Search results for: two-photon fluorescence microscopy

Authors: Ali Obeydavi, Majid Rahimi

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This study explores the synthesis and characterization of Fe-Cr-Mo-Co-C-B-Si thin film metallic glasses fabricated using the pulsed laser deposition (PLD) technique on silicon wafer and 304 stainless steel substrates. it systematically varied the laser pulse numbers (20,000; 30,000; 40,000) and energies (130, 165, 190 mJ) to investigate their effects on the microstructural, mechanical, and corrosion properties of the deposited films. Comprehensive characterization techniques, including grazing incidence X-ray diffraction, field emission scanning electron microscopy, atomic force microscopy, and transmission electron microscopy with selected area electron diffraction, were utilized to assess the amorphous structure and surface morphology. Results indicated that increased pulse numbers and laser energies led to enhanced deposition rates and film thicknesses. Nanoindentation tests demonstrated that the hardness and elastic modulus of the amorphous thin films significantly surpassed those of the 304 stainless steel substrate. Additionally, electrochemical polarization and impedance spectroscopy revealed that the Fe-based metallic glass coatings exhibited superior corrosion resistance compared to the stainless steel substrate. The observed improvements in mechanical and corrosion properties are attributed to the unique amorphous structure achieved through the PLD process, highlighting the potential of these materials for protective coatings in aggressive environments.

Keywords: thin film metallic glasses, pulsed laser deposition, mechanical properties, corrosion resistance

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Authors: Aigin Bashti

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Preparation of multicomponent reactions (MCRs) via a simple one-pot strategy is considered a novel procedure which has attracted a lot of interest from organic and medicinal chemists. Due to the great importance of phthalazide triones, it was decided to introduce a novel and cost-effective green procedure for the preparation of these derivatives. In this methodology, an efficient 4,4ʹ-Bipyridinium Dichloride Ordered Mesoporous Silica functionalized catalyst (BP-SBA-15) was utilized. The catalyst was characterized by X-ray diffraction analysis (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), thermo-gravimetric analysis (TGA), and Fourier-transform infrared spectroscopy (FT-IR) analysis. In conclusion, it should be mentioned that this methodology has some advantages, including short reaction time, high yield of the products, recyclable catalyst, green procedure, and facile work-up procedure. The catalyst was successfully utilized for the one-pot preparation of various phthalazinetrione derivatives.

Keywords: dimedone, green procedure, multicomponent reactions, phthalhydrazide

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Authors: Raana Babadi Fathipour

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Hydrogels are three-dimensional structures formed by the interweaving of polymeric materials, possessing the remarkable ability to imbibe copious amounts of water. Numerous methodologies have been devised for examining and understanding the properties of these synthesized gels. Amongst them, spectroscopic techniques such as ultraviolet/visible (UV/Vis) and Fourier-transform infrared (FTIR) spectroscopy offer a glimpse into molecular and atomic aspects. Additionally, diffraction methods like X-ray diffraction (XRD) enable one to measure crystallinity within the gel's structure, while microscopy tools encompassing scanning electron microscopy (SEM) and transmission electron microscopy (TEM) provide insights into surface texture and morphology. Furthermore, rheology serves as an invaluable tool for unraveling the viscoelastic behavior inherent in hydrogels—a parameter crucial not only to numerous industries, including pharmaceuticals, cosmetics, food processing, agriculture and water treatment, but also pivotal to related fields of research. Likewise, the ultimate configuration of the product is contingent upon its characterization at a microscopic scale in order to comprehend the intricacies of the hydrogel network's structure and interaction dynamics in response to external forces. Within this present scrutiny, our attention has been devoted to unraveling the intricate rheological tendencies exhibited by materials founded on synthetic, natural, and semi-synthetic hydrogels. We also explore their practical utilization within various facets of everyday life from an industrial perspective.

Keywords: rheology, hydrogels characterization, viscoelastic behavior, application

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Authors: Supanyika Sengsai, Aree Thongpukdee, Chalermchai Kanchanakachain

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The study aimed to collect morphological data of secretory structures that contribute to taxonomy of Indigofera. Detail features of trichomes occurrence in vegetative and reproductive organs of Indigofera wightii Grah. ex Wigh & Arn., a species traditionally used as source of indigo to dye “Thaisongdam” clothing were investigated. Examination through light microscopy and scanning electrom microscopy were done. Non secretory, T-shaped trichomes appeared throughout surfaces of stems, leaves, flowers and fruits. Secretory or glandular trichomes occurred in two types; one has big cylindrical head and short peduncle, distributed on adaxial surface of sepals and around the pedicel, whereas another possesses smaller cylindrical head but long peduncle. The latter was found on apical surface of immature pods. No phenolic and lipophilic compounds were detected from these glands.

Keywords: indigofera, trichome, Thaisongdam, Thailand

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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: D. Zahran, M. AlKhazindar, M. Khalil, E. T. A. Sayed

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Streptomyces scabies is a pathogenic actinomycete that infects potato crop causing severe production losses. Actinophages affect the composition and diversity of the bacterial population, thereby, can be used as a biological control. Samples of actinomycetes and phages were collected from different cultivated soils including farms of Faculty of Science, Faculty of Agriculture and different locations in Giza, Egypt. Actinomycetes were identified by using biochemical, morphological tests and molecular studies using 16S rRNA sequencing. Two specific phages (E1 and E2) against Streptomyces scabies and other hosts were isolated. Phages were identified using dilution end point (DEP), longevity in vitro (LIV), thermal inactivation point (TIP), host range and electron microscopy. PhageE1 was characterized by 10-8 (DEP),180 days(LIV), 95°C(TIP), narrow host range and electron microscopy showed ahead (59.9 nm) and neck (10.4nm). On the other hand phageE2 had 10-20 (DEP),180 days(LIV), 90°C(TIP), and the size of head was (67.2 nm) and tail (114nm). Antiviral activity was also studied using different chemicals (NaCL, KCL, CaCL2, BaCL2, CoCL2, AgNO3, ALCL3and HgCL2) with different concentrations and different plant extracts with different concentrations (star anise, tea, tillia, peppermint, ginger, cumin, chamomile, turmeric cinnamon, marjoram and black cumin). Both Phage E1and phage E2 were vulnerable to (cumin, ginger, chamomile, guavas leaves and star anise) but resistant to (Tillie, marjoram, fennelflower seeds, peppermint, and cinnamon).

Keywords: potato scab, actinophages, biological control, electron microscopy, TIP, DEP, LIV, antiviral activity

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Authors: Humaira Khan, Mohsin Javed, Sammia Shahid

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The reinforced photocatalytic activity of graphene oxide (GO) along with composites of ZnO nanoparticles and copper-doped ZnO nanoparticles were studied by synthesizing ZnO and copper- doped ZnO nanoparticles by co-precipitation method. Zinc acetate and copper acetate were used as precursors, whereas graphene oxide was prepared from pre-oxidized graphite in the presence of H2O2.The supernatant was collected carefully and showed high-quality single-layer characterized by FTIR (Fourier Transform Infrared Spectroscopy), TEM (Transmission Electron Microscopy), SEM (Scanning Electron Microscopy), XRD (X-ray Diffraction Analysis), EDS (Energy Dispersive Spectrometry). The degradation of methylene blue as standard pollutant under UV-Visible irradiation gave results for photocatalytic activity of dopants. It could be concluded that shrinking of optical band caused by composites of Cu-dopped nanoparticles with GO enhances the photocatalytic activity.

Keywords: degradation, graphene oxide, photocatalysis, ZnO nanoparticles and copper-doped ZnO nanoparticles

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Authors: P. Bublíkova, P. Halodova, H. K. Namburi, J. Stodolna, J. Duchon, O. Libera

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Neutron radiation-induced microstructural changes cause degradation of mechanical properties and the lifetime reduction of reactor internals during nuclear power plant operation. Investigating the effects of neutron irradiation on mechanical properties of the irradiated material (hardening, embrittlement) is challenging and time-consuming. Although the fast neutron spectrum has the major influence on microstructural properties, the thermal neutron effect is widely investigated owing to Irradiation-Assisted Stress Corrosion Cracking firstly observed in BWR stainless steels. In this study, 300-series austenitic stainless steels used as material for NPP's internals were examined after neutron irradiation at ~ 15 dpa. Although several nanoindentation experimental publications are available to determine the mechanical properties of ion irradiated materials, less is available on neutron irradiated materials at high dpa tested in hot-cells. In this work, we present particular methodology developed to determine the mechanical properties of neutron irradiated steels by nanoindentation technique. Furthermore, radiation-induced damage in the specimens was investigated by High Resolution - Transmission Electron Microscopy (HR-TEM) that showed the defect features, particularly Frank loops, cavity microstructure, radiation-induced precipitates and radiation-induced segregation. The results of nanoindentation measurements and associated nanoscale defect features showed the effect of irradiation-induced hardening. We also propose methodologies to optimized sample preparation for nanoindentation and microscotructural studies.

Keywords: nanoindentation, thermal neutrons, radiation hardening, transmission electron microscopy

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Authors: Ahbdelfattah M. Khourshid, T. Elabeidi

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Friction Stir Welding (FSW), a solid state joining technique, is widely being used for joining Al alloys for aerospace, marine automotive and many other applications of commercial importance. FSW were carried out using a vertical milling machine on Al 5083 alloy pipe. These pipe sections are relatively small in diameter, 5mm, and relatively thin walled, 2mm. In this study, 5083 aluminum alloy pipe were welded as similar alloy joints using (FSW) process in order to investigate mechanical and microstructural properties .rotation speed 1400 r.p.m and weld speed 10,40,70 mm/min. In order to investigate the effect of welding speeds on mechanical properties, metallographic and mechanical tests were carried out on the welded areas. Vickers hardness profile and tensile tests of the joints as a metallurgical investigation, Optic Microscopy and Scanning Electron Microscopy (SEM) were used for base and weld zones.

Keywords: friction stir welding (FSW), Al alloys, mechanical properties, microstructure

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Authors: Tatiana Franco, Hugo A. Estupinan

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Banana pseudostem fiber (BPF) and pineapple leaf fiber (PLF) for their excellent mechanical properties and biodegradability characteristics arouse interest in different areas of research. F In tropical regions, where the banana pseudostem and the pineapple leaf are transformed into hard-to-handle solid waste, they can be low-cost raw material and environmentally sustainable in research for composite materials. In terms of functionality of this type of fiber, an open structure would allow the adsorption and retention of organic, inorganic and metallic species. In general, natural fibers have closed structures on their surface with intricate internal arrangements that can be used for the solution of environmental problems and other technological uses, however it is not possible to access their internal structure and sublayers, exposing the fibers in the natural state. An alternative method to chemical and enzymatic treatment are the processes with the plasma treatments, which are known to be clean, economical and controlled. In this type of treatment, a gas contained in a reactor in the form of plasma acts on the fiber generating changes in its structure, morphology and topography. This work compares the effects on fibers of PLF and BPF treated with cold argon plasma, alternating time and current. These fibers are grown in the regions of Antioquia-Colombia. The morphological, compositional and wettability properties of the fibers were analyzed by Raman microscopy, contact angle measurements, scanning electron microscopy (SEM) and atomic force microscopy analysis (AFM). The treatment with cold plasma on PLF and BPF allowed increasing its wettability, the topography and the microstructural relationship between lignin and cellulose.

Keywords: cold plasma, contact angle, natural fibers, Raman, SEM, wettability

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Authors: M. Kowalik, J. Masternak, K. Kazimierczuk, O. V. Khavryuchenko, B. Kupcewicz, B. Barszcz

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Recently, the growing interest of chemists in metal-organic coordination polymers (MOCPs) is primarily derived from their intriguing structures and potential applications in catalysis, gas storage, molecular sensing, ion exchanges, nonlinear optics, luminescence, etc. Currently, we are devoting considerable effort to finding the proper method of synthesizing new coordination polymers containing S- or N-heteroaromatic carboxylates as linkers and characterizing the obtained Pb(II) compounds according to their structural diversity, luminescence, and thermal properties. The choice of Pb(II) as the central ion of MOCPs was motivated by several reasons mentioned in the literature: i) a large ionic radius allowing for a wide range of coordination numbers, ii) the stereoactivity of the 6s2 lone electron pair leading to a hemidirected or holodirected geometry, iii) a flexible coordination environment, and iv) the possibility to form secondary bonds and unusual non-covalent interactions, such as classic hydrogen bonds and π···π stacking interactions, as well as nonconventional hydrogen bonds and rarely reported tetrel bonds, Pb(lone pair)···π interactions, C–H···Pb agostic-type interactions or hydrogen bonds, and chelate ring stacking interactions. Moreover, the construction of coordination polymers requires the selection of proper ligands acting as linkers, because we are looking for materials exhibiting different network topologies and fluorescence properties, which point to potential applications. The reaction of Pb(NO₃)₂ with 1H-pyrrole-2-carboxylic acid (2prCOOH) leads to the formation of a new four-nuclear Pb(II) polymer, [Pb4(2prCOO)₈(H₂O)]ₙ, which has been characterized by CHN, FT-IR, TG, PL and single-crystal X-ray diffraction methods. In view of the primary Pb–O bonds, Pb1 and Pb2 show hemidirected pentagonal pyramidal geometries, while Pb2 and Pb4 display hemidirected octahedral geometries. The topology of the strongest Pb–O bonds was determined as the (4·8²) fes topology. Taking the secondary Pb–O bonds into account, the coordination number of Pb centres increased, Pb1 exhibited a hemidirected monocapped pentagonal pyramidal geometry, Pb2 and Pb4 exhibited a holodirected tricapped trigonal prismatic geometry, and Pb3 exhibited a holodirected bicapped trigonal prismatic geometry. Moreover, the Pb(II) lone pair stereoactivity was confirmed by DFT calculations. The 2D structure was expanded into 3D by the existence of non-covalent O/C–H···π and Pb···π interactions, which was confirmed by the Hirshfeld surface analysis. The above mentioned interactions improve the rigidity of the structure and facilitate the charge and energy transfer between metal centres, making the polymer a promising luminescent compound.

Keywords: coordination polymers, fluorescence properties, lead(II), lone electron pair stereoactivity, non-covalent interactions

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Authors: Ruitao Li, Zhili Dong, Nay Win Khun, Khiam Aik Khor

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In this study, microstructure and sintering mechanism as well as wear resistance properties of Ti/Al-Cr-Fe metal matrix composites (MMCs) fabricated by spark plasma sintering (SPS) with Ti as matrix and Al-Cr-Fe as reinforcement were investigated. Phases and microstructure of the sintered samples were analyzed using X-ray diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and transmission electron microscopy (TEM). Wear resistance properties were tested by ball-on-disk method. An Al3Ti ring forms around each Al-Cr-Fe particle as the bonding layer between Ti and Al-Cr-Fe particles. The Al content in Al-Cr-Fe particles experiences a decrease from 70 at.% to 60 at.% in the sintering process. And these particles consist of quasicrystalline icosahedral AlCrFe and quasicrystal approximants γ-brass Al8(Cr,Fe)5 and Al9(Cr,Fe)4 in the sintered compact. The addition of Al-Cr-Fe particles into the Ti matrix can improve the microhardness by about 40% and the wear resistance is improved by more than 50% due to the increase in the microhardness and the change of wear mechanism.

Keywords: metal matrix composites, spark plasma sintering, phase transformation, wear

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Authors: Ana Paula Rosifini Alves Claro, André Luiz Reis Rangel, Nathan Trujillo, Ketul C. Popat

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In the present work, in vitro cytotoxicity was evaluated after nanotubes growth on Ti15Mo alloy surface. TiO2 nanotubes were obtained by anodizing technique at room temperature in an electrolyte with 0.25 %NH4F and glycerol at a constant anodic potential of 20 V for 24 hours. The morphology of nanotubes was observed by field emission scanning electron microscopy (FE-SEM; XL 30 FEG, Philips). Crystal structure was analyzed by wide-angle X-ray diffraction. A cell culture model using human fibroblast-like cells was used to study the effect of TiO2 nanotubes growth on the cytotoxicity of the Ti15Mo alloy for 1, 4 and 7 days culture period. The MTT assay was used to evaluate cell viability and cell adhesion was evaluated by scanning electron microscopy. Results show that Ti15Mo alloy with TiO2 nanotubes on surface is nontoxic and exhibit good interaction with surface.

Keywords: titanium alloys, TiO2 nanotubes, cell growth, Ti-15Mo alloy

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Authors: Navneet Dabra, Baljinder Kaur, Lakhbir Singh, V. Annapu Reddy, R. Nath, Dae-Yong Jeong, Jasbir S. Hundal

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Nano-composite films of sodium nitrite (NaNO2): Starch with different proportions of NaNO2 and Starch have been prepared by drop cast technique. The ferroelectric hysteresis loops (P-V) have been traced using modified Sawyar-Tower circuit. The films containing equal proportions of NaNO2 and Starch exhibit optimized ferroelectric properties. The stability of the remanent polarization, Pr in the optimized nano-composite films exhibit improved stability over the pure NaNO2 films. The Atomic Force Microscopy (AFM) has been employed to investigate the surface morphology. AFM images clearly reveal the nano sized particles of NaNO2 dispersed in starch with small value of surface roughness.

Keywords: ferroelectricity, nano-composite films, Atomic Force Microscopy (AFM), nano composite film

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Authors: Anil Kumar, Rajnish Kaur, Mateusz Czyzycki, Alessandro Migilori, Andreas Germanos Karydas, Sanjiv Puri

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The radiative decay of Li(i=1-3) sub-shell vacancies produced through photoionization results in production of the characteristic emission spectrum comprising several X-ray lines, whereas non-radiative vacancy decay results in Auger electron spectrum. Accurate reliable data on the Li(i=1-3) sub-shell X-ray production (XRP) cross sections is of considerable importance for investigation of atomic inner-shell ionization processes as well as for quantitative elemental analysis of different types of samples employing the energy dispersive X-ray fluorescence (EDXRF) analysis technique. At incident photon energies in vicinity of the absorption edge energies of an element, the many body effects including the electron correlation, core relaxation, inter-channel coupling and post-collision interactions become significant in the photoionization of atomic inner-shells. Further, in case of compounds, the characteristic emission spectrum of the specific element is expected to get influenced by the chemical environment (coordination number, oxidation state, nature of ligand/functional groups attached to central atom, etc.). These chemical effects on L X-ray fluorescence parameters have been investigated by performing the measurements at incident photon energies much higher than the Li(i=1-3) sub-shell absorption edge energies using EDXRF spectrometers. In the present work, the cross sections for production of the Lk(k= γ2,3, γ4) X-rays have been measured for some compounds of 66Dy, namely, Dy2O3, Dy2(CO3)3, Dy2(SO4)3.8H2O, DyI2 and Dy metal by tuning the incident photon energies few eV above the L1 absorption-edge energy in order to investigate the influence of chemical effects on these cross sections in presence of the many body effects which become significant at photon energies close to the absorption-edge energies. The present measurements have been performed under vacuum at the IAEA end-station of the X-ray fluorescence beam line (10.1L) of ELETTRA synchrotron radiation facility (Trieste, Italy) using self-supporting pressed pellet targets (1.3 cm diameter, nominal thicknesses ~ 176 mg/cm2) of 66Dy compounds (procured from Sigma Aldrich) and a metallic foil of 66Dy (nominal thickness ~ 3.9 mg/cm2, procured from Good Fellow, UK). The present measured cross sections have been compared with theoretical values calculated using the Dirac-Hartree-Slater(DHS) model based fluorescence and Coster-Kronig yields, Dirac-Fock(DF) model based X-ray emission rates and two sets of L1 sub-shell photoionization cross sections based on the non-relativistic Hartree-Fock-Slater(HFS) model and those deduced from the self-consistent Dirac-Hartree-Fock(DHF) model based total photoionization cross sections. The present measured XRP cross sections for 66Dy as well as for its compounds for the L2,3 and L4 X-rays, are found to be higher by ~14-36% than the two calculated set values. It is worth to be mentioned that L2,3 and L4 X-ray lines are originated by filling up of the L1 sub-shell vacancies by the outer sub-shell (N2,3 and O2,3) electrons which are much more sensitive to the chemical environment around the central atom. The present observed differences between measured and theoretical values are expected due to combined influence of the many-body effects and the chemical effects.

Keywords: chemical effects, L X-ray production cross sections, Many body effects, Synchrotron radiation

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Authors: M. Kaviani Darani, S. Bastani, M. Ghahari, P. Kardar

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In this paper the NaYF4: Yb3+, Tm3+ nanocrystals were synthesized by hydrothermal method. Different chelating ligand type (citric acid, butanoic acid, and AOT) was selected to investigate the effect of their concentration on upconversion efficiency. Crystal structure and morphology have been well characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis. Photo luminescence were recorded on a spectrophotometer equipped with 980 nm laser diode az excitation source and an integerating sphere. The products with various morphologies range from sphere to cubic, hexagonal,prism and nanorods were prepared at different ratios. The particle size was found to be dependent on the nucleation rate, which, in turn, was affected by type and concentration of ligands. The optimum amount of chelate to RE ratio was obtained 0.75, 1.5, and 1 for Citric Acid, Butanoic Acid and AOT, respectively. Emissions in the UV (1D2-3H6), blue-violet(1D2-3F4), blue (1G4-3H6), red (1G4-3F4), and NIR (1G4-3H5) were observed and were the direct result of subsequent transfers of energy from the Yb3+ ion to the Tm3+ ion.

Keywords: upconversion nanoparticles, NaYF4, lanthanide, hydrothermal

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Authors: Emrah Ersoy, Yusuf Ozcatalbas

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The aim of this study is to investigate formability of Al based closed cell metallic foams at high temperature. The foam specimens with rectangular section were produced from AlMg1Si0.6TiH20.8 alloy preform material. Bending and free bending tests based on gravity effect were applied to foam specimens at high temperatures. During the tests, the time-angular deformation relationships with various temperatures were determined. Deformation types formed in cell walls were investigated by means of Scanning Electron Microscopy (SEM) and optical microscopy. Bending deformation about 90° was achieved without any defect at high temperatures. The importance of a critical temperature and deformation rate was emphasized in maintaining the deformation. Significant slip lines on surface of cell walls at tensile zones of bending specimen were observed. At high strain rates, the microcrack formation in boundaries of elongated grains was determined.

Keywords: Al alloy, Closed cell, Hot deformation, Metallic foam

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Authors: Sergey N. Ermoliev, Margarita A. Belousova, Aida D. Goncharenko

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Application of the diagnostic complex of highly informative functional methods (electromyography, reodentography, laser Doppler flowmetry, reoperiodontography, vital computer capillaroscopy, optical tissue oximetry, laser fluorescence diagnosis) allows to perform a multifactorial analysis of the dental status and to prescribe complex etiopathogenetic treatment. Introduction. It is necessary to create a complex of innovative highly informative and safe functional diagnostic methods for improvement of the quality of patient treatment by the early detection of stomatologic diseases. The purpose of the present study was to investigate the etiology and pathogenesis of functional disorders identified in the pathology of hard tissue, dental pulp, periodontal, oral mucosa and chewing function, and the creation of new approaches to the diagnosis of dental diseases. Material and methods. 172 patients were examined. Density of hard tissues of the teeth and jaw bone was studied by intraoral ultrasonic densitometry (USD). Electromyographic activity of masticatory muscles was assessed by electromyography (EMG). Functional state of dental pulp vessels assessed by reodentography (RDG) and laser Doppler flowmetry (LDF). Reoperiodontography method (RPG) studied regional blood flow in the periodontal tissues. Microcirculatory vascular periodontal studied by vital computer capillaroscopy (VCC) and laser Doppler flowmetry (LDF). The metabolic level of the mucous membrane was determined by optical tissue oximetry (OTO) and laser fluorescence diagnosis (LFD). Results and discussion. The results obtained revealed changes in mineral density of hard tissues of the teeth and jaw bone, the bioelectric activity of masticatory muscles, regional blood flow and microcirculation in the dental pulp and periodontal tissues. LDF and OTO methods estimated fluctuations of saturation level and oxygen transport in microvasculature of periodontal tissues. With LFD identified changes in the concentration of enzymes (nicotinamide, flavins, lipofuscin, porphyrins) involved in metabolic processes Conclusion. Our preliminary results confirmed feasibility and safety the of intraoral ultrasound densitometry technique in the density of bone tissue of periodontium. Conclusion. Application of the diagnostic complex of above mentioned highly informative functional methods allows to perform a multifactorial analysis of the dental status and to prescribe complex etiopathogenetic treatment.

Keywords: electromyography (EMG), reodentography (RDG), laser Doppler flowmetry (LDF), reoperiodontography method (RPG), vital computer capillaroscopy (VCC), optical tissue oximetry (OTO), laser fluorescence diagnosis (LFD)

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Authors: Abiola A. Ojesanmi, Eric O. Amonsou

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The formation of soluble complexes is usually within a narrow pH range characterized by weak interactions. Moreover, the rigid conformation of globular proteins restricts the number of charged groups capable of interacting with polysaccharides, thereby limiting food applications. Hence, this study investigated the impact of tryptic-limited hydrolysis on the formation of Bambara protein-gum arabic soluble complexes formation. The electrostatic interactions were monitored through turbidimetry analysis. The Bambara protein hydrolysates at a specified degree of hydrolysis, and DHs (2, 5, and 7.5) were characterized using size exclusion chromatography, zeta potential, surface hydrophobicity, and intrinsic fluorescence. The stability of the complexes was investigated using differential scanning calorimetry and rheometry. The limited tryptic hydrolysis significantly widened the pH range of the formation of soluble complexes, with DH 5 having a wider range (pH 7.0 - 4.3) compared to DH 2 and DH 7.5, while there was no notable difference in the optimum complexation pH of the insoluble complexes. Larger peptides (140, 118 kDa) were detected in DH 2 relative to 144, 70, and 61 kDa in DH 5, which were larger than 140, 118, 48, and 32 kDa in DH 7. 5. An increase in net negative charge (- 30 Mv for DH 7.5) and a slight shift in the net neutrality (from pH 4.9 to 4.3) of the hydrolysates were observed which consequently impacted the electrostatic interaction with gum arabic. There was exposure of the hydrophobic amino acids up to 4-fold in comparison with the isolate and a red shift in maximum fluorescence wavelength in DH dependent manner following the hydrolysis. The denaturation temperature of the soluble complex from the hydrolysates shifted to higher values, having DH 5 with the maximum temperature (94.24 °C). A highly interconnected gel-like soluble complex network was formed having DH 5 with a better structure relative to DH 2 and 7.5. The study showed the use of limited tryptic hydrolysis at DH 5 as an effective approach to modify Bambara protein and provided a more stable and wider pH range of formation for soluble complex, thereby enhancing the food application.

Keywords: Bambara groundnut, gum arabic, interaction, soluble complex

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Authors: Thiago E. Goto, Carla C. Lopes, Helena B. Nader, Anielle C. A. Silva, Noelio O. Dantas, José R. Siqueira Jr., Luciano Caseli

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Quantum dots (QD) are semiconductor nanocrystals that can be employed in biological research as a tool for fluorescence imagings, having the potential to expand in vivo and in vitro analysis as cancerous cell biomarkers. Particularly, cadmium selenide (CdSe) magic-sized quantum dots (MSQDs) exhibit stable luminescence that is feasible for biological applications, especially for imaging of tumor cells. For these facts, it is interesting to know the mechanisms of action of how such QDs mark biological cells. For that, simplified models are a suitable strategy. Among these models, Langmuir films of lipids formed at the air-water interface seem to be adequate since they can mimic half a membrane. They are monomolecular films formed at liquid-gas interfaces that can spontaneously form when organic solutions of amphiphilic compounds are spread on the liquid-gas interface. After solvent evaporation, the monomolecular film is formed, and a variety of techniques, including tensiometric, spectroscopic and optic can be applied. When the monolayer is formed by membrane lipids at the air-water interface, a model for half a membrane can be inferred where the aqueous subphase serve as a model for external or internal compartment of the cell. These films can be transferred to solid supports forming the so-called Langmuir-Blodgett (LB) films, and an ampler variety of techniques can be additionally used to characterize the film, allowing for the formation of devices and sensors. With these ideas in mind, the objective of this work was to investigate the specific interactions of CdSe MSQDs with tumorigenic and non-tumorigenic cells using Langmuir monolayers and LB films of lipids and specific cell extracts as membrane models for diagnosis of cancerous cells. Surface pressure-area isotherms and polarization modulation reflection-absorption spectroscopy (PM-IRRAS) showed an intrinsic interaction between the quantum dots, inserted in the aqueous subphase, and Langmuir monolayers, constructed either of selected lipids or of non-tumorigenic and tumorigenic cells extracts. The quantum dots expanded the monolayers and changed the PM-IRRAS spectra for the lipid monolayers. The mixed films were then compressed to high surface pressures and transferred from the floating monolayer to solid supports by using the LB technique. Images of the films were then obtained with atomic force microscopy (AFM) and confocal microscopy, which provided information about the morphology of the films. Similarities and differences between films with different composition representing cell membranes, with or without CdSe MSQDs, was analyzed. The results indicated that the interaction of quantum dots with the bioinspired films is modulated by the lipid composition. The properties of the normal cell monolayer were not significantly altered, whereas for the tumorigenic cell monolayer models, the films presented significant alteration. The images therefore exhibited a stronger effect of CdSe MSQDs on the models representing cancerous cells. As important implication of these findings, one may envisage for new bioinspired surfaces based on molecular recognition for biomedical applications.

Keywords: biomembrane, langmuir monolayers, quantum dots, surfaces

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Authors: Mai M. Khalaf, Hany M. Abd El-Lateef

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A new good application for the sol gel method is to improve the corrosion inhibition properties of carbon steel by the dip coating method of Nano TiO2 films and its modification with Poly Ethylene Glycol (PEG). The prepared coating samples were investigated by different techniques, X-ray diffraction, Scanning Electron Microscopy (SEM), transmission electron microscopy and Energy Dispersive X-ray Spectroscopy (EDAX). The corrosion inhibition performance of the blank carbon steel and prepared coatings samples were evaluated in 0.5 M H2SO4 by using Electrochemical Impedance Spectroscopy (EIS) and potentiodynamic polarization measurements. The results showed that corrosion resistance of carbon steel increases with increasing the number of coated layers of both nano–TiO2 films and its modification of PEG. SEM-EDAX analyses confirmed that the percentage atomic content of iron for the carbon steel in 0.5 M H2SO4 is 83% and after the deposition of the steel in nano TiO2 sol and that with PEG are 94.3% and 93.7% respectively.

Keywords: dip-coatings, corrosion protection, sol gel, TiO2 films, PEG

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Authors: C. L. Popa, S. L. Iconaru, A. Costescu, C. S. Ciobanu, M. Motelica Heino, R. Guegan, D. Predoi

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Surface functionalization of ceramic composites with a special focus on tetraethyl orthosilicate (TEOS) and hydroxyapatite (HAp) is discoursed. Mesoporous ceramic HAp-TEOS composites were prepared by the incorporation of hydroxyapatite into tetraethyl orthosilicate by sol-gel method. The resulting samples were analysed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, and Raman spectroscopy and nitrogen physisorption. The removal of Pb2+ ions from aqueous solutions was evaluated using Atomic Absorbtion Spectroscopy (AAS). Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled Pb2+ at pH ~ 3 and pH ~ 5. After removal experiment of Pb2+ at pH 3 and pH 5, porous hydroxyapatite nanoparticles is transformed into PbHAp_3 and PbHAp_5 via the adsorption of Pb2+ ions followed by the cation exchange reaction. The diffraction patterns show that THAp nanoparticles were successfully coated with teos without any structural changes. On the other, the AAS analysis showed that THAp can be useful in the removal Pb2+ from water contaminated.

Keywords: teos, hydroxyapatite, environment applications, biosystems engineering

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Authors: Stephen Rathinaraj Benjamin, Flavio Colmati Junior, Maria Izabel Florindo Guedes, Rosa Amalia Fireman Dutra

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A new enzymatic electrochemical biosensor based on multiwall carbon nanotubes and cerium oxide nanoparticles for the detection of rutin has been developed. The cerium oxide nanoparticles /HRP/ multiwall carbon nanotubes/ carbon paste electrode (HRP/ CeO2/MWCNTs/CPE) was prepared by ensuing addition of MWCNTs and HRP on the CPE, followed by the mixing with cerium oxide nanoparticles. Surface physical characteristics of the modified electrode and the electrochemical properties of the composite were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), cylic voltammetry (CV), differential pulse voltammetry (DPV) and square wave voltammetry (SWV). The HRP/ CeO2/MWCNTs/CPE showed good selectivity, stability and reproducibility, which was further applied to detect rutin tablet and capsule samples with satisfactory results.

Keywords: cerium dioxide nanoparticles, horseradish peroxidase, multiwall carbon nanotubes, rutin

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Authors: Lamia L. G. Al-Mahamad, Benjamin R. Horrocks, Andrew Houlton

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Hydrogels based on metal coordination polymers of nucleosides and a range of metal ions (Au, Ag, Cu) have been prepared and characterized by atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, ultraviolet-visible absorption spectroscopy, and powder X-ray diffraction. AFM images of the xerogels revealed the formation of extremely long polymer molecules (> 10 micrometers, the maximum scan range). This result is also consistent with TEM images which show a fibrous morphology. Oxidative doping of the Au-nucleoside fibres produces an electrically conductive nanowire. No sharp Bragg peaks were found at the at the X-ray diffraction pattern for metal ions hydrogels indicating that the samples were amorphous, but instead the data showed broad peaks in the range 20 < Q < 40 and correspond to distances d=2μ/Q. The data was analysed using a simplified Rietveld method by fitting a regression model to obtain the distance between atoms.

Keywords: hydrogel, metal ions, nanowire, nucleoside

Procedia PDF Downloads 263

Authors: V. K. Rajaletchumy, S. L. Chia, M. I. Setyawati, M. S. Muthu, S. S. Feng, D. T. Leong

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Triple negative breast cancers (TNBC) can be classified as one of the most aggressive with a high rate of local recurrences and systematic metastases. TNBCs are insensitive to existing hormonal therapy or targeted therapies such as the use of monoclonal antibodies, due to the lack of oestrogen receptor (ER) and progesterone receptor (PR) and the absence of overexpression of human epidermal growth factor receptor 2 (HER2) compared with other types of breast cancers. The absence of targeted therapies for selective delivery of therapeutic agents into tumours, led to the search for druggable targets in TNBC. In this study, we developed a targeted micellar system of cetuximab-conjugated micelles of D-α-tocopheryl polyethylene glycol succinate (vitamin E TPGS) for targeted delivery of docetaxel as a model anticancer drug for the treatment of TNBCs. We examined the efficacy of our micellar system in xenograft models of triple negative breast cancers and explored the effect of the micelles on post-treatment tumours in order to elucidate the mechanism underlying the nanomedicine treatment in oncology. The targeting micelles were found preferentially accumulated in tumours immediately after the administration of the micelles compare to normal tissue. The fluorescence signal gradually increased up to 12 h at the tumour site and sustained for up to 24 h, reflecting the increases in targeted micelles (TPFC) micelles in MDA-MB-231/Luc cells. In comparison, for the non-targeting micelles (TPF), the fluorescence signal was evenly distributed all over the body of the mice. Only a slight increase in fluorescence at the chest area was observed after 24 h post-injection, reflecting the moderate uptake of micelles by the tumour. The successful delivery of docetaxel into tumour by the targeted micelles (TPDC) exhibited a greater degree of tumour growth inhibition than Taxotere® after 15 days of treatment. The ex vivo study has demonstrated that tumours treated with targeting micelles exhibit enhanced cell cycle arrest and attenuated proliferation compared with the control and with those treated non-targeting micelles. Furthermore, the ex vivo investigation revealed that both the targeting and non-targeting micellar formulations shows significant inhibition of cell migration with migration indices reduced by 0.098- and 0.28-fold, respectively, relative to the control. Overall, both the in vivo and ex vivo data increased the confidence that our micellar formulations effectively targeted and inhibited EGF-overexpressing MDA-MB-231 tumours.

Keywords: biodegradable polymers, cancer nanotechnology, drug targeting, molecular biomaterials, nanomedicine

Procedia PDF Downloads 281

Authors: Khamael M. Abualnaja, Lidija Šiller, Benjamin R. Horrocks

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Metal-enhanced luminescence of silicon nano crystals (SiNCs) was determined using two different particle sizes of silver nano particles (AgNPs). SiNCs have been characterized by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR) and X-ray photo electron spectroscopy (XPS). It is found that the SiNCs are crystalline with an average diameter of 65 nm and FCC lattice. AgNPs were synthesized using photochemical reduction of AgNO3 with sodium dodecyl sulphate (SDS). The enhanced luminescence of SiNCs by AgNPs was evaluated by confocal Raman microspectroscopy. Enhancement up to ×9 and ×3 times were observed for SiNCs that mixed with AgNPs which have an average particle size of 100 nm and 30 nm, respectively. Silver NPs-enhanced luminescence of SiNCs occurs as a result of the coupling between the excitation laser light and the plasmon bands of AgNPs; thus this intense field at AgNPs surface couples strongly to SiNCs.

Keywords: silver nanoparticles, surface enhanced raman spectroscopy (SERS), silicon nanocrystals, luminescence

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Authors: Harpreet Singh Kainth

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Rubidium salts have been commonly used as an electrolyte to improve the efficiency cycle of Li-ion batteries. In recent years, it has been implemented into the large scale for further technological advances to improve the performance rate and better cyclability in the batteries. X-ray absorption spectroscopy (XAS) is a powerful tool for obtaining the information in the electronic structure which involves the chemical state analysis in the active materials used in the batteries. However, this technique is not well suited for the industrial applications because it needs a synchrotron X-ray source and special sample file for in-situ measurements. In contrast to this, conventional wavelength dispersive X-ray fluorescence (WDXRF) spectrometer is nondestructive technique used to study the chemical shift in all transitions (K, L, M, …) and does not require any special pre-preparation planning. In the present work, the fluorescent Lα, Lβ₁ , Lβ₃,₄ and Lγ₂,₃ X-ray spectra of rubidium in different chemical forms (Rb₂CO₃ , RbCl, RbBr, and RbI) have been measured first time with high resolution wavelength dispersive X-ray fluorescence (WDXRF) spectrometer (Model: S8 TIGER, Bruker, Germany), equipped with an Rh anode X-ray tube (4-kW, 60 kV and 170 mA). In ₃₇Rb compounds, the measured energy shifts are in the range (-0.45 to - 1.71) eV for Lα X-ray peak, (0.02 to 0.21) eV for Lβ₁ , (0.04 to 0.21) eV for Lβ₃ , (0.15 to 0.43) eV for Lβ₄ and (0.22 to 0.75) eV for Lγ₂,₃ X-ray emission lines. The chemical shifts in rubidium compounds have been measured by considering Rb₂CO₃ compounds taking as a standard reference. A Voigt function is used to determine the central peak position of all compounds. Both positive and negative shifts have been observed in L shell emission lines. In Lα X-ray emission lines, all compounds show negative shift while in Lβ₁, Lβ₃,₄, and Lγ₂,₃ X-ray emission lines, all compounds show a positive shift. These positive and negative shifts result increase or decrease in X-ray energy shifts. It looks like that ligands attached with central metal atom attract or repel the electrons towards or away from the parent nucleus. This pulling and pushing character of rubidium affects the central peak position of the compounds which causes a chemical shift. To understand the chemical effect more briefly, factors like electro-negativity, line intensity ratio, effective charge and bond length are responsible for the chemical state analysis in rubidium compounds. The effective charge has been calculated from Suchet and Pauling method while the line intensity ratio has been calculated by calculating the area under the relevant emission peak. In the present work, it has been observed that electro-negativity, effective charge and intensity ratio (Lβ₁/Lα, Lβ₃,₄/Lα and Lγ₂,₃/Lα) are inversely proportional to the chemical shift (RbCl > RbBr > RbI), while bond length has been found directly proportional to the chemical shift (RbI > RbBr > RbCl).

Keywords: chemical shift in L emission lines, bond length, electro-negativity, effective charge, intensity ratio, Rubidium compounds, WDXRF spectrometer

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Authors: Marisa Chrysochoou, James Mahoney, Kay Wille

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Pyrrhotite is an iron-sulfide mineral which releases sulfuric acid when exposed to water and oxygen. The presence of this mineral in concrete foundations across Connecticut and Massachusetts in the US is causing in some cases premature failure. This has resulted in a devastating crisis for all parties affected by this type of failure which can take up to 15-25 years before internal damage becomes visible on the surface. This study shares laboratory results aimed to investigate the fundamental mechanisms of pyrrhotite reaction and to further the understanding of its deterioration kinetics within concrete. This includes the following analyses: total sulfur, wavelength dispersive X-ray fluorescence, expansion, reaction rate combined with ion-chromatography, as well as damage evolution using electro-chemical acceleration. This information is coupled to a statistical analysis of over 150 analyzed concrete foundations. Those samples were obtained and process using a developed and validated sampling method that is minimally invasive to the foundation in use, provides representative samples of the concrete matrix across the entire foundation, and is time and cost-efficient. The processed samples were then analyzed using a developed modular testing method based on total sulfur and wavelength dispersive X-ray fluorescence analysis to quantify the amount of pyrrhotite. As part of the statistical analysis the results were grouped into the following three categories: no damage observed and no pyrrhotite detected, no damage observed and pyrrhotite detected and damaged observed and pyrrhotite detected. As expected, a strong correlation between amount of pyrrhotite, age of the concrete and damage is observed. Information from the laboratory investigation and from the statistical analysis of field samples will aid in forming a scientific basis to support the decision process towards sustainable financial and administrative solutions by state and local stakeholders.

Keywords: concrete, pyrrhotite, risk of failure, statistical analysis

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Authors: Parvaneh Eskandari, Rachel O'Reilly

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In the last years, controlling the self-assembly behavior of stimuli-responsive nano-objects, including micelles, vesicles, worm-like, etc., at different conditions is considered a pertinent challenge in the polymer community. The aim of the project was to synthesize aggregation-induced emission (AIE)-active stimuli-responsive polymeric nano-objects to control the self-assemblies morphologies of the prepared nano-objects. Two types of nanoobjects, micelle and vesicles, including PDMAEMA-b-P(BzMA-TPEMA) [PDMAEMA: poly(N,Ndimethylaminoethyl methacrylate); P(BzMA-TPEMA): poly[benzyl methacrylate-co- tetraphenylethene methacrylate]] were synthesized by using reversible addition−fragmentation chain-transfer (RAFT)- mediated polymerization-induced self-assembly (PISA), which combines polymerization and self-assembly in a single step. Transmission electron microscope and dynamic light scattering (DLS) analysis were used to confirm the formed self-assemblies morphologies. The controlled self-assemblies were applied as nitrophenolic compounds (NPCs) adsorbents from wastewater, thanks to their CO2-responsive part, PDMAEMA. Moreover, the fluorescence-active part of the prepared nano-objects, P(BzMA-TPEMA), played a key role in the detection of the NPCs at the aqueous solution. The optical properties of the prepared nano-objects were studied by UV/Vis and fluorescence spectroscopies. For responsivity investigations, the hydrodynamic diameter and Zeta-potential (ζ-potential) of the sample's aqueous solution were measured by DLS. In the end, the prepared nano-objects were used for the detection and adsorption of different NPCs.

Keywords: aggregation-induced emission polymers, stimuli-responsive polymers, reversible addition−fragmentation chain-transfer polymerization, polymerization-induced self-assembly, wastewater treatment

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Authors: Seyedmahdi Mousavihashemi

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Natural Akermanite (NAM) has been successfully prepared by a modified sol-gel method. Optimization in calcination temperature and mechanical ball milling resulted in a pure and nano-sized powder which characterized by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier transform infrared Spectroscopy (FT–IR). We hypothesized that nano-sized Akermanite (AM) would mimic more efficiently the nanocrystal structure and function of natural bone apatite, owing to the higher surface area, compare to conventional micron-size Akermanite (AM). Accordingly, we used the unique advantage of nanotechnology to improve novel nano akermanite particles as a potential candidate for bone tissue regeneration whether as a per implant filling powder or in combination with other biomaterials as a composite scaffold. Pure Akermanite (PAM) powders were successfully obtained via a simple sol-gel method followed by calcination at 1250 °C. Mechanical grinding in a ceramic ball mill for 7 hours resulted in akermanite (AM) nanoparticles in the range of about 30- 45 nm.

Keywords: biomedical engineering, nano composite, SEM, TEM

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