It was recently revealed that some processes of hydrating tricalcium silicate are altered by the addition of dicalcium silicate. Previous neutron scattering results revealed two critical tri/dicalcium silicate compositions. At one composition, changes in the early time hydration kinetics were observed that result in the formation of more products (reflected in increased 28 day strength), despite dicalcium silicate being essentially unreactive at early times. At the other composition, changes in the early-time hydration kinetics were observed that correspond to reduced strength. The current work uses scanning electron microscope analysis with backscattered electron imaging of 50 day hydrated tri- and dicalcium silicate mortars to reveal that at the former critical composition increased hydration of the tricalcium silicate phase occurs, and at the latter critical composition, the amount of dicalcium silicate reacted is decreased.

Ti–Si–O thin films were deposited using an aerosol chemical vapor deposition process at atmospheric pressure. The film structure and microstructure were analyzed using several techniques before and after thermal annealing. Diffraction results indicate that the films remain x-ray amorphous after annealing, whereas Fourier transform infrared spectroscopy gives evidence of a phase segregation between amorphous SiO2 and well-crystallized anatase TiO2. Crystallization of anatase TiO2 is also clearly shown in the Raman spectra. Transmission electron microscopy analysis indicates that anatase TiO2 nanograins are embedded in a SiO2 matrix in an alternated SiO2/TiO2 multilayer structure.

The combustion synthesis of Al50Ir48Ni2 (at.%) was conducted at different heating rates in both a differential scanning calorimetry (DSC) chamber and a vacuum furnace. It was found that a higher heating rate, a sufficient amount of reactant powder, and effective control of the heat loss facilitated the complete reaction and resulted in combusted single IrAl phase products. Otherwise, multiphase products containing IrAl, unreacted Ir, and Al3Ir were synthesized. The reactions involved in different processes were discussed in terms of the thermal competition between heat generation and loss during the reaction. All ignition temperatures were below 773 K, indicating that the combustion reaction occurs at the solid–solid state. With increasing heating rate, the ignition temperature increased while the product density decreased.

It will be shown that in the considered paper, a mistake occurred by handling or editing of experimental data for one of two investigated materials, namely, for cubic germanium nitride having spinel structure (γ-Ge3N4). This mistake led to incorrect values of the shear modulus G0, Young’s modulus E0, and Poisson’s ratio ν0 of this compound. My effort to recover the elastic moduli of γ-Ge3N4 from the available data gave the following results: G0 = 124 GPa, E0 = 326 GPa, and ν0 = 0.32.

Part I [D.J. Morris and R.F. Cook, J. Mater. Res.23, 2429 (2008)] of this two-part work explored the instrumented indentation and fracture phenomena of compliant, low-dielectric constant (low-κ) films on silicon substrates. The effect of film thickness and probe acuity on the fracture response, as well as the apparent connection of this response to the perceived elastic modulus, were demonstrated. These results motivate the creation of a fracture model that incorporates all of these variables here in Part II. Indentation wedging is identified as the mechanism that drives radial fracture, and a correction is introduced that adjusts the wedging strength of the probe for the attenuating influence of the relatively stiff substrate. An estimate of the film fracture toughness can be made if there is an independent measurement of the film stress; if not, a critical film thickness for channel-cracking under the influence of film stress may be estimated.

This article is focused on a fractography study of cleavage cracking at triple grain boundary junctions in freestanding silicon thin films. At a triple junction, as the crystallographic orientations of the two grains ahead of the crack are different by only a few degrees, the cleavage front advance becomes quite jerky. The crack first enters the grain of smaller boundary toughness and then turns into the other grain from the lateral direction. Consequently, the overall fracture resistance cannot be analyzed in the framework of line-average theory. The nonuniform characteristic of crack behavior can be attributed to the increase in local stress intensity. A few typical crack front advance modes are identified.

Bulk samples of an ultrafine-grained tungsten–tantalum composite alloy have been synthesized by consolidating mechanically milled composite powders. The grain growth during densification is limited due to the submicron-scale layering of the individual metals in the composite particles and the relatively low sintering temperature (1300 °C). The ultrafine microstructure of the high-density (∼99% theoretical density) samples leads to a high yield stress of ∼3 GPa under quasi-static uniaxial compression. A tendency for Ta-rich solid-solution formation during densification was observed, and the high-temperature phase equilibria in the composite powders were examined further using high-energy x-ray diffraction at temperatures up to 1300 °C.

Three different strategies, wet impregnation, in situ reduction, and grafting with silane coupling agents, have been used to introduce CoNi nanoparticles with different existing forms into mesoporous silica. These composites were used as catalysts to grow nanostructured carbons by catalytic chemical vapor deposition using ethene. Carbon nanotubes (CNTs) with different inner diameters can grow out of mesoporous silica particles incorporated with CoNi nanoclusters. Many fewer CNTs could be found in the pore channels of the sample prepared by using silane coupling agents than in those of the sample synthesized via wet impregnation. No CNTs formed in the pore channels of the sample prepared by in situ reduction. After the removal of silica, different carbon nanostructures have been obtained in the pore channels. Ordered graphite carbon mesostructure was obtained from the sample prepared by in situ reduction. Highly dispersed metal catalysts inside mesopore channels are favorable for the formation of graphite carbons with ordered mesostructures.

The structure evolution and oxidation behavior of ZrB2–SiC composites in air from room temperature to ultrahigh temperature were investigated using furnace testing, arc jet testing, and thermal gravimetric analysis (TGA). The oxide structure changed with the increasing temperature. SiC content has no apparent influence on the evolution of structure during the oxidation of ZrB2–SiC below 1600 °C. However, the evolution of structure for ZrB2–SiC above 1800 °C was significantly affected by the SiC content. The formation of the SiC depleted layer in the ZrB2–SiC system not only depends on the surrounding conditions of pressure and temperature but also on the structure distribution of the SiC in the ZrB2 matrix. The apparent recrystallization of the ZrO2 occurred above 1800 °C. The SiC content should be controlled at ∼16% in the ZrB2–SiC system for the ultrahigh-temperature application. The mechanisms of the structure evolution during oxidation in air were also analyzed.

Hollow capsules have been intensively investigated due to their high capacity of encapsulating large quantities of guest molecules, making them promising candidate materials for various encapsulation applications. In this work, CaCO3 hollow capsules were successfully synthesized via an emulsion route. The interior hollow structure of the capsules was confirmed by using scanning electron microscopy and transmission electron microscopy (TEM). The vaterite polymorph of the as-synthesized CaCO3 capsules was determined by using x-ray diffraction, high-resolution TEM, and Fourier transform infrared spectroscopy. A self-assembly model was proposed to explain the formation mechanism of the vaterite capsules. By adjusting experimental parameters such as the internal solution amount and the surfactant amount of the double-emulsion system, the average capsule size could be adjusted accordingly. However, the increase in capsule size was at a compensation of size-uniformity degradation. The capsule size uniformity was then further optimized by increasing the magnetic stirring rate. The resultant vaterite capsules demonstrated biodegradability behavior after immersion in phosphate-buffered saline solution, leading to their promising applications in the area of controlled drug delivery.

A post heat treatment of reaction-sintered SiC at 1700 °C in nitrogen atmosphere significantly reduced electrical resistivity. A trace of insulating Si3N4 phase was detected via nitrogen heat treatment in high-resolution transmission electron microscopy observation; however, based on x-ray photoelectron spectroscopy, the evidence of nitrogen doping into SiC lattice has been claimed as the mechanism to the decreased resistivity. The increase of the total volume of SiC was apparent in x-ray diffraction during the nitrogen heat treatment, which was interpreted to stem from the growth of the nitrogen-doped intergranular SiC particles and surface doping of the primary SiC to reduce the contact resistance between the primary SiC particles.

The (Ga1−xMnx)N nanorods were grown on Al2O3 (0001) substrates by using rf-associated molecular beam epitaxy. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected-area diffraction pattern (SADP) results showed that the (Ga1−xMnx)N nanorods had (0001) preferential orientations. XRD patterns showed that the (Ga1−xMnx)N nanorods contained a small number of grains with different preferred orientations. High-resolution TEM (HRTEM) images showed that the (Ga1−xMnx)N nanorods consisted of different preferentially oriented grains. The initial formation mechanisms for the (Ga1−xMnx)N nanorods grown on Al2O3 (0001) substrates are described on the basis of the XRD, the TEM, the SADP, and the HRTEM results.

A combustion synthesis method for the synthesis of α-Si3N4 from a reactant compact composed of Si, NaN3, and NH4X and wrapped up with an igniting agent was investigated. Wrapping the reactant compact with the igniting agent (i.e., a mixture of Ti and C powders) was found necessary for the synthesis of Si3N4. In addition to NH4Cl, which was considered previously to function as a catalytic agent, other ammonium halides (i.e., NH4F, NH4Br, and NH4I) were found to be capable of catalyzing the synthesis reaction with NH4Cl being the most effective. Si3N4 could not be produced when NaN3 was replaced by C3H6N6. NaN3 was thus considered to exert an essential effect on the combustion synthesis reaction other than functioning as a solid-state nitrogen source as considered previously. It was proposed that Na vapor produced by decomposition of NaN3 reduces SiXx (formed by reaction of Si and NH4X), promoting the nitridation reaction to form Si3N4. NaN3 thus plays a role as a reducing agent in the synthesis reaction.

The structure and configuration of threading dislocations (TDs) in AlN films grown on (0001) sapphire by metal–organic vapor phase epitaxy (MOVPE) were characterized by high-resolution transmission electron microscopy (HRTEM). It was found that the TDs formed in the films were mainly the perfect edge dislocations with the Burgers vector of b = ⅓〈11¯20〉. The majority of the edge TDs were not randomly formed but densely arranged in lines. The arrays of the edge TDs were mainly observed on the {11¯20} and {10¯10} planes. These two planes showed different configurations of TDs. TD arrays on both of these planes constituted low-angle boundaries. We suggest that these TDs are introduced to compensate for slight misorientations between the subgrains during the film growth.

The coexistence of high Fe content and high glass-forming ability (GFA) has been earnestly desired from academia to industry. We report a novel Fe76Si9B10P5 bulk metallic glass with an unusual combination of high magnetization of 1.51 T due to high Fe content as well as high GFA leading to a glassy rod with a diameter of 2.5 mm despite not containing any glass-forming metal elements. This alloy composed of familiar and low-priced elements, also exhibiting very excellent magnetic softness, has a great advantage for engineering and industry, and thus should make a contribution to energy saving and conservation of earth’s resources and environment.

Small-scale depth-sensing indentation (nanoindentation) is a popular technique for measuring the mechanical properties of a wide range of materials. Contact mechanics solutions used in data analysis are based on the indentation of a homogeneous half-space, but the experiments are frequently conducted on mineralized biological tissues—biocomposite materials with nanometer-scale features—such as bone and dentin. The current study examines the experimental indentation response of bone across orders of magnitude in contact dimension length-scale, from nanometers to micrometers. Scaling arguments are used to establish the need for nanoscale simulations of mineralized tissue indentation. A finite element model of an inhomogeneous contact problem is developed and used to interpret experimental indentation data on bone and dentin. Both experimental data and modeling results demonstrate a convergence in apparent elastic modulus at increasing contact length-scales. Models results are used to estimate a feature size associated with inhomogeneity of the indentation response; for experiments conducted here the characteristic feature size is found to be substantially larger for bone than for dentin, and in both cases larger than for individual nanometer-scale mineral platelets.

Direct current (dc) electrodeposition was used to co-deposit cobalt and antimony in citric-based solutions. Growth behavior of Co–Sb alloy thin films was systematically studied under various deposition conditions. Effects of deposition parameters (i.e., deposition potential, cobalt sulfate concentration, and pH value) on the microstructure, chemical, and phase composition of the deposited materials were also studied and are discussed in detail.

MgO thin films are widely used in plasma display panels (PDPs) to protect the dielectric layer, which is composed of PbO2, B2O3, and SiO2 compound, against ion bombardment during discharge. To improve the electrical properties of the MgO thin films, (Ba,Sr,Ca)CO3 or LaB6, which has a lower work function than that of MgO, added to the MgO films. The effects of (Ba,Sr,Ca)CO3 or LaB6 addition on the electrical properties, microstructure, and electronic band structure were investigated. In the case where (Ba,Sr,Ca)CO3 was added, the firing voltage, which is the voltage when the panel is ignited the first time during increasing input voltage, was about 18.4 V lower than that of the conventional MgO films. In the case where LaB6 was added, the firing voltage was also reduced by about 24 V. The luminance and luminous efficiency were also increased. Of particular interest was the valence band spectra changed after adding (Ba,Sr,Ca)CO3 or LaB6. The valence band edge, which is the top of the valence band, was shifted to lower binding states and the width of the valence band was increased. Moreover, the band gap was slightly reduced. Considering the emission mechanism of MgO films in plasma display panels, these results mean that the secondary electrons can be ejected more easily and the ejected electrons have more energy. Therefore, the addition of (Ba,Sr,Ca)CO3 or LaB6 might improve the electrical properties.

The effects of ball milling on lithium (Li) insertion/extraction properties into/from single-walled carbon nanotubes (SWNTs) were investigated. The SWNTs were synthesized on supported catalysts by thermal chemical-vapor deposition method, purified, and mechanically ball-milled by high-energy ball milling. The purified SWNTs and the ball-milled SWNTs were electrochemically inserted/extracted with Li. The structural and chemical modifications in the ball-milled SWNTs change the insertion/extraction properties of Li ions into/from the ball-milled SWNTs. The reversible capacity (Crev) increases with increase in the ball milling time, from 616 mAh/g (Li1.7C6) for the purified SWNTs to 988 mAh/g (Li2.7C6) for the ball-milled SWNTs. The undesirable irreversible capacity (Cirr) decreases continuously with increase in the ball milling time, from 1573 mAh/g (Li4.2C6) for the purified SWNTs to 845 mAh/g (Li2.3C6) for the ball-milled SWNTs. The enhanced Crev of the ball-milled SWNTs is presumably due to a continuous decrease in the Cirr because the SWNTs develop a densely packed structure on the ball milling process. The insertion of Li ions into the ball-milled SWNTs is facilitated by various Li insertion sites formed during the ball milling process in spite of small surface area than the purified SWNTs. Lithium ions inserted into various insertion sites enhance the Crev in the ball-milled SWNTs with the large voltage hysteresis by hindrance of the extraction of Li ions from the ball-milled SWNTs. In addition, the ball-milled samples exhibit more stable cycle capacities than the purified samples during the charge/discharge cycling.

The surface enthalpy of ZnO nanoneedles has been measured by oxide melt solution calorimetry of samples with different surface areas. Water adsorption calorimetry was carried out to characterize the stabilization effect of surface hydration. The surface enthalpies of hydrated and anhydrous surfaces (8.21 ± 0.67 and 9.81 ± 0.69 J/m2, respectively) are larger than those of nanorods. The less stable surface of nanoneedles provides a driving force for the transformation of nanoneedles into nanorods during aging. The formation of bushlike assemblies of nanoneedles is also discussed.