Search results for: Scanning Electron Microscopy (SEM)

Authors: Mohamed Ahmed Abd El Kader

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This paper describes the conservation processes of an Ancient Egyptian wooden coffin dating back to the Middle Kingdom, ancient Egypt, using several scientific and analytical methods in order to provide a deeper understanding of the deterioration status and a greater awareness of how well preserved the object is. Visual observation and 2D Programs, as well as Optical Microscopy (OM), Environmental scanning Electron Microscopy (ESEM), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) were used in our study. The identification of wood species and the composition of the pigments and previous restoration materials were made. The coffin was previously conserved and stored in improper conditions, which led to its further deterioration; the surface of the lid dust, which obscured the decorations as well as all necessary restoration work was promptly carried out as soon as the coffin was transferred from the display hall from the Egyptian Museum to the Wood Conservation Laboratory of the Grand Egyptian Museum-Conservation Center (GEM-CC). The analyses provided detailed information concerning the original materials and the materials added during the previous treatment interventions, which was considered when applying the conservation plan. Conservation procedures have been applied with high accuracy to conserve the coffin including cleaning, consolidation of fragile painted layers, and the wooden boards forming the sides of the coffin were reassembled in their original positions. The materials and methods that were applied were extremely effective in stability and reinforcement of the coffin without harmfulness to the original materials and the coffin was successfully conserved and ready to display in the Grand Egyptian Museum (GEM).

Keywords: coffin, middle kingdom, deterioration, 2d program

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Authors: Fernández-Brito David, Lopez-Medina Javier Alonso, Murillo-Bracamontes Eduardo Antonio, Palomino-Ovando Martha Alicia, Gervacio-Arciniega José Juan

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Magnetic Force Microscopy (MFM) is an Atomic Force Microscopy (AFM) technique that characterizes, at a nanometric scale, the magnetic properties of ferromagnetic materials. Conventional MFM works by scanning in two different AFM modes. The first one is tapping mode, in which the cantilever has short-range force interactions with the sample, with the purpose to obtain the topography. Then, the lift AFM mode starts, raising the cantilever to maintain a fixed distance between the tip and the surface of the sample, only interacting with the magnetic field forces of the sample, which are long-ranged. In recent years, there have been attempts to improve the MFM technique. Bimodal MFM was first theoretically developed and later experimentally proven. In bimodal MFM, the AFM internal piezoelectric is used to cause the cantilever oscillations in two resonance modes simultaneously, the first mode detects the topography, while the second is more sensitive to the magnetic forces between the tip and the sample. However, it has been proven that the cantilever vibrations induced by the internal AFM piezoelectric ceramic are not optimal, affecting the bimodal MFM characterizations. Moreover, the Secondary Resonance Magnetic Force Microscopy (SR-MFM) was developed. In this technique, a coil located below the sample generates an external magnetic field. This alternating magnetic field excites the cantilever at a second frequency to apply the Bimodal MFM mode. Nonetheless, for ferromagnetic materials with a low coercive field, the external field used in SR-MFM technique can modify the magnetic domains of the sample. In this work, a Hybrid Bimodal MFM (HB-MFM) technique is proposed. In HB-MFM, the bimodal MFM is used, but the first resonance frequency of the cantilever is induced by the magnetic field of the ferromagnetic sample due to its vibrations caused by a piezoelectric element placed under the sample. The advantages of this new technique are demonstrated through the preliminary results obtained by HB-MFM on a hard disk sample. Additionally, traditional two pass MFM and HB-MFM measurements were compared.

Keywords: magnetic force microscopy, atomic force microscopy, magnetism, bimodal MFM

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Authors: Najme Lari, Shahrokh Ahangarani, Ali Shanaghi

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Sol-gel technology is a promising manufacturing method to produce anti reflective silica thin films for solar energy applications. So to improve the properties of the films, controlling parameter of the sol - gel method is very important. In this study, soaking treatment effect on optical properties of silica anti reflective thin films was investigated. UV-Visible Spectroscopy, Fourier-Transformed Infrared Spectrophotometer and Field Emission Scanning Electron Microscopy was used for the characterization of silica thin films. Results showed that all nanoporous silica layers cause to considerable reduction of light reflections compared with uncoated glasses. With single layer deposition, the amount of reduction depends on the dipping time of coating and has an optimal time. Also, it was found that solar transmittance increased from 91.5% for the bare slide up to 97.5% for the best made sample corresponding to two deposition cycles.

Keywords: sol–gel, silica thin films, anti reflective coatings, optical properties, soaking treatment

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Authors: Annu Sheokand, Vinay Kumar

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Hydrogen sulfide (H₂S) detection is essential for environmental monitoring and industrial safety due to its high toxicity, even at low concentrations. This study explores the H₂S gas sensing properties of Cu-doped Fe₂O₃ materials derived from metal-organic frameworks (MOFs), which offer high surface area and controlled porosity for optimized gas sensing. The structural and morphological characteristics of the synthesized material were thoroughly analyzed using techniques such as X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), and UV-Vis Spectroscopy. The resulting sensor exhibited remarkable sensitivity and selectivity, achieving a detection limit at the ppb level for H₂S. The study indicates that Cu doping significantly enhances the gas sensing performance of Fe₂O₃ by introducing abundant active sites within the material. These enhanced sensing properties emphasize the potential of MOF-derived Cu-doped Fe₂O₃ as a highly effective material for H₂S gas sensors in various applications.

Keywords: detection limit, doping, MOF, sensitivity, sensor

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Authors: Linlin Wang, Guangdong Bian, Jifeng Shen, Jingzhu Zeng

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Zinc-aluminum alloys have been applied as alternatives to bronze, aluminum alloys, and cast iron due to their distinguishing features such as high as-cast strength, excellent bearing properties, as well as low energy requirements for melting. In this study, oxide coatings were produced on ZA27 zinc-aluminum alloy by a plasma electrolytic oxidation (PEO) method. Three coatings were deposited by using three various electrolytes, i.e. silicate, aluminate and aluminate/borate composite solutions. The current density is set at 0.1A/cm2, deposition time is 40 mins for all the deposition processes. The surface morphology and phase structure of the three coatings were characterized by scanning electron microscopy （SEM） and X-ray diffraction (XRD). Pin-on-disc sliding wear tests were conducted to test the tribological properties of coatings. The results indicated that the coating produced using the aluminate/borate composite electrolyte had the highest deposition rate and best wear resistance among the three coatings.

Keywords: oxide coating, PEO, tribological properties, ZA27

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Authors: P. Gomathi Priya, M. E. Thenmozhi

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Iron nanoparticles were used to cleanup effluents. This paper involves synthesis of iron nanoparticles chemically by sodium borohydride reduction of ammonium ferrous sulfate solution (FAS). Iron oxide nanoparticles have lesser efficiency of adsorption than Zero Valent Iron nanoparticles (nZVI). Glucosamine acts as a stabilizing agent and chelating agent to prevent Iron nanoparticles from oxidation. nZVI particles were characterized using Scanning Electron Microscopy (SEM). Thus, the synthesized nZVI was subjected to entrapment in biopolymer, viz. barium (Ba)-alginate beads. The beads were characterized using SEM. Batch dye degradation studies were conducted using Reactive black Water soluble Nontoxic Natural substances (WNN) dye which is one of the most hazardous dyes used in textile industries. Effect of contact time, effect of pH, initial dye concentration, adsorbent dosage, isotherm and kinetic studies were carried out.

Keywords: ammonium ferrous sulfate solution, barium, alginate beads, reactive black WNN dye, zero valent iron nanoparticles

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Authors: Katia Ayouz-Chebout, Fatima Boudeffar, Maha Ayat, Malika Berouaken, Chafiaa Yaddaden, Saloua Merazga, Nouredine Gabouze

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Transition metal oxide composites have been widely reported in energy storage and conversion systems. In this regard, an attempt has been made to synthesize NiO@V₂O₅ nanocomposite. The structures and morphology of synthesized powder are investigated by X-ray diffraction, scanning electron microscope (SEM), and Attenuated Total Reflection (ATR). The electrochemical properties and performances as cathode electrodes based on active material NiO@V₂O₅ were studied by cyclic voltammetry (CV), between potential bias [0.01V to 3V], with scanning speed of 0,1mVs⁻¹, the galvanostatic charge/discharge (CDG) for 100 cycles was also measured.

Keywords: composite nanobelts, vanadium pentoxide, nickel oxide, Li-ion batteries

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Authors: Askar Kilmametov, Julia Ivanisenko, Boris Straumal, Horst Hahn

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The high-pressure α- to ω-phase transition was discovered in elemental Ti and Zr fifty years ago using static high pressure and then observed to appear between 2 and 12 GPa at room temperature, depending on the experimental technique, the pressure environment, and the sample purity. The fact that ω-phase is retained in a metastable state in ambient condition after the removal of the pressure has been used to check the changes in magnetic and superconductive behavior, electron band structure and mechanical properties. However, the fundamental knowledge on a combination of both mechanical treatment and high applied pressure treatments for ω-phase formation in Ti alloys is currently lacking and has to be studied in relation to improved mechanical properties of bulk nanostructured states. In the present study, nanostructured (α+β) Ti alloys containing β-stabilizing elements such as Co, Fe, Cr, Nb were performed by severe plastic deformation, namely high pressure torsion (HPT) technique. HPT-induced α- to ω-phase transformation was revealed in dependence on applied pressure and shear strains by means of X-ray diffraction, transmission electron microscopy, and differential scanning calorimetry. The transformation kinetics was compared with the kinetics of pressure-induced transition. Orientation relationship between α-, β- and ω-phases was taken into consideration and analyzed according to theoretical calculation proposed earlier. The influence of initial state before HPT appeared to be considerable for subsequent α- to ω-phase transition. Thermal stability of the HPT-induced ω-phase was discussed as well in the frame of mechanical behavior of Ti and Ti-based alloys produced by shear deformation under high applied pressure.

Keywords: bulk nanostructured materials, high pressure phase transitions, severe plastic deformation, titanium alloys

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Authors: A. Fernandez Zuvich, I. Gana Watkins, H. Zolotucho, H. Troiani, A. Caneiro, M. Prado, A. L. Soldati

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The study of actinide nanoparticles (NPs) has attracted the attention of the scientific community not only because the lack of information about their ecotoxicological effects but also because the use of NPs could open a new way in the production of nuclear energy. Indeed, it was recently demonstrated that UO2 NPs sintered pellets exhibit closed porosity with improved fission gas retention and radiation-tolerance , ameliorated mechanical properties, and less detriment of the thermal conductivity upon use, making them an interesting option for new nuclear fuels. In this work, we used a combination of diffraction and microscopy tools to characterize the morphology, the crystalline structure and the composition of UO2 nanoparticles doped with 10%wt Gd2O3. The particles were synthesized by a modified sol-gel method at low temperatures. X-ray Diffraction (XRD) studies determined the presence of a unique phase with the cubic structure and Fm3m spatial group, supporting that Gd atoms substitute U atoms in the fluorite structure of UO2. In addition, Field Emission Gun Scanning (FEG-SEM) and Transmission (FEG-TEM) Electron Microscopy images revealed the presence of micrometric agglomerates of nanoparticles, with rounded morphology and an average crystallite size < 50 nm. Energy Dispersive Spectroscopy (EDS) coupled to TEM determined the presence of Gd in all the analyzed crystallites. Besides, FEG-SEM-EDS showed a homogeneous concentration distribution at the micrometer scale indicating that the small size of the crystallites compensates the variation in composition by averaging a large number of crystallites. These techniques, as combined tools resulted thus essential to find out details of morphology and composition distribution at the sub-micrometer scale, and set a standard for developing and analyzing nanoparticulated nuclear fuels.

Keywords: actinide nanoparticles, burnable poison, nuclear fuel, sol-gel

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Authors: Maryam Kiani

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The aim of this study was to investigate the influence of nanoparticles additive on the properties of fly ash-based geopolymer. The geopolymer samples were prepared using fly ash as the primary source material, along with an alkali activator solution and different concentrations of carbon black additive. The effects of nanoparticles flexural strength, water absorption, and micro-structural properties of the cured samples. The results revealed that the inclusion of nanoparticles additive significantly enhanced the mechanical and electrical properties of the geopolymer binder. Micro-structural analysis using scanning electron microscopy (SEM) revealed a more compact and homogeneous structure in the geopolymer samples with nanoparticles. The dispersion of nanoparticles particles within the geopolymer matrix was observed, suggesting improved inter-particle bonding and increased density. Overall, this study demonstrates the positive impact of nanoparticles additive on the qualities of fly ash-based geopolymer, emphasizing its potential as an effective enhancer for geopolymer binder applications for the development of construction and infrastructure for energy buildings.

Keywords: fly-ash, geopolymer, energy buildings, nanotechnology

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Authors: Bhavesh D. Gajbhiye, Divya Raghunandanan, C. S. Sona, Channamallikarjun S. Mathpati

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Molten fluoride salt FLiNaK (LiF-NaF-KF: 46.5-11.5-42 mol %) is a promising candidate as high temperature coolant for next generation nuclear reactors due to its superior thermophysical properties. Corrosion of alloys in molten FLiNaK has however been recognized as a serious issue in the selection of structural materials. Corrosion experiments of alloys Inconel-625 (Fe-Ni alloy) and Hastelloy-B (Ni-Mo alloy) were performed in FLiNaK salt. The tests were carried out at a temperature of 650°C in graphite crucibles for 60 hours under inert atmosphere. Corrosion experiments were performed to study the effect of moisture removal in the salt by pre heating and vacuum drying. Weight loss of the alloy samples due to corrosion was measured and corrosion rate was estimated. The surface morphology of the alloy samples was analyzed by Scanning Electron Microscopy. A significant decrease in the corrosion rate was observed for the alloys studied in moisture removed salt.

Keywords: FLiNaK, hastelloy, inconel, weight loss

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Authors: Ghazi Faisal Najmuldeen, Noridah Abdullah, Mimi Sakinah

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Bioethanol is an alcohol made by fermentation, mostly from carbohydrates, Cellulosic biomass, derived from non-food sources, such as castor shell waste, is also being developed as a feedstock for ethanol production Cellulose extracted from biomass sources is considered the future feedstock for many products due to the availability and eco-friendly nature of cellulose. In this study, castor shell (CS) biowaste resulted from the extraction of Castor oil from castor seeds was evaluated as a potential source of cellulose. The cellulose was extracted after pretreatment process was done on the CS. The pretreatment process began with the removal of other extractives from CS, then an alkaline treatment, bleaching process with hydrogen peroxide, and followed by a mixture of acetic and nitric acids. CS cellulose was analysed by infrared absorption spectroscopy (FTIR), scanning electron microscopy (SEM), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). The result showed that the overall process was adequate to produce cellulose with high purity and crystallinity from CS waste. The cellulose was then hydrolyzed to produce glucose and then fermented to bioethanol.

Keywords: bioethanol, castor shell, cellulose, biowaste

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Authors: W. Handoko, F. Pahlevani, V. Sahajwalla

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Dual-phase high carbon steels (DHCS) are commonly known for their improved strength, hardness, and abrasive resistance properties due to co-presence of retained austenite and martensite at the same time. Retained austenite is a meta-stable phase at room temperature, and stability of this phase governs the response of DHCS at different conditions. This research paper studies the effect of RA stability on corrosion behaviour of high carbon steels after they have been immersed into 1.0 M NaCl solution for various times. For this purpose, two different steels with different RA stabilities have been investigated. The surface morphology of the samples before and after corrosion attack was observed by secondary electron microscopy (SEM) and atomic force microscopy (AFM), along with the weight loss and Vickers hardness analysis. Microstructural investigations proved the preferential attack to retained austenite phase during corrosion. Hence, increase in the stability of retained austenite in dual-phase steels led to decreasing the weight loss rate.

Keywords: high carbon steel, austenite stability, atomic force microscopy, corrosion

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Authors: M. Abdel-Hamid, P. Saporito, R. V. Mateiu, A. Osman, E. Romeih, H. Jenssen

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Camel milk whey (CMW) was hydrolyzed with papain from Carica papaya and fractionated by size exclusion chromatography (SEC). The antibacterial and anti-biofilm activity of the CMW, Camel milk whey hydrolysate (CMWH) and the obtained SEC-fractions was assessed against Pseudomonas aeruginosa and Methicillin-resistant Staphylococcus aureus (MRSA). SEC-F2 (fraction 2) exhibited antibacterial effectiveness against MRSA and P. aeruginosa with the minimum inhibitory concentration of 0.31 and 0.156 mg/ml, respectively. Furthermore, SEC-F2 significantly decreased biofilm biomass by 71% and 83 % for MRSA and P. aeruginosa in a crystal violet microplate assay. Scanning electron microscopy showed that the SEC-F2 caused changes in the treated bacterial cells. Additionally, LC/MS analysis was used to characterize the peptides of SEC-F2. Two major peptides were detected in SEC-F2 having masses of 414.05 Da and 456.06 Da. In conclusion, this study has demonstrated that hydrolysis of CMW with papain generates small and extremely potent antibacterial and anti-biofilm peptides against both MRSA and P. aeruginosa.

Keywords: camel milk, whey proteins, antibacterial peptide, anti-biofilm

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Authors: Mirijam Vrabec, Marian Janak, Bojan Ambrozic, Angelja K. Surca, Nastja Rogan Smuc, Nina Zupancic, Saso Sturm

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Natural microdiamonds and moissanite (SiC) can form during the orogenic events under ultrahigh-pressure metamorphic conditions (UHP), when parts of Earth’s crust are subducted to extreme depths. So far, such processes were identified only in few places on the Earth, and therefore, represent unique opportunity to study the evolution of the Earth’s deep interior. An important discovery of microdiamonds and moissanite was reported from Pohorje, (Slovenia), where they occurred as single or polyphase inclusions in garnets. Metasedimentary rocks from Pohorje are predominantly gneisses representing parts of the Austroalpine metamorphic units of the Eastern Alps. During Cretaceous orogeny, (ca. 95–92 Ma) continental crustal rocks were deeply subducted to the mantle depths (below 100 km) and metamorphosed at pressures exceeding 3.5 GPa and temperatures between 800–850 °C. Microstructural and phase analysis of the inclusions as well as detailed elemental analysis of host garnets were carried out combining several analytical techniques: optical microscope in plane polarized transmitted light, electron probe microanalysis (EPMA) with wavelength-dispersive x-ray spectrometry (WDS) and field-emission scanning microscope (FEG-SEM) with energy-dispersive x-ray spectroscopy (EDS). Micro-Raman analysis revealed sharp, first order diamond bands sometimes accompanied by graphite bands implying that transformation of diamond back to graphite occurred. To study the chemical and crystallographic relationship between microdiamonds and co-inclusions, advanced techniques of transmission electron microscopy (TEM) were applied, which included high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), combined with EDS and electron energy-loss spectroscopy (EELS). To prepare electron transparent TEM lamellae selectively a dual-beam Focused Ion Beam/SEM (FIB/SEM) was employed. Detailed study of TEM lamellae, which was cross-sectioned from the highly faceted inclusion body located within the host garnet crystal matrix, revealed rich and rather complex internal structure. Namely, the negative crystal facets of the main inclusion body were typically decorated with up to 1 μm thick amorphous layer, reflecting the general garnet composition with slight variations in Fe/Ca content. Within these layers, ELNES analysis revealed the presence of a 28–30 nm thick layer of amorphous carbon. The very last section of this layer corresponds to composition of SiO2. Within the inclusion, besides diamond and moissanite alumosilicate mineral with pronounced layered structure, iron sulfides and chlorine were identified under TEM and CO2 and CH4 using Raman. Moissanite is found as single crystal or composed from numerous highly textured nano-crystals with the average size of 10 nm. Moissanite inclusions were found embedded inside the amorphous crust implying that moissanite crystalized well before the deposition of the amorphous layer. From the microstructural, crystallographic and chemical observations so far we can deduce, that polyphase inclusions in diamond bearing garnets from Pohorje most probably crystallized from reduced supercritical fluids. Based on layered interface structure of the host mineral multiphase process of crystallization is possible. The presence of microdiamonds and moissanite in rocks from Pohorje demonstrates that these parts of the Eastern Alps were subducted to extreme depths, and were subsequently exhumed back to the Earth's surface without complete breakdown of UHP mineral phases, allowing a rear and exceptional opportunity to study them in-situ.

Keywords: diamond, fluid inclusions, moissanite, TEM, UHP metamorphism.

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Authors: Anastasia Beketova, Emmanouil-George C. Tzanakakis, Ioannis G. Tzoutzas, Eleana Kontonasaki

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In restorative dentistry, yttria-stabilized zirconia (YSZ) nanoparticles can be applied as fillers to improve the mechanical properties of various resin-based materials. Using sol-gel based synthesis as simple and cost-effective method, nano-sized YSZ particles with high purity can be produced. The aim of this study was to synthesize YSZ nanoparticles by the Pechini sol-gel method at different temperatures and to investigate their composition, structure, and morphology. YSZ nanopowders were synthesized by the sol-gel method using zirconium oxychloride octahydrate (ZrOCl₂.8H₂O) and yttrium nitrate hexahydrate (Y(NO₃)₃.6H₂O) as precursors with the addition of acid chelating agents to control hydrolysis and gelation reactions. The obtained powders underwent TG_DTA analysis and were sintered at three different temperatures: 800, 1000, and 1200°C for 2 hours. Their composition and morphology were investigated by Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction Analysis (XRD), Scanning Electron Microscopy with associated with Energy Dispersive X-ray analyzer (SEM-EDX), Transmission Electron Microscopy (TEM) methods, and Dynamic Light Scattering (DLS). FTIR and XRD analysis showed the presence of pure tetragonal phase in the composition of nanopowders. By increasing the calcination temperature, the crystallinity of materials increased, reaching 47.2 nm for the YSZ1200 specimens. SEM analysis at high magnifications and DLS analysis showed submicron-sized particles with good dispersion and low agglomeration, which increased in size as the sintering temperature was elevated. From the TEM images of the YSZ1000 specimen, it can be seen that zirconia nanoparticles are uniform in size and shape and attain an average particle size of about 50 nm. The electron diffraction patterns clearly revealed ring patterns of polycrystalline tetragonal zirconia phase. Pure YSZ nanopowders have been successfully synthesized by the sol-gel method at different temperatures. Their size is small, and uniform, allowing their incorporation of dental luting resin cements to improve their mechanical properties and possibly enhance the bond strength of demanding dental ceramics such as zirconia to the tooth structure. This research is co-financed by Greece and the European Union (European Social Fund- ESF) through the Operational Programme 'Human Resources Development, Education and Lifelong Learning 2014- 2020' in the context of the project 'Development of zirconia adhesion cements with stabilized zirconia nanoparticles: physicochemical properties and bond strength under aging conditions' (MIS 5047876).

Keywords: dental cements, nanoparticles, sol-gel, yttria-stabilized zirconia, YSZ

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Authors: Rudolf L. Kanyane, Nicolaus Malatji, Patritia A. Popoola

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Tribological failure of materials during application can lead to catastrophic events which also carry economic penalties. High entropy alloys (HEAs) have shown outstanding tribological properties in applications such as mechanical parts were moving parts under high friction are required. This work aims to investigate the effect of sintering temperature on microhardness properties and tribological properties of novel equiatomic TiAlMoSiW HEAs fabricated via spark plasma sintering. The effect of Spark plasma sintering temperature on morphological evolution and phase formation was also investigated. The microstructure and the phases formed for the developed HEAs were examined using scanning electron microscopy (SEM) and X-ray diffractometry (XRD) respectively. The microhardness and tribological properties were studied using a diamond base microhardness tester Rtec tribometer. The developed HEAs showed improved mechanical properties as the sintering temperature increases.

Keywords: sintering, high entropy alloy, microhardness, tribology

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Authors: Adrian Travieso Disotuar, J. Antonio Travieso Rodriguez, Ramon Jerez Mesa, Montserrat Vilaseca

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The effect of the non-vibration-assisted and vibration-assisted ball burnishing on both the surface and mechanical properties of C300 obtained by Selective Laser Melting additive manufacturing technology is studied in this paper. Different vibration amplitudes preloads, and burnishing strategies were tested. A topographical analysis was performed to determine the surface roughness of the different conditions. Besides, micro tensile tests were carried out in situ on Scanning Electron Microscopy to elucidate the post-treatment effects on damaging mechanisms. Experiments show that vibration-assisted ball burnishing significantly enhances mechanical properties compared to the non-vibration-assisted method. Moreover, it was found that the surface roughness was significantly improved with respect to the reference surface.

Keywords: additive manufacturing, ball burnishing, mechanical properties, metals, surface roughness

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Authors: Charles Klein O. Gorit, Mark Tristan J. Quimque Jr., M. Cecilia V. Almeda, Concepcion M. Salvana

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Chitosan is a promising biopolymer commonly found in crustacean shells that has plausible effects in water purification and wastewater treatment. It is a primary derivative of chitin and considered second of the most abundant biopolymer prior to cellulose. Morphological analysis had been done using Scanning Electron Microscopy with Energy Dispersive Microscopy (SEM/EDS), and due to its porous nature, it showcases a certain degree of porosity, hence, larger adsorption site of heavy metal. The Energy Dispersive Spectroscopy of the chitosan and ‘lead-bound’ chitosan, shows a relative increase of percent abundance of lead cation from 1.44% to 2.08% hence, adsorption occurs. Chitosan, as a nitrogenous polysaccharide, subjected to Fourier transform infrared spectroscopy (FTIR) analysis shows amide bands ranging from 1635.36 cm⁻¹ for amide 1 band and 1558.40 cm-1 for amide 2 band with NH stretching. For ‘lead-bound’ chitosan, the FT-IR analysis shows a change in peaks upon adsorption of Pb(II) cation. The spectrum shows broadening of OH and NH stretching band. Such observation can be attributed to the probability that the attachment of Pb(II) ions is in these functional groups. A column filter was devised with lead-bound chitosan to determine the zero point charge (pHzpc) of the biopolymer. The results show that at pH 8.34, below than the zpc level of literatures cited for lead which ranges from pH 4 to 7, favors the adsorption site of chitosan and its capability to adsorb traces amount of aqueous lead.

Keywords: chitosan, biopolymer, FT-IR, SEM, zero-point charge, heavy metal, lead ions

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Authors: Mohamed E. Harb, Enas Moustafa, Shaker Ebrahim, Moataz Soliman

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In this paper pressure detectors were synthesized and characterized using hybrid perovskite/PVDF composites as an active layer. Methylammonium lead iodide (MAPbI₃) was synthesized from methylammonium iodide (MAI) (CH₃NH₃I) and lead iodide (PbI₂). Composites of perovskite/PVDF using different weight ratio were prepared as the active material. PVDF with weights percentages of 6%, 8%, and 10% was used. All prepared materials were investigated by x-ray diffraction (XRD), Fourier transforms infrared spectrum (FTIR) and scanning electron microscopy (SEM). A Versastat 4 Potentiostat Galvanostat instrument was used to perform the current-voltage characteristics of the fabricated sensors. The pressure sensors exhibited a voltage increase with applying different forces. Also, the current-voltage characteristics (CV) showed different effects with applying forces. So, the results showed a good pressure sensing performance.

Keywords: perovskite semiconductor, hybrid perovskite, PVDF, Pressure sensing

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Authors: Ismail Seckin Cardakli, Mustafa Engin Kocadagistan, Ersin Arslan

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In this study, mechanochemical behaviour of aluminium - boron oxide - melamine ternary system was investigated by high energy ball milling. According to the reaction Al + B₂O₃ = Al₂O₃ + B, stochiometric amount of aluminium and boron oxide with melamine up to ten percent of total weight was used in the experiments. The powder characterized by X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy (SEM) after leaching of product by 1M HCl acid. Results show that mechanically induced self-sustaining reaction (MSR) between aluminium and boron oxide takes place after four hours high energy ball milling. Al₂O₃/h-BN composite powder is obtained as the product of aluminium - boron oxide - melamine ternary system.

Keywords: high energy ball milling, hexagonal boron nitride, mechanically induced self-sustaining reaction, melamine

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Authors: Mohamed A. Deyab, Ahmed E. Awadallah

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Under various conditions, we present a promising method for producing pure hydrogen energy from the electrochemical reaction of Mg metal in waste oilfield water (WOW). Mg metal and WOW are primarily consumed in this process. The results show that the hydrogen gas output is highly dependent on temperature and solution pH. The best conditions for hydrogen production were found to be a low pH (2.5) and a high temperature (338 K). For the first time, the Allyl methylimidazolium bis-trifluoromethyl sulfonyl imide) (IL) ionic liquid is used to regulate the rate of hydrogen generation. It has been confirmed that increasing the solution temperature and decreasing the solution pH accelerates Mg dissolution and produces more hydrogen per unit of time. The adsorption of IL on the active sites of the Mg surface is unrestricted by mixing physical and chemical orientation. Inspections using scanning electron microscopy (SEM), energy dispersive X-ray (EDX), and FT-IR spectroscopy were used to identify and characterise surface corrosion of Mg in WOW. This process is also completely safe and can create energy on demand.

Keywords: hydrogen production, Mg, wastewater, ionic liquid

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Authors: Mahdi Amne Elahi, Marcus Koch, Peter Plapper

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Due to the demand of miniaturizing in automotive industry, the application of laser welding is quite promising. The current study focused on laser micro-welding of CuSn6 bronze and nickel wire for a miniature electromechanical hybrid component. Due to the advantages of laser welding, the welding can be tailored specifically for the requirements of the part. Scanning electron and optical microscopy were implemented to study the microstructure and tensile-shear test was selected to represent the mechanical properties. Different welding sides, beam oscillations, and speeds have been investigated to optimize the tensile-shear load and microstructure. The results show that the mechanical properties and microstructure of the joint is highly under the influence of the mentioned parameters. Due to the lack of intermetallic compounds, the soundness of the joint is achievable by manipulating the geometry of the weld seam and minimize weld defects.

Keywords: bronze, laser micro-welding, microstructure, nickel, tensile shear test

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Authors: S. Gvazava, N. Khidasheli, V. Tediashvili, M. Donadze

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The work presented in this paper studied the of austempered ductile iron (ADI) with different combinations of structural composition (upper bainite, lower bainite, retained austenite) in rainwater. A range of structural states of the metal matrix was obtained by changing the regimes of thermal treantments of a high-strength cast iron. The specimens were austenised at 900 0C for 30, 60, 90, 120 minutes. Afterwards, isothermal quenching was performed at 280 and 400 0C for40 seconds. The study was carried out using weight-change (WC), cyclic potentiodynamic polarization (CPP), open-circuit potential (OCP), and electrochemical impedance spectroscopy (EIS) measurements and complemented by scanning electron microscopy (SEM-EDS). According to the results, corrosion resistance of the boron microallyedbainitic ADI greatly depends on the type of the bainitic matrix and the amount of the retained austenite, which is driven by diffusion permeability of interphase and intergrain boundaries.

Keywords: austempered ductile iron, corrosion behaviour, retained austenite, corrosion rate, interphase boundary, upper bainite, lower bainite

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Authors: Fadwa Jewilli

Abstract:

A sudden leak of a 6-inch gas line pipe after being in service for one year was observed. The pipe had been designed to transport dry gas. The failure had taken place in 6 o’clock position at the stage discharge of the flow process. Laboratory investigations were conducted to find out the cause of the pipe rupture. Visual and metallographic observations confirmed that the pipe split was due to a crack initiated in circumferential and then turned into longitudinal direction. Sever wall thickness reduction was noticed on the internal pipe surface. Scanning electron microscopy observations at the fracture surface revealed features of ductile fracture mode. Corrosion product analysis showed the traces of iron carbonate and iron sulphate. The laboratory analysis resulted in the conclusion that the pipe failed due to the effect of wet fluid (condensate) caused severe wall thickness dissolution resulted in pipe could not stand the continuation at in-service working condition.

Keywords: gas line pipe, corrosion prediction ductile fracture, ductile fracture, failure analysis

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Authors: Mauricio Gómez, Esmeralda López, Ian Becar, Jaime Pizarro, Paula A. Zapata

Abstract:

A biodegradable material is developed with adsorptive capacity for metals ion for intended use in mining tailings mitigating the environmental impact with economic retribution, two types of fibers were elaborated by electrospinning: (1) a cellulose acetate (CA) matrix and (2) a cellulose acetate (CA)/chitosan (CH) matrix evaluating the effect of CH in CA on its physicochemical properties. Through diffuse reflectance infrared fourier transform spectroscopy (DRIFTS) the incorporation of chitosan in the matrix was identified, observing the band of the amino group at 1500 - 1600 [cm-1]. By scanning electron microscopy (SEM), Hg porosimetry, and CO2 isotherm at 273 [K], the intrafiber microporosity and interfiber macroporosity were identified, with an increase in the distribution of macropores for CA/CH fibers. In the tensile test, CH into the matrix produces a more ductile and tenacious behavior, where the % elongation at break increased by 33% with the other parameters constant. Thermal analysis by differential scanning calorimetry (DSC) and Thermogravimetric Analysis (TGA) showed that the incorporation of chitosan produces higher retention of water molecules due to the functional groups (amino groups (- NH3)), but there is a decrease in the specific heat and thermoplastic properties of the matrix since the glass transition temperature and softening temperature disappear. The effect of the optimum pH for CA and CA/CH fibers were studied in a batch system. In the adsorption kinetic study, the best isotherm model adapted to the experimental results corresponds to the Sips model and the kinetics corresponds to pseudo-second order

Keywords: environmental materials, wastewater treatment, electrospun fibers, biopolymers (cellulose acetate/chitosan), metals recovery

Procedia PDF Downloads 80

Authors: Preshanthan Moodley, E. B. Gueguim-Kana

Abstract:

The objective of this study was to develop a method to pretreat sugarcane leaf waste using microwave-assisted (MA) inorganic salt. The effects of process parameters of salt concentration, microwave power intensity and pretreatment time on reducing sugar yield from enzymatically hydrolysed sugarcane leaf waste were investigated. Pretreatment models based on MA-NaCl, MA-ZnCl2 and MA-FeCl3 were developed. Maximum reducing sugar yield of 0.406 g/g was obtained with 2 M FeCl3 at 700W for 3.5 min. Scanning electron microscopy (SEM) and Fourier Transform Infrared analysis (FTIR) showed major changes in lignocellulosic structure after MA-FeCl3 pretreatment with 71.5 % hemicellulose solubilization. This pretreatment was further assessed on sorghum leaves and Napier grass under optimal MA-FeCl3 conditions. A 2 fold and 3.1-fold increase in sugar yield respectively were observed compared to previous reports. This pretreatment was highly effective for enhancing enzymatic saccharification of lignocellulosic biomass.

Keywords: acid, pretreatment, salt, sugarcane leaves

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Authors: T. Aldeeb, M. Abduelmula

Abstract:

This study examines the fatigue life of S275 mild steel at room temperature. Mechanical components can fail under cyclic loading during period of time, known as the fatigue phenomenon. In order to prevent fatigue induced failures, material behavior should be investigated to determine the endurance limit of the material for safe design and infinite life, thus leading to reducing the economic cost and loss in human lives. The fatigue behavior of S275 mild steel was studied and investigated. Specimens were prepared in accordance with ASTM E3-11, and fatigue tests of the specimen were conducted in accordance with ASTM E466-07 on a smooth plate, with a continuous radius between ends (hourglass-shaped plate). The method of fatigue testing was applied with constant load amplitude and constant frequency of 4 Hz with load ratio (Fully Reversal R= -1). Surface fractures of specimens were investigated using Scanning Electron Microscope (SEM). The experimental results were compared with the results of a Finite Element Analysis (FEA), using simulation software. The experiment results indicated that the endurance fatigue limit of S275 mild steel was 195.47 MPa.

Keywords: fatigue strength, fatigue life, finite element analysis(FEA), S275 mild steel, scanning electron microscope (SEM)

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Authors: Pooria Pasbakhsh, Rangika T. De Silva, Vahdat Vahedi, Hanafi Ismail

Abstract:

The influence of three different types of halloysite nanotubes (HNTs) with different dimensions, namely as camel lake (CLA), Jarrahdale (JA) and Matauri Bay (MB), on their reinforcing ability of ethylene propylene dine monomer (EPDM) were investigated by varying the HNTs loading (from 0-15 phr). Mechanical properties of the nanocomposites improved with addition of all three HNTs, but CLA based nanocomposites exhibited a significant enhancement compared to the other HNTs. For instance, tensile properties of EPDM nanocomposites increased by 120%, 256% and 340% for MB, JA, and CLA, respectively with addition of 15 phr of HNTs. This could be due to the higher aspect ratio and higher surface area of CLA compared to others. Scanning electron microscopy (SEM) of nanocomposites at 15 phr of HNT loadings showed low amounts of pulled-out nanotubes which confirmed the presence of more embedded nanotubes inside the EPDM matrix, as well as aggregates within the fracture surface of EPDM/HNT nanocomposites.

Keywords: aspect ratio, halloysite nanotubes (HNTs), mechanical properties, rubber/clay nanocomposites

Procedia PDF Downloads 375

Authors: Iannello G., Coppa F., Pennisi S., Giuffrida G., Lo Faro R., Cartelli S., Ferruggia G., Brundo M. V.

Abstract:

Skin is the largest multifunctional human organ and possesses a complex, multilayered structure with the ability to regenerate and renew. The key role in skin regeneration is played by fibroblasts, which also occupy an important role in the wound healing process. Different methods, including dynamic light scattering, scanning electron microscopy, ELISA, and MTT assay, were employed to evaluate on fibroblasts the in vitro effects of plant-derived nanovesicles and cord blood stem cells‐derived exosomes. We compared the results with those of cells exposed to a technology called AMPLEX PLUS, containing a mixture of 20 different biologically active factors (GF20) and exosomes isolated and purified from bovine colostrum. AMPLEX PLUS was able to significantly enhance the cell proliferation status of cells at both 24 and 48 hours compared to untreated cells (control). The obtained results suggest how AMPLEX PLUS could be potentially effective in treating skin rejuvenation.

Keywords: AMPLEX PLUS, cell vitality, colostrum, nanovesicles

Procedia PDF Downloads 39