Successful application of sol-gel, metalorganic decomposition, or hydrothermal routes to ceramic thin films depends on the mechanical integrity of the precursor film. Above a critical thickness, a precursor film will crack or decohere from the substrate during drying. The cracking and thickness of thin metalorganic precursor films were simultaneously observed during drying using a standard optical microscope. Isochromatic color fringes produced by interference of reflected white light were used to monitor film thickness. The critical film thickness was determined by the color fringe corresponding to the thickness at which propagating cracks terminated. As a demonstration of the technique, the critical thickness of titanium di(isopropoxide) bis(ethyl acetoacetate) films was measured, showing increased critical thickness with the addition of small amounts of an elastomeric polymer.

PbTiO3 (PT) thin films have been deposited by sol-gel on Pt/Si, SiO2/Si, Pt/Ti/SiO2/Si, and Ti/Pt/Ti/SiO2/Si and annealed for 45 min in the 400–670 °C range. Analysis by x-ray diffraction (XRD) and spectroscopic ellipsometry shows that the Ti overlayer promotes early crystallization in the tetragonal perovskite phase, reducing the presence of a second phase, tentatively identified as pyrochlore, starting by 450 %C. The refractive index and extinction coefficient (n, k) of the PT film increase rapidly with the sintering temperature in the range of 450–570 °C and saturate by 570 °C to values of n varying from 2.4 to 2.9, and k from 0.03 to 0.3, over the 1.65–2.95 eV range. Most of the increase of n is related to thin film densification.

In this paper, a new method to study cyclic plastic deformation in thin metal films is presented. Cu films were deposited onto compliant substrates allowing the film to be subjected to tensile and compressive stresses on loading and unloading of the film/substrate composite. The film stress was measured in situ by x-ray diffraction. First results lend to characteristic stress-strain hysteresis curves, indicative of fatigue processes in small dimensions.

Profile evolution simulations during chemical vapor deposition based on a 2D continuum model reveal that the type of surface kinetics plays an important role in determining step coverage of films deposited in high aspect ratio trenches and vias. Linear surface kinetics, resulting from an adsorption rate limited process, is found to cause difficulty in bringing about conformal step coverage in deep narrow trenches without reducing the growth rate considerably. Under such condition, void-free filling cannot be achieved while maintaining a growth rate acceptable to integrated circuit (IC) manufacturing. The numerical study also suggests that the high tendency of the precursor for chemical equilibrium on a surface, resulting in nonlinear kinetics by a surface reaction limited process, is crucial to achieve a uniform step coverage as typically observed in SiO2 deposition from tetraethylorthosilicate (TEOS).

In hydroxylated poly(styrene-b-butadiene-b-styrene) (HO–SBS) micelle, ZnS/CdS composite nanocrystals were prepared by adding Cd2+ ions and Zn2+ ions to the system sequentially. The resulting composites were identified with elemental analysis, transmission electron microscopy, x-ray diffraction, surface photovoltage spectroscopy, and electric field induced surface photovoltage spectroscopy.

CeO2 films with thicknesses ranging from 8.8 to 199 nm were grown on Al2O3 (1102) (R-cut) substrates by off-axis rf magnetron sputtering. X-ray diffraction showed an epitaxial relationship with the CeO2 (001) planes parallel to the Al2O3 (1102) planes for all film thicknesses. Atomic force microscopy (AFM) revealed a rough surface morphology consisting of crystallites with lateral dimensions of 10–90 nm. In the thinnest film, these crystallites were regularly shaped and uniformly distributed on the substrate, while they were rectangularly shaped and oriented mainly in two directions, orthogonal to each other, in the thicker films. The surface roughness of the films increased with increasing layer thickness. Characterization of the microstructure was done by cross-sectional transmission electron microscopy (XTEM) and showed a polycrystalline, highly oriented, columnar structure with a top layer terminated by (111)-facets. High-quality YBa2Cu3O7−δ (YBCO) thin films were deposited directly onto the CeO2 layers. XTEM, rather surprisingly, showed a smooth interface between the YBCO and CeO2 layer. Postdeposition ex situ annealing was carried out on two CeO2 films and evaluated by AFM. Upon annealing samples at 930 °C, a relatively smooth morphology without facets was obtained. Annealing films at 800 °C caused no appreciable change in surface morphology, whereas igniting a YBCO plasma during a similar anneal clearly altered the sample surface, giving facets that were rounded.

The texture in the melt-processed GdBCO superconductor is studied as a function of Gd2BaCuO5 additions, using a texture goniometer. A systematic variation observed in the background intensity is connected to the microstructural variations and the powder x-ray diffraction spectra.

A transmission electron microscope (TEM) micrograph of cross-sectionally viewed Vickers indentation made on the surface of (001) silicon at ambient temperature was obtained. The picture clearly reveals a triangle area, pointing downward and having nondiffraction-contrast, left after unloading, which further confirms the amorphized range induced by indentation in silicon. Analysis of the picture directly manifests a significant recovery of indentation depth. Surface shape and range of the amorphous silicon region do not coincide with that of the indenter and the corresponding distribution pattern of hydrostatic stress beneath indentation predicted by elastoplastic theory, respectively. It seems that the amorphization could not be attributed to the result of hydrostatic stress alone.

A numerical model has been developed to examine the temperature history of a multilayer wafer undergoing rapid thermal processing (RTP) for various doping densities. Partial transparency and thin film interference effects are considered. Doping levels from ∼1015 to ∼1018 cm−3 are examined. Numerical temperature predictions of the lightly doped wafer are compared with experimental measurements. Heating rates for the lightly doped wafer fluctuate due to partial transparency effects and reach a maximum of ∼50 °C/s. The heavily doped wafer sees a maximum heating rate of ∼100 °C/s. Because the wafers are opaque above 700 °C regardless of their level of doping, all wafers reach steady state at ∼845 °C.

Polycrystalline, wurtzitic indium nitride was synthesized by saturating indium with nitrogen from microwave plasma sources. The structure was confirmed by x-ray diffraction, electron diffraction, and elemental analysis. Two types of growth were observed: (i) dendritic crystals on the original melt surface, and (ii) hexagonal platelets adjacent to the In metal source on the upper edge of the crucible. The method does not involve a foreign substrate to initiate growth and is a potential alternative to the high-pressure techniques normally associated with bulk growth of indium nitride. The lattice parameters were a = 3.5366 ± 0.0005 Å and c = 5.7009 ± 0.0005 Å, with c/a = 1.612 ± 0.0005.

An attempt has been made to improve the intermediate temperature strength of cryomilled NiAl by utilizing third element solid solution or precipitation strengthening mechanisms. To this end an NiAl–0.7 (at.%) Zr alloy was cryomilled, densified by hot extrusion, and tested between 1000 and 1400 K. Although over 3 wt% nitrogen was introduced via cryomilling, mechanical testing revealed that the cryomilled NiAl–0.7Zr was significantly weaker than the base alloy between 1000 and 1200 K. Chemical and microstructural analyses revealed that, in addition to ∼ 16 vol% AlN, all the Zr had been converted into ZrN. A thermodynamic analysis of cryomilling indicated that the formation of ZrN could have been anticipated since it is a more stable nitride than AlN. While Zr was an unsatisfactory addition in NiAl, thermodynamics also suggest several alloying elements that might lead to good intermediate temperature strength after cryomilling.

X-ray diffraction and microstructural studies were carried out on 2 : 17 type Sm–Co alloys containing Fe, Cu, and Zr (13–14 at.% Sm, 57–60 at.% Co, 20–22 at.% Fe, 4 at.% Cu, and 3 at.% Zr) in as-cast and heat-treated conditions. Microstructural studies revealed that the as-cast alloys contain three phases. It was observed that the samples subjected to sintering at 1463 K for 45 min followed by a solution treatment at 1448 K for 1 h resulted in nearly a single-phase, rhombohedral crystal structure (Th2Zn17-type). Subsequent isothermal aging at 1123 K and ramp-cooling to 673 K resulted in a mixture of Sm2Co17- and SmCo5-type phases with the former as major phase. It was also found that samples (Sm > 13 at.%) sintered at temperatures >1463 K showed incipient melting and multiphase formation.

Gravimetry and x-ray diffraction were used to study the kinetics and mechanism of internal oxidation in air at 300–600 °C of Ag–2 and 4 at.% Mg alloys. All the features typical of the non-Wagnerian behavior in more dilute alloys (the slower initial and faster intermediate kinetics, oxygen release from the samples at the late stages, and stabilization of highly hyperstoichiometric oxides with O/Mg up to 1.74 ± 0.02) are also observed in these more concentrated alloys. A linear correlation between the lattice parameter of oxidized alloys, magnesium content, and amount of excess oxygen is found and used for analyzing the published data on the lattice parameters in other oxidized Ag–Mg alloys. Such analysis suggests that, at early stages of low-temperature oxidation, O/Mg ratios could be higher than 4 ± 0.8, which is interpreted as evidence that O–Mg interaction at these stages is the trapping of mobile O atoms by immobile Mg atoms, so that oxidation of Ag–Mg alloys can be considered as formation and subsequent decomposition of Ag–Mg–O solid solutions, and it is the decomposition stage that significantly affects the oxidation kinetics. Possible impact of these findings on optimization of alloy-sheath composition and microstructure in Bi2223/AgMg superconducting tapes is discussed.

A scanning acoustic microscope (SAM) has been used to investigate the structure of thermoplastic leather. This material is formed by pressing fibers of leather under high pressure and moderate temperature. The result is a matrix from transformed, melted fibers in which leftover fibers act as reinforcement. Unlike the scanning electron microscope (SEM), the SAM is able to distinguish between completely and incompletely transformed fibers and also to penetrate the material beneath the surface. The results show that the matrix is built as a domain structure. The advantages of the SAM over the SEM for organic materials are indicated.

Ag, S, Ag + S, and S + Ag single and double ion implantations in silica glass were performed at room temperature. The implantation energies were chosen in order to get a projected range of 40 nm. The fluences were 2 × 1016 S+ cm−2 and 5 × 1016 Ag+ cm−2. Silver interacts weakly with the host silica matrix and forms essentially metallic clusters; this weak interaction between Ag and SiO2 induces formation of silver silicate rather than silver oxide. Double ion implantations of silver and sulfur lead to chemical interaction between the two species that is critically influenced by the implantation sequence. In particular, in the Ag + S sample silver and sulfur atoms react to form crystalline core (Ag)–shell (Ag2S) nanoclusters.

KTiOPO4 (KTP) phase formation in stoichiometric mixtures corresponding to chemical formulas of {A1} [B5+1/2C3+1/2]O(D5+)O4 (A = K+; B = Nb5+ and Ta5+; C = Al3+, Cr3+, Ga3+, Fe3+, and In3+; and D + P5+ and As5+), and {A+} [B5+2/3C2+1/3]O(D5+)O4 (C = Mg2+ and Zn2+) prepared by solid-state reaction technique is reported. It was found that the mixtures containing Nb5+, Ga3+, Fe3+, and As5+ form the longest series of members of the KTP structural family. KTP phase formation was detected by x-ray powder diffraction analysis. Comparison of the lattice parameters measured with those known for the nonsubstituted crystals of the KTP family was carried out. The data obtained were used for the discussion of variations of KTP structural stability on composition.

The surface morphology of TiO2- and ZrO2-based thin films, deposited from aqueous solution at 70–80 °C onto functionalized organic self-assembled monolayers (SAMs) on silicon has been examined using atomic force microscopy (AFM). The films have been previously shown to consist, respectively, of nanocrystalline TiO2 (anatase) and of nanocrystalline tetragonal ZrO2 with amorphous basic zirconium sulfate. The films exhibit characteristic surface roughnesses on two length scales. Roughness on the nanometer scale appears to be dictated by the size of the crystallites in the film. Roughness on the micron scale is postulated to be related to several factors, including the topography of the SAM and the effects of larger, physisorbed particles or agglomerates. The topographies of the oxide thin films, on both the nanometer and micron scales, are consistent with a particle-attachment mechanism of film growth.

Mixed composition layered lead zirconate titanate (PZT) films sZr/Ti ratio = 30/70 + 65/35d with stoichiometric lead containing PZT thin layer at the film/electrode interface were successfully fabricated by a modified chemical solution deposition method. These modified PZT thin films are highly (111) textured, and have square-shaped P-E hysteresis loops with large remanent polarization and low coercive field, as well as low saturation voltage. In addition, these films show good fatigue and imprint behavior with Pt electrodes; the retained polarization of the modified film was above 50% after fatigue testing to 109 cycles, and the thermally induced voltage shifts (ΔV) were 0.51 V after heating at 150 °C for 4410 s, two times lower than for films without a stoichiometric thin layer.

Ln(Mg1/2Ti1/2)O3 (Ln = Dy, La, Nd, Pr, Sm, Y) compositions have been prepared, and their pertinent properties for use as thin film substrates for YBa2Cu3Ox (YBCO) were measured. X-ray diffraction shows that Ln(Mg1/2Ti1/2)O3 compositions have noncubic symmetry and the GdFeO3-type structure. Dielectric constant measurements revealed values between 22 and 27, which are larger than those of the LnAlO3 family. Quality factor (=1/ tan δ) of the ceramic specimens measured at room temperature was larger than 3000 at 10 GHz. Among the compounds, La(Mg1/2Ti1/2)O3 exhibited the highest dielectric constant and the lowest dielectric loss. Chemical reaction was observed between Ln(Mg1/2Ti1/2)O3 (Ln = Dy, Sm, Y) and YBCO after annealing a 1 : 1 mixture at 950 °C. Considering dielectric and physical properties, La(Mg1/2Ti1/2)O3 and Sm(Mg1/2Ti1/2)O3 were determined to be suitable substrates for YBCO thin film used in microwave applications.

The possibility of stabilizing the theoretically predicted β–C3N4 phase by high-energy ball milling is investigated. Charges of graphitic carbon were milled with and without minor alloying additions under different atmospheric media, namely gas and/or liquid phases of nitrogen, air, or ammonia. Milling was performed at either of two energy levels for periods of up to 48 h. The β–C3N4 phase was found to exist as small crystallites in a matrix of primarily amorphous carbon at volume fractions estimated between 5 and 10 at.%. High-resolution electron diffraction and x-ray diffraction indicate that the crystalline nature of the C3N4 phase corresponds with a hexagonal lattice with a = 6.46 Å and c/a = 0.374, which are within 2% of the theoretically calculated lattice parameter values. Analysis of electron energy-loss spectroscopy (EELS), x-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectra verify the presence of chemically bonded carbon and nitrogen with chemical states reflecting combined sp2 and sp3 hybridization. Chemical analysis confirms nitrogen enrichment at levels consistent with the C3N4 stoichiometry and the estimated degree of stabilization. The possible mechanism(s) responsible for the stabilization of the β–C3N4 phase are briefly discussed.