Microstructural evolution and interfacial reaction in the eutectic SnBi solder joint on the Ni/Au metallization with and without the current stressing of 6.5 × 103 A/cm2 at 70 °C for 5 to 15 days were investigated. Electromigration is found to have significant effects not only on the phase formation at the joint interface but also on the phase coarsening and mass accumulation of Bi in the solder. In the solder joint without the current stressing, only a thin Ni3Sn4 phase was formed at the joint interface. For the solder joint with the current stressing, in addition to the Ni3Sn4 phase, a thick Au–Ni–Bi–Sn phase was formed at the joint interface after 10 days. However, the Au–Ni–Bi–Sn phase was not observed at the anode-side joint interface after 15 days of current stressing. Coarsening of the Bi-rich grain in the solder joint with the current stressing was much faster than that without the current stressing. Mass accumulation of Bi was observed at the anode side of the solder joint with the current stressing and the thickness of the Bi-rich accumulation layer increased with current stressing time. Based on the accumulation rate of the Bi-rich layer and the growth rate of the Bi-rich grain, the product of diffusivity and effective charge number of Bi in the eutectic SnBi solder is calculated to be 4.72 × 10−10 cm2/s.

In this study, the rate-dependent mechanical behavior of a Zr41.2Ti13.8Cu12.5Ni10Be22.5 bulk metallic glass was studied using quasi-static and dynamic shear-punch testing at room temperature. The results demonstrate that the shear strength of this alloy is insensitive to the applied strain rate. However, the formation of shear bands and the serrated flow exhibits a significant strain rate effect. The shear banding-induced fracture patterns and the fracture-melting phenomenon were analyzed based on the free volume theory and the energy transfer model.

Nacre, the shiny inner layer of mollusk shells is a model biomimetic nanocomposite system. Its exceptional mechanical properties have been the inspiration for materials scientists for several decades. Nacre exhibits a layered brick and mortar structure. It is composed of 95% inorganic (aragonitic CaCO3) phase and 5% organic (mainly proteins and polysaccharides) phase that are arranged in interlocked brick and mortar architecture with the mineral as bricks and organics as the mortar. In the current work, we describe the dynamic nanomechanical behavior of nacre using dynamic nanoindentation (nano-DMA) experiments. Two sets of loads were applied to obtain the dynamic response from varying depths in nacre. These tests were performed at three different frequencies (25, 50, and 100 Hz) to study the effect of frequency on the dynamic properties of nacre. The loss modulus (E″) and the loss factor (tan δ) were measured. Both of these parameters were observed to increase with increase in depth. Significant increase in tan δ was observed with the increase in frequency. Photoacoustic Fourier transform infrared spectroscopic studies on nacre indicate the presence of water in nacre. This water may be present at nanograin interfaces in nacre platelets, at organic–inorganic interfaces, and also in the organic phase in nacre. We believe that water is one of the significant contributors to the viscoelasticity of nacre. Our results indicate that the aragonite platelets in nacre may also contribute to viscoelasticity.

Sintering behavior and thermal expansion properties of the solid solution series Nd2-xCexCuO4±δ (0 ≤ x ≤ 0.20) have been investigated over the temperature range of 298 to 1100 K. Significant anisotropy in the lattice expansion coefficient in the a/b and c crystallographic axes was noted on increasing Ce content, which is consistent with the tetragonal unit cell. The lattice expansion in the c axis was found to decrease on increasing temperature for compositions up to x = 0.10, which is likely to be from variations in the oxygen stoichiometry. A variation in the sintering behavior was also noted on varying Ce content, with the onset of sintering temperature reaching a maximum at x = 0.10. A secondary sintering stage was noted for compositions with x > 0.10. Associated with the introduction of a secondary stage on sintering is an overall increase in the temperature at which the sintering is at a maximum.

We succeeded in fabricating c-axis (00l) oriented ZnO ceramics by using a rotating magnetic field and a subsequent sintering treatment. The degree of orientation in the green compact was about 0.5 along (00l) on the Lotgering scale. The degree of orientation increased to 0.99 after sintering at 1573 K. Particles can also be oriented in a static magnetic field, but along the direction of the a-axis or a,b-axes (h00), (hk0). These results show that selected axes can be oriented by controlling the magnetic field. Control of the crystal form in microstructures is expected to result in improvements in and better miniaturization of functional ceramics.

The present study investigated the effect of passivation on the kinetics of interfacial mass transport by measuring stress relaxation in electroplated Cu films with four different cap layers: SiN, SiC, SiCN, and a Co metal cap. Stress curves measured under thermal cycling showed different behaviors for the unpassivated and passivated Cu films, but were essentially indifferent for the films passivated with different cap layers. On the other hand, stress relaxation measured under an isothermal condition revealed clearly the effect of passivation, indicating that interface diffusion controls the kinetics of stress relaxation. The relaxation rates in the passivated Cu films were found to decrease in the order of SiC, SiCN, SiN, and metal caps. This correlates well with previous studies on the relationship between interfacial adhesion and electromigration. A kinetic model based on coupling of interface and grain-boundary diffusion was used to deduce the interface diffusivities and the corresponding activation energies.

Reliable measurement of mechanical properties of thin solid films has been challenging, despite widespread usage of thin films in applications such as semiconductor, magnetic storage, and microelectromechanical systems. Some of the challenges include instrument limitations and inadequacy of theoretical models to obtain quantitative prediction of thin film properties. In this article, we propose a technique to extract the shear strength of thin films from nanoscratch experiments using a contact mechanics analysis of a sliding sphere. Based on the stress field analysis by Hamilton, the stress status around the contact point is obtained at the initiation of yield, and is used to establish a direct correlation between contact pressure/surface traction and shear strength. Nanoscratch experiments were also performed on an extremely thin diamond carbon overcoat used in supersmooth magnetic storage disks, and the shear strength was successfully obtained using the proposed technique. These results were comparable with hardness values reported in the literature, assuming Tabor’s empirical relation (hardness ≈ 3*yield strength) and Tresca yield criterion. Finally, a finite element model was developed to simulate a rigid sphere sliding over a deformable solid to further verify the validity of the proposed model. The finite element analysis confirmed that the calculation results from the proposed relation are in good agreement with experimentally measured bulk property values of shear strength.

This work presents an original way for preparing TiO-based coatings by thermal spraying. As titanium monoxide is oxidized by the mere trace of oxygen contained in hydrogen, it is obvious that plasma spraying of TiO powder does not lead easily to the formation of a titanium monoxide coating. However, thermodynamical calculations show that the conditions necessary for the preparation of TiO can be reached, at the titanium melting temperature (Tm=1933 K), when oxygen reacts with liquid metal in the presence of excess carbon. These results have led to experiments in which TiO-based coatings have been prepared by spraying a stoichiometric mixture of graphite and titanium grains onto cast iron in air. In optimal conditions, a gas-tight hard coating (1000 ± 15 HV3) of a TiO-based phase (composition: TiO0.81±0.06C0.04±0.02) has been obtained.

Ceramics in the system ZrB2–Ta5Si3 were studied as candidates for the development of new ultra high-temperature ceramic materials. The ceramics were prepared by hot pressing at 1900–2200 °C in He. Mutual additions of ZrB2 and Ta5Si3 even in small amounts had significant densifying effects due to chemical interactions and solid solubility between the components, which have not been reported in the literature. Materials containing between 8 and 30 vol% Ta5Si3 exhibited less oxidation than pure ZrB2, which is the result of phase separation in surface borosilicate glass induced by Ta2O5. For higher concentrations, oxidation resistance substantially decreased with increasing Ta5Si3 content. The trend in the oxidation behavior of the materials showed significant dependence on the volume of oxidation products. Ceramics containing up to 10 mol% (30 vol%) Ta5Si3, which showed the highest oxidation resistance, also had the highest strength and hardness in the system, and are of interest for high-temperature structural applications in oxidizing environments.

The thermoelectric properties of Gd intercalated compounds GdxTiS2 have been investigated at the temperatures from 5 to 310 K. The results indicate that Gd intercalation into TiS2 leads to substantial decrease of both its electrical resistivity and its lattice thermal conductivity κL (κL is lowered by 20% and 46% at 300 K for x = 0.025 and 0.05, respectively). Specially, as compared to the pristine TiS2 the figure of merit ZT of the intercalated compound GdxTiS2 has been improved at all temperatures investigated, and specifically, the ZT value of Gd0.05TiS2 at 300 K is about three times as large as that of TiS2.

We propose a new theory with the potential for measuring the elastoplastic properties of compliant and soft materials using one sharp indentation test. The method makes use of the substrate effect, which is usually intended to be avoided during indentation tests. For indentation on a compliant and soft specimen of finite thickness bonded to a stiff and hard testing platform (or a compliant/soft thin film deposited on a stiff/hard substrate), the presence of the substrate significantly enhances the loading curvature which, theoretically, enables the determination of the material power-law elastic-plastic properties by using just one conical indentation test. Extensive finite element simulations are carried out to correlate the indentation characteristics with material properties. Based on these relationships, an effective reverse analysis algorithm is established to extract the material elastoplastic properties. By utilizing the substrate effect, the new technique has the potential to identify plastic materials with indistinguishable indentation behaviors in bulk forms. The error sensitivity and uniqueness of the solution are carefully investigated. Validity and application range of the proposed theory are discussed. In the limit where the substrate is taken to be rigid, the fundamental research is one of the first steps toward understanding the substrate effect during indentation on thin films deposited on deformable substrates.

Position-selective growth of carbon nanotubes (CNTs) and vertically aligned CNTs (VACNTs) on patterned metal were prepared using thermal chemical vapor deposition (TCVD) and direct current (DC) plasma-enhanced chemical vapor deposition. We propose a new position-controlling method of CNTs by controlling not only the position of Ni as a catalyst, but also the morphology of Mo as an underlayer for the catalysts. Selective growth of CNTs was achieved at the edges of the patterned metal using TCVD. The minimum width of selectively grown CNTs, approximately 2.6 μm, was approximately one-eightieth that of the patterned metal, 200 μm. The VACNTs were synthesized using the PECVD method, but the VACNTs grew throughout the patterned metal. A position-controlled method of CNT growth was demonstrated in optimum conditions of the TCVD.

A template-based, electroless wet-chemical method for synthesis of nanotubes and nanowires of nanocrystalline anatase titanium oxide (titania) at 45 °C is reported. Single-nanowire electrical property measurements reveal low dc resistivities (7–21 × 10−4 Ω cm) in these titania nanowires. In the presence of 1000 parts per million of CO gas at 100 °C, the resistivity is found to increase reversibly, indicating low-temperature gas-sensing capability in these titania nanowires. Thin films of nanocrystalline anatase titania, deposited using a similar wet-chemical method, also have low room-temperature dc resistivities (6–8 × 10−3 Ω cm), and they are transparent to visible light. Nanostructure-properties relations, together with possible electrical conduction, optical absorption, and gas-sensing mechanisms, are discussed. The ability to fashion transparent-conducting and gas-sensing nanocrystalline anatase titania into nanotubes/nanowires and thin films at near-ambient conditions could open a wider field of applications for titania, including nanoelectronics, chemical sensing, solar cells, large-area windows and displays, invisible security circuits, and incorporation of biomolecules and temperature-sensitive moieties.

An amorphous carbon coating, approximately 1.7 μm thick, deposited onto a ductile steel substrate, was indented using a 5-μm radius spherical-tipped diamond indenter to a maximum load of 150 mN. Displacement discontinuities were observed during loading, indicative of crack formation in the system. After indentation, a focused ion beam instrument was used to prepare cross-sections, which revealed the presence of ring, radial, and lateral cracks. A three-dimensional reconstruction of the deformation zone beneath the indent was conducted using a dual ion/electron beam instrument, assisted by a commercial three-dimensional visualization software package. These three-dimensional images enabled a detailed analysis of indentation-induced cracking in this film at submicron resolution. In contrast to traditional understanding and modeling, it was observed that the development of ring cracks was asymmetric for this type of coating/substrate system. Based on this observation, it can be deduced that the strain energy release rate was different for the growth of the spiral ring crack compared with the traditional concentric-ring model. Consequently, the concentric ring-crack fracture model may not be appropriate for the evaluation of the fracture toughness of this type of coating. Hence, three-dimensional images have presented a requirement that the asymmetrical nature of ring and radial cracks should be addressed and carefully considered in the fracture mechanics analysis of this type of hard coating system.

Multilayered manganese oxide films were prepared on a platinum electrode by potentiostatic oxidation of aqueous Mn2+ ions in the presence of n-tetra-alkylammonium compounds. Alkylammonium cations were intercalated between manganese oxide layers to balance the negative layer charge. Effects of several preparative parameters such as the size of alkylammonium molecules, counteranions, and bath composition on the structure of products were investigated. The interlayer distance of the products increased with increasing alkyl chain length up to C4, and the change became obviously small among C4–C6 compounds. The multilayer formation was achieved only when the manganese concentration was lower than 10 mM, and the highest crystallinity was obtained from a bath composed of 2 mM manganese sulfate and 50 mM alkylammonium chloride. At low concentrations of alkylammonium (<10 mM), a product intercalated with hydrated protons was formed, in which the protons were generated by anodic oxidation of Mn2+ with H2O.

The elastic modulus of an amorphous polymer was investigated by nanoindentation using combinations of ten total penetration depths and three constant unload rates. This experimental design provided a range of unloading strain rates coexisting with a range of depths. The elastic modulus of the material was found to correlate strongly with the unloading strain rate, whereas its correlation with the indentation depth was statistically nonsignificant. Thus, the increase of elastic modulus that occurred with decreasing depth at each constant unload rate was merely due to the increasing unloading strain rate associated with the decreasing depth. The true depth dependence of a rate-dependent material can therefore be studied only by maintaining a constant unloading strain rate across the entire depth range. The implications of these results to the continuous stiffness measurement technique are considered.

The adequacy of instrumented Vickers depth-sensing microindentation to determine Young's modulus of alumina-based ceramics was analyzed. Monophase alumina materials and alumina + 10 vol% aluminium titanate composites, with different microstructures, were tested to determine the effect of microcracking. The load–depth penetration of the indenter curves together with the observation of the imprints by scanning electron microscopy were used to analyze the behavior of the materials. Maximum stiffness was determined from the derivatives of the load-depth curves during unloading. The areas of the imprints measured optically were more representative of the behavior of the materials than the areas calculated from depth-penetration measurements. The formation of microcracks affected the shape of the unloading portion of the curves. Significant differences between the values of Young's modulus determined for different materials and definite relationships between the microstructural parameters of the materials and the Young's modulus were found.

Polymeric fibers have been used since the 1980s for improvement of the concrete. However, high mechanical performance has been obtained at high cost and using complex technologies. At least two parameters are important here: dimensions and surface characteristics of the fibers. We have modified nylon 6,12 fiber surfaces by 5, 10, 50, and 100 kGy gamma irradiation dosages. Tensile strength of the irradiated fibers was determined and then the fibers mixed at 1.5%, 2.0%, and 2.5% in volume with Portland cement, gravel, sand, and water. The compressive strength of the fiber reinforced concrete (FRC) was evaluated and the results were compared with results for similar materials reported before. The highest values of the compressive strength of FRC are seen for fibers at 50 kGy and 2.0% in volume of fiber; the strength is 122.2 MPa, as compared to 35 MPa for simple concrete without fibers. We advance a mechanism by which the fiber structure can be affected by gamma irradiation resulting in the compressive strength improvement of the concrete.

The paper presents the results of combined experimental, analytical, and computational studies of contact-induced deformation and cracking in dental multilayers. These include studies of individual layers and composite structures that consist of tri-layers of glass bonded to ceramic-filled polymer foundation with an acrylate-based join material. Loading-rate-dependent Young's moduli of the join and foundation materials were obtained from monotonic compression tests. Critical loads were also determined for the tri-layers from Hertzian contact tests at different loading rates. The fracture onset (sub-surface radial cracking) was detected using an in situ telescope. The measured rate-dependent Young's moduli were then incorporated into a finite element model that was used to predict the rate-dependent critical loads in the tri-layer system. Finally, the paper shows that the observed loading rate-dependence of the critical load (for radial cracking) is due to the combined effects of slow crack growth in glass and rate-dependent Young's moduli in the join and foundation layers.

White spot lesions are clinically detectable areas of demineralized enamel that often form during orthodontic treatment. Fluoride has been shown to prevent demineralization from occurring. Mechanical properties of white spot lesions are not well characterized. Bovine enamel slabs, with and without fluoride treatment, were placed under demineralization conditions. Through a series of microindentations at incremental loads, mechanical strength was measured using a novel method, specific volume absorbing energy (SVAE). SVAE is equal to work energy divided by the indentation volume. The supra-surface area (outermost 5 μm) of enamel slabs with fluoride demonstrated decreased mechanical strength compared to enamel slabs without fluoride. Fluoride may not impart protection over long periods of demineralization.