The hardness of amorphous metal multilayered films was investigated by nanoindenation. Bilayer material systems of amorphous CuNb, FeB, and FeTi were produced by dc sputtering on 〈112￣0〉 sapphire substrates to a total thickness of 1 μm. The bilayer periods (Λ) ranged from 2 to 50 nm. The films’ noncrystallinity was verified by x-ray diffraction (XRD) and electron diffraction. The layer structure was verified by transmission electron microscopy and grazing angle XRD. The hardness and elastic modulus properties of the films, measured by nanoindentation, were shown to be statistically equivalent to the rule mixtures predictions. The hardness behavior is in contrast with the behavior of crystalline multilayered films, which generally display significant enhancements as the bilayer period is decreased below 10 nm. The lack of a significant hardness variation in the amorphous films strongly suggests that dislocation-mediated mechanisms do not govern inhomogeneous flow in amorphous metals.

The extent of BiInO3 substitution in the perovskite system xBiInO3–(1 - x)PbTiO3 and the corresponding raise in the Curie temperature were investigated using thermal analysis, dielectric measurements, x-ray diffraction, and electron microscopy. Maximum tetragonal perovskite distortion (c/a = 1.082) was obtained for x = 0.20, with a corresponding Curie temperature of 582 °C. Phase-pure tetragonal perovskite was obtained for x ⩽ 0.25. Compound formation after calcining mixed oxide powders resulted in agglomerated cube-shaped tetragonal perovskite particles, which could be fired to 94.7% of theoretical density (TD). Sol-gel fabrication resulted in nano-sized tetragonal or pseudo-cubic perovskite particles, which after two-step firing, resulted in a tetragonal perovskite microstructure at as high as (x = 0.20) 98.1% of TD.

In the pharmaceutical industries, mixing is a critical process. Pharmaceutical products consist of various components, including active ingredient and excipient. After mixing, we should get a homogeneous mixture to ensure the quality of the final products, such as tablets or capsules. For that reason, segregation is an unwanted phenomena in the mixing process. In this study, discrete-element method (DEM) was applied to investigate the mechanism of segregation in a rotating cylinder; basic equipment for powder mixing. In addition, segregation of particles in a rotating cylinder is a very interesting phenomenon and has captured the curiosity of not only industrial engineers, but also physicists. DEM can simulate segregation in a rotating cylinder three-dimensionally. In particular, radial segregation, which was quickly observed, was quantified by computing the granular temperature of the system. Furthermore, particle migration in axial direction, which may be the source of axial segregation, was also shown by the DEM simulation.

Solid-state recycling for machined chips of pure iron by hot extrusion at 823 K and annealing at 1073–1273 K was carried out. The as-extruded solid recycled specimen without annealing was fractured prior to yielding at room temperature. However, high ductility was recovered by annealing at 1073–1273 K. This is because the oxides at the interface of the machined chips dispersed in grain by annealing. The annealed solid recycled specimens showed higher yield stress than the annealed virgin extruded specimens. Grain refinement for the solid recycled specimens was enhanced by the high dislocation density in the machined chips, resulting in higher strength in the recycled specimens. Thus, the solid-state recycling is a low energy upgrade recycle process.

The use of an analytical approach to determine the relation between hardness and yield strength for materials with a high ratio of yield strength to Young's modulus is re-examined. It is shown that predictions using the analogy of the spherical cavity fail to reproduce experimental and finite element results because the surface deflection that occurs during loading is not taken into account. A modification is proposed to allow this. This gives a greatly improved prediction of the relationship between the hardness and yield strength of a material. It also enables the effect of the indenter shape on the measured hardness to be incorporated and explains why in some very hard materials, indentation is observed to be completely elastic.

The development and relaxation of stress in metal interconnects strained by their surroundings (substrate and passivation layers) is predicted by a discrete dislocation analysis. The model is based on a two-dimensional plane strain formulation, with deformation fully constrained in the line direction. Plastic deformation occurs by glide of edge dislocations on three slip systems in the single-crystal line. The substrate and passivation layers are treated as elastic materials and therefore impenetrable for the dislocations. Results of the simulations show the dependence of the stress evolution and of the effectiveness of plastic relaxation on the geometry of the line. The dependence of stress development on line aspect ratio, line size, slip plane orientation, pitch length, and passivation layer thickness are explored.

The glass formability of high-manganese amorphous steel alloys reported earlier by us has been found to improve upon additions of yttrium and lanthanide elements, enabling the formation of bulk glassy samples with diameter thicknesses reaching 7 mm by casting. Based on extensive studies using different Ln additions and systematic measurements of alloy oxygen contents, the intrinsic roles of Y/Ln in attaining good glass formability in both the high-Mn alloys and previously reported high-Cr alloys are revealed. The yield strengths of the non-ferromagnetic glassy alloys obtained are estimated to be three times those of high-strength stainless steel alloys, and high elastic moduli in the range 150–200 GPa are measured. Furthermore, in the supercooled liquid regions, the glassy rods can be bent into various configurations by hand without fracturing. The observed plastic behavior together with the measured high mechanical strengths suggests that the present Fe–based bulk metallic glasses can potentially be developed as formable non-ferromagnetic amorphous steel alloys.

The determination of the mechanical properties of ultra-thin coatings has become more and more important because of the increasing number of applications using such films. However, an accurate mechanical testing of coatings with a thickness down to some nanometers is still a challenge, despite the improvements of existing measurement techniques. Nanoindentation is an often used mechanical nanoprobe. Using the conventional test method with a sharp Berkovich indenter, the problem of the influence of the substrate on the results arises with decreasing film thickness. Therefore, it is nearly impossible to measure the modulus of films with a thickness less than 100–200 nm. The problem can be overcome by using spherical indenters in combination with an analytical solution for the Hertzian contact of coated systems. It allows a separation of film and substrate properties from the load–displacement curve of the compound. Indentation measurements were done at a 44 nm TiN film and at diamondlike carbon coatings in the thickness range between 4.3 nm and 125 nm on Si substrates. Several corrections were applied to obtain wholly elastic force–displacement curves with high accuracy. It is shown in more detail how zero point and thermal drift corrections are used to obtain statistical depth errors below 0.2 nm. Laser-acoustic measurements based on ultrasonic surface waves were chosen as a second method, which also measures the Young’s modulus in this thickness range. Although the indentation technique is a local probe and the laser-acoustic technique gives an integrated value for a surface range of some millimeters, the results agree well for the investigated samples. In contrast, it was impossible to get the correct Young’s modulus results by conventional indentation measurements with Berkovich indenter, even for ultra-low loads.

The structure and mechanical properties of Mg–Zn–Al–Y base cast alloys containing an icosahedral quasicrystal phase (i-phase) as a main strengthening phase were investigated. Mg–8Zn–4Al–xY base bulk alloys containing the i-phase were prepared by casting into a copper mold at moderate cooling rates. The Y addition was effective for decreasing the size of the i-phase and the increasing the homogeneity of its dispersed state. The mechanical properties examined by compression tests at room temperature were much superior to those of a conventional AZ91 Mg alloy. The creep tests at elevated temperatures indicated a promising high temperature creep resistance of the quasicrystal-reinforced Mg–Zn–Al–Y cast alloy. The strengthening mechanism was also discussed.

This article was originally published in [J. Mater. Res. 19, 1139 (2004)] and was incorrectly printed. The correct version appears below.

The formation of U-type hexaferrites with the composition Ba4B2Fe36O60 (B = Co, Ni, Zn) was studied. Samples were characterized by means of x-ray diffraction, electron microscopy (with energy-dispersive spectroscopy), and thermogravimetric and thermomagnetic analyses. U-hexaferrites are formed from the intermediate phases M-hexaferrite (BaFe12O19) and Y-hexaferrite (Ba2B2Fe12O22), which at the same time represent units in the U-hexaferrites’ crystal structure. The preparation of monophase U-hexaferrites was made possible by combining high-energy milling or chemical coprecipitation with a calcination at 1250–1300 °C. Structural defects, such as stacking faults, were observed in monophase samples with a high-resolution transmission electron microscope. The observed defects can be regarded as seeds for the formation of other hexaferrite phases after prolonged calcination times or higher calcination temperatures.

After this article appeared in the September 2004 issue of Journal of Materials Research, the authors noticed that the y2-axis labels for Fig. 1 were printed incorrectly. The correct figure is shown below:

A semi-analytical approach was developed to study the creep response of a viscoelastic polymeric thin film on a hard elastic substrate under flat-ended punch indentation. This approach allows one to separate mechanical properties of the film from its substrate. To verify the approach, flat-ended punch creep indentation tests were performed to obtain the long-time viscoelastic behaviors of a polymethyl-methacrylide film overlying on an aluminum substrate. Three viscoelastic models describing the constitutive equations of the polymer film are compared in this paper. “Film-only” viscoelastic parameters were extracted by fitting with the experimental creep curves of flat-ended punch indentation. It is shown that the present approach provides an effective way to characterize the mechanical properties of a polymeric film on an elastic substrate.

A comprehensive study was undertaken to identify the extent to which the mechanical properties of thin metal films on substrates could be determined quantitatively from instrumented sharp indentation. The mechanical behavior of thin Cu films on substrates was investigated using three different methods: nanoindentation, cantilever microbeam deflection, and microtensile testing. Finite element calculations of the nanoindentation and microbeam deflection experiments were conducted to extract yield strength and hardening modulus. Systematic experiments were performed to investigate the consistency of the different experimental techniques. The mechanical behavior of the Cu films was observed to depend on the film thickness. However, the results from finite element modeling of nanoindentation and microbeam deflection are quite different. In both cases, unique solutions for yield strength and hardening modulus were found. This is particularly noteworthy for the nanoindentation experiments; it is argued that the substrate destroys the self-similarity that is present during indentation of bulk material using a Berkovich tip. Microbeam deflection experiments seem to be more sensitive to the elastic–plastic transition, whereas the nanoindentation results describe the mechanical behavior at larger plastic strains. This is corroborated by microtensile tests.

Described is a room-temperature hydrogen sensor comprised of a TiO2-nanotube array able to recover substantially from sensor poisoning through ultraviolet (UV) photocatalytic oxidation of the contaminating agent; in this case, various grades of motor oil. The TiO2 nanotubes comprising the sensor are a mixture of both anatase and rutile phases, having nominal dimensions of 22-nm inner diameter, 13.5-nm wall thickness, and 400-nm length, coated with a 10-nm-thick noncontinuous palladium layer. At 24 °C, in response to 1000 ppm of hydrogen, the sensors show a fully reversible change in electrical resistance of approximately 175,000%. Cyclic voltammograms using a 1 N KOH electrolyte under 170 mW/cm2 UV illumination show, for both a clean and an oil-contaminated sensor, anodic current densities of approximately 28 mA/cm2 at 2.5 V. The open circuit oxidation potential shows a shift from 0.5 V to −0.97 V upon UV illumination.

Hydrophilic Co–Pt alloy nanoparticles nearing the equiatomic ratio and dispersedin water-soluble sodium carboxymethyl cellulose were synthesized by the aqueous reduction of CoCl2⋅6H2O and [Pt(NH3)4]Cl2⋅H2O with NaBH4 in presence of the cellulosic derivative. The as-received Co–Pt nanoparticles in the cellulosic matrix possess a disordered fcc structure that, upon calcination under an Ar atmosphereand carbonization of the cellulosic mantle of the particles, transformed to an ordered fcc phase. Both as-synthesized and calcined samples are magnetically soft at room temperature and exhibit a strong magnetic response when a magnetic field is applied. On account of the chemical composition of the carboxymethyl cellulose, the coated Co–Pt nanoparticles are easily soluble in water in high concentrations and exhibit interesting ion-exchange properties.

The deformation behavior of Ti-based bulk metallic glass (BMG) and metallic glass matrix composite (MGMC), both having a multistep crystallization behavior upon heating, has been investigated in the supercooled liquid region. The BMG deforms homogeneously and exhibits moderate elongation to failure due to its multistep crystallization behavior, but shows a significant variation of the flow stress during deformation. For the MGMC containing an in situ β-phase, a stress-overshoot characteristic, observed in the BMG, is not presented, but elongation to failure is rather limited because the crystalline β-phase prevents the viscous flow of the amorphous phase. The different presence of the crystalline phases in the metallic glasses can differently affect the flow behavior of metallic glass in the supercooled liquid region.

The wear properties under low loads of β Si3N4 and α sialon materials sintered with different rare-earth oxide sintering additives have been studied under dry sliding conditions using block-on-ring wear tests. All the worn surfaces showed an absence of fracture and smooth surfaces with the presence of an oxygen-rich filmlike debris indicating tribochemically induced oxidation of the surfaces. Extensive grain boundary removal was observed on the worn surfaces thought to be due to adhesion between this silicate phase and the tribochemically oxidized surfaces. The resistance to such oxidation and the properties of the residual grain boundary phase are thought to be important parameters affecting the wear behavior under the present testing conditions. For both the β Si3N4 and α sialon materials, there was an increase in wear resistance with decreasing cationic radius of the rare earth, thought to be due to improved oxidation resistance, and this was more remarkable in the case of the sialon materials where the incorporation of the sintering additives into the Si3N4 structure results in a lower amount of residual boundary phase.

New lead-free relaxors have been produced from the K0.5Na0.5NbO3–SrTiO3 (KNN-STO) system. The solid solubility within the studied range of compositions (1 - x) K0.5Na0.5NbO3–xSrTiO3 was observed for x up to 0.33. A pseudo-cubic perovskite structure was determined for x = 0.15 to 0.25. The high density and the uniform distribution of fine grains and pores were confirmed by the translucency of these ceramics. The 0.85KNN-0.15STO composition reaches the dielectric permittivity of above 3000 at room temperature. Dielectric spectroscopy measurements revealed that, as with lead-based complex perovskites, the cationic distribution disorder is reflected in relaxorlike properties, thus suggesting possible applications based on this environmentally friendly lead-free ceramic system.

The luminescence properties of nanocrystalline Y2O3:Er3+ prepared via wet chemical synthesis were investigated. A broadening of both the reflectance spectrum and 77 K luminescence spectrum (λexc = 488 nm) was observed in the nanocrystalline material compared to bulk Y2O3:Er3+. The spectral broadening was attributed to the presence of Er3+ ions on the surface of the particle, which experienced different crystal fields than the ions buried in the core of the particle. Upconversion was observed in both the bulk and nanocrystal material following excitation with 650-nm or 800-nm radiation. Following excitation with 800-nm radiation, an enhancement of the red (4F9/2 → 4I15/2) upconverted emission was observed and occurred as a result of the (4I9/2, 4I11/2) → (4I13/2, 4F9/2) ion-pair process that directly populated the 4F9/2 state. The magnitude of the red enhancement in the nanocrystalline material prepared via wet chemical synthesis was less than that of the identically doped bulk sample and less still than Y2O3:Er3+ nanocrystals prepared via a combustion synthesis technique. An explanation is proposed to account for the drastic difference in the red upconverted luminescence intensity.