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.

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.

We report studies on the correlation between the microstructure, the magneto-crystalline structure, and the magnetic properties of barium hexaferrite powders. The samples consisted of typical hexagonal plate-like particles with approximate sizes of 80, 180, and 500 nm, obtained by microemulsion, coprecipitation, and solid-state reaction techniques, respectively, and were characterized by x-ray powder diffraction and scanning and transmission electron microscopy. The hyperfine parameters of the hexaferrite powders with different particle size were investigated by Mössbauer spectroscopy. We also measured the magnetization-versus-magnetic field dependence of the submicron powders at high magnetic fields up to 30 T at 4.2 K. Finally, we comment on the surface effects observed because of particle size reduction from micron to nanoscale dimensions.

Monolithic nanoporous copper was synthesized by dealloying Mn0.7Cu0.3 by two distinct methods: potentiostatically driven dealloying and free corrosion. Both the ligament size and morphology were found to be highly dependent on the dealloying methods and conditions. For example, ligaments from 16 nm–125 nm were obtained by dealloying either electrochemically or by free corrosion, respectively. Optimization of the starting Mn–Cu alloy microstructure allowed us to synthesize uniform porous structures; but we found cracking to be unavoidable. Despite the presence of unavoidable defects, the nanoporous material still exhibits higher than expected yield strength.

Existing indentation models (both analytical models and numerical analysis) show a linear relationship between δr/δm and H/Er, where δr and δm are the residual and maximum indentation depth, and Er and H are the reduced Young's modulus and hardness of the test material. Based on the analysis of Oliver and Pharr, a new relationship between δr/δm and H/Er has been derived in a different way without any additional assumptions, which is nonlinear, and this has been verified by finite element analysis for a range of bulk materials. Furthermore, this new relationship for residual depth is used to derive an analytical relationship for the radius of the plastic deformation zone Rp in terms of the residual depth, Young’s modulus, and hardness, which has also been verified by finite element simulations for elastic perfectly plastic materials with different work hardening behavior. The analytical model and finite element simulation confirms that the conventional relationship used to determine Rp developed by Lawn et al. overestimates the plastic deformation, especially for those materials with high E/H ratio. The model and finite element analysis demonstrate that Rp scales with δr, which is sensible given the self-similarity of the indentations at different scales, and that the ratio of Rp/δr is nearly constant for materials with different E/H, which contradicts the conventional view.

Instrumented nanoindentation experiments, especially with sharp tips, are a well-established technique to measure the hardness and moduli values of a wide range of materials. However, and despite the fact that they can accurately delineate the onset of the elasto-plastic transition of solids, spherical nanoindentation experiments are less common. In this article we propose a technique in which we combine (i) the results of continuous stiffness measurements with spherical indenters – with radii of 1 μm and/or 13.5 μm, (ii) Hertzian theory, and (iii) Berkovich nanoindentations, to convert load/depth of indentation curves to their corresponding indentation stress–strain curves. We applied the technique to fused silica, aluminum, iron and single crystals of sapphire and ZnO. In all cases, the resulting indentation stress–strain curves obtained clearly showed the details of the elastic-to-plastic transition (i.e., the onset of yield, and, as important, the steady state hardness values that were comparable with the Vickers microhardness values obtained on the same surfaces). Furthermore, when both the 1 μm and 13.5 μm indenters were used on the same material, for the most part, the indentation stress–strain curves traced one trajectory. The method is versatile and can be used over a large range of moduli and hardness values.

Cu46Zr47Al7 bulk metallic glass (BMG) and its composites in plate with different thicknesses up to 6 mm were prepared by copper mold casting. Primary crystallizing phases with different microstructures and volume fractions could be obtained under different cooling rates, forming some composites with different mechanical properties. Under compression tests, the 2-mm-thick monolithic BMG has a yield strength of 1894 MPa and a high fracture strength of up to 2250 MPa at plastic strain up to 6%, exhibiting apparent “work-hardening” behavior. The 4-mm-thick Cu46Zr47Al7 BMG composite containing martensite phase yields at 1733 MPa and finally fails at 1964 MPa with a plastic strain of 3.7%.

Partial graphitization of carbon nanofibers by high-temperature heat treatment can give improved composite properties. The intrinsic electrical conductivity of the bulk carbon nanofibers measured under compression is maximized by giving the fibers an initial heat treatment at 1500 °C. Similarly, for carbon nanofiber/polypropylene composites containing up to 12 vol% fiber, initial fiber heat treatments near 1500 °C give tensile modulus and strength superior even to composites made from fibers graphitized at 2900 °C. However, optimum composite conductivity is obtained with a somewhat lower heat-treatment temperature, near 1300 °C. Transmission electron microscopy (TEM) along with x-ray diffraction (XRD) explains these results, showing that heat treating the fibers alters the exterior planes from continuous, coaxial, and poorly crystallized to discontinuous nested conical crystallites inclined at about 25° to the fiber axis.

The reliability of microelectronic interconnections depends on hot deformation of solders. In this work, we studied the localized stress relaxation of Sn3.5Ag eutectic alloy using the impression testing in the temperature range of 393–488 K. By incorporating the effect of internal stress in the analysis, we obtained the strain rate-stress exponent of 6.59. The activation energy for the stress relaxation is in the range from 38.6 to 43.8 kJ/mol, which compares well with the estimated activation energy of dislocation pipe diffusion, 46 kJ/mol, in pure tin. This suggests that a single mechanism of dislocation climb limited by dislocation pipe diffusion might be the controlling mechanism for the localized stress relaxation of the Sn3.5Ag eutectic alloy.

An elementary theory for a rigid spherical indenter contacting a thin, linear elastic coating that is bonded to a rigid substrate was developed. This theory predicts that contact area varies as the square root of the compressive load in contrast to Hertz theory where contact area varies as the two-thirds power of the compressive load. Finite element analysis confirmed an approximate square root dependence of contact area on compressive load when the coating thickness-to-indenter radius ratio is less than 0.1 and when the coating Poisson’s ratio is less than 0.45. Thin-coating contact mechanics theories that use either the Derjaguin-Muller-Toporov (DMT) approximation or the Johnson-Kendall-Roberts (JKR) approximation were also developed. In addition, a finite element simulation capability that includes adhesion was developed and verified. Illustrative finite element simulations that include adhesion were then performed for a thin elastic coating (rigid indenter/substrate). Results were compared with the thin-coating contact theories and the transition from DMT-like to JKR-like response was examined.

Studies of RE5(SixGe1-x)4 alloys, where RE equals rare earth, have revealed a second-phase having a thin-plate morphology in essentially every alloy examined, independent of exact composition and matrix crystal structure. Identified as having a composition approximating Gd5(SixGe1-x)3 and a hexagonal crystal structure in the Gd-based system, it has been suggested that the observed thin-plate second phases seen in this family of rare earth alloys are all most likely of the form RE5(SixGe1-x)3. A number of interesting observations suggest that the formation of these second-phase plates is somewhat unusual. The purpose of this article is to investigate the stability of this second phase in Gd- and Er-based compounds. The stability was investigated as a function of thermal cycling and large-scale composition fluctuations. The results of scanning and transmission electron microscopy (SEM, TEM) studies indicate that the RE5(SixGe1-x)3 phase is extremely stable once it forms in a RE5(SixGe1-x)4 matrix.

Ultrasmooth nanostructured diamond (USND) films were synthesized on Ti–6Al–4V medical grade substrates by adding helium in H2/CH4/N2 plasma and changing the N2/CH4 gas flow from 0 to 0.6. We were able to deposit diamond films as smooth as 6 nm (root-mean-square), as measured by an atomic force microscopy (AFM) scan area of 2 μm2. Grain size was 4–5 nm at 71% He in (H2 + He) and N2/CH4 gas flow ratio of 0.4 without deteriorating the hardness (∼50–60 GPa). The characterization of the films was performed with AFM, scanning electron microscopy, x-ray diffraction (XRD), Raman spectroscopy, and nanoindentation techniques. XRD and Raman results showed the nanocrystalline nature of the diamond films. The plasma species during deposition were monitored by optical emission spectroscopy. With increasing N2/CH4 feedgas ratio (CH4 was fixed) in He/H2/CH4/N2 plasma, a substantial increase of CN radical (normalized by Balmer Hα line) was observed along with a drop in surface roughness up to a critical N2/CH4 ratio of 0.4. The CN radical concentration in the plasma was thus correlated to the formation of ultrasmooth nanostructured diamond films.

The effect of surface interaction on nanoindentation testing using a rigid conical indenter is analyzed. A relation between the indentation depth and the indentation load is established as a function of the adhesion energy between the indenter and the surface of an elastic material. A closed-form solution of the contact stiffness for adhesive contact is obtained. The contact stiffness in the presence of surface interaction is always less than that for contact without surface interaction at the same indentation depth, while it is always larger than that for adhesion-less contact subjected to the same indentation load. A lower bound is established, which determines the working zone to operate to avoid the effect of surface interaction in the characterization of the contact modulus.

We present a unique approach combining biological manipulation with advanced imaging tools to examine silica cell wall synthesis in the diatom Thalassiosira pseudonana. The innate capabilities of diatoms to form complex 3D silica structures on the nano- to micro-scale exceed current synthetic approaches because they use a fundamentally different formation process. Understanding the molecular details of the process requires identifying structural intermediates and correlating their formation with genes and proteins involved. This will aid in development of approaches to controllably alter structure, facilitating the use of diatoms as a direct source of nanostructured materials. In T. pseudonana, distinct silica morphologies were observed during formation of different cell wall substructures, and three different scales of structural organization were identified. At all levels, structure formation correlated with optimal design properties for the final product. These results provide a benchmark of measurements and new insights into biosilicification processes, potentially also benefiting biomimetic approaches.

We like to take this opportunity to rectify an error in the schematic drawing in two of our recently published research articles. A typographical error of a number appeared in Fig. 5 of J. Mater. Res. 20, 2225 (2005), p. 2229 and in Fig. 2 of J. Mater. Res. 21, 947 (2006), p. 948: these two figures are the same schematic drawing. In both figures, the number “1” on the slopes should be changed to “2.” The correct figure is given as Fig. 1 in this erratum.