We used x-ray diffractometry (XRD), x-ray photoelectron spectrometry (XPS), and secondary-ion mass spectrometry (SIMS) to investigate the mechanism of the interfacial room-temperature (RT) chemical reaction between cation-deficient La0.56Li0.33TiO3 solid electrolytes and metallic lithium anodes in all-solid-state lithium batteries. A stoichiometric mixture of La2O3, Li2CO3, and TiO2 powders was calcined at 1250 °C for 8 h to obtain a single perovskite structure of La0.56Li0.33TiO3. When this La0.56Li0.33TiO3 sample and lithium were placed in contact at room temperature for 24 h, the phase of the La0.56Li0.33TiO3 remained unchanged. The XPS results indicate that 12% of the tetravalent Ti4+ ions were converted into trivalent Ti3+ ions. The valence conversion and degree of conversion were limited by the structural rigidity of the host crystal. Our SIMS analysis suggests the existence of a local electric field near the contact surface and indicates that the 6Li+ isotope ions were inserted into the specimen through the effect of this field. The change in the electrical properties of La0.56Li0.33TiO3 supports this mechanism for the interfacial reaction. The ionic conductivities of the grain and total grain boundary decreased and increased, respectively, after the insertion of Li+, and the total electronic conductivity increased as a result of the presence of intervalence electron hopping between mixed Ti3+/Ti4+ states. The mechanism of the lithium-activated RT interfacial reaction is associated with the reduction of Ti4+ transition metal ions from tetravalent to trivalent states and the local-electric-field-induced Li+ insertion into La3+/Li+-site vacancies of La0.56Li0.33TiO3.

Ultrathin films (6–10 nm) of silver and nickel were deposited by pulsed laser deposition (PLD) in high vacuum (1 × 10−6 mbar). Microstructural evolution of these films as function of incident laser energy, substrate temperature, substrate material [borosilicate glass, fused silica, MgO(100) and Si (311)] and target–substrate distance was studied in detail using dynamic force microscopy. It is shown that with increase in laser energy incident on the target, there is a substantial increase in particle size in the film. The effect of increased laser energy on microstructure is much more drastic than that for the increase of substrate temperature. In general, denser packing of nanoparticles and increased clustering have been observed at elevated substrate temperature. Increase in laser energy gives rise to higher average grain size, packing density, and clustering in comparison to substrate temperature. It is observed that the aspect ratio of grains is dependent on incident laser fluence and substrate temperature, but more drastically on the substrate material. Substrate coverage and aspect ratio of the grains are particularly dependent on the nature of crystallinity of the substrates. It is demonstrated that PLD provides a greater degree of microstructural manipulation than other physical vapor deposition techniques.

Differential thermal analysis, as the main means of measurement, was used to prepare bulk MgB2 samples and monitor the sintering reaction process. Combined with microstructure observation by scanning electron microscopy and x-ray diffraction analysis, the formation process of MgB2 phase at the temperature before Mg melting was summarized. Additionally, a new kinetic analysis (a variant on the Flynn–Wall–Ozawa) method under nonisothermal conditions was used to determine that the reaction between Mg and B powders involves random nucleation followed by an instantaneous growth of nuclei (Avrami–Erofeev equation, n = 2), which can properly explain the in situ formation process of bulk MgB2 at the temperature before Mg melting. The value of activation energy E and the function of conversion f(α) are obtained independently, and thereby the determination of mechanism function is not affected by the value of E. The values of E decrease from 175.418 to 160.395 kJ mol−1 with the increase of the conversion degrees (α) from 0.1 to 0.8. However, as the conversion degrees approach 0.9, the value of E increases to 222.647 kJ mol−1, and the corresponding pre-exponential factor A is about three orders of magnitude larger than the previous ones.

A stable nano body-centered cubic (bcc) CoFe2 alloy was isolated by employing a combination of N2H4.H2O reduction and sonochemical route under basic conditions. This alloy has proved to be a potential precursor for CoFe2O4 production. X-ray diffraction and transmission electron microscopy confirms the formation of a bcc phase CoFe2 alloy with particle size <10 nm and spherical morphology. Thermogravimetric analysis confirmed the oxidation of the alloy composition showing a weight gain between 200 and 500 °C, which corresponds to fully oxidized CoFe2O4. A significant increase in the saturation magnetization (Ms = 230 emu/g) for the nano CoFe2 alloy was observed in comparison with that of the theoretical bulk value (200 emu/g) at 300 K.

A Raman spectrometer was used to probe the structure and luminescence of a range of europium-doped zirconia phosphors prepared by different routes. We have demonstrated that the synthesis method and precursor type have a strong influence on the structure and luminescence of the final phosphor product. Raman spectroscopy has also demonstrated the presence of local order around the dopant ions that is not apparent in x-ray diffraction (XRD) and corresponds with changes in luminescence. As europium concentration is increased from 1 mol% to 20 mol%, the long range structure (from XRD) changes from tetragonal to cubic. Raman spectroscopy, however, shows that the 1 mol% material has a localized structure similar to the monoclinic undoped zirconia. This localized symmetry can explain the differences observed previously in emission spectra.

The deformation behavior of diamondlike carbon (DLC) coatings on silicon substrates induced by Berkovich indentation has been investigated. DLC coatings deposited by a plasma-assisted chemical vapor deposition technique were subjected to nanoindentation with a Berkovich indenter over a range of maximum loads from 100 to 300 mN. Distinct pop-ins were observed for loads greater than 150 mN. However, no pop-out was observed for the loads studied. The top surface of the indents showed annular cracks with associated fragmented material. The cross sections showed up to 20% localized reduction in thickness of the DLC coating beneath the indenter tip. Cracking, {111} slip, stacking faults, and localized phase transformations were observed in the silicon substrate. The discontinuities in the load–displacement curves at low loads are attributed to plastic deformation of the silicon substrate, whereas at higher loads they are attributed to plastic deformation as well as phase transformation.

This is the second in a series of articles demonstrating the unique character of the aerosol-through-plasma (A-T-P) process for producing nanoparticles. This study is focused on the impact of two parameters, cation ratio (1:3, 1:1, 3:1) and solvent (evaporated prior to generation of aerosol), on the structures of Ce:Al oxides particles. These two simple changes were found to impact virtually every aspect of particle structure, including the fraction of hollow versus solid, fraction of nanoparticles, phase structure, and even the existence of surface phase segregation. CeAl mixed oxides were found only over a limited range of compositions, and that range was a function of the solvent. At all other cation ratios, only ceria was a crystalline phase, and most if not all the alumina is amorphous. It is notable that the fraction of hollow micron-sized particles and nanoparticles is greatly influenced by the cation ratio and solvent identity. Indeed, significant numbers of nanoparticles were only produced using an aqueous precursor with a Ce:Al ratio of 1:1. Another unique finding is that phase segregation exists in individual particles on the length scale of nanometers. This study compliments an earlier study of the influence of operating conditions on particle structure. Taken together, the studies suggest a means to engineer (as well as limits to the engineering possibilities) ceramic particle structures using the A-T-P method.

Microstructural evolution occurred in 5Sn–95Pb/63Sn–37Pb composite flip-chip solder bump during electromigration. Scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) observations for 5Sn–95Pb/63Sn–37Pb composite flip-chip solder joints subjected to 5 kA/cm2 current stressing at 150 °C revealed a gradual orientation transformation of Pb grains from random textures toward (101) grains. We proposed that the combination of reducing the surface energy of Pb grain boundaries and resistance of the entire polycrystalline system are the driving force for the orientation transformation of Pb grains during an electromigration test.

ZrC-based composites were produced by pressureless sintering thanks to the addition of MoSi2 as sintering aid. After preliminary tests, a baseline ZrC material and two mixed ZrC–HfC and ZrC–ZrB2 composites with 20 vol% MoSi2 were densified at 1900 to 1950 °C reaching final relative densities of 96%–98%. Mean particle size of the dense bodies ranged from 5 to 9 μm. Secondary phases were found to form during sintering, such as SiC and Zr–Mo–Si-based compounds. Room-temperature mechanical properties were in the range of the values reported in the literature for similar materials densified by pressure-assisted techniques. The flexural strength was tested at room temperature, 1200 and 1500 °C.

In this paper, we report on the multicolor luminescence in oxygen-deficient Tb3+-doped calcium aluminogermanate glasses. A simple method was proposed to control oxygen-deficient defects in glasses by adding metal Al instead of the corresponding oxide (Al2O3), resulting in efficient blue and red emissions from Tb3+-undoped glasses with 300 and 380 nm excitation wavelengths, respectively. Moreover, in Tb3+-doped oxygen-deficient glasses, bright three-color (sky-blue, green or yellow, and red) luminescence was observed with 300, 380, and 395 nm excitation wavelengths, respectively. These glasses are useful for the fabrication of white light-emitting diode (LED) lighting.

Sn–0.7 wt% Cu alloy is an important Pb-free solder, and Ni–7 wt% V is the major diffusion barrier layer material of flip chip technology. Reactions at the Sn–0.7 wt% Cu/Ni–7 wt% V interface are examined at 160, 180, and 210 °C. Only the Cu6Sn5 phase is formed in the Sn–0.7 wt% Cu/Ni–7 wt% V couple reacted at 160 and 180 °C; however, in addition to the Cu6Sn5 and Ni3Sn4 phases, a quaternary Q phase is formed in the Sn–0.7 wt% Cu/Ni–7 wt% V couple reacted at 210 °C. The Q phase is a mixture of nanocrystalline Ni3Sn4 phase and an amorphous phase. With longer reaction time at 210 °C in the Ni–V/Q/Sn–Cu couple where the Q phase is in direct contact with solder, the Ni3Sn4 phase nucleates inside the preformed Q phase, and the alternating layer phenomenon Ni–V/Q/Ni3Sn4/Q/Ni3Sn4/Cu6Sn5/Sn–Cu is observed. The interesting solid state amorphization and alternating layer phenomena at 210 °C are primarily caused by the fact that Sn and Cu are fast diffusing species, while V is relatively immobile.

As a liquid moves in the nanopores of a silica gel, because of the hysteresis of sorption behavior, significant energy dissipation can take place. Through a calometric measurement, the characteristics of associated heat generation are investigated. The temperature variation increases with the mass of silica gel, which consists of a reversible part and an irreversible part. The residual temperature change is about 30% to 60% of the maximum temperature increase and can be accumulated as multiple loading cycles are applied.

Crystalline samples of zinc oxide on a mesoporous amorphous silica substrate were prepared by 5 to 15 atomic layer deposition cycles with diethyl zinc and water at 150 °C. Samples were characterized by x-ray diffraction, thermogravimetry, and nitrogen adsorption–desorption isotherms. High-temperature oxide melt solution calorimetry and water adsorption calorimetry experiments were performed to measure surface enthalpy for crystalline ZnO particles supported on the substrate. The measured enthalpies 1.23 ± 0.35 and 2.07 ± 0.59 J/m2 for hydrous and anhydrous surfaces, respectively, are in agreement with previously reported measurements for unsupported ZnO nanoparticles. Feasibility of thermochemical characterization of complex system of atomic layer deposition (ALD) prepared particles on a substrate was demonstrated.

Pure CdSe and Mg-doped CdSe nanocrystal quantum dots were synthesized into the zinc-blende structure at a low temperature by the inverse micelle technique using paraffin oil and oleic acid as surface capping agents. The ripening behavior of the nanocrystals was monitored using the red shift in ultraviolet (UV)-visible light absorption peaks, and their size variation was estimated using the so-called, quantum confinement theory. The Lifshitz–Slyozov–Wagner (LSW) kinetics analyses were performed based on the variation in size according to the ripening temperature and time period. The activation energy (Q) and reaction rate constant (Ko) were determined for the ripening reaction using Arrhenius-type plots. The kinetics analyses reveal that the volume diffusion through the liquid-phase solution is the governing mechanism for the ripening of both nanocrystals. The Mg-doped CdSe nanocrystals showed enhanced ripening kinetics due to the low activation energy for the volume diffusion.

Nickel ferrite nanostructured particles coated with chemisorbed oleic acid were successfully synthesized by nonhydrolytic sol-gel method. By varying the composition of metal precursors, two microstructures were obtained, i.e., dispersed nanocrystals (9.7 ± 1.8 nm) and submicron aggregates (152 ± 21 nm) consisted of many nanocrystals (8.1 ± 1.3 nm). Because oleic acid could form complex with iron (III) ions, but not with nickel (II), increasing the concentration of iron precursor consumed more oleic acid and led to insufficient oleic acid coating on particle surface. Strong intercrystallite interaction was induced from less protected nanocrystals, and aggregation thus occurred between different crystallites.

A novel technique based in the combination of vapor silanization and chemical vapor deposition, hereafter referred to as activated vapor silanization (AVS), is shown to be an effective biofunctionalization technique. The AVS process results in thin organic films with a high surface amine concentration when deposited on substrates with different chemical characteristics, such as silicon, porous silicon, or gold. Chemical characterization shows that the films are composed of carbon (hydrocarbon, C–Si, C–C), silicon (different oxidation states), nitrogen (primary and secondary amines), oxygen, and hydrogen. Relevantly, the amines are also distributed along the film thickness, ensuring functionality even after some degradation of the films. AVS films behave practically as monocrystalline silicon substrates under loading–unloading tests. In addition, the AVS films behave as permeable membranes for molecules smaller than 5 Å, and the amine surface concentration is estimated to be 8 NH2/nm2 for molecules of about 12 Å, which is three times higher than that obtained with standard silanization procedures.

The formation of bulk metallic glasses (BMGs) and their room temperature mechanical properties have been investigated in a serial of Ni65−xZr20Nb15Pdx (x = 0∼15; at.%) quaternary alloys, which are hopefully hydrogen-permeation materials. The partial substitution of Ni with Pd in Ni65Zr20Nb15 alloy has proved to be effective in improving glass-forming ability (GFA) and thermal stability. In particular, good BMG-forming compositions were revealed within the Pd content range of 2.5–12.5 at.%, and BMG rods of 3 mm in diameter were successfully made at compositions Ni57.5Zr20Nb15Pd7.5 and Ni55Zr20Nb15Pd10 by copper mold casting. The addition of Pd enhanced the thermal stability of the supercooled liquid. With an increase of Pd content, the supercooled liquid span, ΔTx = Tx − Tg, increased from 29 K at Ni65Zr20Nb15 to 47 K at Ni52.5Zr20Nb15Pd12.5. The Pd-bearing BMGs exhibited high fracture strength, which ranged from 2750 to 2850 MPa. These Pd-bearing BMGs showed a certain degree of toughness, and the highest plastic strain, about 2%, was reached in the Ni60Zr20Nb15Pd5 BMG.

Dopamine covalently chelated ZnO nanoparticles were synthesized by a nonaqueous one-step chemical process at a temperature as low as 60 °C. The formation of ZnO/dopamine hybrid structure was proved by x-ray powder diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) techniques. Detailed absorption, luminescence, and time-resolved decay studies were performed for these ZnO/dopamine hybrid nanoparticles. We observed an enhanced green emission, which could be assigned to a new band-gap emission based on the fast of nanosecond lifetime of the green emission. Our results demonstrated that the change of optical properties of ZnO nanoparticles after covalently chelated by dopamine ligands is closely associated with the formation of new band 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.

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.