bluuebunny/crossref_metadata_2025 huggingface dataset:
Interfacial reactions and impact reliability of Sn–Zn solder joints on Cu or electroless Au/Ni(P) bond-pads
Authors: Date M. , Tu K.N. , Shoji T. , Fujiyoshi M. , Sato K.
Published: May 2005

Sn–9Zn and Sn–8Zn–3Bi solder balls were bonded to Cu or electroless Au/Ni(P)pads, and the effect of aging on joint reliability, including impact reliability, was investigated. For the purpose of quantitatively evaluating the impact toughness ofthe solder joints, a test similar to the classic Charpy impact test was performed.The interfacial compounds formed in the solder/Cu joint during soldering wereCu–Zn intermetallic compounds (IMCs), not Cu–Sn IMCs. One of the Cu–Zn IMCs, γ–Cu5Zn8, thickened remarkably with aging, and eventually its morphology changed from layer-type into discontinuous. The rapid growth of the γ–Cu5Zn8 and void formation at the bond interface led to the significant degradation of the joint reliability due to a ductile-to-brittle transition of the joint. Meanwhile, the compound formed in the solder/Au/Ni(P) joint during soldering was a Au–Zn IMC, above which Zn redeposited during aging. Both the dissolution and diffusion of Ni into the solders were extremely slow, which contributes to negligible void formation at the bond interface. As a result, the solder bumps on the Au/Ni(P) pads were able to maintain the high joint strength and impact toughness even after prolonged aging.
Crystallization kinetics of amorphous Ga–Sb–Te films: Part II. Isothermal studies by a time-resolved optical transmission method
Authors: Lee Chain-Ming , Lin Yeong-Iuan , Chin Tsung-Shune
Published: May 2005

Isothermal crystallization kinetics of amorphous Ga–Sb–Te films was studied by means of a time-resolved optical transmission method. Thin films with compositions along the pseudo-binary tie-lines Sb7Te3–GaSb and Sb2Te3–GaSb in the ternary phase diagram were prepared by the co-sputtering method. Crystallization of GaSbTe films reveals a two-stage process: an initial surface nucleation and coarsening (Stage 1) followed by the one-dimensional grain growth (Stage 2). The kinetic exponent (n) value in Stage 1 shows strong dependence on film compositions, while that of Stage 2 is less dependent. The activation energy in Stage 1 increases with increasing GaSb content and reaches the maximum values at compositions close to GaSb, but a decreasing trend was observed in Stage 2. Kinetics parameters between isothermal crystallization of thin films and non-isothermal crystallization of powder samples analyzed by differential scanning colorimetry [J. Mater. Res. 19, 2929 (2004)] are compared. The kinetic parameters in Stage 1 show much correspondence with those of non-isothermal cases in comparable kinetic exponents but with lower activation energies. The discrepancies between nonisothermal and isothermal kinetics are attributed to the sample morphology and the constraint effects.
Growth behavior and microstructure of oxide scale formed on MoSi2 coating at 773 K
Authors: Lee Kyung-Hwan , Yoon Jin-Kook , Kim Gyeung-Ho , Doh Jung-Mann , Hong Kyung-Tae , Yoon Woo-Young
Published: May 2005

Growth behavior and microstructure of oxide scale formed on MoSi2 coating by cyclic oxidation testing in air at 500 °C were investigated using field emission scanning electron microscopy, cross-sectional transmission electron microscopy, glancing angle x-ray diffraction, and x-ray photoelectron spectroscopy. MoSi2 coating was prepared by chemical vapor deposition of Si on a Mo substrate at 1100 °C for 5 h using SiCl4–H2 precursor gas mixtures. After the incubation period of about 454 cycles, accelerated oxidation behavior was observed in MoSi2 coating and the weight gain increased linearly with increasing oxidation cycles. Microstructural analyses revealed that pest oxide scale was formed in three sequential processes. Initially, nanometer-sized crystalline Mo4O11 particles were formed with an amorphous SiO2 matrix at MoSi2 interface region. Inward diffusing oxygen reacted with Mo4O11 to form Mo9O26 nano-sized particles. At final stage of oxidation, MoO3 was formed from Mo9O26 with oxygen and growth of MoO3 took place forming massive precipitates with irregular and wavy shapes. The internal stress caused by the growth of massive MoO3 precipitates and the volatilization of MoO3 was attributed to the formation of many lateral cracks into the matrix leading to pest oxidation of MoSi2 coating.
Growth kinetics of MgB2 layer and interfacial MgO layer during ex situ annealing of amorphous boron film
Authors: Kim Hyun-Mi , Yim Sung-Soo , Kim Ki-Bum , Moon Seung-Hyun , Kim Young-Woon , Kang Dae-Hwan
Published: May 2005

This paper describes the growth kinetics of an interfacial MgO layer as well as those of an MgB2 layer during ex situ annealing of the evaporated amorphous boron (a-B) film under Mg vapor overpressure. A thin MgO layer is formed at the interface between a-B and Al2O3 substrate before the formation of crystalline MgB2 layer and the interfacial layer is epitaxially related with Al2O3 substrate (MgO (111)[110] // Al2O3 (0001)[1100]). The interfacial MgO layer continues to grow during the annealing, and its apparent growth rate is about 0.1 nm/min. The analysis of MgB2 layer growth kinetics using cross-sectional transmission electron microscopy reveals that there exist two distinct growth fronts at both sides of an MgB2 layer. The growth kinetics of the lower MgB2 layer obeys the parabolic rate law during the entire annealing time. The growth of the upper MgB2 layer is controlled by the surface reaction between out-diffused boron and Mg vapor up to 10 min, resulting in a rough surface morphology of MgB2 layer. By considering the mass balance of Mg and boron during ex situ annealing, we obtained the diffusivities of Mg and boron in MgB2 layer which were in the same order range of approximately 10−12 cm2/s.
X-ray diffraction study revealing phase coexistence in barium titanate stannate
Authors: Mueller Volkmar , Beige Horst , Abicht Hans-Peter , Eisenschmidt Christian
Published: May 2005

In this paper, the results of a temperature dependent x-ray diffraction (XRD) study on BaTi0.95Sn0.05O3 (BTS-5) ceramics are compared with dielectric measurements. The orthorhombic-tetragonal phase transition at T2 = 306 K is found to proceed in a considerably wider temperature range than expected from the dielectric anomaly. Although the macroscopic properties of BTS-5 indicate a rather sharp ferroelectric phase transition at Tc = 358K, we observe anomalous XRD-patterns in a 25 K wide temperature range. This is interpreted in terms of mechanically clamped tetragonal and cubic phase, coexisting in the vicinity of Tc in grains with inhomogeneous Sn-distribution.
Influence of variation (V2O5/P2O5) ratio on the local structure of iron in V2O5–BaO–Fe2O3–P2O5 glasses
Authors: Abdel-Wahab F. , Yahya G.A. , Ali Karam A. , Salem S.M. , Mostafa A.G.
Published: May 2005

The influence of the variation in (V2O5/ P2O5) ratio on the local structure of iron in V2O5–BaO–Fe2O3–P2O5 glass system was investigated. Infrared analysis and Mössbauer spectroscopy were used for this propose. Infrared spectroscopic analysis showed that vanadium cations act mainly as network former (NWF) while iron ions occupy both NWF and network modifier (NWM) positions. On the other hand, Mössbauer spectra indicated that, at the lowest V2O5 content, about 29% of iron ions take their positions in the glass matrix as NWF and about 71% of iron ions enter the matrix as network modifier NWM. At the highest value of V2O5 content the iron ions that enter the glass as NWF decrease to about 15%, and the iron ions which enter the glass as NWM increase to about 85%. The density and molar volume measurements also indicate the changes in the structure of these glasses.
Metalorganic chemical vapor deposition of highly oriented thin film composites of V2O5 and V6O13: Suppression of the metal–semiconductor transition in V6O13
Authors: Sahana M.B. , Shivashankar S.A.
Published: May 2005

Thin films of vanadium oxides were grown on fused quartz by metalorganic chemical vapor deposition using vanadyl acetylacetonate as the precursor. Growth at temperatures ⩾560 °C results in composites of strongly (00l)-oriented V2O5 and V6O13. The dominant phase of the film changes from V2O5 to V6O13, and back to V2O5, as the growth temperature is raised from 560 to 570 °C, then to 580 °C, as evidenced by x-ray diffraction and Rutherford backscattering analyses. This reentrant-type growth trend was interpreted on the basis of the small difference in the free energy of formation of V2O5 and V6O13 and the presence of metal–oxygen bonds in the precursor. In contrast with single-crystalline V6O13, the film predominantly composed of highly oriented single-crystalline platelets of V6O13 did not undergo the semiconductor–metal transition at −123° K, despite the connectivity being well above the percolation threshold. Instead, a semiconductor-to-semiconductor transition was observed in this film, which is explained in terms of the observed relaxation of the edges of all the platelets of metallic V6O13 to semiconducting V2O5.
Improved growth of aligned carbon nanotubes by mechanical activation
Authors: Chen Y. , Chadderton L.T.
Published: May 2005

Straight aligned carbon nanotubes with multiwalled cylindrical structure have been produced by pyrolysis of iron phthalocyanine (FePc) after ball milling treatment. The pre-ball milling treatment prevented the formation of curved nanotubes with bamboo or conelike structures. X-ray diffraction analysis revealed that the milled FePc has an activated and disordered structure, which contributes a lower vaporization temperature determined by thermal gravimetric analysis. The low formation temperature and an increased nanotube growth rate are favorable to the formation of cylindrical structure than bamboo tubes.
Synthesis of gold colloids by laser ablation in thiol-alkane solutions
Authors: Compagnini Giuseppe , Scalisi A. Alessandro , Puglisi Orazio , Spinella Corrado
Published: May 2005

In this paper, we present a study on the formation of gold colloids by laser ablation of a gold metal target in alkanes and thiol-alkane solutions. The results show a decrease of the gold particles’ size up to 2 nm when thiol molecules are present in the liquid environment. The observation of a blue-shift of the surface plasmon resonance is discussed together with transmission electron microscopy analyses accounting the cluster size decrease and the stabilization of the obtained suspensions.
Microstructure of ZnO shell on Zn nanoparticles
Authors: Sun Haiping , Pan Xiaoqing
Published: May 2005

When exposed to air at room temperature, Zn nanoparticles oxidize gradually to form crystalline ZnO shells with a thickness of a few nanometers. Electron diffraction and high-resolution lattice imaging revealed that the ZnO layer on the Zn {0001} surface is composed of many epitaxial domains with small rotation angles relative to the lattice of the Zn core. The oxidized Zn particle bends when irradiated by the electron beam in a transmission electron microscope. This is due to the increase of internal stress in the ZnO layer as a result of the realignment of adjacent domains under electron beam irradiation. Corrosion of Zn nanoparticles was observed and the scaling and spalling start to occur on the {1010} prismatic faces.
Examining pressure-induced phase transformations in silicon by spherical indentation and Raman spectroscopy: A statistical study
Authors: Juliano Tom , Domnich Vladislav , Gogotsi Yury
Published: May 2005

Unloading rate and maximum load have been previously shown to affect the response of silicon to sharp indentation, but no such study exists for spherical indentation. In this work, a statistical analysis of over 1900 indentations made with a 13.5-μm radius spherical indenter on a single-crystal silicon wafer over a range of loads (25–700 mN) and loading/unloading rates (1–30 mN/s) is presented. The location of “pop-in” and “pop-out” events, most likely due to pressure-induced phase transformations, is noted, as well as pressures at which they occur. Multiple occurrences of pop-in and pop-out events are reported. Raman micro-spectroscopy shows a higher intensity of metastable silicon phases at some depth under the surface of the residual impression, where the highest shear stresses are present. A stability range for Si-II is demonstrated and compared with previous results for Berkovich indentation.
Void evolution and its dependence on segment length in Cu interconnects
Authors: Leon R. , Colon J.A. , Evans K.C. , Vu D.T. , Blaschke V. , Bavarian B. , Ogawa E.T. , Ho P.S.
Published: May 2005

Void evolution during electromigration was studied by recording void nucleation, growth, and displacements at various intervals during thermal (240 °C) and electrical stress tests (2 × 106 amps/cm2) of Cu interconnects. Structural data was collected for various serially arranged line segment lengths and correlated with resistance and increases in resistance due to electromigration-induced thinning and voiding. These results allowed determination of void growth rates in Cu interconnects. Void nucleation and growth show a clear dependence on segment length. Void formation did not occur at the via/interconnect interface, which improved interconnect reliability by allowing extensive voiding before catastrophic failure.
Atomistic simulation of the influence of pre-existing stress on the interpretation of nanoindentation data
Authors: Schall J. David , Brenner Donald W.
Published: May 2005

By using molecular dynamics simulations, we have accurately determined the true contact area during plastic indentation of materials under an applied in-plane stress. We found that the mean pressure calculated from the true contact area varied slightly with applied pre-stress with higher values in compression than in tension and that the modulus calculated from the true contact area is essentially independent of the press-stress level in the substrate. These findings are largely consistent with the findings of Tsui, Pharr, and Oliver. On the other hand, if the contact area is estimated from approximate formulae, the contact area is underestimated and shows a strong dependence on the pre-stress level. When it is used to determine mean pressure and modulus, the empirically determined area leads to large errors. Our simulations demonstrate that this phenomenon, first reported for macroscale hardness measurements dating back to 1932, also exists at the nanometer-scale contact areas, apparently scaling over 10 orders of magnitude in contact area, from ∼mm2 to ∼100 nm2.
Preparation and characterization of Sr0.09Ce0.91O1.91, SrCeO3, and Sr2CeO4 by glycine–nitrate combustion: Crucial role of oxidant-to-fuel ratio
Authors: Chavan S.V. , Tyagi A.K.
Published: May 2005

The title compositions were prepared by the gel-combustion process using glycine as the fuel and the corresponding metal nitrates as oxidants. The powders after calcination at 600 °C were characterized by x-ray diffraction for phase identification. The lattice parameters were refined by least squares method for each of the title compounds. Sr0.09Ce0.91O1.91 could be prepared in situ, that is, without any further external heating at higher temperatures, whereas phase pure SrCeO3 and Sr2CeO4 could be prepared only after calcination at 950 °C for 3 h. Sr0.09Ce0.91O1.91 was prepared using three different oxidant-to-fuel ratios: the fuel-deficient ratio, the propellant chemistry (stoichiometric) ratio, and the fuel-excess ratio. The crystallite size as calculated by x-ray line broadening was found to be 13 nm, 20 nm, and 42 nm for the products from fuel-deficient, propellant, and fuel-excess ratios, respectively. It was found that the extreme fuel-deficient ratio of 1:0.5 failed to give phase pure Sr0.09Ce0.91O1.91. The transmission electron microscopy studies showed that majority of the particles were in the range 80–100 nm and 200–250 nm for SrCeO3 and Sr2CeO4, respectively. The compositional characterization was done by energy dispersive x-ray. A careful control of the oxidant-to-fuel ratio was found to be necessary to get the desired products, due to their different thermodynamic stabilities. Thus, the versatility of combustion process in synthesizing the products with different thermodynamic stabilities has been shown, which was hitherto unexplored.
Photoelectrochemical properties and crystalline structure change of Sb-doped TiO2thin films prepared by the sol-gel method
Authors: Bei Zongmin , Ren Dasen , Cui Xiaoli , Shen Jie , Yang Xiliang , Zhang Zhuangjian
Published: May 2005

Ti1−XSbXO2samples were obtained from dip-coating sol-gel method and a subsequent anneal at 450 °C. They had an average crystallite size of 13.3–20 nm. Cyclic voltammograms taken under ultraviolet (UV) and Xe lamp illumination in a 0.5 M Na2SO4electrolyte showed that the Sb-doped samples had greater photocurrent densities than pure titania electrode, with an optimal Sb concentration of 0.2%. Oxidative peaks were observed in the cyclic voltammograms obtained in the dark after certain exposure duration to UV light. X-ray diffraction patterns and Raman spectra show a phase transformation from brookite to anatase in the samples with Sb concentration up to 0.2%. Ti4+ions were substituted by Sb to form the anatase structure of Sb–O–Ti, improving the crystallization efficiency. The Sb–Sb bonds were formed due to the introduction of excessive Sb atoms.
Mechanochemical study of the hydriding properties of nanostructured Mg2Ni–Ni composites
Authors: Mulas G. , Schiffini L. , Cocco G.
Published: May 2005

A comprehensive approach is presented for defining hydrogen activation and absorbing kinetics in heterogeneous Mg2Ni/Ni powder composites that were subjected to mechanical refinement. Hydriding tests were performed under conventional hydrogen dissolving and under reactive milling. Irrespective of the absorbing mode, the absorption kinetics is deceleratory throughout. Under conventional thermodynamic conditions, the hydriding rate depends strongly on the microstructural features of both the absorbing Mg2Ni intermetallic and the Ni phase. The latter plays an important role in the dissociative chemisorption of hydrogen. Under milling the hydrogen uptake and the hydriding kinetics also depend on the intensity of the milling processing, IM (watt g−1), with the absorption rate increasing exponentially with IM. The mechanical treatment was found effective even when thermodynamic absorption reached saturation level. Hydriding rates, mechanochemical gains, and instantaneous mechanochemical yields (mol J−1) were used to compare the processes on an absolute scale and to spotlight possible mechanisms controlling kinetics trends and absorbing features under milling.
Analysis of sharp-tip-indentation load–depth curve for contact area determination taking into account pile-up and sink-in effects
Authors: Choi Yeol , Lee Ho-Seung , Kwon Dongil
Published: May 2005

Hardness and elastic modulus of micromaterials can be evaluated by analyzing instrumented sharp-tip-indentation load–depth curves. The present study quantified the effects of tip-blunting and pile-up or sink-in on the contact area by analyzing indentation curves. Finite-element simulation and theoretical modeling were used to describe the detailed contact morphologies. The ratio f of contact depth, i.e., the depth including elastic deflection and pile-up and sink-in, to maximum indentation depth, i.e., the depth measured only by depth sensing, ignoring elastic deflection and pile-up and sink-in, was proposed as a key indentation parameter in evaluating real contact depth during indentation. This ratio can be determined strictly in terms of indentation-curve parameters, such as loading and unloading slopes at maximum depth and the ratio of elastic indentation energy to total indentation energy. In addition, the value of f was found to be independent of indentation depth, and furthermore the real contact area can be determined and hardness and elastic modulus can be evaluated from f. This curve-analysis method was verified in finite-element simulations and nanoindentation experiments.
Spark plasma sintering and characterization of bulk nanostructured fully stabilized zirconia: Part I. Densification studies
Authors: Anselmi-Tamburini U. , Garay J.E. , Munir Z.A. , Tacca A. , Maglia F. , Spinolo G.
Published: May 2005

The sintering of nanosize powders of fully stabilized zirconia was investigated using the spark plasma sintering (SPS) method. The influence of sintering temperature, heating rate, direct current pulse pattern, sintering time, and sintering pressure on the final density and grain size of the product was investigated. The dependence of densification on temperature showed a maximum at 1200 °C, resulting with nearly fully dense zirconia with a crystallite size of about 100 nm. Heating rate (50∼300 °C min−1) and sintering time (5–16 min) had no significant influence on the final density and the crystallite size. Pulsing patterns ranging from 2:2 to 48:2 (on:off) had no influence on the density or the crystallite size. However, the applied pressure had a significant influence on the final density but no apparent effect on crystallite size for a sintering temperature of 1200 °C and a hold time of 5 min.
Spark plasma sintering and characterization of bulk nanostructured fully stabilized zirconia: Part II. Characterization studies
Authors: Anselmi-Tamburini U. , Garay J.E. , Munir Z.A. , Tacca A. , Maglia F. , Chiodelli G. , Spinolo G.
Published: May 2005

Dense fully stabilized cubic zirconia, sintered by the spark plasma sintering (SPS) method, was characterized through hardness, fracture toughness, and electrical impedance measurements. The effect of sintering temperature on hardness and fracture toughness was evaluated. Samples sintered at 1200 °C for 5 min, which had crystallite size of <100 nm, exhibited the highest hardness. Impedance measurements showed an increase in bulk contribution relative to grain boundaries as sintering temperature is increased. Calculation of the activation energy for conduction gave a value, 1.13 eV, in agreement with previously published results.
Reconciliation of nanoscratch hardness with nanoindentation hardness including the effects of interface shear stress
Authors: Tayebi Noureddine , Conry Thomas F. , Polycarpou Andreas A.
Published: May 2005

The definitions of hardness from nanoscratch and nanoindentation analyses with a spherical indenter were compared and shown to be mathematically equivalent for the case of zero interface shear stress (surface traction). The definition of nanoindentation hardness was taken as the ratio of the resultant force to the area of contact projected on a plane normal to the line of action of the resultant force, whereas in the case of the nanoscratch technique, the hardness and interfacial shear stress were related to the measured normal and lateral forces in a nanoscratch experiment, as well as to the cross-sectional area of the groove. The two definitions of hardness were then applied to nanoscratch experimental data from material systems covering a wide range of hardness values. The calculated values of hardness from the two definitions were based on the contact area, determined from the scratch residual profile and the elastic recovery of the plastically deformed surface, and yielded the same values of hardness within experimental error. The contact angle, and thus the contact area, was shown experimentally to be sensitive to interface shear stress: a positive increase in interface shear stress led to a reduction in contact area as compared to the case of a frictionless contact. For a material with given hardness, normal indenter force, and contact area, a positive or negative interface shear stress is balanced by a positive or negative change, respectively, in the lateral force about the value needed to maintain a static balance for a frictionless nanoscratch contact. A comparison of these effects with experimental data indicates that very hard materials tend to have negative to zero interface shear stress, which correlates to a sink-in effect, whereas the soft materials tend to have positive interface shear stress, which correlates to a pileup effect.
Atomic layer deposition of noble metals: Exploration of the low limit of the deposition temperature
Authors: Aaltonen Titta , Ritala Mikko , Tung Yung-Liang , Chi Yun , Arstila Kai , Meinander Kristoffer , Leskelä Markku
Published: May 2005

The low limit of the deposition temperature for atomic layer deposition (ALD) of noble metals has been studied. Two approaches were taken; using pure oxygen instead of air and using a noble metal starting surface instead of Al2O3. Platinum thin films were obtained by ALD from MeCpPtMe3 and pure oxygen at deposition temperature as low as 200 °C, which is significantly lower than the low-temperature limit of300 °C previously reported for the platinum ALD process in which air was used as the oxygen source. The platinum films grown in this study had smooth surfaces, adhered well to the substrate, and had low impurity contents. ALD of ruthenium, on the other hand, took place at lower deposition temperatures on an iridium seed layer than on an Al2O3 layer. On iridium surface, ruthenium films were obtained from RuCp2 and oxygen at 225 °C and from Ru(thd)3 and oxygen at 250 °C, whereas no films were obtained on Al2O3 at temperatures lower than 275 and 325 °C, respectively. The crystal orientation of the ruthenium films was found to depend on the precursor. ALD of palladium from a palladium β-ketoiminate precursor and oxygen at 250 and 275 °C was also studied. However, the film-growth rate did not saturate to a constant level when the precursor pulse times were increased.
Preparation of good mechanical property polystyrene nanotubes with array structure in anodic aluminum oxide template using simple physical techniques
Authors: Song Guojun , She Xilin , Fu Zhifeng , Li Jianjiang
Published: May 2005

The stable mechanical property polystyrene (PS) nanotubes with array structure were first prepared by filtrating a solution or melt of normal molecular weight PS (Mn ≈ 180,000) into anodic aluminum oxide (AAO) template with only 200-nm pores. The results of transmission electron microscopy and scanning electron microscopy illuminated that PS tubules were successfully obtained and the wall thickness of PS tubules prepared by the 2.5 wt%, 5.0 wt%, and 10.0 wt% PS solution were respectively 50 nm, 70 nm, and 80 nm. The structure of polymer nanotubes depends strongly on the concentration of PS solution. It was found that the wall of the nanotubes derived from melt is thicker than that of the nanotubes from solution. When the polymer solution wets AAO template, a thin polymer film will be formed on the inner porous wall. The thin film/AAO composite membrane acts as a “second-order” template and is soaked repeatedly. So PS solution wets the template and forms nanotubes according to the multi-time wetting mechanism.
A new method for the determination of the diffusion-induced concentration profile and the interdiffusion coefficient for thin film systems by Auger electron spectroscopical sputter depth profiling
Authors: Wang J.Y. , Mittemeijer E.J.
Published: May 2005

A new Auger electron spectroscopical sputter depth profiling method was developed to determine the interdiffusion coefficient for the initial stage of diffusion annealing of thin films. The method is based on (i) adoption of an interdiffusion model appropriate for the specimen investigated and (ii) convolution of an accordingly calculated diffusion-induced concentration profile with the smearing effects due to atomic mixing, surface/interface roughness, escape depth of the Auger electrons, and preferential sputtering. The diffusion-induced concentration profile and the interdiffusion coefficient are determined by fitting in an iterative least-squares procedure of the calculated Auger electron spectroscopical depth profile to the measured one. The method was applied to bilayered and multilayered structures, exhibiting dominant grain-boundary diffusion and dominant volume diffusion, respectively. A very small extent of interdiffusion, characterized by diffusion distances as small as 1 nm, could be quantified.
Impact of printed wiring board coatings on the reliability of lead-free chip-scale package interconnections
Authors: Mattila T.T. , Vuorinen V. , Kivilahti J.K.
Published: May 2005

When lead-free solder alloys mix with lead-free component and board metallizations during reflow soldering, the solder interconnections become multicomponent alloy systems whose microstructures cannot be predicted on the basis of the SnPb metallurgy. To better understand the influences of these microstructures on the reliability of lead-free electronics assemblies, SnAgCu-bumped components were reflow-soldered with near-eutectic SnAgCu solder pastes on Ni(P)|m.Au- and organic solderability preservative (OSP)-coated printed wiring boards and tested under cyclic thermal shock loading conditions. The reliability performance under thermomechanical loading was found to be controlled by the kinetics of recrystallization. Because ductile fracturing of the as-soldered tin-rich colonies would require a great amount of plastic work, the formation of continuous network of grain boundaries by recrystallization is needed for cracks to nucleate and propagate intergranularly through the solder interconnections. Detailed microstructural observations revealed that cracks nucleate and grow along the grain boundaries especially between the recrystallized part and the non-recrystallized part of the interconnections. The thermal cycling test data were analyzed statistically by combining the Weibull statistics and the analysis of variance. The interconnections on Ni(P)|m.Au were found out to be more reliable than those on Cu|m.OSP. This is due to the extensive dissolution of Cu conductor, in the case of the Cu|m.OSP assemblies, into molten solder that makes the microstructure to differ noticeably from that of the Ni(P)|m.Au interconnections. Because of large primary Cu6Sn5 particles, the Cu-enriched interconnections enhance the onset of recrystallization, and cracking of the interconnections is therefore faster. The solder paste composition had no statistically significant effect on the reliability performance.
Critical evaluation of the Lotgering degree of orientation texture indicator
Authors: Jones Jacob L. , Slamovich Elliott B. , Bowman Keith J.
Published: May 2005

Preferred orientation in textured ceramics is often assessed by comparing the relative intensities of x-ray diffraction reflections to those of a randomly oriented ceramic using the Lotgering degree of orientation (f). However, this paper provides evidence that indiscriminate assessments of f can be misleading. Using measured intensities of a modestly textured tape cast bismuth titanate (Na0.5Bi4.5Ti4O15) ceramic, calculated f values vary from 7.4 to 73.2% depending on the reflections included in the calculation. The texture is also quantified by calculating the orientation distribution function (ODF) using measured pole figures. A model is then presented that demonstrates f is nonlinear with the multiple of preferred (00l)-orientations, the standard unit of the 00l pole figure.
High-temperature annealing behavior of ion-implanted spinel single crystals
Authors: Enescu S.E. , Thomé L. , Gentils A. , Thomé T.
Published: May 2005

This paper reports modifications of the chemical and structural properties of MgAl2O4 single crystals implanted with Cs ions and submitted to high-temperature annealing. The composition changes, the damage created in the three sublattices (Al, Mg and O) of the crystals, and the behavior of implanted ions were studied by Rutherford backscattering and channeling experiments as a function of the Cs fluence and annealing temperature. The data show that annealing above 700–800 °C induces a huge modification of the stoichiometry of the material, a decrease of the lattice disorder, and an increase of the fraction of Cs atoms located in substitutional lattice sites. These results have to be taken into account for the future use of spinel as a matrix for the transmutation of nuclear waste.
Observation and numerical simulation of an elastic-plastic solid loaded by a spherical indenter
Authors: Fujisawa Naoki , Li Wei , Swain Michael V.
Published: May 2005

The observation and finite element simulation of Ti–6Al–4V loaded by a spherical indenter were compared. The contact radius at the maximum load was 40% of the indenter radius, which resulted in a high degree of plasticity induced beneath the indenter. The spherical impression profile predicted by the simulation was in agreement with that of the observation. The local curvature of the spherical impression was shown to vary with radial distance. The overall curvature change with radial distance was more distinctive in the presence of static friction. Due to the large plastic zone in the material, neither the Field–Swain nor the Oliver–Pharr method was able to predict the elastic recovery depths in the center of indentation and at the perimeter of contact. The ratio of the two depths predicted by the latter method, however, may be used to verify the applicability of the method itself in determining the elastic modulus of a ductile material.
Aluminum nitride films synthesized by dual ion beam sputtering
Authors: Han Sheng , Chen Hong-Ying , Cheng Chih-Hsuan , Lin Jian-Hong , Shih Han C.
Published: May 2005

Aluminum nitride films were deposited by varying the voltages of argon ion beams from 400 to 1200 V in dual ion beam sputtering. The crystal structure, microstructure, and elemental distributions of the aluminum nitride films were analyzed by x-ray diffraction, field emission scanning electron microscopy, and secondary ion mass spectroscopy, respectively. The aluminum nitride films exhibited the 〈002〉 preferred orientation at an optimal ion beam voltage of 800 V. The orientation changed to a mixture of {100} and {002} planes above 800 V, accounting for radiation damage. The thickness of the film increases with increasing ion beam voltage, reaching a steady state value of 210 nm at an ion beam voltage of 1200 V. Under optimal condition (800 V), the c-axis orientation of the aluminum nitride 〈002〉 film was obtained with a dense and high-quality crystal structure.
Effect of oxide and nitride films on strength of silicon: A study using controlled small-scale flaws
Authors: Jung Yeon-Gil , Pajares Antonia , Lawn Brian R.
Published: May 2005

Strength properties of silicon substrates containing dense oxide and nitride surface films are investigated using nanoindentations to introduce small flaws of predetermined scale. The indentation flaws provide favored sites for failure in subsequent flexure loading, even in the subthreshold region for indentations without visible corner cracking, confirming that microflaws generated within the indentation zone act as effective crack sources in the substrate. Deposition of the oxide films increases the strength while the nitride films diminish it at any given indentation load. The strength shifts are attributed primarily to the presence of residual compressive stress in the oxide, tensile stress in the nitride. A fracture mechanics formulation based on a previous analysis for monolithic substrates is here adapted to allow for a superposed crack closing or opening stress-intensity factor term associated with the residual stresses. Allowance is also made in the mechanics for the influence of the film on effective hardness and modulus of the substrate. The formulation accounts for the basic strength shifts and enables evaluation of the magnitude of the residual stresses. The results quantify the susceptibility of basic device materials to damage from small-scale contacts and impacts.
Microstructure and dielectric properties of Ba(Cd1/3Ta2/3)O3 microwave ceramics synthesized with a boron oxide sintering aid
Authors: Liu Shaojun , Sun Jian , Taylor Richard , Smith David J. , Newman N.
Published: May 2005

The use of boron as a sintering aid reduces the sintering temperature, enhances the sintering density, and improves the microwave properties of Ba(Cd1/3Ta2/3)O3 ceramic dielectrics. Observations by transmission electron microscopy indicate that the liquid sintering mechanism contributes to the improvement in sintering density for boron concentrations exceeding 0.5 wt%. The introduction of as small as 0.01% boron also results in the production of high-density samples (∼95%), presumably indicating that a point defect mechanism may also play an important role in the sintering process. X-ray diffraction data combined with high-resolution transmission electron microscopy images show that boron-doped Ba(Cd1/3Ta2/3)O3 ceramic material has a well-ordered hexagonal structure. Annealing treatment is found to improve the microwave properties. The best sample has a dielectric constant of 32, a temperature coefficient of resonant frequency of 80 ± 15 ppm/°C, and a quality factor of >25,000 at 2 GHz.
Nanoparticles of a doped oxide phosphor prepared by direct-spray pyrolysis
Authors: Lenggoro I. Wuled , Itoh Yoshifumi , Okuyama Kikuo , Kim Tae Oh
Published: May 2005

A gas-phase synthesis route based on spray pyrolysis with a residence/heating time of less than 0.1 s was designed to directly prepare Eu-doped Y2O3 phosphor nanoparticles. The average size of the phosphor particles decreased from the submicron size to around 10 nm when the concentration of the starting solution was increased. By increasing the operating temperature, from 1500 to 1700 °C, the submicron-particles were converted into a nano-particle phosphor, and their photoluminescence intensities at 611 nm (254-nm excitation) were greatly improved. This synthesis procedure has considerable potential for preparing a variety of doped luminescent nanoparticles without the need for post-treatment processing.
Low-temperature transport properties of polycrystalline Ba8Ga16Sn30
Authors: Nolas G.S. , Cohn J.L. , Dyck J.S. , Uher C. , Lamberton G.A. , Tritt T.M.
Published: May 2005

Low-temperature resistivity, Seebeck coefficient, thermal conductivity, and heat-capacity measurements were performed on Ba8Ga16Sn30. This compound crystallizes in a cubic type-VIII clathrate phase, space group I¯43m, with the Baatoms residing inside voids created by a tetrahedrally bonded network of Ga andSn atoms. Ba8Ga16Sn30 exhibits semiconducting behavior above 150 K with a low thermal conductivity and thus may hold potential for thermoelectric applications.
Role of nitrogen on the atomistic structure of the intergranular film in silicon nitride: A molecular dynamics study
Authors: Su Xiaotao , Garofalini Stephen H.
Published: May 2005

Molecular dynamics simulations of intergranular films (IGFs) containing Si, O, N, and Ca in contact with three different types of surface terminations of Si3N4 were performed using a multi-body interatomic potential. IGFs with the same Ca concentration (12 mol% CaO) but different nitrogen concentrations [N/(N + O) = 0, 15, 30, and 50%] were studied. In all 12 IGFs, Ca ions did not compete with the first adsorbed layer of Si at the IGF/basal crystal interface, but did so at the IGF/prism crystal interface. The simulations show the epitaxial adsorption of Si, O, and N from the IGF onto the basal and prism crystal surfaces. While more adsorbed N was expected as nitrogen concentration increases, there was a significantly larger amount of N adsorbed to the basal surface than to the prism surface. It was found that Ca ions sit closer to the prism surface than the basal surface but move closer to the crystal at both surfaces with increasing nitrogen concentration, although the effect was more pronounced at the basal interface. With the increase of nitrogen concentration, the percentage of two-coordinated oxygen remained about the same, but there was a change in the type of defect oxygen present. In all the simulations, the central position of the first peak in the Si–O pair distribution fixation (PDF) ranges from 1.63 to 1.65 Å, and that of Si–N PDF ranges from 1.71 to 1.73 Å, both consistent with experimental findings. Furthermore, the first peak of both the Si–O and Si-N PDF shifts to larger values as the nitrogen concentration increases, indicating the elongation of the Si–O and Si–N bond in the IGF with the increase of nitrogen concentration. Elongation of both the Si–N and Si–O bonds could lead to weakening of the IGF as nitrogen concentration increases, although competing changes in bonding of the O complicate the effect of N addition on the strength of the IGF.
Synthesis, characterization, and magnetic properties of FeCoNi ternary alloy nanowire arrays
Authors: Sharma Gaurav , Grimes Craig A.
Published: May 2005

FeCoNi ternary alloy nanowire arrays 32–106 nm in diameter were fabricated within nanoporous alumina membranes using 15 Vrms alternating current electrodeposition at frequencies of 50, 250, 500, 750, and 1000 Hz. The magnetic coercivity and hysteresis loop squareness-ratio (Mr/Ms) were studied as functions of electrolyte composition, nanowire diameter, and nanowire aspect ratio.
Influence of the Microstructure on the Optical Characteristics of SrTiO3 thin films
Authors: Gaidi M. , Stafford L. , Amassian A. , Chaker M. , Margot J. , Martinu L. , Kulishov M.
Published: May 2005

The influence of the microstructure of strontium-titanate-oxide (SrTiO3 or STO) thin films on their optical properties was investigated through an extensive characterization. The STO films have been deposited on silicon substrates by reactive pulsed laser deposition. The effect of the oxygen deposition pressure on the crystalline quality of the films was systematically studied by x-ray diffraction and scanning electron microscopy. Rutherford backscattering spectrometry, x-ray photoelectron spectroscopy, and secondary ion mass spectrometry were used to determine the atomic density and depth concentration profiles of the various species forming the film. The refractive index and extinction coefficient were obtained using variable angle spectroscopic ellipsometry. Based on this full characterization, it is demonstrated that the optical characteristics of the films are directly correlated to their microstructural properties. In particular, the refractive index increases with film density, while losses decrease. In addition, the interface between STO and Si is characterized by an interdiffusion layer. As the deposition pressure is enhanced, the width of this layer significantly increases, inducing localized inhomogeneity of the refractive index.
Alternative Chemical Route to Mesoporous Titania From a Titanatrane Complex
Authors: Trakanprapai Chavalit , Esposito Vincenzo , Licoccia Silvia , Traversa Enrico
Published: May 2005

High-purity, mesoporous titania was prepared by reaction of dimethylaminotitanatrane, [NMe2–Ti(OCH2CH2)3N] in the presence of micellar aggregates as templating agents followed by thermal treatments in the temperature range 350–450 °C. The powders were characterized by nitrogen adsorption–desorption isotherms, thermogravimetry–differential thermal analysis, Fourier transform infrared, field-emission scanning electron microscopy, and x-ray diffraction. Analysis of the morphological characteristics of titanium oxide powders calcined at 350 °C for 120 h and at 450 °C for 6 h showed the presence of a mesoporous structure, with an average pore size of about 3.5 nm. Firing temperatures above 450 °C caused the collapse of the mesoporous structure. Composite Nafion-based membranes, containing 5 wt% mesoporous titania fired at 450 °C as a filler were successfully prepared. Preliminary tests in a prototype direct methanol fuel cell demonstrated that the composite membrane allowed cell operation up to 145 °C, thus showing a significant performance improvement over pure Nafion.
Fabrication of Al2O3/BN Nanocomposites by Chemical Processing and Their Mechanical Properties
Authors: Kusunose Takafumi , Kim Yoon-Ho , Sekino Tohru , Matsumoto Takuya , Tanaka Norihito , Nakayama Tadachika , Niihara Koichi
Published: May 2005

Al2O3/BN nanocomposites were fabricated through a novel chemical route involving hot-pressing of α–Al2O3powders covered partly with turbostratic BN (t-BN). The nano-sized hexagonal BN (h-BN) particles were found to be homogeneously dispersed within the Al2O3grains as well as at grain boundaries, which is indicative of nanocomposite structures. Thus, the present nanocomposites exhibited the unique properties of high strength and low Young’s modulus associated with nanocomposites. This paper discusses in detail the synthesis process and microstructural features of these materials.
Epitaxial Growth of Solution-Based Rare-Earth Niobate, RE3NbO7, Films on Biaxially Textured Ni–W Substrates
Authors: Paranthaman M. , Bhuiyan M.S. , Sathyamurthy S. , Zhai H.Y. , Goyal A. , Salama K.
Published: May 2005

A new series of rare earth-niobate, RE3NbO7 (RE=Y,Gd,Eu), buffer layers were developed for the growth of superconducting YBa2Cu3O7−δ (YBCO) films on biaxially textured Ni–W (3 at.%) substrates. Using chemical solution deposition, smooth, crack-free, and epitaxial RE3NbO7 (RE = Y,Gd,Eu) films were grown on cube-textured Ni–W substrate. YBCO film with a critical current density of 1.1 × 106 A/cm2 in self-field at 77 K was grown directly on a single Gd3NbO7-buffered Ni–W substrate using pulsed laser deposition.
Enthalpy of Formation of Yttria-Doped Ceria
Authors: Chen Weiqun , Lee Theresa A. , Navrotsky Alexandra
Published: May 2005

Solid solutions (1 − x)CeO2 − xYO1.5 (0 ≤ x ≤ 0.36) were prepared by coprecipitation and sol-gel methods. Their enthalpy of formation relative to the end-members, fluorite-type cubic CeO2 and C-type YO1.5 was determined by oxide melt solution calorimetry. The enthalpy of drop solution shows a roughly linear trend with composition. Extrapolation to x = 1 gives the transition enthalpy of C-type to cubic fluorite YO1.5 as 22.2 ± 6.7 kJ/mol. This linear behavior is in contrast to the strong curvature seen in the ZrO2 − YO1.5 and HfO2 − YO1.5 systems. The slightly positive enthalpy of formation of CeO2 − YO1.5 is strikingly different from the strongly negative enthalpies of formation of ZrO2 − YO1.5 and HfO2 − YO1.5. The thermodynamics of CeO2 − YO1.5 is analyzed in terms of defect association and oxygen vacancy distribution. Specifically, the association of oxygen vacancies with the tetravalent cations in the zirconia and hafnia systems, in contrast to the preference of vacancies for nearest neighbor yttrium sites in the ceria systems, may explain the different energetics.
The Effect of Electrolyte Composition on the Fabrication of Self-Organized Titanium Oxide Nanotube Arrays by Anodic Oxidation
Authors: Cai Qingyun , Paulose Maggie , Varghese Oomman K. , Grimes Craig A.
Published: May 2005

We report on the fabrication of self-organized titanium oxide nanotube arrays of enhanced surface area prepared by anodic oxidation of a pure titanium sheet in electrolyte solutions containing potassium fluoride (KF) or sodium fluoride (NaF). The effects of electrolyte composition and concentration, solution pH, and the anodic potential on the formation of nanotubes and dimensions of the resulting nanotubes are detailed. Although nanotube arrays of length greater than 500 nm are not possible with hydrofluoric acid containing electrolytes [G.K. Mor, O.K. Varghese, M. Paulose,N. Mukherjee, C.A. Grimes, J. Mater. Res. 18, 2588 (2003)], by adjusting the pH of a KF containing electrolyte to 4.5 using additives such as sulfuric acid, sodium hydroxide, sodium hydrogen sulfate, and/or citric acid, we could increase the length of the nanotube-array to approximately 4.4 μm, an order of magnitude increase in length. The as-prepared nanotubes are composed of amorphous titanium oxide. Independent of the electrolyte composition, crystallization of the nanotubes to anatase phase occurred at temperatures ⩾280 °C. Rutile formation occurred at the nanotube-Ti substrate interface at temperatures near 480 °C. It appears geometry constraints imposed by the nanotube walls inhibit anatase to rutile transformation. No disintegration of the nanotube array structure is observed at temperatures as high as 580 °C. The excellent structural and crystal phase stability of these nanotubes make them promising for both low- and high-temperature applications.