Search results for: powder X-ray diffraction

Authors: Mohd Ishfaq Bhat, Navin Chandra Shahi, Umesh Chandra Lohani

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The present study aimed to evaluate the effect of microwave application in synergy with the conventional sodium chlorite delignification of rice straw biomass. For the study, Box-Behnken experimental design involving four independent parameters, each with three levels viz. microwave power (480-800 W), irradiation time (4-12 min), bleaching solution concentration (0.4-3.0%), and bleaching time (1-5h) was used. The response was taken in the form of delignification percentage. The optimization of process parameters was done through response surface methodology. The respective optimum parameters of microwave power, irradiation time, bleaching solution concentration, and bleaching time were obtained as 671 W, 8.66 min, 2.67%, and 1h. The delignification percentage achieved at optimum conditions was 93.51%. The spectral, morphological, and x-ray diffraction characteristics of the rice straw powder after delignification showed a complete absence of lignin peaks, deconstruction of lignocellulose complex, and an increase of crystallinity (from 39.8 to 61.6 %).

Keywords: lignocellulosic biomass, delignification, microwaves, rice straw, characterization

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Authors: Fatih Hattatoglu, Abdulrezzak Bakiş

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In this study, fiberless reactive powder concrete (RPC) was produced with high pressure and flexural strength. C30/37 concrete was chosen as the control sample. In this study, 9 different cure types were applied to fiberless RPC. the most suitable combined cure type was selected according to the pressure and flexure strength. Pressure and flexural strength tests were applied to these samples after curing. As a result of the study, the combined cure type with the highest pressure resistance was obtained. The highest pressure resistance was achieved with consecutive standard water cure at 20 °C for 7 days – hot water cure at 90 °C for 2 days - drying oven cure at 180 °C for 2 days. As a result of the study, the highest pressure resistance of fiberless RPC was found as 123 MPa with water cure at 20 °C for 7 days - hot water cure at 90 °C for 2 days - drying oven cure at 180 °C for 2 days; and the highest flexural resistance was found as 8.37 MPa for the same combined cure type.

Keywords: combined cure, flexural test, reactive powder concrete (RPC), rigid pavement, pressure test

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Authors: Thu Nhi Tran Caliste

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X-ray Bragg diffraction imaging (“topography”)entered into practical use when Lang designed an “easy” technical setup to characterise the defects / distortions in the high perfection crystals produced for the microelectronics industry. The use of this technique extended to all kind of high quality crystals, and deposited layers, and a series of publications explained, starting from the dynamical theory of diffraction, the contrast of the images of the defects. A quantitative version of “monochromatic topography” known as“Rocking Curve Imaging” (RCI) was implemented, by using synchrotron light and taking advantage of the dramatic improvement of the 2D-detectors and computerised image processing. The rough data is constituted by a number (~300) of images recorded along the diffraction (“rocking”) curve. If the quality of the crystal is such that a one-to-onerelation between a pixel of the detector and a voxel within the crystal can be established (this approximation is very well fulfilled if the local mosaic spread of the voxel is < 1 mradian), a software we developped provides, from the each rocking curve recorded on each of the pixels of the detector, not only the “voxel” integrated intensity (the only data provided by the previous techniques) but also its “mosaic spread” (FWHM) and peak position. We will show, based on many examples, that this new data, never recorded before, open the field to a highly enhanced characterization of the crystal and deposited layers. These examples include the characterization of dislocations and twins occurring during silicon growth, various growth features in Al203, GaNand CdTe (where the diffraction displays the Borrmannanomalous absorption, which leads to a new type of images), and the characterisation of the defects within deposited layers, or their effect on the substrate. We could also observe (due to the very high sensitivity of the setup installed on BM05, which allows revealing these faint effects) that, when dealing with very perfect crystals, the Kato’s interference fringes predicted by dynamical theory are also associated with very small modifications of the local FWHM and peak position (of the order of the µradian). This rather unexpected (at least for us) result appears to be in keeping with preliminary dynamical theory calculations.

Keywords: rocking curve imaging, X-ray diffraction, defect, distortion

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Authors: Suneeta Kumari, Abanti Sahoo

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Industrial effluents treatment is a major problem in the world. All wastewater treatment methods have some problems in the environment. Due to this reason, today many natural biopolymers are being used in the waste water treatment because those are safe for our environment. In this study, synthesis and characterization of polyethersulfone/chitosan membranes (Thin film composite membrane) are carried out. Fish scales are used as raw materials. Different characterization techniques such as Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), scanning electron microscope (SEM) and Thermal gravimetric analysis (TGA) are analysed for the synthesized membrane. The performance of membranes such as flux, rejection, and pore size are also checked. The synthesized membrane is used for the treatment of steel industry waste water where Biochemical oxygen demand (BOD), Chemical Oxygen Demand (COD), pH, colour, Total dissolved solids (TDS), Total suspended solids (TSS), Electrical conductivity (EC) and Turbidity aspects are analysed.

Keywords: fish scale, membrane synthesis, treatment of industrial effluents, chitosan

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Authors: Suresh Palla, Kalpna Sharma, Gaurav Bhatnagar, S. K. Chaturvedi, B. N. Mohapatra

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Determining the content of free lime is especially important to judge reactivity of the raw materials and clinker quality. The free lime limit isn’t the same for all cements; it depends on several factors, especially the temperature reached during the cooking and the grain size distribution in cement after grinding. Estimation of free lime by conventional method is influenced by the presence of portlandite and misleads the actual free lime content in the clinker for quality check up conditions. To ensure the product quality according to the standard specifications in terms of within the quality limits or not, a reliable, precise, and very reproducible method to quantify the relative phase abundances in the Portland Cement clinker and Portland Cements is to use X-ray diffraction (XRD) in combination with the Rietveld method. In the present study, a methodology was proposed using XRD to validate the obtained results of free lime by conventional method. The XRD and TG/DTA results confirm the presence of portlandite in the clinker to take the decision on the obtained free lime results through conventional method.

Keywords: free lime, quantitative phase analysis, conventional method, x ray diffraction

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Authors: Leila Mosafa, Majid Moghadam, Mohammad Shahedi

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In this work, pectinase was immobilized on the surface of silica-coated magnetite nanoparticles via covalent attachment. The magnetite-immobilized enzyme was characterized by Fourier transform infrared spectroscopy, X-ray powder diffraction, scanning electron microscopy and vibrating sample magnetometry techniques. Response surface methodology using Minitab Software was applied for statistical designing of operating conditions in order to immobilize pectinase on magnetic nanoparticles. The optimal conditions were obtained at 30°C and pH 5.5 with 42.97 µl pectinase for 2 h. The immobilization yield was 50.6% at optimized conditions. Compared to the free pectinase, the immobilized pectinase was found to exhibit enhanced enzyme activity, better tolerance to the variation of pH and temperature, and improved storage stability. Both free and immobilized samples reduced the viscosity of apple juice from 1.12 to 0.88 and 0.92 mm2s-1, respectively, after 30 min at their optimum temperature. Furthermore, the immobilized enzyme could be reused six consecutive cycles and the efficiency loss in viscosity reduction was found to be only 8.16%.

Keywords: magnetite nanoparticles, pectinase enzyme, immobilization, juice clarification, enzyme activity

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Authors: Ammar Z. Alshemary, Zafer Evis

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In this study, nanorods of Cr³⁺/SiO₄⁴⁻ codoped hydroxyapatite (Cr³⁺/SiO₄⁴⁻-HA) were synthesized successfully and rapidly through microwave irradiation technique, using (Ca(NO₃)₂•4H₂O), ((NH₄)₂HPO₄), (SiC₈H₂₀O₄) and (Cr(NO₃)₃.9H₂O) as source materials for Ca²⁺, PO₄³⁻, SiO₄⁴⁻ and Cr³⁺ ions, respectively. The impact of dopants on the phase formation and microstructure of the powders were investigated by means of X-ray diffraction (XRD), Fourier transform infrared spectrum analysis (FT-IR) and Field emission electron microscopy (FESEM) techniques. XRD analysis showed that with an incorporation of Cr³⁺/SiO₄⁴⁻ ions into HA structure resulted in peak broadening and reduced peak height due to the amorphous nature and reduced crystallinity of the resulting HA powder. FTIR spectroscopy revealed the existence of the different vibrational modes matching to phosphates and hydroxyl groups. The FESEM analysis showed a change in the crystal shape from spherical to rod shaped particles upon Cr³⁺ doping into the crystal structure. Acknowledgments: This study was supported by Karabük University (Project no. KBÜBAP-17-YD-144). The authors would like to thank for support.

Keywords: nano-hydroxyapatite, microwave, dopants, characterization, microstructure

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Authors: H. Farokhi, A. Bahadoran

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This paper is focused on the absorbance and magnetic properties of a novel nanocomposite based on conducting polymer, carbon black and barium hexaferrite in epoxy resin on the E-glass fibre substrate. The highly conductive nanocomposite was provided by in-situ polymerization of aniline in the presence of carbon black (C) and barium hexaferrite (BaFe12O19) as electromagnetic absorbance material. The structure, morphology, and magnetic properties of samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). SEM images showed the uniformly coated PAni on the surface of carbon black and barium hexaferrite. XRD peaks also verified the presence of carbon black and barium hexaferrite in the nanocomposite. The microwave characteristics determined from the magnetic and dielectric properties of the elastomeric composites obtained from scattering data by fitting the samples in a waveguide, where measured in the frequency in X-band frequency range, the range of 8 to 12 GHz. The reflection losses were evaluated to be less than −5dB over the whole X-band frequency (8–12 GHz) for the thickness of 1.4mm.

Keywords: conductive polymer, magnetic materials, capacitance, electrochemical cell

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Authors: Raphaelle Guillou, Matthieu Le Saux, Jean-Christophe Brachet, Thomas Guilbert, Elodie Rouesne, Denis Menut, Caroline Toffolon-Masclet, Dominique Thiaudiere

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In some hypothetical accidental situations, such as during a Loss Of Coolant Accident (LOCA) in pressurized water reactors, fuel cladding tubes made of zirconium alloys can be exposed for a few minutes to steam at High Temperature (HT up to 1200°C) before being cooled and then quenched in water. Under LOCA-like conditions, the cladding undergoes a number of metallurgical changes (phase transformations, oxygen diffusion and growth of an oxide layer...) and is consequently submitted to internal stresses whose state evolves during the transient. These stresses can have an effect on the oxide structure and the oxidation kinetics of the material. They evolve during cooling, owing to differences between the thermal expansion coefficients of the various phases and phase transformations of the metal and the oxide. These stresses may result in the failure of the cladding during quenching, once the material is embrittled by oxidation. In order to progress in the evaluation of these internal stresses, X-ray diffraction experiments were performed in-situ under synchrotron radiation during HT oxidation and subsequent cooling on Zircaloy-4 sheet samples. First, structural evolutions, such as phase transformations, have been studied as a function of temperature for both the oxide layer and the metallic substrate. Then, internal stresses generated within the material oxidized at temperatures between 700 and 900°C have been evaluated thanks to the 2θ diffraction peak position shift measured during the in-situ experiments. Electron backscatter diffraction (EBSD) analysis was performed on the samples after cooling in order to characterize their crystallographic texture. Furthermore, macroscopic strains induced by oxidation in the conditions investigated during the in-situ X-ray diffraction experiments were measured in-situ in a dilatometer.

Keywords: APRP, stains measurements, synchrotron diffraction, zirconium allows

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Authors: Ahmet Yönetken

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Al metal matrix composites reinforced with AlN have been fabricated by Tube furnace sintering at various temperatures. A uniform nickel layer on Al(%1AlN)%19Ni, Al(%2AlN)%18Ni, Al(%3AlN)%17Ni, Al(%4AlN)%16Ni, Al(%5AlN)%15Ni powders were deposited prior to sintering using electroless plating technique, allowing closer surface contact than can be achieved using conventional methods such as mechanical alloying. A composite consisting of quaternary additions, a ceramic phase, AlN, within a matrix of Al, AlN, Ni has been prepared at the temperature range between 550°C and 650°C under Ar shroud. X-Ray diffraction, SEM (Scanning Electron Microscope) density, and hardness measurements were employed to characterize the properties of the specimens. Experimental results carried out for 650°C suggest that the best properties as comprehension strength σmax and hardness 681.51(HV) were obtained at 650°C, and the tube furnace sintering of electroless Al plated (%5AlN)%15Ni powders is a promising technique to produce ceramic reinforced Al (%5AlN)%15Ni composites.

Keywords: electroless nickel plating, ceramic-metal composites, powder metallurgy, sintering

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Authors: Sheo K. Mishra, Rajneesh K. Srivastava, R. K. Shukla

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In the present work, we report on the optical properties including UV-vis absorption and photoluminescence (PL) of ZnO nanostructures synthesized by sol-gel method. Structural and morphological investigations have been performed by X-ray diffraction method (XRD) and scanning electron microscopy (SEM). The XRD result confirms the formation of hexagonal wurtzite phase of ZnO nanostructures. The presence of various diffraction peaks suggests polycrystalline nature. The XRD pattern exhibits no additional peak due to by-products such as Zn(OH)2. The average crystallite size of prepared ZnO sample corresponding to the maximum intensity peaks is to be ~38.22 nm. The SEM micrograph shows different nanostructures of pure ZnO. Photoluminescence (PL) spectrum shows several emission peaks around 353 nm, 382 nm, 419 nm, 441 nm, 483 nm and 522 nm. The obtained results suggest that the prepared phosphors are quite suitable for optoelectronic applications.

Keywords: ZnO, sol-gel, XRD, PL

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Authors: S. Lekhavat, U. Srimongkoluk, P. Ratanachamnong, G. Laungsopapun

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Quercetin was encapsulated with whey protein and high methoxyl pectin by spray drying technique. Feed solution, consisting of 0.1875 0.125 and 0.0625 % w/w quercetin, respectively, was prepared and then sprays at outlet temperature of 70, 80 and 90 °C. Quercetin contents either in feed solution or in spray dried powder were determined by HPLC technique. Physicochemical properties such as viscosity and total soluble solid of feed solution as well as moisture content and water activity of spray dried powder were examined. Particle morphology was imaged using scanning electron microscope. The results showed that feed solution has total soluble solid and viscosity in range of 1.73-5.60 ºBrix and 2.58-8.15 cP, in that order. After spray drying, the moisture content and water activity value of powder are in range of 0.58-2.72 % and 0.18-0.31, respectively. Quercetin content in dried sample increased along with outlet drying temperature but decreased when total soluble solid increased. It was shown that particles are likely to shrivel when spray drying at high temperature. The suggested conditions for encapsulation of quercetin are feed solution with 0.0625 % (w/w) quercetin and spray drying at drying outlet temperature of 90°C.

Keywords: drying temperature, particle morphology, spray drying, quercetin

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Authors: S. Ahmad, M. Rizwan, B. Ayub, S. Mehmood, P. Akhtar

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This experiment was conducted to investigate the effect of supplementation of pure herbal blend on growth performance of boilers. One hundred and twenty birds were randomly distributed into 4 experimental units of 3 replicates (10 birds/replicate) as: negative control (basal diet), positive control (Lincomycin at the rate of 5g/bag), pure herbal blend at the rate of 150g/bag and pure herbal blend at the rate of 300g/bag. The data regarding weekly feed intake, body weight gain and feed conversion ratio were recorded, and fecal samples were collected at the end of starter and finisher phase for nutrient digestibility trial. The results of feed intake showed significant (P < 0.05) results in 1st (305g), 2nd (696.88g), 3rd (1046.9g) and 4th (1173.2g) week and feed conversion ratio indicated significant (P < 0.05) variations in 1st (2.54) and 4th (2.28) week of age. Also, both starter and finisher phase indicated significant (P < 0.05) differences among all treatment groups in feed intake (2023.4g) and (2302.6g) respectively. The statistical analysis indicated significant (P < 0.05) results in crop filling percentage (86.6%) after 2 hours of first feed supplementation. In case of nutrient digestibility trial, results showed significant (P < 0.05) values of crude protein and crude fat in starter phase as 69.65% and 56.62% respectively, and 69.57% and 48.55% respectively, in finisher phase. Based on overall results, it was concluded that the dietary inclusion of pure herbal blend containing neem tree leaves powder, garlic powder, ginger powder and turmeric powder increase the production performance of broilers.

Keywords: neem tree leave, garlic, ginger, herbal blend, broiler

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Authors: Sang Kompiang Wirawan, Pandu Prabowo Jati, I Wayan Warmada

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Klaten Indonesian natural zeolite can be used as powder or pellet adsorbent. Pellet adsorbent has been made from activated natural zeolite powder by a conventional pressing method. Starch and formaldehyde were added as binder to strengthen the construction of zeolite pellet. To increase the absorptivity and its capacity, natural zeolite was activated first chemically and thermally. This research examined adsorption process of water from Isopropyl Alcohol (IPA)-water system using zeolite adsorbent pellet from natural zeolite powder which has been activated with H2SO4 0.1 M and 0.3 M. Adsorbent was pelleted by pressing apparatus at certain pressure to make specification in 1.96 cm diameter, 0.68 cm thickness which the natural zeolite powder (-80 mesh). The system of isopropyl-alcohol water contained 80% isopropyl-alcohol. Adsorption process was held in close-loop continuous apparatus which the zeolite pellet was put inside a column and the solution of IPA-water was circulated at certain flow. Concentration changing was examined thoroughly at a certain time. This adsorption process included mass transfer from bulk liquid into film layer and from film layer into the solid particle. Analysis of rate constant was using first order isotherm model that simulated with MATLAB. Besides using first order isotherm, intra-particle diffusion model was proposed by using pore diffusion model. The study shows that adsorbent activated by H2SO4 0.1 M has good absorptivity with mass transfer constant at 0.1286 min-1.

Keywords: intra-particle diffusion, fractional attainment, first order isotherm, zeolite

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Authors: Catherine Kuforiji, Michel Nganbe

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The abrasive wear of composite materials is a major challenge in highly demanding wear applications. Therefore, this study focuses on fabricating, testing and assessing the properties of 50wt% SS316L stainless steel–50wt% Al2O3 particle composites. Composite samples were fabricated using the powder metallurgy route. The effects of the powder metallurgy processing parameters and hard particle reinforcement were studied. The microstructure, density, hardness and toughness were characterized. The wear behaviour was studied using pin-on-disc testing under dry sliding conditions. The highest hardness of 1085.2 HV, the highest theoretical density of 94.7% and the lowest wear rate of 0.00397 mm3/m were obtained at a milling speed of 720 rpm, a compaction pressure of 794.4 MPa and sintering at 1400 °C in an argon atmosphere. Compared to commercial SS316 and fabricated SS316L, the composites had 7.4 times and 11 times lower wear rate, respectively. However, the commercial 90WC-10Co showed 2.2 times lower wear rate compared to the fabricated SS316L-Al2O3 composites primarily due to the higher ceramic content of 90 wt.% in the reference WC-Co. However, eliminating the relatively high porosity of about 5 vol% using processes such as HIP and hot pressing can be expected to lead to further substantial improvements of the composites wear resistance.

Keywords: SS316L, Al2O3, powder metallurgy, wear characterization

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Authors: Shams Ul Khaliq, Khan Shahzada, Bashir Alam, Fawad Bilal, Mushtaq Zeb, Faizan Akbar

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Marble industry contributes its fair share in environmental deterioration, producing voluminous amounts of mud and other excess residues obtained from marble and granite processing, polluting soil, water and air. Reusing these products in other products will not just prevent our environment from polluting but also help with economy. In this research, an attempt has been made to study the expediency of waste Marble Powder (MP) in concrete production. Various laboratory tests were performed to investigate permeability, physical and mechanical properties, such as slump, compressive strength, split tensile test, etc. Concrete test samples were fabricated with varying MP content (replacing 5-30% cement), furnished from two different sources. 5% replacement of marble dust caused 6% and 12% decrease in compressive and tensile strength respectively. These parameters gradually decreased with increasing MP content up to 30%. Most optimum results were obtained with 10% replacement. Improvement in consistency and permeability were noticed. The permeability was improved with increasing MP proportion up to 10% without substantial decrease in compressive strength. Obtained results revealed that MP as an alternative to cement in concrete production is a viable option considering its economic and environment friendly implications.

Keywords: marble powder, strength, permeability, consistency, environment

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Authors: Wilaisri Limphapayom

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Lime is one of the economically important produced in Thailand. The objective of this research is to increase utilization in food and cosmetic. Extraction of essential oil and pectin from lime (Citrus aurantifolia (Christm & Panz ) Swing) have been studied. Extraction of essential oil has been made by using hydro-distillation .The essential oil ranged from 1.72-2.20%. The chemical composition of essential oil composed of alpha-pinene , beta-pinene , D-limonene , comphene , a-phellandrene , g-terpinene , a-ocimene , O-cymene , 2-carene , Linalool , trans-ocimenol , Geraniol , Citral , Isogeraniol , Verbinol , and others when analyzed by using GC-MS method. Pectin extraction from lime waste , boiled water after essential oil extraction. Pectin extraction were found 40.11-65.81 g /100g of lime peel. The best extraction condition was found to be higher in yield by using ethanol extraction. The potential of this study had satisfactory results to improve lime processing system for value-added . The present study was also focused on Lime powder production as source of vitamin C or ascorbic acid and the potential of lime waste as a source of essential oil and pectin. Lime powder produced from Spray Dryer . Lime juice with 2 different level of maltodextrins DE 10 , 30 and 50% w/w was sprayed at 150 degrees celsius inlet air temperature and at 90-degree celsius outlet temperature. Lime powder with 50% maltodextrin gave the most desirable quality product. This product has vitamin C contents of 25 mg/100g (w/w).

Keywords: extraction, pectin, essential oil, lime

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Authors: Sang Beom Kim, Kyung Ju Kim, Myung Hoon Cho, Ji Hoon Kim, Soo Hyung Kim

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In this study, we systematically investigated the effect of nanoscale energetic materials in formulations of aluminum nanoparticles (Al NPs; heat source)/copper oxide nanoparticles (CuO NPs; oxidizer) on the combustion and gas-generating properties of sodium azide microparticles (NaN3 MPs; gas-generating agent) for potential applications in gas generators. The burn rate of the NaN3 MP/CuO NP composite powder was only ~0.3 m/s. However, the addition of Al NPs to the NaN3 MP/CuO NP matrix caused the rates to reach ~5.3 m/s, respectively. In addition, the N2 gas volume flow rate generated by the ignition of the NaN3 MP/CuO NP composite powder was only ~0.6 L/s, which was significantly increased to ~3.9 L/s by adding Al NPs to the NaN3 MP/CuO NP composite powder. This suggested that the highly reactive NPs, with the assistance of CuO NPs, were effective heat-generating sources enabling the complete thermal decomposition of NaN3 MPs upon ignition. Al NPs were highly effective in the gas generators because of the increased reactivity induced by the reduced particle size. Finally, we successfully demonstrated that a homemade airbag with a specific volume of ~140 mL could be rapidly and fully inflated by the thermal activation of nanoscale energetic material-added gas-generating agents (i.e., NaN3 MP/Al NP/CuO NP composites) within the standard time of ~50 ms for airbag inflation.

Keywords: nanoenergetic materials, aluminum nanoparticles, copper oxide nanoparticles, gas generators

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Authors: A. K. Jain, M. C. Paliwal

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The production of cement leads to the emission of large amounts of carbon-dioxide gas into the atmosphere which is a major contributor for the greenhouse effect and the global warming; hence it is mandatory either to quest for another material or partly replace it with some other material. According to the practical demonstrations and reports, Egg Shell Powder (ESP) can be used as a binding material for different field applications as it contains some of the properties of lime. It can partially replace the cement and further; it can be used in different proportion for enhancing the performance of cement. It can be used as a first-class alternative, for material reuse and waste recycling practices. Eggshell is calcium rich and analogous to limestone in chemical composition. Therefore, use of eggshell waste for partial replacement of cement in concrete is feasible. Different studies reveal that plasticity index of the soil can be improved by adding eggshell wastes in all the clay soil and it has wider application in construction projects including earth canals and earthen dams. The scarcity of aggregates is also increasing nowadays. Utilization of industrial waste or secondary materials is increasing in different construction applications. Coconut shell was successfully used in the construction industry for partial or full replacement for coarse aggregates. The use of coconut shell gives advantage of using waste material to partially replace the coarse aggregate. Studies carried on coconut shell indicate that it can partially replace the aggregate. It has good strength and modulus properties along with the advantage of high lignin content. It absorbs relatively low moisture due to its low cellulose content. In the paper, study carried out on eggshell powder and coconut shell will be discussed. Optimum proportions of these materials to be used for partial replacement of cement and aggregate will also be discussed.

Keywords: greenhouse, egg shell powder, binding material, aggregates, coconut shell, coarse aggregates

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Authors: Olga Yu Kurapova, Alexander V. Shorokhov, Vladimir G. Konakov

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Nowadays, due to their exceptional anion conductivity at high temperatures cubic zirconia solid solutions, stabilized by rare-earth and alkaline-earth metal oxides, are widely used as a solid electrolyte (SE) materials in different electrochemical devices such as gas sensors, oxygen pumps, solid oxide fuel cells (SOFC), etc. Nowadays the intensive studies are carried out in a field of novel fully stabilized zirconia based SE development. The use of precursor powders for SE manufacturing allows predetermining the microstructure, electrical and sensor characteristics of zirconia based ceramics used as SE. Thus the goal of the present work was the investigation of the effect of precursor powder size on the electrical and sensor characteristics of fully stabilized zirconia-based solid electrolytes with compositions of 0,08Y2O3∙0,92ZrO2 (YSZ), 0,06Ce2O3∙ 0,06Y2O3∙0,88ZrO2 and 0,09Ce2O3∙0,06Y2O3-0,85ZrO2. The synthesis of precursors powders with different mean particle size was performed by sol-gel synthesis in the form of reversed co-precipitation from aqueous solutions. The cakes were washed until the neutral pH and pan-dried at 110 °С. Also, YSZ ceramics was obtained by conventional solid state synthesis including milling into a planetary mill. Then the powder was cold pressed into the pellets with a diameter of 7.2 and ~4 mm thickness at P ~16 kg/cm2 and then hydrostatically pressed. The pellets were annealed at 1600 °С for 2 hours. The phase composition of as-synthesized SE was investigated by X-Ray photoelectron spectroscopy ESCA (spectrometer ESCA-5400, PHI) X-ray diffraction analysis - XRD (Shimadzu XRD-6000). Following galvanic cell О2 (РО2(1)), Pt | SE | Pt, (РО2(2) = 0.21 atm) was used for SE sensor properties investigation. The value of РО2(1) was set by mixing of O2 and N2 in the defined proportions with the accuracy of  5%. The temperature was measured by Pt/Pt-10% Rh thermocouple, The cell electromotive force (EMF) measurement was carried out with ± 0.1 mV accuracy. During the operation at the constant temperature, reproducibility was better than 5 mV. Asymmetric potential measured for all SE appeared to be negligible. It was shown that the resistivity of YSZ ceramics decreases in about two times upon the mean agglomerates decrease from 200-250 to 40 nm. It is likely due to the both surface and bulk resistivity decrease in grains. So the overall decrease of grain size in ceramic SE results in the significant decrease of the total ceramics resistivity allowing sensor operation at lower temperatures. For the SE manufactured the estimation of oxygen ion transfer number tion was carried out in the range 600-800 °С. YSZ ceramics manufactured from powders with the mean particle size 40-140 nm, shows the highest values i.e. 0.97-0.98. SE manufactured from precursors with the mean particle size 40-140 nm shows higher sensor characteristic i.e. temperature and oxygen concentration EMF dependencies, EMF (ENernst - Ereal), tion, response time, then ceramics, manufactured by conventional solid state synthesis.

Keywords: oxygen sensors, precursor powders, sol-gel synthesis, stabilized zirconia ceramics

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Authors: Mohsen Sanayei, Jerzy Szpunar, Sami Penttilä

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Exposure of Nickel-based superalloys to high temperature and harsh environment such as Super-Critical Water (SCW) environment leads to the formation of oxide scales composed of multiple and complex phases that are difficult to differentiate with conventional analysis techniques. In this study, we used simultaneous Electron Backscatter Diffraction (EBSD) and Energy Dispersive X-ray Spectroscopy (EDS) to analyze the complex oxide scales formed on several Nickel-based Superalloys exposed to high temperature SCW. Multi-layered structures of Iron, Nickel, Chromium and Molybdenum oxides and spinels were clearly identified using the simultaneous EBSD-EDS analysis technique. Furthermore, the orientation relationship between the oxide scales and the substrate has been investigated.

Keywords: electron backscatter diffraction, energy dispersive x-ray spectroscopy, superalloy, super-critical water

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Authors: Gonzalo Reyes, Magdalena Walczak, Esteban Ramos-Moore, Jorge Ramos-Grez

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Metal additive manufacture technologies have gained strong support and acceptance as a promising and alternative method to manufacture high performance complex geometry products. The main purpose of the present work is to study the microstructure and phase transformation temperatures of Cu-Al-Ni shape memory alloys fabricated from a direct laser additive process using metallic powders as precursors. The potential application is to manufacture self-centering seismic dampers for earthquake protection of buildings out of a copper based alloy by an additive process. In this process, the Cu-Al-Ni alloy is melted, inside of a high temperature and vacuum chamber with the aid of a high power fiber laser under inert atmosphere. The laser provides the energy to melt the alloy powder layer. The process allows fabricating fully dense, oxygen-free Cu-Al-Ni specimens using different laser power levels, laser powder interaction times, furnace ambient temperatures, and cooling rates as well as modifying concentration of the alloying elements. Two sets of specimens were fabricated with a nominal composition of Cu-13Al-3Ni and Cu-13Al-4Ni in wt.%, however, semi-quantitative chemical analysis using EDX examination showed that the specimens’ resulting composition was closer to Cu-12Al-5Ni and Cu-11Al-8Ni, respectively. In spite of that fact, it is expected that the specimens should still possess shape memory behavior. To confirm this hypothesis, phase transformation temperatures will be measured using DSC technique, to look for martensitic and austenitic phase transformations at 150°C. So far, metallographic analysis of the specimens showed defined martensitic microstructures. Moreover, XRD technique revealed diffraction peaks corresponding to (0 0 18) and (1 2 8) planes, which are too associated with the presence of martensitic phase. We conclude that it would be possible to obtain fully dense Cu-Al-Ni alloys having shape memory effect behavior by direct laser fabrication process, and to advance into fabrication of self centering seismic dampers by a controllable metal additive manufacturing process.

Keywords: Cu-Al-Ni alloys, direct laser fabrication, shape memory alloy, self-centering seismic dampers

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Authors: Flóra Pomázi, Sándor Baranya, Zoltán Szalai

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A harmonized monitoring of the suspended sediment transport along such a large river as the world’s most international river, the Danube River, is a rather challenging task. The traditional monitoring method in Hungary is obsolete but using indirect measurement devices and techniques like optical backscatter sensors (OBS), laser diffraction or acoustic backscatter sensors (ABS) could provide a fast and efficient alternative option of direct methods. However, these methods are strongly sensitive to the particle characteristics (i.e. particle shape, particle size and mineral composition). The current method does not provide sufficient information about particle size distribution, mineral analysis is rarely done, and the shape of the suspended sediment particles have not been examined yet. The aims of the study are (1) to determine the particle characterisation of suspended sediment in the Danube River using advanced particle characterisation methods as laser diffraction and automated imaging, and (2) to perform a sensitivity analysis of the indirect methods in order to determine the impact of suspended particle characteristics. The particle size distribution is determined by laser diffraction. The particle shape and mineral composition analysis is done by the Morphologi G3ID image analyser. The investigated indirect measurement devices are the LISST-Portable|XR, the LISST-ABS (Sequoia Inc.) and the Rio Grande 1200 kHz ADCP (Teledyne Marine). The major findings of this study are (1) the statistical shape of the suspended sediment particle - this is the first research in this context, (2) the actualised particle size distribution – that can be compared to historical information, so that the morphological changes can be tracked, (3) the actual mineral composition of the suspended sediment in the Danube River, and (4) the reliability of the tested indirect methods has been increased – based on the results of the sensitivity analysis and the previous findings.

Keywords: advanced particle characterisation, automated imaging, indirect methods, laser diffraction, mineral composition, suspended sediment

Procedia PDF Downloads 111

Authors: H. Karakoc, A. Uzun, G. Kırmızı, H. Çinici, R. Çitak

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The main objective of this investigation was to apply friction welding for joining of AA7039 rods produced by powder metallurgy. Friction welding joints were carried out using a rotational friction welding machine. Friction welds were obtained under different rotational speeds between (2700 and 2900 rpm). The friction pressure of 10 MPa and friction time of 30 s was kept constant. The cross sections of joints were observed by optical microscopy. The microstructures were analyzed using scanning electron microscope/energy dispersive X-ray spectroscopy. The Vickers micro hardness measurement of the interface was evaluated using a micro hardness testing machine. Finally the results obtained were compared and discussed.

Keywords: Aluminum alloy, powder metallurgy, friction welding, microstructure

Procedia PDF Downloads 337

Authors: I. Bouhaf Kharkhachi, A. Attaf

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Tin sulfide thin films on glass substrate were prepared by spray ultrasonic technique, at different experimental conditions. The influence of deposition time (2, 4, 6, 8 and 10 min) on different properties of thin films, such us, (XRD) and (UV) spectroscopy visible spectrum was investigated. X-ray diffraction showing that thin films crystallized in SnS, SnS2, and Sn2S3 phases. The results of (UV) spectroscopy visible spectrum show that films deposited at 4 min are large transmittance 60% in the visible region.

Keywords: SnS, thin films, ultrasonic spray, X-ray diffraction, UV spectroscopy visible

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Authors: Chandni Rani, S. D. Tiwari

Abstract:

Ferrihydrite is one of the distinct minerals in the family of oxides, hydroxides and oxyhydroxides of iron. It is a nanocrystalline material. It occurs naturally in different sediments, soil systems and also found in the core of ferritin, an iron storage protien. This material can also be synthesized by suitable chemical methods in laboratories. This is known as less crystalline Iron (III) Oxyhydroxide. Due to its poor crystallinity, there are very broad peaks in x-ray diffraction. Depending on the number of peaks in x-ray diffraction pattern, it is classified as two lines and six lines ferrihydrite. The average crystallite size for these two forms is found to be about 2nm to 5nm. The exact crystal structure of this system is still under debate. Out of these two forms, the six lines ferrihydrite is more ordered in comparison to two lines ferrihydrite. The magnetic behavior of two lines ferrihydrite nanoparticles is somewhat well studied. But the magnetic behavior of six lines ferrihydrite nanoparticles could not attract the attention of researchers much. This motivated us to work on the magnetic properties of six lines ferrihydrite nanoparticles. In this work, we present synthesis, structural characterization and magnetic behavior of 5 nm six lines ferrihydrite nanoparticles. X-ray diffraction and transmission electron microscope are used for structural characterization of this system. Magnetization measurements are performed to fit the data at different temperatures. Then the effect of magnetic moment distribution is also found. All these observations are discussed in detail.

Keywords: nanoparticles, magnetism, superparamagnetism, magnetic anisotropy

Procedia PDF Downloads 311

Authors: Abdalla A. Elbashir, Maali Saad Mokhtar, FakhrEldin O. Suliman

Abstract:

The inclusion complexes of imazapyr (IMA) with 2-hydroxypropyl(β/γ) cyclodextrins (HP β/γ-CD), have been studied in aqueous media and in the solid state. In this work, fluorescence spectroscopy, electrospray-ionization mass spectrometry (ESI-MS), and HNMR were used to investigate and characterize the inclusion complexes of IMA with the cyclodextrins in solutions. The solid-state complexes were obtained by freeze-drying and were characterized by Fourier transform infrared spectroscopy (FTIR), and powder X-ray diffraction (PXRD). The most predominant complexes of IMA with both hosts are the 1:1 guest: host complexes. The association constants of IMA-HP β-CD and IMA-HP γ -CD were 115 and 215 L mol⁻¹, respectively. Molecular dynamic (MD) simulations were used to monitor the mode of inclusion and also to investigate the stability of these complexes in aqueous media at atomistic levels. The results obtained have indicated that these inclusion complexes are highly stable in aqueous media, thereby corroborating the experimental results. Additionally, it has been demonstrated that in addition to hydrophobic interactions and van der Waals interactions the presence of hydrogen bonding interactions of the type H---O and CH---O between the guest and the host have enhanced the stability of these complexes remarkably.

Keywords: imazapyr, inclusion complex, herbicides, 2-hydroxypropyl-β/γ-cyclodextrin

Procedia PDF Downloads 142

Authors: Haidy N. Salem, Nada O. Kamel, Shahinaz N. Hassan, Sherif M. Elhefnawy

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Aim: to assess the effect of using turmeric powder extract on changes of tooth color with extra-coronal and intra-coronal bleaching methods. Methods: Turmeric powder extract was weighted and mixed with two different hydrogen peroxide concentrations (3% and 6%) to be used as a bleaching agent. Thirty teeth were allocated into three groups (n=10): Group A: Bleaching agent (6%) was applied on the labial surface, Group B: Bleaching agent (3%) was applied inside the pulp chamber and Group C: Extra and intra-coronal bleaching techniques were used (6% and 3% respectively). A standardized access cavity was opened in the palatal surface of each tooth in both Groups B and C. Color parameters were measured using a spectrophotometer. Results: A statistically significant difference in color difference values (∆E*) and enamel brightness (∆L*) was found between Group C and each of Groups A and B. There was no statistically significant difference in (∆E*) and (∆L*) between Group A and Group B. The highest mean value of (∆E*) and (∆L*) was found in Group C, while the least mean value was found in Group B. Conclusion: Bleaching the external and internal tooth structure with low concentrations of hydrogen peroxide solution mixed with turmeric extract has a promising effect in color enhancement.

Keywords: bleaching, hydrogen peroxide, spectrophotometer, turmeric

Procedia PDF Downloads 83

Authors: Anna M. Salejda, Urszula Tril, Grażyna Krasnowska

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The aim of this study was to analyze selected quality characteristics of cooked pork sausages manufactured with the addition of Sea buckthorn (Hippophae rhamnoides L.) berries preparations. Stuffings of model sausages consisted of pork, backfat, water and additives such a curing salt and sodium isoascorbate. Functional additives used in production process were two preparations obtained from dried Sea buckthorn berries in form of powder and brew. Powder of dried berries was added in amount of 1 and 3 g, while water infusion as a replacement of 50 and 100% ice water included in meat products formula. Control samples were produced without functional additives. Experimental stuffings were heat treated in water bath and stored for 4 weeks under cooled conditions (4±1ºC). Physical parameters of colour, texture profile and technological parameters as acidity, weight losses and water activity were estimated. The effect of Sea buckthorn berries preparations on lipid oxidation during storage of final products was determine by TBARS method. Studies have shown that addition of Sea buckthorn preparations to meat-fatty batters significant (P≤0.05) reduced the pH values of sausages samples after thermal treatment. Moreover, the addition of berries powder caused significant differences (P ≤ 0.05) in weight losses after cooking process. Analysis of results of texture profile analysis indicated, that utilization of infusion prepared from Sea buckthorn dried berries caused increase of springiness, gumminess and chewiness of final meat products. At the same time, the highest amount of Sea buckthorn berries powder in recipe caused the decrease of all measured texture parameters. Utilization of experimental preparations significantly decreased (P≤0.05) lightness (L* parameter of color) of meat products. Simultaneously, introduction of 1 and 3 grams of Sea buckthorn berries powder to meat-fatty batter increased redness (a* parameter) of samples under investigation. Higher content of substances reacting with thiobarbituric acid was observed in meat products produced without functional additives. It was observed that powder of Sea buckthorn berries added to meat-fatty batters caused higher protection against lipid oxidation in cooked sausages.

Keywords: sea buckthorn, meat products, texture, color parameters, lipid oxidation

Procedia PDF Downloads 275

Authors: Yanbing Feng, Deqing Mei, Yancheng Wang, Zichen Chen

Abstract:

With the advantage of low volume density, high specific surface area, light weight and good permeability, porous aluminum material has the potential to be used in automotive, railway, chemistry and construction industries, etc. A layered powder sintering and dissolution method were developed to fabricate the porous surface Al structure with high efficiency. However, the densification mechanism during the cold compaction of laminar composite powders is still unclear. In this study, multi particle finite element modelling (MPFEM) based on the cohesive zone method (CZM) is used to simulate the cold compaction behavior of laminar Al and NaCl composite powders. To obtain its densification mechanism, the macro and micro properties of final compacts are characterized and analyzed. The robustness and accuracy of the numerical model is firstly verified by experimental results and data fitting. The results indicate that the CZM-based multi particle FEM is an effective way to simulate the compaction of the laminar powders and the fracture process of the NaCl powders. In the compaction of the laminar powders, the void is mainly filled by the particle rearrangement, plastic deformation of Al powders and brittle fracture of NaCl powders. Large stress is mainly concentrated within the NaCl powers and the contact force network is formed. The Al powder near the NaCl powder or the mold has larger stress distribution on its contact surface. Therefore, the densification process of cold compaction of laminar Al and NaCl composite powders is successfully analyzed by the CZM-based multi particle FEM.

Keywords: cold compaction, cohesive zone, multi-particle FEM, numerical modeling, powder forming

Procedia PDF Downloads 121