Search results for: single crystal x-ray diffraction

Authors: Santanu Pakhira, Chandan Mazumdar, R. Ranganathan, Maxim Avdeev

Abstract:

Magnetically frustrated systems are of great interest and one of the most adorable topics for the researcher of condensed matter physics, due to their various interesting properties, viz. ground state degeneracy, finite entropy at zero temperature, lowering of ordering temperature, etc. Ternary intermetallics with the composition RE₂TX₃ (RE = rare-earth element, T= d electron transition metal and X= p electron element) crystallize in hexagonal AlB₂ type crystal structure (space group P6/mmm). In a hexagonal crystal structure with the antiferromagnetic interaction between the moments, the center moment is geometrically frustrated. Magnetic frustration along with disorder arrangements of non-magnetic ions are the building blocks for metastable spin-glass ground state formation for most of the compounds of this stoichiometry. The newly synthesized compound Er₂NiSi₃ compound forms in single phase in AlB₂ type structure with space group P6/mmm. The compound orders antiferromagnetically below 5.4 K and spin freezing of the frustrated magnetic moments occurs below 3 K for the compound. The compound shows magnetic relaxation behavior and magnetic memory effect below its freezing temperature. Neutron diffraction patterns for temperatures below the spin freezing temperature have been analyzed using FULLPROF software package. Diffuse magnetic scattering at low temperatures yields spin glass state formation for the compound.

Keywords: antiferromagnetism, magnetic frustration, spin-glass, neutron diffraction

Procedia PDF Downloads 235

Authors: G. Çelik Gül, F. Kurtuluş

Abstract:

Rare earths containing complex metal oxides have drawn much attention due to physical, chemical and optical properties which make them feasible in so many areas such as non-linear optical materials and ion exchanger. We have researched a systematic study to obtain rare earth containing zirconium molybdate compound, characterization, investigation of crystal system and calculation of unit cell parameters.  After a successful synthesis of Nd₂Zr₃(MoO₄)₉ which is a member of rare earth metal containing complex oxides family, X-ray diffraction (XRD), High Score Plus/Rietveld refinement analysis, and Fourier Transform Infrared Spectroscopy (FTIR) were completed to determine the crystal structure. Morphological properties and elemental composition were determined by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. Thermal properties were observed via Thermogravimetric-differential thermal analysis (TG/DTA).

Keywords: Nd₂Zr₃(MoO₄)₉, powder x-ray diffraction, solid state synthesis, zirconium molybdates

Procedia PDF Downloads 367

Authors: N. Renuka, R. Ramesh Babu, N. Vijayan

Abstract:

Ion beams play a significant role in the process of tuning the properties of materials. Based on the radiation behavior, the engineering materials are categorized into two different types. The first one comprises organic solids which are sensitive to the energy deposited in their electronic system and the second one comprises metals which are insensitive to the energy deposited in their electronic system. However, exposure to swift heavy ions alters this general behavior. Depending on the mass, kinetic energy and nuclear charge, an ion can produce modifications within a thin surface layer or it can penetrate deeply to produce long and narrow distorted area along its path. When a high energetic ion beam impinges on a material, it causes two different types of changes in the material due to the columbic interaction between the target atom and the energetic ion beam: (i) inelastic collisions of the energetic ion with the atomic electrons of the material; and (ii) elastic scattering from the nuclei of the atoms of the material, which is extremely responsible for relocating the atoms of matter from their lattice position. The exposure of the heavy ions renders the material return to equilibrium state during which the material undergoes surface and bulk modifications which depends on the mass of the projectile ion, physical properties of the target material, its energy, and beam dimension. It is well established that electronic stopping power plays a major role in the defect creation mechanism provided it exceeds a threshold which strongly depends on the nature of the target material. There are reports available on heavy ion irradiation especially on crystalline materials to tune their physical and chemical properties. L-Arginine Acetate [LAA] is a potential semi-organic nonlinear optical crystal and its optical, mechanical and thermal properties have already been reported The main objective of the present work is to enhance or tune the structural and optical properties of LAA single crystals by heavy ion irradiation. In the present study, a potential nonlinear optical single crystal, L-arginine acetate (LAA) was grown by slow evaporation solution growth technique. The grown LAA single crystal was irradiated with oxygen ions at the dose rate of 600 krad and 1M rad in order to tune the structural and optical properties. The structural properties of pristine and oxygen ions irradiated LAA single crystals were studied using Powder X- ray diffraction and Fourier Transform Infrared spectral studies which reveal the structural changes that are generated due to irradiation. Optical behavior of pristine and oxygen ions irradiated crystals is studied by UV-Vis-NIR and photoluminescence analyses. From this investigation we can concluded that oxygen ions irradiation modifies the structural and optical properties of LAA single crystals.

Keywords: heavy ion irradiation, NLO single crystal, photoluminescence, X-ray diffractometer

Procedia PDF Downloads 224

Authors: T. Wejrzanowski, M. Grybczuk, E. Tymicki, K. J. Kurzydlowski

Abstract:

In the present study numerical simulations silicon carbide single crystal growth process in Physical Vapor Transport reactor are addressed. Silicon Carbide is a perspective material for many applications in modern electronics. One of the main challenges for wider applications of SiC is high price of high quality mono crystals. Improvement of silicon carbide manufacturing process has a significant influence on the product price. Better understanding of crystal growth allows for optimization of the process, and it can be achieved by numerical simulations. In this work Virtual Reactor software was used to simulate the process. Predicted geometrical properties of the final product and information about phenomena occurring inside process reactor were obtained. The latter is especially valuable because reactor chamber is inaccessible during the process due to high temperature inside the reactor (over 2000˚C). Obtained data was used for improvement of the process and reactor geometry. Resultant crystal quality was also predicted basing on crystallization front shape evolution and threading dislocation paths. Obtained results were confronted with experimental data and the results are in good agreement.

Keywords: Finite Volume Method, semiconductors, Physical Vapor Transport, silicon carbide

Procedia PDF Downloads 506

Authors: Saleh Gorji, Sahil Gulati, Ana Pakzad

Abstract:

Continuous electron diffraction tomography, also known as microcrystal electron diffraction (MicroED) or three-dimensional electron diffraction (3DED), is a powerful technique, which in combination with cryo-electron microscopy (cryo-ED), can provide atomic-scale 3D information about the crystal structure and composition of different classes of crystalline materials such as proteins, peptides, and small molecules. Unlike the well-established X-ray crystallography method, 3DED does not require large single crystals and can collect accurate electron diffraction data from crystals as small as 50 – 100 nm. This is a critical advantage as growing larger crystals, as required by X-ray crystallography methods, is often very difficult, time-consuming, and expensive. In most cases, specimens studied via 3DED method are electron beam sensitive, which means there is a limitation on the maximum amount of electron dose one can use to collect the required data for a high-resolution structure determination. Therefore, collecting data using a conventional scintillator-based fiber coupled camera brings additional challenges. This is because of the inherent noise introduced during the electron-to-photon conversion in the scintillator and transfer of light via the fibers to the sensor, which results in a poor signal-to-noise ratio and requires a relatively higher and commonly specimen-damaging electron dose rates, especially for protein crystals. As in other cryo-EM techniques, damage to the specimen can be mitigated if a direct detection camera is used which provides a high signal-to-noise ratio at low electron doses. In this work, we have used two classes of such detectors from Gatan, namely the K3® camera (a monolithic active pixel sensor) and Stela™ (that utilizes DECTRIS hybrid-pixel technology), to address this problem. The K3 is an electron counting detector optimized for low-dose applications (like structural biology cryo-EM), and Stela is also a counting electron detector but optimized for diffraction applications with high speed and high dynamic range. Lastly, data collection workflows, including crystal screening, microscope optics setup (for imaging and diffraction), stage height adjustment at each crystal position, and tomogram acquisition, can be one of the other challenges of the 3DED technique. Traditionally this has been all done manually or in a partly automated fashion using open-source software and scripting, requiring long hours on the microscope (extra cost) and extensive user interaction with the system. We have recently introduced Latitude® D in DigitalMicrograph® software, which is compatible with all pre- and post-energy-filter Gatan cameras and enables 3DED data acquisition in an automated and optimized fashion. Higher quality 3DED data enables structure determination with higher confidence, while automated workflows allow these to be completed considerably faster than before. Using multiple examples, this work will demonstrate how to direct detection electron counting cameras enhance 3DED results (3 to better than 1 Angstrom) for protein and small molecule structure determination. We will also show how Latitude D software facilitates collecting such data in an integrated and fully automated user interface.

Keywords: continuous electron diffraction tomography, direct detection, diffraction, Latitude D, Digitalmicrograph, proteins, small molecules

Procedia PDF Downloads 57

Authors: Zohreh Derikvand

Abstract:

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 305

Authors: Takashi Shimizu, Tomoaki Hashimoto

Abstract:

Recently, crystal growth technologies have made progress by the requirement for the high quality of crystal materials. To control the crystal growth dynamics actively by external forces is useuful for reducing composition non-uniformity. In this study, a control method based on model predictive control using thermal inputs is proposed for crystal growth dynamics of semiconductor materials. The control system of crystal growth dynamics considered here is governed by the continuity, momentum, energy, and mass transport equations. To establish the control method for such thermal fluid systems, we adopt model predictive control known as a kind of optimal feedback control in which the control performance over a finite future is optimized with a performance index that has a moving initial time and terminal time. The objective of this study is to establish a model predictive control method for crystal growth dynamics of semiconductor materials.

Keywords: model predictive control, optimal control, process control, crystal growth

Procedia PDF Downloads 326

Authors: Arpit Bhardwaj, Koushik Roy

Abstract:

The work includes derivation of the exact-closed form solution for simply supported quasicrystal and crystal plates by using propagator matrix method under surface loading and free vibration. As a numerical example a quasicrystal and a crystal plate are considered, and after investigation, the variation of displacement and stress fields along the thickness of these two plates are presented. Further, it includes analyzing the displacement and stress fields for two plates having two different stacking arrangement, i.e., QuasiCrystal/Crystal/QuasiCrystal and Crystal/QuasiCrystal/Crystal and comparing their results. This will not only tell us the change in the behavior of displacement and stress fields in two different materials but also how these get changed after trying their different combinations. For the free vibration case, Crystal and Quasicrystal plates along with their different stacking arrangements are considered, and displacements are plotted in all directions for different Mode Shapes.

Keywords: free vibration, multilayered plates, surface loading, quasicrystals

Procedia PDF Downloads 118

Authors: Hao Qu, Xiang Liu, Michael Crosby, Brian Kozak, Andreas K. Freund

Abstract:

The outstanding performance of highly oriented pyrolytic graphite (HOPG) as an optical element for neutron beam conditioning is unequaled by any other crystalline material in the applications of monochromator, analyzer, and filter. This superiority stems from the favorable nuclear properties of carbon (small absorption and incoherent scattering cross-sections, big coherent scattering length) and the specific crystalline structure (small thermal diffuse scattering cross-section, layered crystal structure). The real crystal defect structure revealed by imaging techniques is correlated with the parameters used in the mosaic model (mosaic spread, mosaic block size, uniformity). The diffraction properties (rocking curve width as determined by both the intrinsic mosaic spread and the diffraction process, peak and integrated reflectivity, filter transmission) as a function of neutron wavelength or energy can be predicted with high accuracy and reliability by diffraction theory using empirical primary extinction coefficients extracted from a great amount of existing experimental data. The results of these calculations are given as graphs and tables permitting to optimize HOPG characteristics (mosaic spread, thickness, curvature) for any given experimental situation.

Keywords: neutron optics, pyrolytic graphite, mosaic spread, neutron scattering, monochromator, analyzer

Procedia PDF Downloads 108

Authors: Shabbir Chowdhury

Abstract:

A signal is broadened when it is gone through a channel, this phenomenon is known as dispersion. And dispersion is different for different wavelength. So bandwidth become limited. Research have tried to design an optical fiber with flattened dispersion to use more bandwidth and also for wavelength division multiplexing. In this paper, a single mode photonic crystal fiber with a flattened dispersion and less effective area has been proposed where silica is used as fiber materials. The effective dispersion varies from -1.996 to 0.1783 [ps/(nm-km)] for enter E-band to U-band. This fiber will take only 3.048 [micrometer^2] (for 1.75 micrometer wavelength). Silica is being used as the fiber material.

Keywords: photonic crystal fiber, dispersion, bandwidth, chromatic dispersion, effective dispersion, dispersion compensation, effective area, effective refractive index

Procedia PDF Downloads 384

Authors: A. Fakhri Makram, Marwa S. Alwazni, Al-Douri Yarub, Evan T. Salim, Hashim Uda, Chin C. Woei

Abstract:

Lithium niobate (LiNbO₃) nanostructures are prepared on quartz substrate by the sol-gel method. They have been deposited with different molarity concentration and annealed at 500°C. These samples are characterized and analyzed by X-ray diffraction (XRD), Scanning Electron Microscope (SEM) and Atomic Force Microscopy (AFM). The measured results showed an importance increasing in molarity concentrations that indicate the structure starts to become crystal, regular, homogeneous, well crystal distributed, which made it more suitable for optical waveguide application.

Keywords: lithium niobate, morphological properties, thin film, pechini method, XRD

Procedia PDF Downloads 415

Authors: Juiwen Liang, Choliang Chung

Abstract:

In this study, the silicon-base oxide nanofibers with hollow structure were prepared using single-nozzle electrospinning and heat treatment. Firstly, precursor solution was prepared: the Polyvinylpyrrolidone (PVP) and Tetraethyl orthosilicate (TEOS) dissolved in ethanol and to make sure the concentration of solution in appropriate using single-nozzle electrospinning to produce the nanofibers. Secondly, control morphology of the electrostatic spinning nanofibers was conducted, and design the temperature profile to created hollow nanofibers, exploring the morphology and properties of nanofibers. The characterized of nanofibers, following instruments were used: Atomic force microscopy (AFM), Field Emission Scanning Electron Microscope (FE-SEM), Transmission electron microscopy (TEM), Photoluminescence (PL), X-ray Diffraction (XRD). The AFM was used to scan the nanofibers, and 3D Graphics were applied to explore the surface morphology of fibers. FE-SEM and TEM were used to explore the morphology and diameter of nanofibers and hollow nanofiber. The excitation and emission spectra explored by PL. Finally, XRD was used for identified crystallization of ceramic nanofibers. Using electrospinning technique followed by subsequent heat treatment, we have successfully prepared silicon-base oxide nanofibers with hollow structure. Thus, the microstructure and morphology of electrostatic spinning silicon-base oxide hollow nanofibers were explored. Major characteristics of the nanofiber in terms of crystalline, optical properties and crystal structure were identified.

Keywords: electrospinning, single-nozzle, hollow, nanofibers

Procedia PDF Downloads 327

Authors: Fatima Melit, Nedjemeddine Bounar

Abstract:

Polycrystalline samples of Ce1-xMxO2-δ (x=0.1, 0.15, 0.2)(M=Gd, Y) were prepared by solid-state chemical reaction from mixtures of pre-dried oxides powders of CeO2, Gd2O3 and Y2O3 in the appropriate stoichiometric ratio to explore their use as solid electrolytes for intermediate temperature solid oxide fuel cells (IT-SOFCs). Their crystal structures and ionic conductivities were characterised by X-ray powder diffraction (XRD) and AC complex impedance spectroscopy (EIS). The XRD analyses confirm that all the resulting synthesised co-doped cerium oxide powders are single-phase and crystallise in the cubic structure system with the space group Fm3m. On the one hand, the lattice parameter (a ) of the phases increases with increasing Gd content; on the other hand, with increasing Y-substitution rate, the latter decreases. The results of complex impedance conductivity measurements have shown that doping has a remarkable effect on conductivity. The co-doped cerium phases showed significant ionic conductivity values, making these materials excellent candidates for solid oxide electrolytes at intermediate temperatures.

Keywords: electrolyte, Ceria, X-ray diffraction, EIS, SEM, SOFC

Procedia PDF Downloads 113

Authors: Hong Seung Kim, Chang Hoi Kim, Lili Yue

Abstract:

Single-phase, high band gap energy Zn0.5Mg0.5O films were grown under oxygen pressure, using pulse laser deposition with a Zn0.5Mg0.5O target. Structural characterization studies revealed that the crystal structures of the ZnX-1MgXO films could be controlled via changes in the oxygen pressure. TEM analysis showed that the thickness of the deposited Zn1-xMgxO thin films was 50–75 nm. As the oxygen pressure increased, we found that one axis of the crystals did not show a very significant increase in the crystallization compared with that observed at low oxygen pressure. The X-ray diffraction peak intensity for the hexagonal-ZnMgO (002) plane increased relative to that for the cubic-ZnMgO (111) plane. The corresponding c-axis of the h-ZnMgO lattice constant increased from 5.141 to 5.148 Å, and the a-axis of the c-ZnMgO lattice constant decreased from 4.255 to 4.250 Å. EDX analysis showed that the Mg content in the mixed-phase ZnMgO films decreased significantly, from 54.25 to 46.96 at.%. As the oxygen pressure was increased from 100 to 150 mTorr, the absorption edge red-shifted from 3.96 to 3.81 eV; however, a film grown at the highest oxygen pressure tested here (200 mTorr).

Keywords: MgO, UV LED, ZnMgO, ZnO

Procedia PDF Downloads 384

Authors: Lukman O. Alimi, Vincent J. Smith, Leonard J. Barbour

Abstract:

The thermosalient effect is an extremely rare propensity of certain crystalline solids for self-actuation by elastic deformation or a ballistic event1. Thermosalient compounds, colloquially known as ‘jumping crystals’ are promising materials for fabrication of actuators that are also being considered as materials for clean energy conversion because of their capabilities to convert thermal energy into mechanical motion directly. Herein, an organic aminonitrile and its derivatives have been probed by a combination of structural, microscopic and thermoanalytical techniques. Crystals of these compounds were analysed by means of single crystal XRD and hotstage microscopy in the temperature range of 100 to 298 K and found to exhibit the thermosalient effect. We also carried out differential scanning calorimetric analysis at the temperature corresponding to that at which the crystal jumps as observed under a hotstage microscope.

Keywords: aminonitrile, jumping crystal, self actuation, thermosalient effect

Procedia PDF Downloads 408

Authors: Nesrine Benarous, Hassiba Bougueria, Nabila Moussa Slimane, Aouatef Cherouana

Abstract:

Crystal polymorphism is important for the synthesis of more potent and bioactive pharmaceutical compounds, including their different properties, such as packing arrangement and conformation. In fact, polymorphism plays a vital role in drug development. Different parameters affect the crystallization and give their degree of freedom. Severalproperties affected polymorphism, like kinetics, thermodynamics, spectroscopy, and mechanical property. Various techniques are used for characterizing polymorphs, are crystallography, morphology, phase transitions, molecular motion, and chemical environment. In this work, crystal structures of two polymorphs (I and II) of the Schiff base (SB) title compound were prepared by condensation reaction. The crystal structures of both polymorphs were determined by single X-ray analysis. The two polymorphs crystallize in two different space groups: P21/c for I and Pbca for II. The dihedral angles between the two phenyl rings are 4.81º for I and 82.27º for II. Both crystal structures are built on the basis of moderate and weak hydrogen bonds, 𝜋-stacking, and halogen⋯halogeninteractions. On the other hand, Hirshfeld surface (HS) analysis indicates that the most important contributions to the crystal packing for the two polymorphs are from Cl⋯H/H⋯Cl, H⋯H, and N⋯H/H⋯N contacts. These are followed by C⋯H/H⋯C for compound I and C⋯C and by C⋯H/H⋯C contacts for compound II. Afterwards, the in vitro antibacterial activity revealed that the SB have been found effective against G- bacteria Klebsiella pneumonia andG+ bacteria Staphylococcus aureuswith MIC value of14.37μg/mL. Moreover, the SBexhibited moderate toxicity against Brine Shrimp with LC50 value of 44.19μg/mL.

Keywords: polymorph, crystal structure, hirshfeld surface analysis, in vitro antibacterial activity, toxicity

Procedia PDF Downloads 65

Authors: Rabindranath Bag, Surjeet Singh

Abstract:

Materials in which the electrons are strongly correlated provide some of the most challenging and exciting problems in condensed matter physics today. After the discovery of high critical temperature superconductivity in layered or two-dimensional copper oxides, many physicists got attention in cuprates and it led to an upsurge of interest in the synthesis and physical properties of copper-oxide based material. The quest to understand superconducting mechanism in high-temperature cuprates, drew physicist’s attention to somewhat simpler compounds consisting of spin-chains or one-dimensional lattice of coupled spins. Low-dimensional quantum magnets are of huge contemporary interest in basic sciences as well emerging technologies such as quantum computing and quantum information theory, and heat management in microelectronic devices. Spin ladder is an example of quasi one-dimensional quantum magnets which provides a bridge between one and two dimensional materials. One of the examples of quasi one-dimensional spin-ladder compounds is Sr14Cu24O41, which exhibits a lot of interesting and exciting physical phenomena in low dimensional systems. Very recently, the ladder compound Sr14Cu24O41 was shown to exhibit long-distance quantum entanglement crucial to quantum information theory. Also, it is well known that hole-compensation in this material results in very high (metal-like) anisotropic thermal conductivity at room temperature. These observations suggest that Sr14Cu24O41 is a potential multifunctional material which invites further detailed investigations. To investigate these properties one must needs a large and high quality of single crystal. But these systems are showing incongruently melting behavior, which brings many difficulties to grow a large and quality of single crystals. Hence, we are using TSFZ (Travelling Solvent Floating Zone) method to grow the high quality of single crystals of the low dimensional magnets. Apart from this, it has unique crystal structure (alternating stacks of plane containing edge-sharing CuO2 chains, and the plane containing two-leg Cu2O3 ladder with intermediate Sr layers along the b- axis), which is also incommensurate in nature. It exhibits abundant physical phenomenon such as spin dimerization, crystallization of charge holes and charge density wave. The maximum focus of research so far involved in introducing defects on A-site (Sr). However, apart from the A-site (Sr) doping, there are only few studies in which the B-site (Cu) doping of polycrystalline Sr14Cu24O41 have been discussed and the reason behind this is the possibility of two doping sites for Cu (CuO2 chain and Cu2O3 ladder). Therefore, in our present work, the crystals (pristine and Cu-site doped) were grown by using TSFZ method by tuning the growth parameters. The Laue diffraction images, optical polarized microscopy and Scanning Electron Microscopy (SEM) images confirm the quality of the grown crystals. Here, we report the single crystal growth, magnetic and transport properties of Sr14Cu24O41 and its lightly doped variants (magnetic and non-magnetic) containing less than 1% of Co, Ni, Al and Zn impurities. Since, any real system will have some amount of weak disorder, our studies on these ladder compounds with controlled dilute disorder would be significant in the present context.

Keywords: low-dimensional quantum magnets, single crystal, spin-ladder, TSFZ technique

Procedia PDF Downloads 247

Authors: Morteza Mohri Esfahani, Amir S. H. Rozatian, Morteza Mozaffari

Abstract:

Single phase magnetite nanoparticles and Bi-substituted ones were prepared by mechanochemical processing (MCP). The effects of Bi-substitution on the structural and magnetic properties of the nanoparticles were studied by X-ray Diffraction (XRD) and magnetometry techniques, respectively. The XRD results showed that all samples have spinel phase and by increasing Bi content, the main diffraction peaks were shifted to higher angles, which means the lattice parameter decreases from 0.843 to 0.838 nm and then increases to 0.841 nm. Also, the results revealed that increasing Bi content lead to a decrease in saturation magnetization (Ms) from 74.9 to 48.8 emu/g and an increase in coercivity (Hc) from 96.8 to 137.1 Oe.

Keywords: bi-substituted magnetite nanoparticles, mechanochemical processing, X-ray diffraction, magnetism

Procedia PDF Downloads 505

Authors: Kei Kamada, Rikito Murakami, Masahiko Ito, Mototaka Arakawa, Yasuhiro Shoji, Toshiyuki Ueno, Masao Yoshino, Akihiro Yamaji, Shunsuke Kurosawa, Yuui Yokota, Yuji Ohashi, Akira Yoshikawa

Abstract:

Techniques of energy harvesting y have been widely developed in recent years, due to high demand on the power supply for ‘Internet of things’ devices such as wireless sensor nodes. In these applications, conversion technique of mechanical vibration energy into electrical energy using magnetostrictive materials n have been brought to attention. Among the magnetostrictive materials, Fe-Ga and Fe-Al alloys are attractive materials due to the figure of merits such price, mechanical strength, high magnetostrictive constant. Up to now, bulk crystals of these alloys are produced by the Bridgman–Stockbarger method or the Czochralski method. Using these method big bulk crystal up to 2~3 inch diameter can be grown. However, non-uniformity of chemical composition along to the crystal growth direction cannot be avoid, which results in non-uniformity of magnetostriction constant and reduction of the production yield. The micro-pulling down (μ-PD) method has been developed as a shaped crystal growth technique. Our group have reported shaped crystal growth of oxide, fluoride single crystals with different shape such rod, plate tube, thin fiber, etc. Advantages of this method is low segregation due to high growth rate and small diffusion of melt at the solid-liquid interface, and small kerf loss due to near net shape crystal. In this presentation, we report the shaped long plate crystal growth of Fe-Ga and Fe-Al alloys using the μ-PD method. Alloy crystals were grown by the μ-PD method using calcium oxide crucible and induction heating system under the nitrogen atmosphere. The bottom hole of crucibles was 5 x 1mm² size. A <100> oriented iron-based alloy was used as a seed crystal. 5 x 1 x 320 mm³ alloy crystal plates were successfully grown. The results of crystal growth, chemical composition analysis, magnetostrictive properties and a prototype vibration energy harvester are reported. Furthermore, continuous crystal growth using powder supply system will be reported to minimize the chemical composition non-uniformity along the growth direction.

Keywords: crystal growth, micro-pulling-down method, Fe-Ga, Fe-Al

Procedia PDF Downloads 306

Authors: P. Mirahmadpour, M. H. Banitaba, D. Nematollahi

Abstract:

The chemistry of coordination polymers in recent years has grown exponentially not only because of their interesting architectures but also due to their various technical applications in many fields including ion exchange, chemical catalysis, small molecule separations, and drug release. The use of bridging ligands for the controlled self-assembly of one, two or three dimensional metallo-supramolecular species is the subject of serious study in last decade. Numerous different synthetic methods have been offered for the preparation of coordination polymers such as (a) diffusion from the gas phase, (b) slow diffusion of the reactants into a polymeric matrix, (c) evaporation of the solvent at ambient or reduced temperatures, (d) temperature controlled cooling, (e) precipitation or recrystallisation from a mixture of solvents and (f) hydrothermal synthesis. The electrosynthetic process suggested several advantages over conventional approaches. A general advantage of electrochemical synthesis is that it allows synthesis under milder conditions than typical solvothermal or microwave synthesis. In this work we have introduced a simple electrochemical method for growing metal coordination polymers based on copper with a flexible 2,2’-thiodiacetic acid (TDA) and rigid 1,2,4,5-benzenetetracarboxylate (BTC) ligands. The structure of coordination polymers were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), elemental analysis, thermal gravimetric (TG) and differential thermal analyses (DTA). The single-crystal X-ray diffraction analysis revealed that different conformations of the ligands and different coordination modes of the carboxylate group as well as different coordination geometries of the copper atoms. Electrochemical synthesis of coordination polymers has different advantages such as faster synthesis at lower temperature in compare with conventional chemical methods and crystallization of desired materials in a single synthetic step.

Keywords: 1, 2, 4, 5-benzenetetracarboxylate, coordination polymer, copper, 2, 2’-thiodiacetic acid

Procedia PDF Downloads 179

Authors: Jatupon Em-Udom, Nirand Pisutha-Arnond

Abstract:

The phase-field-crystal, PFC, approach is a density-functional-type material model with an atomic resolution on a diffusive timescale. Spatially, the model incorporates periodic nature of crystal lattices and can naturally exhibit elasticity, plasticity and crystal defects such as grain boundaries and dislocations. Temporally, the model operates on a diffusive timescale which bypasses the need to resolve prohibitively small atomic-vibration time steps. The PFC model has been used to study many material phenomena such as grain growth, elastic and plastic deformations and solid-solid phase transformations. In this study, the pressure-controlled dynamic equation for the PFC model was developed to simulate a single-component system under externally applied pressure; these coupled equations are important for studies of deformable systems such as those under constant pressure. The formulation is based on the non-equilibrium thermodynamics and the thermodynamics of crystalline solids. To obtain the equations, the entropy variation around the equilibrium point was derived. Then the resulting driving forces and flux around the equilibrium were obtained and rewritten as conventional thermodynamic quantities. These dynamics equations are different from the recently-proposed equations; the equations in this study should provide more rigorous descriptions of the system dynamics under externally applied pressure.

Keywords: driving forces and flux, evolution equation, non equilibrium thermodynamics, Onsager’s reciprocal relation, phase field crystal model, thermodynamics of single-component solid

Procedia PDF Downloads 280

Authors: Sakshi Tomar, Renu Chadha

Abstract:

Cocrystallization comprises a selective route to the intensive design of pharmaceutical products with desired physiochemical and pharmacokinetic properties. The present study is focused on the preparation, characterization, and evaluation of etodolac (ET) co-crystals with coformers nicotinamide (ETNI) and Glutaric acid (ETGA), using cocrystallization approach. Preliminarily examination of the prepared co-crystal was done by differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (PXRD). DSC thermographs of ETNI and ETGA cocrystals showed single sharp melting endotherms at 144°C and 135°C, respectively, which were different from the melting of drugs and coformers. FT-IR study points towards carbonyl-acid interaction sandwiched between the involving molecules. The emergence of new peaks in the PXRD pattern confirms the formation of new crystalline solid forms. Both the cocrystals exhibited better apparent solubility, and 3.8-5.0 folds increase in IDR were established, as compared to pure etodolac. Evaluations of these solid forms were done using anti-osteoarthritic activities. All the results indicate that etodolac cocrystals possess better anti-osteoarthritic efficacy than free drug. Thus loom of cocrystallization has been found to be a viable approach to resolve the solubility and bioavailability issues that circumvent the use of potential antiosteoarthritic molecules.

Keywords: bioavailability, etodolac, nicotinamide, osteoarthritis

Procedia PDF Downloads 174

Authors: I. Shuro

Abstract:

The crystal structure of Tin Sulfide prepared by certain chemical methods is investigated using High-Resolution Transmission Electron Microscopy (HRTEM), Scanning Electron Microscopy (SEM), and X-ray diffraction (XRD) methods. An anomalous HRTEM Fast Fourier Transform (FFT) exhibited a central scatter of diffraction spots, which is surrounded by secondary clusters of spots arranged in a hexagonal pattern around the central cluster was observed. FFT analysis has revealed a long lattice parameter and mostly viewed along a hexagonal axis where there many columns of atoms slightly displaced from one another. This FFT analysis has revealed that the metal sulfide has a long-range order interwoven chain of atoms in its crystal structure. The observed crystalline structure is inconsistent with commonly observed FFT patterns of chemically synthesized Tin Sulfide nanocrystals and thin films. SEM analysis showed the morphology of a myriad of multi-shaped crystals ranging from hexagonal, cubic, and spherical micro to nanostructured crystals. This study also investigates the presence of quasi-crystals as reflected by the presence of mixed local symmetries.

Keywords: fast fourier transform, high resolution transmission electron microscopy, tin sulfide, crystalline structure

Procedia PDF Downloads 113

Authors: Soufiane Zerraf, Malika Tridane, Said Belaaouad

Abstract:

CuHPO₃.2H₂O was synthesized by the direct method. CuHPO₃.2H₂O crystallizes in the orthorhombic system, space group P2₁2₁2₁, a = 6.7036 (2) Å, b = 7.3671 (4) Å, c = 8.9749 (4) Å, Z = 4, V = 443.24 (4) ų. The crystal structure was refined to R₁= 0.0154, R₂= 0.0380 for 19018 reflections satisfying criterion I ≥ 2σ (I). The structural resolution shows the existence of chains of ions HPO₃- linked together by hydrogen bonds. The crystalline structure is formed by chains consisting of Cu[O₃(H₂O)₃] deformed octahedral, which are connected to the vertices. The chains extend parallel to b and are mutually linked by PO₃ groups. The structure is closely related to that of CuSeO₃.2H₂O and CuTeO₃.2H₂O. The experimental studies of the infrared and Raman spectra were used to confirm the presence of the phosphate ion and were compared in the (0-4000) cm-1 region with the theoretical results calculated by the density functional theory (DFT) method to provide reliable assignments of all observed bands in the experimental spectra.

Keywords: crystal structure, X-ray diffraction, vibration study, thermal behavior, density functional theory

Procedia PDF Downloads 82

Authors: Mihai I. Sturza, Laura T. Corredor, Kaustuv Manna, Gizem A. Cansever, Tushar Dey, Andrey Maljuk, Olga Kataeva, Sabine Wurmehl, Anja Wolter, Bernd Buchner

Abstract:

Recently, the iridate double perovskite Sr₂YIrO₆ has attracted considerable attention due to the report of unexpected magnetism in this Ir⁵⁺ material, in which according to the Jeff model, a non-magnetic ground state is expected. Structural, magnetic and thermodynamic investigations of Sr₂YIrO₆ and Ba2YIrO6 single crystals, with emphasis on the temperature and magnetic field dependence of the specific heat will be presented. The single crystals were grown by using SrCl₂ and BaCl₂ as flux. Single-crystal X-ray diffraction measurements performed on several crystals from different preparation batches showed a high quality of the crystals, proven by the good internal consistency of the data collected using the full-sphere mode and an extremely low R factor. In agreement with the expected non-magnetic ground state of Ir⁵⁺ (5d4) in these iridates, no magnetic transition is observed down to 430 mK. Moreover, our results suggest that the low-temperature anomaly observed in the specific heat is not related to the onset of long-range magnetic order. Instead, it is identified as a Schottky anomaly caused by paramagnetic impurities present in the sample, of the order of

Keywords: double perovskites, iridates, self-flux grown synthesis, spin-orbit coupling

Procedia PDF Downloads 300

Authors: Yalçın Kılıç, İbrahim Kani

Abstract:

The conversion of hydrocarbons to carbonyl compounds by oxidation reaction is one of the most important reactions in the synthesis of fine chemicals. As a result of the oxidation of hydrocarbons containing aliphatic sp3-CH groups in their structures, aldehydes, ketones or carboxylic acids can be obtained. In this study, OSSO-type 2,2'-[1,4-butanedylbis(thio)]bis-benzoic acid (tsabutH2) ligand and [Zn(µ-tsabut)(phen)]n complex (where phen = 1,10-phenantroline) were synthesized and their structures were characterized by single crystal x-ray diffraction method. The catalytic efficiency of the complex in the catalytic oxidation studies of organic compounds such as cyclohexane, ethylbenzene, diphenylmethane, and p-xylene containing sp3-C-H in its structure was investigated.

Keywords: metal complex, OSSO-type ligand, catalysis, oxidation

Procedia PDF Downloads 69

Authors: F. Karim

Abstract:

In this paper, triangular lattice index-guiding photonic crystal fibers (PCFs) are synthesized to compensate the chromatic dispersion of a single mode fiber (SMF-28) for an 80 km optical link operating at 1.55 µm, by using the directed tabu search algorithm. Hole-to-hole distance, circular air-hole diameter, solid-core diameter, ring number and PCF length parameters are optimized for this purpose. Three Synthesized PCFs with different physical parameters are compared in terms of their objective functions values, residual dispersions and compensation ratios.

Keywords: triangular lattice index-guiding photonic crystal fiber, dispersion compensation, directed tabu search, synthesis

Procedia PDF Downloads 406

Authors: Kanda Wongwailikhit

Abstract:

Copper (I) oxide microparticles with the morphology of cubic and hollow sphere were synthesized with the assistance of a surfactant as the shape controller. Both particles were then subjected to a study of the catalytic activity and the results of shape effects of catalysts on rate of catalytic reaction was observed. The decolorizing reaction of crystal violet and sodium hydroxide was chosen and the decrease of reactant with respect to time was measured using a spectrophotometer. The result revealed that morphology of the crystal had no effect on the catalytic activity for the crystal violet reaction but contributed to total surface area predominantly.

Keywords: copper (I) oxide, catalytic activity, crystal violet

Procedia PDF Downloads 471

Authors: Andrei Bejan, Luminita Marin, Dalila Belei

Abstract:

Phenothiazine with electron-rich nitrogen and sulfur heteroatoms has a high electron-donating ability which promotes a good conjugation and therefore low band-gap with consequences upon charge carrier mobility improving and shifting of light emission in visible domain. Moreover, its non-planar butterfly conformation inhibits molecular aggregation and thus preserves quite well the fluorescence quantum yield in solid state compared to solution. Therefore phenothiazine and its derivatives are promising hole transport materials for use in organic electronic and optoelectronic devices as light emitting diodes, photovoltaic cells, integrated circuit sensors or driving circuits for large area display devices. The objective of this paper was to obtain a series of new phenothiazine derivatives by introduction of different electron withdrawing substituents as formyl, carboxyl and cyanoacryl units in order to create a push pull system which has potential to improve the electronic and optical properties. Bromine atom was used as electrono-donor moiety to extend furthermore the existing conjugation. The understudy compounds were structural characterized by FTIR and 1H-NMR spectroscopy and single crystal X-ray diffraction. Besides, the single crystal X-ray diffraction brought information regarding the supramolecular architecture of the compounds. Photophysical properties were monitored by UV-vis and photoluminescence spectroscopy, while the electrochemical behavior was established by cyclic voltammetry. The absorption maxima of the studied compounds vary in a large range (322-455 nm), reflecting the different electronic delocalization degree, depending by the substituent nature. In a similar manner, the emission spectra reveal different color of emitted light, a red shift being evident for the groups with higher electron withdrawing ability. The emitted light is pure and saturated for the compounds containing strong withdrawing formyl or cyanoacryl units and reach the highest quantum yield of 71% for the compound containing bromine and cyanoacrilic units. Electrochemical study show reversible oxidative and reduction processes for all the compounds and a close correlation of the HOMO-LUMO band gap with substituent nature. All these findings suggest the obtained compounds as promising materials for optoelectronic devices.

Keywords: electrochemical properties, phenothiazine derivatives, photoluminescence, quantum yield

Procedia PDF Downloads 305

Authors: Kirsten Techmer, Jan-Erik Rybak, Simon Rudolph

Abstract:

Natural formed pyrites (FeS2) are frequent sulfides in sedimentary and metamorphic rocks. Growth textures of idiomorphic pyrite assemblages reflect the conditions during their formation in the geologic sequence, furtheron the local texture analyses of the growth patterns of pyrite assemblages by EBSD reveal the possibility to resolve the growth conditions during the formation of pyrite at the micron scale. The spatial resolution of local texture measurements in the Scanning Electron Microscope used can be in the nanomete scale. Orientation contrasts resulting from domains of smaller misorientations within larger pyrite crystals can be resolved as well. The electron optical studies have been carried out in a Field-Emission Scanning Electron Microscope (FEI Quanta 200) equipped with a CCD camera to study the orientation contrasts along the surfaces of pyrite. Idiomorphic cubic single crystals of pyrite, polycrystalline assemblages of pyrite, spherically grown spheres of pyrite as well as pyrite-bearing ammonites have been studied by EBSD in the Scanning Electron Microscope. Samples were chosen to show no or minor secondary deformation and an idiomorphic 3D crystal habit, so the local textures of pyrite result mainly from growth and minor from deformation. The samples studied derived from Navajun (Spain), Chalchidiki (Greece), Thüringen (Germany) and Unterkliem (Austria). Chemical analyses by EDAX show pyrite with minor inhomogeneities e.g., single crystals of galena and chalcopyrite along the grain boundaries of larger pyrite crystals. Intergrowth between marcasite and pyrite can be detected in one sample. Pyrite may form intense growth twinning lamellae on {011}. Twinning, e.g., contact twinning is abundant within the crystals studied and the individual twinning lamellaes can be resolved by EBSD. The ammonites studied show a replacement of the shale by newly formed pyrite resulting in an intense intergrowth of calcite and pyrite. EBSD measurements indicate a polycrystalline microfabric of both minerals, still reflecting primary surface structures of the ammonites e.g, the Septen. Discs of pyrite (“pyrite dollar”) as well as pyrite framboids show growth patterns comprising a typical microfabric. EBSD studies reveal an equigranular matrix in the inner part of the discs of pyrite and a fiber growth with larger misorientations in the outer regions between the individual segments. This typical microfabric derived from a formation of pyrite crystals starting at a higher nucleation rate and followed by directional crystal growth. EBSD studies show, that the growth texture of pyrite in the samples studied reveals a correlation between nucleation rate and following growth rate of the pyrites, thus leading to the characteristic crystal habits. Preferential directional growth at lower nucleation rates may lead to the formation of 3D framboids of pyrite. Crystallographic misorientations between the individual fibers are similar. In ammonites studied, primary anisotropies of the substrates like e.g., ammonitic sutures, influence the nucleation, crystal growth and habit of the newly formed pyrites along the surfaces.

Keywords: Electron Back Scatter Diffraction (EBSD), growth pattern, Fe-sulfides (pyrite), texture analyses

Procedia PDF Downloads 258