Search results for: nanoporous oxides

Authors: Chandni Rani, S. D. Tiwari

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

Keywords: nanoparticles, magnetism, superparamagnetism, magnetic anisotropy

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Authors: Sabina Żołędowska, Tadeusz Ossowski, Robert Bogdanowicz, Jacek Ryl, Paweł Rostkowski, Michał Kruczkowski, Michał Sobaszek, Zofia Cebula, Grzegorz Skowierzak, Paweł Jakóbczyk, Lilit Hovhannisyan, Paweł Ślepski, Iwona Kaczmarczyk, Mattia Pierpaoli, Bartłomiej Dec, Dawid Nidzworski

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The circular economy of water presents a pressing environmental challenge in our society. Water contains various harmful substances, such as drugs, antibiotics, hormones, and dioxides, which can pose silent threats. Water pollution has severe consequences for aquatic ecosystems. It disrupts the balance of ecosystems by harming aquatic plants, animals, and microorganisms. Water pollution poses significant risks to human health. Exposure to toxic chemicals through contaminated water can have long-term health effects, such as cancer, developmental disorders, and hormonal imbalances. However, effective remediation systems can be implemented to remove these contaminants using electrocatalytic processes, which offer an environmentally friendly alternative to other treatment methods, and one of them is the innovative iCLARE system. The project's primary focus revolves around a few main topics: Reactor design and construction, selection of a specific type of reticulated vitreous carbon foams (RVC), analytical studies of harmful contaminants parameters and AI implementation. This high-performance electrochemical reactor will be build based on a novel type of electrode material. The proposed approach utilizes the application of reticulated vitreous carbon foams (RVC) with deposited modified metal oxides (MMO) and diamond thin films. The following setup is characterized by high surface area development and satisfactory mechanical and electrochemical properties, designed for high electrocatalytic process efficiency. The consortium validated electrode modification methods that are the base of the iCLARE product and established the procedures for the detection of chemicals detection: - deposition of metal oxides WO3 and V2O5-deposition of boron-doped diamond/nanowalls structures by CVD process. The chosen electrodes (porous Ferroterm electrodes) were stress tested for various parameters that might occur inside the iCLARE machine–corosis, the long-term structure of the electrode surface during electrochemical processes, and energetic efficacy using cyclic polarization and electrochemical impedance spectroscopy (before and after electrolysis) and dynamic electrochemical impedance spectroscopy (DEIS). This tool allows real-time monitoring of the changes at the electrode/electrolyte interphase. On the other hand, the toxicity of iCLARE chemicals and products of electrolysis are evaluated before and after the treatment using MARA examination (IBMM) and HPLC-MS-MS (NILU), giving us information about the harmfulness of using electrode material and the efficiency of iClare system in the disposal of pollutants. Implementation of data into the system that uses artificial intelligence and the possibility of practical application is in progress (SensDx).

Keywords: waste water treatement, RVC, electrocatalysis, paracetamol

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Authors: Karkour Selma

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We conducted first principles full potential calculations using the Wien2k code to explore the structural, electronic, magnetic, and optical properties of SiNi₂O₄, a cubic normal spinel oxide. Our calculations, based on the GGA-PBEsol of the generalized gradient approximation, revealed several key findings. The spinel oxides exhibited a stable cubic structure in the ferromagnetic phase and showed 100% spin polarization. We determined the equilibrium lattice constant and internal parameter values. In terms of the electronic properties, we observed a direct bandgap of 2.68 eV for the spin-up configuration, while the spin-down configuration exhibited an indirect bandgap of 0.82 eV. Additionally, we calculated the total density of states and partial densities for each atom, finding a magnetic moment spin density of states of 8.0 μB per formula unit. The optical properties have been calculated. The real, Ԑ₁(ω) and the imaginary, Ԑ₂(ω) parts of the complex dielectric constants, refractivity, reflection and energy loss when light scattered from the material. The absorption region spanned from 1.5 eV to 14 eV, with significant intensity. The calculated results confirm the suitability of this material for optical and spintronic devices application.

Keywords: DFT, spintronic, GGA, spinel

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Authors: Gabriel K. Nzulu, Hans Högberg, Per Eklund, Lars Hultman, Martin Magnuson

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X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX) are applied to investigate the properties of rock samples from a drill hole from the Kubi Gold Project of the Asante Gold Corporation near Dunwka-on-Offin in the Central Region of Ghana. The distribution of these minerals in the rocks were observed in the drill hole sections. X-ray diffraction indicates that the samples contain garnet, pyrite, periclase, and quartz as the main indicator minerals. SEM revealed morphologies of these minerals. From EDX and XPS, Fe, Mg, Al, S, O, Hg, Ti, Mn, Na, Ag, Au, Cu, Si, and K are identified as the pathfinder elements in the area that either form alloys with gold or inherent elements in the sediments. This finding can be ascribed to primary geochemical distribution, which developed from crystallization of magma and hydrothermal liquids as well as the movement of metasomatic elements and the precipitous rate of chemical weathering of lateralization in secondary processes. The results indicate that Au mineralization in the Kubi Mine area is controlled by garnet, pyrite, goethite, and kaolinite that grades up to the surface (oxides) with hematite and limonite alterations.

Keywords: gold, minerals, pathfinder element, spectroscopy, X-ray

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Authors: Charmaine Lamiel, Van Hoa Nguyen, Marjorie Baynosa, Jae-Jin Shim

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Electrochemical supercapacitors have attracted considerable attention because of their high potential as an efficient energy storage system. The combination of carbon-based material and transition metal oxides/sulfides are studied because they have long and improved cycle life as well as high energy and power densities. In this study, a hierarchical mesoporous carbon sphere/nickel cobalt sulfide (CS/Ni-Co-S) core/shell structure was synthesized using a facile hydrothermal method without any further sulfurization or post-heat treatment. The CS/Ni-Co-S core/shell microstructures exhibited a high capacitance of 724 F g−1 at 2 A g−1 in a 6 M KOH electrolyte. After 2000 charge-discharge cycles, it retained 86.1% of its original capacitance, with high Coulombic efficiency of 97.9%. The electrode exhibited a high energy density of 58.0 Wh kg−1 at an energy density of 1440 W kg−1, and high power density of 7200 W kg−1 at an energy density of 34.2 Wh kg−1. The successful synthesis was considered to be simple and cost-effective which supports the viability of this composite as an alternative activated material for high performance supercapacitors.

Keywords: carbon sphere, electrochemical, hydrothermal, nickel cobalt sulfide, supercapacitor

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Authors: Qasem Drmosh, Zain Yamai, Amar Mohamedkhair, Abdulmajid Hendi

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In recent years, there has been a growing interest in the reduction of the nitrogen oxides NOx (NO2, NO) gases resulting from automotive or combustion emissions. Recently, metal additives in nanometer dimension onto the surface of SnO2 nanorods, nanowires and nanotubes sensitizer to further increase the sensor response have been used. In contrast, there is a lack study focused on modifying the surface of SnO2 thin films by nanoparticles. The challenge in case of thin films is how to fabricate these nanoparticles on the surfaces in cost-effective method, high purity as well as without hampering electrical and topographical properties. Here in this report, a simple and facile strategy has been demonstrated to acquire high sensitive and fast response NO2 gas sensor. Structural, electrical, morphological, optical, and compositional properties of the fabricated sensors were investigated through different analytical technique including X-ray diffraction (XRD), Field emission scanning emission microscope (FESEM) and X-ray photoelectron spectroscopy (XPS). The sensing performance of the prepared sensors are studied at different temperatures for various concentrations of NO2 and compared with pristine SnO2 film.

Keywords: NO2 sensor, SnO2, sputtering, thin films

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Authors: Alok Tiwari, Ming Show Wong

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Lanthanum (La) doped Barium Tin Oxide (BaSnO₃) film is an excellent alternative for expensive Transparent Conducting Oxides (TCOs) film such as Indium Tin Oxide (ITO). However single crystal film of La-doped BaSnO₃ has been reported with a good amount of conductivity and transparency but in order to improve its reachability, it is important to grow doped BaSO₃ films on an inexpensive substrate. La-doped BaSnO₃ thin films have been grown on quartz substrate by Radio Frequency (RF) sputtering at a different substrate temperature (from 200⁰C to 750⁰C). The thickness of the film measured was varying from 360nm to 380nm with varying substrate temperature. Structure, optical and electrical properties have been studied. The carrier concentration is seen to be decreasing as we enhance the substrate temperature while mobility found to be increased up to 9.3 cm²/V-S. At low substrate temperature resistivity found was lower (< 3x10⁻³ ohm-cm) while sudden enhancement was seen as substrate temperature raises and the trend continues further with increasing substrate temperature. Optical transmittance is getting better with higher substrate temperature from 70% at 200⁰C to > 80% at 750⁰C. Overall, understanding of changes in microstructure, electrical and optical properties of a thin film by varying substrate temperature has been reported successfully.

Keywords: conductivity, perovskite, mobility, TCO film

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Authors: Junkal Gutierrez, Hernane S. Barud, Sidney J. L. Ribeiro, Agnieszka Tercjak

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Nowadays the interest on green nanocomposites and on the development of more environmental friendly products has been increased. Bacterial cellulose has been recently investigated as an attractive environmentally friendly material for the preparation of low-cost nanocomposites. The formation of cellulose by laboratory bacterial cultures is an interesting and attractive biomimetic access to obtain pure cellulose with excellent properties. Additionally, properties as molar mass, molar mass distribution, and the supramolecular structure could be control using different bacterial strain, culture mediums and conditions, including the incorporation of different additives. This kind of cellulose is a natural nanomaterial, and therefore, it has a high surface-to-volume ratio which is highly advantageous in composites production. Such property combined with good biocompatibility, high tensile strength, and high crystallinity makes bacterial cellulose a potential material for applications in different fields. The aim of this investigation work was the fabrication of novel hybrid inorganic-organic composites based on bacterial cellulose, cultivated in our laboratory, as a template. This kind of biohybrid nanocomposites gathers together excellent properties of bacterial cellulose with the ones displayed by typical inorganic nanoparticles like optical, magnetic and electrical properties, luminescence, ionic conductivity and selectivity, as well as chemical or biochemical activity. In addition, the functionalization of cellulose with inorganic materials opens new pathways for the fabrication of novel multifunctional hybrid materials with promising properties for a wide range of applications namely electronic paper, flexible displays, solar cells, sensors, among others. In this work, different pathways for fabrication of multifunctional biohybrid nanopapers with tunable properties based on BC modified with amphiphilic poly(ethylene oxide-b-propylene oxide-b-ethylene oxide) (EPE) block copolymer, sol-gel synthesized nanoparticles (titanium, vanadium and a mixture of both oxides) and functionalized iron oxide nanoparticles will be presented. In situ (biosynthesized) and ex situ (at post-production level) approaches were successfully used to modify BC membranes. Bacterial cellulose based biocomposites modified with different EPE block copolymer contents were developed by in situ technique. Thus, BC growth conditions were manipulated to fabricate EPE/BC nanocomposite during the biosynthesis. Additionally, hybrid inorganic/organic nanocomposites based on BC membranes and inorganic nanoparticles were designed via ex-situ method, by immersion of never-dried BC membranes into different nanoparticle solutions. On the one hand, sol-gel synthesized nanoparticles (titanium, vanadium and a mixture of both oxides) and on the other hand superparamagnetic iron oxide nanoparticles (SPION), Fe2O3-PEO solution. The morphology of designed novel bionanocomposites hybrid materials was investigated by atomic force microscopy (AFM) and scanning electron microscopy (SEM). In order to characterized obtained materials from the point of view of future applications different techniques were employed. On the one hand, optical properties were analyzed by UV-vis spectroscopy and spectrofluorimetry and on the other hand electrical properties were studied at nano and macroscale using electric force microscopy (EFM), tunneling atomic force microscopy (TUNA) and Keithley semiconductor analyzer, respectively. Magnetic properties were measured by means of magnetic force microscopy (MFM). Additionally, mechanical properties were also analyzed.

Keywords: bacterial cellulose, block copolymer, advanced characterization techniques, nanoparticles

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Authors: Jenaidullah Batur, Sebghatullah Mudaber

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Currently, there is a list of catalysts that can reduce CO₂ to valuable chemicals and fuels, among them metal oxides such as TiO₂, known as promising photocatalysts to produce hydrogen and CO unless they are at an earlier age and still need to promote activity to able for produce fabricated values. Herein, in this work, we provided a novel, facile and eco-friendly synthesis strategy to synthesize more effective TiO₂-organic composite materials to selectively reduce CO₂ to CO. In this experiment, commercial nanocrystalline TiO₂ and saccharin with Li (LiBr, LiCl) were synthesized using the facile physical grinding in the motel pestle for 10 minutes, then added 10 mL of deionized water (18.2 megaohms) on the 300mg composite catalyst before samples moving for hydrothermal heating for 24 hours at 80 C in the oven. Compared with nanosized TiO₂, the new TiO₂-Sac-Li indeed displays a high CO generation rate of 70.83 μmol/g/h, which is 7 times higher than TiO₂, which shows enhancement in CO₂ reduction and an apparent improvement in charge carrier dynamic. The CO₂ reduction process at the gas-solid interface on TiO₂-Sac-Li composite semiconductors is investigated by functional calculations and several characterization methods. The results indicate that CO₂ can be easily activated by the TiO₂-Sac-Li atoms on the surface. This work innovatively investigates CO₂ reduction in novel composite materials and helps to broaden the applications of composite materials semiconductors.

Keywords: green chemistry, green synthesis, TiO₂, photocatalyst

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Authors: Yogendar Singh, Parasmani Rajput, Pawan Kumar Kulriya

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Understanding the radiation response of the pyrochlore structured ceramics in the nuclear reactor core-like environment is of quite an interest for their utilization as host matrices. Electronic excitation (100 MeV I7+) induced crystalline to amorphous phase transition in Nd2Zr2O7 pyrochlore synthesized through three steps solid-state sintering method was investigated. The x-ray diffraction, along with Raman spectroscopy and x-ray absorption spectroscopy experiments conducted on pristine and irradiated pyrochlore, showed an increase in the rate of amorphization with ion fluence. XRD results indicate that specimen is completely amorphized on irradiation at the highest fluence of 5×1013 ions/cm2. The EXAFS spectra of the K-Zr edge and the Nd LIII edge confirmed a significant change in the chemical environment of Nd upon swift heavy ion irradiation. Observation of a large change in the intensity of K-Zr pre-edge spectra is also a good indicator of the phase transition from pyrochlore to the amorphous phase, which is supported by the FT modulus of the LIII-Nd edge. However, the chemical environment of Zr is less affected by irradiation, but it clearly exhibits an increase in the degree of disorder.

Keywords: nuclear host matrices, swift heavy ion irradiation, x-ray absorption spectroscopy, pyrochlore oxides

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Authors: Bindhu Lal, Karnika Kochal

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Clayey soil contains clay minerals with traces of metal oxides and organic matter, which exhibits properties like low drainage, high plasticity, and shrinkage. To overcome these issues, various soil reinforcement techniques are used to elevate the stiffness, water tightness, and bearing capacity of the soil. Such techniques include cementation, bituminization, freezing, fiber inclusion, geo-synthetics, nailing, etc. Reinforcement of soil with fibers has been a cost-effective solution to soil improvement problems. An experimental study was undertaken involving the inclusion of cotton waste fibers in clayey soil as reinforcement with different fiber contents (1%, 1.5%, 2%, and 2.5% by weight) and analyzing its effects on the unconfined compressive strength of the soil. Two categories of soil were taken, comprising of natural clay and clay mixed with 5% sodium bentonite by weight. The soil specimens were subjected to proctor compaction and unconfined compression tests. The validated outcome shows that fiber inclusion has a strikingly positive impact on the compressive strength and axial strain at failure of the soil. Based on the commendatory results procured, compressive strength was found to be directly proportional to the fiber content, with the effect being more pronounced at lower water content.

Keywords: bentonite clay, clay, cotton fibers, unconfined compressive strength

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Authors: Jay J. Vora, Vishvesh J. Badheka

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This work attempts to investigate the effect of oxide fluxes on 6mm thick Reduced Activation ferritic/martensitic steels (RAFM) during Activated TIG (A-TIG) welding. Six different fluxes Al₂O₃, Co₃O₄, CuO, HgO, MoO₃, and NiO were mixed with methanol for conversion into paste and bead-on-plate experiments were then carried out. This study, systematically investigates the influence of oxide-based flux powder and carrier solvent composition on the weld bead shape, geometric shape of weld bead and dominant depth enhancing mechanism in tungsten inert gas (TIG) welding of reduced activation ferritic/martensitic (RAFM) steel. It was inferred from the study that flux Co₃O₄ and MoO₃ imparted full and secure (more than 6mm) penetration with methanol owing to dual mechanism of reversed Marangoni and arc construction. The use of methanol imparted good spreadabilty and coverability and ultimately higher peak temperatures were observed with its use owing to stronger depth enhancing mechanisms than use of acetone with same oxide fluxes and welding conditions.

Keywords: A-TIG, flux, oxides, penetration, RAFM, temperature, welding

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Authors: J. M. Muñoz, Y. Vasquez, P. Oyola, M. Rubio

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All emissions of contaminants inside of homes, offices, school and another enclosure closer that affect the health of those who inhabit or use them are cataloged how indoor pollution. The importance of this study is because individuals spend most of their time in indoors ambient. The main indoor pollutants are oxides of nitrogen (NOₓ), sulfur dioxide (SO₂), carbon monoxide (CO) and particulate matter (PM). Combustion heaters are an important source of pollution indoors. It will be measured: NOₓ, SO₂, CO, PM₂,₅ y PM₁₀ continuous and discreet form at indoor and outdoor of two households with different heating energy; kerosene and electricity (control home) respectively, in addition to environmental parameters such as temperature. With the values obtained in the 'control home' it will be possible estimate the contaminants transport from outside to inside of the household and later the contribution generated by kerosene heating. Transporting the emissions from burning kerosene to a photochemical chamber coupled to a continuous and discreet measuring system of contaminants it will be evaluated the oxidation of the emissions and formation of secondary particulate matter. It will be expected watch a contaminants transport from outside to inside of the household and the kerosene emissions present a high potential of formation secondary particulate matter.

Keywords: heating, indoor pollution, kerosene, secondary particulate matter

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Authors: E. Fathallahi Aghdam, V. Hosseini

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Environmental pollution is not limited to a specific region or country; that is why sustainable development, as a necessary process for improvement, pays attention to issues such as destruction of natural resources, degradation of biological system, global pollution, and climate change in the world, especially in the developing countries. According to the World Health Organization, as a developing city, Tehran (capital of Iran) is one of the most polluted cities in the world in terms of air pollution. In this study, three pollutants including particulate matter less than 10 microns, nitrogen oxides, and sulfur dioxide were evaluated in Tehran using data mining techniques and through Crisp approach. The data from 21 air pollution measuring stations in different areas of Tehran were collected from 1999 to 2013. Commercial softwares Clementine was selected for this study. Tehran was divided into distinct clusters in terms of the mentioned pollutants using the software. As a data mining technique, clustering is usually used as a prologue for other analyses, therefore, the similarity of clusters was evaluated in this study through analyzing local conditions, traffic behavior, and industrial activities. In fact, the results of this research can support decision-making system, help managers improve the performance and decision making, and assist in urban studies.

Keywords: data mining, clustering, air pollution, crisp approach

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Authors: Demet Tatar, Bahattin Düzgün

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In this study, we have newly developed titanium-tin oxide (TiSnO) thin films as the transparent conducting oxides materials by the spray pyrolysis technique. Tin oxide thin films doped with different Ti content were successfully grown by spray pyrolysis and they were characterized as a function of Ti content. The effect of Ti contents on the crystalline structure and optical properties of the as-deposited SnO2:Ti films was systematically investigated by X-ray diffraction (XRD), scanning electronic microscopy (SEM), atomic force microscopy (AFM), UV-vis spectrometer and photoluminecenc spectrophotometer. The X-ray diffraction patterns taken at room temperature showed that the films are polycrystalline. The preferred directions of crystal growth appeared in the difractogram of SnO2: Ti (TiTO) films were correspond to the reflections from the (110), (200), (211) and (301) planes. The grain size varies from 21.8 to 27.8 nm for (110) preferred plane. SEM and AFM study reveals the surface of TiTO to be made of nanocrystalline particles. The highest visible transmittance (570 nm) of the deposited films is 80 % for 20 wt % titanium doped tin oxide films. The obtained results revealed that the structures and optical properties of the films were greatly affected by doping levels. These films are useful as conducting layers in electro chromic and photovoltaic devices.

Keywords: transparent conducting oxide, gas sensors, SnO2, Ti, optoelectronic, spray pyrolysis

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Authors: Vikas Chawla, Buta Singh Sidhu, Amita Rani, Amit Handa

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The main objective of the present work is microstructural and mechanical characterization of the conventional and nanostructured TiAlN and AlCrN coatings deposited on T-11 boiler steel. In case of conventional coatings, Al-Cr and Ti-Al metallic powders were deposited using plasma spray process followed by gas nitriding of the surface which was done in the lab with optimized parameters after conducting several trials on plasma-sprayed coated specimens. The physical vapor deposition process (PAPVD) was employed for depositing nanostructured TiAlN and AlCrN coatings. The field emission scanning electron microscopy (FE-SEM) with energy dispersive X-ray analysis (EDAX) attachment, X-ray diffraction (XRD) analysis, atomic force microscopy (AFM) analysis and the X-Ray mapping analysis techniques have been used to study surface and cross-sectional morphology of the coatings. The surface roughness and micro-hardness were also measured. A good adhesion of the conventional thick TiAlN and AlCrN coatings was found. The coatings under study are recommended for the applications to super-heater and re-heater tubes of the boilers based upon the outcomes of the research work.

Keywords: nanostructure, physical vapour deposition, oxides, thin films, electron microscopy

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Authors: Yeon Woo Seo, Haeyoung Choi, Jung Hyun Jeong

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Recently, the UC phosphors have attracted much attention owing to their wide applicability in areas such as biological fluorescence labeling, three-dimensional color displays, temperature sensor, solar cells, white light emitting diodes (WLEDs), fiber optic communication, anti-counterfeiting and other areas. The UC efficiency is mainly dependent on the host lattice and the interaction between the host lattice and doped ions. Up to date, various host matrices, such as oxides, fluorides, vanadates and phosphates, have been investigated as efficient UC luminescent hosts. Recently, oxide materials with low phonon energy have been investigated as the host matrices of UC materials due to their high chemical durability and physical stability. A series of Sr2CeO4: Tm3+/Yb3+ phosphors with different concentrations of Yb3+ ions have been successfully prepared using the high-energy ball milling method. In this study, we reported the UC luminescent properties of Tm3+/Yb3+ ions co-doped Sr2CeO4 phosphors under an excitation wavelength of 975 nm. Furthermore, the structural and morphological characteristics, as well as the UC luminescence mechanism were investigated in detail. The X-ray diffraction patterns confirmed their orthorhombic structure. Under 975 nm excitation, the emission peaks were observed at 478 nm (blue) and 652 nm (red), corresponding to the 1G4 → 3H6 and 1G4 → 3F4 transitions of Tm3+, respectively. The optimized doping concentration of Yb3+ ion was 10 mol%.

Keywords: Strontium Cerate, up-conversion, luminescence, Tm3+, Yb3+

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Authors: Samir Hmaimou, Marouane Ait Lahcen, Mohamed Adardour, Mohamed Maatallah, Abdesselam Baouid

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Due to (3 + 2) cycloaddition and condensation reaction, a wide range of synthetic routes can be used to obtain biologically active heterocyclic compounds. Condensation and (3+2) cycloaddition reactions in heterocyclic syntheses are versatile due to the wide variety of possible combinations of several atoms of the reactants. In this article, we first outline the synthesis of benzodiazepine 4 with two dipolarophilic centers (C=C and C=N) by condensation reaction. Then, we use it for cycloaddition reactions (3+2) with nitrile oxides to prepare oxadiazole-benzodiazepines and pyrazole-benzodiazepine compounds. ¹H and ¹³C NMR are used to establish all the structures of the synthesized products. These condensation and cycloaddition reactions were then analyzed using density functional theory (DFT) calculations at the B3LYP/6-311G(d,p) theoretical level. In this study, the mechanism of the one-step cycloaddition reaction was investigated. Molecular electrostatic potential (MEP) was used to identify the electrophilic and nucleophilic attack sites of the molecules studied. Additionally, Fukui investigations (electrophilic f- and nucleophilic f+) in the various reaction centers of the reactants demonstrate that, whether in the condensation reaction or cycloaddition, the reaction proceeds through the atomic centers with the most important Fukui functions, which is in full agreement with experimental observations. In the condensation reaction, thermodynamic control of regio, chemo, and stereoselectivity is observed, while those of cycloaddition are subject to kinetic control.

Keywords: cycloaddition reaction, regioselectivity, mechanism reaction, NMR analysis

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Authors: Deepti Mishra, Arindam Modak, K. K. Pant, Xiu Song Zhao

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The promotional effect of mixed ceria-zirconia oxides (CZO) over the Mo/HZSM-5 catalyst for methane dehydroaromatization (MDA) reaction was studied. The surface and structural properties of the synthesized catalyst were characterized using a range of spectroscopic and microscopic techniques, and the correlation between catalytic properties and its performance for MDA reaction is discussed. The impregnation of CZO solid solution on Mo/HZSM-5 was observed to give an excellent catalytic performance and improved benzene formation rate (4.5 μmol/gcat. s) as compared to the conventional Mo/HZSM-5 (3.1 μmol/gcat. s) catalyst. In addition, a significant reduction in coke formation was observed in the CZO-modified Mo/HZSM-5 catalyst. The prevailing comprehension for higher catalytic activity could be because of the redox properties of CZO deposited Mo/HZSM-5, which acts as a selective oxygen supplier and performs hydrogen combustion during the reaction, which is indirectly probed by O₂-TPD and H₂-TPR analysis. The selective hydrogen combustion prevents the over-oxidation of aromatic species formed during the reaction while the generated steam helps in reducing the amount of coke generated in the MDA reaction. Thus, the advantage of CZO incorporated Mo/HZSM-5 is manifested as it promotes the reaction equilibrium to shift towards the formation of benzene which is favourable for MDA reaction.

Keywords: Mo/HZSM-5, ceria-zirconia (CZO), in-situ combustion, methane dehydroaromatization

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Authors: Sijo S. Thomas, S. Hridya, Manoj Mohan, Bibin Jacob, Hysen Thomas

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Ferrites are iron based oxides with technologically significant magnetic properties and have widespread applications in medicine, technology, and industry. There has been a growing interest in the study of magnetic, electrical and structural properties of mixed ferrites. In the present work, structural and magnetic properties of Nickel and Calcium substituted Fe₃O₄ nanoparticles were investigated. NiₓCa₁₋ₓFe₂O₄ nanoparticles (x = 0, 0.1, 0.3, 0.5, 0.7, 0.9) were synthesized by chemical co-precipitation method and the samples were subsequently sintered at 900°C. The magnetic and structural properties of NiₓCa₁₋ₓFe₂O₄ were investigated using Vibrating Sample Magnetometer and X-Ray diffraction. The XRD results revealed that the synthesized particles have nanometer size and it varies from 46-72 nm as the calcium concentration diminishes. The variation is explained based on the increase in the reaction rate with Ni concentration which favors the formation of ultrafine particles of mixed ferrites. VSM results show pure CaFe₂O₄ exhibit paramagnetic behavior with low saturation value. As the concentration of Ca decreases, a transition occurs from paramagnetic state to ferromagnetic state. When the concentration of Ni becomes dominant, magnetic saturation, coercivity, and retentivity become high, indicating near ferromagnetic behavior of the compound.

Keywords: co-precipitation, ferrites, magnetic behavior, structure

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Authors: M. Budakoglu, M. Karaman, D. Kiran, Z. Doner, B. Zeytuncu, B. Tanç, M. Kumral

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Lake Acıgöl is one of the large saline lacustrine environment in Turkey. Eleven trace metals (Cr, Mn, Fe, Al, Co, Ni, Cu, Zn, Cd, Pb and As) in 9 surface and subsurface sediment samples from the Lake Acıgöl were analyzed with the bulk and sequential extraction analysis methods by ICP-MS to obtain the metal distribution patterns in this extreme environment. Five stepped sequential extraction technique (1- exchangeable, 2- bond to carbonates, 3- bond to iron and manganese oxides/hydroxides, 4- bond to organic matter and sulphides, and 5- residual fraction incorporated into clay and silicate mineral lattices) was used to characterize the various forms of metals in the <63μ size sediments. The metal contents (ppm) and their percentages for each extraction step were reported and compared with the results obtained from the total digestion. Results indicate that sum of the four fraction are in good agreement with the total digestion results of Ni, Cd, As, Zn, Cu and Fe with the satisfactory recoveries (94.04–109.0%) and the method used is reliable and repeatable for these elements. It was found that there were high correlations between Fe vs. Ni loads in the fraction of F2 and F4 with R2= 0,91 and 0,81, respectively. Comparison of totally 135 chemical analysis results in three sampling location and for 5 fraction between Fe-Co, Co-Ni and Fe-Ni element couples were presented elevated correlations with R2=0,98, 0,92 and 0,91, respectively.

Keywords: Lake Acigol, sequancial extraction, recent lake sediment, geochemical speciation of heavy metals

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Authors: Radia Bagtache, Karima Boudjedien, Ahmed Malek Djaballah, Mohamed Trari

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The compounds with a spinel structure have received special attention because of their numerous applications in electronics, magnetism, catalysis, electrocatalysis, photocatalysis, etc. Among these oxides, CuCo₂O₄ was selected because of its optimal band gap, very close to the ideal value for solar devices, its low cost, and a potential candidate in the field of energy storage. Herein, we reported the junction Ag/CuCo₂O₄ (5/95 % wt.) prepared by co-precipitation, characterized physically and photo electrochemically. Moreover, its performance was evaluated for the oxidation of methyl orange (MO) under solar light. The X-ray diffraction exhibited narrow peaks ascribed to the spinel CuCo₂O₄ and Ag. The SEM analysis displayed grains with regular shapes. The band gap of CuCo₂O₄ (1.38 eV) was deducted from the diffuse reflectance, and this value decreased down to 1.15 eV due to the synergy effect in the junction. The current-potential (J-E) curve plotted in Na₂SO₄ electrolyte showed a medium hysteresis, characteristic of good chemical stability. The capacitance-2 – potential (C⁻² – E) graph displayed that the spinel behaves as a p-type semiconductor, a property supported by chrono-amperometry. The conduction band, located at 4.05 eV (-0.94 VNHE), was made up of Co³⁺: 3d orbital. The result showed a total discoloration of MO after 2 h of illumination under solar light.

Keywords: junction Ag/CuCo₂O₄, semiconductor, environment, sunlight, characterization, depollution

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Authors: T. A. Adesiyan, J. A. Adekoya A. Akinlua, N. Torto

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One hundred and eighty six in situ soil samples of the B–horizon were collected around Gbongan–Odeyinka-Orileowu area, southwestern Nigeria, delineated by longitude 4°15l and 4°30l and latitude 7°14l and 7°31 for a reconnaissance geochemical soil survey. The objective was to determine the distribution pattern of some trace metals in the area with a view to discovering any indication of metallic mineralization. The samples were air–dried and sieved to obtain the minus 230 µ fractions which were used for pH determinations and subjected to hot aqua regia acid digestion. The solutions obtained were analyzed for Ag, As, Au, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sn, and Zn using atomic absorption spectrometric methods. The resulting data were subjected to simple statistical treatment and used in preparing distribution maps of the elements. With these, the spatial distributions of the elements in the area were discussed. The pH of the soils range from 4.70 to 7.59 and this reflects the geochemical distribution patterns of trace metals in the area. The spatial distribution maps of the elements showed similarity in the distributions of Co, Cr, Fe, Ni, Mn and Pb. This suggests close associations between these elements none of which showed any significant anomaly in the study. The associations might be due to the scavenging actions of Fe–Mn oxides on the elements. Only Ag, Au and Sn on one hand and Zn on the other hand showed significant anomalies, which are thought to be due to mineralization and anthropogenic activities respectively.

Keywords: distribution, metals, Gbongan, Nigeria, mineralization anthropogenic

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Authors: R. Sanchez-Salcedo, N. H. Voelcker

Abstract:

Currently, low breast milk production in women is one of the leading health complications in infants. Recently, It has been demonstrated that exclusive breastfeeding, especially up to a minimum of 6 months, significantly reduces respiratory and gastrointestinal infections, which are the main causes of death in infants. However, the current data shows that a high percentage of women stop breastfeeding their children because they perceive an inadequate supply of milk, and only 45% of children are breastfeeding under 6 months. It is, therefore, clear the necessity to design and develop a biosensor that is sensitive and selective enough to identify and validate a panel of milk biomarkers that allow the early diagnosis of this condition. In this context, electrochemical biosensors could be a powerful tool for assessing all the requirements in terms of reliability, selectivity, sensitivity, cost efficiency and potential for multiplex detection. Moreover, they are suitable for the development of POC devices and wearable sensors. In this work, we report the development of two types of sensing platforms towards several biomarkers, including miRNAs and hormones present in breast milk and dysregulated in this pathological condition. The first type of sensing platform consists of an enzymatic sensor for the detection of lactose, one of the main components in milk. In this design, we used gold surface as an electrochemical transducer due to the several advantages, such as the variety of strategies available for its rapid and efficient functionalization with bioreceptors or capture molecules. For the second type of sensing platform, nanoporous silicon film (pSi) was chosen as the electrode material for the design of DNA sensors and aptasensors targeting miRNAs and hormones, respectively. pSi matrix offers a large superficial area with an abundance of active sites for the immobilization of bioreceptors and tunable characteristics, which increase the selectivity and specificity, making it an ideal alternative material. The analytical performance of the designed biosensors was not only characterized in buffer but also validated in minimally treated breastmilk samples. We have demonstrated the potential of an electrochemical transducer on pSi and gold surface for monitoring clinically relevant biomarkers associated with the heightened risk of low milk production in women. This approach, in which the nanofabrication techniques and the functionalization methods were optimized to increase the efficacy of the biosensor highly provided a foundation for further research and development of targeted diagnosis strategies.

Keywords: biosensors, electrochemistry, early diagnosis, clinical markers, miRNAs

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Authors: Andrey V. Samokhin, Nikolay V. Alekseev, Mikhail A. Sinaiskii

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The report presents the results of R&D of plasma-chemical production of W, W-Cu, W-Ni-Fe nanopowders as well as spherical micropowders of these compounds for their use in modern 3D printing technologies. Plasma-chemical synthesis of nanopowdersis based on the reduction of tungsten oxide compounds powders in a stream of hydrogen-containing low-temperature thermal plasma generated in an electric arc plasma torch. The synthesis of W-Cu and W-Ni-Fe nanocompositesiscarried out using the reduction of a mixture of the metal oxides. Using the synthesized tungsten-based nanocomposites powders, spherical composite micropowders with a submicron structure canbe manufactured by spray dryinggranulation of nanopowder suspension and subsequent densification and spheroidization of granules by melting in a low-temperature thermal plasma flow. The DC arc plasma systems are usedfor the synthesis of nanopowdersas well as for the spheroidization of microgranuls. Plasma systems have a capacity of up to 1 kg/h for nanopowder and up to 5 kg/h for spheroidized powder. All synthesized nanopowders consist of aggregated particles with sizes less than 100 nm, and nanoparticles of W-Cu and W-Ni-Fe composites have core (W) –shell (Cu or Ni-Fe) structures. The resulting dense spherical microparticles with a size of 20-60 microns have a submicron structure with a uniform distribution of metals over the particle volume. The produced tungsten-based nano- and spherical micropowderscan be used to develop new materials and manufacture products using advanced modern technologies.

Keywords: plasma, powders, production, tungsten-based

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Authors: Ainur Sharip, Jose E. Perez, Nouf Alsharif, Aldo I. M. Bandeas, Enzo D. Fabrizio, Timothy Ravasi, Jasmeen S. Merzaban, Jürgen Kosel

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Bone marrow-derived human mesenchymal stem cells (MSCs) are attractive candidates for tissue engineering and regenerative medicine, due to their ability to differentiate into osteoblasts, chondrocytes or adipocytes. Differentiation is influenced by biochemical and biophysical stimuli provided by the microenvironment of the cell. Thus, altering the mechanical characteristics of a cell culture scaffold can directly influence a cell’s microenvironment and lead to stem cell differentiation. Mesenchymal stem cells were cultured on densely packed, vertically aligned magnetic iron nanowires (NWs) and the effect of NWs on the cell cytoskeleton rearrangement and differentiation were studied. An electrochemical deposition method was employed to fabricate NWs into nanoporous alumina templates, followed by a partial release to reveal the NW array. This created a cell growth substrate with free-standing NWs. The Fe NWs possessed a length of 2-3 µm, with each NW having a diameter of 33 nm on average. Mechanical stimuli generated by the physical movement of these iron NWs, in response to a magnetic field, can stimulate osteogenic differentiation. Induction of osteogenesis was estimated using an osteogenic marker, osteopontin, and a reduction of stem cell markers, CD73 and CD105. MSCs were grown on the NWs, and fluorescent microscopy was employed to monitor the expression of markers. A magnetic field with an intensity of 250 mT and a frequency of 0.1 Hz was applied for 12 hours/day over a period of one week and two weeks. The magnetically activated substrate enhanced the osteogenic differentiation of the MSCs compared to the culture conditions without magnetic field. Quantification of the osteopontin signal revealed approximately a seven-fold increase in the expression of this protein after two weeks of culture. Immunostaining staining against CD73 and CD105 revealed the expression of antibodies at the earlier time point (two days) and a considerable reduction after one-week exposure to a magnetic field. Overall, these results demonstrate the application of a magnetic NW substrate in stimulating the osteogenic differentiation of MSCs. This method significantly decreases the time needed to induce osteogenic differentiation compared to commercial biochemical methods, such as osteogenic differentiation kits, that usually require more than two weeks. Contact-free stimulation of MSC differentiation using a magnetic field has potential uses in tissue engineering, regenerative medicine, and bone formation therapies.

Keywords: cell substrate, magnetic nanowire, mesenchymal stem cell, stem cell differentiation

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Authors: Hossein Arfaeinia, Ahmad Jonidi Jafari, Sina Dobaradaran, Sadegh Niazi, Mojtaba Ehsanifar, Amir Zahedi

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Street dust and surface soil samples were collected from very heavy, heavy, medium and low traffic areas and natural site in Tehran, Iran. These samples were analyzed for some physical–chemical features, total and chemical speciation of selected metals and metalloids (Zn, Al, Sr, Pb, Cu, Cr, Cd, Co, Ni, and V) to study the effect of traffic on their mobility and accumulation in the environment. The pH, electrical conductivity (EC), carbonates and organic carbon (OC) values were similar in soil and dust samples from similar traffic areas. The traffic increases EC contents in dust/soil matrixes but has no effect on concentrations of metals and metalloids in soil samples. Rises in metal and metalloids levels with traffic were found in dust samples. Moreover, the traffic increases the percentage of acid soluble fraction and Fe and Mn oxides associated fractions of Pb and Zn. The mobilization of Cu, Zn, Pb, Cr in dust samples was easier than in soil. The speciation of metals and metalloids except Cd is mainly affected by physicochemical features in soil, although total metals and metalloids affected the speciation in dust samples (except chromium and nickel).

Keywords: street dust, surface soil, traffic, metals, metalloids, chemical speciation

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Authors: Ayed S. Al-Shihri, Abul Kalam, Abdullah G. Al-Sehemi, Gaohui Du, Tokeer Ahmad, Ahmad Irfan

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We report here the synthesis of nickel oxide (NiO) nanoparticles by microwave-assisted method, using a common precipitating agent followed by calcination in air at 400°C. The effect of the microwave and pH on the crystallite size, morphology, structure, energy band gap and surface area of NiO have been investigated by means of powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR), ultraviolet visible spectroscopy (UV-vis) and BET surface area studies. X-ray diffraction studies showed the formation of monophasic and highly crystalline cubic NiO. TEM analysis led to decrease the average grain size of NiO nanoparticles from 16.5 nm to 14 nm on increasing the amount of NaOH. FTIR studies also confirm the formation of NiO nanoparticles. It was observed that on increasing the volume of NaOH, the optical band gap energy (2.85 eV to 2.95 eV) and specific surface area (33.1 to 39.8 m2/g) increases, however the average particles size decreases (16.5 nm to 14 nm). This method may be extended to large scale synthesis of other metal oxides nanoparticles and the present study could be used for the potential applications in water treatment and many other fields.

Keywords: BET surface area analysis, electron microscopy, optical properties, X-ray techniques

Procedia PDF Downloads 396

Authors: Saad Mohamed Elsaid Abdelrahman

Abstract:

The adsorption method is one of the best modern techniques used in removing pollutants, especially organic hydrocarbon compounds, from polluted water. Through this research, bentonite clay can be used to remove organic hydrocarbon compounds, such as heptane and octane, resulting from oil spills in seawater. Bentonite clay can be obtained from the Kholayaz area, located north of Jeddah, at a distance of 80 km. Chemical analysis shows that bentonite clay consists of a mixture of silica, alumina and oxides of some elements. Bentonite clay can be activated in order to raise its adsorption efficiency and to make it suitable for removing pollutants using an ionic organic solvent. It is necessary to study some of the factors that could be in the efficiency of bentonite clay in removing oily organic compounds, such as the time of contact of the clay with heptane and octane solutions, pH and temperature, in order to reach the highest adsorption capacity of bentonite clay. The temperature can be a few degrees Celsius higher. The adsorption capacity of the clay decreases when the temperature is raised more than 4°C to reach its lowest value at the temperature of 50°C. The results show that the friction time of 30 minutes and the pH of 6.8 is the best conditions to obtain the highest adsorption capacity of the clay, 467 mg in the case of heptane and 385 mg in the case of octane compound. Experiments conducted on bentonite clay were encouraging to select it to remove heavy molecular weight pollutants such as petroleum compounds under study.

Keywords: adsorbent, bentonite clay, oil spills, removal

Procedia PDF Downloads 88

Authors: A. A. Vasin, N. V. Klassen, A. M. Likhter

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Water suspensions of in-organic (metals and oxides) and organic nano-objects (chitozan and collagen) were subjected to the treatment of direct and alternative electrical fields. In addition to quasi-periodical spatial patterning resonance-like performance of spatial distributions of these suspensions has been found at low frequencies of alternating electrical field. These resonances are explained as the result of creation of equilibrium states of groups of charged nano-objects with opposite signs of charges at the interparticle distances where the forces of Coulomb attraction are compensated by the repulsion forces induced by relatively negative polarization of hydrated regions surrounding the nanoparticles with respect to pure water. The low frequencies of these resonances are explained by comparatively big distances between the particles and their big masses with t\respect to masses of atoms constituting molecules with high resonance frequencies. These new resonances open a new approach to detailed modeling and understanding of mechanisms of the influence of electrical fields on the functioning of internal organs of living organisms at the level of cells and neurons.

Keywords: bio-polymers, chitosan, collagen, nanoparticles, coulomb attraction, polarization repulsion, periodical patterning, electrical low frequency resonances, transformations

Procedia PDF Downloads 546