Representative strain plays an important role in indentation analysis; by using the representative strain and stress, the normalized indentation load becomes a function of one variable, which facilitates the reverse analysis of obtaining the material plastic properties. The accuracy of such function is critical to indentation analysis. Traditionally, polynomial functions are used to fit the function, which does not incorporate correct elastic/plastic limits and has no physical basis. In this paper, we have proposed a new limit analysis-based functional formulation based on the theoretical solutions of conical/wedge indentation on elastic and rigid plastic solids. It is found that both limits agree well with numerical results, and the new approach involves no—or at most one—fitting parameter, which can be obtained with much less effort compare with the traditional polynomial approach. Reverse analyses on five different materials have shown that the new and simple limit analysis-based formulation works better than the traditional polynomial fit. The new technique may be used to quickly and effectively measure material plastic properties for any conical indenter if the elastic modulus is known a priori.

Nacre, the inner iridescent layer of seashells is a model biomimetic system composed of 95% of inorganic (aragonite) phase and 5% of organic phase. Nacre exhibits an interlocked layered “brick and mortar” structure where the bricks are made up of aragonitic calcium carbonate and mortar is an organic phase. Here, we report the role of indentation load and penetration depth on measurement of nanomechanical properties of nacre. A range of loads from 10 μN to 10,000 μN were applied to obtain the response from different depths of nacre. The values of hardness and elastic modulus decrease with increasing load (i.e., increase in penetration depth). The variation in these values is significant at lower loads and decreases with increase in indentation load. From our results, it appears that the nanoindentation tests done at lower loads are highly influenced by micro and nanostructure in nacre. The indentation experiments performed at low loads indicate an elastic modulus of about 15 GPa for the organic phase. The low load, low penetration experiments appear to be better indicators of nanomechanical behavior. Also, we have observed a step-like behavior in the load-displacement curves at high load indentations on nacre. These features are attributed to the organic layer between the aragonite platelets. The indentation tests with penetration depths more than ∼250-300 nm often disrupt the organic layer and the behavior is not recovered in the unloading part of the curve. The microarchitecture and the composition of nacre contribute to the decrease in hardness values with increasing depth along with the indentation size effects.

(Zr62Cu15.4Ni12.6) (x = 6–12) in situ glassy composites containing uniformly distributed Ta-rich particles were prepared by arc-melting and copper mould casting. The results show that addition of 6–10 at.% Ta to Zr62Cu15.4Ni12.6Al10 results in dissolution of 2.4 to 4.6 at.% Ta in the glassy matrix, which promotes glass-forming ability, and the remaining Ta precipitates out as body-centered cubic (BCC) Ta-rich particles dispersed on the glassy matrix. The critical diameters for the composites with 6, 8, and 10 at.% Ta are 7, 7, and 6 mm, respectively. At 12 at.% Ta addition, the glass-forming ability is dramatically reduced because of the precipitation of secondary dendritic Ta-rich particles and other nanocrystallites from melts during copper mould casting. Also, owing to the solid-liquid reaction during induction heating, some Ta-rich particles formed in the master alloys will redissolve into the glassy matrix, resulting in a smaller volume fraction of Ta-rich particles in the as-cast glassy rods than that of the corresponding ingots. The glassy matrix composites exhibit enhanced plastic strain of about 7.5 to 22.5% at room temperature. The optimum Ta content in the glassy alloys is determined to be 10 at.%, which corresponds to the highest ultimate stress of 2220 MPa and the largest plastic strain of 22.5%. The plastic strain increases with increasing volume fraction of in situ BCC Ta-rich particles. This is apparently ascribed to the impedance of Ta-rich particles to shear bands. Ta-rich particles seed the initiation of multiple shear bands and block the shear band propagation, leading to intensive multiplication and bifurcation of shear bands.

A ferromagnetic shape-memory alloy Ni48Mn25Ga22Co5 was prepared by the induction melting and isothermal forging process. Dynamic recrystallization occurs during the isothermal forging. The deformation texture was studied by the neutron diffraction technique. The main texture components consist of (110)[112] and (001)[100], which suggested that in-plane plastic flow anisotropy should be expected in the as-forged condition. The uniaxial compression fracture strain in the forged alloy reaches over 9.5%. The final room-temperature fracture of the polycrystalline Ni48Mn25Ga22Co5 is controlled mainly by intergranular mode.

The effect of stress, resulting from the presence of hydrogen, on the aluminum-induced crystallization of hydrogenated amorphous silicon films was studied. Layered thin films of hydrogenated and unhydrogenated amorphous silicon and aluminum, deposited by sputtering, were used to study this effect. The stress of the deposited films was determined by measuring the radius of curvature of c-Si substrates before and after deposition of the films. It was observed that unhydrogenated amorphous silicon films exhibit a high compressive stress compared with hydrogenated ones. The amount of stress is shown to decrease with increasing hydrogen content. It was also observed that aluminum always provides tensile stress. After the initial stress measurements, all the samples were annealed for 30 min at temperatures between 200 °C and 400 °C. X-ray diffraction was used to determine the crystallinity of the silicon films. The results of the study show that the temperature at which crystallization of amorphous silicon is initiated is lower for films with a lower initial stress.

The underlying relationships between the microstructure and time-dependent mechanical properties of hydrated fibrin, collagen, and fibrin/collagen composite materials have been explored using an adaptation of the classical rigid, cylindrical, flat punch loaded normally to a planar specimen surface. A suite of quasi-static elastic and viscoelastic indentation experiments have been conducted with uniformly mixed fibrin, collagen, and fibrin/collagen composites, in addition to macrolayered collagen materials. Coupled with insights obtained from optical and confocal fluorescence microscopy, a simple micromechanics model has been developed for the effect of local microstructural variables on the macroscopic mechanical stiffness. These results demonstrate the efficacy of this technique to efficiently and reproducibly probe hydrated engineered tissue replacement materials for local variations in viscoelastic material behavior without the need for extensive specimen preparation or grips, as well as being suitable for performing directly comparable measurements with explants of human skin.

Influence of low and medium energy electron beam (E-beam) irradiation on the single-walled (SW) and multiwalled (MW) carbon nanotube films grown by microwave chemical vapor deposition are investigated. These films were subjected to electron beam energy of 50 keV from scanning electron microscope for 2.5, 5.5, 8.0, and 15 h and 100, 200, and 300 keV from transmission electron microscope electron gun for a few minutes to approximately 2 h continuously. To assess the surface modifications/structural degradation, the films were analyzed prior to and post-irradiation using x-ray diffraction and micro-Raman spectroscopy in addition to in situ monitoring by scanning and high-resolution transmission electron microscopy. A minimal increase in intertube or interplanar spacing (i.e., d002) for MW nanotubes ranging from 3.25–3.29 Å (∼3%) can be analogized to change in c-axis of graphite lattice due to thermal effects measured using x-ray diffraction. Resonance Raman spectroscopy revealed that irradiation generated defects in the lattice evaluated through variation of: the intensity of radial breathing mode (RBM), intensity ratio of D to G band (ID/IG), position of D and G bands and their harmonics (D* and G*). The increase in the defect-induced D band intensity, quenching of RBM intensity, and only a slight increase in G band intensity are some of the implications. The MW nanotubes tend to reach a state of saturation for prolonged exposures, while SW transforming semiconducting to quasi-metallic character. Softening of the q = 0 selection rule is suggested as a possible way to explain these results. It is also suggestive that knock-on collision may not be the primary cause of structural degradation, rather a local gradual reorganization, i.e., sp2+δ ⇔ sp2+δ, sp2 C seems quite possible. Experiments showed that with extended exposures, both kinds of nanotubes displayed various local structural instabilities including pinching, graphitization/amorphization, and forming intra-molecular junction (IMJ) within the area of electron beam focus possibly through amorphous carbon aggregates. They also displayed curling and closure forming nano-ring and helix-like structures while mending their dangling bonds. High-resolution transmission electron microscopy electrons corroborated these conclusions. Manufacturing of nanoscale structures “nano-engineering” of carbon-based systems is tentatively ascribed to irradiation-induced solid-state phase transformation, in contrast to conventional nanotube synthesis from the gas phase.

The improvement of optical reflectance of BaO–ZnO–B2O3–SiO2 (BZBS) glass by the addition of various types of micron-scale crystalline fillers (TiO2, SiO2, ZrO2, Al2O3, MgO, and cordierite) was investigated for application of the materials to barrier ribs of plasma display panels. The fillers were partially dissolved during sintering, yielding an increased local volume of the fillers in the submicron range, filler rearrangement along boundaries of sintered glass frits, and rather irregular and rugged filler shapes differing from the original morphologies. The measured optical reflectance of the various filler added specimens was within the 30–70% range, which was much higher than the predicted values (less than 10%) based on the rule of mixture of the refractive index. Here we report that the high reflectance of the barrier rib glass for plasma display panels is explained by light scattering by the increased submicron portion of the partially dissolved residual fillers, the size of which is similar to the visual spectrum range (0.4–0.7 μm). The order of reflectance improvement among different types of filler-embedded specimens was consistent with that of the degree of dispersion of the residual fillers in the glass matrix.

Bulk glass formation of the Co–Cr–Mo–C–B–Er alloy system was investigated in this paper. The Co50Cr15Mo14C15B6 (at.%) alloy could be cast into fully glassy rod with a diameter up to 2 mm. By adding 2 at.% Er to this alloy, the critical diameter for glass formation reached 10 mm. The excellent glass formability of the Er-doped alloy was mainly attributed to its relatively large reduced glass transition temperature of 0.61, near-eutectic composition, and the necessity of redistribution of the Er atoms for precipitation of crystalline Co6Mo6C phase in the undercooled liquid on cooling.

The deformation behavior of single-crystal GaN nanowires was studied by directly performing three-point bending tests on each individual nanowire in an atomic force microscope. The elastic modulus calculated from the load–displacement response of the nanowires was 43.9 ± 2.2 GPa. Single-crystal GaN nanowires investigated in this study were synthesized by chemical vapor deposition techniques based on the vapor–liquid–solid growth mechanism and had a diameter range from 60 to 110 nm. Crystalline GaN nanowires did not show obvious plastic deformation in bending and usually failed in a brittle manner.

Effect of electromigration on mechanical shear behavior of flip chip solder joints consisting of 97Pb3Sn and 37Pb63Sn composite solder joints was studied. The under bump metallurgy (UBM) on the chip side was TiW/Cu/electroplated Cu, and the bond pad on the board side was electroless Ni/Au. It was found that the mode of shear failure has changed after electromigration and the mode depends on the direction of electron flow during electromigration. The shear induced fracture occurs in the bulkof 97Pb3Sn solder without current stressing, however, after 10 h current stressing at 2.55 × 104 A/cm2 at 140 °C, it occurs alternately at the cathode interfaces between solder and intermetallic compounds (IMCs). In the downward electron flow, from the chip to substrate, the failure site was at the Cu–Sn IMC/solder interface near the Si chip. However, in the upward electron flow, from the substrate to chip, failure occurred at the Ni–Sn IMC/solder interface near the substrate. The failure mode has a strong correlation to microstructural change in the solder joint. During the electromigration, while Pb atoms moved to the anode side in the same direction as with the electron flow, Sn atoms diffused to the cathode side, opposite the electron flow. In addition, electromigration dissolves and drives Cu or Ni atoms from UBM or bond pad at the cathode side into the solder. These reactions resulted in the large growth of Sn-based IMC at the cathode sides. Therefore, mechanical shear failure occurs predominantly at the cathode interface.

We have investigated the effect that the Ta content has on the ferroelectric properties of strontium bismuth tantalate (SBT) thin films synthesized using metalorganic decomposition (MOD) and spin coating techniques. The physical properties of these SBT samples were strongly dependent upon the Ta ratio. Polarization measurements revealed that Ta-deficient SBT exhibited a relatively low coercive field (2Ec ∼ 87 kV/cm) and a high remanent polarization (2Pr ∼ 15 μC/cm2). The value of 2Pr decreased as the Ta ratio in SBT increased. The improved ferroelectric properties of the Ta-deficient SBT samples may have resulted from the uniformly well-grown bismuth-layered-structured (BLS) phases of the films and their highly preferential orientation along the a and b axes. We suggest that the incorporation of Ta vacancies plays an important role in enhancing the crystallinities and microstructures of Ta-deficient SBT films.

Spider silk is a material with unique mechanical properties under tension. In this study, we explore the anisotropic mechanical properties of spider silk using instrumented indentation. Both quasistatic indentation and dynamic stiffness imaging techniques were used to measure the mechanical properties in transverse and longitudinal sections of silk fibers. Quasistatic indentation yielded moduli of 10 ± 2 GPa in transverse sections and moduli of 6.4 ± 0.5 GPa in longitudinal sections, demonstrating mechanical anisotropy in the fiber. This result was supported by dynamic stiffness imaging, which also showed the average reduced modulus measured in the transverse section to be slightly higher than that of the longitudinal section. Stiffness imaging further revealed an oriented microstructure in the fiber, showing microfibrils aligned with the drawing axis of the fiber. No spatial distribution of modulus across the silk sections was observed by either quasistatic or stiffness imaging mechanics.

An instrumented indentation microscope was constructed and applied to the measurements of the Meyer hardness and the elastic modulus of several engineering materials ranging from ductile metals to brittle ceramics. Because of the in situ optical observation and determination of the indentation contact area that is synchronized to the indentation load versus depth relation, the mechanical properties determined on the indentation microscope are precise and reliable without any undesirable approximations and assumptions required for estimating the contact area. It is also demonstrated that the instrumented indentation microscope is capable of determining in a quantitative manner the in situ contact profiles of impression (sinking-in/piling-up profiles). The present work suggests that the instrumented indentation microscope will be a powerful tool in the science and engineering of indentation contact mechanics.

Two cubic boron nitride (c-BN) thin films (thickness, 80 nm), which were grown on silicon by mass-selected ion beam deposition and thin diamond film-coated silicon by magnetron sputtering technique respectively, were investigated by x-ray absorption near-edge spectroscopy (XANES) at the B K-edge. The angular dependences of the XANES recorded in fluorescence yield (FY) were used to show that the preferable orientation of the sp2-bonded turbostratic BN (t-BN) basal planes at the interfacial layers between the top c-BN film and Si substrate is normal or nearly normal to the substrate, which is consistent with previous transmission electron microscope analysis. The angular dependence was also used to show that the film deposited on diamond-coated Si has a higher relative amount of ordered t-BN at its film-substrate interface than the film on Si substrate. This work that shows a technique to determine the thin film structure, especially the interfacial structure between the thin films and their substrates x-ray absorption fine structure is a powerful mode.

Tantalum disulfide (TaS2) nanoplatelets were produced by laser ablation of a TaS2 target under an argon atmosphere. The nanoplatelet dimensions and morphology were characterized by transmission electron microscopy and x-ray diffraction. The effect of the ablation laser power density on the size distribution of the nanoplatelets was studied. The TaS2 nanoplatelets were prone to oxidation upon exposure to air but could be stabilized by using 3-mercaptopropionic acid as the capping agent.

Hardness, elastic modulus, and stress directly influence the ability of tantalum carbide/amorphous hydrocarbon (TaC/a-C:H) thin films to enhance the wear-resistance of steel tribological component surfaces. Designed factorial experiments enabled an evaluation of the effects of acetylene flow rate (QC2H2), direct current bias voltage level (Vb), and substrate rotation rate (ωRot) during deposition on the mechanical properties of reactively sputtered TaC/a-C:H films. Significant relationships were found between compressive stress level and Vb, whereas hardness and elastic modulus were dependent primarily on Vb and secondarily on QC2H2 within the studied parameter space. It is proposed that effects of ion bombardment on the a-C:H phase during growth are responsible for property dependencies on Vb. Decreases in hardness and elastic modulus with increasing QC2H2 are attributed to increased hydrogen concentration and a concomitant decreased volume fraction of TaC crystallites in the films.

The influence of the molecular weight of poly(acrylic acid) (PAA) on chemical mechanical planarization (CMP) for shallow trench isolation (STI) was investigated. The adsorption behaviors of PAA as a function of molecular weight on deposited plasma-enhanced tetraethylorthosilicate and chemical vapor deposition Si3N4 films were analyzed by the force measurement using atomic force microscopy (AFM). The AFM results revealed that the affinity of PAA with the nitride film is higher than the affinity with the oxide film, and thus a denser adsorption layer on the nitride film is formed with higher molecular weight of PAA, which leads to higher selectivity in STI CMP. Additionally, to determine the correlation between the dispersion stability of the CeO2 resulting from the presence of PAA with different molecular weight and CMP performance, the colloidal properties of the slurry as a function of the molecular weight of PAA were examined.

The debonding behavior of perfluorocyclobutane (PFCB) films on silicon (Si) has been investigated using Vickers indentation as a function of cure temperature and film thickness. PFCB films on Si were processed by spin coating (1–4 μm) and solution casting (20–60 μm). The interfacial shear strength of solution-cast PFCB films was independent of film thickness. The interfacial shear strength increased with cure temperature. The PFCB/Si cured at 225 °C exhibited interfacial shear strength of 123 MPa, and the strength increased to 163 MPa when the cure temperature was raised to 275 °C. The increase in interfacial-shear strength with temperature has been attributed to the increase in the density of bonds between PFCB and Si due to an increase in the density of crosslinks. Spin-coated films exhibited cracking due to the penetration of the indenter into the substrate, and the extent of cracking increased with the load.

Bulk Ta4AlC3, a new layered-ternary carbide in the Ta–Al–C system, was synthesized and characterized. Transmission electron microscopy investigations on this new phase are reported here. Selected area electron diffraction and convergent beam electron diffraction analyses indicated that this ternary carbide crystallized with the space group P63/mmc. Atomic-scale microstructures of Ta4AlC3 were achieved by means of high-resolution transmission electron microscopy and Z-contrast scanning transmission electron microscopy. The experimental crystal structural parameters agreed well with the theoretical values obtained using density-functional calculations.