Occurrence of brittle interfacial fracture at an electroless Ni(P)/immersion gold–solder joint has long been a serious problem not yet fully understood. In our previous report on the electroless Ni(P) [J. Mater. Res.19, 2428 (2004)], it was shown that crystallization of the Ni(P) film and growth of the Ni3SnP layer were accelerated after the intermetallic compound (IMC) spalling, and accurate failure locus of the brittle fracture due to so-called “IMC spalling induced microstructure degradation of the Ni(P) film” is presented for the first time in this communication. For Sn–3.0Ag–0.5Cu solder joints, (Ni,Cu)3Sn4 and/or (Cu,Ni)6Sn5 ternary IMCs formed at the interface, and neither spalling nor interfacial fracture was observed. For Sn–3.5Ag joints, Ni3Sn4 compound formed, and the brittle fracture occurred through the Ni3SnP layer in the solder pads where Ni3Sn4 had spalled. Since the Ni3SnP layer is getting thicker during or after Ni3Sn4 spalling, control of IMC spalling is crucial to ensure the reliability of Ni(P)/solder system.

The development of Mg–Ca–Zn metallic glasses with improved bulk glass forming ability, high strength, and significant ductility is reported. A typical size of at least 3–4 mm amorphous samples can be prepared using conventional casting techniques. By varying the composition, the mass density of these light metal based bulk amorphous alloys ranges from 2.0 to 3.0 g/cm3. The typical measured microhardness is 2.16 GPa, corresponding to a fracture strength of about 700 MPa and specific strength of around 250–300 MPa cm3/g. Unlike other Mg- or Ca-based metallic glasses, the present Mg–Ca–Zn amorphous alloys show significant ductility.

A comparative study on the wet and dry milling of the intermediates for the Z-type hexagonal ferrite (Ba3Co2Fe24O41, Z phase) was performed. Phase-pure Z phase was synthesized by wet milling the intermediates comprising M and Y-type hexaferrites. The intermediates were obtained by calcining the stoichiometric powder mixture at 1080 °C. Subsequent wet milling by a planetary mill for 1 h increased the crystallization rate of Z phase upon subsequent heating at 1230 °C. In contrast, dry milling the intermediates resulted in the severe surface amorphization and led to heterogeneous crystalline states. The observed favorable effect of wet milling the intermediates was explained by the particle size reduction for the decrease of diffusion distance while preserving the basic layer units common to the related hexaferrites.

Amorphous transition behavior of silica polymorphs under high pressure has been extensively studied by using diamond-anvil cells or shock wave technologies at ambient temperature. Here, we report the amorphization of crystalline silica fiber in cristobalite polymorph in the temperature range of 1050–1350 °C without pressure applied in vacuum. X-ray diffraction, infrared spectra, and Raman spectra illustrated the transition. Raman spectra revealed that no significant changes had happened to the SiO4 unit during the transition. It is suggested that the driven-off of interstitial oxygen attributed to the transition and the reaction between the diffusing hydrogen and interstitial oxygen promoted the process.

Dislocation nucleation in solid solutions of face-centered-cubic metallic materials was studied using nanoindentation. The effects of solute impurities in the copper–nickel system on the formation of dislocations in a previously dislocation-free region were demonstrated to be minimal. The shear stress required to nucleate dislocations in copper is approximately 1.6 GPa, while in nickel a 3.9 GPa shear stress is required. Changes in shear stress for nucleation track closely with changes in elastic modulus showing the nucleation stress is approximately 1/30 to 1/20 of the shear modulus. The expected solid-solution strengthening is identified within the same experimental method, demonstrating unambiguously the fact that solid-solution impurities in this system will impact the propagation of dislocations during plastic deformation but not alter the homogeneous nucleation of dislocations in these materials.

We review experimental results—over the past 10–15 years and more recent theoretical modeling and computer simulations—on the effects of surface subnanoscale texture on adhesion and friction and the implications for certain mechanical properties of materials such as Mode I and Mode II failure. Examples and comparisons include surfaces that are adhesive or nonadhesive, rough or smooth, hard or soft (e.g., viscoelastic polymers), dry (unlubricated) or lubricated. One important conclusion is that the ultrafine picoscale details of a surface lattice or its roughness (“texture”) can be the most important factor in determining its friction and Mode II fracture, whereas such effects are less important for determining adhesion forces and Mode I fracture processes. Such studies are also clarifying the molecular and atomic basis of many well-established adhesion and tribological laws and empirical observations and are revealing new fundamental insights and relationships between nanoscale (molecular) and macroscale processes.

Results of simple computer simulations and model calculations for ion conducting rotor phases are compared to quasi-elastic neutron scattering data from solid solutions of sodium orthophosphate and sodium sulphate, xNa2SO4⋅(1 − x)Na3PO4. These materials are not only sodium fast-ion conductors in their high-temperature cubic phases but also show considerable dynamic reorientation disorder of their tetrahedral anions. At an elastic energy resolution of about 100 μeV, neutron spectrometry monitored oxygen scattering due to anion reorientation which occurs on the picosecond time scale. This thermally activated process exhibits activation energies between 0.184 eV (x = 0.0) and 0.052 eV (x = 0.5). Analysis of the quasielastic intensities as a function of scattering vector Q gives clear evidence of the involvement of cations in the anion reorientation. Increasing the elastic resolution to about 1 μeV full width at half-measure (FWHM) (thereby shifting the dynamic window to the nanosecond scale) allowed examination of sodium diffusion in xNa2SO4⋅(1 − x)Na3PO4. This process consists predominantly of thermally activated jumps between tetrahedrally coordinated sites, the activation energies ranging from 0.64 eV for x = 0.0 to 0.30 eV for x = 0.5.

To address the growing interest in nanoindentation for biomaterials, the following finite element study investigated the influence of indentation testing protocol and substrate geometry on quasi-static and dynamic load-displacement behavior of linear viscoelastic materials. For a standard linear solid, the conventional quasi-static indentation modulus, EQS, fell between the instantaneous and equilibrium modulus of the model. EQS approached the equilibrium modulus only for indentation unloading times 1000 times greater than the characteristic relaxation time of the model. It was nearly insensitive to other changes in the indentation testing protocol, such as tip radius and penetration depth, exhibiting variations of only 5–10%. Dynamic nanoindentation provided a quantitatively accurate assessment of the complex dynamic modulus (within ±12%) for a range material of parameters at physiologically relevant testing parameters. Both quasi-static and dynamic moduli calculated from the irregular surfaces varied with the size and shape of the irregularities but were still within 10% of the smooth surface values for penetration depths larger than the dimensions of the surface irregularities.

A new patterning technique for the deposition of sol-gels and chemical solution precursors was developed to address some of the limitations of soft lithography approaches. When using micromolding in capillaries to pattern precursors that exhibit large amounts of shrinkage during drying, topographical distortions develop. In place of patterning the elastomeric mold, the network of capillary channels was patterned directly into the substrate surface and an elastomer membrane is used to complete the channels. When the wetting properties of the substrate surfaces were carefully controlled using self-assembled monolayers (SAMs), lead zirconate titanate thin films with nearly rectangular cross-sections were successfully patterned. This technique, called microchannel molding (μCM), also provided a method for aligning multiple layers such as bottom electrodes for device fabrication.

In this paper, we present a method for determining the initial contact point and nanoindentation load–indentation depth characteristics for soft materials. The method is applied to the prediction of the load–indentation depth characteristics of polydimethylsiloxane. It involves the combined use of Johnson–Kendall–Roberts and Maugis–Dugdale adhesion theories and nonlinear least squares fitting in the determination of the initial contact point, the transition parameter, and the contact radius at zero contact load. The elastic modulus and the work of adhesion are also extracted from the load–indentation depth curves.

It has been generally accepted that YBa2Cu3O7−x (YBCO) films deposited on deformation textured polycrystalline metal tapes result in YBCO grain boundary (GB) networks that essentially replicate the GBs of the underlying substrate. Here we report that for thicker YBCO films produced by a BaF2 ex situ process, this is not true. Using electron backscatter diffraction combined with ion milling, we have been able to map the evolution of the YBCO grain structure and compare it to the underlying template in several coated conductors. For thin (≤0.5 μm) YBCO films deposited on rolling-assisted biaxially textured substrates (RABiTS), the YBCO GBs nearly directly overlap the substrate GBs. For 0.7–1.4 μm YBCO films, the GBs were found to meander along the substrate GBs and along the sample normal, with displacements several times the film thickness. In very thick films (2.5–2.9 μm), the YBCO grains can completely overgrow substrate grains and GBs, resulting in a substantial disconnection of the YBCO and substrate GB networks. Similar behavior is found for BaF2 ex situ YBCO films on ion-beam-assisted deposition-type templates. The ability of the YBCO to overgrow substrate grains and GBs is believed to be due to liquid-phase mediated laminar grain growth. Although the behavior of the YBCO GB networks changes with YBCO film thickness, the samples maintained high critical current density (Jc) values of >2 MA/cm2 for films up to 1.4 μm thick, and up to0.9 MA/cm2 for 2.5–2.9-μm-thick films.

The competition between fracture modes in monolithic brittle materials loaded in cyclic contact in aqueous environments with curved indenters is examined. Three main modes are identified: conventional outer cone cracks, which form outside the maximum contact; inner cone cracks, which form within the contact; and median–radial cracking, which form below the contact. Relations describing short-crack initiation and long-crack propagation stages as a function of number of cycles, based on slow crack growth within the Hertzian field, are presented. Superposed mechanical driving forces—hydraulic pumping in the case of inner cone cracks and quasiplasticity in the case of median–radials—are recognized as critically important modifying elements in the initial and intermediate crack growth. Ultimately, at large numbers of cycles, the cracks enter the far field and tend asymptotically to a simple, common relation for center-loaded pennylike configurations driven by slow crack growth. Crack growth data illustrating each mode are obtained for thick soda-lime glass plates indented with tungsten carbide spheres in cyclic loading in water, for a range of maximum contact loads and sphere radii. Generally in the glass, outer cone cracks form first but are subsequently outgrown in depth as cycling proceeds by inner cones and, especially, radial cracks. The latter two crack types are considered especially dangerous in biomechanical applications (dental crowns, hip replacements) where ceramic layers of finite thickness are used as load-bearing components. The roles of test variables (contact load, sphere radius) and material properties (hardness, modulus, toughness) in determining the relative importance of each fracture mode are discussed.

The crystallization mechanisms for potentially high mobility molybdenum-indium-oxide (IMO) film were studied. The crystalline IMO films were deposited on unheated glass substrates via high-density plasma evaporation, and subsequent vacuum annealing was performed at 150, 200, and 250 °C for 30 min. The results of x-ray diffraction and x-ray photoelectron spectroscopy and electrical properties suggested that the room-temperature crystallization was induced from the highest compressive strain, caused by the charged clusters and oxygen vacancies. The highest mobility of 75.8 cm2/Vs obtained at 250 °C was due to the charged In–Mo+6–O clusters and strain relaxation with (222)/(440) orientation change.

A splat-quenched, thick Al–Si deposit was manufactured by low-pressure plasma spraying (LPPS) and investigated in terms of microstructural inhomogeneity, Si solid solubility in α–Al, formation of metastable phases, and thermal stability. The LPPS Al–Si deposit had an inhomogeneous, layered microstructure consisting of splat-quenched lamellae and the incorporation of unmelted or partially melted particles. The splat-quenched Al–Si lamellae were formed by deposition of a fully liquid droplet and had an almost featureless microstructure at relatively low magnifications. There was a significant reduction in the α–Al lattice parameter in the LPPS Al–Si deposit because of extended Si solubility in the α–Al matrix. Transmission electron microscopy investigations showed that the splat quenching of liquid Al–Si droplet led to (i) columnar grain growth of α–Al(Si), (ii) formation of nano-sized Si precipitates in the Al matrix which was supersaturated with Si; and (iii) formation of amorphous Si phase embedded in the crystalline Al matrix. On reheating, the amorphous Si transformed into fine crystalline Si by interdiffusion of Al and Si atoms. Simultaneously, Si precipitation occurred in the supersaturated α–Al matrix. The overall activation energy for the Si crystallization/precipitation was estimated as ∼81 kJ/mol from a modified Kissinger analysis.

We investigated the effects of elevated temperature vacuum annealing on the morphological stability and hardness of self-supported, textured, polycrystalline Cu–Nb nanolayered films with individual layer thickness varying from 15 to 75 nm. Films with layer thickness greater than approximately 35 nm are found to resist layer pinch-off and spheroidization even after long annealing times at 700 °C, while films with layer thickness ∼15 nm exhibit layer pinch-off and evolve into an equiaxed grain microstructure. Nanoindentation measurements indicate almost no change in hardness after annealing for films that retain the layered morphology, in spite of the increase of in-plane grain dimensions. Significant decreases in hardness are noted for films that develop a coarsened equiaxed grain microstructure after annealing. The mechanism that leads to the development of a thermally stable nanolayered structure is analyzed. Also, the relative effects of in-plane grain size and layer thickness on the multilayer hardness are discussed.

We conducted a comparative study of microstructural properties for YBa2Cu3O7 (YBCO) films on single-crystal MgO and polycrystalline Ni-based metal substrates with ion-beam-assisted deposited (IBAD) MgO as a template. The film grown on the metal substrate shows more crystalline imperfections with density of screw dislocations four times higher than that of the film on single-crystal MgO, as revealed by high-resolution x-ray diffraction (HRXRD). These high-density screw dislocation cores connect well and form bigger clustered grains as detected by scanning tunneling microscopy. Transmission electron microscopy studies confirm that the structural quality of YBCO on the Ni-based alloy is comparable to that on single-crystal MgO. All these factors contribute to our routine fabrication of high-quality YBCO films on metal substrates with critical current densities in self-field as high as those for the films grown on single-crystal MgO substrates. Superconducting properties in fields are also discussed.

We optimized synthesis conditions of blue-emitting CaMgSi2O6:Eu2+ (CMS:Eu2+) with conventional solid-state reaction and successfully determined structure parameters by Rietveld refinement method with neutron powder diffraction data. The final weighted R-factor Rwp was 6.42% and the goodness-of-fit indicator S (= Rwp/Re) was 1.34. The refined lattice parameters of CMS:Eu2+ were a = 9.7472(3) Å, b = 8.9394(2) Å, and c = 5.2484(1) Å. The β angle was 105.87(1)°. The concentration quenching process was observed, and the critical quenching concentration of Eu2+ in CMS:Eu2+ was about 0.01 mol and critical transfer distance was calculated as 12 Å. With the help of the Rietveld refinement and Dexter theory, the critical transfer distance was also calculated as 27 Å. In addition, the dominant multipolar interaction of CMS:Eu2+ was investigated from the relationship between the emission intensity per activator concentration and activator concentration. The dipole–dipole interaction was a dominant energy transfer mechanism of electric multipolar character of CMS:Eu2+.

Piezoelectric ceramics with TC > 500 °C were projected in the perovskite BiInO3–PbTiO3 (BIPT) system based on their low tolerance factor (∼0.884). However, a stable perovskite phase could be synthesized only when the PbTiO3 (PT) content was greater than 75%. Furthermore, the large tetragonality (c/a > 1.08) and low electrical resistivity made the ceramics difficult to pole. Niobium-modified BIPT ceramics with PT contents of 80% and 85% were found to possess significantly lower dielectric loss at elevated temperatures, making it possible to polarize the materials. Piezoelectric properties were measured for a BIPT85–1.5 mol% Nb composition with a Curie temperature of 542 °C; the longitudinal piezoelectric coefficient and coercive field were found to be 60 pC/N and 125 kV/cm, respectively.

Using Blech’s structure, we studied the electromigration (EM) behaviors of four different Sn(Cu) and Sn(Ni) alloys, which are Sn, Sn0.7Cu, Sn3.0Cu, and Sn1Ni. The order of the EM rates was determined to be Sn0.7Cu > Sn > Sn3Cu > Sn1Ni. We believe that the lower yielding strength and higher grain boundary density of Sn0.7Cu were the main reasons that Sn0.7Cu had the fastest EM rate. Moreover, we found that the addition at Ni could effectively retard EM. The critical products of Sn, Sn0.7Cu, and Sn3.0Cu, which were determined to be 1500, 500, and 1580 A/cm, respectively. The diffuse-effective charge (DZ*) values of the solder stripes from this present work have same order magnitude of the reported values, which were measured by using actual solder bumps.

Carbon-doped oxide SiCOH films with low to ultralow dielectric constants were prepared on a Si substrate by plasma-enhanced chemical vapor deposition (PECVD) from mixtures of SiCOH precursors with organic materials. The films have different levels of nanoscale porosity resulting in different dielectric constants and mechanical properties. The mechanical properties of the films have been characterized by continuous-stiffness nanoindentation measurements. To study the effect of film thickness, each group of samples with the same dielectric constant was composed of samples prepared with different film thicknesses. It is shown that the effective hardness and modulus of the SiCOH/Si substrate system depends significantly on indentation depth due to substrate constraint effects. The “true” film properties were determined using both an empirical formulation of the effective modulus and direct inversion based on a finite element model. The hardness and modulus of three groups of samples with different degrees of dielectric constants have been measured. The hardness increases from 0.7 to 2.7 GPa and modulus from 3.6 to 17.0 GPa as the dielectric constants change from 2.4 to 3.0. While for stiffer films the modulus measured at an indentation depth 10% of the film thickness is close to the “true” value for films thicker than 0.5 μm, the measured value can give an overestimate of up to 35% for softer films. Thin film cracking and film–substrate debonding have been observed with scanning electron and atomic force microscopy at the indentation sites in softer films. The damage initiation is indicated by pop-in events in the loading curve and sharp peaks in the normalized contact stiffness curves versus indentation depth.