A low-temperature plasma-enhanced atomic layer deposition (PEALD) process has been developed for the growth of ultrathin WNxCy films, using a halide-free W precursor. A 32-nm-thick PEALD WNxCy film deposited using this process at 250 °C possesses a composition of W72C20N5, resistivity of ∼250 μΩ·cm, a root-mean-square (rms) surface roughness of 0.23 nm, and a thickness conformality of more than 80% on trench structures with a width of 120 nm and an aspect ratio of 11. The WNxCy films exhibited excellent thermal stability, whereby resistivity, thickness, surface roughness, and crystal structure were stable after 30 min anneals in 700 Torr, forming gas ambient at temperatures up to 700 °C. Copper diffusion barrier performance measurements show that a 9 nm thick WNxCy film could prevent copper diffusion after a 30 min anneal at 700 °C, while a 2-nm-thick film could prevent copper diffusion after a 30 min anneal at 500 °C.

We demonstrate that diffusion of aqueous buffered solutions into strongly hydrophobic nanoporous methyl silsesquioxane glass films can occur without the application of external pressure. The organic component of these glasses in the form of methyl groups imparts the strong hydrophobicity and perception that they are impervious to the ingress of aqueous solutions by capillary action or diffusion. The presence of small concentrations of organic buffering agents in buffered solutions appears to facilitate the diffusion. The diffusion distance followed a square root of time dependence characteristic of Fick’s Law. The diffusion coefficients varied markedly with the concentration of buffering agents, solution pH, and temperature. Similar effects were not observed for nonbuffered solutions that exhibited no detectable diffusion. Likely mechanisms responsible for the observed behavior are proposed.

We investigated the acoustic properties in the sub-GHz frequency regime of a multilayer system comprising alternating 100-nm scale TiO2/poly(methyl methacrylate) (PMMA) layers through a laser photoacoustic method, impulsive stimulated thermal scattering (ISTS). The acoustic dispersion curves were determined, and the mechanical properties were extracted from the experimental results.

The nucleation mechanism of deformation-induced martensite was investigated by x-ray diffraction and transmission electron microscope in an ultra-low carbon austenitic stainless steel deformed by equal channel angular pressing at room temperature. It was found that two types of martensite transformation mechanism, stress-assisted and strain-induced, occurred via the sequences of γ (fcc) → ɛ (hcp) → α′ (bcc) and/or γ → α′. In both cases, the crystallographic relationships among γ, ɛ, and α′ followed the Kurdjumov-Sachs orientation relationships: {111}γ //{0001}ɛ //{011}α′ and 〈110〉γ//〈1120〉ɛ//〈111〉α′.

The effects of ionic doping in Bi0.5Na0.5TiO3 (BNT) ceramics were investigated. Pure and doped BNT samples containing 0 to 16 at.% Ba2+ and 0 to 1.0 at.% Ce4+ were synthesized at 1135 to 1200 °C for 2 h in ambient atmosphere. Temperature dependences of dielectric properties were analyzed. These results suggest that Ba2+ and Ce4+ replace the ions in A and B sites of perovskite structures, and the lattice structure is altered. The component differences of each crystal domain lead to variance of phase transition temperature, which enhances the relaxation character in BNT ceramics, and the dielectric properties were consequently improved.

Eutectic SnPb solder has been widely used in packaging for several decades. The stability of the interface between solder and under-bump metallization (UBM) is an important issue that has led to many studies. Even though Ni atoms dissolve much slower into SnPb solder than Cu, the intermetallic compound, Ni3Sn4, which forms when eutectic SnPb solder reacts with Ni(V)/Ti UBM, is not stable on Ti layer, creates V-rich zone, and causes spalling. To prevent the phenomenon, and the resulting reduction of mechanical reliability in solder joints, we propose the addition of a layer of Cu thin film to serve as a sacrificial layer. Both eutectic SnPb solder and composite solder (high-Pb solder with eutectic SnPb solder) were studied in severe reflow conditions to simulate the worst case of die attach and later reflow process. Cu film first was consumed completely to form a compound. Due to lower interfacial energy between Cu6Sn5 and Ni(V), the interface was stable and no spalling occurred. However, the same thickness of Cu was insufficient to prevent Ni from diffusing into solder or compound. Not only diffusion of Ni atoms was observed; Sn atoms also diffused into the Ni(V) layer. The Sn–Ni reaction caused the interface between the compound and Ni(V) to retreat into the Ni(V) layer. The compound was not stable at the interface, and spalling could be seen. Due to the interdiffusion of Ni and Sn, many Kirkendall voids were also observed at both side of the interface.

Molecular dynamic simulation was used to study the melting behavior of gallium nitride (GaN) nanowires with the Stillinger-Weber potential. Our results reveal that the melting of the nanowires starts from the surface and rapidly extends to the inner regions of nanowires as temperature increases. The melting temperatures increase to saturation values ∼3100 and ∼2900 K when the diameters of nanowires are larger than 3.14 and 4.14 nm for the nanowires with [100]- and [110]-oriented lateral facets, respectively. The saturated values are close to the melting temperature of bulk GaN. The low melting temperature of GaN nanowires with small diameter may be associated with the large surfaces of nanowires.

Sputtered amorphous Ge4Sb1Te5, Ge1Sb2Te4, Ge2Sb2Te5, and Ag0.055In0.065Sb0.59Te0.29 thin films were studied by differential scanning calorimetry. Upon continuous heating, heat release due to structural relaxation of the amorphous phase between 0.5 and 1.0 kJ/mol was observed. This value depends on the thermal history of the sample. Preannealing of the amorphous phase revealed the glass transition temperature Tg within 10 K of the crystallization temperature upon continuous heating at 40 K/min.

Biomorphic SiO2 fibers were synthesized with cotton tissue as the template and with cetyltrimethylammonium bromide (CTAB) as surfactant through a surface sol-gel process. The as-prepared samples retain well the original morphology of cotton and show a uniform and large amount of nanopores. Sliver nanoparticles were successfully incorporated into the nanopores through impregnation and chemical reduction to form SiO2/Ag composite fibers. Ag nanoparticles with mean diameter approximately 3 nm have a size distribution in accordance with the nanoporosity of SiO2 matrix. Such composite fibers show prominent surface plasma resonance (SPR) effect, and during heat treatment under increasing temperatures, the SPR intensity is enhanced because of the size effect, and the SPR position undergoes a redshift first and then a blueshift.

The electromigration-induced failure in flip-chip eutectic SnPb solder joints with a 10-μm-thick Cu under-bump metallization (UBM) was studied without the effect of current crowding in the solder region. The current crowding occurred inside the UBM instead of in the solder joint at the current density of 3.0 × 104 A/cm2 because of the spreading of current in the very thick Cu UBM. In these joints, the failure occurred through a two-stage consumption of the thick Cu UBM in the joint where electrons flowed from the chip to the substrate. In the first stage, the Cu UBM dissolved layer by layer rather uniformly across the entire Cu UBM–solder interface. In the second stage, after half of the Cu UBM was dissolved, an asymmetrical dissolution of Cu UBM took place at the corner where electrons entered from the Al interconnect to the Cu UBM. Experimental observation of dissolution steps of the 10-μm-thick Cu UBM is presented. The transition from the first stage to the second stage has been found to depend on the location of current crowding in the flip-chip joints as the UBM thickness changes during the electromigration test. The current distribution in the flip-chip solder joints as a function of UBM thickness was simulated by three-dimensional finite element analysis. The dissolution rate of Cu UBM in the second stage was faster than that in the first stage. The mechanism of electromigration-induced failure in the flip-chip solder joints with a 10-μm-thick Cu UBM is discussed.

Copper was supplied to Sn–3.5Ag by electroplating Cu/Ni double under-bump metallization (UBM), and the amount of Cu was controlled by varying the Cu UBM thickness. Supposed Cu contents in the solder were; 0.2, 0.5, and 1.0 wt%, respectively, and the solder joint microstructure was investigated after 1, 5, and 10 reflows. In the case of specimens with 0.2 and 1.0 wt% Cu, only one type of intermetallic compound (IMC) formed, either (Cu,Ni)6Sn5 or (Ni,Cu)3Sn4, while two types formed in specimen with 0.5 wt% Cu. No correlation could be found between the solder joint microstructure and the ball shear test. However, drop test results showed two opposite trends. The drop resistance of 0.2 and 1.0 wt% Cu specimens was quite good initially but degraded dramatically with multiple reflows, in contrast to that of the 0.5 wt% Cu specimen, which was very poor after one reflow but improved substantially later on. The former was ascribed to thickening of IMC during reflow, while the latter was related to (Ni,Cu)3Sn4 thickening beneath (Cu,Ni)6Sn5 and subsequent spalling of (Cu,Ni)6Sn5 from (Ni,Cu)3Sn4.

The effects of the molecular weight and concentration of poly(acrylic acid) (PAA) with different primary abrasive sizes in ceria slurry on the nitride film loss, removal rate, film surface roughness, and removal selectivity of SiO2-to-Si3N4 films were investigated by performing chemical mechanical polishing (CMP) experiments using blanket and patterned wafers. In the case of the blanket wafers, we found that for a lower PAA molecular weight, the removal selectivity of SiO2-to-Si3N4 films increased more significantly with increasing PAA concentration in slurry containing a larger primary abrasive size. For the patterned wafers, with a higher PAA molecular weight in the ceria slurry suspension, the erosion of the Si3N4 film was less, but the removed amount was also smaller, and the surface roughness became worse after CMP. These results can be qualitatively explained by the layer of PAA adsorbed on the film surface, in terms of electrostatic interaction and rheological behavior.

The structural transformation of natural montmorillonite clay with different acids and superacids (hydrochloric, HCl; sulfuric, H2SO4; hydrofluoric, HF; perchloric, HClO4; chlorosulfonic, HSO3Cl; and trifluoromethanesulfonic, HSO3CF3 acids) is evaluated by various techniques, allowing its full characterization. The process involves the modulated digestion of the aluminum and silicon atoms from the original clay without the loss of the original mass in the material from a careful drying methodology. The x-ray diffraction technique suggests that the process is disruptive, causing different magnitudes of modification, depending on the acidic source, taking the material with natural lamellar structure as reference. By 27Al and 29Si magnetic resonance, it is also shown that all the silicon and aluminum atoms were removed from the chemical structure to be physisorbed or dispersed in the interstices of the clay lattice when HF, HSO3Cl, and H2SO4 acid treatments were carried out. However, with treatment of HClO4, the results suggest that only was achieved partial digestion and physisorption of the aluminosilicate core. Treatment with HCl led to a mild digestion that increased the laminar distance of the montmorillonite. Finally, HSO3CF3 acid achieved a total disorder of the lamellar structure of the clay. In addition, by infrared spectrometry, the disappearance of the absorption peaks assigned to Al2OH, AlMgOH, and Al-O-Si are other evidence of the complete digestion of silicon and aluminum atoms caused by the acidic medium. On the other hand, the Brunauer–Emmett–Teller (BET) surface areas of the acidified clays showed a great enlargement in comparison with the unmodified clay. The porosimetry measurements demonstrate the presence of mesopores and hysteresis as observed in the physisorption isotherms, which indeed exhibited a capillary condensation into the porous structures. The present results are the first full characterization research and structural comparison between the acidic and the not-extensively-studied superacidic modified clays of this type.

The role of MgAl2O4 spinel particle dispersion for attaining high-strain-rate superplasticity (HSRS) was examined in tetragonal ZrO2. Microstructural examination shows that the dispersed spinel particles provide the following positive factors to ZrO2 simultaneously: (i) stable fine grain size by retarding grain growth due to pinning effect; and (ii) enhanced accommodation due to accelerated lattice diffusivity caused by the dissolution of aluminum and magnesium into ZrO2 from the spinel particles, and accelerated relaxation of stress concentrations exerted by grain boundary sliding through dislocation motion. These positive factors make it possible to attain HSRS in ZrO2.

“Extracting the elastic and viscoelastic properties of a polymeric film using a sharp indentation relaxation test” [J. Mater. Res. 21, 2991 (2006)]

“In situ x-ray study of the γ- to α-Al2O3 phase transformation during atmospheric pressure oxidation of NiAl(110)” [J. Mater. Res. 21, 3047 (2006)]

“Structural characterization of a new layered-ternary Ta4AlC3 ceramic” [J. Mater. Res. 21, 2587 (2006)]