Search results for: Scanning electron microscopy

Authors: Amna Abdalla Mohammed Khalid, Pietro Parisse, Silvia Onesti, Loredana Casalis

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Basic cellular processes as DNA replication are crucial to cell life. Understanding at the molecular level the mechanisms that govern DNA replication in proliferating cells is fundamental to understand disease connected to genomic instabilities, as a genetic disease and cancer. A key step for DNA replication to take place, is unwinding the DNA double helix and this carried out by proteins called helicases. The archaeal MCM (minichromosome maintenance) complex from Methanothermobacter thermautotrophicus have being studied using Atomic Force Microscopy (AFM), imaging in air and liquid (Physiological environment). The accurate analysis of AFM topographic images allowed to understand the static conformations as well the interaction dynamic of MCM and DNA double helix in the present of ATP.

Keywords: DNA, protein-DNA interaction, MCM (mini chromosome manteinance) complex, atomic force microscopy (AFM)

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Authors: A. Kabir, D. Boulainine, I. Bouanane, N. Benslim, B. Boudjema, C. Sedrati

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SnO₂ is an n-type semiconductor with a direct gap of about 3.6 eV. It is largely used in several domains such as nanocrystalline photovoltaic cells. Due to its interesting physic-chemical properties, this material was elaborated in thin film forms using different deposition techniques. It was found that SnO₂ properties were directly affected by the deposition method parameters. In this work, the RGTO method (Rheotaxial Growth and Thermal Oxidation) was used to deposit elaborate SnO₂ thin films. This technique consists on thermal oxidation of the Sn films deposited onto a substrate heated to a temperature close to Sn melting point (232°C). Such process allows the preparation of high porosity tin oxide films which are very suitable for the gas sensing. The films structural, morphological and optical properties pre and post thermal oxidation were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-Visible spectroscopy and Fourier transform infrared spectroscopy (FTIR) respectively. XRD patterns showed a polycrystalline structure of the cassiterite phase of SnO₂. The grain growth was found affected by the oxidation temperature. This grain size evolution was confronted to existing grain growth models in order to understand the growth mechanism. From SEM images, the as deposited Sn film was formed of difference diameter spherical agglomerations. As a function of the oxidation temperature, these spherical agglomerations shape changed due to the introduction of oxygen ions. The deformed spheres started to interconnect by forming bridges between them. The volume porosity, determined from the UV-Visible reflexion spectra, Changes as a function of the oxidation temperature. The variation of the crystalline fraction, determined from FTIR spectra, correlated with the variation of both the grain size and the volume porosity.

Keywords: tin oxide, RGTO, grain growth, volume porosity, crystalline fraction

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Authors: Athina Puype, Lorenzo Malerba, Nico De Wispelaere, Roumen Petrov, Jilt Sietsma

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Reduced Activation Ferritic/Martensitic (FM) steels like EUROFER are of interest for first wall application in the future demonstration (DEMO) fusion reactor. Depending on the final design codes for the DEMO reactor, the first wall material will have to function in low-temperature mode or high-temperature mode, i.e. around 250-300°C of above 550°C respectively. However, the use of RAFM steels is limited up to a temperature of about 550°C. For the low-temperature application, the material suffers from irradiation embrittlement, due to a shift of ductile-to-brittle transition temperature (DBTT) towards higher temperatures upon irradiation. The high-temperature response of the material is equally insufficient for long-term use in fusion reactors, due to the instability of the matrix phase and coarsening of the precipitates at prolonged high-temperature exposure. The objective of this study is to investigate the influence of thermal ageing for 1000 hrs and 4000 hrs on microstructural features and mechanical properties of lab-cast EUROFER. Additionally, the ageing behavior of the lab-cast EUROFER is compared with the ageing behavior of standard EUROFER97-2 and T91. The microstructural features were investigated with light optical microscopy (LOM), electron back-scattered diffraction (EBSD) and transmission electron microscopy (TEM). Additionally, hardness measurements, tensile tests at elevated temperatures and Charpy V-notch impact testing of KLST-type MCVN specimens were performed to study the microstructural features and mechanical properties of four different F/M grades, i.e. T91, EUROFER97-2 and two lab-casted EUROFER grades. After ageing for 1000 hrs, the microstructures exhibit similar martensitic block sizes independent on the grain size before ageing. With respect to the initial coarser microstructures, the aged microstructures displayed a dislocation structure which is partially fragmented by polygonization. On the other hand, the initial finer microstructures tend to be more stable up to 1000hrs resulting in similar grain sizes for the four different steels. Increasing the ageing time to 4000 hrs, resulted in an increase of lath thickness and coarsening of M23C6 precipitates leading to a deterioration of tensile properties.

Keywords: ageing experiments, EUROFER, ferritic/martensitic steels, mechanical properties, microstructure, T91

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Authors: A. Chiker, A. Benamor, A. Haddad, Y. Hadji, M. Hadji

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Metal matrix composites (MMCs) have been of big interest for a few decades. Their major drawback lies in their enhanced mechanical performance over unreinforced alloys. They found ground in many engineering fields, such as aeronautics, aerospace, automotive, and other structural applications. One of the most used alloys as a matrix is nickel alloys, which meet the need for high-temperature mechanical properties; some attempts have been made to develop nickel base composites reinforced by high melt point and high modulus particulates. Among the carbides used as reinforcing particulates, chromium carbide is interesting for wear applications; it is widely used as a tribological coating material in high-temperature applications requiring high wear resistance and hardness. Moreover, a set of properties make it suitable for use in MMCs, such as toughness, the good corrosion and oxidation resistance of its three polymorphs -the cubic (Cr23C6), the hexagonal (Cr7C3), and the orthorhombic (Cr3C2)-, and it’s coefficient of thermal expansion that is almost equal to that of metals. The in-situ synthesis of CrC-reinforced Ni matrix composites could be achieved by the powder metallurgy route. To ensure the in-situ reactions during the sintering process, the use of phase precursors is necessary. Recently, new precursor materials have been proposed; these materials are called MAX phases. The MAX phases are thermodynamically stable nano-laminated materials displaying unusual and sometimes unique properties. These novel phases possess Mn+1AXn chemistry, where n is 1, 2, or 3, M is an early transition metal element, A is an A-group element, and X is C or N. Herein, the pressureless sintering method is used to elaborate Ni/Cr2AlC composites. Four composites were elaborated from 5, 10, 15 and 20 wt% of Cr2AlC MAX phase precursor which fully reacted with Ni-matrix at 1100 °C sintering temperature for 4 h in argon atmosphere. XRD results showed that Cr2AlC MAX phase was totally decomposed forming chromium carbide Cr7C3, and the released Al and Cr atoms diffused in Ni matrix giving rise to γ-Ni(Al,Cr) solid solution and γ’-Ni3(Al,Cr) intermetallic. Scanning Electron Microscopy (SEM) of the elaborated samples showed the presence of nanosized Cr7C3 reinforcing particles embedded in the Ni metal matrix, which have a direct impact on the tribological properties of the composites and their hardness. All the composites exhibited higher hardness than pure Ni; whereas adding 15 wt% of Cr2AlC gives the highest hardness (1.85 GPa). Using a ball-on-disc tribometer, dry sliding tests for the elaborated composites against 100Cr6 steel ball were studied under different applied loads. The microstructures and worn surface characteristics were then analyzed using SEM and Raman spectroscopy. The results show that all the composites exhibited better wear resistance compared to pure Ni, which could be explained by the formation of a lubricious tribo-layer during sliding and the good bonding between the Ni matrix and the reinforcing phases.

Keywords: composites, microscopy, sintering, wear

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Authors: H. Aripin, I. Made Joni, Edvin Priatna, Nundang Busaeri, Svilen Sabchevski

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In this investigation, manganese has been produced from medium grade manganese ore from Karangnunggal mine (West Java, Indonesia). The ores were grinded using a jar mill to pass through a 150 mesh sieve. The effects of keeping it at a temperature of 1200 °C in methane gas on the structural properties have been studied. The material’s properties have been characterized on the basis of the experimental data obtained using X-ray fluorescence (XRF), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), and Fourier transform infrared (FTIR) spectroscopy. It has been found that the ore contains MnO₂ as the main constituents at about 46.80 wt.%. It can be also observed that the ore particles are agglomerated forming dense grains with different texture and morphology. The irregular-shaped grains with dark contrast, the large brighter grains, and smaller grains with bright texture and smooth surfaces are associated with the presence of manganese, calcium, and quartz, respectively. From XRD patterns, MnO₂ is reduced to hausmannite (Mn₃O₄), manganosite (MnO) and manganese carbide (Mn₇C₃). At a temperature of 1200°C the keeping time does not have any effect on the formation of crystals and the crystalline phases remain almost unchanged in the time range from 15 to 90 minutes. An increase of the keeping time up to 45 minutes during the sintering process leads to an increase of the MnO concentration, while at 90 minutes, the concentration decreases. At longer keeping times the excess reaction of the methane gas and manganese oxide in the ore causes an increase of carbon deposition. As a result, it blocks the particle surface and then hinders the reduction process of manganese oxide. From FTIR spectrum allows one to explain that the appearance of C=O stretching mode arises from absorption of atmospheric methane and manganese oxide of the ore. The intensity of this band increases with increasing the keeping time, indicating an increase of carbon deposition on the surface of manganese oxide.

Keywords: manganese, medium grade manganese ore, structural properties, keeping the temperature, carbon deposition

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Authors: Varun A Baheti, Sanjay Kashyap, Kamanio Chattopadhyay, Praveen Kumar, Aloke Paul

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Ni–Sn system finds applications in the microelectronics industry, especially with respect to flip–chip or direct chip, attach technology. Here the region of interest is under bump metallization (UBM), and solder bump (Sn) interface due to the formation of brittle intermetallic phases there. Understanding the growth of these phases at UBM/Sn interface is important, as in many cases it controls the electro–mechanical properties of the product. Cu and Ni are the commonly used UBM materials. Cu is used for good bonding because of fast reaction with solder and Ni often acts as a diffusion barrier layer due to its inherently slower reaction kinetics with Sn–based solders. Investigation on the growth kinetics of phases in Ni–Sn system is reported in this study. Just for simplicity, Sn being major solder constituent is chosen. Ni–Sn electroplated diffusion couples are prepared by electroplating pure Sn on Ni substrate. Bulk diffusion couples prepared by the conventional method are also studied along with Ni–Sn electroplated diffusion couples. Diffusion couples are annealed for 25–1000 h at 50–215°C to study the phase evolutions and growth kinetics of various phases. The interdiffusion zone was analysed using field emission gun equipped scanning electron microscope (FE–SEM) for imaging. Indexing of selected area diffraction (SAD) patterns obtained from transmission electron microscope (TEM) and composition measurements done in electron probe micro−analyser (FE–EPMA) confirms the presence of various product phases grown across the interdiffusion zone. Time-dependent experiments indicate diffusion controlled growth of the product phase. The estimated activation energy in the temperature range 125–215°C for parabolic growth constants (and hence integrated interdiffusion coefficients) of the Ni₃Sn₄ phase shed light on the growth mechanism of the phase; whether its grain boundary controlled or lattice controlled diffusion. The location of the Kirkendall marker plane indicates that the Ni₃Sn₄ phase grows mainly by diffusion of Sn in the binary Ni–Sn system.

Keywords: diffusion, equilibrium phase, metastable phase, the Ni-Sn system

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Authors: Soad Ali Yehia, Mohamed Shafik El-Ridi, Mina Ibrahim Tadros, Nolwa Gamal El-Sherif

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Fexofenadine hydrochloride (FXD) is a slightly soluble, bitter-tasting, drug having an oral bioavailability of 35%. The maximum plasma concentration is reached 2.6 hours (Tmax) post-dose. The current work aimed to develop taste-masked FXD orodispersible tablets (ODTs) to increase extent of drug absorption and reduce Tmax. Taste masking was achieved via solid dispersion (SD) with chitosan (CS) or sodium alginate (ALG). FT-IR, DSC and XRD were performed to identify physicochemical interactions and FXD crystallinity. Taste-masked FXD-ODTs were developed via addition of superdisintegrants (crosscarmelose sodium or sodium starch glycolate, 5% and 10%, w/w) or sublimable agents (camphor, menthol or thymol; 10% and 20%, w/w) to FXD-SDs. ODTs were evaluated for weight variation, drug-content, friability, wetting time, disintegration time and drug release. Camphor-based (20%, w/w) FXD-ODT (F12) was optimized (F23) by incorporation of a more hydrophilic lubricant, sodium stearyl fumarate (Pruv®). The topography of the latter formula was examined via scanning electron microscopy (SEM). The in vivo estimation of FXD pharmacokinetics, relative to Allegra® tablets, was evaluated in healthy human volunteers. Based on the gustatory sensation test in healthy volunteers, FXD:CS (1:1) and FXD:ALG (1:0.5) SDs were selected. Taste-masked FXD-ODTs had appropriate physicochemical properties and showed short wetting and disintegration times. Drug release profiles of F23 and phenylalanine-containing Allegra® ODT were similar (f2 = 96) showing a complete release in two minutes. SEM micrographs revealed pores following camphor sublimation. Compared to Allegra® tablets, pharmacokinetic studies in healthy volunteers proved F23 ability to increase extent of FXD absorption (14%) and reduce Tmax to 1.83 h.

Keywords: fexofenadine hydrochloride, taste masking, chitosan, orodispersible

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Authors: Jin Lin, Shouxiang Lu, Kim Meow Liew

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In a fire accident, fire smoke often poses a serious threat to human safety especially in the enclosed space such as submarine and space-crafts environment. Efficient removal of the hazardous gas products particularly a large amount of CO and CO₂ gases from these confined space is critical for the security of the staff and necessary for the post-fire environment recovery. In this work, Cu-Mn-Ce composite oxide catalysts coupled with CO₂ sorbents were prepared using wet impregnation method, solid-state impregnation method and wet/solid-state impregnation method. The as-prepared samples were tested dynamically and isothermally for CO oxidation and CO₂ sorption and further characterized by the X-ray diffraction (XRD), nitrogen adsorption and desorption, and field emission scanning electron microscopy (FE-SEM). The results showed that all the samples were able to catalyze CO into CO₂ and capture CO₂ in situ by chemisorption. Among all the samples, the sample synthesized by the wet/solid-state impregnation method showed the highest catalytic activity toward CO oxidation and the fine ability of CO₂ sorption. The sample prepared by the solid-state impregnation method showed the second CO oxidation performance, while the coupled sample using the wet impregnation method exhibited much poor CO oxidation activity. The various CO oxidation and CO₂ sorption properties of the samples might arise from the different dispersed states of the CO₂ sorbent in the CO catalyst, owing to the different preparation methods. XRD results confirmed the high-dispersed sorbent phase in the samples prepared by the wet and solid impregnation method, while that of the sample prepared by wet/solid-state impregnation method showed the larger bulk phase as indicated by the high-intensity diffraction peaks. Nitrogen adsorption and desorption results further revealed that the latter sample had a higher surface area and pore volume, which were beneficial for the CO oxidation over the catalyst. Hence, the Cu-Mn-Ce oxide catalyst coupled with CO₂ sorbent using wet/solid-state impregnation method could be a good choice for fire smoke removal in the enclosed space.

Keywords: CO oxidation, CO₂ sorption, preparation methods, smoke removal

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Authors: M. Ertas, A. C. Onel, G. Ekinci, B. Toydemir, S. Durdu, M. Usta, L. Colakerol Arslan

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To develop AZ91D magnesium alloys with improved properties, we have applied TiN and VN/TiN multilayer coatings using DC magnetron sputter technique. Coating structure, surface morphology, chemical bonding and corrosion resistance of coatings were analyzed by x-ray diffraction (XRD), scanning electron microscope (SEM), x-ray photoelectron spectroscopy (XPS), and tafel extrapolation method, respectively. XPS analysis reveal that VN overlayer reacts with oxygen at the VN/TiN interface and forms more stable TiN layer. Morphological investigations and the corrosion results show that VN/TiN multilayer thin film coatings are quite effective to optimize the corrosion resistance of Mg alloys.

Keywords: AZ91D Mg alloys, high corrosion resistance, transition metal nitride coatings, magnetron sputter

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Authors: Meera A. Albloushi, Adel B. Gougam

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The development in the field of piezoelectrics has led to a renewed interest in ZnO nanowires (NWs) as a promising material in the nanogenerator devices category. It can be used as a power source for self-powered electronic systems with higher density, higher efficiency, longer lifetime, as well as lower cost of fabrication. Highly aligned ZnO nanowires seem to exhibit a higher performance compared with nonaligned ones. The purpose of this study was to develop ZnO nanowires and to investigate their electrical and chemical properties for various applications. They were grown on silicon (100) and glass substrates. We have used a low temperature and non-hazardous method: aqueous chemical growth (ACG). ZnO (non-doped) and AZO (Aluminum doped) seed layers were deposited using RF magnetron sputteringunder Argon pressure of 3 mTorr and deposition power of 180 W, the times of growth were selected to obtain thicknesses in the range of 30 to 125 nm. Some of the films were subsequently annealed. The substrates were immersed tilted in an equimolar solution composed of zinc nitrate and hexamine (HMTA) of 0.02 M and 0.05 M in the temperature range of 80 to 90 ᵒC for 1.5 to 2 hours. The X-ray diffractometer shows strong peaks at 2Ө = 34.2ᵒ of ZnO films which indicates that the films have a preferred c-axis wurtzite hexagonal (002) orientation. The surface morphology of the films is investigated by atomic force microscope (AFM) which proved the uniformity of the film since the roughness is within 5 nm range. The scanning electron microscopes(SEM) (Quanta FEG 250, Quanta 3D FEG, Nova NanoSEM 650) are used to characterize both ZnO film and NWs. SEM images show forest of ZnO NWs grown vertically and have a range of length up to 2000 nm and diameter of 20-300 nm. The SEM images prove that the role of the seed layer is to enhance the vertical alignment of ZnO NWs at the pH solution of 5-6. Also electrical and optical properties of the NWs are carried out using Electrical Force Microscopy (EFM). After growing the ZnO NWs, developing the nano-generator is the second step of this study in order to determine the energy conversion efficiency and the power output.

Keywords: ZnO nanowires(NWs), aqueous chemical growth (ACG), piezoelectric NWs, harvesting enery

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Authors: Amir Khaleghipour, Amirhossein Moghanian, Elhamalsadat Ghaffari

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Modified bioactive glass has been considered as a promising multifunctional candidate in bone repair and regeneration due to its attractive properties. The present study mainly aims to evaluate how the individual substitution of lithium (L-BG) and magnesium (M-BG) for calcium can affect the in vitro bioactivity of sol-gel derived substituted 58S bioactive glass (BG); and to present one composition in both of the 60SiO₂–(36-x)CaO–4P₂O₅–(x)Li₂O and 60SiO₂–(36-x)CaO–4P₂O₅–(x)MgO quaternary systems (where x= 0, 5, 10 mol.%) with improved biocompatibility, enhanced alkaline phosphatase (ALP) activity, and the most efficient antibacterial activity against methicillin-resistant Staphylococcus aureus bacteria. To address these aims, and study the effect of CaO/Li₂O and CaO/MgO substitution up to 10 mol % in 58S-BGs, the samples were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, inductively coupled plasma atomic emission spectrometry and scanning electron microscopy after immersion in simulated body fluid up to 14 days. Results indicated that substitution of either CaO/ Li₂O and CaO/ MgO had a retarding effect on in vitro hydroxyapatite (HA) formation due to the lower supersaturation degree for nucleation of HA compared with 58s-BG. Meanwhile, magnesium had a more pronounced effect. The 3-(4, 5dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) and alkaline phosphatase (ALP) assays showed that both substitutions of CaO/ Li₂O and CaO/ MgO up to 5mol % in 58s-BGs led to increased biocompatibility and stimulated proliferation of the pre-osteoblast MC3T3 cells with respect to the control. On the other hand, substitution of either Li or Mg for Ca in the 58s BG composition resulted in improved bactericidal efficiency against MRSA bacteria. Taken together, sample 58s-BG with 5 mol % CaO/Li₂O substitution (BG-5L) was considered as a multifunctional biomaterial in bone repair/regeneration with improved biocompatibility, enhanced ALP activity as well enhanced antibacterial efficiency against methicillin-resistant Staphylococcus aureus (MRSA) bacteria among all of the synthesized L-BGs and M-BGs.

Keywords: alkaline, alkaline earth, bioactivity, biomedical applications, sol-gel processes

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Authors: I. Kerti, G. Sezen, S. Daglilar

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This present work is focused on studying to improve low wetting behaviour between liquid metal and ceramic particles. Ceramic particles like SiC and B4C have attracted great attention because of their usability as reinforcement for composite materials. However, poor wettability of particles is one of the major drawbacks of metal matrix composite production. Various methods have been studied to enhance the wetting properties between ceramic materials and metal substrates during ceramic reinforced metal matrix composites. Among these methods, autocatalytic nickel deposition is a unique process for the enhancement of the surface properties of ceramic particles. In fact, it is difficult to obtain continuous and uniform metallic coating on ceramic powders. In this study deposition of nickel boron layer on ceramic particles via autocatalytic plating in borohydride baths were investigated. Firstly, powders with different particle sizes were sensitized and activated respectively in order to ensure catalytic properties. Following the pre-treatment operations, particles were transferred into the coating bath containing nickel sulphate or nickel chloride as the Ni2+ source. The results show that a better bonding and uniform coating layer were obtained for Ni-B coatings with the Ni2+ source of NiCl2.6H2O as compared to NiSO4.6H2O. With the progress of the time, both particle surfaces are completely covered by a continuous and thin nickel boron layer. The surface morphology of the coatings that were analysed using scanning electron microscopy (SEM) show that SiC and B4C particles both distributed and different thickness of Ni-B nanolayers have been successfully coated onto the particles. The particles were mounted into a polimeric resin and polished in order to observe the thickness and the continuity of the coating layer. The composition of the coating layers were also evaluated by EDS analyses. The SEM morphologies and the EDS results of the coatings at different reaction times were adopted for detailed discussion of the Ni-B electroless plating mechanism.

Keywords: boron carbide, electroless coating, nickel boron deposition, silicon carbide

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Authors: Atabaev I. G., Fayziev Sh. A., Irmatova Sh. K.

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Raw materials with high content of Kalium oxide widely used in ceramic technology for prevention or decreasing of deformation of ceramic goods during drying process and under thermal annealing. Becouse to low melting temperature it is also used to decreasing of the temperature of thermal annealing during fabrication of ceramic goods [1,2]. So called “Porceline or China stones” - quartz-sericite (muscovite) minerals is also can be used for prevention of deformation as the content of Kalium oxide in muscovite is rather high (SiO2, + KAl2[AlSi3O10](OH)2). [3] . To estimation of possibility of use of this mineral for ceramic manufacture, in the presented article the influence of thermal processing on phase and a chemical content of this raw material is investigated. As well as to other ceramic raw materials (kaoline, white burning clays) the basic requirements of the industry to quality of "a porcelain stone» are following: small size of particles, relative high uniformity of disrtribution of components and phase, white color after burning, small content of colorant oxides or chromophores (Fe2O3, FeO, TiO2, etc) [4,5]. In the presented work natural minerale from the Boynaksay deposit (Uzbekistan) is investigated. The samples was mechanically polished for investigation by Scanning Electron Microscope. Powder with size of particle up to 63 μm was used to X-ray diffractometry and chemical analysis. The annealing of samples was performed at 900, 1120, 1350oC during 1 hour. Chemical composition of Boynaksay raw material according to chemical analysis presented in the table 1. For comparison the composition of raw materials from Russia and USA are also presented. In the Boynaksay quartz – sericite the average parity of quartz and sericite makes 55-60 and 30-35 % accordingly. The distribution of quartz and sericite phases in raw material was investigated using electron probe scanning electronic microscope «JEOL» JXA-8800R. In the figure 1 the scanning electron microscope (SEM) micrograps of the surface and the distributions of Al, Si and K atoms in the sample are presented. As it seen small granular, white and dense mineral includes quartz, sericite and small content of impurity minerals. Basically, crystals of quartz have the sizes from 80 up to 500 μm. Between quartz crystals the sericite inclusions having a tablet form with radiant structure are located. The size of sericite crystals is ~ 40-250 μm. Using data on interplanar distance [6,7] and ASTM Powder X-ray Diffraction Data it is shown that natural «a porcelain stone» quartz – sericite consists the quartz SiO2, sericite (muscovite type) KAl2[AlSi3O10](OH)2 and kaolinite Al203SiO22Н2О (See Figure 2 and Table 2). As it seen in the figure 3 and table 3a after annealing at 900oC the quartz – sericite contains quartz – SiO2 and muscovite - KAl2[AlSi3O10](OH)2, the peaks related with Kaolinite are absent. After annealing at 1120oC the full disintegration of muscovite and formation of mullite phase Al203 SiO2 is observed (the weak peaks of mullite appears in fig 3b and table 3b). After annealing at 1350oC the samples contains crystal phase of quartz and mullite (figure 3c and table 3с). Well known Mullite gives to ceramics high density, abrasive and chemical stability. Thus the obtained experimental data on formation of various phases during thermal annealing can be used for development of fabrication technology of advanced materials. Conclusion: The influence of thermal annealing in the interval 900-1350oC on phase composition and structure of quartz-sericite minerale is investigated. It is shown that during annealing the phase content of raw material is changed. After annealing at 1350oC the samples contains crystal phase of quartz and mullite (which gives gives to ceramics high density, abrasive and chemical stability).

Keywords: quartz-sericite, kaolinite, mullite, thermal processing

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Authors: Mohamed Ayoub

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We perform computational investigation using density functional theory, B3LYP with aug-cc-pVTZ basis set followed by natural bond orbital analysis (NBO), which provides best single “natural Lewis structure” (NLS) representation of chosen wavefunction (Ψ) with natural resonance theory (NRT) to provide an analysis of molecular electron density in terms of resonance structures (RS) and weights (w). We selected for the study a wide range of gas phase dimers (B…HA), with hydrogen bond dissociation energies (ΔEB…H) that span more than two orders of magnitude. We demonstrate that charge transfer from a donor Lewis-type NBO (nB:) to an acceptor non-Lewis-type NBO (σHA*) is the primary cause for H-bonding not classical electrostatic (dipole-dipole or ionic). We provide a variety of structure, and spectroscopic descriptors to support the conclusion, such as IR frequency shift (ΔνHA), H-bond penetration distance (ΔRB..H), bond order (bB..H), charge-transfer (CTB→HA) and the corresponding donor-acceptor stabilization energy (ΔE(2)).

Keywords: natural bond orbital, hydrogen bonding, electron donor, electron acceptor

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Authors: Parastou Kharazmi, Folke Björk

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Some of the main causes for degradation of polymeric materials are thermal aging, hydrolysis, oxidation or chemical degradation by acids, alkalis or water. The first part of this paper provides a brief summary of advances in technology, methods and specification of composite materials for relining as a rehabilitation technique for sewage systems. The second part summarizes an investigation on frequently used composite materials for relining in Sweden, the rubber filled epoxy composite and reinforced polyester composite when they were immersed in deionized water or in dry conditions, and elevated temperatures up to 80°C in the laboratory. The tests were conducted by visual inspection, microscopy, Dynamic Mechanical Analysis (DMA), Differential Scanning Calorimetry (DSC) as well as mechanical testing, three point bending and tensile testing.

Keywords: composite, epoxy, polyester, relining, sewage

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Authors: M. G. Smitha, M. V. Murugendrappa

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Perovskite manganite La_0.7Ca_0.3MnO₃ was synthesized by Sol-gel method. Polymerization of pyrrole was carried by in-situ polymerization method. The composite of pyrrole (Py)/La_0.7Ca_0.3MnO₃ composite in the presence of oxidizing agent ammonium per sulphate to synthesize polypyrrole (PPy)/La_0.7Ca_0.3MnO₃ (LCM) composite was carried out by the same in-situ polymerization method. The PPy/LCM composites were synthesized with varying compositions like 10, 20, 30, 40, and 50 wt.% of LCM in Py. The surface morphologies of these composites were analyzed by using scanning electron microscope (SEM). The images show that LCM particles are embedded in PPy chain. The impedance measurement of PPy/LCM at different temperature ranges from 30 to 180 °C was studied using impedance analyzer. The study shows that impedance is frequency and temperature dependent and it is found to decrease with increase in frequency and temperature.

Keywords: polypyrrole, sol gel, impedance, composites

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Authors: Omkar Gaonkar, Indumathi Nambi, Suresh G. Kumar

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The functional and morphological aspects of soil structure determine the soil quality. The dispersion of colloidal soil particles, especially the clay fraction and rupture of soil aggregates, both of which play an important role in soil structure development, lead to degradation of soil quality. The main objective of this work was to determine the effect of the behaviour of soil colloids on the agricultural soil structure and quality. The effect of commercial humic acid and soil natural organic matter on the electrical and structural properties of the soil colloids was also studied. Agricultural soil, belonging to the sandy loam texture class from northern part of India was considered in this study. In order to understand the changes in the soil quality in the presence and absence of humic acids, the soil fabric and structure was analyzed by X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) Spectroscopy and Scanning Electron Microscopy (SEM). Electrical properties of natural soil colloids in aqueous suspensions were assessed by zeta potential measurements at varying pH values with and without the presence of humic acids. The influence of natural organic matter was analyzed by oxidizing the natural soil organic matter with hydrogen peroxide. The zeta potential of the soil colloids was found to be negative in the pH range studied. The results indicated that hydrogen peroxide treatment leads to deflocculation of colloidal soil particles. In addition, the humic acids undergoes effective adsorption onto the soil surface imparting more negative zeta potential to the colloidal soil particles. The soil hydrophilicity decreased in the presence of humic acids which was confirmed by surface free energy determination. Thus, it can be concluded that the presence of humic acids altered the soil fabric and structure, thereby affecting the soil quality. This study assumes significance in understanding soil aggregation and the interactions at soil solid-liquid interface.

Keywords: humic acids, natural organic matter, zeta potential, soil quality

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Authors: Abhishek Soti, Aditya Sharma, Akhilendra Bhushan Gupta

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Fouled reverse osmosis membranes are primarily characterized by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectrometer (EDS) for a detailed investigation of foulants; however, this has severe limitations on several accounts. Apart from inaccuracy in spectral properties and inevitable interferences and interactions between sample and instrument, misidentification of elements due to overlapping peaks is a significant drawback of EDS. This paper discusses this limitation by analyzing fouled polyamide RO membranes derived from community RO plants of Rajasthan treating brackish water via a combination of results obtained from EDS and Raman spectroscopy and cross corroborating with ICP-MS analysis of water samples prepared by dissolving the deposited salts. The anomalous behavior of different morphic forms of CaCO₃ in aqueous suspensions tends to introduce false reporting of the presence of certain heavy metals and rare earth metals in the scales of the fouled RO membranes used for treating brackish groundwater when analyzed using the commonly adopted techniques like SEM-EDS or Raman spectrometry. Peaks of CaCO₃ reflected in EDS spectra of the membrane were found to be misinterpreted as Scandium due to the automatic assignment of elements by the software. Similarly, the morphic forms merged with the dominant peak of CaCO₃ might be reflected as a single peak of Molybdenum in the Raman spectrum. A subsequent ICP-MS analysis of the deposited salts showed that both Sc and Mo were below detectable levels. It is always essential to cross-confirm the results through a destructive analysis method to avoid such interferences. It is further recommended to study different morphic forms of CaCO₃ scales, as they exhibit anomalous properties like reverse solubility with temperature and hence altered precipitation tendencies, for an accurate description of the composition of scales, which is vital for the smooth functioning of RO systems.

Keywords: reverse osmosis, foulant analysis, groundwater, EDS, artifacts

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Authors: Hasnaa Benchorfi

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The Tellurite glasses exhibit interesting properties, notably their low melting point (700-900°C), high refractive index (≈2), high transparency in the infrared region (up to 5−6 μm), interesting linear and non-linear optical properties and high rare earth ions solubility. These properties give tellurite glasses a great interest in various optical applications. Transparent ceramics present advantages compared to glasses, such as improved mechanical, thermal and optical properties. But, the elaboration process of these ceramics requires complex sintering conditions. The full crystallization of glass into transparent ceramics is an alternative to circumvent the technical challenges related to the ceramics obtained by conventional processing. In this work, a crystallization study of a specific glass composition in the system TeO2-Ta2O5-Bi2O3 shows structural transitions from the glass to the stabilization of an unreported anti-glass phase to a transparent ceramic upon heating. An anti-glass is a material with a cationic long-range order and a disordered anion sublattice. Thus, the X-ray diffraction patterns show sharp peaks, while the Raman bands are broad and similar to those of the parent glass. The structure and microstructure of the anti-glass and corresponding ceramic were characterized by Powder X-Ray Diffraction, Electron Back Scattered Diffraction, Transmission Electron Microscopy and Raman spectroscopy. The optical properties of the Er3+-doped samples are also discussed.

Keywords: glass, congruent crystallization, anti-glass, glass-ceramic, optics

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Authors: Justice Zakhele Msomi

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Nanoparticles of CdFe2O4 with particle size of about 10 nm have been synthesized by high energy ball milling and co-precipitation processes. The synthesis route appears to have some effects on the properties. The compounds have been characterized by X-ray diffraction, Fourier Transform Infrared (FTIR), transmission electron microscopy (TEM), Mössbauer and magnetization measurements. The XRD pattern of CdFe2O4 provides information about single-phase formation of spinel structure with cubic symmetry. The FTIR measurements between 400 and 4000 cm-1 indicate intrinsic cation vibration of the spinel structure. The Mössbauer spectra were recorded at 4 K and 300 K. The hyperfine fields appear to be highly sensitive on particle size. The evolution of the properties as a function of particle size is also presented.

Keywords: ferrite, nanoparticles, magnetization, Mössbauer

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Authors: Manisha Mathur, Manisha Choudhary, Sandeep Khare

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The present study was carried out for the comprehensive analysis of lumpy skin disease (LSD) in cattle and to elucidate the histopathology of vital organs in natural outbreaks. Lumpy skin disease (LSD) is a viral infection that primarily affects cattle. It is caused by a Capri pox virus and is characterized by the formation of skin nodules or lesions. For this study, a postmortem of 20 cows who died of Lumpy skin disease in different regions of Rajasthan was conducted. This study aimed to examine a cow's external and internal organs to confirm if lumpy skin disease was the cause of death. Accurate diagnosis is essential for improving disease surveillance, understanding the disease's progression, and informing control measures. Pathological examinations reveal virus-induced changes across organs, while histopathological analyses provide crucial insights into the disease's pathogenesis, aiding in the development of advanced diagnostics and effective prevention strategies. Histopathological examination of nodular skin lesions revealed edema, hyperemia, acanthosis, severe hydropic degeneration/ballooning degeneration, and hyperkeratosis in the epidermis. In the lungs, congestion, oedema, emphysema, and atelectasis were observed grossly. Microscopically changes were suggestive of interstitial pneumonia, suppurative pneumonia, bronchopneumonia post pneumonic fibrosis, and stage of resolution. Grossely liver showed congestion and necrotic foci microscopically in most of the cases, and the liver showed acute viral hepatitis. Microscopically in kidneys, multifocal interstitial nephritis was observed. There was marked interstitial inflammation and zonal fibrosis with cystically dilated tubules and bowman's capsules. Microscopically, most of the heart tissue section showed normal histology with few sarcocysts in between cardiac muscles. In some cases, loss of cross striation, sarcoplasmic vacuolation, fregmentation, and disintegration of cardiac fibres were observed. The present study revealed the characteristic gross and histopathological changes in different organs in natural cases of lumpy skin disease. Further, the disease was confirmed based on the molecular diagnosis and transmission electron microscopy of capripox infection in the affected cattle in the study area.

Keywords: Capripoxvirus, lumpy skin disease, polymerage chain reaction, transmission electron microscopy

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Authors: Mahendrasingh J. Pawar, M. D. Gaoner

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Ta-doped Nb2O5 (Ta content 0.5-2% mole fraction) nanoparticles in the range of 20-40 nm were synthesized by combustion technique. The crystalline phase, morphology and size of the nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and UV-vis spectroscopy. The specific surface area of the nanoparticles was measured by nitrogen adsorption (BET analysis). The undoped Nb2O5 nanoparticles were found to have the particles size in the range of 50−80 nm. The photocatalytic performance of the samples was characterized by degrading 20 mg/L toluene under UV−Vis irradiation. The results show that the Ta-doped Nb2O5 nanoparticles exhibit a significant increase in photocatalytic performance over the undoped Nb2O5 nanoparticles, and the Nb2O5 nanoparticles doped with 1.5% Ta and calcined at 450°C show the best photocatalytic performance.

Keywords: Nb2O5, Ta-doped Nb2O5, photodegradation of Toluene, combustion method

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Authors: F. A. Rodríguez-Prada, W Gutierrez, I. D. Mikhailov

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We study the spectral properties of one-electron non-uniform crater-shaped quantum dot whose thickness is increased linearly with different slopes in different radial directions between the central hole and the outer border and which is deposited over thin wetting layer in the presence of the external vertically directed magnetic field. We show that in the adiabatic limit, when the crater thickness is much smaller than its lateral dimension, the one-particle wave functions of the electron confined in such structure in the zero magnetic field case can be found exactly in an analytical form and they can be used subsequently as the base functions in framework of the exact diagonalization method to study the effect of the wetting layer and an external magnetic field applied along of the grown axis on energy levels of one-electron non-uniform quantum dot. It is shown that both the structural non-uniformity and the increase of the thickness of the wetting layer provide a quenching of the Aharonov-Bohm oscillations of the lower energy levels.

Keywords: electronic properties, quantum rings, volcano shaped, wetting layer

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Authors: Pratima Kumari, Sukha Ranjan Samadder

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This research aims to contribute to the sustainable production of graphene materials by exploring the extraction of graphite from spent primary and secondary batteries. The increasing demand for graphene materials, a versatile and high-performance material, necessitates environmentally friendly methods for its synthesis. The process involves a well-planned methodology, beginning with the gathering and categorization of batteries, followed by the disassembly and careful removal of graphite from anode structures. The use of environmentally friendly solvents and mechanical techniques ensures an efficient and eco-friendly extraction of graphite. Advanced approaches such as the modified Hummers' method and chemical reduction process are utilized for the synthesis of graphene materials, with a focus on optimizing parameters. Various analytical techniques such as Fourier-transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, thermogravimetric analysis, and Raman spectroscopy were employed to validate the quality and structure of the produced graphene materials. The major findings of this study reveal the successful implementation of the methodology, leading to the production of high-quality graphene materials suitable for advanced material applications. Thorough characterization using various advanced techniques validates the structural integrity and purity of the graphene. The economic viability of the process is demonstrated through a comprehensive economic analysis, highlighting the potential for large-scale production. This research contributes to the field of sustainable production of graphene materials by offering a systematic methodology that efficiently transforms spent batteries into valuable graphene resources. Furthermore, the findings not only showcase the potential for upcycling electronic waste but also address the pressing need for environmentally conscious processes in advanced material synthesis.

Keywords: spent primary batteries, spent secondary batteries, graphite extraction, advanced material synthesis, circular economy approach

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Authors: Magdalena Blachnio, Viktor Bogatyrov, Mariia Galaburda, Anna Derylo-Marczewska

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Agricultural waste materials from traditional oil mill and after extraction of natural raw materials in supercritical conditions were used for the preparation of carbon nanomaterials (activated carbons) by two various methods. Chemical activation using acetic acid and physical activation with a gaseous agent (carbon dioxide) were chosen as mild and environmentally friendly ones. The effect of influential factors: type of raw material, temperature and activation agent on the porous structure characteristics of the materials was discussed by using N₂ adsorption/desorption isotherms at 77 K. Furthermore scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were employed to examine the physicochemical properties of the obtained sorbents. Selection of a raw material and an optimization of the conditions of the synthesis process, allowed to obtain the cheap sorbents with a targeted distribution of pores enabling effective adsorption of the model organic pollutants carried out in the multicomponent systems. Adsorption behavior (capacity and rate) of the chosen activated carbons was estimated by utilizing Crystal violet (CV), 4-chlorophenoxyacetic acid (4-CPA), 2.4-dichlorophenoxyacetic acid (2.4-D) as the adsorbates. Both rate and adsorption capacity of the organics on the sorbents evidenced that the activated carbons could be effectively used in sewage treatment plants. The mechanisms of organics adsorption were studied and correlated with activated carbons properties.

Keywords: activated carbon, adsorption equilibrium, adsorption kinetics, organics adsorption

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Authors: El-Said I. El-Shafey, Syeda Naheed F. Ali, Saleh S. Al-Busafi, Haider A. J. Al-Lawati

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Date palm leaflets were utilized as a precursor for activated carbon (AC) preparation using KOH activation. AC produced was oxidized using nitric acid producing oxidized activated carbon (OAC). OAC that possesses acidic surface was surface functionalized to produce basic activated carbons using linear diamine compounds (ethylene diamine and propylene diamine). OAC was also functionalized to produce hydrophobic activated carbons using ethylamine (EA) and aniline (AN). Dehydrated carbon was also prepared from date palm leaflets using sulfuric acid dehydration/ oxidation and was surface functionalized in the same way as AC. Nitric acid oxidation was not necessary for DC as it is acidic carbon. The surface area of AC is high (823 m2/g) with microporosity domination, however, after oxidation and surface functionalization, both the surface area and surface microporosity decrease tremendously. DC surface area was low (15 m2/g) with mesoporosity domination. Surface functionalization has decreased the surface area of activated carbons. FTIR spectra show that -COOH group on DC and OAC almost disappeared after surface functionalization. The surface chemistry of all carbons produced was tested for pHzpc, basic sites, boehm titration, thermogravimetric analysis and zeta potential measurement. Scanning electron microscopy and energy dispersive spectroscopy in addition to CHN elemental analysis were also carried out. DC and OAC possess low pHzpc and high surface functionality, however, basic and hydrophobic carbons possess high pHzpc and low surface functionality. The different behavior of carbons is related to their different surface chemistry. Methylene blue adsorption was found to be faster on hydrophobic carbons based on AC and DC. The Larger adsorption capacity of methylene blue was found for hydrophobic carbons. Dominating adsorption forces of methylene blue varies from carbon to another depending on its surface nature. Sorption forces include hydrophobic forces, H-bonding, electrostatic interactions and van der Waals forces.

Keywords: carbon, acidic, basic, hydrophobic

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Authors: Hiroyuki Aoki

Abstract:

The physical properties of polymer materials are dependent on the conformation and molecular motion of a polymer chain. Therefore, the structure and dynamic behavior of the single polymer chain have been the most important concerns in the field of polymer physics. However, it has been impossible to directly observe the conformation of the single polymer chain in a bulk medium. In the current work, the novel techniques to study the conformation and dynamics of a single polymer chain are proposed. Since a fluorescence method is extremely sensitive, the fluorescence microscopy enables the direct detection of a single molecule. However, the structure of the polymer chain as large as 100 nm cannot be resolved by conventional fluorescence methods because of the diffraction limit of light. In order to observe the single chains, we developed the labeling method of polymer materials with a photo-switchable dye and the super-resolution microscopy. The real-space conformational analysis of single polymer chains with the spatial resolution of 15-20 nm was achieved. The super-resolution microscopy enables us to obtain the three-dimensional coordinates; therefore, we succeeded the conformational analysis in three dimensions. The direct observation by the nanometric optical microscopy would reveal the detailed information on the molecular processes in the various polymer systems.

Keywords: polymer materials, single molecule, super-resolution techniques, conformation

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Authors: Rajeev Jain, Nimisha Jadon, Kshiti Singh

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Titanium oxide nanoparticles and 1-butyl-2,3-dimethylimidazolium bis (trifluoromethane- sulfonyl) imide modified glassy carbon electrode (TiO2/IL/GCE) has been fabricated for electrochemical sensing of flunarizine dihydrochloride (FRH). The electrochemical properties and morphology of the prepared nanocomposite were studied by electrochemical impedance spectroscopy (EIS) and transmission electron microscopy (TEM). The response of the electrochemical sensor was found to be proportional to the concentrations of FRH in the range from 0.5 µg mL-1 to 16 µg mL-1. The detection limit obtained was 0.03 µg mL-1. The proposed method was also applied to the determination of FRH in pharmaceutical formulation and human serum with good recoveries.

Keywords: flunarizine dihydrochloride, ionic liquid, nanoparticles, voltammetry, human serum

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Authors: Zainab D. Abd Ali, Thamir H. Khalaf

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In this paper, the characteristics of electric discharge in gap between two (parallel-plate) dielectric plates are studies, the gap filled with Argon gas in atm pressure at ambient temperature, the thickness of gap typically less than 1 mm and dielectric may be up 10 cm in diameter. One of dielectric plates a sinusoidal voltage is applied with Rf frequency, the other plates is electrically grounded. The simulation in this work depending on Boltzmann equation solver in first few moments, fluid model and plasma chemistry, in one dimensional modeling. This modeling have insight into characteristics of Dielectric Barrier Discharge through studying properties of breakdown of gas, electric field, electric potential, and calculating electron density, mean electron energy, electron current density ,ion current density, total plasma current density. The investigation also include: 1. The influence of change in thickness of gap between two plates if we doubled or reduced gap to half. 2. The effect of thickness of dielectric plates. 3. The influence of change in type and properties of dielectric material (gass, silicon, Teflon).

Keywords: computational diagnostics, Boltzmann equation, electric discharge, electron density

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Authors: Fatih Kılıç, Burak Birol, Necmettin Maraşlı

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The directional solidification process is generally used for homogeneous compound production, single crystal growth, and refining (zone refining), etc. processes. The most important two parameters that control eutectic structures are temperature gradient and grain growth rate which are called as solidification parameters The solidification behavior and microstructure characteristics is an interesting topic due to their effects on the properties and performance of the alloys containing eutectic compositions. The solidification behavior of multicomponent and multiphase systems is an important parameter for determining various properties of these materials. The researches have been conducted mostly on the solidification of pure materials or alloys containing two phases. However, there are very few studies on the literature about multiphase reactions and microstructure formation of multicomponent alloys during solidification. Because of this situation, it is important to study the microstructure formation and the thermodynamical, thermophysical and microstructural properties of these alloys. The production process is difficult due to easy oxidation of magnesium and therefore, there is not a comprehensive study concerning alloys containing high Mg (> 30 wt.% Mg). With the increasing amount of Mg inside Al alloys, the specific weight decreases, and the strength shows a slight increase, while due to formation of β-Al8Mg5 phase, ductility lowers. For this reason, production, examination and development of high Mg containing alloys will initiate the production of new advanced engineering materials. The original value of this research can be described as obtaining high Mg containing (> 30% Mg) Al based multicomponent alloys by melting under vacuum; controlled directional solidification with various growth rates at a constant temperature gradient; and establishing relationship between solidification rate and microstructural, mechanical, electrical and thermal properties. Therefore, within the scope of this research, some > 30% Mg containing ternary or quaternary Al alloy compositions were determined, and it was planned to investigate the effects of directional solidification rate on the mechanical, electrical and thermal properties of these alloys. Within the scope of the research, the influence of the growth rate on microstructure parameters, microhardness, tensile strength, electrical conductivity and thermal conductivity of directionally solidified high Mg containing Al-32,2Mg-0,37Si; Al-30Mg-12Zn; Al-32Mg-1,7Ni; Al-32,2Mg-0,37Fe; Al-32Mg-1,7Ni-0,4Si; Al-33,3Mg-0,35Si-0,11Fe (wt.%) alloys with wide range of growth rate (50-2500 µm/s) and fixed temperature gradient, will be investigated. The work can be planned as; (a) directional solidification of Al-Mg based Al-Mg-Si, Al-Mg-Zn, Al-Mg-Ni, Al-Mg-Fe, Al-Mg-Ni-Si, Al-Mg-Si-Fe within wide range of growth rates (50-2500 µm/s) at a constant temperature gradient by Bridgman type solidification system, (b) analysis of microstructure parameters of directionally solidified alloys by using an optical light microscopy and Scanning Electron Microscopy (SEM), (c) measurement of microhardness and tensile strength of directionally solidified alloys, (d) measurement of electrical conductivity by four point probe technique at room temperature (e) measurement of thermal conductivity by linear heat flow method at room temperature.

Keywords: directional solidification, electrical conductivity, high Mg containing multicomponent Al alloys, microhardness, microstructure, tensile strength, thermal conductivity

Procedia PDF Downloads 253