Exchange bias phenomena of amorphous CoFeSiB ribbons have been probed at room temperature. The dramatic loop shift away from zero point occurred when the ribbons were annealed in ambient atmosphere with longitudinal field. The possible crystalline phases grown in our ribbons are discussed based on the grazing incidence diffraction and energy dispersive x-ray spectroscopy. The magnetic domain configuration of ribbon surface was also observed to make clear the dependence of bias behavior on the induced magnetic anisotropy in the ribbon. A simple phenomenological explanation was given to discuss the exchange bias in ribbons.

The oxidation resistances of ZrB2 containing SiC, TaB2, and TaSi2 additions of various concentrations were studied using isothermal thermogravimetry at 1200, 1400, and 1500 °C, and specimens were further characterized using x-ray diffraction and electron microscopy. Increasing SiC concentration resulted in thinner glassy surface layers as well as thinner ZrO2-rich underlayers deficient in silica. This silica deficiency was argued to occur by a wicking process of interior-formed borosilicate liquid to the initially-formed borosilicate liquid at the surface. Small (3.32 mol%) concentrations of TaB2 additions were more effective at increasing oxidation resistance than equal additions of TaSi2. The benefit of these additives was related to the formation of a zirconium-tantalum boride solid solution during sintering, which during oxidation, fragmented into fine particles of ZrO2 and TaC. These particles resisted wicking of their liquid/glassy borosilicate encapsulation, which increased overall oxidation resistance. With increasing TaB2 or TaSi2 concentration, oxidation resistance degraded, most egregiously with TaB2 additions. In these cases, zirconia dendrites appeared to grow through the glassy layers, providing conduits for oxygen migration.

Al-based high-aspect-ratio microscale structures (HARMS) are basic building blocks for all-Al microdevices. Bonding of Al-based HARMS is essential for device assembly. In this paper, bonding of Al-based HARMS to flat Al plates using Al-Ge thin film intermediate layers is investigated. The structure of sputter codeposited Al-Ge thin films was studied by high-resolution transmission electron microscopy as a function of the average film composition. The structure of the interface region between Al-based HARMS bonded to flat Al plates is studied by combining focused ion beam sectioning and scanning electron microscopy. An extended bonding interface region, ∼100 μm in width, is observed and suggested to result from liquidus/solidus reactions as well as diffusion of Ge in solid Al at the bonding temperature of 500 °C. The extended interface region is suggested to be beneficial to Al-Al bonding via Al-Ge intermediate layers.

The spherical indentation strength of a lead zirconate titanate (PZT) piezoelectric ceramic was investigated under poled and unpoled conditions and with different electrical boundary conditions (arising through the use of insulating or conducting indenters). Experimental results show that the indentation strength of the poled PZT is higher than that of the unpoled PZT. The strength of a poled PZT under a conducting indenter is higher than that under an insulating indenter. Poling direction (with respect to the direction of indentation loading) did not significantly affect the strength of material. Complementary finite element analysis (FEA) of spherical indentation of an elastic, linearly coupled piezoelectric half-space is conducted for rationalizing the experimental observations. Simulations show marked dependency of the contact stress on the boundary conditions. In particular, contact stress redistribution in the coupled problem leads to a change in the fracture initiation, from Hertzian cracking in the unpoled material to subsurface damage initiation in poled PZT. These observations help explain the experimental ranking of strength the PZT in different material conditions or under different boundary conditions.

We have demonstrated that 30BaO–15TiO2–30GeO2–25SiO2 (BTGS25) glass is a candidate for fiber-type nonlinear optical devices using crystallization of glass matrix. We determined the glass composition is suitable for crystallized fiber using partial substitution of Ge in 30BaO–15TiO2–55GeO2 (BTG55) by Si. The BTGS25 satisfied both thermal stability for fiber drawing and electronic polarizability for nonlinear optical property. After crystallization, the BTGS25 bulk crystallized glass showed surface crystallization behavior with the polar c-orientation of fresnoite phase, which was favorable for large second-order optical susceptibility. Following the results of the bulk glass, we prepared the BTGS25 glass fiber without precipitation of fresnoite crystallites. The BTGS25 crystallized fiber also showed c-oriented surface crystallization of fresnoite and second harmonic generation, which shows that the crystallized fiber is a promising material for fiber-type optical active devices.

Erbium dihydride Er(H,D,T)2 is a fluorite structure rare-earth dihydride useful for the storage of hydrogen isotopes in the solid state. However, thermodynamic predictions indicate that erbium oxide formation will proceed readily during processing, which may detrimentally contaminate Er(H,D,T)2 films. In this work, transmission electron microscopy (TEM) techniques including energy-dispersive x-ray spectroscopy, energy-filtered TEM, selected area electron diffraction, and high-resolution TEM are used to examine the manifestation of oxygen contamination in ErD2 thin films. An oxide layer ∼30–130 nm thick was found on top of the underlying ErD2 film, and showed a cube-on-cube epitaxial orientation to the underlying ErD2. Electron diffraction confirmed the oxide layer to be Er2O3. While the majority of the film was observed to have the expected fluorite structure for ErD2, secondary diffraction spots suggested the possibility of either nanoscale oxide inclusions or hydrogen ordering. In situ heating experiments combined with electron diffraction ruled out the possibility of hydrogen ordering, so epitaxial oxide nanoinclusions within the ErD2 matrix are hypothesized. TEM techniques were applied to examine this oxide nanoinclusion hypothesis.

A novel optimization approach, capable of extracting the mechanical properties of an elasto-plastic material from indentation data, is proposed. Theoretical verification is performed on two simulated configurations. The first is based on the analysis of the load–displacement data and the topography of the residual imprint of a single conical indenter. The second is based on the load–displacement data obtained from two conical indenters with different semi-angles. In both cases, a semi-analytical approach [e.g., Dao et al., Acta Mater.49, 3899 (2001) and Bucaille et al., Acta Mater.51, 1663 (2003)] is used to estimate Young’s modulus, yield stress, and strain hardening coefficient from the load–displacement data. An inverse finite element model, based on a commercial solver and a newly developed optimization algorithm based on a robust stochastic methodology, uses these approximate values as starting values to identify parameters with high accuracy. Both configurations use multiple data sets to extract the elastic-plastic material properties; this allows the mechanical properties of materials to be determined in a robust way.

The knowledge of thermophysical properties of active metals is critical to understand their metallurgical processes and further industrial applications. However, due to high reactivity and melt contamination from a crucible and gaseous environment, accurate values of the properties are hard to obtain using conventional methods such as the sessile-drop method. In the present study, a vacuum electrostatic levitator was used to circumvent these difficulties and enabled the noncontact determination of thermophysical properties of liquid cerium even in an undercooled state. The data of density, surface tension, and viscosity of molten cerium were reported, as well as their temperature dependence.

MAX-phase carbides (M is an early transition metal, A is an A-group element) exhibit an interesting bonding characteristic of alternative stacking of strong M–C bonds and relatively weak M–A bonds in one direction. In the present first-principles total energy calculations, we establish the relationship between mechanical properties and electronic structure for ternary M2AC (M = Ti, V, Cr, A = Al, Si, P, S) carbides. By systematically tuning elements on the M and A sites, pronounced enhancements of bulk modulus, elastic stiffness, and ideal shear strength are achieved in V-containing V2AC (A = Al, Si, P, and S) carbides. It is suggested that tailoring on the A site is more efficient than on the M site in strengthening the mechanical properties of studied serial carbides. The results highlight a general trend for tailor-made mechanical properties of ternary M2AC carbides by control of chemical bonding.

Molecular dynamics simulations were performed to gain fundamental insight into crystal plasticity, and its size effects in nanowires deformed by spherical indentation. This work focused on <111>-oriented single-crystal, defect-free Ni nanowires of cylindrical shape with diameters of 12 and 30 nm. The indentation of thin films was also comparatively studied to characterize the influence of free surfaces in the emission and absorption of lattice dislocations in single-crystal Ni. All of the simulations were conducted at 300 K by using a virtual spherical indenter of 18 nm in diameter with a displacement rate of 1 m·s−1. No significant effect of sample size was observed on the elastic response and mean contact pressure at yield point in both thin films and nanowires. In the plastic regime, a constant hardness of 21 GPa was found in thin films for penetration depths larger than 0.8 nm, irrespective of variations in film thickness. The major finding of this work is that the hardness of the nanowires decreases as the sample diameter decreases, causing important softening effects in the smaller nanowire during indentation. The interactions of prismatic loops and dislocations, which are emitted beneath the contact tip, with free boundaries are shown to be the main factor for the size dependence of hardness in single-crystal Ni nanowires during indentation.

Reverse atom transfer radical polymerization of methacrylonitrile (MAN) initiated by azobisisobutyronitrile (AIBN) was approached for the first time in the absence of any ligand in four novel ionic liquids, 1-methylimidazolium acetate ([mim][AT]), 1-methylimidazolium butyrate ([mim][BT]), 1-methylimidazolium caproate ([mim][CT]), and 1-methylimidazolium heptylate ([mim][HT]). The polymerization in [mim][AT] not only showed the best control of molecular weight and its distribution but also provided a more rapid reaction rate with the ratio of [MAN]:[FeCl3]:[AIBN] at 300:2:1. The block copolymer PMAN-b-PSt was obtained via a conventional ATRP process in [mim][AT] by using the resulting PMAN as a macroinitiator. After simple purification, [mim][AT] and FeCl3 could be easily recycled and reused and had no effect on the living nature of reverse atom transfer radical polymerization of MAN.

The strain-induced austenite (γ) to martensite (α′) transformation in AISI 316L austenitic stainless steel, either in powders or bulk specimens, has been investigated. The phase transformation is accomplished using either ball-milling processes (in powders)—dynamic approach—or by uniaxial compression procedures (in bulk specimens)—quasi-static approach. Remarkably, an increase in the loading rate causes opposite effects in each case: (i) it increases the amount of transformed α′ in ball-milling procedures, but (ii) it decreases the amount of α′ in pressed samples. Both the microstructural changes (e.g., crystallite size refinement, microstrains, or type of stacking faults) in the parent γ phase and the role of the concomitant temperature rise during deformation seem to be responsible for these opposite trends. Furthermore, the results show the correlation between the γ → α′ phase transformation and the development of magnetism and enhanced hardness.

The crystallization behavior of melt-spun ribbons and bulk samples of the Cu36Zr48Al8Ag8 glassy alloy on heating is presented here. The crystallization kinetics and structural changes in the Cu36Zr48Al8Ag8 glassy alloy were studied using x-ray diffraction, transmission electron microscopy, differential scanning, and isothermal calorimetry methods. A clear comparison is made of the differences in the crystallization kinetics of the melt-spun ribbons and the copper-mold-cast bulk rod samples. It was suggested that the kinetics of crystallization in the rod sample, at any given temperature, are somewhat different than in the ribbon samples, probably because of size and free volume effects. Differences in the crystallization behavior of this alloy with other Cu-Zr-Al-Ag alloys have also been discussed.

Indentation tests were performed, using a flat punch probe, on silicone gels to induce failure under compression. The silicone gels were formed from networks of vinyl-terminated polydimethylsiloxane (PDMS) with molecular weights of 800 and 28,000 g/mol and a sol fraction of trimethylsiloxy-terminated PDMS with molecular weights ranging from 1250 to 139,000 g/mol. Cone cracks were observed in samples that fractured from defects at the sample surface, but failure more commonly originated from the corners of the indenter. Ring cracks were observed for the most highly compliant samples that fractured at indentation depths approaching the overall thickness of the sample. In these cases we generally observed a delayed fracture response, with a time delay that increased with increasing sol fraction and decreased with increasing indentation load.

The indentation size effect, in which the contact pressure increases as the size of contact decreases, has been observed for many years for both spherical and pointed indenters. The concept of strain gradient plasticity has been used to describe this phenomenon, but it is often necessary to introduce a material length scale l* to fit experimental data. Here we present a theory based on the concept of dislocation slip distance, which naturally generates the scaling and incorporates the material parameters that influence the size effect. We compare this model with experimental data for a range of ceramics and tungsten metal and show that the yield strain and Burgers vector are the important material parameters in the indentation size effect.

Measurement of the mechanical behavior of hydrated gels is challenging due to a relatively small elastic modulus and dominant time-dependence compared with traditional engineering materials. Here polyacrylamide gel materials are examined using different techniques (indentation, unconfined compression, dynamic mechanical analysis) at different length-scales and considering both viscoelastic and poroelastic mechanical frameworks. Elastic modulus values were similar for nanoindentation and microindentation, but both indentation techniques overestimated elastic modulus values compared to homogeneous loading techniques. Hydraulic and intrinsic permeability values from microindentation tests, deconvoluted using a poroelastic finite element model, were consistent with literature values for gels of the same composition. Although elastic modulus values were comparable for viscoelastic and poroelastic analyses, time-dependent behavior was length-scale dependent, supporting the use of a poroelastic, instead of a viscoelastic, framework for future studies of gel mechanical behavior under indentation.

The indentation properties of human fingernails at varying humidity are reported. The samples were indented using both microindentation, to obtain their Vickers hardness and also nanoindented using a Berkovich indenter tip. The relative humidity (RH) of the samples was controlled by using salt solutions with a sealed and enclosed environment surrounding the testing equipment. It was shown that the Vickers hardness of the samples is sensitive to RH, with recovery of the nail material more readily occurring for nails tested at >55% RH. This recovery mechanism is discussed in terms of the structure of the nails, and this approach is also suggested as a technique for following recovery mechanisms in natural materials under varying humidity. The hardness obtained by nanoindentation is similar to previously published data, but does not change with humidity. The modulus of the nails is also insensitive to relative humidity, but in the same range as the value derived from the microindentation tests.

The interfacial fracture toughness and the adhesion strength of two dissimilar materials are governed by the diffusion interfacial thickness and its mechanical characteristics. A new testing methodology is implemented here to estimate the actual interfacial thickness from a series of nanoindentations across the interface, under the same applied load, with tip radius and indentation depth many times larger than the interface thickness. The bimaterial system used is a semicrystalline polymer interface of isotactic polypropylene and linear low-density polyethylene. The laminate is prepared under a range of diffusion temperature to yield diffusion interfaces of 0 to 50 nm. A numerical relationship is developed using two-dimensional (2D) finite element simulation to correlate the true interfacial thickness, measured by transmission electron microscopy, with the experimentally estimated apparent interfacial thickness, derived from the transition domain of a series of indents across the interface. A range of material-pairs property combinations are examined for Young’s modulus ratio E1/E2 = 1 to 3, yield strength ratio σY1/σY2 = 1 to 2.5, and interfacial thickness of 0 to 100 nm. The proposed methodology and the numerically calibrated relationship are in good agreement with the true interfacial thickness.

In this work, the time-dependent plastic deformation behavior of Ti40Zr25Ni3Cu12Be20 bulk and ribbon metallic glass alloys was investigated using a nanoindentation technique at room temperature with the applied load ranging from 5 to 100 mN. The stress exponent n, defined as, has been derived as a measure of the creep resistance. It was found that the measured stress exponent increases rapidly with increasing indentation size, exhibiting a positive size effect. The size effect on the stress exponent n obtained from the bulk sample is more pronounced than that obtained from the ribbon sample. The deformation mechanism involved will be discussed.

Recent computational parametric studies have developed reverse algorithms to extract material properties of elastoplastic materials using experimental sharp nanoindentation. These methods used reduced modulus in their parameters to include the effect of indenter compliance. To investigate the validity of using reduced modulus, we conducted experimental indentation of a couple of representative cases for elastoplastic metals with a diamond and a sapphire Berkovich tip. Then, we performed a finite element study for sharp indentation of the same material systems. Both computational and experimental results indicate that the use of reduced modulus is invalid to describe indentation loading response for elastoplastic materials in a certain material regime. Our results show that indenter compliance is overestimated by the previous predictions using reduced modulus. This overestimation leads to underestimation of indenter curvature and causes error in extracting material properties by reverse algorithms.