Epitaxial PbTiO3 (PTO) thin films were grown on (001) LaAlO3 (LAO) substrates by a preseeded, two-step process via spin coating a Pb–Ti double alkoxide precursor solution. In the first step, a substrate was preseeded with epitaxial islands of PTO by coating the substrate with a very thin layer of the precursor solution and heat treating to 800 °C for 1 h. The isolated islands had an epitaxial orientation relationship of [100] (001)PTO || [100] (001)LAO. In the second step, another PTO thin film was deposited by spin coating to produce an epitaxial film via grain growth from the seeded islands. The sequence of epitaxy during heating between 400 and 800 °C was characterized by x-ray diffraction, scanning electron microscopy, atomic force microscopy, and transmission electron microscopy (TEM). This sequence was compared to the case where the LAO substrate was not seeded. Regardless of whether the substrate was seeded or not, perovskite PTO grains nucleated and grew within the pyrolyzed, amorphous film. Films grown on the unseeded substrates were, at best, only highly textured, polycrystalline films. TEM observations showed that only a low number of epitaxial nuclei formed at the substrate/film interface due, apparently, to the large strain energy associated with the large lattice mismatch (~4%) between PTO and LAO. Other, unoriented, PTO grains that nucleated within the amorphous film were not consumed as the epitaxial grains grew larger with increasing temperature. On the other hand, good epitaxial films could be produced when the number density of epitaxial nuclei was increased by first forming a seeded substrate.

Thin films possessing microstructure composed of isolated vertical pillars were deposited by glancing angle deposition (GLAD) without the need for subsequent etch processing. The GLAD technique uses substrate rotation and oblique angle flux incidence to deposit a porous columnar thin film with engineered microstructures. Thin films with a pillar microstructure were fabricated from a variety of metals, metal oxides and fluorides, and semiconductors. The rate and incident angle of vapor flux, as well as the substrate rotation speed during deposition, were found to critically affect pillar microstructure. Thin films with pillar diameters and densities as low as 30 nm and 3 pillars per μm2, respectively, were deposited. The low stress, high surface area, and porous nature of these films suggests use of pillar microstructure films in optical, chemical, biological, mechanical, magnetic, and electrical applications.

PbS nanoparticles modified with di-n-hexadecyldithiophosphate (DDP) were prepared by the chemical surface modification method. The structure of the PbS nanoparticles coated with DDP was investigated by means of infrared spectroscopy (ir), x-ray photoelectron spectroscopy (XPS), x-ray diffraction (XRD), transmission electron microscopy (TEM), and 31P nuclear magnetic resonance spectroscopy (31P NMR). The thermal stability of DDP coating on the PbS nanoparticles was compared with that of pyridinium di-n-hexadecyldithiophosphate (PyDDP) using a thermogravimetric analyzer (TGA). It was found that coated PbS nanoparticles had an average diameter of about 5 nm. Surface modification with DDP prevented water adsorption and effectively improved the dispersive capacity and antioxidative stability of PbS nanoparticles. The thermal stability of DDP coating on the surface of nano-PbS particles was higher than that of modifier PyDDP because of the chemical interaction between PyDDP and PbS during the coating process.

Erasable optical storage on an organic complex thin film m-nitrobenzal malononitrile and diamine benzene (m-NBMN/DAB) has been demonstrated. High contrast pattern can be produced by 780 nm laser pulses and can be erased by heating. The static optical recording characteristics were studied by the homemade static characterizer, and the structural properties of the thin films were investigated by the high resolution scanning electron microscope (HRSEM) and transmission electron microscope (TEM).

B–C–N compounds were prepared on molybdenum by means of bias-assisted hot filament chemical vapor deposition (HFCVD). Effect of the substrate temperature (Ts) on the growth of B–C–N films has been investigated systematically by x-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) based on the detailed analysis and calculation of the XPS. The substrate temperature plays a key role in the formation of the bonding states, the composition, and the surface morphology. Boron carbonitride is the main phase at all depositing temperatures, and the obtained compounds are as follows: B0.83C0.17 + B0.39C0.35N0.26 at 873 K, B0.30C0.34N0.36 at 973 K, B0.64C0.36 + B0.51C0.23N0.26 at 1073 K, B0.51C0.31N0.18 at 1173 K, and B0.37C0.54N0.09 at 1273 K.

When polycrystalline films form by nucleation, growth, impingement, and coalescence of islands on a substrate surface, the grain size at impingement depends on the relative magnitudes of the nucleation rate, the growth rate, and the dimension of the zone from which adatoms diffuse to a growing island. A simple description of the interdependence of these parameters is developed. It is used to discuss the dependence of the grain-size-at-impingement and the intrinsic stress resulting from coalescence on the deposition rate and the substrate temperature, and to discuss how these might affect texture evolution during film growth.

The influence of the synthesis temperature of a new fly ash–belite cement (FABC) on its hydraulic activity and microstructural characteristics is discussed in this work. Three types of FABC were synthesized at 700, 800, and 900 °C after a previous hydrothermal treatment at 200 °C of the fly ash, CaO, and water mixture. The hydraulic activity of the pastes was evaluated during a period of 200 days from mixing through the combined water content, previously determined from thermogravimetric analyses, and the hydration advance degree by x-ray diffraction (XRD). The microstructure characterization of the pastes was studied by scanning electron microscopy (SEM).

The effect of heat treatment on the corrosion behavior of seven amorphous melt-spun Mg–Ni–Nd alloys containing 10–20 at.% Ni and 5–15 at.% Nd has been studied. Hydrogen evolution testing was used to determine the dissolution rate of the heat-treated specimens immersed in a 3% NaCl solution saturated with Mg(OH)2. The dissolution rates of the partially crystallized specimens were found to be lower than those of the untreated specimens, while the fully crystallized specimens exhibited marked deterioration of corrosion resistance. X-ray diffraction (XRD) and transmission electron microscopy (TEM) studies on the heat-treated specimens revealed precipitation of Mg3Nd, Mg12Nd, and Mg2Ni phases during the crystallization. TEM results show that the partially crystallized structure consists of uniform dispersion of either Mg3Nd or Mg2Ni in the amorphous matrix. In contrast, multiple phases precipitate in the fully crystallized specimen.

This paper presents a model to evaluate quantitatively the adhesion of diamond coating according to indentation tests. It is found that small indentation load causes round spallation of the coating, no matter what the shape of the indenter. An exponential sink-in deformation of the coating under the indentation is proposed [y = −a × exp(−bx)]. The deformation stress at the spallation edge is considered the coating adhesion. Using an experimentally observed relation of the indentation load versus the film spallation radius, we evaluate the adhesion of a diamond coating on copper to be about 1.921–1.956 GPa, which is in agreement with thermal quench results. The validity of this model is also verified by its self-consistence.

Elastic modulus of small specimens and thin films can be determined in bending tests using cantilever or three-point arrangement. The paper presents the basic formulae for these measurements, analyzes the errors which can arise, and shows how they can be reduced. The use of the method is illustrated on glass, silicon, and glass coated with TbDyFe.

Shock compression experiments on powder mixtures of niobium metal and quartz were conducted for the pressure range of 30–40 GPa by a 25-mm single-stage propellant gun. Chemical reaction occurred above 35 GPa, and products were found to be mainly so-called “Cu3Au-type” Nb3Si, which contained a small amount of oxygen. Microtextures of the specimen were examined by scanning and transmission electron microscopy. A field-emission transmission electron microscope was used for energy-dispersive x-ray analysis of microtextures in small particles found in the SiO2 matrix, and various species with different Nb/Si ratio and oxygen content were shown to be produced through the nonequilibrium process of shock compression.

Electrodeposited Ni and Ni-diamond composite layers were used as diffusion barriers for Fe to facilitate the diamond growth on stainless steel substrates. Raman spectroscopy and scanning electron microscopy show the formation of good quality diamond crystallites by chemical vapor deposition. X-ray diffraction results indicate that the expansion of Ni unit cell has taken place due to the formation of the Ni–C solid solution. This observation is also well supported by x-ray photoelectron spectroscopy studies. The lattice constant of the expanded Ni unit cell matches closely with the diamond, and this may be helpful in explaining the epitaxial growth of diamond on single-crystal Ni observed by others.

Thin films of polychloroprene (CR; Neoprene-W) were made by casting its solution (2.0 wt%) in benzene onto the water surface, and some of them were stretched by a desired amount of strain (ε) in their “molten” state. The specimens thus prepared were then crystallized and examined by transmission electron microscopy. Morphological observations in bright- and dark-field imaging modes and selected-area electron diffraction analysis revealed directly that filamentous entities observed in the bright-field image are the edge-on lamellar crystals. It was, therefore, confirmed that the morphological results obtained from the thin specimens of CR without any electron staining are basically in accord with those reported so far for the OsO4-stained thin films of CR.

A new thin film synthesis route based on the electrochemical oxidation of PcLi2 and deposition of lithium phthalocyanine (PcLi) onto indium tin oxide (ITO) substrate is demonstrated. The effects on the thin film morphology of various parameters such as the electrolysis time, the nature of the solvent, and the oxidation potential are investigated. The thin film growth is studied via x-ray diffraction, potential step experiments, and ex situ scanning electron microscopy. Various morphologies of the x-form thin films are observed for different electrolysis times and solvents. Thin films grown in acetonitrile of thickness above 1 μm consist in unidirectionally oriented needle-shaped crystallites.

In this paper, we report our findings in the deposition of carbon nitride by radio-frequency–plasma-enhanced chemical vapor deposition (RF-PECVD) at temperatures slightly above room temperature (RT) and pressures of 800 mTorr using NH3 and C2H4 as source gases. The variation of the NH3/C2H4 source gas ratio and rf power is shown to affect the N/C ratio and sp3/sp2 ratio in a reproducible manner. An NyC ratio as high as 1.17 has been obtained under optimized growth conditions of NH3/C2H4 ratio of 7.3 and rf power of 90 W. X-ray diffraction (XRD) indicates the presence of microcrystalline carbon nitride in an amorphous CNx matrix with preferred orientation along the (100) direction. X-ray photoelectron microscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) studies show that our assignment of the XPS peaks and FTIR absorption bands are mutually consistent and in good agreement with published data. Both methods of analysis show the increase in the sp3 component with increase in N incorporation in the film.

Manganese oxide films for lithium secondary batteries were prepared using a reactive evaporation method. Mn was evaporated from a molybdenum boat by resistive heating and deposited on a glass slide under oxygen atmosphere. These films were examined with x-ray photoelectron spectroscopy (XPS) and x-ray diffraction. The Mn oxide films with a wide valency of Mn were prepared in this study. A rapid change of the back pressure was found as the deposition of Mn was started. This implies that Mn atoms start to react with O2. This means that in situ detection of reactive evaporation process can be utilized.

The fracture behavior of diamondlike carbon (DLC) coatings on Si substrates has been examined using microindentation. The presence of DLC coatings reduces the radial crack length to less than one-half the crack length observed in uncoated Si at the same indenter load. A total work of fracture analysis of the radial cracks formed in the DLC-coating/Si-substrate system gives 10.1 MPa m1/2 as the average fracture toughness for DLC alone. A bond-breaking calculation for DLC suggests that the elastic limit fracture toughness should be 1.5 MPa (m)1/2. The higher value obtained from experiment and total work analysis suggests that plastic work and/or a tortuous path crack evolution occurred during DLC fracture process.

Microstructure modification of amorphous carbon films containing about 30 at.% hydrogen (a-CHx) and nonhydrogenated amorphous carbon (a-C) films was accomplished with a vacuum arc metal plasma implanter and a cathodic arc plasma system, respectively. The films were implanted with Si, Ti, Hf, W, and Al of ion doses approximately equal to 1 and 3 × 1016 ions/cm2 and mean ion kinetic energies in the range of 3–70 keV, depending on the implantation method. Simulation results demonstrated a profound effect of the size of implant species, ion dose, mean ion kinetic energy, and implantation processes on the implant spatial distributions. Statistical roughness results showed a negligible effect of ion implantation on the film surface topography. Elastic recoil spectroscopy revealed a decrease in the hydrogen content of the a-CHx films due to the ion bombardment. A monotonic decrease in the Raman scattering intensities and a downward shift of the carbon peak position occurred with increasing ion dose for both types of films and implantation techniques. Nanoindentation experiments demonstrated an effect of ion implantation on the apparent film hardness, depending on the flux and kinetic energy of implanted species. Changes in the hardness characteristics of the implanted films are interpreted in terms of the chemical reactivity of implant elements and microstructure modifications caused by irradiation damage, dehydrogenation, and higher contents of tetrahedral (s p3) carbon hybridization due to carbide bond formation.

The microstructure of the amorphous, silicide, and crystalline Fe films grown on Si(001) substrates by a radio-frequency (rf) magnetron sputtering was studied in synchrotron x-ray scattering experiments. During the growth, iron-silicide interlayers were always formed. The silicide interlayer became crystalline β–FeSi2 at high rf power (⩾20 W/cm2) and at the substrate temperature of 100 °C. The formation of the β–FeSi2 was also promoted by postannealing to 300 °C. The Fe films grown on top of the silicide interlayer were amorphous at low substrate temperatures (⩽100 °C). It became crystalline only at high substrate temperature (300 °C) with the low rf power of 2 W/cm2. The crystalline Fe film was nonepitaxial but had the [111] preferred orientation.

Inelastic neutron scattering is applied for the first time to monitor directly the concentration of calcium hydroxide formed during the hydration of tricalcium silicate. Results taken between 10 and 40 °C show that the onset of calcium hydroxide formation is delayed at lower temperatures but that the final quantity formed appears to be converging to a temperature-independent value. At 20°C, the 28 day value is 1.3 moles per mole of tricalcium silicate. Combining these results with previous measurements of the free water index made using quasielastic neutron scattering reveals that the hydrogen content of the C–S–H gel decreases significantly at increased curing temperature.