X-ray Diffractometry Methods Research Articles

Electron doping of NbSe2

The influence of fast-electron irradiation on the properties of the hexagonal modification of niobium diselenide, 2H–NbSe2, is investigated by the methods of x-ray and electron diffractometry. The observed changes in the diffractograms are explained by a redistribution of the electron density under irradiation, viz., an increase of the electron density in the planes with high packing density—the basal and prismatic planes {110}, {210}. The appearance of diffuse scattering of x rays and electrons at high doses of irradiation is attributed to growth of the electron density of the Fermi liquid.

Microstructure and mechanical properties of Al–20Si–5Fe–2 X ( X = Cu, Ni, Cr) alloys produced by melt-spinning

Al–20Si–5Fe–2X ( X = Cu, Ni and Cr) ribbons were produced by melt-spinning and consolidated by hot pressing at 400 °C for 60 min. The microstructure of the ribbons and the consolidated alloys was investigated using optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffractometry (XRD) method, and transmission electron microscopy (TEM). The hardness and compressive strength of the specimens at ambient and elevated temperatures were examined. The microstructure of the ribbons exhibited featureless and dendritic zones. Results of XRD and TEM showed formation of spherically shaped Si particles with an average diameter of 20 nm. Ultrafine Si (110–150 nm) and iron-containing intermetallic particles were noticed in the microstructure of the consolidated ribbons. An improved strength was achieved by alloying of Al–20Si–5Fe with Cu, Ni, and Cr. Nickel was found to be the most effective element in increasing the maximum stress, particularly at elevated temperatures.

Phase Stability of 10mol%Sc2O3-1mol%CeO2-ZrO2 Ceramics

ABSTRACTScandia-doped zirconia is a very promising material for solid oxide fuel cells due to its high oxygen conductivity in the 700-850°C temperature range. 10 mol% Sc2O3 - 1 mol% CeO2 - ZrO2 ceramics were sintered at temperatures 1100-1600°C using different heating rates and dwell times. Ceramics sintered at temperatures higher 1300°C were found to exist in cubic phase at room temperature and exhibit slow phase transformation from cubic (c) to rhombohedral (beta) phase between 330 and 400°C. Analysis of c-β phase transition efficiency in the ceramics shows a strong correlation between the transition rate and sintering temperature. Kinetics of phase transitions were studied by high temperature X-ray diffractometry (HTXRD) and differential scanning calorimetry methods. The reversible c-β phase transition was found to have very wide hysteresis (45-70°C), which depends on sintering temperature and density. Coefficients of thermal expansion of c- and β-phases were calculated from temperature dependence of lattice parameters obtained by HTXRD in the temperature range of 25-800°C. Microstructural changes on the surface of the cubic phase due to c-β phase transition studied by SEM and AFM.

Defects of the structure of semiconductor superlattices grown on the basis of II–VI alloys

The specific features of defects of crystal lattices in multilayer device structures containing small-period (T ≲ 20 nm) superlattices of type I ZnSe/Cd x Zn1 − x Se/ZnSe/.../ZnSe/(001)GaAs and type II ZnS/ZnSe1 − x S x /ZnS/.../ZnS/(001)GaAs are studied by the methods of X-ray diffractometry and diffraction rocking pseudocurves, and partially by the X-ray topography. According to the data of quantitative analysis of the X-ray diffraction spectra, the periods of superlattices are in the range T I = 11.3–16.1 nm (for the compositions Cd x Zn1 − x Se with x 1 = 0.047 and x 2 = 0.107) for type I superlattices and T II = 15.6–17.2 nm for type II superlattices (for the compositions ZnSe1 − x S x with x 1 = 0.20 and x 2 = 0.10). The widths of diffraction peaks from both the ZnSe layers and small-period superlattices in the diffraction rocking pseudocurves considerably exceed their widths in the X-ray diffraction spectra. This fact proves that a pronounced plastic strain with the formation of series of rectilinear dislocations in the crossing slip systems took place in the studied device structures. In order to exclude the generation of dislocations in the growth processes, it is necessary to decrease the concentration of the solid solution to the values x < 0.047 for the first type of superlattices and to the values x ≲ 0.062 for the second type of superlattices, and to decrease the thickness of the ZnSe and ZnS layers.

Changes in the crystal structure of metals under laser radiation

The change in the crystal structure of a number of metals (Cu, Al, Ag) under laser radiation of power density 104–105 W/cm2 was detected by the method of x-ray diffractometry. It was suggested that this effect is due to the large microstresses arising in the zone of rapid anisotropic heating of the metal under irradiation.

The potential of SilviScan’s X-ray diffractometry method for the rapid assessment of spiral grain in softwood, evaluated by goniometric measurements

The orientation of the tracheid cells with respect to the stem axis (grain angle, spiral grain) exerts a strong influence on numerous material properties. Therefore, several methods have been developed to assess this wood anatomical feature. The current study compares SilviScan spiral grain measurements, which uses X-ray diffractometry, with direct goniometer readings. The correlation between these two methods yielded an r2 of 0.874 and a root mean square error of prediction (RMSEP) of 1.21 clearly demonstrating that X-ray diffractometry can provide accurate and rapid information on the grain orientation in Norway spruce (Picea abies (L.) Karst.) or similar structured softwoods.

Thermoluminescence (TL) of europium-doped ZrO2 obtained by sol–gel method

This article reports the preparation and characterization of europium-doped zirconium oxide (ZrO2:Eu3+) formed by homogeneous precipitation from propoxyde of zirconium [Zr(OC3H7)4]. The alkoxide sol gel process is an efficient method to prepare the zirconium oxide matrix by the hydrolysis of alkoxide precursors followed by condensation to yield a polymeric oxo-bridged ZrO2 network. All compounds were characterized by thermal analysis and the X-ray diffractometry method. The thermoluminescence (TL) emission properties of ZrO2:Eu3+ under beta radiation effects are studied. The europium-doped sintered zirconia powder presents a TL glow curve with two peaks (Tmax) centered at around 204 and around 292 °C, respectively. TL response of ZrO2:Eu3+ as a function of beta-absorbed dose was linear from 2 Gy up to 90 Gy. The europium ion (Eu3+)-doped ZrO2 was found to be more sensitive to beta radiation than undoped ZrO2 obtained by the same method and presented a little fading of the TL signal compared with undoped zirconium oxide.

Characterization of In/Pd and Pd/In/Pd thin films by ellipsometric, XRD and AES methods

In/Pd and Pd/In/Pd thin films were prepared by thermal evaporation on the SiO2 substrate in a vacuum. The structural and optical properties of the films were investigated by means of X-ray diffractometry (XRD), Auger electron spectroscopy (AES) and spectroscopic ellipsometry (SE). Auger depth profile studies were performed in order to determine the composition of elements in the Pd-In systems. Interdiffusion of metals was detected at room temperature. Optical properties of Pd-In composite layers formed due to the interdiffusion were derived from ellipsometric quantities Ψ and Δ measured in the photon energy range 0.75–6.50eV at different angles of incidence. The effective optical spectra show absorption peaks dependent on the composition of nonuniform films. The XRD patterns indicated formation of Pd1−xInx intermetallic phases in the samples.

Establishing Composition and Structure of Intact Urinary Calculi by X-Ray Coherent Scatter for Clinical Laboratory Investigations

Current urinary stone analysis techniques are limited in their abilities to simultaneously characterize composition and structure. Laboratory techniques such as IRS and x-ray diffractometry require small powdered samples for analysis, rendering composition results dependent on the choice of sample and its preparation. We investigated the application of x-ray CS analysis to identify topographic urinary stone composition ex vivo. CS is essentially a transmission based x-ray diffractometry method that depends on molecular structure and, therefore, can distinguish different compounds. Diagnostic x-ray equipment facilitates the examination of structural arrangements of minerals in intact calculi. Tomographic images of intact calculi CS properties were acquired with a purposely built scanner. Composition is extracted from CS by fitting a library of common pure stone component CS signatures to those of the unknown sample in each image pixel. Two zones per stone were isolated (powdered) for IRS composition analysis for comparison with CS maps at these locations. Each stone was also independently analyzed for bulk composition by IRS analysis. CS composition maps revealed the spatial arrangement of minerals in intact calculi. IRS results showed good agreement with CS in the selected regions of interest. Bulk composition by IRS was noted to miss some important stone components, indicating that the choice of sample may skew composition results. CS from diagnostic x-rays can be used to identify structure and composition in mixed urinary calculi nondestructively. The tissue specific CS images presented support the development of CS analysis as a means of identifying stone composition characteristics in the laboratory.

Effect of electropulse treatment on the structure of the surface layer of alloy VT3-1

The structure and the fatigue resistance of titanium alloy VT3-1 after electropulse treatment (EPT) are studied by the method of x-ray diffractometry. The effect of EPT on the relaxation of residual stresses, the size of mosaic blocks, the elastic modulus of the surface layer, and the yield strength of the alloy is determined.

Characterization of In/Pd and Pd/In/Pd thin films by ellipsometric, XRD and AES methods

Abstract In/Pd and Pd/In/Pd thin films were prepared by thermal evaporation on the SiO 2 substrate in a vacuum. The structural and optical properties of the films were investigated by means of X-ray diffractometry (XRD), Auger electron spectroscopy (AES) and spectroscopic ellipsometry (SE). Auger depth profile studies were performed in order to determine the composition of elements in the Pd-In systems. Interdiffusion of metals was detected at room temperature. Optical properties of Pd-In composite layers formed due to the interdiffusion were derived from ellipsometric quantities Ψ and Δ measured in the photon energy range 0.75–6.50 eV at different angles of incidence. The effective optical spectra show absorption peaks dependent on the composition of nonuniform films. The XRD patterns indicated formation of Pd 1− x In x intermetallic phases in the samples.

Special features of the deformation-induced order-disorder phase transition and its modeling

Methods of x-ray diffractometry are used to investigate the influence of plastic deformation on the state of the long-range order in alloys with the L12, L12(M), and L12(MM) superstructure. It is demonstrated that the heterogeneous order-disorder phase transition accompanied by intensive accumulation of antiphase boundaries occurs under plastic deformation. The antiphase boundaries play an important role in the destruction of long-range order. Based on the available experimental results, a model of destruction of long-range order is constructed that takes into account the dislocation mechanisms of accumulation of antiphase boundaries under deformation.

Influences of ZrO2 nanoparticles on the microstructure and mechanical behavior of Ce-TZP/Al2O3 nanocomposites

Influences of ZrO2 nanoparticles on the mechanical properties and microstructure of hot-pressing Ce-TZP/Al2O3 ceramics were investigated. Meanwhile, t-ZrO2 to m-ZrO2 transformation toughening mechanism was investigated by X-ray diffractometry (XRD) method, and deflection of samples under applied stress were recorded too. The results show that when the percentage of ZrO2 was 20%, the mechanical properties and microstructures of materials are optimum. Moreover, TEM observation show dislocation structures formation both in the Al2O3 and on the grain boundary. Because the dislocation agglomeration and fixation by ZrO2 nanoparticles could deflect cracking or stop cracking development, a strengthening and toughening effect could be achieved.

Structural characterization of interfaces in the AlxGa1−x As/GaAs/AlxGa1−x As heterostructures by high-resolution X-ray reflectometry and diffractometry

The structural properties of multiplayer AlxGa1−xAs/GaAs/AlxGa1−xAs systems (x ≈ 0.2) grown on GaAs(001) substrates are studied by the methods of double-crystal X-ray diffractometry and reflectometry. The depth profiles of deformation, amorphization, and density of the layers are obtained. It is shown that despite small differences (5–7%) in the densities of the AlxGa1−xAs layers and the substrate and the small thickness of the AlAs layer (1–2 nm) separating the GaAs quantum well, it is possible to reconstruct the heterostructure model by the method of X-ray reflectometry and to determine the thickness of the transitional layers at a resolution of 0.1–0.2 nm. It is also established that the reflectometry data obtained complement the X-ray diffraction data considerably and allow one to estimate the roughness and the character of the aluminum distribution at the interfaces.

Influence of Moisture on the Structure and Properties of the Interphase Layer of a Composite Based on an Epoxy Binder with a Disperse Filler

Properties of a model composite based on an ED-22 epoxy binder, cured with polyprophylene polyamine, and disperse LiF crystals as a filler were investigated by the methods of dilatometry and X-ray diffractometry. It was established that the density of cross-links of the epoxy binder in the interphase layer was lower than in a block specimen. Therefore, the thermal expansion of the composite on heating to 120°C, in terms of that of the binder, grew significantly with the degree of filling ϕ, and the water uptake also increased at the initial stage. The presence of absorbed water led to considerable changes in the structure and properties of the composite interphase: the binder became more cross-linked, its structural ordering decreased, the thermal expansion at heating diminished by a factor of 3. 7 (at ϕ = 50%), and the glass-transition temperature increased. As a result of long-term action of moisture, changes in the internal stresses had an extreme character.

X-Ray Diffraction Analysis of Epigrowth on Porous 4H-SiC Substrates

The methods of X-ray topography and diffractometry have been applied to characterize the structure of epilayers grown on porous layers. Two geometrical configurations of defects determined to be stacking faults (SF) were revealed: i) with the images of triangular shape with the edge size 560 µm along the &lt;10-10&gt; directions; ii) linear shape along the [11-20] direction. The sources of SFs are located within the epilayer and start from the epilayer / porous layer interface. We propose that the source of SFs is connected with graphitization of porous layer at the temperature of epitaxy.

Structural features of Ge(Ga) single crystals grown under conditions simulating the microgravity perturbation factors

Peculiarities of the real structure of Ge(Ga) single crystals grown under external mechanical perturbations of the crystallization process simulating actual microgravity environment aboard spacecrafts were investigated by X-ray topography and diffractometry methods, etching analysis and spreading resistance measurements. The applied perturbations included vibrations and variations of growth facility orientation with respect to the direction of gravity force. It has been shown that microinhomogeneity of the crystals grown is defined not only by formation of dopant growth striations at peculiar vibrational perturbations of a melt, but also by specific features of dislocation structure of crystals related with the formation of small angle boundaries, slip bands and other inhomogeneities in dislocation distribution. (© 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)

Preparation of Nanocrystalline Copper and Copper Silicon Sulphide by Mechanochemical Route

The composition and properties of powders prepared by high-energy milling of copper sulphides with silicon have been studied by methods of X-ray diffractometry and surface area measurement. The combination of several methods was utilized to develop a coherent picture of the process. The overall process of mechano-chemical transformations in copper sulphide-silicon system proceeds via complicated mechanism with several overlapping steps. Phase transformations in copper sulphide phases, the formation of elemetal nanocopper with X-ray determined particle size of 23 nm and creation of ternary sulphide Cu8SiS6 with anomalous surface area values are the main products of the mechanochemical reaction.

Fractal nature of the dislocation structure of low-alloyed steel after controlled rolling

Methods of x-ray diffractometry and transmission electron microscopy are used to study the crystallographic texture and dislocation structure of low-alloyed steel after controlled rolling. It is demonstrated that the formation of crystallographic texture and the corresponding dislocation structure are interrelated. These processes are a manifestation of different sides of one phenomenon of developed plastic strain. The fractal dimensions of cellular dislocation structure boundaries of the main texture components in deformed steel are determined using the multiple grid method.

Production of copper and brass nanoparticles upon laser ablation in liquids

The production of nanoparticles upon ablation of copper and brass by pulsed radiation from Nd:YAG and copper lasers in water, ethanol, and acetone is studied. The nanoparticles were investigated by the methods of X-ray diffractometry, optical spectroscopy, and transmission electron microscopy. The produced copper and brass nanoparticles were shown to exhibit a plasmon resonance lying in the visible spectral range near 580 and 510 nm. The brass nanoparticles produced by ablation in ethanol have a shell approximately 10-nm thick for an average dimension of 20–30 nm. A chemical modification of ethanol was observed, which manifested itself in the appearance of intense UV absorption bands. Upon laser irradiation of brass nanoparticles in a liquid their absorption spectrum gradually transformed into the spectrum of copper nanoparticles.