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Coating of nanowires is being investigated to broaden potential uses for future applications. Coatings of Ni and Pt nanoparticles have been synthesized on silicon carbide nanowires by plasma enhanced chemical vapor deposition. Coatings with high particle densities with average particle diameters of 2.76 and 3.28 nm for Pt and Ni, respectively, were formed with narrow size distributions. Plasma enhanced chemical vapor deposition appears to be an efficient method for production of metal coatings on nanowires.
We describe a two-step dealloying/compaction process to produce nanocrystalline Au. First, nanocrystalline/nanoporous Au foam was synthesized by electrochemically driven dealloying. The resulting Au foams exhibited porosities of ∼60% with pore sizes of 40 and 100 nm and a typical grain size of <50 nm. Second, the nanoporous foams were fully compacted to produce nanocrystalline monolithic Au. The compacted Au was characterized by transmission electron microscopy and x-ray diffraction and tested by depth-sensing nanoindentation. The compacted nanocrystalline Au exhibited an average grain size of <50 nm and hardness values ranging from 1.4 to 2.0 GPa, which were up to 4.5 times higher than the hardness values obtained from polycrystalline Au.
High-resolution transmission electron microscopy studies of hydrothermally derived platelike lead titanate nanoparticles reveal that below a critical size of approximately 70 nm, the single ferroelectric domain polarization axis reorients from perpendicular to parallel to the plate. We suggest that during particle growth, ions in the hydrothermal processing medium compensate for the ferroelectric depolarization energy. When the processing medium is removed by washing and drying, single domain nanoparticles minimize their depolarization energy by c-axis flipping.
We report a new compression shearing method for the production of bulk amorphous materials. In this study, amorphous Nd–Fe–B melt-spun ribbons were successfully consolidated into bulk form at room temperature by the compression shearing method. X-ray diffraction and transmission electron microscopy studies revealed that the amorphous structure was well maintained in the bulk materials. The resultant bulk materials exhibited the same magnetic properties as the original amorphous Nd–Fe–B materials.
Transparent ceramic scintillators of La2Hf2O7:Ti4+ were developed by a novel combustion synthesis method. The optical transmittance for a 1.0-mm-thick specimen is about 60% of the incident light, and the x-ray stopping power is also quiet high. The broad emission band centered at 475 nm originates from the oxide-Ti4+ charge-transfer transitions, which renders fast decay time on the order of 10 μs. The highest relative light output has reached about 1.5 times that of Bi4Ge3O12 (BGO) single crystal when excited by 120 kV x-rays.
Microstructures in the thin film of La0.8Sr0.2MnO3 grown on (100) SrTiO3 by laser molecular beam epitaxy were characterized by transmission electron microscopy. Highly dense and dimensionally uniform nano-agglomerates were found embedded in thin film of La0.8Sr0.2MnO3. High-angle angular dark-field imaging, elemental mapping, and compositional analysis revealed that the nano-agglomerates are rich in manganese and poor in lanthanum. The ratio of Mn/La in the nano-agglomerates fluctuates. A salient feature of this compositional fluctuation within the nanoscale isthe formation of cubic MnO phase, which appears as the core of the nano-agglomerates.The La0.8Sr0.2MnO3 film is domain-oriented and two domains were identified on the basis of orthorhombic lattice. The orientation relationships between La0.8Sr0.2MnO3 domains and MnO were determined as LSMO,1//MnO and (100)LSMO,1//(110)MnO; LSMO,2//MnO and (010)LSMO,2//(100)MnO. The domain structuresand compositional inhomogeneities within nanoscale result in a textured microstructure, which is one of the most important parameters for tuning electronic properties in colossal magnetoresistance oxides.
This work represents an attempt to understand the nature of micron and attrition milled nano-sized titanium powders on two different aspects, i.e., pressure-induced phase change and thermal expansion. Contraction in the volume of unit cell in terms of decrease in interplaner spacing (d) has been observed in both powders and tends to restore upon annealing. At a given pressure, nano titanium shows a smaller decrease in d relative to micron titanium. The stress analysis of the compacts indicates higher value of residual stresses and deformations in micron powder than in nano powder. The dilatometric study reveals, first, the release of internal stresses and entrapped gases causes huge expansion in nanopowder compacts during heating. Secondly, there is no significant difference in the expansion coefficients of sintered micro- and nanocrystalline titanium samples.
We investigated adsorption and dissociation of water and HfCl4 on a Ge/Si(100) −(2 × 1) surface with a density-functional theory. The Si–Ge and Ge–Ge homodimers are used to represent the Si1−xGex surface. (i) Water first adsorbs on the bare Ge/Si(100) − (2 × 1) surface and then dissociates into OH and H. The activation energy for adsorption of water on the Ge–Ge homodimer is much higher than that on the Si–Ge heterodimer. (ii) HfCl4 dissociates upon adsorption on the Ge/Si(100) − (2 × 1) surface into HfCl3 and Cl. No net activation barrier exists during the adsorption of HfCl4 on both SiGe surface dimers. The molecular adsorption state is found to be metastable according to the calculation, which implies that the reaction tends to move toward to the product rather than trapping in HfCl4 adsorbed state. The difference in the potential energy surface between reactions on Si–Ge and Ge–Ge dimers is due to different bond strengths.
The syntheses of modified ortho or meta methylbenzoic acid by (3-aminopropyl)triethoxysilane and the preparation of their corresponding organic–inorganic molecular-based hybrid material with the two components equipped with covalent bonds are described. The organic part is a derivative of methyl benzoic acid, which is used to coordinate to Tb3+ and further introduced into silica matrices by Si–O bonds after hydrolysis and polycondensation processes. The Judd–Ofelt theory proves that covalency increases along with increasing reciprocal energy difference between the 4fN and 4fN−15d1 configurations. Ultraviolet absorption, phosphorescence spectra, and luminescence spectra were applied to characterize the photophysical properties of the obtained hybrid material, and the above spectroscopic data reveal that the triplet energy of modified methyl benzoic acid matches with the emissive energy level of Tb3+. In this way, the intramolecular energy transfer process took place within these molecular-based hybrids, and strong green emission of Tb3+ was obtained.
Explosive shock compaction was used to consolidate powders obtained from melt-spun Pr2Fe14B/α–Fe nanocomposite ribbons, to produce fully dense cylindrical compacts of 17–41-mm diameter and 120-mm length. Characterization of the compacts revealed refinement of the nanocomposite structure, with approximately 15 nm uniformly sized grains. The compact produced at a shock pressure of approximately 1 GPa maintained a high coercivity, and its remanent magnetization and maximum energy product were measured to be 0.98 T and 142 kJ/m3, respectively. The compact produced at 4–7 GPa showed a decrease in magnetic properties while that made at 12 GPa showed a magnetic softening behavior. However, in both of these cases, a smooth hysteresis loop implying exchange coupling and a coercivity of 533 kA/m were fully recovered after heat treatment. The results illustrate that the explosive compaction followed by post-shock heat treatment can be used to fabricate exchange-coupled nanocomposite bulk magnets with optimized magnetic properties.
In the relationship between unloading contact stiffness, elastic modulus, and contact area, which is the fundamental basic equation for nanoindentation analysis, a multiplicative correction factor is generally needed. Sometimes this correction factor is called γ to take into account the elastic radial inward displacements, and sometimes it is called β to correct for the fact that the indenter shape is not a perfect cone. In reality, these two effects simultaneously coexist and thus it is proposed that this correction factor is α = βγ. From nanoindentation data measured on three materials of different elastic moduli with a sharp Berkovich indenter and a worn one, the tip of which was blunt, it is demonstrated that the correction factor α does not have a constant value for a given material and indenter type but depends on the indenter tip rounding and also on the deformation of the indenter during indentation. It seems that α increases with the tip radius and also with the elastic modulus of the measured materials.
A family of microporous phases with compositions Na2Nb2−xTixO6−x(OH)x⋅H2O (0 ≤ x ≤ 0.4) transform to Na2Nb2−xTixO6−0.5x perovskites upon heating. In this study, we have measured the enthalpies of formation of the microporous phases and their corresponding perovskites from the constituent oxides and from the elements by drop solution calorimetry in 3Na2O·4MoO3 solvent at 974 K. As Ti/Nb increases, the enthalpies of formation for the microporous phases become less exothermic up to x = ∼0.2 but then more exothermic thereafter. In contrast, the formation enthalpies for the corresponding perovskites become less exothermic across the series. The energetic disparity between the two series can be attributed to their different mechanisms of ionic substitutions: Nb5+ + O2− → Ti4+ + OH− for the microporous phases and Nb5+ → Ti4+ + 0.5VO.. for the perovskites. From the calorimetric data for the two series, the enthalpies of the dehydration reaction, Na2Nb2−xTixO6−x(OH)x⋅H2O → Na2Nb2−xTixO6−0.5x + H2O, have been derived, and their implications for phase stability at the synthesis conditions are discussed.
Catalytic synthesis of spindle-type hematite particles was studied for the first time under the conditions of boiling reflux and pH values ranging from 4 to 7, using Fe2(SO4)3 and NaOH as raw material, a trace amount of FeSO4 as the catalyst, and NaH2PO4 as the growth-regulating agent. The final products were characterized by x-ray diffraction, high-resolution electron microscopy, scanning electron microscopy, and Fourier transform infrared techniques. Primarily, the catalytic effect of ferrous ion on the conversion of ferric hydroxide was investigated. It was found that the addition of a trace amount of ferrous ion promoted fast conversion of ferric hydroxide and remarkably accelerated the transformation process to hematite. The reaction conditions affecting the conversion rate and morphologies in the presence of trace amount of ferrous ion were investigated. The final particles prepared had the characteristics of controlled size, a narrow particle size distribution, and good reproducibility.
We investigated a new method of ceramic-to-metal joining, referred to as reactive air brazing, as a potential method of sealing ceramic components in high-temperature electrochemical devices. Sessile drop wetting experiments and joint strength testing were conducted using yttria stabilized zirconia (YSZ) substrates and CuO–Ag-based air brazes. Results from our studies indicate that the wettability of the braze improves substantially with increasing CuO content, over a compositional range of 1–8 mol% CuO, which is accompanied by an increase in the bend strength of the corresponding brazed YSZ joint. The addition of a small amount of TiO2 (0.5 mol%) to the CuO–Ag braze further improves wettability due to the formation of a titanium zirconate reaction product along the braze/substrate interface. However, with one notable exception, the bend strength of these ternary braze joints remained nearly identical to those measured in comparable binary braze joints. Scanning electron microscopy analysis conducted on the corresponding fracture surfaces indicated that in the binary braze joints, failure occurs primarily at the braze/YSZ interface. Similarly in the case of the ternary, TiO2-doped brazes joint failure occurs predominantly along the interface between the braze filler metal and the underlying titanium zirconate reaction layer.
We report on photoreduction of Ag+ in aluminoborate glasses induced by irradiation of a femtosecond laser. Novel fluorescence was observed in the femtosecond laser irradiated glass when excited by a 365 nm ultraviolet lamp. Optical absorption, emission, and electron spin resonance spectra of the glass samples demonstrated that after the laser irradiation, portions of silver ions near the focused part of the laser beam inside the glass were reduced to silver atoms, which resulted in the formation of the characteristic fluorescence. The observed phenomenon may have promising applications in the fabrication of functional optical devices.
Continuous miniaturization of solder joints in high-density packaging makes it important to study how the joint size could affect the solder microstructure and thereby the subsequent in-service reliability. In this study, a printed circuit board with electroless nickel immersion gold (i.e., Au/Ni–P) over Cu bond pads of size approximately ∼80 μm and ∼1500 μm in diameter was dipped into a Sn–3.5Ag solder bath. The study shows that the smaller bumps, which cool more quickly, include much finer Ag3Sn particles. In addition, substantial differences in the thickness of the interfacial intermetallics and the microstructure for different dipping times are observed for different bump sizes. The results from a combined thermodynamic–kinetic model also suggest that the solder bump geometry can influence the dissolution kinetics of the pad metal into the molten solder and therefore the microstructure at the solder-pad interface and within the bulk solder.
The particle size and shape effects of starting raw powders on the synthesis of aluminum nitride by combustion reaction technique were investigated with four sizes of AlN powder as diluent and two shapes of Al powder as reactant. It was found that the structure of beds of starting particles significantly affected the pore channels for nitrogen gas accessibility into a mixture compact and the passages for combustion wave propagation through particles, resulting in changes of AlN product morphology and purity. Through control of the starting particle size and shape, high-purity (over 98%) AlN products several tens of microns in size were synthesized.
The early dissolution behavior of Cu in a molten Sn–Zn–Ag solder was studied at 250 °C by fast quenching the dissolving specimen in liquid nitrogen. The atomic level dissolution behavior of Cu in the molten solder was revealed by high-resolution transmission electron microscopy. The dissolution of Cu occurs through channel dissolution and thermal vibrational dissolution. The dissolution channel has a dimension of less than 0.5 nm. The formation of channels, and thus the channel zone, is initiated by preferential removal of Cu atoms from the surface vacant site of Cu lattice. Relict strips of lattice between channels subsequently dissolve into the molten solder with the aid of thermal vibration and the interaction with liquid Zn atoms. The dissolved atoms form an atomic cluster zone. These clusters are the intermediate state of the dissolution of Cu from the channel zone into the molten Sn–Zn–Ag solder. The clusters convert into an amorphous structure prior to further formation of compound.
Porous Al2O3/Al catalyst supports were fabricated using a mixture of Al(OH)3 and Al powders, followed by pressureless sintering at a temperature of 600 °C in vacuum. Different pressures were used to prepare green compacts. High compaction pressure led to a high surface area and good mechanical and electrical properties for the sintered specimens. However, when the Al content in the sintered specimen exceeded a definite value, high compaction pressure decreased the surface area abruptly. Scanning electron microscopy observations revealed that agglomeration in the starting mixture has a significant effect on the microstructure of the sintered specimens. High compaction pressure greatly eliminated the agglomerates and led to a uniform microstructure for the sintered specimens. However, when the Al content in the starting mixture was too high, Al particles in the compacts prepared by the high pressure were largely sintered due to the high compact density so that most of the pores were closed. The present study indicates that a suitable compaction pressure is critical to obtaining superior Al2O3/Al supports.
Hybrid organic–inorganic nanoporous thin-film glasses are extremely fragile and prone to stress-corrosion cracking in reactive environments. This has limited their integration as ultra low dielectric constant layers in high density integrated circuits. We demonstrate how crack growth is influenced by non-buffered aqueous solutions and show that with increasing pH, crack-growth rates are significantly accelerated. Interestingly, a crack growth regime limited by the transport of hydroxide ions to the crack tip was observed. Existing models commonly used to predict crack growth are shown to over estimate the experimental data by 6 orders of magnitude. We rationalize this behavior in terms of a significant difference in the crack tip solution chemistry as compared to that of the bulk and propose both chemical reaction and transport mechanisms to support this hypothesis.