Search results for: x-ray diffraction analysis

Authors: Marwa M. Abu-Serie, Marwa M. Eltarahony

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The search for reliable, effective, and safe nanoparticles (NPs) as a treatment for cancer is a pressing priority. In this study, Cu-NPs were fabricated by Streptomyces cyaneofuscatus through simultaneous bioreduction strategy of copper nitrate salt. The as-prepared Cu-NPs subjected to structural analysis; energy-dispersive X-ray spectroscopy, elemental mapping, X-ray diffraction, transmission electron microscopy, and ζ-potential. These biological synthesized Cu-NPs were mixed with disulfiram (DS), forming a nanocomplex of Cu-DS with a size of ~135 nm. The prepared nanocomplex (nanoCu-DS) exhibited higher anticancer activity than that of free complex of DS-Cu, Cu-NPs, and DS alone. This was illustrated by the lowest IC50 of nanoCu-DS (< 4 µM) against human breast and liver cancer cell lines comparing with DS-Cu, Cu-NPs, and DS (~8, 22.98-33.51 and 11.95-14.86, respectively). Moreover, flow cytometric analysis confirmed that higher apoptosis percentage range of nanoCu-DS-treated in MDA-MB 231, MCF-7, Huh-7, and HepG-2 cells (51.24-65.28%) than free complex of Cu-DS ( < 4.5%). Regarding inhibition potency of liver and breast cancer cell migration, no significant difference was recorded between free and nanocomplex. Furthermore, nanoCu-DS suppressed gene expression of β-catenine, Akt, and NF-κB and upregulated p53 expression (> 3, >15, > 5 and ≥ 3 folds, respectively) more efficiently than free complex (all ~ 1 fold) in MDA-MB 231 and Huh-7 cells. Our finding proved this prepared nano complex has a powerful anticancer activity relative to free complex, thereby offering a promising cancer treatment.

Keywords: biologically prepared Cu-NPs, breast cancer cell lines, liver cancer cell lines, nanoCu- disulfiram

Procedia PDF Downloads 164

Authors: Michella Alnajjar, Frederic Christien, Krzysztof Wolski, Cedric Bosch

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Additive manufacturing (AM) has gained more interest in the past few years because it allows 3D parts often having a complex geometry to be directly fabricated, layer by layer according to a CAD model. One of the AM techniques is the selective laser melting (SLM) which is based on powder bed fusion. In this work, the corrosion resistance of 17-4 PH steel obtained by SLM is investigated. Wrought 17-4 PH steel is a martensitic precipitation hardenable stainless steel. It is widely used in a variety of applications such as aerospace, medical and food industries, due to its high strength and relatively good corrosion resistance. However, the combined findings of X-Ray diffraction and electron backscatter diffraction (EBSD) proved that SLM-ed 17-4 PH steel has a fully ferritic microstructure, more specifically δ ferrite. The microstructure consists of coarse ferritic grains elongated along the build direction, with a pronounced solidification crystallographic texture. These results were associated with the high cooling and heating rates experienced throughout the SLM process (10⁵-10⁶ K/s) that suppressed the austenite formation and produced a 'by-passing' phenomenon of this phase during the numerous thermal cycles. Furthermore, EDS measurements revealed a uniform distribution of elements without any dendritic structure. The extremely high cooling kinetics induced a diffusionless solidification, resulting in a homogeneous elemental composition. Consequently, the corrosion properties of this steel are altered from that of conventional ones. By using electrochemical means, it was found that SLM-ed 17-4 PH is more resistant to general corrosion than the wrought steel. However, the SLM-ed material exhibits metastable pitting due to its high porosity density. In addition, the hydrogen embrittlement of SLM-ed 17-4 PH steel is investigated, and a correlation between its behavior and the observed microstructure is made.

Keywords: corrosion resistance, 17-4 PH stainless steel, selective laser melting, hydrogen embrittlement

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Authors: Zohreh Derikvand

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One new 2D metal-organic coordination polymer of Ni(II) namely [Ni2(ndc)2(DMSO)4(H2O)]n, where ndc = naphthalene-1,4-dicarboxylic acid and DMSO= dimethyl sulfoxide has been synthesized and characterized by elemental analysis, spectral (IR, UV-Vis), thermal (TG/DTG) analysis and single crystal X-ray diffraction. Compound 1 possesses a 2D layer structure constructed from dinuclear nickel(II) building blocks in which two crystallographically independent Ni2+ ions are bridged by ndc2– ligands and water molecule. The ndc2– ligands adopt μ3 bridging modes, linking the metal centers into a two-dimensional coordination framework. The two independent NiII cations are surrounded by dimethyl sulfoxide and naphthalene-1,4-dicarboxylate molecules in distorted octahedron geometry. In the crystal structures of 1 there are non-classical hydrogen bonding arrangements and C-H–π stacking interactions. Electrochemical behavior of [Ni2(ndc)2(DMSO)4(H2O)]n, (Ni-NDA) on the surface of carbon nanotube (CNTs) glassy carbon electrode (GCE) was described. The surface structure and composition of the sensor were characterized by scanning electron microscopy (SEM). Oxidation of fructose on the surface of modified electrode was investigated with cyclic voltammetry and electrochemical impedance spectroscopy (EIS) and the results showed that the Ni-NDA/CNTs film displays excellent electrochemical catalytic activities towards fructose oxidation.

Keywords: naphthalene-1, 4-dicarboxylic acid, crystal structure, coordination polymer, electrocatalysis, impedance spectroscopy

Procedia PDF Downloads 307

Authors: Osman Adiguzel

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Shape-memory alloys are a new class of functional materials with a peculiar property known as shape memory effect. These alloys return to a previously defined shape on heating after deformation in low temperature product phase region and take place in a class of functional materials due to this property. The origin of this phenomenon lies in the fact that the material changes its internal crystalline structure with changing temperature. Shape memory effect is based on martensitic transitions, which govern the remarkable changes in internal crystalline structure of materials. Martensitic transformation, which is a solid state phase transformation, occurs in thermal manner in material on cooling from high temperature parent phase region. This transformation is governed by changes in the crystalline structure of the material. Shape memory alloys cycle between original and deformed shapes in bulk level on heating and cooling, and can be used as a thermal actuator or temperature-sensitive elements due to this property. Martensitic transformations usually occur with the cooperative movement of atoms by means of lattice invariant shears. The ordered parent phase structures turn into twinned structures with this movement in crystallographic manner in thermal induced case. The twinned martensites turn into the twinned or oriented martensite by stressing the material at low temperature martensitic phase condition. The detwinned martensite turns into the parent phase structure on first heating, first cycle, and parent phase structures turn into the twinned and detwinned structures respectively in irreversible and reversible memory cases. On the other hand, shape memory materials are very important and useful in many interdisciplinary fields such as medicine, pharmacy, bioengineering, metallurgy and many engineering fields. The choice of material as well as actuator and sensor to combine it with the host structure is very essential to develop main materials and structures. Copper based alloys exhibit this property in metastable beta-phase region, which has bcc-based structures at high temperature parent phase field, and these structures martensitically turn into layered complex structures with lattice twinning following two ordered reactions on cooling. Martensitic transition occurs as self-accommodated martensite with inhomogeneous shears, lattice invariant shears which occur in two opposite directions, <110 > -type directions on the {110}-type plane of austenite matrix which is basal plane of martensite. This kind of shear can be called as {110}<110> -type mode and gives rise to the formation of layered structures, like 3R, 9R or 18R depending on the stacking sequences on the close-packed planes of the ordered lattice. In the present contribution, x-ray diffraction and transmission electron microscopy (TEM) studies were carried out on two copper based alloys which have the chemical compositions in weight; Cu-26.1%Zn 4%Al and Cu-11%Al-6%Mn. X-ray diffraction profiles and electron diffraction patterns reveal that both alloys exhibit super lattice reflections inherited from parent phase due to the displacive character of martensitic transformation. X-ray diffractograms taken in a long time interval show that locations and intensities of diffraction peaks change with the aging time at room temperature. In particular, some of the successive peak pairs providing a special relation between Miller indices come close each other.

Keywords: Shape memory effect, martensite, twinning, detwinning, self-accommodation, layered structures

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Authors: C. Busuioc, S. I. Jinga, E. Pavel

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The continuous need of more non-volatile memories with a higher storage capacity, smaller dimensions and weight, as well as lower costs, has led to the exploration of optical lithography on active media, as well as patterned magnetic composites. In this context, optical lithography is a technique that can provide a significant decrease of the information bit size to the nanometric scale. However, there are some restrictions that arise from the need of breaking the optical diffraction limit. Major achievements have been obtained by employing a vitoceramic material as active medium and a laser beam operated at low power for the direct writing procedure. Thus, optical discs with ultra-high density were fabricated by a conventional melt-quenching method starting from analytical purity reagents. They were subsequently used for 3D recording based on their photosensitive features. Naturally, the next step consists in the elucidation of the composition and structure of the active centers, in correlation with the use of silver and rare-earth compounds for the synthesis of the optical supports. This has been accomplished by modern characterization methods, namely transmission electron microscopy coupled with selected area electron diffraction, scanning transmission electron microscopy and electron energy loss spectroscopy. The influence of laser diode parameters, silver concentration and fluorescent compounds formation on the writing process and final material properties was investigated. The results indicate performances in terms of capacity with two order of magnitude higher than other reported information storage systems. Moreover, the fluorescent photosensitive vitroceramics may be integrated in other applications which appeal to nanofabrication as the driving force in electronics and photonics fields.

Keywords: data storage, fluorescent compounds, laser writing, vitroceramics

Procedia PDF Downloads 207

Authors: Preeti Makkar, R. C. Agarwala, Vijaya Agarwala

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The present study focuses on the preparation of Al2O3 nanoparticles by top down approach i.e. mechanical milling using high energy planetary ball mill at 250 rpm for 40h. The milled Al2O3 nanoparticles are then used as the second phase to develop electroless (EL) Ni-P- Al2O3 nanocomposite coatings on mild steel substrate. An alkaline bath was used with a suspension of Al2O3 particles (4 g/L) for the synthesis of Ni-P-Al2O3 nanocomposite coating. The surface morphology, size range and phase analysis of as-prepared Al2O3 particles and the coatings were characterized using X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The coatings were heat treated at 400°C for 1h in argon atmosphere and the hardness of the nanocomposite coatings was investigated with respect to Ni-P before and after heat treatment. The results showed that as milled Al2O3 nanoparticles exhibit irregular shaped and size ranges around 40-45 nm. The Al2O3 particles are uniformly distributed in Ni-P matrix. The microhardness of the coatings is found to be significantly improved after heat treatment (1126 VHN).

Keywords: Electroless (EL), Ni-P-Al2O3, nanocomposite, mechanical milling, microhardness

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Authors: Murtaza Adil, Sen Yang, Zhou Chao, Song Xiaoping

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The morphotropic phase boundary (MPB) recently has attracted constant interest in ferromagnetic systems for obtaining enhanced large magnetoelastic response. In the present study, structural and magnetoelastic properties of MPB involved ferromagnetic Tb_1-xGd_xFe₂ (0≤x≤1) system has been investigated. The change of easy magnetic direction from <111> to <100> with increasing x up MPB composition of x=0.9 is detected by step-scanned [440] synchrotron X-ray diffraction reflections. The Gd substitution for Tb changes the composition for the anisotropy compensation near MPB composition of x=0.9, which was confirmed by the analysis of detailed scanned XRD, magnetization curves and the calculation of the first anisotropy constant K₁. The spin configuration diagram accompanied with different crystal structures for Tb_1-xGd_xFe₂ was designed. The calculated first anisotropy constant K₁ shows a minimum value at MPB composition of x=0.9. In addition, the large ratio between magnetostriction, and the absolute values of the first anisotropy constant │λ_S∕K₁│ appears at MPB composition, which makes it a potential material for magnetostrictive application. Based on experimental results, a theoretically approach was also proposed to signify that the facilitated magnetization rotation and enhanced magnetoelastic effect near MPB composition are a consequence of the anisotropic flattening of free energy of ferromagnetic crystal. Our work specifies the universal existence of MPB in ferromagnetic materials which is important for substantial improvement of magnetic and magnetostrictive properties and may provide a new route to develop advanced functional materials.

Keywords: free energy, magnetic anisotropy, magnetostriction, morphotropic phase boundary (MPB)

Procedia PDF Downloads 249

Authors: Burcu Kiren, Alattin CAkan, Nezihe Ayas

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Hydrogen will be arguably the best fuel in the future as it is the most abundant element in the universe. Hydrogen, as a fuel, is notably environmentally benign, sustainable and has high energy content compared to other sources of energy. It can be generated from both conventional and renewable sources. The hydrolysis reaction of metal hydrides provides an option for hydrogen production in the presence of a catalyst. In this study, Ni/dolomite catalyst was synthesized by the wet impregnation method for hydrogen production by hydrolysis reaction of sodium borohydride (NaBH4). Besides, the synthesized catalysts characterizations were examined by means of thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer –Emmett – Teller (BET) and scanning electron microscopy (SEM). The influence of reaction temperature (25-75 °C), reaction time (15-60 min.), amount of catalyst (50-250 mg) and active metal loading ratio (20,30,40 wt.%) were investigated. The catalyst prepared with 30 wt.% Ni was noted as the most suitable catalyst, achieving of 35.18% H₂ and hydrogen production rate of 19.23 mL/gcat.min at 25 °C at reaction conditions of 5 mL of 0.25 M NaOH and 100 mg NaBH₄, 100 mg Ni/dolomite.

Keywords: sodium borohydride, hydrolysis, catalyst, Ni/dolomite, hydrogen

Procedia PDF Downloads 131

Authors: Manel Hannachi, Mustapha Nechiche, Said Azem

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This study focuses on biodegradable materials made from Poly-lactic acid (PLA) and vegetal reinforcements. Three materials are developed from PLA, as a matrix, and : (i) olive kernels (OK); (ii) alfa (α) short fibers and (iii) OK+ α mixture, as reinforcements. After processing of PLA pellets and olive kernels in powder and alfa stems in short fibers, three mixtures, namely PLA-OK, PLA-α, and PLA-OK-α are prepared and homogenized in Turbula®. These mixtures are then compacted at 180°C under 10 MPa during 15 mn. Scanning Electron Microscopy (SEM) examinations show that PLA matrix adheres at surface of all reinforcements and the dispersion of these ones in matrix is good. X-ray diffraction (XRD) analyses highlight an increase of PLA inter-reticular distances, especially for the PLA-OK case. These results are explained by the dissociation of some molecules derived from reinforcements followed by diffusion of the released atoms in the structure of PLA. This is consistent with Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC) analysis results.

Keywords: alfa short fibers, biodegradable composite, olive kernels, poly-lactic acid

Procedia PDF Downloads 127

Authors: Anjela Koblischka-Veneva, Michael R. Koblischka

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To increase the flux pinning performance of bulk YBa2Cu3O7-δ (YBCO or Y-123) superconductors, it is common to employ secondary phase particles, either Y2BaCuO5 (Y-211) particles created during the growth of the samples or additionally added (nano)particles of various types, embedded in the superconducting Y-123 matrix. As the crystallographic parameters of all the particles indicate a misfit to Y-123, there will be residual strain within the Y-123 matrix around such particles. With a dedicated analysis of electron backscatter diffraction (EBSD) data obtained on various bulk, Y-123 superconductor samples, the strain distribution around such embedded secondary phase particles can be revealed. The results obtained are presented in form of Kernel Average Misorientation (KAM) mappings. Around large Y-211 particles, the strain can be so large that YBCO subgrains are formed. Therefore, it is essential to properly control the particle size as well as their distribution within the bulk sample to obtain the best performance. The impact of the strain distribution on the flux pinning properties is discussed.

Keywords: Bulk superconductors, EBSD, Strain, YBa2Cu3Oy

Procedia PDF Downloads 119

Authors: Veronique Jubera, Ka-Young Kim, U-Chan Chung, Amelie Veillere, Jean-Marc Heintz

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Emitting materials and all solid state lasers are widely used in the field of optical applications and materials science as a source of excitement, instrumental measurements, medical applications, metal shaping etc. Recently promising optical efficiencies were recorded on ceramics which result from a cheaper and faster ways to obtain crystallized materials. The choice and optimization of the sintering process is the key point to fabricate transparent ceramics. It includes a high control on the preparation of the powder with the choice of an adequate synthesis, a pre-heat-treatment, the reproducibility of the sintering cycle, the polishing and post-annealing of the ceramic. The densification is the main factor needed to reach a satisfying transparency, and many technologies are now available. The symmetry of the unit cell plays a crucial role in the diffusion rate of the material. Therefore, the cubic symmetry compounds having an isotropic refractive index is preferred. The cubic Y3NbO7 matrix is an interesting host which can accept a high concentration of rare earth doping element and it has been demonstrated that SPS is an efficient way to sinter this material. The optimization of diffusion losses requires a microstructure of fine ceramics, generally less than one hundred nanometers. In this case, grain growth is not an obstacle to transparency. The ceramics properties are then isotropic thereby to free-shaping step by orienting the ceramics as this is the case for the compounds of lower symmetry. After optimization of the synthesis route, several SPS parameters as heating rate, holding, dwell time and pressure were adjusted in order to increase the densification of the Eu3+ doped Y3NbO7 pellets. The luminescence data coupled with X-Ray diffraction analysis and electronic diffraction microscopy highlight the existence of several distorted environments of the doping element in the studied defective fluorite-type host lattice. Indeed, the fast and high crystallization rate obtained to put in evidence a lack of miscibility in the phase diagram, being the final composition of the pellet driven by the ratio between niobium and yttrium elements. By following the luminescence properties, we demonstrate a direct impact on the SPS process on this material.

Keywords: emission, niobate of rare earth, Spark plasma sintering, lack of miscibility

Procedia PDF Downloads 232

Authors: Abdul Salam Turkmani

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Clay of the northern Palmyra region is one of the most important raw materials used in the Syrian ceramics industry. This study is focused on the evaluation of various laboratory analyses such as chemical analysis (XRF), mineral X-ray diffraction analysis (XRD), differential thermal analysis (DTA), and semi-industrial tests carried out on samples collected on two representative locations of the upper Oligocene in AlMkamen valley (MK) and lower Miocene in AlZukara valley (ZR) of the northern part of Palmyra, Syria. Chemical results classify the (MK) and (ZR) clays as semi-plastic red clay slightly carbonate and (eliminate probable) illite-chlorite clays with a very fine particle size distribution. Content of SiO₂ between 46.28-57.66%, Al2O3 13.81-25.2%, Fe₂O₃ 3.47-11.58%, CaO 1.15-7.19%, Na₂O+K₂O varied between 3.34-3.71%. Based on clay chemical composition and iron and carbonate content, these deposits can be considered as red firing clays. Their mineralogical composition is mainly represented by illite, kaolinite and quartz, and accessories minerals such as calcite, feldspar, phillipsite, and goethite. The results of the DTA test confirm the presence of gypsum and quartz phases in (MK) clay. Ceramic testing shows good green and dry bending strength values, which varied between 9-14 kg/cm², at 1160°C to 1180°C. Water absorption moves from 14.6 % at 1120°C to 2.2% at 1180°C to 1.6% at 1200°C. Breaking load after firing changes from 400 to 590 kg/cm². At 1200°C (MK), clay reaches perfect vitrification. After firing, the color of the clay changes from orange-hazel to red-brown at 1180°C. Technological results confirmed the suitability of the studied clays to produce floor and wall ceramic tiles. Using one of the two types of clay into the ceramic body or both types together gave satisfactory industrial results.

Keywords: ceramic, clay, industry , Palmyra

Procedia PDF Downloads 166

Authors: Nan KANG, Pierre Coddet, Hanlin Liao, Christian Coddet

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In this study, the almost dense eutectic Al-12Si alloys were fabricated by selective laser melting (SLM) from the powder mixture of pure Aluminum and pure Silicon, which show the mean particle sizes of 30 μm and 5μm respectively, under the argon environment. The image analysis shows that the highest value of relative density (95 %) was measured for the part obtained at the laser power of 280 W. X ray diffraction (XRD), Optical microscope (OM) and scanning electron microscope (SEM) equipped with X-ray energy dispersive spectroscopy (EDS) were employed to determine the microstructures of the SLM-processed Al-Si alloy, which illustrate that the SLM samples present the ultra-fine microstructure. The XRD results indicate that no clearly phase transformation happened during the SLM process. Additionally, the vaporization behavior of Aluminum was detected for the parts obtained at high laser power. Besides, the maximum microhardness value, about 95 Hv, was measured for the samples obtained at laser power of 280 W, and which shows the highest wear resistance.

Keywords: al-Si alloy, selective laser melting, wear behavior, microstructure

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Authors: Esra Öztürk, Erkul Karacaoglu

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Pyrochlores, having compounds of the general formula, A2B2O7 (A and B are metals/rare earths) are important class of materials thanks to having technological applications like in luminescence, ionic conductivity, nuclear waste immobilization etc. The rare earths included pyrochlore compounds have also potential photoluminescence characteristics. In this context, Er3+-activated Lu2Ti2O7 pyrochlore was chosen and synthesized through a high-temperature solid-state reaction route that was sintered under the open atmosphere in this study. The optimal reaction conditions to obtain expected single phase system, the thermal analysis (DTA/TG) were carried out. The X-ray powder diffraction (XRD) was used to determine phase properties of the sample. The photoluminescence (PL) results were done to obtain excitation, emission and decay time properties by a PL spectrometer under room temperature. According to the PL, there are excitation bands at 352 nm, 388 nm, 423 nm and 453 nm that are due to 4I15/2 → 2G7/2, 4I15/2 → 4G11/2 and 4I15/2 → 4F5/2 transitions of Er3+ ions, respectively. The emission bands are placed at 582 nm, 677 nm and 762 nm that are associated with 2H11/2, 4S3/2 → 4I15/2, 4F9/2 → 4I15/2, 4I9/2 → 4I15/2 transitions of Er3+ ions, respectively.

Keywords: Er3+, Lu2Ti2O7, photoluminescence, pyrochlore, rare-earths

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Authors: J. Alvarez, J. Pimienta, R. Sarmiento

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Diode lasers working in free mode present different shifting and broadening determined by external factors such as temperature, current or mechanical vibrations, and they are not more useful in applications such as spectroscopy, metrology, and cooling of atoms, among others. Different configurations can reduce the spectral width of a laser; one of the most effective is to extend the optical resonator of the laser diode and use optical feedback either with the help of a partially reflective mirror or with a diffraction grating; this latter configuration is not only allowed to reduce the spectral width of the laser line but also to coarsely adjust its working wavelength, within a wide range typically ~ 10nm by slightly varying the angle of the diffraction grating. Two settings are commonly used for this purpose, the Littrow configuration and the Littmann Metcalf. In this paper, we present the design, construction, and characterization of a compact extended laser cavity in Littrow configuration. The designed cavity is compact and was machined on an aluminum block using computer numerical control (CNC); it has a mass of only 380 g. The design was tested on laser diodes with different wavelengths, 650nm, 780nm, and 795 nm, but can be equally efficient at other wavelengths. This report details the results obtained from the extended cavity working at a wavelength of 780 nm, with an output power of around 35mW and a line width of less than 1Mhz. The cavity was used to observe the spectrum of the corresponding Rubidium D2 line. By modulating the current and with the help of phase detection techniques, a dispersion signal with an excellent signal-to-noise ratio was generated that allowed the stabilization of the laser to a transition of the hyperfine structure of Rubidium with an integral proportional controller (PI) circuit made with precision operational amplifiers.

Keywords: Littrow, Littman-Metcalf, line width, laser stabilization, hyperfine structure

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Authors: Seyed Mahdi Rafiaei

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In this investigation, firstly Eu3+ doped YVO4 phosphor was synthesized using solid-state method. Then silica was coated on the surface of particles via sol-gel method. To study the influence of SiO2 addition on microstructure and photoluminescence characteristics of YVO4:4% Eu3+ phosphor materials, we employed X-ray Diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), High-Resolution Transmitted Electron Microscope (HRTEM), Focused Ion Beam (FIB), Brunauer Emmett Teller (BET), Inductively coupled plasma (ICP), Electron Spin Resonance (ESR) and Photoluminescence (PL) equipments. The XPS characterization confirmed the formation of Y–O–Si and V-O-Si bondings between YVO4:Eu3+ phosphor particle and SiO2 coating. In addition, it was found that although the amounts of added SiO2 were not remarkable, but it resulted in enhancement of emission intensity of the phosphors. Finally by employing ESR analysis, it was shown that surface oxygen vacancies, result in reduction of V5+ to the lower valence state of V4+.

Keywords: solid state, sol-gel, silica, coating, photoluminescence

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Authors: Zeid A. Alothman

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Silver nanoparticle (AgNP) has been synthesized using adrenaline. Adrenaline readily undergoes an autoxidation reaction in an alkaline medium with the dissolved oxygen to form adrenochrome, thus behaving as a mild reducing agent for the dissolved oxygen. This reducing behavior of adrenaline when employed to reduce Ag(+) ions yielded a large enhancement in the intensity of absorbance in the visible region. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) studies have been performed to confirm the surface morphology of AgNPs. Further, the metallic nanoparticles with size greater than 2 nm caused a strong and broad absorption band in the UV-visible spectrum called surface plasmon band or Mie resonance. The formation of AgNPs caused the large enhancement in the absorbance values with λmax at 436 nm through the excitation of the surface plasmon band. The formation of AgNPs was adapted to for the quantitative assessment of adrenaline using spectrophotometry with lower detection limit and higher precision values.

Keywords: silver nanoparticle, adrenaline, XRD, TEM, analysis

Procedia PDF Downloads 181

Authors: M. Haghnegahdar, G. Naderi, M. H. R. Ghoreishy

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Polypropylene(PP)/Ethylene Propylene Diene Monomer (EPDM) samples (80/20) containing 0, 0.5, 1, 1.5, 2, 2.5, and 3 (expressed in mass fraction) graphene were prepared using melt compounding method to investigate microstructure, mechanical properties, and thermal stability as well as electrical resistance of samples. X-Ray diffraction data confirmed that graphene platelets are well dispersed in PP/EPDM. Mechanical properties such as tensile strength, impact strength and hardness demonstrated increasing trend by graphene loading which exemplifies substantial reinforcing nature of this kind of nano filler and it's good interaction with polymer chains. At the same time it is found that thermo-oxidative degradation of PP/EPDM nanocomposites is noticeably retarded with the increasing of graphene content. Electrical surface resistivity of the nanocomposite was dramatically changed by forming electrical percolation threshold and leads to change electrical behavior from insulator to semiconductor. Furthermore, these results were confirmed by scanning electron microscopy(SEM), dynamic mechanical thermal analysis (DMTA), and transmission electron microscopy (TEM).

Keywords: nanocomposite, graphene, microstructure, mechanical properties

Procedia PDF Downloads 307

Authors: Quoc Ngoc Phan, Hieu Van Nguyen, Minh Hong Nguyen

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This study presents an integrated approach using Mercury Injection Capillary Pressure (MICP) and petrographic analysis to assess the seal quality of the inter-bedded shale formations which are considered the intra-formation top seals of hydrocarbon bearing zones in Green Dragon structure. Based on the hydrocarbon column height (HCH) at leak point derived from capillary pressure data, four seal types were identified. Furthermore, the results of scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis were interpreted to clarify the influence of clay minerals on seal capacity. The result of the study indicated that the inter-bedded shale formations are the good sealing quality with a majority of analyzed samples ranked type A and B seals in the sample set. Both seal types occurred mainly in mudstones with pore radius estimated less than 0.251 µm. Overall, type A and B seals contained a large amount of authigenic clay minerals such as illite, chlorite which showed the complexity of morphological arrangement in pore space. Conversely, the least common seal type C and D were presented in moderately compacted sandstones with more open pore radius. It is noticeable that there was a reduction of illite and chlorite in clay mineral fraction of these seal type. It is expected that the integrated analysis approach using Mercury Injection Capillary Pressure and petrographic data employed in this study can be applied to assess the sealing quality of future well sites in Green Dragon or other structures.

Keywords: seal capacity, hydrocarbon height column, seal type, SEM, XRD

Procedia PDF Downloads 136

Authors: Shaya Mahmoudian, Mohammad Reza Sazegar, Nazanin Afshari

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Graphene, a single layer of carbon atoms in a hexagonal lattice, has recently attracted great attention due to its unique mechanical, thermal and electrical properties. The high aspect ratio and unique surface features of graphene resulted in significant improvements of the nano composites properties. In this study, nano composite fibres made of cellulose and graphene nano platelets were wet spun from solution by using ionic liquid, 1-ethyl-3-methylimidazolium acetate (EMIMAc) as solvent. The effect of graphene loading on the thermal and electrical properties of the nanocomposite fibres was investigated. The nano composite fibres characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis. XRD analysis revealed a cellulose II crystalline structure for regenerated cellulose and the nano composite fibres. SEM images showed a homogenous morphology and round cross section for the nano composite fibres along with well dispersion of graphene nano platelets in regenerated cellulose matrix. The incorporation of graphene into cellulose matrix generated electrical conductivity. At 6 wt. % of graphene, the electrical conductivity was 4.7 × 10-4 S/cm. The nano composite fibres also showed considerable improvements in thermal stability and char yield compared to pure regenerated cellulose fibres. This work provides a facile and environmentally friendly method of preparing nano composite fibres based on cellulose and graphene nano platelets that can find several applications in cellulose-based carbon fibres, conductive fibres, apparel, etc.

Keywords: nanocomposite, graphene nanoplatelets, regenerated cellulose, electrical properties

Procedia PDF Downloads 324

Authors: Yuvraj Singh Dangi, Kamta Prasad Namdeo, Surendra Bodhake

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The purpose of this research was to develop and evaluate mucoadhesive films for buccal administration of itraconazole using film-forming and mucoashesive polymers. Buccal films of chitosan bearing Itraconazole were prepared by solvent casting technique. The films have been evaluated in terms of film weight, thickness, density, surface pH, FTIR, X-ray diffraction analysis, bioadhesion, swelling properties, and in vitro drug release studies. It was found that film formulations of 2 cm2 size having weight in the range of 204 ± 0.76 to 223 ± 2.09 mg and film thickness were in the range of 0.44 ± 0.11 to 0.57 ± 0.19 mm. Density of the films was found to be 0.102 to 0.126 g/ml. Drug content was found to be uniform in the range of 8.23 ± 0.07 to 8.73 ± 0.09 mg/cm2 for formulation A1 to A4. Maximum bioadhesion force was recorded for HPMC buccal films (A2) i.e. 0.57 ± 0.47 as compared to other films. In vitro residence time was in range of 1.7 ± 0.12 to 7.65 ± 0.15 h. The drug release studies show that formulations follow non-fickian diffusion. These mucoadhesive formulations could offer many advantages in comparison to traditional treatments.

Keywords: biovariability, buccal patches, itraconazole, Mucoadhesion

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Authors: E. Gandomkar, S. Sabbaghi

Abstract:

In this paper, the effects of variation synthesized methods on morphology and size of silica nanostructure via modifying sol-gel and precipitation method have been investigated. Meanwhile, resulting products have been characterized by particle size analyzer, scanning electron microscopy (SEM), X-ray Diffraction (XRD) and Fourier transform infrared (FT-IR) spectra. As result, the shape of SiO2 with sol-gel and precipitation methods was spherical but with modifying sol-gel method we have been had nanolayer structure.

Keywords: modified sol-gel, precipitation, nanolayer, Na2SiO3, nanoparticle

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Authors: Atef Y. Shenouda, Anton A. Momchilov

Abstract:

Graphene and CdO with different stoichiometric ratios of Cd(CH₃COO)₂ and graphene samples were prepared by hydrothermal reaction. The crystalline phases of pure CdO and 3CdO:1graphene were identified by X-ray diffraction (XRD). The particle morphology was studied with SEM. Furthermore, impedance measurements were applied. Galvanostatic measurements for the cells were carried out using potential limits between 0.01 and 3 V vs. Li/Li⁺. The current cycling intensity was 10⁻⁴ A. The specific discharge capacity of 3CdO-1G cell was about 450 Ah.Kg⁻¹ up to more than 100 cycles.

Keywords: CdO, graphene, negative electrode, lithium battery

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Authors: N.Quaranta, M. Caligaris, R. Varoli, A. Cristobal, M. Unsen, H. López

Abstract:

Corncobs are agricultural wastes and they can be used as fuel or as raw material in different industrial processes like cement manufacture, contaminant adsorption, chemical compound synthesis, etc. The aim of this work is to characterize this waste and analyze the feasibility of its use as a pore-forming material in the manufacture of lightweight ceramics for the civil construction industry. The characterization of raw materials is carried out by using various techniques: electron diffraction analysis X-ray, differential and gravimetric thermal analyses, FTIR spectroscopy, ecotoxicity evaluation, among others. The ground corncobs, particle size less than 2 mm, are mixed with clay up to 30% in volume and shaped by uniaxial pressure of 25 MPa, with 6% humidity, in moulds of 70mm x 40mm x 18mm. Then the green bodies are heat treated at 950°C for two hours following the treatment curves used in ceramic industry. The ceramic probes are characterized by several techniques: density, porosity and water absorption, permanent volumetric variation, loss on ignition, microscopies analysis, and mechanical properties. DTA-TGA analysis of corncobs shows in the range 20°-250°C a small loss in TGA curve and exothermic peaks at 250°-500°C. FTIR spectrum of the corncobs sample shows the characteristic pattern of this kind of organic matter with stretching vibration bands of adsorbed water, methyl groups, C–O and C–C bonds, and the complex form of the cellulose and hemicellulose glycosidic bonds. The obtained ceramic bodies present external good characteristics without loose edges and adequate properties for the market requirements. The porosity values of the sintered pieces are higher than those of the reference sample without waste addition. The results generally indicate that it is possible to use corncobs as porosity former in ceramic bodies without modifying the usual sintering temperatures employed in the industry.

Keywords: ceramic industry, biomass, recycling, hemicellulose glycosidic bonds

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Authors: Suneeta Kumari, Abanti Sahoo

Abstract:

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

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

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Authors: S. M. Giripunje, Shikha Jindal

Abstract:

Zinc sulphide (ZnS) quantum dots (QDs) were synthesized successfully via simple sonochemical method. X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) analysis revealed the average size of QDs of the order of 3.7 nm. The band gap of the QDs was tuned to 5.2 eV by optimizing the synthesis parameters. UV-Vis absorption spectra of ZnS QD confirm the quantum confinement effect. Fourier transform infrared (FTIR) analysis confirmed the formation of single phase ZnS QDs. To fabricate the diode, blend of ZnS QDs and P3HT was prepared and the heterojunction of PEDOT:PSS and the blend was formed by spin coating on indium tin oxide (ITO) coated glass substrate. The diode behaviour of the heterojunction was analysed, wherein the ideality factor was found to be 2.53 with turn on voltage 0.75 V and the barrier height was found to be 1.429 eV. ZnS-Graphene QDs nanocomposite was characterised for the surface morphological study. It was found that the synthesized ZnS QDs appear as quasi spherical particles on the graphene sheets. The average particle size of ZnS-graphene nanocomposite QDs was found to be 8.4 nm. From voltage-current characteristics of ZnS-graphene nanocomposites, it is observed that the conductivity of the composite increases by 10⁴ times the conductivity of ZnS QDs. Thus the addition of graphene QDs in ZnS QDs enhances the mobility of the charge carriers in the composite material. Thus, the graphene QDs, with high specific area for a large interface, high mobility and tunable band gap, show a great potential as an electron-acceptors in photovoltaic devices.

Keywords: graphene, heterojunction, quantum confinement effect, quantum dots(QDs), zinc sulphide(ZnS)

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Authors: Sidi Mohamed Mesli, Mohamed Habchi, Arslane Boudghene Stambouli, Rafik Benallal

Abstract:

The BaMnMF7 (M=Fe,V, transition metal fluoride glass, assuming isomorphous replacement) have been structurally studied through the simultaneous simulation of their neutron diffraction patterns by reverse Monte Carlo (RMC) and by the Hybrid Reverse Monte Carlo (HRMC) analysis. This last is applied to remedy the problem of the artificial satellite peaks that appear in the partial pair distribution functions (PDFs) by the RMC simulation. The HRMC simulation is an extension of the RMC algorithm, which introduces an energy penalty term (potential) in acceptance criteria. The idea of this work is to apply the Buckingham potential at the title glass by ignoring the van der Waals terms, in order to make a fit of the partial pair distribution functions and give the most possible realistic features. When displaying the partial PDFs, we suggest that the Buckingham potential is useful to describe average correlations especially in similar interactions.

Keywords: fluoride glasses, RMC simulation, hybrid RMC simulation, Buckingham potential, partial pair distribution functions

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Authors: Aiswarea Mathew, Smita Mohanty, Jr., S. K. Nayak

Abstract:

Polyurethane networks based on castor oil (CO) as a renewable resource polyol were synthesized. Polyurethane/epoxy resin interpenetrating network nanocomposites containing modified montmorillonite organoclay (C30B-PU/EP nanocomposites) were prepared by an in situ intercalation method. The conventional spectroscopic characterization of the synthesized samples using FT-IR confirms the existence of the proposed castor oil based PU structure and also showed that strong interactions existed between C30B and EP/PU matrix. The dispersion degree of C30B in EP/PU matrix was characterized by X-Ray diffraction (XRD) method. Scanning electronic microscopy analysis showed that the interpenetrating process of PU and EP increases the exfoliation degree of C30B, and it improves the compatibility and the phase structure of polyurethane/epoxy resin interpenetrating polymer networks (PU/EP IPNs). The thermal stability improves compared to the polyurethane when the PU/EP IPN is formed. Mechanical properties including the Young’s modulus and tensile strength reflected marked improvement with addition of C30B.

Keywords: castor oil, epoxy, montmorillonite, polyurethane

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Authors: Noor Ul Huda, Mushtaq Ahmed, Nadia Mushtaq, Naila Sher, Rahmat Ali Khan

Abstract:

Purpose: The green synthesis of AgNPs has been favored over chemical synthesis due to their distinctive properties such as high dispersion, surface-to-volume ratio, low toxicity, and easy preparation. In the present work, the biosynthesis of AgNPs (KE-AgNPs) was carried out in one step by using the traditionally used plant Kickxia elatine (KE) extract and then investigated its enzyme inhibiting activity against rat’s brain acetylcholinesterase (AChE) in vitro. Methods: KE-AgNPs were synthesized from 1mM AgNO₃ using KE extract and characterized by UV–spectroscopy, SEM, EDX, XRD, and FTIR analysis. Rat’s brain acetylcholinesterase (AChE) inhibition activity was evaluated by the standard protocol. Results: UV–spectrum at 416 nm confirmed the formation of KE-AgNPs. X-ray diffraction (XRD) pattern presented 2θ values corresponding to the crystalline nature of KE-AgNPs with an average size of 42.47nm. The scanning electron microscope (SEM) analysis confirmed the presence of spherical-shaped and huge density KE-AgNPs with a size of 50nm. Fourier transform infrared spectroscopy (FT-IR) suggested that the functional groups present in KE extract and on the surface of KE-AgNPs are responsible for the stability of biosynthesized NPs. Energy dispersive X-ray (EDX) displayed an intense sharp peak at 3.2 keV, presenting that Ag was the chief element with 61.67%. Both KE extract and KE-AgNPs showed good and potent anti-AChE activity, with higher inhibition potential at a concentration of 175 µg/ml. Statistical analysis showed that both KEE and AgNPs exhibited non-competitive type inhibition against AChE, i.e., Vmax decreased (34.17-68.64% and 22.29- 62.10%) in the concentration-dependent mode for KEE and KE-AgNPs respectively and while Km values remained constant. Conclusions: KEE and KE-AgNPs can be considered an inhibitor of rats’ brain AChE, and the synthesis of KE-AgNPs-based drugs can be used as a cheaper and alternative option against diseases such as Alzheimer’s disease.

Keywords: Kickxia elatine, AgNPs, brain homogenate, acetylcholinesterase, kinetics

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Authors: K. N. Kipreou, E. Efthmiadou, G. Kordas

Abstract:

Biofouling represents one of the most crucial problems in the present maritime industries when its control still challenges the researchers all over the world. The present work is referred to the synthesis and characterization CeMo and Cu2O nanocontainers by using a wide range of techniques including scanning electron microscopy (SEM), X-ray diffraction (XRD) and thermogravimetric analysis (TGA) for marine applications. The above nanosystems will be loaded with active monomers and corrosion rendering healing ability to marine paints. The objective of this project is their ability for self-healing, self-polishing and finally for anti-corrosion activity. One of the driving forces for the exploration of CeMo, is the unique anticorrosive behavior, which will be confirmed by the electrochemistry methodology. It has be highlighted that the nanocontainers of Cu2O with the appropriate antibacterial inhibitor will improve the hydrophobicity and the morphology of the coating surfaces reducing the water friction. In summary, both novel nanoc will increase the lifetime of the paints releasing the antifouling agent in a control manner.

Keywords: marinepaints, nanocontainer, antifouling, anticorrosion, copper, electrochemistry, coating, biofouling, inhibitors, copper oxide, coating, SEM

Procedia PDF Downloads 312