X-ray Diffractometer Method Research Articles

Temperature dependences of structure and physical properties of eutectic InSn49.1 melt

The temperature dependences of structure and some physical properties of eutectic InSn49.1 (wt%) melt were investigated by means of high temperature X-ray diffractometer, internal friction and DC four-probe method. In the heating procedure of the melt, a discontinuous temperature induced liquid–liquid structure change was observed within the temperature range of 620–850°C. The X-ray diffraction results show that both mean nearest neighbour distance and coordination number altered anomalously within 650–800°C; in addition, the size of the ordering domain and ordering degree of the melt all decreased evidently at the end of the structure change. It is presumed that this structure change resulted from the adjustment of the atomic bonds of Sn–Sn and In–In. A theoretical discussion on the correlation between structure and physical properties of InSn49.1 melt was also given.

The effect of heat treatment on the physical properties of sol–gel derived ZnO thin films

Zinc oxide (ZnO) thin films were deposited on microscope glass substrates by sol–gel spin coating method. Zinc acetate (ZnAc) dehydrate was used as the starting salt material source. A homogeneous and stable solution was prepared by dissolving ZnAc in the solution of monoethanolamine (MEA). ZnO thin films were obtained after preheating the spin coated thin films at 250 °C for 5 min after each coating. The films, after the deposition of the eighth layer, were annealed in air at temperatures of 300 °C, 400 °C and 500 °C for 1 h. The effect of thermal annealing in air on the physical properties of the sol–gel derived ZnO thin films are studied. The powder and its thin film were characterized by X-ray diffractometer (XRD) method. XRD analysis revealed that the annealed ZnO thin films consist of single phase ZnO with wurtzite structure (JCPDS 36-1451) and show the c-axis grain orientation. Increasing annealing temperature increased the c-axis orientation and the crystallite size of the film. The annealed films are highly transparent with average transmission exceeding 80% in the visible range (400–700 nm). The measured optical band gap values of the ZnO thin films were between 3.26 eV and 3.28 eV, which were in the range of band gap values of intrinsic ZnO (3.2–3.3 eV). SEM analysis of annealed thin films has shown a completely different surface morphology behavior.

Synthesis of nano B 2O 3/TiO 2 composite material as a new solid phase extractor and its application to preconcentration and separation of cadmium

A new solid phase extractor, nano-scale diboron trioxide/titanium dioxide composite material, was synthesized and used for separation and/or preconcentration of trace cadmium ion from various samples. The characterization of the synthesized material was performed by scanning electron microscope (SEM), transmission electron microscope (TEM) and X-ray diffractometer methods (XRD). The specific surface area of the material was also determined and found as 3.4 m 2/g. Analytical parameters including pH of sample solution, sample volume, flow rate of sample solution, volume and concentration of eluent for the column solid phase extraction (SPE) procedure were examined. The effect of common matrix ions on the recovery of the cadmium has also been investigated and found that they did not interfere on cadmium preconcentration. Under the optimum experimental conditions, preconcentration factor and analytical detection limit were determined as 50 and 1.44 μg/L, respectively. The reusability (stabile up to 100 run) and adsorption capacity (49 mg/g) of the sorbent were excellent. The accuracy of the method was confirmed by analyzing certified reference materials (Tea leaves GBW-07605). The results demonstrated good agreement with the certified values (relative error <10%). The precision of the method was also satisfactory. The recovery of cadmium under the optimum conditions was found to be 96 ± 3% at 95% confidence level. The method was applied for the determination of cadmium in tap water and tea leaves.

Study of alkaline nanocomposite polymer electrolytes based on PVA–ZrO 2–KOH

A novel alkaline nanocomposite polymer electrolyte composed of PVA polymer matrix with nanosized ZrO 2 ceramic fillers, KOH and H 2O, was prepared by a solution casting method. The characteristic properties of nanocomposite PVA polymer electrolytes with 2–20 wt.% ZrO 2 fillers were studied by using a DSC, TGA, X-ray diffractometer (XRD), SEM, and AC impedance method. The PVA polymer electrolyte directly blended with nanosized ZrO 2 fillers shows extraordinary ionic conductivity, transport and thermal properties. The highest ionic conductivity value of alkaline nanocomposite PVA polymer electrolyte with 20 wt.% of ZrO 2 fillers is around 0.267 S cm −1 at 20 °C and the anionic transport number ( t −) is in the range of 0.98–0.99. In this work, it was found that the addition of nano-ZrO 2 fillers into the PVA polymer matrix could significantly improve the electrochemical properties of alkaline PVA polymer electrolyte; it can be realized through a simple blend technique.

The effect of annealing treatment on microstructure and properties of indium tin oxides films

Indium tin oxide (ITO) thin films were prepared by radio frequency (r.f.) magnetron sputtering system with high-density ITO target (90 wt.% In 2O 3 and 10 wt.% SnO 2). The microstructure of the thin films at various processing parameters was measured using an X-ray diffractometer (XRD) method. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were used to observe the microstructure and surface morphology of the thin films. The composition of the thin films was measured by energy dispersive X-ray (EDX). The result shows that the as-deposited ITO film is amorphous-like and includes some round shaped particles in the matrix. The transformed temperature of amorphous to crystal is the range of 150–250 °C. The resistivity is increased sharply at 250 °C with the film fine grain and minimum optical band gap. We could get the minimum resistivity of 3.5 × 10 −4 Ω cm and over 80% of the average transmittance in a visible region at the optimum condition of our deposition technique.

Residual stress in PZT thin films prepared by pulsed laser deposition

In this investigation, ferroelectric thin films Pb(Zr x Ti 1− x )O 3(PZT) with x=0.58 were deposited on Pt/Ti/Si(001) by pulsed laser deposition (PLD). The residual stresses in PZT thin films were measured by an X-ray diffractometer (XRD) and indentation fracture method. In the indentation fracture method, the surface crack model and half-penny crack model were adopted. For PZT thin films with thickness of 0.05 μm, 0.5 μm and 1.0 μm, the residual stresses determined by a half-penny crack model were −74.73 MPa, −22.86 MPa and −14.74 MPa and those measured by XRD method were −57.6 MPa, −48.5 MPa and −25.6 MPa, respectively. The residual stresses determined by a half-penny crack model were closer to the results measured by XRD. A theoretical model is proposed to predict the residual stress in PZT thin film and the analytical results are essentially consistent with the experimental results. The effect of residual stress on piezoelectric properties is also discussed. The good ferroelectrics behaviors were demonstrated ( P r=22–35 μC cm −2, E c=25–315 kV cm −1) by the hysteresis loops.

Growth, Microstructural and Ferroelectric Properties of PZT Films Prepared by Pulsed Laser Deposition Method

AbstractPb(ZrxTi1−xO3 (lead zirconate titanate or PZT) ferroelectric thin film capacitors are of considerable interest for the realization of memory devices such as nonvolatile random access memories (NVRAMs). The PZT capacitors were prepared on platinized silicon Pt/(100)Si using conducting oxide LaxSrl.xCOO (lanthanum strontium cobalt oxide or LSCO) as electrodes. The PZT and LSCO thin films were deposited by the KrF excimer laser ablation technique. The optimum preparation conditions such as oxygen pressure, laser energy influence and substrate temperature were investigated. The PZT and LSCO films grown on Pt/(100)Si are polycrystalline. The crystallographic properties of the films were determined using X-ray diffractometer (XRD) method. The cross-sectional transmission electron microscope showed very smooth interface among different layers of films. The electrical characterizations of the films including hysteresis loop, fatigue, and retention properties were determined by the RT66A Standardized Ferroelectric Test System.

Synthesis and Characterization of Ferroelectric Thin Films by KrF Excimer Laser Ablation for Memory Applications

AbstractPb(ZrxTi1-x)O3 (lead zirconate titanate or PZT) ferroelectric thin film capacitors are of considerable interest for the realization of memory devices such as nonvolatile random access memories (NVRAMs). The PZT capacitors were prepared on platinized silicon Pt/(100)Si using conducting oxide LaxSr1-xCoO3 (lanthanum strontium cobalt oxide or LSCO) as electrodes. The PZT and LSCO thin films were deposited by the KrF excimer laser ablation technique. The optimum preparation conditions such as oxygen pressure, laser energy influence and substrate temperature were investigated. The PZT and LSCO films grown on Pt/(100)Si are polycrystalline. The crystallographic properties of the films were determined using X-ray diffractometer (XRD) method. The electrical characterizations of the films including hysteresis loop, fatigue, and retention properties were determined by the RT66A Standardized Ferroelectric Test System.

Synthesis of the PZT films deposited on pt-coated (100) Si substrates for nonvolatile memory applications

Ferroelectric lead-zirconate-titanate (PZT) thin films were deposited by the pulsed laser deposition technique on Pt-coated (100) Si substrates. This study was focused on the investigation of the PZT film growth on (100) Si substrate at varying deposition parameters and electrical characterization of the films including hysteresis loop and fatigue properties by RT66A Standardized Ferroelectric Test System. PZT deposited at higher temperature (575°C in 450 mTorr O2 partial pressure) showed the best crystalline structure. The remnant polarization and the retained polarization of the ferroelectric capacitors were 13 µC/cm2 and 20 µC/cm2, respectively. The crystallographic properties of the films were determined using the x-ray diffractometer method. The cross-sectional transmission electron microscope results showed very smooth interfaces among different layers of films.

Structural and hardness studies of CN X /TiN composite coatings on Si (100) substrates by laser ablation method

CN x /TiN composite coatings were deposited on Si (100) substrates using the pulsed laser deposition (PLD) method. Previous results showed that a seed of titanium nitride (TiN) layer between silicon substrates and a top layer of carbon nitride increased the hardness and modulus values of overall composite coatings (Ref 1). This paper describes the same approach to growing carbon nitride composite coatings with varying thicknesses of different kinds of buffer layers and carbon nitride films on Si (100) substrates at different temperatures and pressures. Preliminary results showed the presence of carbon nitride films by the Fourier transform infrared spectroscopy (FTIR) method. The mechanical properties of the films were characterized using the nanoindentation technique. The crystallographic properties of the films were characterized using the x-ray diffractometer method.

Éléments de parure du Néolithique syrien ; identification et provenances des matériaux

85 neolithic stone ornaments from Mureybet (Middle Euphrates, Syria) have been studied by X-Ray diffractometer method. The mineralogical compositions were determined ; die question of the geographic origin of the materials utilised is discussed by reference with the geological environment From the quantitative point of view, three main mineralogical groups were thus identified : (1) Mg-rich chlorites of opbiolitic origin which most probably come from Turkey ; (2) Phosphates and associated minerals come from the syrian or turkish economic deposits ; (3) Carbonates, associated with gypsum and halite are typical of the surrounding epicontinental series on the Arabian microplate. Some other mineral groups are less abundant such as : (4) talc, which is also of ophiolitic origin ; (5) kaolinite which was of local origin as well as the carbonates ; and a few other ones. Among the choice criteria, besides the availability of the various materials, there could be the colours and the hardness (most of the minerals utilised are no more than degree 4 compared with the Mohs scale). It also appears that, depending upon the different kinds of ornaments and the successive chronological periods, the selected minerals were not the same. Generally speaking, the carbonates were first preferred. Then the phosphates were used during the khiamian times. Finally, the chlorites were mostly selected during the mureybetian final periods.

Crystal structure of Nd3Au4 and Nd17Au36

Abstract The crystal structures of two phases in the neodymium-gold system were determined by single crystal X-ray diffractometer methods, λ(MoKα = 0.7107 Å. Nd3Au4 (hR42) is trigonal, R[unk] (n. 148), a = 13.739(3) Å, c = 6.088(2) Å, Z = 6, R = 0.083 with 405 reflections, isotypic with Pu3Pd4. Nd17Au36 (tP106) is tetragonal, P4/nmm(n.129), a = 15.835(4) Å, c = 9.278(2) Å, Z = 2, R = 0.082 with 540 reflections. The structure of Nd17Au36, which represents a new type, can be described as packing of bicapped square antiprisms with vertices occupied by five Nd and five Au atoms and centered by part of the gold atoms. This kind of polyhedron is identical to that of aluminium in the pyramidal site of the BaAl4 structure. In the Nd–Au system the phase Nd17Au36 replaces the phase given as “NdAu2”.

Effect of Heat Treatment and Cold Working on Aging in Logarithmic Decrement of Al&amp;ndash;Zn Alloys

Aging at room-temperature in the logarithmic decrement 6 and crystal structure were investigated for heat-treated and cold-drawn Al-Zn alloys. The value of 6 was measured by an inverted pendulum method and the crystal structure was confirmed by using an X-ray diffractometer method. The value 6 of the Al-Zn alloys containing Zn less than 70 mass% is very low just after water quenching from a temperature of 673 K in the region of the α phase, but becomes higher over time,decreasing gradually after reaching a maximum. The nearer the eutectoid composition, the shorter the decomposition time at which the maximum of 6 appears

An Experimental Examination of Error Functions for Bragg-Brentano Powder Diffractometry

AbstractA single function for the elimination of errors in precision lattice parameter determination has not been developed for the Bragg-Brentano x-ray diffractometer method, because of the different angular dependencies of the systematic errors. A review of the error functions shows that all but one can be calculated from the instrumental settings and known properties of a sample under investigation. The residual sample displacement error can be then be eliminated by using extrapolation plots or computer methods to correct the data to cosθcotθ plots. The slopes of cosθcotθ plots can also be used to align high temperature furnaces and low temperature cryostats mounted on x-ray diffractometers.

Formative process and microscopic structure of Mn-ferrite thin films.

Mn-ferrite films were obtained in atmosphere by the heat treatment of film samples which is prepared by evaporation from Fe-Mn-Bi source. There was tries to clarify its relation to microscopic structure and magnetic properties in terms of the formative process of Mn-ferrite thin films. The qualitative and quantitative analysis of Mn-ferrite was made measurements by X-ray diffractometer method and the chemical effect in the low energy Auger spectrum, respectively. The prepared films showed perpendicular magnetic anisotropy. The saturation magnetization (4πMs), remanent magnetization (4πMr⊥), coercive force (Hc⊥) and anisotropy field (Hk) were 4.4 (kG), 0.6 (kG), 350 (Oe), and 1.5 (kOe), respectively. The cause for the perpendicular anisotropy is attributed to the effects of the perpendicular configuration of column grains in the films and of induced magnetic annealing effect.

An assessment of instrumental parameters which control the accuracy of stress measurement using the X-ray diffractometer method

The sources of systematic error in the X-ray diffractometer method of stress measurement are discussed. The errors in stress measurement and correction procedures for their elimination are described and quantitatively assessed.

Kristallstruktur von α-Bromo(2-dibutylaminoäthanolato)kupfer(II) / The Crystal Structure of a-Bromo(2-dibutylaminoethanolato)copper(II)

The crystal structure of α-Bromo(2-dibutylaminoethanolato)copper(II) has been determined by single-crystal X-ray diffractometer methods using 1488 independent reflexions and MoKα radiation. The compound crystallized in the orthorhombic space group P212121 with four dimers in a unit cell of dimensions a = 21.235(13), b = 15.220(8) and c = 8.390(5) Å. The structure was refined by least-squares methods giving a final residue of R = 0.087. The dimer molecules with Cu-Cu-separations of 3.019(4) Å consist of nonplanar Cu2O2-rings with Cu-O-distances of 1.92(2) Å (mean value). The coordination around each copper atom is distorted square planar. The averaged Cu-N-distance is 2.06(2) Å and Cu-Br-separations are 2.333(4) A. In good agreement with the calculated density of 1.55 g cm-3 is the experimental value of 1.53(3) g cm-3.

ChemInform Abstract: THE CRYSTAL STRUCTURE OF PHENOXATELLURINE DINITRATE, C12H8O7N2TE (I)

The crystal structure of phenoxatellurine dinitrate, C12H8O7N2Te, has been determined by x-ray diffractometer methods. The crystals are monoclinic, C2/c, a = 12.916(3), b = 14.050(5), c = 7.532(2) A; β = 96.65(3)° at t = 22°. The molecule is nearly planar (175°), with the Te and O atoms of the central ring in special positions on the twofold symmetry axis. The bond distances for the central ring are: Te-C = 2.068(4) A, C-O = 1.366(5), C-C = 1.388(6) with C-Te-C = 93.5(2)° and C-O-C = 128.2(5). The bond distances and angles in the phenyl rings do not differ significantly from the normally accepted values of 1.40 A and 120°. The two nitrate groups are close to Te and are related by the twofold axis of symmetry. The independent distances and angles are: Te-O1 = 2.201(3), O1-N = 1.325(5), N-02 = 1.229(6), N-O3 = 1.204(6) A, O2-N-O3 = 126.3(4), O1-N-02 = 117.1(4), O1-N-03 = 116.6(4)°. All hydrogen atoms were located at or near their calculated positions. The final R value for 1679 independent reflections was 0.031. The planarity of the molecule is discussed qualitatively in terms of simple molecular orbital theory.

The crystal structure of n-propylarsonic acid

The crystal structure of n-propylarsonic acid has been determined by single crystal X-ray diffractometer methods. The crystal is orthorhombic, Pccn, a = 14.561(4), b = 11.024(4), c = 7.692(3) at 22°, 8 molecules/unit cell. The coordination around As is roughly tetrahedral, with As-O(1) = 1.708(5), As-O(2) = 1.719(5), As-O(3) = 1.652(4) and As-C(1) = 1.917(7) «, and the molecules are linked into chains of dimers along the caxis by hydrogen bonds O(1)⋯O(2) = 2.581(6) and O(3)⋯O(2) = 2.573(6) «. The other bond distances are C(1)-C(2) = 1.51 (2) and C(2)-C(3) = 1.28(2) «, where the pronounced apparent shortening of the latter bond seems to be associated with very large thermal motions of C(2) and C(3). These large thermal movements probably occur since the chains along the c axis are held together by van der Waal's forces. The hydrogen atoms could not be located with certainty, and the final R for As, O and C atoms only was 0.036.

X-ray Measurements of Surface Residual Stresses in Cold Rolled α-Brass

AbstractResidual elastic stresses have been measured in cold rolled α-brass (30% zinc) using the available x-ray diffractometer methods. Residual stress values obtained by the two exposure and sin2ψ methods of stress analysis are compared with data obtained using Wagner's extrapolation method.For deformations up to 50% reduction in thickness, tensile surface stresses prevailed, and in most cases could be detected by these methods. Uncertainty of the value of a0, the lattice parameter of the deformed' material, presents a serious limitation to the extrapolation technique. Using the approximation a0 = a0ann, residual stresses appear lower than, and frequently of opposite sign to those given by the two exposure method. In addition, lattice parameter variations in the near surface regions of the rolled sheet were opposite to those expected from the true macrostress distributions shown to exist by the two exposure method and by strain gauge techniques. The distributions of ahkl points in the extrapolation plots were in agreement with theory for a combination of anisotropic elastic stresses and low stacking fault density.