A finite element analysis of frictionless indentation of an elastic–plastic half-space by a rigid sphere is presented and the deformation behavior during loading and unloading is examined in terms of the interference and elastic–plastic material properties. The analysis yields dimensionless constitutive relationships for the normal load, contact area, and mean contact pressure during loading for a wide range of material properties and interference ranging from the inception of yielding to the initiation of fully plastic deformation. The boundaries between elastic, elastic–plastic, and fully plastic deformation regimes are determined in terms of the interference, mean contact pressure, and reduced elastic modulus-to-yield strength ratio. Relationships for the hardness and associated interference versus elastic–plastic material properties and truncated contact radius are introduced, and the shape of the plastic zone and maximum equivalent plastic strain are interpreted in light of finite element results. The unloading response is examined to evaluate the validity of basic assumptions in traditional indentation approaches used to measure the hardness and reduced elastic modulus of materials. It is shown that knowledge of the deformation behavior under both loading and unloading conditions is essential for accurate determination of the true hardness and reduced elastic modulus. An iterative approach for determining the reduced elastic modulus, yield strength, and hardness from indentation experiments and finite element solutions is proposed as an alternative to the traditional method.

To investigate the directional dependence of the Faraday effect in terbium–scandium–aluminum garnet (TSAG) single crystals, grown by the Czochralski method, the Verdet constant was measured at 〈111〉, 〈110〉, and 〈100〉 orientations. Extinction ratio and magnetic susceptibility were measured. From the linear dependence of the Verdet constant and inverse wavelength square 1/λ2, 〈111〉 direction shows the highest value of Verdet constant (for λ⋅ = 649.1 nm, Vav = 8.256 × 10−3 deg · Oe−1 · cm−1). Significant anisotropy of magnetic susceptibility was not observed. The extinction ratio of TSAG shows the highest value for 〈111〉 orientation 38.7 dB, which implies that it can be used as an optical isolator.

Transmission electron microscopy (TEM) and analytic TEM were used to study the microstructure of amorphous carbon (a-C) films of thickness in the range of 5–100 nm deposited on Si(100) by radio-frequency (rf) sputtering. High-resolution cross-section TEM revealed a two-layer structure consisting of the a-C film and an ultrathin interface layer, in agreement with electron energy loss spectroscopy results. The presence of a 35-Å-thick interface layer (regardless of the deposition conditions) indicates that nucleation and initial growth of the a-C films were mainly controlled by the substrate surface condition. Mass-thickness contrast in bright-field TEM images showed an interface layer denser than the a-C film. This layer, believed to consist of Si, a-C, and SiC, enhances the adhesion of the film to the silicon substrate and accommodates the residual stress in the film. High-resolution cross-section TEM images revealed the presence of platelike nanocrystallites (∼35 Å in size) randomly distributed in the a-C film and oriented parallel to the surface. The possible mechanisms leading to the formation of these nanocrystalline structures are discussed in terms of sputtering phenomena occurring during film deposition.

Transmission electron microscopy and x-ray diffraction were used to study SrTiO3 films grown on platinized (0001) Al2O3 substrates. The Pt films were epitaxial with an orientation relationship described by (111)Pt‖(0001)Al2O3 and [110]Pt‖[10¯10]Al2O3. SrTiO3 films with two different Sr to Ti ratios, 1.02 and 1.4, were deposited by radio-frequency magnetron sputtering. In the film with a large amount of Sr excess, the grain sizes were smaller and a high density of planar defects was observed. The films were predominantly (111) textured, but a weaker (110) texture component was also found, independent of stoichiometry. While the (111) texture could be explained with the excellent lattice match with (111) Pt, the (110) textured grains had a large mismatch with the Pt electrode. We propose that the presence of the (110) oriented grains is due to nucleation at Pt surface defects. Planar defects in the films with a large amount of Sr excess served to accommodate the nonstoichiometry. Comparison with homoepitaxial SrTiO3 films showed that the density of planar defects in the SrTiO3 films on (111)Pt/Al2O3 is insufficient to accommodate all the excess Sr. The influence of the film microstructure on the dielectric properties is also discussed.

The static magnetic field and the alternating electric field were simultaneously imposed on AZ91D magnesium alloy melt, and α-dendrite particles were refined by the electromagnetic vibrations. The effect of the frequency of electromagnetic vibrations on microstructural refinement was quantitatively investigated. In the frequency range from 60 to 1000 Hz, the vibration frequency near 200 Hz was the most effective for the refinement of α-dendrite particles, and α-dendrite particles were refined up to approximately 100 μm from 1800 μm at this frequency. However, the effect of refinement by the electromagnetic vibrations became weak at frequencies above 400 Hz. Although the degree of refinement of the primary particles differed with the frequency of the electromagnetic vibrations, the dendrite arm spacing was almost constant, 30–40 μm, in our experiment. Therefore, the refinement of primary α-dendrite particles is likely to be caused by collapse of dendrite arms due to the cavitation phenomenon and the stirring of the melt.

A comparative study on the effects of the substrate on the determination of hardness of thin films by the use of the nanoscratch and nanoindentation techniques was conducted. Gold films deposited on fused quartz substrates and silicon dioxide films deposited on aluminum substrates with variant film thicknesses were investigated. These two systems correspond to a soft film on a hard substrate and a hard film on a soft substrate, respectively. The effect of substrate interaction on the measurement of hardness using the nanoscratch technique was found to be less pronounced compared to that of the nanoindentation technique due to: (i) the lower normal loads applied to achieve the penetration depths that occur at higher loads when using the nanoindentation method; (ii) the direct imaging of the residual deformation profile that is used in the nanoscratch technique, which allows for the effects of pileup or sink-in to be taken into account, whereas in the nanoindentation technique the contact area is estimated from the load-displacement data, which does not include such effects; and (iii) the account of elastic recovery of the plastically deformed surfaces from scratch tests. The film thickness did not appear to have any effect on the hardness of Au and SiO2 films obtained from nanoscratch data. This observation allowed, for the case of SiO2 films, the determination of the “free substrate effect region” and the derivation of an empirical relationship that relates the composite hardness of the film/substrate system to the contact-depth-to-film-thickness ratio, even when the indenter penetrates into the substrate. Such findings can allow for the determination of the intrinsic hardness of ultrathin hard films (∼1–5 nm thick), where the substrate effect is unavoidable.

Highly crystalline-textured pure dense alumina ceramics were fabricated from spherical alumina powder without any seed particles and sintering additives by electrophoretic deposition (EPD) in a strong magnetic field of 10 T. The crystalline texture was confirmed by x-ray diffraction (XRD) for alumina ceramics deposited at 10 T followed by sintering at 1873 K. The angle between the directions of the magnetic and electric fields (φB-E) was altered to control the dominant crystal faces of the α-alumina monoliths. The average orientation angles estimated from the XRD diagram of the samples prepared at φB-E = 0°, 45°, and 90° were 16.52°, 45.15°, and 84.90°, respectively. Alumina/alumina laminar composites with different crystalline-oriented layers were also fabricated by alternately changing the φB-E layer by layer during EPD in a 10 T magnetic field. It was demonstrated that by using this technique, it is possible to control the crystalline orientation by changing the angle of E versus B during the EPD.

With the help of instrumented indentation, the mechanical behavior of a variety of biological systems was studied: the waxy zone of the pitcher plant (Nephenthes alata) adapted for attachment prevention, the head-to-thorax articulation system of a beetle (Pachnoda marginata) as an example of friction minimization, and the wing arresting system of the dung beetle (Geotrupes stercorarius) adapted for mechanical interlocking. We demonstrate that nanoindentation can successfully be applied to compliant and highly structured biological composite materials. Measuring the mechanical performance of these surfaces can provide important information for understanding the overall functioning of these systems. Tests on fresh and dried samples show the influence of desiccation on the results and point out the importance of native conditions during the measurements. However, these preliminary results also point to current limits of the test method and the need for adapting it and current theories to meet the specific requirements of biological materials.

The diffusion behavior of elements constituting Hastelloy C-276 (C, Si, Mn, Co, W, Fe, Cr, Mo, and Ni) in alumina films was investigated using secondary ion mass spectroscopy. The films were deposited by ion-beam-assisted deposition and annealed in vacuum over a temperature range of 500–1000 °C. Characterization of film microstructure was performed using transmission electron microscopy and selected area diffraction analyses. The films were predominantly amorphous with alumina nanocrystallites nonuniformly dispersed throughout the volume both before and after annealing. A relatively wide interface region between the Hastelloy substrate and alumina film was formed in the as-deposited sample due to ion beam mixing. No diffusion of any of the substrate elements was observed after annealing, except for Mn, Cr, and Ni. The impurity depth distributions consisted of two components, which differed by several orders of magnitude with respect to diffusion coefficient and solubility. Activation energies and temperature dependencies of the diffusion coefficients were determined, and a diffusion mechanism was discussed.

Hafnium oxide films were deposited on silicon substrates at deposition temperatures ranging from 190 to 500 °C by metalorganic chemical vapor deposition using an amide precursor, Hf[N(C2H5)2]4, and O2 as source materials. The effect of deposition temperature on the deposition characteristics and electrical properties of the resultant films were investigated. Reaction-limited deposition of hafnium oxide films occurred at deposition temperatures under 380 °C. Concentration of residues, such as carbon, nitrogen, and hydrogen, monotonously decreased with increasing deposition temperature, with nitrogen being the most thermally susceptible. However, surface roughness reached a minimum value at 400 °C. Amorphous films were obtained for deposition temperatures up to 450 °C, but obviously became crystallized at 500 °C. Accumulation capacitance increased with increasing deposition temperature but saturated above 400 °C. Moreover, postdeposition annealing at 800 °C caused no obvious degradation in the electrical properties of the film deposited at 400 °C.

While the dimension of solder bumps keeps shrinking to meet higher performance requirements, the formation of interfacial compounds may be affected more profoundly by the other side of metallization layer due to a smaller bump height. In this study, cross interactions on the formation of intermetallic compounds (IMCs) were investigated in eutectic SnPb, SnAg3.5, SnAg3.8Cu0.7, and SnSb5 solders jointed to Cu/Cr–Cu/Ti on the chip side and Au/Ni metallization on the substrate side. It is found that the Cu atoms on the chip side diffused to the substrate side to form (Cux,Ni1−x)6Sn5 or (Niy,Cu1−y)3Sn4 for the four solders during the reflow for joining flip chip packages. For the SnPb solder, Au atoms were observed on the chip side after the reflow, yet few Ni atoms were detected on the chip side. In addition, for SnAg3.5 and SnSn5 solders, the Ni atoms on the substrate side migrated to the chip side during the reflow to change binary Cu6Sn5 into ternary (Cux,Ni1−x)6Sn5 IMCs, in which the Ni weighed approximately 21%. Furthermore, it is intriguing that no Ni atoms were detected on the chip side of the SnAg3.8Cu0.7 joint. The possible driving forces responsible for the diffusion of Au, Ni, and Cu atoms are discussed in this paper.

Processes and preparation conditions for growing epitaxial thin films of Cu-based, layered oxychalcogenides LnCuOCh (Ln = La, Ce, Pr or Nd; Ch = S1-xSex or Se1-yTey) are reported. Epitaxial thin films on MgO (001) substrates were prepared by a reactive solid-phase epitaxy method. Four-axes high-resolution x-ray diffraction measurements revealed that the crystallographic orientation is (001)[110] LnCuOCh || (001)[110] MgO and the internal stress of the crystalline lattices in the films are relaxed during thermal-annealing process of the reactive solid-phase epitaxy. Furthermore, except for CeCuOS, systematic variations in the lattice constant by chalcogen or lanthanide ion substitutions were observed. These results demonstrated that the reactive solid-phase epitaxy is an efficient technique for fabricating LnCuOCh epitaxial films.

Nanowhiskers and needle-like precipitates obtained by the liquid-liquid interfacial precipitation method for the systems of isopropyl alcohol and toluene solutions of C60 and (η2-C60)Pt(PPh3)2 were examined by transmission electron microscopy. Morphology of the C60 precipitates was remarkably changed by the addition of (η2-C60)Pt(PPh3)2 in the C60 toluene solution, and capsular needle-like crystals of C60 were formed. C60 cages were found to be directly contacted along the growth axis of (η2-C60)Pt(PPh3)2 needle-like crystals.

Electroconductive ceramic composites, constituted of an insulating matrix (a composite AlN-SiC) containing 30 vol% of an electroconductive phase (MoSi2, ZrB2, or ZrC), were densified through hot-pressing. Microstructure and mechanical properties were compared to those of the AlN-SiC matrix material. All the ternary composites are good electrical conductors, with resistivities in the range 0.3 × 10-3 to 4 × 10-3 Ω·cm. Room temperature properties are improved by the addition of the electroconductive particles. Strength and toughness measurements at high temperature show that MoSi2-containing composite is stable up to 1300 °C (strength 611 MPa, toughness 3.7 MPa·m1/2), whereas ZrB2-containing composite is stable up to 1000 °C. ZrC-containing composite is not suitable for high-temperature applications due to poor oxidation resistance.

The deformation of polymer films under repetitive contact at high strain rates was investigated using nanoscale impact testing. Four systems were studied: (i) rubber-modified acrylonitrile-butadiene-styrene (ABS) (0–25 wt% rubber), (ii) uniaxially and biaxially drawn poly(ethylene terephthalate) film; (iii) poly(ethylene oxide)–clay nanocomposites, and (iv) nylon 6–organoclay nanocomposites. The initial results suggest that the technique has much potential in evaluating the fatigue behavior of thinner polymer films and coatings that are unsuitable for conventional methods designed for bulk samples. The extent of impact-induced deformation may be used as a measure of ductility because ductile failures are associated with significant plastic deformation before failure whereas brittle failures usually involve little plastic deformation. The nano-impact technique provides valuable highly localized information about deformation under high strain rate, which is complementary to low strain rate tests such as nanoindentation and nano-scratch. The technique has been shown to be sensitive to nano-/microstructural variations in ABS–rubber film when Berkovich indenters and low impact forces were used. The impact behavior of the nanocomposites is only significantly worse than that of the virgin polymers at the highest clay loading studied (15 wt%). This could be a factor when assessing the suitability of novel nanocomposite materials for applications where toughness is important. On ABS film, there is only an approximate correlation between the plastic work function determined from nanoindentation and the rubber loading in the film while the correlation between the rubber loading and nano-impact data is clear, suggesting that the dynamic test is a more useful predictor of thin polymer film toughness than the slow-loading quasi-static indentation test.

An acetate-based polymeric precursor for producing yttrium-stabilized zirconia (YSZ) was developed. The precursor was prepared under ambient conditions and contains only yttrium and zirconium cations. Dense, crack-free films were fabricated with this precursor on alumina substrates at a rate of 60 nm per deposition, producing polycrystalline YSZ at temperatures as low as 600 °C. Grain growth in thin YSZ films followed Arrhenius equation with an activation energy approximately 0.45 eV. The residual strain in YSZ films decreased with increasing annealing temperature from 600 to 900 °C.

Solid solution Pb1-xBaxTiO3, with particular emphasis on Pb0.5Ba0.5TiO3, was prepared using a sol-gel process incorporating lead acetate trihydrate, barium acetate, and titanium isopropoxide as precursors, acetylacetone (2,4 pentanedione) as a chelating agent, and ethylene glycol as a solvent. The synthesis procedure was optimized by systematically varying acetylacetone: Ti and H2O:Ti molar ratios and calcination temperature. The resulting effects on sol and powder properties were studied using thermogravimetric analysis/differential scanning calorimetry, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller analysis, and x-ray diffraction (XRD). Crystallization of the perovskite structure occurred at a temperature as low as 450 °C. Thin films were prepared by spin coating on (100) MgO. Pyrolysis temperature and heating rate were varied, and the resultant film properties investigated using field-emission scanning electron microscopy, atomic force microscopy, and XRD. Under optimized conditions, highly oriented films were obtained at a crystallization temperature of 600 °C.

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.

For an interface to be considered thermodynamically stable, the phases in contact must be in equilibrium with each other (connected by a stable tie-line) and have negligible mutual solubility on the phase diagram. The stability of Co based magnetic tunnel junctions (MTJs), with Co/MxO1-x/Co structures (M = Al, Gd, Hf, La, Mg, Si, Ti, Ta, Y and Zr), were evaluated with regard to these two conditions. Specifically, low temperature ternary isothermal phase diagrams were calculated and evaluated for the Co–M–O systems. All of these systems have at least one oxide in equilibrium with Co and thus have at least one thermodynamically stable tunnel barrier candidate for use in Co based MTJs. In light of the assumptions made in this analysis, along with the uncertainty in applying bulk enthalpy data to thin films, the current evaluation of interfacial stability serves as a first step in identifying suitable stable tunneling barrier materials in MTJs for detailed study.

Nanostructured Ti5Si3–TiC–Ti3SiC2 and Ti5Si3–TiC composites were in situfabricated through the spark plasma sintering (SPS) technique using Ti and SiC powders as reactants. It was found that the composites could be prepared in arelatively short time (6 min at 1260 °C) above 98% theoretical density. The phase constituents and microstructures of the samples were analyzed by x-ray diffractionand observed by scanning electron microscopy. Transmission electron microscopywas used for detailed microstructural analysis. The results showed that the reaction products mainly consisted of Ti5Si3 and TiC phases or Ti5Si3, TiC and Ti3SiC2phases, depending on the molar ratio of reactants (Ti to SiC). The composites exhibited fine microstructure; TiC grain size was less than 200 nm. Fracturetoughness at room temperature was also measured by indentation tests.