzed using XRD and thermogravimetric analyses together with NIR-spectroscopy to investigate the dependency between the drying and the milling processes on one and the NIR-signal on the other side. As a result, different characteristic parameters have been defined. A short overview of the Celitement process and the challenging tasks of the online measurement and evaluation of the product quality will be presented. Subsequently, methods for systematic development of near-infrared calibration models and the determination of the final calibration model will be introduced. The application of the model on experimental data illustrates that NIR-spectroscopy allows for a quick and sufficiently exact determination of crucial process parameters.

Synthesis, Structural, and Dielectric Characterization of Cadmium Oxide Nanoparticles

Year: 2014 Volume: 8 Issue: 12 1492 - 1495 Pages

Abstract: Cadmium oxide (CdO) nanoparticles have been prepared by chemical coprecipitation method. The synthesized nanoparticles were characterized by X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV analysis, and dielectric studies. The crystalline nature and particle size of the CdO nanoparticles were characterized by Powder X-ray diffraction analysis (XRD). The morphology of prepared CdO nanoparticles was studied by scanning electron microscopy. The particle size was studied using the transmission electron microscopy (TEM).The optical properties were obtained from UV-Vis absorption spectrum. The dielectric properties of CdO nanoparticles were studied in the frequency range of 50 Hz–5 MHz at different temperatures. The frequency dependence of the dielectric constant and dielectric loss is found to decrease with an increase in the frequency at different temperatures. The ac conductivity of CdO nanoparticle has been studied.

Keywords:
Cadmium Oxide (CdO)
XRD
SEM
Dielectric constant and Dielectric loss.

Amino Acid Coated Silver Nanoparticles: A Green Catalyst for Methylene Blue Reduction

Year: 2016 Volume: 10 Issue: 1 1 - 7 Pages

Abstract: Highly stable and homogeneously dispersed amino acid coated silver nanoparticles (ANP) of ≈ 10 nm diameter, ranging from 420 to 430 nm are prepared on AgNO3 solution addition to gum of Azadirachta indica solution at 373.15 K. The amino acids were selected based on their polarity. The synthesized nanoparticles were characterized by UV-Vis, FTIR spectroscopy, HR-TEM, XRD, SEM and 1H-NMR. The coated nanoparticles were used as catalyst for the reduction of methylene blue dye in presence of Sn(II) in aqueous, anionic and cationic micellar media. The rate of reduction of dye was determined by measuring the absorbance at 660 nm, spectrophotometrically and followed the order: Kcationic > Kanionic > Kwater. After 12 min and in absence of the ANP, only 2%, 3% and 6% of the dye reduction was completed in aqueous, anionic and cationic micellar media respectively while, in presence of ANP coated by polar neutral amino acid with non-polar -R group, the reduction completed to 84%, 95% and 98% respectively. The ANP coated with polar neutral amino acid having non-polar -R group, increased the rate of reduction of the dye by 94, 3205 and 6370 folds in aqueous, anionic and cationic micellar media respectively. Also, the rate of reduction of the dye increased by three folds when the micellar media was changed from anionic to cationic when the ANP is coated by a polar neutral amino acid having a non-polar -R group.

Utilization of Nanoclay to Reinforce Flax Fabric-Geopolymer Composites

Year: 2015 Volume: 9 Issue: 12 1405 - 1413 Pages

Abstract: Geopolymer composites reinforced with flax fabrics and nanoclay are fabricated and studied for physical and mechanical properties using X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Scanning Electron Microscope (SEM). Nanoclay platelets at a weight of 1.0%, 2.0%, and 3.0% were added to geopolymer pastes. Nanoclay at 2.0 wt.% was found to improve density and decrease porosity while improving flexural strength and post-peak toughness. A microstructural analysis indicated that nanoclay behaves as filler and as an activator supporting geopolymeric reaction while producing a higher content geopolymer gel improving the microstructure of binders. The process enhances adhesion between the geopolymer matrix and flax fibres.

The Effects and Interactions of Synthesis Parameters on Properties of Mg Substituted Hydroxyapatite

Year: 2015 Volume: 9 Issue: 12 1398 - 1404 Pages

Abstract: In this study, the effects and interactions of reaction time and capping agent assistance during sol-gel synthesis of magnesium substituted hydroxyapatite nanopowder (MgHA) on hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P ratio and mean crystallite size was examined experimentally as well as through statistical analysis. MgHA nanopowders were synthesized by sol-gel technique at room temperature using aqueous solution of calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and potassium dihydrogen phosphate as starting materials. The reaction time for sol-gel synthesis was varied between 15 to 60 minutes. Two process routes were followed with and without addition of triethanolamine (TEA) in the solutions. The elemental compositions of as-synthesized powders were determined using X-ray fluorescence (XRF) spectroscopy. The functional groups present in the assynthesized MgHA nanopowders were established through Fourier Transform Infrared Spectroscopy (FTIR). The amounts of phases present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders were determined using X-ray diffraction (XRD). The HA content in biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized MgHA nanopowders increased effectively with reaction time of sols (p0.15, two way ANOVA). The MgHA nanopowders synthesized with TEA assistance exhibited 14 nm lower crystallite size (p

Vapor Phase Transesterification of Dimethyl Malonate with Phenol over Cordierite Honeycomb Coated with Zirconia and Its Modified Forms

Year: 2015 Volume: 9 Issue: 12 1383 - 1386 Pages

Abstract: The transesterification of dimethyl malonate (DMM) with phenol has been studied in vapour phase over cordierite honeycomb coated with solid acid catalysts such as ZrO2, Mo(VI)/ZrO2 and SO42-/ZrO2. The catalytic materials were prepared honeycomb coated, powder forms, and characterized for their total surface acidity by NH3-TPD and crystalinity by powder XRD methods. Phenyl methyl malonate (PMM) and diphenyl malonate (DPM) were obtained as the reaction products. A good conversion of DMM (up to 82%) of MPM with 95% selectivity was observed when the reactions were carried out at a catalyst bed temperature of 200 °C and flow-rate of 10 mL/h in presence of Mo(VI)/ZrO2 as catalyst. However, over SO4^2-/ZrO2 catalyst, the yield of DPM was found to be higher. The results have been interpreted based on the variation of acidic properties and powder XRD phases of zirconia on incorporation of Mo(VI) or SO42– ions. Transesterification reactions were also carried out over powder forms of the catalytic materials and the yield of the desired phenyl ester products were compared with that of the HC coated catalytic materials. The solid acids were found to be reusable when used for at least 5 reaction cycles.

A Structural and Magnetic Investigation of the Inversion Degree in Spinel NiFe2O4, ZnFe2O4 and Ni0.5Zn0.5Fe2O4 Ferrites Prepared by Soft Mechanochemical Synthesis

Year: 2015 Volume: 9 Issue: 8 1066 - 1070 Pages

Abstract: NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2/Fe(OH)3, Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 25 h, 18 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase ferrite samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Inventive Synthesis and Characterization of a Cesium Molybdate Compound: CsBi(MoO4)2

Year: 2015 Volume: 9 Issue: 9 1171 - 1175 Pages

Abstract: Cesium molybdates with general formula CsMIII(MoO4)2, where MIII = Bi, Dy, Pr, Er, exhibit rich polymorphism, and crystallize in a layered structure. These properties cause intensive studies on cesium molybdates. CsBi(MoO4)2 was synthesized by microwave method by using cerium sulphate, bismuth oxide and molybdenum (VI) oxide in an appropriate molar ratio. Characterizations were done by x-ray diffraction (XRD), fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS), thermo gravimetric/differantial thermal analysis (TG/DTA).

Zinc Borate Synthesis Using Hydrozincite and Boric Acid with Ultrasonic Method

Year: 2015 Volume: 9 Issue: 8 1052 - 1055 Pages

Abstract: Zinc borate is an important inorganic hydrate borate material, which can be used as a flame retardant agent and corrosion resistance material. This compound can loss its structural water content at higher than 290°C. Due to thermal stability; Zinc Borate can be used as flame retardant at high temperature process of plastic and gum. In this study, the ultrasonic reaction of zinc borates were studied using hydrozincite (Zn5(CO3)2·(OH)6) and boric acid (H3BO3) raw materials. Before the synthesis raw materials were characterized by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). Ultrasonic method is a new application on the zinc borate synthesis. The synthesis parameters were set to 90°C reaction temperature and 55 minutes of reaction time, with 1:1, 1:2, 1:3, 1:4 and 1:5 molar ratio of starting materials (Zn5(CO3)2·(OH)6 : H3BO3). After the zinc borate synthesis, the products were analyzed by XRD and FT-IR. As a result, optimum molar ratio of 1:5 is determined for the synthesis of zinc borates with ultrasonic method.

Reinforcement of Calcium Phosphate Cement with E-Glass Fibre

Year: 2015 Volume: 9 Issue: 9 1230 - 1237 Pages

Abstract: Calcium Phosphate Cement (CPC) due to its high bioactivity and optimum bioresorbability shows excellent bone regeneration capability. Despite it has limited applications as bone implant due to its macro-porous microstructure causing its poor mechanical strength. The reinforcement of apatitic CPCs with biocompatible fibre glass phase is an attractive area of research to improve upon its mechanical strength. Here, we study the setting behaviour of Si-doped and un-doped α tri calcium phosphate (α - TCP) based CPC and its reinforcement with addition of E-glass fibre. Alpha Tri calcium phosphate powders were prepared by solid state sintering of CaCO3 , CaHPO4 and Tetra Ethyl Ortho Silicate (TEOS) was used as silicon source to synthesize Si doped α-TCP powders. Both initial and final setting time of the developed cement was delayed because of Si addition. Crystalline phases of HA (JCPDS 9- 432), α-TCP (JCPDS 29-359) and β-TCP (JCPDS 9-169) were detected in the X-ray diffraction (XRD) pattern after immersion of CPC in simulated body fluid (SBF) for 0 hours to 10 days. As Si incorporation in the crystal lattice stabilized the TCP phase, Si doped CPC showed little slower rate of conversion into HA phase as compared to un-doped CPC. The SEM image of the microstructure of hardened CPC showed lower grain size of HA in un-doped CPC because of premature setting and faster hydrolysis of un-doped CPC in SBF as compared that in Si-doped CPC. Premature setting caused generation of micro and macro porosity in un-doped CPC structure which resulted in its lower mechanical strength as compared to that in Si-doped CPC. It was found that addition of 10 wt% of E-glass fibre into Si-doped α-TCP increased the average DTS of CPC from 8 MPa to 15 MPa as the fibres could resists the propagation of crack by deflecting the crack tip. Our study shows that biocompatible E-glass fibre in optimum proportion in CPC matrix can enhance the mechanical strength of CPC without affecting its biocompatibility.

Pioneer Synthesis and Characterization of Boron Containing Hard Materials

Year: 2015 Volume: 9 Issue: 9 1155 - 1159 Pages

Abstract: The first laboratory synthesis of hard materials such as diamond proceeded to attack of developing materials with high hardness to compete diamond. Boron rich solids are good candidates owing to their short interatomic bond lengths and strong covalent character. Boron containing hard material was synthesized by modifiedmicrowave method under nitrogen atmosphere by using a fuel (glycine or urea), amorphous boron and/or boric acid in appropriate molar ratio. Characterizations were done by x-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS), thermo gravimetric/differential thermal analysis (TG/DTA).

Photocatalytic Degradation of Organic Pollutant Reacting with Tungstates: Role of Microstructure and Size Effect on Oxidation Kinetics

Year: 2015 Volume: 9 Issue: 2 376 - 380 Pages

Abstract: The aim of this study was to investigate the photocatalytic activity of polycrystalline phases of bismuth tungstate of formula Bi2WO6. Polycrystalline samples were elaborated using a coprecipitation technique followed by a calcination process at different temperatures (300, 400, 600 and 900°C). The obtained polycrystalline phases have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Crystal cell parameters and cell volume depend on elaboration temperature. High-resolution electron microscopy images and image simulations, associated with X-ray diffraction data, allowed confirming the lattices and space groups Pca21. The photocatalytic activity of the as-prepared samples was studied by irradiating aqueous solutions of Rhodamine B, associated with Bi2WO6 additives having variable crystallite sizes. The photocatalytic activity of such bismuth tungstates increased as the crystallite sizes decreased. The high specific area of the photocatalytic particles obtained at 300°C seems to condition the degradation kinetics of RhB.

Carbon Nanofibers Reinforced P(VdF-HFP) Based Gel Polymer Electrolyte for Lithium-Ion Battery Application

Year: 2015 Volume: 9 Issue: 10 1196 - 1199 Pages

Abstract: The effect of carbon nanofibers (CNFs) on the electrical properties of Poly(vinylidene fluoride-hexafluoropropylene) (P(VdF-HFP)) based gel polymer electrolytes has been investigated in the present work. The length and diameter ranges of CNFs used in the present work are 5-50 μm and 200-600 nm respectively. The nanocomposite gel polymer electrolytes have been synthesized by solution casting technique with varying CNFs content in terms of weight percentage. Electrochemical impedance analysis demonstrates that the reinforcement of carbon nanofibers significantly enhances the ionic conductivity of the polymer electrolyte. The decrease of crystallinity of P(VdF-HFP) due the addition of CNFs has been confirmed by X-ray diffraction (XRD). The interaction of CNFs with various constituents of nanocomposite gel polymer electrolytes has been assessed by Fourier Transform Infrared (FTIR) spectroscopy. Moreover CNFs added gel polymer electrolytes offer superior thermal stability as compared to that of CNFs free electrolytes as confirmed by Thermogravimetric analysis (TGA).

Nonlinear Absorption and Scattering in Wide Band Gap Silver Sulfide Nanoparticles Colloid and Their Effects on the Optical Limiting

Year: 2014 Volume: 8 Issue: 9 1274 - 1277 Pages

Abstract: In this paper, we study the optical nonlinearities of Silver sulfide (Ag2S) nanostructures dispersed in the Dimethyl sulfoxide (DMSO) under exposure to 532 nm, 15 nanosecond (ns) pulsed laser irradiation. Ultraviolet–visible absorption spectrometry (UV-Vis), X-ray diffraction (XRD), and transmission electron microscopy (TEM) are used to characterize the obtained nanocrystal samples. The band gap energy of colloid is determined by analyzing the UV–Vis absorption spectra of the Ag2S NPs using the band theory of semiconductors. Z-scan technique is used to characterize the optical nonlinear properties of the Ag2S nanoparticles (NPs). Large enhancement of two photon absorption effect is observed with increase in concentration of the Ag2S nanoparticles using open Zscan measurements in the ns laser regime. The values of the nonlinear absorption coefficients are determined based on the local nonlinear responses including two photon absorption. The observed aperture dependence of the Ag2S NP limiting performance indicates that the nonlinear scattering plays an important role in the limiting action of the sample. The concentration dependence of the optical liming is also investigated. Our results demonstrate that the optical limiting threshold decreases with increasing the silver sulfide NPs in DMSO.

Preparation of Nanocrystalline Mesoporous ThO2 via Surfactant Assisted Sol-gel Procedure

Year: 2015 Volume: 9 Issue: 8 1026 - 1029 Pages

Abstract: In this research, thorium dioxide mesoporous nanocrystalline powder was synthesized through the sol-gel method using hydrated thorium nitrate and ammonium hydroxide as starting materials and Triton X100 as surfactant. ThO2 gel was characterized by thermogravimetric (TGA), and prepared ThO2 powder was subjected to scanning electron microscopy (SEM), X-ray diffraction (XRD), and Brunauer-Emett-Teller (BET) analyses studies. Detailed analyses show that prepared powder consisted of phase with the space group Fm3m of thoria and its crystalline size was 12.6 nm. The thoria possesses 16.7 m2/g surface area and the pore volume and size calculated to be 0.0423 cc/g and 1.947 nm, respectively.

Synthesis of Gold Nanoparticles Stabilized in Na-Montmorillonite for Nitrophenol Reduction

Year: 2015 Volume: 9 Issue: 7 866 - 869 Pages

Abstract: Synthesis of gold nanoparticles has attracted much attention since the pioneering discovery of the high catalytic activity of supported gold nanoparticles in the reaction of CO oxidation at low temperature. In this research field, we used Na-montmorillonite for gold nanoparticles stabilization; various gold loading percentage 1, 2 and 5% were used for gold nanoparticles preparation. The gold nanoparticles were obtained using chemical reduction method using NaBH4 as reductant agent. The obtained gold nanoparticles stabilized in Na-montmorillonite were used as catalysts for the reduction of 4- nitrophenol to aminophenol with sodium borohydride at room temperature. The UV-Vis results confirmed directly the gold nanoparticles formation. The XRD and N2 adsorption results showed the formation of gold nanoparticles in the pores of montmorillonite with an average size of 5 nm obtained on samples with 2% gold loading percentage. The gold particles size increased with the increase of gold loading percentage. The reduction reaction of 4- nitrophenol into 4-aminophenol with NaBH4 catalyzed by Au-Namontmorillonite catalyst exhibits remarkably a high activity; the reaction was completed within 9 min for 1%Au-Na-montmorillonite and within 3 min for 2%Au-Na-montmorillonite.

Preparation of Protective Coating Film on Metal Alloy

Year: 2015 Volume: 9 Issue: 7 861 - 865 Pages

Authors:
Rana Th. A. Al-Rubaye

Abstract: A novel chromium-free protective coating films based on a zeolite coating was growing onto a FeCrAlloy metal using in – situ hydrothermal method. The zeolite film was obtained using in-situ crystallization process that is capable of coating large surfaces with complex shape and in confined spaces has been developed. The zeolite coating offers an advantage of a high mechanical stability and thermal stability. The physicochemical properties were investigated using X-ray diffraction (XRD), Electron Microscopy (SEM), Energy Dispersive X–ray Analysis (EDX) and Thermogravimetric Analysis (TGA). The transition from oxide-on-alloy wires to hydrothermally synthesised uniformly zeolite coated surfaces was followed using SEM and XRD. In addition, the robustness of the prepared coating was confirmed by subjecting these to thermal cycling (ambient to 550oC).

Synthesizing CuFe2O4 Spinel Powders by a Combustion-Like Process for Solid Oxide Fuel Cell Interconnect Coatings

Year: 2015 Volume: 9 Issue: 7 857 - 860 Pages

Abstract: The synthesis of CuFe2O4 spinel powders by an optimized combustion-like process followed by calcination is described herein. The samples were characterized using X-ray diffraction (XRD), differential thermal analysis (TG/DTA), scanning electron microscopy (SEM), dilatometry and 4-probe DC methods. Different glycine to nitrate (G/N) ratios of 1 (fuel-deficient), 1.48 (stoichiometric) and 2 (fuel-rich) were employed. Calcining the asprepared powders at 800 and 1000°C for 5 hours showed that the G/N ratio of 2 results in the formation of the desired copper spinel single phase at both calcination temperatures. For G/N=1, formation of CuFe2O4 takes place in three steps. First, iron and copper nitrates decompose to iron oxide and pure copper. Then, copper transforms to copper oxide and finally, copper and iron oxides react with each other to form a copper ferrite spinel phase. The electrical conductivity and the coefficient of thermal expansion of the sintered pelletized samples were 2 S.cm-1 (800°C) and 11×10-6 °C-1 (25-800°C), respectively.

Preparation and Characterization of Polyaniline (PANI)-Platinum Nanocomposite

Year: 2015 Volume: 9 Issue: 2 372 - 375 Pages

Abstract: Polyaniline is an indispensible component in lightemitting devices (LEDs), televisions, cellular telephones, automotive, corrosion-resistant coatings, actuators etc. The electrical conductivity properties was found be increased by introduction of metal nano particles. In the present study, an attempt has been made to utilize platinum nano particles to achieve the improved electrical properties. Polyaniline and Pt-polyaniline composite are synthesized by electrochemical routes. X-ray diffractometer confirms the amorphous nature of polyaniline. The Bragg’s diffraction peaks correspond to platinum nanoparticles in Pt-polyaniline composite and thermogravimetric analyzer indicates its decomposition at certain temperature. The Scanning Electron Micrographs of colloidal platinum nanoparticles were spherical, uniform shape in the composite. The current-voltage (I-V) characteristics of the PANI and composites were also studied which indicate a significant decreasing resistivity than PANI-Platinum after introduction of pt nanoparticles in the matrix of polyaniline (PANI).

The Effect of Aging of ZnO, AZO, and GZO Films on the Microstructure and Photoelectric Property

Year: 2015 Volume: 9 Issue: 6 737 - 742 Pages

Authors:
Zue Chin Chang

Abstract: RF magnetron sputtering is used on the ceramic targets, each of which contains zinc oxide (ZnO), zinc oxide doped with aluminum (AZO) and zinc oxide doped with gallium (GZO). The XRD analysis showed a preferred orientation along the (002) plane for ZnO, AZO, and GZO films. The AZO film had the best electrical properties; it had the lowest resistivity of 6.6 × 10-4 cm, the best sheet resistance of 2.2 × 10-1 Ω/square, and the highest carrier concentration of 4.3 × 1020 cm-3, as compared to the ZnO and GZO films.

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