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Nanocrystalline (20 nm) lead magnesium niobate (PMN) powders were prepared via a chemical process. This process involved the addition of aqueous niobium tartrate, lead-ethylenediaminetetraacetic acid, and magnesium-polyvinyl alcohol complex to produce a homogeneous solution. After the complete evaporation of the resulting homogeneous solution, the complexes decomposed and produced a black, fluffy precursor material. The precursor material on calcination up to 850 °C/2 h produced nanocrystalline PMN powders with the corresponding average particle size 20 nm. PMN powders modified with lead iron niobate (PFN) (1 – x)PMN–xPFN (x = 0.1, 0.2, and 1) were also prepared using this route and investigated through x-ray diffraction studies.
Plastic instabilities were investigated by the depth-sensing microhardness test in binary high-purity Al–Mg alloys with different Mg contents. During the tests the applied load was increased from 0 to 2000 mN at constant loading rate. The instabilities appeared as characteristic steps in the load–depth curves during indentation. It was shown that the occurrence and development of the plastic instabilities depend strongly on the solute content. Furthermore, the plastic instabilities occurred only when the solute concentration was larger than a critical value, C0. From room-temperature tests on Al–Mg alloys, C0 was found to be 0.86 wt% Mg. The critical concentration, which is necessary to get plastic instabilities, was also interpreted theoretically.
CeO2-doped YBaCuO monoliths synthesized with a top-seeded melt growth process in a conventional box furnace exhibited values of trapped magnetic field of up to 1.33 T at 77 K. To our knowledge, this is the highest value of trapped field reported for a melt-textured YBaCuO monolith. A suitable temperature profile and the use of high-density Y2BaCuO5 substrates led to reproducible single-domain crack-free samples investigated by optical and scanning electron microscopy and trapped field measurements. The zero-field-cooled levitation forces at 77 K of standard samples amounted to 70–83 N. A transport critical current density of up to 1.3 × 105 A/cm2 in self field at 77 K was obtained.
The B-site cation ordering in Ba(Zn1/3Nb2/3)O3 was studied using a combination of first-principles energy calculations, a cluster expansion technique, and Monte Carlo simulations. Our calculations indicate that the ground state is a 1:2 ordered hexagonal structure, in contrast to x-ray diffraction observations, but consistent with recent Raman work by Kim et al. The order–disorder transition between the 1:2 ordered phase and the cubic perovskite phase is predicted to occur at approximately 2480 K. This prediction indicates that Ba(Zn1/3Nb2/3)O3 in equilibrium should be fully ordered at all practical temperatures. These results indicate that Ba(Zn1/3Nb2/3)O3, previously considered to be disordered, may be ordered on a local scale, consistent with its good microwave characteristics.
Electrodeposition was used to grow epitaxially BaTiO3 thin films on SrTiO3 single-crystal substrates with La0.7Sr0.3MnO3 (LSMO) conducting buffer layers. The epitaxial films appeared to consist of very small (ø10 nm) particles. The film completely covered the substrate when the reaction was performed at temperatures between 60 and 90 °C with LSMO potentials of –0.5 to –1.0 V against a Pt counter-electrode. It appeared that an electrophoretic force, acting on BaTiO3 nuclei within the solution, facilitated the deposition of the film.
Amorphous carbon filaments were synthesized by catalytic pyrolysis of propene over Pd3P colloids. The channel close to the center of the filaments usually contained particles, which were analyzed by analytical electron microscopy to be palladium. The palladium particles could be found anywhere along the filament. The carbon filaments were of two types and of different diameters, about 8–15 nm and about 40–80 nm. The thinner type of filament shows a channel diameter of about 5 nm. The type of filament produced depends on the reaction conditions. Increased reaction time results in a large number of filaments, whereas an increased propene gas flow results in more of the thicker type of filaments.
A new form of transparent condensed nanophase material of GaN was synthesized directly by ammono-thermal synthetic route. Nano-sized effects and thermal stability of that material were investigated through Raman scattering and infrared spectra. Compared with bulk GaN, we observed the Raman low-energy-shift of the phonon frequency of E2(high) and the transverse optical mode [E1(TO)], the infrared high-energy-shift of, ωT, and the variation of relative intensity IE2/E1(TO). These characteristics can be attributed to the existence of the interface effects and the vacancy of N in the GaN nanophase material. This material has a high thermal stability even at 900 °C as indicated through infrared and Raman spectral investigation of annealed samples of as-synthesized nanophase material.
Micropipes in a 6H–SiC semiconductor wafer were studied by scanning electron and atomic force microscopy. The screw dislocations intersecting the wafer's surface were located by etch pitting, and their Burgers vectors determined by x-ray topography. The etch pits were eroded into smooth craters by ion beam etching to expose levels of dislocation line from inside the sample's bulk. There a micropipe's diameter is distant from surface relaxation effects. Hollow cores (micropipes) were observed at the base of the craters whose screw dislocations had Burgers vectors of magnitude three multiples of the c-lattice parameter and higher. Screw dislocations with 1c and 2c Burgers vectors had no associated micropipes.
An allotropic transition from face-centered-cubic (fcc) to hexagonal-close-packed (hcp) Ni(Si) solid solution in Ni95Si5 and Ni90Si10 during nanocrystallization by mechanical alloying is reported. The transformation was identified as a defect-induced melting accompanied by a volume expansion of 8.6% and was observed when fcc Ni(Si) reached a critical crystallite size of 10 nm. Calculation based on equation of state showed that a 37% reduction in tetragonal shear modulus and a negative pressure of about 8.7 GPa were generated at the onset of transformation.
For the first time, we measured Raman spectra from Li(Al1-xCox)O2 (x = 0.5 to 0.9), a new cathode material for lithium batteries. Whereas LiCoO2 sintered at 400 °C develops a spinel structure, Li(Al1-xCox)O2 sintered at 380 °C is amorphous, as shown by its single broad Raman band. Li(Al1-xCox)O2 sintered at 700 or 900 °C shows Raman peaks independent of x that coincide with those from LiCoO2, indicating that Li(Al1-xCox)O2 has the α–NaFeO2 structure (space group R3m). Traces of the impurity phase Co3O4 appear in samples treated at 900 °C but not at 700 °C. The Raman peak widths exceed those in LiCoO2, suggesting that replacement of Co by Al increases disorder among the Li ions.
Epitaxial thin films of LaVO3 were grown on (001) LaAlO3 substrates by pulsed laser deposition from a LaVO4 target in a vacuum ambient at substrate temperatures ≥500 °C. X-ray diffraction studies showed that epitaxial LaVO3 films consist of mixed domains of  and  orientations. Thermoprobe and four-probe conductivity measurements demonstrated the p-type semiconducting behavior of the epitaxial LaVO3 films. The temperature dependence of the conductivity is consistent with a thermally activated hopping mechanism with an activation barrier of 0.16 eV.
Pores in porous 6H–SiC were found to propagate first nearly parallel with the basal plane and gradually change direction and align with the c axis. As a consequence, well-defined columnar pores were formed. It was shown that the rate of change of propagation directions was influenced by the etching parameters, such as hydrofluoric acid concentration and current density. Larger currents resulted in formation of larger pores. Pore sizes were found to increase with depth due to a decrease of the acid concentration. In addition, due to chemical etching effects, larger pore sizes were obtained close to the sample surface.
The microstructure of samples before and after a high current density electropulsing treatment was characterized by using high-resolution transmission electron microscopy. It has been found that in the coarse-grained Cu–Zn alloy subjected to the electropulsing treatment, two nanophases were formed, α–Cu(Zn) and β′–(CuZn), the average grain size of which is about 11 nm. A possible mechanism for the formation of nanophases was proposed. The experimental results indicated that electropulsing, as an instantaneous high-energy input, plays an important role in the nonequilibrium microstructural changes in materials and serves as a potential processing approach to synthesize nanostructured materials.
Ba-filled skutterudite compounds, BayFexCo4−xSb12, were synthesized by a two-step solid reaction method. A binary compound of Sb3Ba and a ternary compound of FexCo1−xSb2 were first synthesized at 900 and 973 K, respectively. The presynthesized Sb3Ba and FexCo1−xSb2 were then mixed with Sb and heated at 973 K in an Ar atmosphere. The resulting powder was of single phase with a composition of BayFexCo4−xSb12, having skutterudite structure with the Sb–dodecahedron voids fractionally filled by Ba. The lattice constant of BayFexCo4−xSb12 increased with Ba and Fe content. The maximum filling fraction of Ba (ymax) in BayFexCo4−xSb12 was found to be greater than that of Ce or La in LnyFexCo4−xSb12, especially in the lower Fe content region. The ymax varied from 0.35 to near 1.0 when Fe content (x) changed from 0 to 4.
An electrolytic process is described to peel off ferroelectric thin films from electroded substrates. This procedure was used to study the evolution of stress in ferroelectric calcium-modified lead titanate thin films. Stresses developed during the different steps of the preparation of the film on the substrate were calculated from curvature radii of the deposited films after each step. During the film preparation, the substrate was permanently deformed by the generated stresses. This was shown by curvature of the substrate after the electrolytic separation of the film. The laminated film liberated a large amount of stresses, as deduced from the lattice parameters of the deposited and laminated film, obtained by x-ray diffraction. The moderate residual stress that the laminated film maintained could be associated with intrinsic defects of the film.
Large, single-grain Y–Ba–Cu–O (YBCO) was fabricated via the infiltration of Ba–Cu–O liquid into a precursor body composed of solid, porous Y2BaCuO5 (Y-211) and observed to trap a magnetic field of 0.15 T at 77 K. In this process a NdBCO seed crystal was used to promote heterogeneous nucleation, which allows the fabrication of single-grain YBCO containing a uniform and very fine distribution of Y-211 inclusions in the YBa2Cu3O7−δ(Y-123) matrix without the addition of Pt. These superior microstructural features and significant field trapping ability compared with samples processed by conventional top-seeded melt growth suggest this technique could be a practical alternative for processing large, single-grain superconductors for engineering applications.
Relationships between melt heat treatment and undercooling of alloy melts were clarified with Bi95Sb5 through four-factor, three-level orthogonal experiments. The results show that the cooling rate plays the most important role in the undercooling of Bi95Sb5 alloy melts. Undercooling as large as 121 K was obtained in the bulk Bi95Sb5 alloy melt. It is presently the highest undercooling of this alloy system. A metastable phase with tetragonal structure was found in the Bi95Sb5 alloy with undercooling of 121 K.
In this work we report a high-tensile ductility in a fully dense bulk nanocrystalline (nc) pure copper sample prepared by electrodeposition. A tensile ductility with an elongation to fracture of 30% was obtained in the nc Cu specimen with an average grain size of 27 nm, which is comparable to that for the coarse-grained polycrystalline Cu. An enhanced yield stress (119 MPa) and a depressed strain hardening exponent (0.22) were observed in the nc Cu sample with respect to the conventional polycrystalline Cu. The high-tensile ductility was attributed to the minimized artifacts in the nc sample, and the grain-boundary sliding deformation mechanism resulted from the numerous amount small-angle grain boundaries and the low microstrain (dislocation density).
The local mechanical properties of silica-reinforced silicone composites were investigated using a modified atomic force microscopy technique. Elastic modulus measurements (1.5 ± 0.1 MPa) are consistent with bulk measurements (1.9 MPa), and changes in the modulus at the surface of the composite samples (E = 1.5 to 3.5 MPa) were observed as a result of α-irradiation (dose = 1.7 × 1010 to 2.0 × 1012 α/cm2). The sensitivity of the technique was demonstrated by a detectable change in modulus at even the small dose of 1.7 × 1010 α/cm2. The penetration depth of the α-particles into the material, estimated to be 22 ± 2 μm from the sample edge, was determined by cross-section depth profiling; and modeling of the ion penetration depth using transport of ions in matter codes (24.4 ± 0.4 μm) closely matched experimental observations.