Ni–P deposits of amorphous, nanocrystalline, and mixed structures were prepared by electroless deposition. The three deposits were hypoeutectic Ni–P alloys with different P concentrations. The overall transformation sequences of the deposits during post-deposition annealing were investigated using differential scanning calorimetry, x-ray diffraction, and transmission electron microscopy. It was found that there existed three heat-release peaks in a mixed-structure deposit during annealing. The first peak came from the precipitation of Ni nanocrystallites from an amorphous matrix, the second peak resulted from the decomposition of the retained amorphous matrix into Ni + Ni3P having a composition close to the eutectic point, and the third peak, newly found in hypoeutectic Ni–P alloys, was assumed to be caused by both grain growth and the precipitation of Ni3P from as-deposited supersaturated Ni(P) nanocrystals interspersed within the amorphous matrix. By comparing the transformation sequences of the amorphous deposit with that of the nanocrystalline deposits, it was concluded that the transformation sequence of the mixed-structure deposit was a superimposition of those of both the amorphous and nanocrystalline deposits.

In this work, the oxide structures of three polycrystalline copper grades, unalloyed oxygen-free (OF) copper and alloyed CuAg and deoxidized high-phosphor (DHP) copper, were studied using cross-sectional analytical transmission electron microscopy (AEM) samples. The oxidation treatments were carried out in air at 200 and 350 °C for different exposure times. The detailed oxide layer structures were characterized by AEM. At 200 °C, a nano-sized Cu2O layer formed on the all copper grades. At 350 °C, a nano-sized Cu2O layer formed first on the all copper grades. After longer exposure time at 350 °C, a crystalline CuO layer grew on the Cu2O layer of the unalloyed OF-copper. In the case of the alloyed CuAg- and DHP-copper, a crystalline and columnar shaped layer, consisting of Cu2O and CuO grains, formed on the nanocrystalline Cu2O layer. At 350 °C, the unalloyed copper oxidized notably slower than the alloyed coppers, and its oxide structures were different than those of the alloyed coppers.

The mechanical properties of thin films are frequently evaluated using nanoindentation. The finite element method (FEM) is very effective for investigating the stress and strain fields of the film–substrate system during nanoindentation. However, the role of residual stress and the thin interlayer between the film and substrate is not well known, especially when the hard coating/interlayer/soft substrate are considered together. In this work, the FEM is used to investigate the load-displacement behavior of the hardness of the hard coating/interlayer/soft substrate system. The load–displacement process is simulated, and the effects of different residual stresses and interlayer thicknesses are discussed.

InTaO4 is an efficient visible-light photocatalyst, which used to be synthesized by solid-state fusion at over 1100 °C. However, irregular morphology and severe agglomeration of particles were acquired due to nonuniform fusion of solid precursors. In this study, InTaO4 was synthesized by two sol-gel routes, the thermal hydrolysis and esterification methods. The precursors were indium (III) nitrate pentahydrate [In(NO3)3] and tantalum(V) butoxide [Ta(OC4H9)5] dissolved in solutions. The InTaO4 powders with a uniform grain size of 17.7 nm were successfully synthesized using the esterification method at a calcination temperature of 950 °C. A uniform InTaO4 thin film nearly 40 nm thick formed on an optical fiber at 1100 °C using the sol prepared by the esterification method. For the first time, InTaO4 was evaluated by the photocatalytic activity of CO2 photo reduction, which was conducted in aqueous solution under visible light irradiation. Cocatalyst NiO was loaded on the surface of InTaO4 to further enhance the methanol yield. The methanol yields of NiO/InTaO4 by esterification method were significantly higher than those by solid-state fusion. The esterification method provided homogeneous mixing of Ta(OC4H9)5 and In(NO3)3, resulting in nano-sized InTaO4 with uniform crystallinity and superior photocatalytic activity.

Three common Al–Au intermetallics, Al2Au, AlAu2, and AlAu4, were oxidized in the air and characterized using x-ray photoelectron spectroscopy in terms of the elemental chemical state. It was found that there is an increasing trend of oxidation in these intermetallics as the Au content increases. AlAu4 shows the greatest tendency to oxidize with two extra peaks appearing on the Au 4f spectra after long exposure time in air. The surface of AlAu2, although fully oxidized, reveals only one Au 4f peak shift as depth increases. Al2Au was the least oxidizing compound, and the oxide is thin. The binding energies of Al 2p and Au 4f peaks were measured and reported. The Au atoms trapped in the oxide layers exhibit higher binding energy emissions compared to those of elemental Au.

A comparison of microcompression and microtensile methods to study mechanical properties of electrodeposited nanocrystalline (nc) nickel has been performed. Microtensile tests that probe a volume of more than 2 × 106 μm3 show reasonable agreement with results from microcompression tests that probe much smaller volumes down to a few μm3. Differences between the two uniaxial techniques are discussed in terms of measurements errors, probed volume and surface effects, strain rate, and influence of stress state. Uniaxial solicitation in compression mode revealed several advantages for studying stress–strain properties.

Temperature-dependent photoluminescence (PL) spectra were measured to characterize the In-doped cadmium zinc telluride (CdZnTe, or CZT) crystals along the growth direction in the range of 10 to 60 K. High-resistivity CZT samples with 1.2 ppm In dopant at the tip and low-resistivity samples with 60 ppm In dopant at the heel have been assessed. The PL intensity quenching of D0X were fitted with two activation energies for high-resistivity CZT sample and only one activation energy for low-resistivity sample, respectively, suggesting different recombination mechanisms. The C-line was observed in the PL spectra of low-resistivity CZT sample and considered to the results of the isoelectronic complexes, InCd–VCd–InCd, while in high-resistivity CZT sample, shallow donor accepted pair (DAP) transition was identified, and thought to be related to InCd–VCd. The A-center in PL spectra was observed in low-resistivity CZT sample, which is indicative of more cadmium vacancies. It turns out that indium in low-resistivity CZT sample has not been doped as efficiently as in high-resistivity CZT sample because of the self-compensation.

Fe-encapsulating carbon nano onionlike fullerenes (NOLFs) were obtained by chemical vapor deposition (CVD) using heavy oil residue as carbon source and ferrocene as catalyst precursor in an argon flow of 150 mL/min at 900 °C for 30 min. Field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive spectroscopy (EDS), x-ray diffraction (XRD), and Raman spectroscopy were used to characterize morphology and microstructure of the products. The results show that Fe-encapsulating NOLFs collected at the outlet zone of quartz tube had core/shell structures with sizes ranging from 3 to 6 nm and outer shells composed of poorly crystallized graphitic layers. Their growth followed particle self-assembling growth mechanism, and all atoms in the graphite sheets primarily arose from Fe-carbide nanoparticles.

The total energies and cohesive properties of 29 Au–Sn intermetallics (stable, metastable, and virtual) are calculated from first-principles density-functional theory (DFT) employing ultrasoft pseudopotentials (USPP) and both local-density approximation (LDA) and generalized gradient approximation (GGA) for the exchange-correlation functional. Among the intermetallics considered, the ground-state structures are found to be AuSn, AuSn2, and AuSn4. Another phase Au5Sn, though present in the equilibrium diagram, lies slightly above the ground state convex hull. The formation energies of stable phases calculated using USPP–LDA and USPP–GGA are nearly the same. Except for AuSn, calorimetric data for enthalpies of formation show a good agreement with the calculated formation energies. Based on our first-principles results, it is argued that the structures of two metastable phases are cP52-type γ brass (isotypic with Al4Cu9) at Au–20.5 at.% Sn and hP1-type γ (isotypic with HgSn6–10) at Sn–8 at.% Au. For the intermetallics considered in this study, we provide optimized values of lattice parameters and Wyckoff positions. The experimental lattice parameters show a better agreement with those calculated using USPP–LDA than with USPP–GGA. The results presented here form the basis for creating a reliable thermodynamic database to facilitate calculations of stable and metastable phase diagrams of binary and multicomponent systems containing Au and Sn, relevant to electronic packaging and many other joining applications.

Commensurate BaTiO3/SrTiO3 superlattices were grown by reactive molecular-beam epitaxy on four different substrates: TiO2-terminated (001) SrTiO3, (101) DyScO3, (101) GdScO3, and (101) SmScO3. With the aid of reflection high-energy electron diffraction (RHEED), precise single-monolayer doses of BaO, SrO, and TiO2 were deposited sequentially to create commensurate BaTiO3/SrTiO3 superlattices with a variety of periodicities. X-ray diffraction (XRD) measurements exhibit clear superlattice peaks at the expected positions. The rocking curve full width half-maximum of the superlattices was as narrow as 7 arc s (0.002°). High-resolution transmission electron microscopy reveals nearly atomically abrupt interfaces. Temperature-dependent ultraviolet Raman and XRD were used to reveal the paraelectric-to-ferroelectric transition temperature (TC). Our results demonstrate the importance of finite size and strain effects on the TC of BaTiO3/SrTiO3 superlattices. In addition to probing finite size and strain effects, these heterostructures may be relevant for novel phonon devices, including mirrors, filters, and cavities for coherent phonon generation and control.

Thick SiOxNy films were deposited by radiofrequency (rf) plasma chemical vapor deposition using silane (SiH4) and nitrous oxide (N2O) source gases. The influence of deposition conditions of gas flow ratio, rf plasma mixed-frequency ratio (100 kHz, 13.56 MHz), and rf power on the refractive index were examined. It was observed that the refractive index of the SiOxNy films increased with N and Si concentration as measured via x-ray photoelectron spectroscopy. Interestingly, a variation of refractive index with N2O:SiH4 flow ratio for the two drive frequencies was observed, suggesting that oxynitride bonding plays an important role in determining the optical properties. The two drive frequencies also led to differences in hydrogen concentration that were found to be correlated with refractive index. Hydrogen concentration has been linked to significant optical absorption losses above index values of ∼1.6, which we identified as a saturation level in our films.

Polyorganosiloxane spherical particles were synthesized by a sol-gel method from methyltrimethoxysilane (MTMS) using a reaction field of W/O emulsion consisting of sorbitantrioleate (SPAN85), n-octane, and aqueous solutions of basic, acid, and oil-soluble organic dyes. The investigation focused on the types of dyes suitable for incorporation into the spherical particles by using this method. The morphology of the particles was observed with scanning electron microscopy (SEM). Fluorescence and ultraviolet-visible (UV-vis) reflectance spectra of dye-doped spherical particles were measured. Basic dyes [Rhodamine B (RB), Rhodamine 6G (R6G), Crystal Violet (CV), Malachite Green (MG), and Thioflavin T (TT)] were doped into the spherical particles. Spherical particles obtained from aqueous solutions of RB, R6G, and CV were colored deeply. However, the MG- and TT-doped particles were scarcely colored. The reason for this color difference was discussed based on the comparison of UV-vis reflectance spectra of dye-doped spherical particles with absorption spectra of starting solutions of the dyes. It is found that the dye that tends to form dimers in aqueous solution was doped more easily than the dyes that tend to form monomers only. On the other hand, spherical particles obtained from acid dyes [Fluorescein Sodium Salt (FSS), Orange G (OG), Naphthol Green B (NGB), and Erythrosin B (EB)] and oil-soluble dye [Fluorescein (FLU)] were all white, confirming that these dyes were not doped in the particles. The reason was discussed in terms of the nature of the dyes and the formation mechanism of the spherical particles.

The melting behavior, thermal stability, and glass-forming ability (GFA) of Cu84−xZrxAg8Al8 (x = 42 to 50) glassy alloys were investigated. The alloy with x = 46 exhibits the highest reduced glass transition temperature (Trg). However, the best GFA was obtained for alloy with x = 48 corresponding to the largest supercooled liquid region (ΔTx) and a deep eutectic composition. At the best GFA composition, full glassy samples with diameters of over 20 mm could be fabricated by injection copper mold casting and water quenching without flux. The underlying mechanism of the unusual GFA of the alloy is discussed.

The effect of nanomaterials in platinum-decorated, multiwalled, carbon nanotube-based electrodes for amperometric glucose sensing was investigated by a comparative study with other carbon material-based electrodes such as graphite, glassy carbon, and multiwalled carbon nanotubes. Scanning and transmission electron microscopy and x-ray diffraction were used to investigate their morphologies and crystallinities. Electrochemical impedance spectroscopy was conducted to compare the electrochemical characteristics of these electrodes. The glucose-sensing results from the chronoamperometric measurements indicated that carbon nanotubes improve the linearity of the current response to glucose concentrations over a wide range, and that platinum decoration of the carbon nanotubes produces improved electrochemical performance with a higher sensitivity.

The deformation behavior of the organic polymer matrix of the biocomposite nacre structure in abalone shell was investigated by in situ straining during transmission electron microscopy (TEM). We observed strong adhesion to mineral plates and high ductility of the organic matrix, confirming a crack-bridging toughening mechanism. In addition, direct observation of reversible mechanical behavior was made in the viscoelastic reformation of matrix ligaments after failure. Crystalline β-sheet structures identified through electron diffraction suggested the presence of protein structures similar to spider or cocoon silk, and the reversible mechanism was attributed to hydration-induced unfolding and refolding of domains in these silklike proteins. This work provides further insight into the molecular and nanoscale behavior of nacre organic matrix and its contribution to bulk mechanical performance.

Hydrogels pose unique challenges to nanoindentation including sample preparation, control of experimental parameters, and limitations imposed by mechanical testing instruments and data analysis originally intended for harder materials. The artifacts that occur during nanoindentation of hydrated samples have been described, but the material properties obtained from hydrated nanoindentation have not yet been related to the material properties obtained from macroscale testing. To evaluate the best method for correlating results from microscale and macroscale tests of soft materials, nanoindentation and unconfined compression stress-relaxation tests were performed on poly-2-hydroxyethyl methacrylate (pHEMA) hydrogels with a range of cross-linker concentrations. The nanoindentation data were analyzed with the Oliver–Pharr elastic model and the Maxwell–Wiechert (j = 2) viscoelastic model. The unconfined compression data were analyzed with the Maxwell–Wiechert model. This viscoelastic model provided an excellent fit for the stress-relaxation curves from both tests. The time constants from nanoindentation and unconfined compression were significantly different, and we propose that these differences are due to differences in equilibration time between the microscale and macroscale experiments and in sample geometry. The Maxwell–Wiechert equilibrium modulus provided the best agreement between nanoindentation and unconfined compression. Also, both nanoindentation analyses showed an increase in modulus with each increasing cross-linker concentration, validating that nanoindentation can discriminate between similar, low-modulus, hydrated samples.

The most frequent cause of failure for wireless, handheld, and portable consumer electronic products is an accidental drop to the ground. The impact may cause interfacial fracture of ball-grid-array solder joints. Existing metrology, such as ball shear and ball pull tests, cannot characterize the impact-induced high speed fracture failure. In this study, a mini-impact tester was utilized to measure the impact toughness and to characterize the impact reliability of both eutectic SnPb and SnAgCu solder joints. The annealing effect at 150 °C on the impact toughness was investigated, and the fractured surfaces were examined. The impact toughness of SnAgCu solder joints with the plating of electroless Ni/immersion Au (ENIG) became worse after annealing, decreasing from 10 or 11 mJ to 7 mJ. On the other hand, an improvement of the impact toughness of eutectic SnPb solder joints with ENIG was recorded after annealing, increasing from 6 or 10 to 15 mJ. Annealing has softened the bulk SnPb solder so that more plastic deformation can occur to absorb the impact energy.

We show that friction anisotropy is an intrinsic property of the atomic structure of Al–Ni–Co decagonal quasicrystals and not only of clean and well-ordered surfaces that can be prepared in vacuum [J.Y. Park et al., Science309, 1354 (2005)]. Friction anisotropy is manifested in both nanometer-size contacts obtained with sharp atomic force microscope tips and macroscopic contacts produced in pin-on-disk tribometers. We show that the friction anisotropy, which is not observed when an amorphous oxide film covers the surface, is recovered when the film is removed due to wear. Equally important is the loss of the friction anisotropy when the quasicrystalline order is destroyed due to cumulative wear. These results reveal the intimate connection between the mechanical properties of these materials and their peculiar atomic structure.

Using periodic density-functional theory (DFT), we investigated the structure and cohesive properties of the α-alumina Σ11 tilt grain boundary, with and without segregated elements, as a model for the thermally grown oxide in jet engine thermal barrier coatings. We identified a new low-energy structure different from what was proposed previously based on electron microscopy and classical potential simulations. We explored the structure and energy landscape at the grain boundary for segregated Al, O, and early transition metals (TMs) Y and Hf. We predict that the TMs preferentially adsorb at the same sites as Al, while some adsites favored by O remain unblocked by TMs. All segregated atoms have a limited effect on grain boundary adhesion, suggesting that adhesion energies alone cannot be used for predictions of creep inhibition. These findings provide some new insights into how TM dopants affect alumina growth and creep kinetics.