X-ray Diffractrometer Research Articles

Wear resistance and hardness properties of TiB2– Fe coating developed on AISI 1020 steel by tungsten inert gas (TIG) cladding

The present work is attempted to improve the microhardness and wear properties of AISI 1020 steel by depositing TiB2–Fe composite coating using tungsten inert gas (TIG) cladding. In this study, different compositions of TiB2–Fe paste form were preplaced on the substrate plates and then TIG heat input was applied to deposit hard composite coating layer. The main objective of the present work was to explore the influence of TIG input current as well as iron content on the microstructure and surface properties of deposited coatings. Microhardness, microstructural and phase characterization of the coating have been done by the Vickers microhardness tester, scanning electron microscope (SEM), Energy dispersive spectroscopy (EDS) and X-ray diffractrometer (XRD). The results showed that the microhardness of the TiB2–Fe coating was strongly influenced by the composition of the coating materials as well as the TIG processing current. The microhardness increases with decreasing Fe contents in the coating materials with constant processing current (90 A) as well as it also increases with decreasing processing current with the fixed composition of coating materials (80TiB2–20Fe). The maximum average microhardness found was 3082 HV0.1 for the coating of 100TiB2–0Fe composition ratio and 90 A processing current which was about 18 times higher than that of the substrate average microhardness value (163 HV0.1). Average wear rate evaluated by considering weight loss of the TIG cladded samples using pin on disc tribometer by the sliding distance of 864 m and 20 N normal loads. The wear results also showed that the coating contains 100 wt% of TiB2 (0 wt% of Fe) exhibited lower rate of wear 6.74 × 10−8 g/Nm which is about 24 times lower as compared to AISI 1020 mild steel wear rate (166.31 × 10−8 g/Nm).

Development of clay ferrite nanocomposite: Electrochemical, sensors and photocatalytic studies

Nano ferrite bentonite clay composite (NFBC) is synthesized in this present work by using manganese (Mn) recovered from waste batteries, ferric nitrate and citric acid prepared by simple and cost-effective Indian sodium bentonite nanoclay (Na-IB) by sol-gel process and by using X-ray diffractrometer (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) Spectroscopy, Energy dispersive Spectroscope (EDS) characterized nanoparticles. The result shows that NFBC is sufficient for the excellent performance of AO dye photocatalytic degradation (98 %). Electrochemical study of prepared material with graphite electrode paste in 0.1 M KCl electrolyte showed excellent redox potential output as calculated by cyclic voltammetry and expanded its sensor activities to biochemical (Dextrose). We examined the efficacy of NFBC in the detection of Dextrose from an aqueous solution and compared the results with pristine MnFe2O4 NPs.

Economic appraisal of iron ore deposit in Buttala, Sri Lanka: Preliminary mineral and chemical evidences

Iron ore deposits have greater industrial significance since they supply raw material for steel based industries and such applications are majorly based on their mineral and chemical characteristics. Therefore, initial clear understandings on mineralogy and geochemistry of these ores would be advantageous. Present study aimed to investigate the mineral and chemical composition of the iron ore deposit exposed in Buttala, Monaragala District, Sri Lanka and to assess its economic potential. Sampling was carried out systematically along the ridge of ore containing mountain and from the host rocks. Textural and weathering characteristics of the ore samples were determined in hand specimen scale. Detail mineralogy was analyzed on X-Ray Diffractrometer (XRD) analyzer while elemental characterization was performed on X-Ray Florescence (XRF) spectrometer. Spatial distributions of iron and gangue elements of the ore were mapped using the Quantum GIS software. The deposit is mostly exposed as fresh ore bodies along the ridge of mountain and is hosted in garnet biotite gneiss. As indicated by the XRD results, common minerals of the ore deposit are magnetite and hematite with minor amounts of spinel, ilmenite and goethite. Average Fe2O3 content of the ore deposit is 78.84 wt. % with 55.14 wt. % of calculated Fe content. The spatial distribution of iron is higher at the northern and southern parts of the ridge than its middle part. The resulted Fe content of the ore is greater than many of the other iron ore deposits in Sri Lanka and comparable to the high grade iron ore deposits found elsewhere in the world. Concentrations of common gangue constituents of Al2O3, SiO2, TiO2 and MgO are 7.54 wt. %, 4.40 wt. %, 3.6 wt. % and 2.54 wt. % respectively. Contents of S and P, which are considered as common deleterious elements are negligible. Therefore, the Buttala iron ore deposit is magnetite and hematite containing, high grade iron ore deposit with greater economic potential.

Photoluminescence of ZnO nanorods prepared by hydrothermal method

In this research, the effects of calcination temperature and reaction time on the photoluminescent properties of ZnO nanorods prepared by hydrothermal processes were studied. Morphology, crystalline structure and photoluminescent properties of the prepared samples were analyzed by scanning electron microscope (SEM), X-ray diffractrometer (XRD) and fluorescent spectrophotometer. The study found that a reaction time of 5 hours on a glass slide and calcination at 500°C was the best preparation condition. The prepared ZnO nanorods were aligned without direction and distributed throughout the substrate. The average diameter of the prepared ZnO nanorods was 91.96 ± 21.16 nm. The prepared ZnO nanorods comprised a hexagonal crystalline structure with an emission peak in the UV range.

Preparation and Physical Characterization of Andrographolide-Chitosan-Alginate Microparticles prepared by Ionic Gelation-Freeze Drying

This study aimed to determine the effect of alginate concentration on physical characterization (morphology, physical state, and encapsulation efficiency) of andrographolide-chitosan-alginate microparticles prepared by ionic gelation- freeze drying method. Andrographolide-chitosan-alginate microparticles were produced with various amount of alginate by ionic gelation method using tripholyphospate (TPP) as crosslinker and maltodextrin as a lyoprotectant. The physical characteristics were evaluated using Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectrophotometer (FT-IR), Differential Thermal Analyzer (DTA), Powder X-ray diffractrometer (PXRD), drug content was evaluated using High Pressure Liquid Chromatography (HPLC). The results showed that andrographolide crystallinity changed after encapsulated inside the microparticles supported by changes in IR spectra, and melting point. Furthermore, increased alginate concentration showed rougher surface morphology. The amount of alginate affected the characteristics of the andrographolide-chitosan-alginate microparticles by altering the crystallinity and lowering melting point. The highest encapsulation efficiency shown by microparticles with 0.5% alginate.

Aliovalent Ho3+ ion doped BaZrO3 thin films; Structural, optical and photoluminescence properties

Ho doped BaZrO3 thin film phosphors with varying Ho content (1, 2, 3 and 4 at%) were prepared via pulsed laser deposition technique. To understand the effect of doping on structural, morphological, optical and emission properties of thin films, X-ray Diffractrometer (XRD), Scanning Electron Microscopy (SEM), Spectroscopic Ellipsometry (SE) and Photoluminescence (PL) Spectroscopy have been used, respectively. Polycrystalline nature with single phase cubic crystalline structure of the films has been obtained. The optical band gap energy, as estimated by SE, has been found to increase with increase in the Ho content. The PL spectra of the synthesized phosphor exhibit green and yellow-orange as prominent emission bands in response to 328 nm as excitation wavelength.

The influence of Zn+2 doping and annealing temperature on grown-up of nanostructures TiO2 thin films prepared by sol-gel dip-coating method and their photocatalytic application

Nanostructures of Zn+2-doped TiO2 thin films were prepared by sol gel dip-coating method deposited on silicon substrate, the films were heated at temperature from 600 °C to 1000 °C for 2 h. The doped thin films were characterized using X-ray diffractrometer (XRD), Raman spectroscopy, FTIR spectroscopy, Scanning electron microscopy (SEM), Atomic force spectroscopy (AFM), Reflectance and Photoluminescence spectroscopy (PL). It was determined that the films crystallize on anatase and ZnTiO3 phase at annealing temperature 600 °C. At high temperature 800 °C, 1000 °C we observed completely transformation of anatase to rutile and ZnTiO3 phase, in addition the Zn2TiO4 phase was taking place. SEM and AFM confirmed the changing morphology with increasing annealing temperature as a progression of nanoprous to nanorods and nanofils structures. Photoluminescence and reflectance results revealed that Zn+2-doped TiO2 thin films have excellent optical properties, which enhance the photocatalytic activity. Following on this, a test photo conversion cell was constructed and cyclic voltammetry was used to study photocurrent response in the dark and under illumination, confirming high conversion efficiency which proved the behavior of the solar cell.

Comparative study of multilayered ZnO/TiO2/ZnO and TiO2/ZnO/TiO2 thin films prepared by sol–gel dip coating method

The aim of this research work is to represent the comparative study of ZnO/TiO2/ZnO (ZTZ) and TiO2/ZnO/TiO2 (TZT) thin films deposited by sol–gel dip coating on FTO substrates. After deposition, the films were annealed at 500 °C for 1 h. Structural, surface morphology, optical and electrical properties of these films were studied by X-ray diffractrometer (XRD), Raman spectra, atomic force microscope (AFM), photoluminescence spectra (PL) and four point probe technique respectively. XRD and Raman spectra confirmed the anatase, brookite phases of TiO2 and cubic phase of ZnO. AFM confirmed the formation of nano particles with average sizes of 18.4 and 47.2 nm of TZT and ZTZ films respectively. According to PL spectra, both the multilayer films slowdown the electron hole recombination rate and enhances the optoelectronic properties of the materials. Also it showed the peaks in the visible region of spectrum. The four point probe results showed that the average sheet resistivity of the films is 450 and 120 (ohm-m) respectively.

Mechanical properties of vacuum plasma sprayed reinforced hydroxyapatite coatings on Ti-6Al-4V alloy

The aim of this present work was to deposit reinforced hydroxyapatite coatings with a bond coat of zirconia on Ti-6Al-4V substrate using the vacuum plasma spray technique in order to improve the surface properties. To achieve that, HA + 10 wt% Al2O3 and HA + 10 wt% ZrO2 coatings with an intermediate layer of zirconia were deposited on Ti-6Al-4V implant substrate. Further, these coatings were subjected to post-coating heat treatment at 700 °C for 1 h. The morphology and phase analysis of bio-ceramic powders, as-sprayed and heat-treated coatings, have been characterized using a scanning electron microscope and an X-ray diffractrometer. Crystallinity, surface roughness, porosity, hardness and shear strength were also investigated. The wear behaviour of the coatings was evaluated using a Taber abrasion tester as per ASTM F1978 standard. The results indicate that heat-treated coatings exhibit lower wear resistance than as-sprayed coatings and show lower porosity and higher crystallinity and hardness after heat treatment. Slight improvement in shear strength was observed after heat treatment.

Sol–gel deposition and characterization of multilayer 2% Cu doped TiO2 nano structured thin films

Multilayer of 2% Cu doped TiO2 thin films have been grown by sol–gel spin coating on glass substrate in the form of three, five and seven layers. X-ray diffractrometer (XRD) confirms the doping of Cu into TiO2. Scanning electron microscopy (SEM) confirms the formation of nano particles with average size of 19, 25 and 35 nm for three, five and seven layers of thin films, respectively. The electrical resistivity of these multilayer films is found as 2.19 × 107, 1.20 × 107 and 1.11 × 107 ohm-m respectively. UV–vis shows that the films have 80% transmittance in the visible region which is good for solar spectrum. The optical band gap energy decreases with an increase in the number of layers as 3.778, 3.768 and 3.736 eV respectively for 3, 5 and 7 layered thin films. This work provides an environment friendly and low cost use of an abundant material for optoelectronic devices.

Structural, morphological and mechanical properties of laser-irradiated copper using continuous wave diode laser

ABSTRACTLaser irradiation effects on morphological, structural and mechanical properties of copper are explored. The targets are exposed by employing low-cost continuous wave (CW) laser (wavelength of 532 nm) in air. The surface morphology, structural and mechanical modification of irradiated targets was investigated by scanning electron microscopy (SEM) (Fei, Quanta 250), an X-ray diffractrometer (XRD) (DMAX III ARigaku, Japan) and a Vickers hardness tester, respectively. The SEM analysis revealed the exfoliation sputtering, electronic sputtering, thermal stresses and cracks. The grain size, dislocation line density, relative intensity and d-spacing of irradiated metals were studied by XRD. Micro hardness is found to increase with the increase in time of laser irradiation, in accordance with the Vickers hardness tester. This work provides a cost-effective, user-friendly and easy-to-handle study of several properties of irradiated targets with good results.

A facile hydrothermal recovery of nano sealed MnO2 particle from waste batteries: An advanced material for electrochemical and environmental applications

This work deliberates a method for manganese (Mn) recovery as manganese oxide obtained by leaching of waste batteries with 3M sulphuric acid. The Experimental test for the recovery of Mn present within the waste dry cell batteries were carried out by a reductive leachant. Elemental composition of leached sample was confirmed by Energy Dispersive X-ray analysis (EDAX), and Surface morphology of the recovered MnO2 was examined by using Scanning Electron microscopy (SEM). Phase composition was confirmed from X-ray Diffractro meter (XRD). The obtained leached solution was treated with 4M NaOH, yielded to Manganese Dioxide with high extraction degree, while it do not touches the Zn content within the solutions. The recovered samples were characterized using XRD, EDAX, SEM and Fourier transform infrared spectrometry (FTIR). The electrochemical properties of the as-recovered sample from leached solution was examined used cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Remarkably, the 80 wt.% MnO2 displays reversibility, diffusion constant, smaller equivalent series resistance and charge transfer resistance in 0.5M NaOH showed superior results as compared to alternative electrolytes. The ideal capacitive behaviour of MnO2 electrode and nano particle was applied to photocatalytic degradation of dyes.

Deposition and Dissolution of Lithium through a Lithium Carbonate Thin Film in an Ionic Liquid Electrolyte

Li-ion batteries are used widely for portable energy storages because of large capacity. Generally, the carbonate-based organic solvents are used as the electrolytes. Most of these organic solvents decompose during the first charge, resulting in formation of the solid electrolyte interphase (SEI) film, which plays an important role for Li-ion batteries on the active materials. Although there are many reports about the SEI film, its nature and function have not been clarified yet. We have already reported that lithium phosphorous oxynitride (LiPON) film acts as an artificial SEI film in 1-butyl-1-methylpyrrolidinium (BMP+) and 1-ethyl-3-methylimidazolium (EMI+) bis(trifluoromethylsulfonyl)amide (TFSA–) ionic liquids containing LiTFSA, and LiTFSA-glyme solvate ionic liquid. [1,2] Ionic liquids are expected to be the alternative electrolytes for Li-ion batteries, since ionic liquids have low flammability and low volatility, which are expected to improve safety of the batteries. However, the SEI film formed by the decomposition of ionic liquids is not preferable for deposition and dissolution of lithium. In this study, deposition and dissolution of lithium through a Li2CO3 thin film prepared by RF magnetron sputtering were investigated in BMPTFSA containing LiTFSA. The Li2CO3 thin film was characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffractrometer, and X-ray photoelectron spectrometer (XPS). All the electrochemical measurements were performed using an airtight three-electrode cell. The Ni electrode with or without the Li2CO3 thin film was used as a working electrode. Li foil was used as a reference and counter electrode. After electrochemical measurements, the electrode was washed with dimethyl carbonate (DMC) and characterized by SEM and XPS. SEM observation and XPS measurement showed that the Ni substrate was covered with the Li2CO3 thin film completely. The Li2CO3 thin film on the substrate was X-ray amorphous. However, the crystalline domains were observed sparsely by TEM observation. The deposition and dissolution of lithium were possible through the Li2CO3 thin film in BMPTFSA containing 1 M LiTFSA. Although the cathodic current attributed to the decomposition of the electrolytes was observed on the Ni electrode, it was suppressed on the Ni electrode with the Li2CO3 thin film. These results indicate that the Li2CO3 thin film has the possibility to act as an artificial SEI film. The depth analysis by XPS revealed that lithium deposited between the Li2CO3 thin film and Ni electrode. From AC impedance measurement, the ionic conductivity of the Li2CO3 thin film was estimated to be 1.3 × 10−8 S cm−1.

Effect of Cu incorporation on the physical properties of CdS thin films deposited by using the thermal evaporation technique

CdS thin films with different Cu concentrations were grown on glass substrates at room temperature by using the resistive thermal evaporation technique. The effect of Cu doping on the structural, optical and vibrational properties of CdS thin films was investigated. The structural, optical and vibrational analysis was completed using an X-ray diffractrometer and a Raman and a UV-VIS-NIR spectrophotometer. X-ray diffraction data revealed that incorporation of Cu ions improved the crystalline structure but did not change the cubic phase of the CdS thin film with a preferential orientation along the (111) direction. Various optical parameters, like the refractive index, extinction co-efficient, absorption co-efficient, urbach tail energy Ee and optical band gap, were determined by using transmission data at different copper concentrations. The Raman peaks appearing at 299 cm−1 and 592 cm−1 for CdS were attributed to the 1LO and 2LO phonons of cubic CdS, and a shift towards low wavenumber region was observed with increasing Cu concentration.

Variation in electrical properties of gamma irradiated cadmium selenate nanowires

Preparation of low-dimensional materials attracts more and more interest in the last few years, mainly due to the wide field of potential commercial applications ranging from life sciences, medicine and biotechnology to communication and electronics. One-dimensional systems are the smallest dimension structures that can be used for efficient transport of electrons and thus expected to be critical to the function and integration of nanoscale devices. Nanowires with well controlled morphology and extremely high aspect ratio can be obtained by replicating a nanoporous polymer ion-track membrane with cylindrical pores of controlled dimensions. With this technique, materials can be deposited within the pores of the membrane by electrochemical reduction of the desired ion. In the present study, cadmium selenate nanowires were synthesized potentiostatically via template method. These synthesized nanowires were then exposed to gamma rays by using a 60Co source at the Inter University Accelerator Centre, New Delhi, India. Structural, morphological, electrical and elemental characterizations were made in order to analyze the effect of gamma irradiation on the synthesized nanowires. I–V measurements of cadmium selenate nanowires, before and after irradiation were made with the help of Keithley 2400 source meter and Ecopia probe station. A significant change in the electrical conductivity of cadmium selenate nanowires was found after gamma irradiation. The crystallography of the synthesized nanowires was also studied using a Rigaku X-ray diffractrometer equipped with Cu-Kα radiation. XRD patterns of irradiated samples showed no variation in the peak positions or phase change.

Structural and Optical Properties of Undoped and Er<sup>3+</sup>-Doped ZnO Nanoparticles Synthesized by Laser Ablation in Ethanol

In this paper ,we report on the fabrication and properties of undoped and 8.4% Er3+-doped ZnO nanoparticles synthesized by laser ablation in ethanol at laser fluence values2.92 J/cm2. The synthesized nanoparticles are characterized by structural properties using X-ray diffractrometer , scanning electron microscope and the optical properties are carried out through UV–Visible spectrophotometer. The X-ray diffractrometer pattern indicates that these nanoparticle were polycrystalline in nature with a hexagonal (wurtzite) phase. SEM reveals that The synthesized ZnO and Er-ZnO NPs have a spherical shape. Moreover, the optical band gaps calculated through UV spectroscopy are found to be decreased with doping from 3.3 to 3.2 eV.

Structural and Optical Properties of Undoped and Er<sup>3+</sup>-Doped ZnO Nanoparticles Synthesized by Laser Ablation in Ethanol

In this paper ,we report on the fabrication and properties of undoped and 8.4% Er3+-doped ZnO nanoparticles synthesized by laser ablation in ethanol at laser fluence values2.92 J/cm2. The synthesized nanoparticles are characterized by structural properties using X-ray diffractrometer , scanning electron microscope and the optical properties are carried out through UV–Visible spectrophotometer. The X-ray diffractrometer pattern indicates that these nanoparticle were polycrystalline in nature with a hexagonal (wurtzite) phase. SEM reveals that The synthesized ZnO and Er-ZnO NPs have a spherical shape. Moreover, the optical band gaps calculated through UV spectroscopy are found to be decreased with doping from 3.3 to 3.2 eV.

Effects of Catalyst on Carbon Nanotubes Synthesized by Thermal Chemical Vapor Deposition Method

The effects of cobalt, nickel and iron catalyst on carbon nanotubes (CNTs) were examined with scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffractrometer (XRD) and Fourier transform Raman spectrometer (FT-Raman). The samples were prepared by the thermal chemical vapor deposition (CVD) method at 780 °C under pressure of acetylene gas (C2H2) at 0.5 bar. The average diameter of CNTs grown on Co, Fe and Ni catalyst obtained from SEM image is 100, 90, 70 nm, respectively. The crystallinity and the yield of CNTs synthesized from Ni catalyst were higher than that from Fe or Co catalyst. The Raman peak of radial breathing mode (RBM) region and the TEM images highlighted the hollow tubes of the CNTs. The results indicated that the diameter, the yield and the crystallinity for synthesis of carbon nanotubes were manipulated by the selection of the catalyst.

Study Of Chemically Synthesized SHI Irradiated CdS Nanostructured Films

Cadmium sulphide (CdS) nanostructured films were prepared by chemical bath deposition (CBD) method at room temperature. The prepared films were subjected to swift heavy ion (SHI) irradiation by using 100 MeV Si 8+ ion beams at various fluences from 1x10 11 to 1x10 13 ions/cm 2 . Structural, morphological, optical properties of the pristine and irradiated films were characterized by X-ray diffractrometer (XRD), high resolution transmission electron microscope (HRTEM), UV-Vis spectroscopy and Raman spectroscopy. XRD study confirms the formation of nanocrystalline cubic phase in all the films. The crystallite size is found to increase from 7nm to 9 nm and shift of peak positions are observed due to irradiation. The lattice strain and dislocation density of the samples are of the order of 10 -3 and 10 16 m -2 respectively and the values are found to decrease upon irradiation. HRTEM images show that the shapes of the particles are nearly spherical and the selected area electron diffraction (SAED) pattern of HRTEM have also supported the formation of cubic phase CdS. The optical absorption spectra exhibit shift in the fundamental absorption edge and the optical band gap decreases from 2.585eV to 2.513 upon SHI irradiation. Three intense Raman lines for pristine as well as irradiated CdS have been observed and all the samples show shift in Raman lines relative to bulk CdS due to phonon localization. The SHI irradiation on chemically deposited CdS films is an important tool used for modification of structural, morphological and optical properties of the films for possible applications in device fabrication. Copyright © 2015 VBRI press.

Preparation of rod shaped nickel oxide thin films by a novel and cost effective nebulizer technique

Nickel oxide thin films have been deposited from 0.3M aqueous solution of nickel chloride onto microscopic glass substrates, which were chemically and ultrasonically cleaned before coating. The film depositions are carried out with 1ml, 2ml, 5ml and 10ml. The substrate temperature, spray rate, distance between substrate and nozzle and air flow rate were fixed at 400°C, 0.5ml per min, ~7cm and 1.2kg/cm2 respectively after optimization of these deposition parameters. The effect of the volume of sprayed solution on structural, optical properties and surface morphology of the films was investigated using X-ray diffractrometer, UV–vis–NIR spectrometer, photoluminescence spectrometer, Raman spectrometer, scanning electron microscope and liner four probe resistivity set-up respectively. The diffraction peak along (111) plane at 2θ=37.2° for all the films was observed. Besides this other low intensity peaks were observed along (200) and (220) Miller planes. The peaks indicated that this corresponds to cubic structure of NiO thin films. Optical transmittance and absorption spectra are recorded using a UV–vis–NIR spectrometer. When the quantity of sprayed volume increased, the transmittance decreased, consequently the band-gap energy wanes from 3.64 to 3.21eV. From PL spectra, the samples show sharp and strong UV emission around 376nm corresponding to the near band-edge emission of NiO under excitation of 275nm. The surface morphology of the films was carried out using SEM to find the smooth, uniform and pin hole free surface. The composition of the films was estimated using EDAX spectrum of the films. The resistivity results show that the activation energy decreases with increase in the sprayed volume solution.