A new essentially nondestructive cross-sectional method is described for measuring the individual thicknesses of multilayer YBa2Cu3O7 (YBCO) and SrTiO3 (STO) thin films using off-axis ion milling and the atomic force microscope (AFM). Since the ion-milling is done during routine patterning of a thin-film device and the AFM requires only a small area for imaging, no additional sample preparation is required. This is a significant improvement over traditional cross-sectional techniques which often require lengthy and destructive sample preparation. Also, there is no a priori reason that this technique would not be amenable to other multilayer thin-film systems.

Dislocations have been observed in deformed Cu/Nb nanolayer composites of wavelength 17 and 7 nm. The dislocations thread through the Cu/Nb interfaces even though there is a change of Burgers vector. Conventional and high resolution transmission electron microscopy studies show that the in-plane bowing direction of these dislocations in the Cu layers is opposite to that in the Nb layers, so that the dislocations appear to zig-zag. These observations are explained by the presence of residual tensile stresses in Cu and residual compressive stresses in Nb, which make dislocations bow in opposite directions in the alternating layers.

Scanning tunneling microscopy (STM) and atomic force microscopy (AFM) investigation of tetracyanoquinodimethane (TCNQ) and the related C60-TCNQ thin films is presented. Periodic molecular chains of the TCNQ on highly oriented pyrolytic graphite (HOPG) substrates were imaged, which demonstrated that the crystalline (001) plane was parallel to the substrate. For the C60-TCNQ thin films, we found that there were grains on the film surface. STM images within the grain revealed that the well-ordered rows and terraces, and the parallel rows in different grains were generally not in the same orientation. Moreover, the grain boundary was also observed. In addition, AFM was employed to modify the organic TCNQ film surface for the application of this type of materials to information recording and storage at the nanometer scale. The nanometer holes were successfully created on the TCNQ thin film by the AFM.

This paper is a comprehensive review of the state-of-knowledge in the field of radiation effects in glasses that are to be used for the immobilization of high-level nuclear waste and plutonium disposition. The current status and issues in the area of radiation damage processes, defect generation, microstructure development, theoretical methods and experimental methods are reviewed. Questions of fundamental and technological interest that offer opportunities for research are identified.

Microstructure control of the SmBCO superconductor was carried out using the floating zone partial melting and solidification method. It is generally recognized that finely and uniformly dispersed nonsuperconductive high temperature stable phase (Sm211) particles included in the superconductive Sm123 matrix act as effective pinning centers. Microstructure formation of the partial molten mixture (Sm211 particles and BaO–CuO liquid) by decomposition of the precursor Sm123 on melting and solidification of Sm123 from the mixture have to be controlled concurrently to fabricate the 123/211 composite fiber with the optimum microstructure. During unidirectional solidification, planar crystal growth which provides the single crystal growth of Sm123 becomes unstable with increased growth rate. During unidirectional melting, the mean diameter of aligned Sm211 particles behind the melting interface decreases with increased growth rate and with decreased temperature gradient at the melting interface. Initial composition of the precursor significantly affects the formation behavior of Sm211 particles. The contribution of process parameters to the microstructure formation is also briefly discussed.

The possibility of controlling Nd-422 phase dimension and morphology, both in the partially melted state and in the final superconducting matrix, was investigated. Nd–Ba–Cu–O samples were prepared by the melt powder melt growth (MPMG) technique. Precursor materials containing Nd as either Nd2O3 or Nd-422, formed during precursor quenching, were used. The role of Pt in Nd-422 refining was analyzed. The effect on Nd-422 nucleation and growth, of stoichiometries with increasing Nd-422 molar excesses (0%, 10%, 20%, and 40%) combined with different heating processes, up to the partially melted state, were examined. Uniformly distributed needle-like particles (1 μm diameter and 10–15 μm length) were obtained at 1120 °C and resulted in a further refined distribution trapped in completely processed samples.

Transparent organic analogues were directionally solidified to investigate, via in situ observation the peritectic reaction occurring in the YBa2Cu3O7−x (YBCO)-superconductor system. Nucleation and growth of peritectic and properitectic phases were examined with respect to similarities with the solidification of the YBCO superconductor. The selected organic system, salicylic acid-acetamide, turned out to match the requirements concerning crystal shape, small nucleation rate of the peritectic phase on the properitectic phase, existence of stoichiometric phases with no solubility limits, and undercooling ability of the peritectic phase. Several features of YBCO growth which were previously deduced only from metallographic cross sections could be verified by direct observation. The organic analogue system will also be used in the future to improve numerical simulations.

Two classes of samples, designated A and B, of layered Bi–Sr–Ca–Cu oxides having the same nominal composition 4 : 3 : 3 : 4, but different thermal histories, were investigated by using field modulated microwave absorption (ESR), powder x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), and x-ray absorption near the edge structure (XANES). Previous electrical resistivity measurements showed that the B samples presented only two superconducting phases with midpoints of the transition temperatures at ∼80 K and ∼105 K. The microwave absorption technique indicated instead the presence of islands which became superconducting at the above-mentioned temperatures also in the A samples. The crystalline and electronic structures of the two types of samples are illustrated and discussed. A plausible theoretical interpretation of the experimental results, based on a quantum percolation model with Coulomb interaction, is also given.

This paper describes the growth and analysis of cubic boron nitride films in a low-density, supersonic nitrogen/argon plasma flow into which boron trichloride gas was injected. Both hexagonal boron nitride (h-BN) and cubic boron nitride (c-BN) were synthesized using this apparatus. Phase selectivity is obtained by applying a relatively low negative bias voltage to the substrate. All of the films described in this paper were grown on {100} silicon wafers at substrate temperatures varying from 400–700 °C. Boron nitride films with greater than 90% cubic phase were successfully synthesized with this method. The films were analyzed using infrared spectroscopy, x-ray photoelectron spectroscopy, and scanning electron microscopy. The volumetric percentages of the hexagonal and cubic phases were determined from model fits to the infrared transmission spectra of the films. X-ray photoelectron spectroscopy provided qualitative evidence for the presence and/or lack of sp2 bonding through the identification of a π-plasmon feature in the spectra. Infrared reflectance spectra are used to provide insight into the growth mechanisms leading to c-BN formation and have revealed features which are not present in the transmission spectra, specifically the 1305 cm−1 LO mode of c-BN and the 1610 cm−1 LO mode of h-BN. The mean ion energies involved with this bias-enhanced chemical vapor deposition (CVD) process are much lower than the ion energies in traditional physical vapor deposition (PVD) processes; however, the ion fluxes (currents) used in this CVD process are at least an order of magnitude higher, resulting in a total momentum transfer to the deposited atoms through ion bombardment that is at least equal to or greater than that reported for many ion-enhanced PVD processes.

Electromigration damage in Al-based interconnects with three compositions (pure Al, Al–1%Si–0.5%Cu, and Al–2%Cu) was studied quantitatively. Using scanning electron microscopy, the spacings between more than 1000 voids and hillocks were measured. The distribution of the spacings was found to be a function of the composition, the applied current density, and the linewidth. The measurements confirm the existence of a threshold product of current density and diffusion length. In particular, a dependence of this threshold product on the Cu content was found. The results of the analysis show that there are clear correlations between the details of the microscopic damage processes and the lifetime of the conductor lines.

The energetics of a simple model of void nucleation on a contaminated patch between the sidewall and metal in an integrated circuit interconnect are examined to determine void nucleation behavior. The conditions under which there is no void nucleation barrier are represented by a simple relationship between the volume driving force, the equilibrium contact angle, the surface energy of the metal, and the contaminated patch radius. The void nucleation barrier, when it exists, is a strong function of these same parameters, and increases sharply as the driving force decreases, and under some conditions, increases with increasing equilibrium contact angle.

The deformation characteristics of icosahedral Al–Cu–Fe quasicrystals were determined by high temperature creep experiments between 680 and 720 °C and 15 and 41 MPa. The deformation process was determined to be controlled by grain boundary mechanisms. Both the stress and grain size sensitivity exponents were found to be 2, suggesting that grain boundary sliding was the rate-controlling deformation mechanism. Microstructural analysis supported this conclusion, as no intragranular defects were produced during the deformation experiments.

A technique for in situ laser light scanning (LLS) was developed to monitor surface damage on nickel-base superalloy specimens under low-cycle fatigue conditions. This technique characterizes the surface state with a parameter called the defect frequency which minimizes memory requirements and data processing time since it does not involve image processing. As a result, the present technique is capable of scanning speeds that are substantially greater than those achieved with image processing methods. Cylindrical Inconel 718 specimens were tested using an automated servo-hydraulic machine at ambient temperature under fully reversed strain control conditions for constant strain amplitudes ranging from 0.3% to 1%. The fatigue damage was monitored by scanning a laser beam along the gauge section of the specimens during periodic interruptions of the cyclic loading. Acetate replicas of the gauge section surface were also made on some of the specimens to characterize the damage using SEM and image analysis techniques. Comparisons of the results demonstrate the capabilities of the present light-scanning technique for characterizing fatigue damage on the surface of the Inconel 718 specimens. In particular, a rapid rise in the mean defect frequency is shown to correspond to an initial increase in microcrack density that saturates at approximately 20% of the fatigue life. This transient behavior is followed by a plateau in defect frequency which corresponds to crack propagation and interlinkage until failure occurs. The number of cycles to microcrack density saturation as indicated by the defect frequency is found to be linearly related to the number of cycles to failure. Accordingly, the present system provides a characterization of microcrack damage that may be used to predict the low-cycle fatigue life of Inconel 718 specimens long before failure occurs.

Ion implantation into amorphous carbon has been initiated to investigate the possibility of superhard carbon-nitride formation. Studies of implantation-temperature effects by 100 keV N+ or 80 keV C+ ions at 50 μA show a narrow temperature window at approximately −100 °C for the optimum surface hardness and elastic modulus (measured by nanoindentation), both values much higher than those for the unimplanted amorphous carbon. No distinguishable properties are found between nitrogen and self (carbon) implantations. At a dose rate of 5 μA, however, the optimum hardness and modulus are found at a lower implantation temperature, with a broader temperature window. The enhanced strengths are well correlated with the asymmetric diffuse peak at around 1500 cm−1 in Raman spectroscopy, and the increased ratio of sp3- over sp2-bonded carbon sites observed by electron energy loss spectroscopy.

The evolution of the contact area during an indentation process has been xamined by an ac technique and also by finite element analysis on five mechanically different materials. Constant contact area regimes were observed during the initial unloading stage and the duration of that regime depends strongly on material properties. The consistency of the results obtained by the two approaches not only proves the validity and advantage of the ac indentation technique but also confirms the applicability of contact stiffness equation. The influence of a hardness impression on unloading characteristics has also been clearly demonstrated by numerically simulating a reloading process.

High quality single-crystal CoSi2 layers have been successfully formed on Si(100) using low energy high dose Co ion implantation followed by subsequent annealing method as a buffer layer for the deposition of YBa2Cu3O7−x (YBCO) thin films. Rutherford backscattering spectrometry with channeling (RBS-C) measurements showed that CoSi2 layers after annealing at temperatures between 850 and 950 °C had a minimum yield Xmin of about 3%. X-ray diffraction (XRD) spectra revealed that CoSi2 layers had the same orientation as the Si(100) substrates. Phi scan XRD spectra proved that CoSi2 layers epitaxially grew in the cube-on-cube epitaxial growth mode with respect to the Si(100) substrates. YBCO films and CeO2/YSZ buffer layers were deposited on CoSi2/Si(100) substrates via laser ablation and electron beam evaporation, respectively. θ-2θ, ω, and φ scan XRD spectra illustrated that YBCO films and CeO2/YSZ buffer layers had the epitaxial structure both in a-b plane and along the c-axis. YBCO films grown on this multilayered structure demonstrated excellent superconducting properties with the zero resistance transition temperature Tc0 of 87–90 K. The transition width (ΔTc) was about 1 K. Orientation and epitaxial crystalline quality of YBCO films and CeO2/YSZ buffer layers were confirmed by XRD and RBS-C characterization. All films consisted of c-axis oriented grains. RBS-C spectra indicated a high degree of crystalline perfection with a channeling minimum yield for Ba as low as 8%, and interdiffusion between the YBCO film and buffer layers or between the YBCO film and the substrate was limited. This multilayer system shows the possibility for the application of YBa2Cu3O7−x thin films on technical Si substrates in the field of hybrid superconductor-semiconductor technology.

Stress driven nucleation of voids in passivated aluminum interconnect lines is analyzed within the context of classical nucleation theory. A discussion of sources of tensile stress in such lines leads to an upper limit of 2 GPa. Calculations suggest that even at this high stress, nucleation rates are far too low to account for observed rates of voiding. Void formation at a circular defect at the line/passivation interface is then considered. In this case, a flaw on the order of nanometers in size may develop into a void under the imposed stress. These results strongly suggest that void nucleation in aluminum interconnect lines can be controlled by eliminating defects in the line/passivation interface.

Hydrogen uptake and discharge by thin metallic films under potentiostatic control was studied using x-ray diffraction at the National Synchroton Light Source (NSLS). The formation of metal-hydrogen phases in Pd, Pd-capped Nb, and Pd/Nb multilayer electrode structures was deduced from x-ray diffraction data and correlated with the cyclic voltammetry (CV) peaks. The x-ray data were also used to construct a plot of the hydrogen concentration as a function of cell potential for a multilayered thin film.

The corrosion characteristics of a-C:H/fluorocarbon composite films deposited on type 301 stainless steel substrates were investigated using potentiometry and electrochemical impedance spectroscopy. The films were deposited by radio frequency (13.56 MHz) plasma deposition from different mixtures of hexafluoroethane, acetylene, and argon. A 10 nm thick polysilicon film was plasma-deposited prior to a-C:H film deposition to improve adhesion. The anodic current densities recorded with all the coated samples, in an electrolyte consisting of 0.1 M NaCl and 0.1 M Na2SO4 at 1.5 V (Standard Calomel Electrode), were at least three orders of magnitude less than that for a bare steel sample. They were also at least 20 times less than that obtained with diamond-like carbon film-coated substrates. EIS spectra obtained for these samples, while exposed to 0.6 M NaCl solution over an extended period of time (30–40 days), confirm their barrier properties. All the coatings showed near capacitive behavior in the frequency range 10 mHz–4 KHz.

The phase formation and microstructural development of SrBi2Ta2O9 thin films prepared via spin-coating using metalorganic solution on Pt/Ti/SiO2/Si substrates have been investigated in this study. The spun-on films started to crystallize from above 550 °C and were well crystallized at 800 °C. At higher than 850 °C a secondary phase having a pyrochlore structure was formed in the films. The analysis of EDS and SIMS confirmed that the interaction between the films and the titanium species which diffused outward from the titanium layer on substrates was the origin for the occurrence of the pyrochlore phase. In addition, varying the thickness of the coated films and platinum layers had remarkable influence on the formation amount of the pyrochlore phase.