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The structure of TeO3, first published by Dumora and Hagenmuller (1968), was redetermined from new X-ray data collected with a powder diffractometer using space group R3̄c with a = 4.901(2), c = 13.030(4) Å, V = 271.05(8) Å3 and Z = 6. Intensity data were obtained with CuKα, radiation (λ = 1.540598 Å). Structure refinement was performed with 49 reflections and led to R = 0.058. The material is isostructural with FeF3. Powder data are given.
A deformed aluminum-copper alloy was studied by X-ray diffraction. The 111 diffraction profile was found to consist of a main peak and a subpeak. They were separated by a numerical differential method combined with a non-linear least square profile fitting procedure. The subpeak could not be ascribed to the θ phase in the alloy since the intensity ratio of the subpeak to main peak is 20-30 times more than the volume ratio of the θ phase to die matrix. On the other hand, the Transmission Electron Microscope (TEM) micrographs showed clearly that there is a highly inhomogeneous dislocation distribution just like the cell structure in pure aluminum. The main X-ray peak was thus assumed to be due to diffraction from the cell interior while the subpeak is determined by the cell wall. After applying a series of standard data processing procedures based on Wilkens' theory and the Pearson VII-Voigt function, the dislocation densities in both the cell interior and wall were evaluated.
The fly ash Standard Reference Materials (SRMs) issued by the U.S. National Bureau of Standards have been studied by X-ray powder diffraction (XRD). Based on observations of large diffuse scattering maxima in their X-ray diffractograms, it was evident that all of the ashes had a high glass content. SRM 1633a and 2689, derived from the combustion of bituminous coal, contained different amounts of quartz, mullite, hematite and ferrite spinel (magnetite). SRM 2891, derived from subbituminous coal had quite a different chemical composition and a more complex crystalline phase assemblage, that included these four phases plus anhydrite, tricalcium aluminate, lime, periclase and minor phases. SRM 2690, also derived from subbituminous coal, had only quartz, mullite and ferrite spinel as detectable phases in its diffractogram. Analytical CaO is an important factor in determining the phase assemblage; SRM 2691 had 25.8 wt%, SRM-2690 had 8.0%, and the ash derived from bituminous coals had only 1.6-3.0%. The changing composition of the glass phases in the SRMs is detected in a shift in the position and shape of the diffuse scattering maximum in the diffractograms. Use of an internal intensity standard permitted quantitative comparisons of the relative amounts of crystalline phases among the four fly ash SRMs.
The diffraction patterns of coarse grained materials are compared to specimens with crystallite sizes of less than 1 µm characterized by diffraction spots. Based on an analysis of spot intensities it is shown that for: (a) an at-random distribution of crystallite orientations and (b) under the assumption of specific crystallite shapes it becomes possible to evaluate the distribution N(l) of linear crystallite dimensions (0.1 µm < l < 20 µm) from measured spot intensity distributions z(i).
Indexed X-ray diffraction powder data for {[Cr3O(C6H5NO2)6(H2O)3](CIO4)7 · 3NaCIO4·0.5(C6H5NO2)· 3H2O}, INICCR (isonicotinato) and {[Cr3O(C6H5NO2)6(H2O)3] (CIO4)7·6NaCIO4·3H2O}, PICOCR (picolinato) are reported. Both INICCR and PICOCR crystallize in the hexagonal space group P63/m. Crystal data determined for INICCR are a = 13.838(3) Å, c = 25.038(8) Å, V = 4152.2 Å3, Dx = 1.71 Mg m−3 (Dm = 1.66(5) Mg m−3), F25 = 26.5(0.020,47) and for PICOCR are a = 13.966(4) Å, c = 24.518(6) Å, V = 4141.5 Å3, Dx = 1.96 Mg m−3 (Dm = 1.94(4) Mg m−3), F21 = 17.9(0.023,51). The JCPDS Diffraction File Number for INICCR is 38-1992 and for PICOCR is 38-1993.
The method described in this paper is a strict protocol for X-ray diffraction (XRD) analysis of mineral phases found in soils. Its application is not restricted to soils and is an attempt to standardize XRD sample preparation and analysis. The protocol requires the particle size of the < 2 mm - 0.002 mm fraction be reduced to 0.002 mm before analysis. In die qualitative section, the clay fraction ( < 0.002 mm particle size) is prepared as oriented slides. The suspended clay fraction is saturated with ethylene glycol, K +, and Mg+2; pipeted; air-dried; heat-treated at 110°C, 350°C, and 550°C; and X-rayed at each step in order to properly identify the clay minerals. In the quantitative section, the method employs a matrix-flushing agent, corundum (Al2O3). The corundum acts also as an internal standard, a calibration standard, and a reference standard. The suspended clay fraction is freeze-dried and corundum is added to each sample. Randomly oriented powder mounts are prepared from the < 2 mm - 0.002 mm fraction, and the < 0.002 mm fraction, and X-rayed. A series of reference standards are prepared based on the existing mineralogy, corundum is added, and each mixture is X-rayed. The software integrates the area under specific peaks (chosen for intensity and no overlap) in each sample, calculates the reference intensity ratios (RIRs) and calculates the percentage of each mineral based on the equation of Chung (1974). The attention to detail allows documentation and verification of the results yielding data of known quality.
The machining of shape memory alloys (SMAs) is fairly essential and integral part in the manufacture of components for utilizing in engineering applications. An effort has been made in the present work to study the effect of wire electro discharge machining process parameters such as pulse on time (Ton), pulse off time (Toff) and servo voltage (SV) have been analyzed on material removal rate and surface roughness. The investigation clearly reveals that an increased pulse on time with decrease in pulse off time as well as SV increases the amount of material removed in machining of SMAs. On the other hand, the surface roughness increases with increased pulse on time and decreases with increased pulse off time as well as SV. The surface topography of the machined surface was analyzed using scanning electron microscope (SEM) and confocal micrographs. Phase changes on the machined surface with respect to pulse on time and SV were evaluated from X-ray diffractometer (XRD) analysis.
Potassium titanyl phosphate crystals in both x-cut and z-cut were irradiated with 185 MeV Au ions. The morphology of the resulting ion tracks was investigated using small angle x-ray scattering (SAXS), transmission electron microscopy (TEM), and atomic force microscopy (AFM). SAXS measurements indicate the presence of cylindrical ion tracks with abrupt boundaries and a density contrast of 1 ± 0.5% compared to the surrounding matrix, consistent with amorphous tracks. The track radius depends on the crystalline orientation, with 6.0 ± 0.1 nm measured for ion tracks along the x-axis and 6.3 ± 0.1 nm for those along the z-axis. TEM images in both cross-section and plan-view show amorphous ion tracks with radii comparable to those determined from SAXS analysis. The protruding hillocks covering the sample surface detected by AFM are consistent with a lower density of the amorphous material within the ion tracks compared to the surrounding matrix. Simulations using an inelastic thermal-spike model indicate that differences in the thermal conductivity along the z- and x-axis can partially explain the different track radii along these directions.
Microstructure evolution and tensile properties of large dimensional bulk 304 stainless steel after being rolled with different thickness reductions were characterized in detail. The results showed that the steel consisted of nano-submicro-microcrystalline austenite and nanocrystalline ferrite. Submicrocrystalline austenite was broken down with the thickness reduction, when thickness reduction was 70%, all submicrocrystalline were broken down to nanocrocrystalline, and dispersed more uniformly in the microcrystalline austenite phase in the steel, but the grain size of the nanocrystalline austenite increased to 70 nm. Tensile strength increased from 850 MPa to 965 MPa, yield strength increased from 652 MPa to 837 MPa, elongation decreased from 33% to 19%, intergranular corrosion rate decreased from 1.36 g/(m2 h) to 0.46 g/(m2 h). Strength and intergranular corrosion properties increased much. When the thickness reduction was 70%, the tensile strength, yield strength, elongation, and intergranular corrosion properties were the best in the reported value of the steel.
Graphite flakes (Gf)/Si/Al composites have been fabricated with different volume fraction of graphite by vacuum gas pressure infiltration. In the composites, the addition of Si played a role of spacing apart graphite layers, which can produce voids between layers for the infiltration of molten aluminum. Microstructural characterization indicated that the reinforcements were fairly distributed in the Al and a clean interface lacking of Al3C4 phase was formed between Al and Gf. With the increase of Gf from 39 to 81 vol%, the longitudinal thermal conductivity (TC) of composites increased from 294 to 390 W/m K, but the open porosity increased from 1.85 to 6.03%. Besides, a joint M1–M2 prediction model was established, which considered that the microstructure of composites lies in between two models: (M1) a layered structure in binary metal-particle composites and (M2) ternary composites that oriented flakes randomly distributed in metal-particle confirmed a better theoretical prediction of TC.
In the present study, the surface properties and the corrosion behavior of a nanocrystalline surface layer fabricated on 45 steel by electropulsing-ultrasonic surface treatment (EUST) were investigated. EUST offered the specimen a smooth (Ra < 0.33 µm) surface layer with nanoscale grains and compressive stress by the synergistic effect of high-energy electropulsing processing and ultrasonic impact. Open-circuit potential, potentiodynamic polarization, and electrochemical impedance spectroscopy studies indicated that EUST-induced surface nanocrystallization decreased the corrosion susceptibility of 45 steel in 3.5 wt% NaCl aqueous solution, leading to a decrease in corrosion current density (icorr) by 55% and an increase in charge transfer resistance (Rct) by 36%. The enhancement in surface comprehensive mechanical properties and corrosion resistance can be explained in terms of the decrease in surface roughness, the extent of grain refinement and the change of stress state, which were closely related to the introduction of high-energy electropulsing processing.
While materials design in the context of texture dependent properties is well developed, theoretical tools for microstructure design in the context of grain boundary sensitive properties have not yet been established. In the present work, we present an invertible relationship between texture and grain boundary network structure for the case of spatially uncorrelated two-dimensional textures. By exploiting this connection, we develop mathematical tools that permit the rigorous optimization of grain boundary network structure. Using a specific multi-objective materials design case study involving elastic, plastic and kinetic properties, we illustrate the utility of this texture mediated approach to grain boundary network design. We obtain a microstructure that minimizes grain boundary network diffusivity while simultaneously improving yield strength by an amount equal to half of the theoretically possible range. The theoretical tools developed here could complement experimental grain boundary engineering efforts to help accelerate the discovery of materials with improved performance.
Inorganic oxides exhibit numerous applications influenced by particle size and morphology. While industrial methods for forming oxides involve harsh conditions, nature has the ability to form intricate structures of silicon dioxide (silica) using small peptides and polyamines under environmentally friendly conditions. Recent research has demonstrated that these biomaterials will precipitate other inorganic oxides, such as titanium dioxide (titania). Using the diatom-derived R5 peptide, new peptides with systematic changes (e.g., truncation and substitution) in the R5 primary structure were surveyed for reactivities and the impact on the morphology of the titania. The results demonstrated that (i) basic residues are vital to initiating the reaction, and a minimum local concentration is necessary to sustain the precipitation, (ii) residues containing hydroxyl side chains are important to imparting morphological control on the precipitate, and (iii) buffer conditions can dramatically alter both precipitation and morphology.
A new ultrahigh strength hot rolled Ti–Mo-bearing ferritic steel was developed through chemical composition design and rolling processing optimization. To maximize the potential of nanometer-sized (Ti, Mo)C carbide in terms of strengthening ferrite matrix, the optimal chemical composition of 0.1C–0.2Ti–0.4Mo (wt%) was determined through considering the atomic ratio of elements, the solubility temperature of (Ti, Mo)C in austenite, and the excessive growth critical temperature of austenite grain during reheating. The rolling condition in the region through austenite recrystallization region to austenite nonrecrystallization region was adopted to realize a homogenous and fine ferrite grain structure. Results showed that the simulated coiling at 600 °C was found to provide an attractive combination of ferrite grain refinement hardening (360 MPa) and precipitation hardening (324 MPa). An optimal combination of strength and ductility was achieved after coiling at 600 °C (yield strength: 912 MPa; ultimate tensile strength: 971 MPa; total elongation: 16.0%). In addition, the nanometer-sized (Ti, Mo)C carbide was characterized by transmission electron microscopy (TEM) and physical–chemical phase analysis, and its role was discussed in details.
As the core materials with excellent soft magnetic properties, Fe–6.5 wt% Si steel was fabricated by using the warm rolling process due to its extremely limited ductility and formability at room temperature. In this work, the effects of warm rolling reduction varying from 50% to 85% on the microstructure, texture, and magnetic properties of sheets were explored. The microstructure and texture evolution at the various processing steps were investigated in detail using optical microscopy, electron backscatter diffraction, and transmission electron microscopy. The results demonstrate that the finer recrystallization grains are accompanied with an increasing warm rolling reduction, and the final annealed sheets are characterized by strong α-fiber and γ-fiber textures. Accordingly, on the whole, as the increase of warm rolling reductions, the values of magnetic induction (B8, B50) in the final annealed sheets increase sharply up to a maximum value and then decrease to a certain value, and the values of iron loss (P15/50, P10/400) increase monotonically.
The mechanical behavior of superconductor lamellar-like BaFe2As2 single crystals was investigated at nanoscale by instrumented indentation. The unique responses of the ab- and a(b)c-crystallographic planes were discussed based on their influence in hardness (H) and elastic modulus (E). The results allowed two main conclusions. (i) The choice of testing parameters strongly affected the scaling of mechanical properties on the lamellar surfaces. Lamellar cracking was the leading mechanism of deformation, featuring a brittle-like behavior and affecting considerably H and E. However, the plastic deformation history allowed different elastic–plastic responses on the ab-plane owing to the compaction of the material. Threshold loads for cracking depended on both loading rate and penetration velocity, pointing out to time-dependent plastic deformation mechanisms. (ii) Proper estimates were achieved for H in multiple loading tests [3.4 GPa for ab- and ∼1 GPa for a(b)c-planes], and for E under loads less than 3 mN (∼55 GPa for both planes).