Energy Dispersive X-ray Analysis Studies Research Articles

Single crystal synthesis and characterization of proposed eight-fold degenerate topological material Bi2PdO4

Materials with nonsymmorphic symmetries have numerous applications and have recently come to the forefront as potentially containing novel topological states of matter, such as eight-fold fermions. In this paper, we report the single crystal growth of eight-fold degenerate topological material, Bi2PdO4 via melt-growth technique. The structural properties and chemical composition are confirmed by X-ray diffraction (XRD) and energy-dispersive x-ray analysis studies, respectively. Powder XRD shows that Bi2PdO4 crystallizes in the tetragonal P4/ncc (#130) type structure which is made up of PdO4 square planar units along the c direction. Because of the decreasing trend of magnetization with field, this sample exhibits room temperature diamagnetism. Our temperature dependent resistivity measurement suggests the semiconducting nature of the compound with an estimated band gap of ∼153 meV from Arrhenius fitting. Our Raman spectroscopy data shows peak shifting with decreasing temperature from 300 K to 100 K. Our density functional theory calculation suggests eightfold band crossing at the A point. From our DFT calculations, we determined a band gap of 176 meV in the absence of Spin-Orbit Coupling (SOC) and 180 meV with SOC. This aligns with our experimental observations. Finally, our present study provides a new direction for further transport and spectroscopic investigation in this compound.

Synthesis of nano hydroxyapatite from Hypopthalmichthys molitrix (silver carp) bone waste by two different methods: a comparative biophysical and in vitro evaluation on osteoblast MG63 cell lines.

More than a thousand tonnes of fish bone wastes can be transformed into biomedical products annually. Alkaline hydrolysis and thermal calcification were used to create nanosized hydroxyapatite (HAp) crystals from Silver carp bone wastes. Biophysical tests were used to determine the nano size and chemical composition of synthesised hydroxyapatite. Alkaline hydrolysis hydroxyapatite (AH-HAp) was 58.3nm, while Thermal calcination hydroxyapatite (TC-HAp) was 64.3nm in size, confirmed by Atomic Force Microscopy. Energy Dispersive X-ray Analysis studies showed Ca/P (Calcium phosphate) ratio of AH-HAp to be 1.65, whereas TC-HAp as 1.45, confirming AH-HAp to be organically rich along with a similar Ca/P ratio as natural HAp. Fourier Transform Infrared Spectroscopy spectra indicated HAp formation from both procedures, however AH-HAp had superior crystallinity than TC-HAp confirmed from X-Ray Diffraction spectra. MG63 osteoblast cell lines showed 91% cell viability in cytotoxicity studies and 70.1% proliferation efficiency in Alkaline Phosphatase assay, which was higher than TC-HAp. The present study shows that HAp produced via alkaline hydrolysis has better biocompatibility which enhances its applicability as a biomaterial, than HAp synthesized through thermal calcination, which tends to incinerate organic moieties.

Synthesis of tetrahedral patchy nanoparticles with controlled patch size

Silica nanoparticles with four circular surface patches made of polystyrene (PS) and arranged in a tetrahedral symmetry are synthesized through the multistep growth of the silica core of silica/PS tetrapods. Transmission electron microscopy and energy dispersive X-ray analysis studies indicate that, as the silica core regrows, its surface conforms to the shape of the polystyrene nodules, allowing good control of the size of the emerged fraction of these. Patches with an angular width as small as 49° were achieved, which is a prerequisite for their assembly in the form of a diamond crystal phase.

Fourier Transform Infrared, X-Ray Diffraction and Energy Dispersive X-Ray Analysis Studies on the Adsorption of Copper Ii Ions Prepared From Mimusops Elengi Leaves in Aqueous Solution against Acid Activated Carbon

Adsorption considers were finished by watching the effects of various preliminary limits ejection of copper (II) particles from watery course of action. Morphology of adsorbent on account of adsorption has been destitute down PH, FT-IR spectra, EDX and XRD examination. The data were fitted into the Langmuir and Freundlich adsorption isotherm conditions. Thermodynamics limits like change in free imperativeness, enthalpy and entropy were resolved.

Synthesis lead sulphide thin films from tartaric acid chemical bath: Study the role of film thickness on the structural, optical and electrical properties

Tartaric acid used as a complexing agent to synthesized crystalline lead sulphide thin films on microscope glass via chemical route. The influence of varying the film thickness on the electrical, morphological, photoluminescence and structural properties of the deposited material were studied by employing different techniques. The X-ray diffraction (XRD) study established that the prepared films had face centered cubic crystal structure irrespective of film thickness, however, their crystalline preferentially growth along the (111), (200) and (220) planes. The XRD study also promoted that film thickness had visible effect on the dislocation density and other structural parameters of the synthesized PbS film. The energy dispersive X-ray analysis study confirmed the presence of Pb and S elements in the prepared samples. The optical band gap calculated from Tauc relation was estimated in the range of 1.02 eV to 0.73 eV. Furthermore, dielectric constant, linear optical susceptibility and the refractive index of the films were estimated systematically. The presence of various functional groups were confirmed by Fourier transform-infrared spectroscopy analyses. The prepared films conductivity estimated in the order of 10−2 (Ωcm)−1 and had direct relations with film thickness. The hot probe measurements verified that the deposited PbS films are n-type semiconductors.

Hydrogen storage properties of Ti2FeV BCC solid solution

This paper deals with hydrogen storage properties of Ti-V based BCC solid solution incorporated with Fe. The alloy with composition Ti2FeV was prepared by arc melting method. X-ray diffraction (XRD) and energy dispersive X-ray analysis studies confirmed formation of solid solution phase with uniform composition and BCC structure. SEM studies revealed the formation of irregular shaped particles with size in the range of few microns up on hydrogenation of the parent alloy. The alloy shows maximum hydrogen storage capacity of 3.41 wt.% at 20 bar and 303 K and the thermodynamic parameters established near room temperature suitability of the alloy for solid state hydrogen storage applications. Hydrogenation kinetics is found to be quite fast and detailed kinetic analysis were done to underscore the hydrogenation mechanism. Activation energy during the initial stage of hydrogenation is found to be 30.8 kJ/mol. The value decreases to 14.4 kJ/mol for extended duration of hydrogenation, and this is explained based on difference in rate determining steps existing at different time scales. Extent of hydrogen absorption as a function of temperature and time for Ti2FeV alloy.

Effect of indium and antimony doping on the transport properties of direct vapour transport (DVT) grown SnSe single crystals

Pure SnSe, 5% In, 10% In, 5% Sb, and 10% Sb doped SnSe single crystals were grown by the direct vapour transport technique. The energy dispersive X-ray analysis study of the samples showed them to be near stoichiometric but slightly Sn deficient. The X-ray diffraction study of all the as-grown single crystal samples showed that they possess an orthorhombic structure and the lattice parameters are in good agreement with the reported parameters. The thermoelectric power (S), dc electrical conductivity (σ), and thermal conductivity (κ) variation with temperature from ambient to 573 K substantiated the semiconducting nature of all the five samples. The sign of “S” was positive for all five samples for all the temperature range stating the sample to be a p-type semiconductor. The power factor (S2σ) and figure of merit (ZT) variation with temperature showed that pure SnSe possesses the highest value compared to doped samples. The obtained results are studied and discussed in detail.

Concomitant preparation of ZnS thin film and nanopowder forms from SILAR baths: An attempt to sort-out wastage problem

As wastage of a large percentage of source material used is the main disadvantage of successive ionic layer adsorption and reaction (SILAR) technique, in the present work, a new approach is adopted by simultaneously preparing thin films and powders from the SILAR bath solutions. The amount of source material used for thin film and powder form is estimated to find the resultant wastage. In this study, ZnS thin film and ZnS powder were prepared from the same SILAR bath. The characteristics of both the product were analyzed using X-ray diffraction, optical, energy dispersive X-ray analysis studies and the photocatalytic abilities of the prepared samples were determined and compared.

A third generation solar cell based on wet-chemically etched Si nanowires and sol-gel derived Cu2ZnSnS4 thin films

Monophase Cu2ZnSnS4 (CZTS) thin films have been succesfully deposited on both soda lime glass substrate and Si nanowire (NW) arrays by a simple and cost-effective production route based on a combination of sol-gel and spin-coating technique. X-ray diffraction and energy dispersive X-ray analysis studies have revealed that post-annealing process at 350 °C is a sufficient temperature for the growth of a stoichiometric mono-phase CZTS thin film. The band gap energy of the films was found to be 1.55 eV. Following the optimization of CZTS thin films, they were deposited on the Si-NWs as an absorber layer for the fabrication of n-Si-NWs/p-CZTS structured solar cell. From the recorded I-V characteristics of the constructed solar cells under standard condition (A.M 15G), the power conversion efficiency was found to be 1.0 ± 0.1%.

Biogenic synthesis of multidimensional gold nanoparticles assisted by Streptomyces hygroscopicus and its electrochemical and antibacterial properties

The fabrication of reliable, green chemistry processes for nanomaterial synthesis is an important aspect of nanotechnology. The biosynthesis of single-pot room-temperature reduction of aqueous chloroaurate ions by Streptomyces hygroscopicus cells has been reported to facilitate the development of an industrially viable greener methodology for the synthesis of technologically important gold nanoparticles (AuNPs). Multidimensional AuNPs are generated via the manipulation of key growth parameters, including solution pH and reaction time. The synthesized nanostructures are characterized by UV/Vis and energy dispersive X-ray analysis studies. Particle morphology is characterized by HRTEM, FE-SEM and BioAFM. Additionally, we have demonstrated the electrochemical and antibacterial properties of AuNPs via cyclic voltammetry analysis and a minimal inhibitory concentration assay. Owing to the drawbacks of chemical synthesis, a biological synthesis method has been developed to generate biocompatible, inexpensive and eco-friendly size-controlled nanoparticles.

Synthesis of Silver–Iron Oxide Nanocomposites by Thermal Decomposition

Silver-iron oxide nanocomposites were synthesized by an easy thermal decomposition method using iron acetyl acetonate and silver acetate as precursors and oleic acid (OA) and oleyl amine (OLA) as the capping agents in a single step. The composite samples were characterized by X-ray diffraction (XRD), infrared spectroscopy, thermal gravimetric analysis (TGA), UV-Visible spectroscopy, scanning electron microscopy (SEM), and magnetic measurements. Powder XRD and UV-Visible spectroscopy results indicate the presence of nanocrystalline silver in the composite and the FT-IR results coupled with TGA results indicate the presence of ligand molecules on surface of the nanocomposites. The FE-SEM images show that the nanocomposite particles are mainly spherical in shape while the energy dispersive X-ray analysis studies indicate the presence of iron and oxygen in the composites. From the magnetic measurements, the composites were found to be superparamagnetic with characteristic blocking temperatures indicating the presence of iron oxide nanoparticles in the nanocomposites.

Comparative study for physical properties and corrosion mechanism of synthetic and in situ MgAl2O4 spinel formation zero cement refractory castables

Magnesium aluminate spinel (MgAl2O4) is an excellent castable refractory product due to its high temperature thermal, chemical and mechanical properties. Alumina spinel castables are produced by addition of synthetic spinel or in situ spinel formation during the firing process. In the first part of the experimental studies, alumina rich MgAl2O4 spinel castable was produced using a solid state reaction technique. Tabular alumina and sea water magnesia (<100 μm) were used as starting raw materials. In the second part of the experimental studies, commercial synthetic spinel added castables were produced. In order to compare experimental results, both parts of the experimental study involved compositions with the same proportions of MgO. α-500 hydratable alumina was used as binder. Castables were sintered at 1500 and 1600°C. Water absorption, apparent porosity, bulk density and cold crushing strength values were considered and the optimum sintering temperature, proportions of synthetic spinel and sea water magnesia were determined. The XRD patterns confirm the phase formation of MgAl2O4. Moreover, the physical properties of the castables were supported by this XRD analysis. Scanning electron microscopy investigations of the fired samples were carried out to compare the effect of synthetic spinel addition and in situ phase formation on the physical properties of the castables. The mechanism of slag penetration to two types of zero cement castables for steel ladles was examined and the penetration layer chemically analysed by energy dispersive X-ray analysis studies.

In vitro calcification of chemically functionalized carbon nanotubes

Bone is composed of two phases. The organic phase is made of collagen fibrils assembled in broad fibers acting as a template for mineralization. The mineral phase comprises hydroxyapatite (HAP) crystals grown between and inside the collagen fibers. We have developed a biomimetic material using functionalized carbon nanotubes as scaffold to initiate in vitro mineralization. Biomimetic formation of HAP was performed on single-walled carbon nanotubes (SWCNTs) which have been grafted with carboxylic groups. Two types of nanotubes, HiPco(R) and Carbon Solutions(R), were oxidized via various acidic processes, leading to five different groups of carboxylated nanotubes, fully characterized by physical methods (thermogravimetric analysis, attenuated total reflectance infrared spectroscopy and X-ray photoelectron spectroscopy). All samples were dispersed in ultra-pure water and incubated for 2weeks in a synthetic body fluid, in order to induce the calcification of the SWCNTs. Scanning electron microscopy (SEM) and energy-dispersive X-ray analysis studies showed that Ca(2+) and PO(4)(3-) ions were deposited as round-shaped nodules (calcospherites) on the carboxylated SWCNTs. Fourier transform infrared and Raman spectroscopic studies confirmed the HAP formation, and image analysis made on SEM pictures showed that calcospherites and carboxylated SWCNTs were packed together. The size of calcospherites thus obtained in vitro from the HiPco(R) series was close to that issued from calcospherites observed in vivo. Functionalization of SWCNTs with carboxylic groups confers the capacity to induce calcification similar to woven bone.

Microbial Synthesis of Multishaped Gold Nanostructures

The development of methodologies for the synthesis of nanoparticles of well-defined size and shape is a challenging one and constitutes an important area of research in nanotechnology. This Full Paper describes the controlled synthesis of multishaped gold nanoparticles at room temperature utilizing a simple, green chemical method by the interaction of chloroauric acid (HAuCl4 x 3H20) and cell-free extract of the fungal strain Rhizopus oryzae. The cell-free extract functions as a reducing, shape-directing, as well as stabilizing, agent. Different shapes of gold nanocrystals, for example, triangular, hexagonal, pentagonal, spherical, spheroidal, urchinlike, two-dimensional nanowires, and nanorods, are generated by manipulating key growth parameters, such as gold ion concentration, solution pH, and reaction time. The synthesized nanostructures are characterized by UV/Vis and Fourier-transform infrared spectroscopy, transmission electron microscopy, and energy dispersive X-ray analysis studies. Electron diffraction patterns reveal the crystalline nature of the nanoparticles and a probable mechanism is proposed for the formation of the different structural entities.

A Rare Endoscopic Finding: Pseudomelanosis Duodeni

Purpose: Pseudomelanosis Duodeni (PD) has been rarely reported in English literature. We present a patient who was found to have this condition incidentally while having upper gastrointestinal endoscopy and present picture with a literature review. A 68-year-old female patient presented to an outpatient gastroenterology clinic with right upper quadrant abdominal of one month duration. Her past medical history was significant for Chronic Kidney Insufficiency, hypertension and Diabetes Mellitus. The medications included hydralazine, furosemide, aspirin, metoprolol and amlodipine. She underwent endoscopy which revealed diffuse pigmentation in the duodenum with dark speckles on the villi (photo 1-4). Biopsy report diagnosed PD. PD was formerly described in the literature as Melanosis Duodeni. It was determined that the pathology was not related to melanocytes or distribution of melanin. The color pattern was instead found to be due to pigment laden lysosomes in macrophages of the lamina propria of duodenal villi. The lysosomes have been reported to contain aluminum, silicon, sulfur, calcium, magnesium, aluminum, iron sulfide and iron oxide in heterogeneous masses. In earlier case reports, authors regarded the pigment in duodenal melanosis as melanin for its positive reaction with Masson-Fontana stain. Later, with electromicroscopy and electron probe energy dispersive X-ray analysis studies, it was found that the pigment is essentially ferrous sulfide. Rex and Jersild proposed that iron in combination with variable amount of sulfur were engulfed by macrophages after iron was released into the mucosa. Shedding blood can add iron moiety while sulfur can be derived from food or certain medications like Hydrochlorothiazide. The clinical association between PD and systemic hypertension may point toward some hidden factors in favor of forming iron sulfide. These factors remain unknown and could be attributed to some extent to antihypertensive treatment. Clinical correlation with PD is unclear. According to literature, it is more common in females in their sixth and seventh decades of life. The youngest reported case involved an 18-month-old child. It is associated with chronic renal insufficiency, hypertension, erosive mucosal lesions, Diabetes Mellitus, upper GI bleeding, congestive heart failure and anemia. There is also a relationship with hydralazine, propranolol, and thiazide diuretics. PD is a benign condition with no associated symptoms. Endoscopic finding reversion has been achieved in some cases by removal of the offending factors such as a medication or treating the existing condition such as an erosive mucosal lesion. The diagnostic and prognostic significance of PD awaits further studies.

Long-Term Tissue Reactions of Three Biomaterials in Craniofacial Surgery

Successful craniofacial reconstruction needs both a well-known and a reliable reconstruction material. However, there is often a lack of long-term knowledge of the tissue reactions and healing process in the human body. In this study, frontal sinus obliterations with bovine bone natural hydroxyapatite derivative (BHA), synthetic bioactive glass S53P4 (BAG) and hydroxyapatite cement (HAC) were investigated with clinical, histologic, scanning electron microscopic (SEM) and energy dispersive x-ray analysis (EDXA) 27, 12 and 3 years postoperatively. The aim was to determine the long-term clinical biocompatibility of the used materials. Histologic studies revealed bone formation with BHA particles and lamellar bone with BAG granule remnants in close contact to the new bone formation. In HAC reconstruction there was scattered fibroconnective tissue growth without new bone formation in the surface of HAC implantation. Neither foreign body reaction nor any abnormal findings were seen. SEM studies revealed a CaP layer on the surface of BAG granule remnants. In EDXA studies, composition profiles showed Ca-, P- and Si- rich layers on the BAG granule surface. No differences were found in CaO and P2O5 levels between BHA granules and HAC implantation and the surrounding bone. All investigated biomaterials were well tolerated in long-term applications.

A Simple Route to the Synthesis of Crystalline InS Nanowires from Indium Foil

Large-scale well-crystalline InS nanowires have been successfully prepared for the first time from a metallic indium precursor by a simple solvothermal route without using any template or catalyst. From X-ray diffraction and energy-dispersive X-ray analysis studies, stability of InS is suggested to be within the temperature range of 180−265 °C. Both the diameter and the yield of nanowires show a proportional increment with temperature.

On the occurrence of Z-phase in a creep-tested 10% Cr steel

Abstract Electron microscopy studies on a creep-tested 10% Cr steel have revealed the presence of a complex nitride precipitate which has been previously assigned as modified Z-phase. This paper describes how the Z-phase can be efficiently detected by energy-filtering transmission electron microscopy. The results of electron diffraction, electron energy-loss spectroscopy and energy-dispersive X-ray analysis studies lead to a quantitative description of the modified Z-phase of the type Cr(V, Nb) N.

A novel way to make Fe 3Al/Al 2O 3 composite

Mechanical smearing and hot isostatic pressing routes have been adopted to make Fe 3Al-4 vol.% Al 2O 3 composite, using very fine size Al 2O 3 particles. In this way compacts with density close to the theoretical density have been produced. Vickers' microhardness values of 390 and 500 HV have been achieved for the Fe 3Al and Fe 3Al-Al 2O 3 materials respectively, indicating a strengthening of the matrix in the composite. Scanning electron microscopy and energy-dispersive X-ray analysis studies confirm the presence of Al 2O 3 as a smeared coating on the Fe 3Al in the composite, and from ultra-microindentation studies the coating thickness is ascertained to be between 0.6 and 1 μm.

Melanoses of the gastrointestinal tract

Electronmicroscopy and electron probe energy dispersive X-ray analysis studies have substantially contributed to our understanding of the various gastrointestinal tract melanoses. The nature of the pigment granules which occur in the various melanoses is discussed; their pattern of distribution in melanosis coli, melanosis ilei, melanosis duodeni and melanosis oesophagi is summarized and current knowledge of the aetiology and pathogenesis of these conditions is reviewed. Brief mention is also made of other examples of lipofuscin pigmentation, and a case of haemosiderosis ilei is described.