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We present a detailed description of the SESAME Materials Science (MS) beamline for X-ray diffraction (XRD) applications, presently under construction in Allan, Jordan. The beamline is based on components previously installed at the Swiss Light Source, but modifications in the beamline design have been introduced to match the characteristics of the SESAME storage ring. The SESAME MS beamline will accommodate XRD experiments in the energy range between 5 and 25 keV. The beamline ray tracing analysis at 10 keV estimates the flux at the sample to be of the order of 1013 (photons s−1), the energy resolution is about 2 eV and the effective beam size at the sample of 300 × 2800 µm2. Investigations of microstruture will be possible as the instrumental broadening, resulted from simulating the diffraction pattern for a standard material, is of the order of 0.01° at 15 keV. A wide range of applications will be possible at the beamline, such as powder diffraction studies, single crystals and in situ XRD. The commisioning of the beamline is expected to be in the second half of 2017.
The rheological behavior of composites made with high-density polyethylene (HDPE) and chitosan was studied. Composites were prepared by melt processing in a laboratory internal mixer. Maleic anhydride grafted HDPE (PE-g-MA) was used as compatibilizer to enhance the dispersion of chitosan in the HDPE matrix. Different percentages of chitosan and compatibilizer (up to a maximum of 25 phr) were added into HDPE to prepare composites. Characterization of the composites with parallel plate rheometer and laboratory internal mixer revealed that the presence of chitosan increases the complex viscosity, loss modulus, storage modulus and the torque (i.e., melt viscosity), and the combination chitosan/compatibilizer has a similar, if slighter, effect. At higher filler levels it is clear that the PE-g-MA affected the microstructure of the compounds, possibly increasing matrix–filler interactions and acting as an effective compatibilizer.
Microstructure and electrochemical behavior of stainless steel weld overlay cladding exposed to post weld heat treatment (PWHT) were investigated, wherein pitting and intergranular corrosion behaviors of the cladding material were evaluated by potentiodynamic polarization and double loop electrochemical potentiokinetic reactivation methods. The results indicated that inclusions, multiple element (Mn, Si, and Al) oxides distributed randomly in the cladding material with a size less than 1 μm. PWHT contributed to carbides precipitation along the δ/γ phase interface and the formation of Cr-depleted zone in the austenite phase. Inclusions acted as the pitting sites in the sample as welded. PWHT reduced the pitting potential and contributed to the formation of larger and deeper pits, which nucleated around the δ/γ phase interface primarily. Existence of carbides and Cr-depleted zone dominated the loss of intergranular corrosion resistance after PWHT.
Hot isotherm compression tests were performed in temperature range of 350–500 °C and at strain rates of 0.0005 to 0.5 s−1 for Al6061 alloy reinforced with alumina nanoparticles. Effect of deformation parameters and optimal conditions for hot working this nanocomposite were comprehended thoroughly via hot working data analyses, electron microscopy images, and X-ray diffractograms. The results indicated the severity of hot deformation process and an increase in the activation energy to 320 kJ/mol due to the addition of nanoparticles. Dynamic recovery (DRV) was considered as the individual determinative softening mechanism during hot deformation of this nanocomposite, and no sign of dynamic recrystallization (DRX) phenomenon observed in the same domain. The unstable region occurred at high strain rates and temperature range of 350–500 °C accompanied with happening drastic defects such as shear bands and cracks. Furthermore, the value of both critical strain and critical stress increased with increasing the strain rate and alumina addition. On the other hand, increasing the temperature decreased the value of critical strain and facilitated the initiation of softening mechanisms.
The present work focuses on the deformation and recovery mechanisms of aged monoclinic U–Nb alloy under tension and load–unload cycle testing using in situ X-ray diffraction (XRD). The U–6.2wt% Nb (U–6.2Nb) alloy was prepared and aged at 200 °C, and then underwent tensile testing followed by the in situ XRD. The experimental results indicate that the change of diffraction peaks can serve to accurately characterize the macroscopic deformation and recovery. Compared with the as-quenched alloy, the aged U–6.2Nb alloy displays different behavior during deformation and subsequent recovery. Phase transformation competes with twin rearrangement to dominate the deformation and recovery between elastic stage and slip stage of the alloy. The lattice plane relationship between α″ and γ° during phase transformation has also been given.
This study investigates the morphology changes in thin diblock copolymer (DiBCP) films occurring in the interaction with modified nanoparticles (NPs). Magnetite (Fe3O4) and silica (SiOx) were prepared and used. Poly(pentyl methacrylate-b-methyl methacrylate) (PPMA-b-PMMA) (70/30 mol mol−1, hcp cylinders of the PMMA phase) DiBCP were employed to prepare thin films having thicknesses to realize standing cylinders in pure DiBCP films. The investigations aimed at two topics: (1) morphology after controlled incorporation of organo-modified NP (gold, silver, Fe3O4, SiOx) and (2) additional solvent vapour annealing (SVA) with tetrahydrofuran (and chloroform for comparison). The laterally ordered morphology in thin films was examined by GISAXS and atomic force microscopy. Keeping the same type of morphology in nanocomposites, the dimensions of the periodic nanostructure altered depending on type and amount of incorporated NP. It was found that SiOx clusters enlarge the lateral distance of the PMMA cylinders, whereas metallic NPs reduce this parameter. Applying SVA improves the phase separation slightly, whereas lateral distances were kept constant or were reduced a little. Switching of domain orientation upon SVA could not be detected in the presence of NPs located at the polymer/substrate interface.
YCrO3 (YCO) perovskite has been originally reported to be a biferroic with antiferromagnetic and ferroelectric (FE) properties, in which the origin of FE in YCO remains ambiguous. However, further studies reveal the presence of a global orthorhombic Pnma structure with a local structural heterogeneity. In this study, we discuss the high temperature phonon modes and their inter-relation to local structural distortions in YCO perovskite through Raman spectroscopy experiments and density functional theory (DFT) calculations. We observe that the Raman active B3g(3) out of phase scissor mode (SM) disappears above the dielectric transition temperature (Tc) commensurate with the local structural distortions. DFT calculations show that the transformation of a room temperature Y-cation distorted orthorhombic structure to a perfect orthorhombic structure above the dielectric transition temperature in which the Y cation is undisplaced could lead to the conversion of SM with symmetry B3g to Raman inactive B1u mode.
Al1.3CrFeNi eutectic high entropy alloy was designed and prepared by arc-melting to investigate the microstructure and oxidation behaviors at 1000 °C. The XRD pattern shows that this alloy had a double bcc/B2 structure. SEM images indicates that the microstructure of the alloy is composed of two precipitates of [Cr, Fe] solid solution and NiAl intermetallic, which form the typical eutectic structure. To explore the thermal application of Al1.3CrFeNi alloy, the oxidation behavior of Al1.3CrFeNi alloy at 1000 °C was investigated. From XRD and SEM results, it could be concluded that Al2O3 and Cr2O3 were the predominant oxides during the oxidation process. In addition, spinel like FeCr2O4 was also observed in the oxide scale. According to the analysis of oxide precipitates, the whole process of oxides’ formation was discussed and a simplified oxidation dynamic model of Al1.3CrFeNi alloy at 1000 °C was obtained. This could promote the development of thermal applications in multi-component alloys field.
This book is focused primarily on polymer nanocomposites, based on the author's research experience as well as open literature. The environmental health and safety aspects of nanomaterials and polymer nanocomposites, risk assessment and safety standards, and fire toxicity of polymer nanocomposites, are studied. In the final chapter, a brief overview of opportunities, trends, and challenges of polymer nanocomposites are included. Throughout the book, the theme is developed that polymer nanocomposites are a whole family of polymeric materials whose properties are capable of being tailored to meet specific applications. This volume serves as a general introduction to students and researchers just entering the field and to scholars from other subfields seeking information.
Having synthesised an AlON-bonded ceramic corundum material, Al5O3N3 (15R) polytype coexisting with α-Al2O3 was identified. The sample was prepared from an alumina-rich mixture of Al2O3 and AlN substrates and fired at 1650 °C in a nitrogen atmosphere. Using the X-ray external standard quantitative method, one of the reaction products, α-Al2O3, was quantified. From the remaining substrates the stoichiometric composition of the second phase was calculated. The applied method of crystal structure determination consisted of three stages. In the first stage, the Le Bail method of X-ray pattern decomposition was used for the extraction of Al5O3N3 (15R) diffraction lines from a two-phase diffractogram. The space group and unit-cell dimensions from the isostructural SiAl4O2N4 SiAlON phase, producing the same X-ray pattern, were used as input data. Next, the direct structure determination in real space was applied for initial structural model derivation, which was followed by Rietveld refinement. The solved crystal structure of Al5O3N3 (15R), except the stacking sequence, proved to be closely related to the structure of Al7O3N5 (21R) polytype. The Al5O3N3 (15R) is trigonal with space group R-3m, unit-cell dimensions a0 = 3.0128 Å, c0 = 41.8544 Å, and volume V = 329.00 Å3. The model of Al5O3N3 (15R) polytype structure has positional disordering in one of three (6c) Al sites, which leads to stacking faults in six tetrahedral layers. Every third tetrahedron from LR3 and LR4, LR8 and LR9, LR13 and LR14 layers is rotated by 180°.
Microstructural and morphological features of the layers forming integrated PTB7/PC71BM organic solar cells with Ca/Al cathode are studied. The effects of vacuum treatment on properties and durability were addressed using complementary approaches: time-resolved experiments revealing the structural evolution of the active layers under illumination were conducted combining the in situ energy dispersive X-ray diffraction (EDXD) technique with atomic force microscopy (AFM); space-resolved characterization of the integrated devices was possible via high resolution X-ray diffraction, using a nano-focused synchrotron radiation X-ray beam to discriminate the device components. Active layers surface morphology is stable under illumination and PC71BM structural properties remain unaltered. PTB7 undergoes crystallinity depletion, mainly at the active layer/cathode interface. This effect is actually inhibited in the device submitted to vacuum treatment, proving that this procedure induces stabilization at the cathode’s buried interface, as verified by fourier transform infrared (FTIR) spectroscopy. Importantly, the protective role of the vacuum treatment results in a significant photovoltaic durability enhancement.
Aluminum (Al) nanoparticles are synthesized by wire explosion process (WEP) in an inert ambience of argon. Thermodynamic analysis and structural characterization of nano Al particles are made in the present work. Transmission electron microscopy (TEM) characterization has shown that the Al nanoparticles produced are spherical in shape and it follows a lognormal distribution. A unimodal size dependent thermodynamic model is formulated to understand the size dependent thermal behavior of aluminum nanoparticles. Three different melting modes such as, homogeneous melting mode (HMM), liquid skin melting (LSM) and liquid nucleation and growth (LNG) are assumed to understand the melting behavior of aluminum nanoparticles synthesized by the WEP process. The effect of saturation ratio on the nucleation rate and the impingement factor is also discussed. The size dependent melting and enthalpy of fusion of Al nanoparticles predicted by thermodynamic model are in tandem with the DSC results.
In present study, the semi-solid slurry of the AZ91–2Ca–1.5Ce alloy was firstly prepared by gas-bubbling processing and then was formed by die casting and squeeze casting, respectively. The influence of processing parameters on microstructure and mechanical properties of the alloy was investigated. The results show that increase of gas-flow rate and appropriate pouring temperature can improve the quality of the semi-solid slurry and change the morphology of primary α-Mg particles to rosette-like shape or roundness. Meanwhile, the addition of calcium and cerium refines the as-cast microstructure and dramatically improves the tensile properties, also the strengthening phase Al4Ce exists around the grain boundary. The peak ultimate tensile strength (UTS), yield strength, and elongation of rheo-die casting AZ91–2Ca–1.5Ce alloy are 202 MPa, 154 MPa, and 2.3%, respectively. Especially, compared with conventional liquid die-casting, the UTS and elongation of rheo-die casting AZ91–2Ca–1.5Ce alloy were improved by 8% and 64%, respectively. Meanwhile, the rheo-die casting alloy also showed higher mechanical properties than rheo-squeeze casting alloy, since the higher speed that die casting provided could induce more compact microstructure and remain the semi-solid characteristic better.
The synthesis of aluminum nitride (AlN) powders from aluminum (Al) particles via a thermal nitridation process was carried out at high temperature (>900 °C) with a long reaction time (∼several hours). This study proposes a two-stage plasma-chemical synthesis process to efficiently minimize the agglomeration of Al particles, reduce the reaction time and temperature, and promote the formation of AlN powders. In the first stage, partially nitrided Al powders were produced at temperatures lower than 600 °C in atmospheric-pressure microwave N2 plasma. The particle size of the as-prepared powders was similar to that of the original Al powders. In the second stage, the reaction temperature was increased to 700–800 °C and the reaction time was less than 5 min in N2 plasma. Well-dispersed AlN powders with almost no agglomeration were produced. Moreover, the particle size was lower than that of the original Al.
One hundred years ago X-ray powder diffraction, one of the premier techniques used in the characterization of materials, was invented. Its origins can be traced to two landmark contributions presented to the scientific community in 1916. They are the better known and celebrated work carried out by Paul Scherrer under the guidance of Peter W. Debye, at the University of Göttingen, Germany, and the lesser known work of Albert W. Hull performed at the Research Laboratory of the General Electric Company, Schenectady, NY, USA. The great contributions of Scherrer and Debye have been prominently recognized. They are presented in many textbooks and in technical and scientific articles published in the area of characterization of materials using powder diffraction techniques. The camera designed by them, later called “the Debye–Scherrer camera”, was used extensively for many years and the experimental setup (“the Debye–Scherrer geometry”) is still used today. On the other hand, the work performed by Hull has not been adequately appreciated and remembered. In this communication, an account of his contributions to X-ray powder diffraction and to crystallography is presented at 100 years of his landmark publication, which appeared in the first issue of Physical Review of 1917.
The hydrogenation behavior of Ti–44Al–6Nb (at.%) alloy was studied at temperature range of 1373–1693 K, and the effect of hydrogen on hot deformability was tested on Gleeble-1500D thermo-simulation machine. It is found that the lnCH increases linearly with 1/T, and hydrogen content increases with increasing of hydrogen time and flow rate logarithmically. The positive heat of solution of hydrogen denotes that hydrogen absorption in TiAl alloys is an endothermic reaction. The results also show that hydrogen promotes the lamellar colony size and lamellar spacing because that hydrogen can promote the diffusion of elements. There is more residual B2 phase in the hydrogenated alloy revealing that hydrogen stabilizes the B2 phase during hydrogenation. The nanohardness and elastic modulus of the alloy are decreased from 4.4 and 213.5 GPa to 4.2 and 199.8 GPa after hydrogenation with 0.033 wt% H. Thermal simulation results show that the peak stress is decreased by 30% after hydrogenation with 0.033 wt% H which corresponds to decreasing the deformation temperature by about 50 K. This is attributed to hydrogen-promoted dynamic recrystallization and dislocation movement.