The formation of 10-nm ZnO nanopyramids using a simple synthetic route has been isolated from the reaction of Zn(OAc)2·2H2O in 1,4-butanediol followed by ripening at 90 °C. This was accomplished by establishing control over the Ostwald ripening process through the use of a carboxylic acid specific adsorbate. Using a variety of analytical methods, it is proposed that the carboxylate groups in the acetate precursor stabilize the {101} habit planes, creating septahedral shapes or nanopyramids. Particle assembly into crystallographically oriented dimers was observed with high specificity, and the association mechanism is suggested to relate to the crystal polarity and the variation in specific adsorption of the carboxylic acid to the surface facets. These materials are a candidate for biological labeling applications in living cells.

In this work, we study the cooling behavior of several typical bulk glassy alloys on casing and present the relationship between the thermal conductivity of a glassy alloy and the cooling rate upon mold casting. The cooling rates obtained for Ti-, Zr-, Pd-, and Cu-based bulk glass forming alloys are found to scale with the thermal conductivities of the studied glassy alloys.

A method for evaluating true interlamellar spacing from micrographs is proposed for a multidomained lamellar structure. The microstructure of these materials is assumed to be composed of many domains with the lamellae aligned roughly parallel to each other within each domain and with the domains themselves randomly oriented relative to one another. An explicit expression for the distribution of apparent interlamellar spacing is derived assuming that the distribution of the true interlamellar spacing is Gaussian. The average interlamellar spacing is close to the peak interlamellar spacing observed in the distribution. The theoretical distributions are compared with experimental ones obtained by analyzing micrographs of PbTe–Sb2Te3 lamellar composites.

Fracture behavior of Zr55Cu30Al10Ni5 bulk metallic glass was investigated under quasi-static compression at strain rate of 10−4/s using an Instron testing machine and dynamic split Hopkinson bar (SHPB) compression with strain rate of about 1900–4300/s. Pronounced strain softening, especially past the peak stress, was observed under SHPB tests and compared with the distinct flow serrations under quasi-static tests. Scanning electron microscope revealed that the angle between the loading axis and major shear plane is less than 45°, deviating from the maximum shear stress plane. Microscopically, unlike the ordinary veinlike pattern found in quasi-static compression, the elongated veinlike pattern was observed at the onset position of rapid shearing under dynamic test. A closely arrayed dendritelike structure dominated the dynamic fracture, consequently, and should be the major pattern representing the rapid shear band propagation. In addition, a transition state from veinlike to dendritelike pattern was observed at the final instantaneous fracture region in quasi-static tests. Evidence revealed the characteristic dimension of dynamic fracture surface complies with Taylor’s meniscus instability criterion. The roles of free volume and adiabatic heating on the fracture strength and stress concentration on the fracture morphology are also discussed.

Rapid thermal annealing (RTA) processing under N2 and O2 ambient is suggested and characterized in this work for improvement of SiCOH ultra-low-k (k = 2.4) film properties. Low-k film was deposited by plasma-enhanced chemical vapor deposition (PECVD) with decamethylcyclopentasiloxane and cyclohexane precursors. The PECVD films were treated by RTA processing in N2 and O2 environments at 550 °C for 5 min, and k values of 1.85 and 2.15 were achieved in N2 and O2 environments, respectively. Changes in the k value were correlated with the chemical composition of C–Hx and Si–O related groups determined from the Fourier transform infrared (FTIR) analysis. As the treatment temperature was increased from 300 to 550 °C, the signal intensities of both the CHx and Si–CH3 peaks were markedly decreased. The hardness and modulus of the film processed by RTA have been determined as 0.44 and 3.95 GPa, respectively. Hardness and modulus of RTA-treated films were correlated with D-group [O2Si–(CH3)2] and T-group [O3Si–(CH3)] fractions determined from the FTIR Si–CH3 bending peak. The hardness and modulus improvement in this work is attributed to the increase of oxygen content in (O)x–Si–(CH3)y by rearrangement.

The effects of the Zr/Ti ratio on the electrical properties of lead zirconate titanate (PZT) thick films prepared by the aerosol deposition (AD) process were investigated to optimize the electrical properties of the thick film. The Zr/Ti ratio was varied among 45/55, 52/48, and 60/40, and the post-annealing temperature was varied from 500 to 900 °C. Microscopic examination of the as-deposited films revealed crack-free and dense microstructures with a thickness of 10 μm. The annealed films showed markedly improved electrical properties in comparison with the as-deposited films with increasing post-annealing temperature. With increasing Zr/Ti ratio, the remnant polarization and coercive field decreased. The dielectric constant and piezoelectric coefficient, d33, were highest for the PZT 52/48 film. This film annealed at 900 °C exhibited the best overall combination of electrical properties, with a dielectric constant, remnant polarization, and piezoelectric coefficient of 1320, 31.1 μC/cm2, and 150 pC/N, respectively.

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.

Guidelines for selecting the shape formed by metal discharged from a narrow Al line were developed. By controlling electromigration in the line, either relatively large microspheres, thin wires, or relatively small microspheres could be formed. Our starting point was a passivated polycrystalline Al line with a slit and small holes at the anode end of it. In the discussion, we describe how the temperature of a part of a wire, T*, at the moment when the part is completely discharged from the hole, affects the shape of the microstructural feature formed from the metal. High, intermediate, and low values of T* were found to correspond to the formation of large microspheres, thin wires, and small microspheres, respectively. The experimental results are explained in the discussion.

Microstructure evolution of YBa2Cu3O7−y (YBCO) films during the two heat-treatments in the advanced trifluoroacetates metalorganic deposition (TFA-MOD) process has been investigated by means of transmission electron microscopy. In the calcination process, precursor films including nanopores were formed through the shrinkage of the film after a remarkable increase of the thickness due to the thermal decomposition of metalorganic salts in the starting solution. During the crystallization process, the densification and shrinkage of the film occurred after agglomeration of nanopores and coarsening of unreacted phase particles such as Y2Cu2O5, CuO, and Ba–O–F in the precursor films. The YBCO films were then epitaxially grown with the remaining unreacted phase particles in the film, finally pores were generated again by a reaction of these unreacted particles to form YBCO accompanied by the volume reduction. It is important to control the densification of precursor films and coarsening of the unreacted phase particles in the crystallization process, to fabricate YBCO final films with fine crystallinity and high critical current values.

We studied the resistivity, photosensitivity, photoluminescence, and surface photovoltage of CdTe crystals doped with Ge or Sn to extend our knowledge of the influence of the deep-donor level on compensation and afterglow effects. We demonstrated a strong correlation between photosensitivity caused by photoelectrons with Fermi-level variations near the GeCd0/2+ or SnCd0/2+ energy levels. Surface photovoltage measurements confirmed that when the concentration of residual acceptors varied along the direction of growth, then trapping conditions dramatically changed as a defect was converted from a neutral state to doubly charged positive one.

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.

Ferroelectric thin films of the 0.1Pb(Ni1/3Nb2/3)O3–0.35Pb(Zn1/3Nb2/3)O3–0.15Pb (Mg1/3Nb2/3)O3–0.1PbZrO3–0.3PbTiO3 (PNN–PZN–PMN–PZ–PT) complex oxide system were prepared on Pt/Ti/SiO2/Si substrates using a polymer-modified sol-gel method followed by a rapid thermal annealing (RTA) process. It was found that the addition of excess NiO is effective in stabilizing the perovskite phase while suppressing the pyrochlore phase. The crystalline structure and morphology of the films with different amounts of access NiO were studied with x-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM), respectively. The electrical properties, including dielectric, ferroelectric, and piezoelectric, showed a significant improvement with excess NiO. The film sample with 3 mol% of excess NiO exhibited optimized electrical properties. Different parameters, including tolerance factors on the basis of ionic radii, electronegativity differences between cations and anions, and oxygen bond valences, were applied to analyze the stability of the perovskite phase with different amount of excess NiO. Analysis results indicated that only the bond-valence theory could explain the effect of excess NiO on the stability of the perovskite phase under the assumption that the excess Ni2+ entered the A sites of the perovskite structure.

Subcritical cracking of thin glass films caused by stress-corrosion phenomena cannot be neglected when it comes to application and manufacturing processes that involve exposure to aqueous environments. A protocol is introduced to allow for a quantitative study of stress corrosion through channel cracking experiments. By this method, an exponential dependence of the crack propagation rate on the pH of the aqueous environment is revealed. Therefore, this behavior should be accounted for through the use of an appropriate pre-exponential factor in the expression of channel cracking rate. This factor should reflect the reduced crack resistance of the glass film caused by the weakening of the silica bonds behind the crack tip in the aqueous environment. A direct comparison between commercial slurries and reference solutions confirms that the crack resistance is a function of the pH of the ambient.

Previous work on YBa2Cu3O7−x (YBCO) + BaSnO3 (BSO) films with a single composition showed significant critical current density (Jc) improvements at higher fields but lowered Jc in low fields. A detailed study on BSO concentrations provided here demonstrates that significant Jc enhancement can occur even up to 20 mol% BSO inclusion, where typical particulate inclusions in these concentrations degrade the YBCO performance. YBCO + BSO films were processed on (100) LaAlO3 substrates using premixed targets of YBa2Cu3O7-x (YBCO) with additions of 2, 4, 10, and 20 mol% BSO. The critical transition temperature Tc of the films remained high (>87 K), even with large amounts (20 mol%) of BSO. YBCO + BSO films showed a gradual increase in Jc at high fields as the amount of BSO was increased. More than an order of magnitude increase in Jc was measured in YBCO + BSO samples as compared to regular YBCO at 4 T. YBCO + 10 mol% BSO films showed overall improvement at all the field ranges while YBCO + 20 mol% BSO was better only at high fields. Transmission electron microscopy revealed the presence of ∼7–8-nm-diameter BSO nanocolumns, the density of which increased with increasing BSO content correlating well with the observed improvements in Jc.

The enthalpy of formation of cubic ceria–zirconia solid solutions (c-Ce(1−x)ZrxO2, 0.05 ⩽ x ⩽ 0.75) at 25 °C with respect to monoclinic zirconia (m-ZrO2) and cubic ceria (c-CeO2) has been measured by high-temperature oxide melt solution calorimetry. In contrast to fluorite solid solutions containing trivalent oxides (e.g., yttria–zirconia), mixing in c-Ce1−xZrxO2 shows moderate positive deviation from ideality. Evaluating the data within the framework of a regular solution model, the interaction parameter, Ω, is +51.0 ± 8.0 kJ/mol. The introduction of undersized Zr into CeO2 severely distorts and destabilizes the oxygen sublattice. Destabilization of c-Ce1−xZrxO2 may be relieved by reduction or clustering. A stable ordered compound in the CeO2–ZrO2 system is thermodynamically unlikely.

To impart machinability to hard and brittle AlN ceramics without losing their high thermal conductivity, a homogeneous dispersion of fine BN particles in an AlN matrix was investigated. A homogeneous dispersion of BN particles was obtained by pressureless sintering of turbostatic BN-coated AlN nanocomposite powder (AlN–BN nanocomposite powder), which was prepared by reducing and heating AlN particles containing a mixture of boric acid, urea, and carbon. Though AlN is slightly oxidized by boric acid during the reduction, the addition of carbon reduced the oxygen content of the AlN–BN composite powder by carbothermal reduction of the oxidized AlN particles. As a result, the thermal conductivity of the sintered material increased with decreasing oxygen content of the nanocomposite powder. AlN–BN nanocomposites containing more than 20 vol% BN showed high strength, machinability, and relatively high thermal conductivity in comparison with the conventional microcomposites.

The effect of minor transition metal (TM) additives of Ni, Co, or Zn on the interfacial reactions of the solder joints between Sn–Ag–Cu (SAC) solder and the Cu/Ni(P)/Au substrate was investigated, especially subsequent to multi-reflowing. (Cu,Ni)6Sn5 formed at the interface of all the joints except that of SAC–Ni, of which the interfacial compound was (Ni,Cu)6Sn5. The interfacial compounds of the SAC–Co and SAC–Zn contained a small amount of alloying elements of less than 3 at.%. Two P-rich layers, Ni3P and Ni–Sn–P emerged at the interface of the SAC joints. Nanoindentation analysis indicates that the hardness and Young’s modulus of these two phases were slightly higher than those of the Ni(P) substrate, which were in turn much greater than those of the Cu–Ni–Sn compounds. Worthy of notice is that with TM additions, the Ni–Sn–P phase between Ni3P and interfacial compounds was absent even after 10 reflows. For the SAC–Co joints, the growth of Ni-containing intermetallic compounds within the solder gave rise to the excess Ni dissolution, which caused a discrete Ni3P layer and over-consumed Ni(P) substrate underneath the grooves in-between (Cu, Ni)6Sn5 scallop grains at the interface. This phenomenon is presented for the first time, and the mechanism is proposed in this study.

By spark-eroding Fe75Si15B10 in water/ethanol mixtures, spherical particles with nanostructured cores consisting of mixed amorphous and crystalline phases were produced. The relative volume fractions of the amorphous and crystalline phases were dependent on the water/ethanol ratio. In the same process, continuous oxide layers were formed on the particle surfaces. The basic mechanisms responsible for the formation of the surface oxide layers and the core nanostructures were modeled. At frequencies ranging from 1 to 100 MHz, the combination of the core nanostructures and the insulating oxide shells yielded exceptionally low-loss magnetic behavior.

The standard Oliver–Pharr nanoindentation analysis tacitly assumes that the specimen is structurally rigid and that it is both semi-infinite and homogeneous. Many specimens violate these assumptions. We show that when the specimen flexes or possesses heterogeneities, such as free edges or interfaces between regions of different properties, artifacts arise in the standard analysis that affect the measurement of hardness and modulus. The origin of these artifacts is a structural compliance (Cs), which adds to the machine compliance (Cm), but unlike the latter, Cs can vary as a function of position within the specimen. We have developed an experimental approach to isolate and remove Cs. The utility of the method is demonstrated using specimens including (i) a silicon beam, which flexes because it is supported only at the ends, (ii) sites near the free edge of a fused silica calibration standard, (iii) the tracheid walls in unembedded loblolly pine (Pinus taeda), and (iv) the polypropylene matrix in a polypropylene–wood composite.

Indentations were performed on silicon using a Berkovich indenter at loads up to 12 mN, at temperatures from 20 to 135 °C. Transmission electron microscopy revealed crystalline silicon phases in the residual indentation imprint at and above 35 °C. Also, the first reconfirmation of the occurrence of Si-VIII during unloading was observed at temperatures of 100 and 125 °C. Interestingly, at 125 °C a cavity was also observed, and an unidentifiable phase was observed at 135 °C. The observations show the strong effect of temperature on pressure-induced phase transformation in silicon.