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We developed a new Cu–Zn wetting layer for Pb-free solders. By adding Zn to the Cu wetting layer, intermetallic growth in the Sn–Ag–Cu (SAC) solder interfaces was delayed. Cu3Sn intermetallic compounds and microvoids were not observed in the SAC/Cu–Zn interfaces after aging. The drop reliability of the SAC solder/Cu–Zn joints was excellent.
The thermal coarsening of nanoporous Au was examined and compared with the thermal instability of Au nanoparticles. The nanoporous Au was coarsened at temperatures far below the melting temperature of Au nanoparticles, which possess sizes similar to the nanoligaments. Differential scanning calorimetry characterization of nanoporous Au exhibited an exothermal peak around 470 K. These results suggest that solid-state process like recrystallization, rather than melting, is responsible for the thermal coarsening of nanoporous Au.
The solid-phase epitaxial growth kinetics of amorphized (011) Si with application of in-plane uniaxial stress to magnitude of 0.9 ± 0.1 GPa were studied. Tensile stresses did not appreciably change the growth velocity compared with the stress-free case, whereas compression tended to retard the growth velocity to approximately one-half the stress-free value. The results are explained using a prior generalized atomistic model of stressed solid-solid phase transformations. In conjunction with prior observations of stressed solid-phase epitaxial growth of (001) Si, it is advanced that the activation volume tensor associated with ledge migration may be substrate orientation-dependent.
Cr3+/Ni2+ co-doped optically transparent magnesium aluminosilicate glass-ceramics containing MgAl2O4 nanocrystals have been prepared by heat-treatment. Greatly enhanced broadband near-infrared emission centered at 1216 nm in Cr3+/Ni2+ co-doped glass ceramics is observed when compared with the Ni2+ single-doped glass ceramics under 532 nm excitation. The observed enhancement of infrared emission is attributed to the energy transfer from Cr3+ to Ni2+ ions in the nanocrystalline phase, which leads to the emission due to 3T2(3F) → 3A2(3F) transition of octahedral Ni2+ ions.
Bulk metallic glasses (BMGs) with high thermal stability and good corrosion resistance were synthesized in the (Cu0.6Hf0.25Ti0.15)100−x−yNiyNbx system by copper mold casting. The addition of Ni element causes an extension of a supercooled liquid region (ΔTx = Tx – Tg) from 60 K for Cu60Hf25Ti15 to 70 K for (Cu0.6Hf0.25Ti0.15)95Ni5. The simultaneous addition of Ni and Nb to the alloy is effective in improving synergistically the corrosion resistance in 1 N HCl, 3 mass% NaCl, and 1 N H2SO4 + 0.01 N NaCl solutions. The highly protective Hf-, Ti-, and Nb-enriched surface film is formed by the rapid initial preferential dissolution of Cu and Ni, which is responsible for the high corrosion resistance of the alloys in the solutions examined.
This paper reports on the preparation and characterization of nickel ferrite (NiFe1.98O4) ceramics doped with Bi2O3 as sintering aid. Focus has been on the effects of concentration of Bi2O3 and sintering temperature on the densification, grain growth, dielectric, and magnetic properties of the NiFe1.98O4 ceramics, with an aim at developing magnetodielectric properties, with almost equal real permeability and permittivity, as well as sufficiently low magnetic and dielectric loss tangents, over 3 to 30 MHz (high frequency or HF band). X-ray diffraction results indicated that there is no obvious reaction between NiFe1.98O4 and Bi2O3, at Bi2O3 levels of up to 7 wt% and temperatures up to 1150 °C. The addition of Bi2O3 facilitated a liquid phase sintering mechanism for the densification of NiFe1.98O4 ceramics. The addition of Bi2O3 not only improved the densification but also promoted the grain growth of NiFe1.98O4 ceramics. To achieve sufficiently low dielectric loss tangent, the concentration of Bi2O3 should not be less than 5 wt%. The low dielectric loss tangents of the samples doped with high concentrations of Bi2O3 can be attributed to the full densification of the ceramics. Magnetic properties of the NiFe1.98O4 ceramics, as a function of sintering temperature and Bi2O3 concentration, can be qualitatively explained by the Globus model. Promising magnetodielectric properties have been obtained in the sample doped with 5% Bi2O3 and sintered at 1050 °C for 2 h. The sample has almost equal values of permeability and permittivity of ∼12, together with low dielectric and magnetic loss tangents, over 3 to 30 MHz. This material might be useful for the miniaturization of HF (3 to 30 MHz) antennas.
Lamellar liquid crystal (Lα) was formed by room temperature ionic liquid [Bmim]PF6, nonionic surfactant Tween 85, and H2O. The microstructure of this lamellar liquid crystal was investigated by small angle x-ray diffraction (SAXD) and 2H NMR (nuclear magnetic resonance). Ag nanoparticles with relatively uniform dispersion were prepared successfully in this Lα phase. The rheological and lubrication properties of the Lα phase and the Lα/Ag nanoparticle mixed system were also investigated. The results showed that the structure strength, anti-wear capacity, and lubrication properties of the Lα phase were enhanced with an increasing amount of Tween 85, but were impaired with an increasing amount of H2O. Increasing the amount of [Bmim] PF6 could also make the structural strength weaker, but the lubrication properties of the system were improved because of the inherent lubrication properties of ionic liquid. The presence of the Ag nanoparticles in the lamellar phase could also enhance the structural strength, anti-wear capacity, and lubrication properties.
A method is presented for recognition of nanograins in high-resolution transmission electron microscope (HRTEM) images of nanocrystalline materials. We suggest a numerical procedure, which is similar to the experimental dynamic hollow cone dark-field method in transmission electron microscopy and the annular dark-field method in scanning transmission electron microscopy. The numerical routine is based on moving a small mask along a circular path in the Fourier spectrum of a HRTEM image and performing at each angular step an inverse Fourier transform. The procedure extracts the amplitude from the Fourier reconstructions and generates a sum picture that is a real space map of the local amplitude. From this map, it is possible to determine both the size and shape of the nanograins that satisfy the selected Bragg conditions. The possibilities of the method are demonstrated by determining the grain size distribution in gadolinium with ultrafine nanocrystalline grains generated by spark plasma sintering.
The MBS (mung bean sprouts) vegetal system, with its high penetrability, high selectivity, and space restriction, was explored to control nanocrystal synthesis. We found that the inside and outside of MBS have different structures and ion transformation properties. Two nanocrystals with distinct morphology, the nanorod and the nanosphere, were grown on the outer surface and the inner stem wall of MBS, respectively. The two XWO4 (X = Ca,Sr,Ba) nanocrystals were characterized by scanning electron microscopy (SEM), x-ray diffraction (XRD), and Fourier transform infrared (FTIR). The FTIR spectra of nanoproducts were different from bulk products due to the nano-size effect. A presumable mechanism was also determined. This work benefits the application of nanotungstates.
Nearly monodisperse Ag nanoparticles capped with octadecylamine were prepared by direct thermal decomposition of silver nitrate in octadecylamine. Then the “oriented attachment” assembly process of these monodisperse nanoparticles was exhibited by exchanging the organic capping ligands, and Ag short nanorods capped with dodecanethiol could be obtained as a result. The composition of Ag was analyzed by x-ray diffraction, and the morphological change from nanoparticle to short-nanorod was examined by transmission electron microscopy. Moreover, we also propose a probable mechanism for this transformation process.
The glass formation in Fe-rich ternary Fe-B-Nd and quaternary (Fe,B,Nd)96Nb4 alloys has been studied and the best ternary and quaternary glass formers are located at Fe67B23Nd10 and (Fe68B25Nd7)Nb4 with critical diameters of 1 and 4 mm, respectively. For (Fe,B,Nd)96Nb4 alloys, the competing phases with glass were identified by monitoring the microstructure change. Fe14Nd2B was discovered to be one competing phase, which is the principle magnetic phase for Nd-Fe-B hard magnets. Composites with uniformly distributed Fe14Nd2B were formed for quaternary alloys with a diameter of 1.5 to 3 mm. Bulk hard magnets could be obtained by directly annealing the composites in a compositional area. A hard magnet with a coercivity of 1,100 kAm−1 and a maximum energy product, (BH)max, of 33 kJm–3 was obtained at (Fe67B23Nd10)96Nb4 by annealing. The combination of hard magnetic properties and the large critical sample size may make these alloys a commercially viable candidate for industrial applications.
Nanostructural characterizations of liquid metal–organic precursors-derived cobalt-doped amorphous silica (Si–Co–O) membranes supported on a mesoporous anodic alumina capillary (MAAC) tube were performed to study their unique high-temperature hydrogen gas permeation properties. Cross-sectional scanning transmission electron microscopy images and selected-area electron diffraction patterns indicated that the metal cobalt and the different oxidation states of cobalt oxides (CoO and Co3O4) nanocrystallites having a size range of 5–20 nm were in situ formed in the mesopore channels of the MAAC tube. In addition, high-resolution transmission electron microscopy micrographs and electron energy loss spectroscopy elemental mapping images indicated that the highly dense Co-doped amorphous Si–O formed within the mesopore channels of the MAAC tube. These nanostructural features could contribute to the hydrogen-selective permeation properties observed for the membranes.
In a previous paper, we have demonstrated that a microcrystalline copper film well bonded to a polymer substrate can be stretched beyond 50% without cracking. The film eventually fails through the coevolution of necking and debonding from the substrate. Here we report much lower strains to failure (approximately 10%) for polymer-supported nanocrystalline metal films, the microstructure of which is revealed to be unstable under mechanical loading. We find that strain localization and deformation-associated grain growth facilitate each other, resulting in an unstable deformation process. Film/substrate delamination can be found wherever strain localization occurs. Therefore, we propose that three concomitant mechanisms are responsible for the failure of a plastically deformable but microstructurally unstable thin metal film: strain localization at large grains, deformation-induced grain growth, and film debonding from the substrate.
Fundamental knowledge on the oxidation behavior of pure indium, commonly used as a low-temperature, fluxless soldering material in micro-electro-mechanical system (MEMS) devices, is of importance as it influences the solder joint reliability. A thermodynamic model of the oxidation and reduction behavior of indium is developed by constructing an Ellingham diagram, and by using H2(g) reactions. Partial pressure (p) of H2O was shown to be the critical parameter in creating a reducing environment in the applicable solder reflow temperature range. Verification of the thermodynamic models was then carried out through heating and melting of indium in controlled glove box environments by adjusting p(H2)/p(H2O). The nanometer scale thickness of the oxide layer grown on indium was measured by a spectroscopic ellipsometer. The growth mechanism for oxidation in air below 220 °C follows Uhlig's logarithmic law where electron transport is the rate-controlling mechanism, implying that there is an incubation period for the onset of initial oxidation. Its activation energy was found to be 0.65 eV.
We have fabricated La0.6Ca0.4MnO3 periodic arrays exhibiting tunable optical properties and magnetic properties using nontoxic and environmentally friendly electron beam resist made from La0.6Ca0.4MnO3 sol-gel precursor. We studied their unique optical properties by using the spectral microreflectometer and their magnetic properties using the superconducting quantum interference device and magnetic force microscopy. Additionally, the resist has the ability to demonstrate both positive and negative resist behaviors depending on the electron beam dosage. With these special characteristics, we can fabricate periodic structure on a thin film possessing controlled optical reflectance properties with one fixed design electron beam pattern without changing the structural parameters but changing the electron beam dosage only. Our approach provides an uncomplicated route for the fabrication of nanometer scale magnetic patterns, which serve as the building blocks in the search for novel properties of periodic magnetic arrays.
A combined experimental/numerical approach was developed to determine the distribution of current density, temperature, and stress arising within the sample during spark plasma sintering (SPS) treatment of zirconium carbide (ZrCx) or oxycarbide (ZrCxOy). Stress distribution was calculated by using a numerical thermomechanical model, assuming that a slip without mechanical friction exists at the interfaces between the sample and the graphite elements. Heating up to 1950 °C at 100 °C min−1 and a constant applied pressure of 100 MPa were retained as process conditions. Simulated temperature distributions were found to be in excellent agreement with those measured experimentally. The numerical model confirms that, during the zirconium oxycarbide sintering, the temperature measured by the pyrometer on the die surface largely underestimates the actual temperature of the sample. This real temperature is in fact near the optimized sintering temperature for hot-pressed zirconium oxycarbide specimens. It is also shown that high stress gradients existing within the sample are much higher than the thermal ones. The amplitude of the stress gradients was found to be correlated with those of temperature even if they are also influenced by the macroscopic sample properties (coefficient of thermal expansion and elastic modulus). At high temperature, the radial and angular stresses, which are much higher than the vertical applied stress, provide the more significant contribution to the stress-related driving force for densification during the SPS treatment. The heat lost by radiation toward the wall chambers controlled both the thermal and stress gradients.
To understand the mechanism of the coercivity enhancement by a trace addition of Cu in Nd-Fe-B sintered magnets, we investigated the microstructure difference between Cu-doped and Cu-free alloys using high resolution scanning electron microscopy (HRSEM), transmission electron microscopy (TEM), and laser assisted three dimensional atom probe (LA-3DAP). From a serial sectioning back scattered electron (BSE) images of the Nd-rich phase obtained by an integration of the focused ion beam (FIB) and HRSEM technique, it was found that Cu addition leads to a continuous formation of Nd-rich thin layers along the grain boundaries. 3DAP analysis has shown that a thin Cu-rich layer with a thickness of approximately 2 nm is present at the interface between the Nd2Fe14B and Nd-rich phase grains.
Irreversible or plastic deformation in bone is associated with both permanent plastic strain as well as localized microdamage. Whereas mechanisms at the molecular and mesoscopic level have been proposed to explain aspects of irreversible deformation, a quantitative correlation of mechanical yielding, microstructural deformation, and macroscopic plastic strain does not exist. To address this issue, we developed and applied a two-dimensional image correlation technique to the tensile deformation of bovine fibrolamellar bone, to determine the spatial distribution of strain fields at the length scale of 10 μm to 1 mm in bone during irreversible tensile deformation. We find that tensile deformation is relatively homogeneous in the elastic regime and starts at the yield point, showing regions of locally higher strain. Multiple regions of high deformation can exist at the same time over a length scale of 1 to 10 mm. Macroscopic fracture always occurs at one of the locally highly deformed regions, but the selection of which region cannot be predicted. Locally, strain rates can be enhanced by a factor of 3 to 10 over global strain rates in the highly deformed zones and are lower but always positive in all other regions. Light microscopic imaging shows the onset of structural “banding” in the regions of high deformation, which is most likely correlated to microstructural damage at the inter- and intrafibrillar level.
The thermoelectric properties of Nb-doped Zn4Sb3 compounds, (Zn1–xNbx)4Sb3 (x = 0, 0.005, and 0.01), were investigated at temperatures ranging from 300 to 685 K. The results showed that by substituting Zn with Nb, the thermal conductivities of all the Nb-doped compounds were lower than that of the pristine β-Zn4Sb3. Among the compounds studied, the lightly substituted (Zn0.995Nb0.005)4Sb3 compound exhibited the best thermoelectric performance due to the improvement in both its electrical resistivity and thermal conductivity. Its figure of merit, ZT, was greater than the undoped Zn4Sb3 compound for the temperature range investigated. In particular, the ZT of (Zn0.995Nb0.005)4Sb3 reached a value of 1.1 at 680 K, which was 69% greater than that of the undoped Zn4Sb3 obtained in this study.
We present a blunt mechanism to explain the serrated flow behavior and slight “work hardening” at the beginning of yielding during the compression of metallic glass, which is in line with the piling-up of parallel shear bands on the fracture surface with a gradually increasing space from the edge of surface to inside. Meanwhile, two intrinsic parameters, i.e., strength intensity of blunt behavior, , and global work-hardening sensitivity exponent, , are introduced to characterize the blunt effect on the net increase in flow stress or work-hardening behavior of metallic glass.