In situ scanning electron microscopy was performed during elevated-temperature (⩽760 °C) tensile-creep deformation of a face-centered-cubic cobalt-based Udimet 188 alloy to characterize the deformation evolution and, in particular, the grain boundary-cracking evolution. In situ electron backscatter diffraction observations combined with in situ secondary electron imaging indicated that general high-angle grain boundaries were more susceptible to cracking than low-angle grain boundaries and coincident site-lattice boundaries. The extent of general high-angle grain-boundary cracking increased with increasing creep time. Grain-boundary cracking was also observed throughout subsurface locations as observed for postdeformed samples. The electron backscattered diffraction orientation mapping performed during in situ tensile-creep deformation proved to be a powerful means for characterizing the surface deformation evolution and in particular for quantifying the types of grain boundaries that preferentially cracked.

Poly(amic acid) (PAA)–clay nacrelike composite films have been prepared by electrophoretic deposition of an emulsion of PAA, which was synthesized from pyromellitic dianhydride and 4,4′-dianminodiphenyl ether (ODA), containing various loadings of ODA-modified montmorillonite (MMT). The layered silicate was intercalated through reacting with PAA, and the ordered layered assembly of the PAA–MMT composite films was successfully accomplished, as conformed by Fourier transform infrared analysis and x-ray diffraction. The structural characterization of the films was supported by scanning electron microscopy, which displayed an ordered layered structure. The thermogravimetric analysis showed the content of the ODA-modified clay in PAA–MMT composite films that changed from 14.3 to 32.1 wt% and the improved thermal properties of the composite films. The mechanical properties of the composites were measured by tensile test. It was found that the modulus and strength of the composite films were greatly improved compared to those of the pure polymer film. An increment of about 155% in the modulus and 40% in the tensile strength were obtained from the composite films.

The integration of ferroelectrics in nanodevices requires firstly the preparation of high-quality ultrathin films. Chemical solution deposition is considered a rapid and cost-effective technique for preparing high-quality oxide films, but one that has traditionally been regarded as unsuitable, or at least challenging, for fabricating films with good properties and thickness below 100 nm. In the present work we explore the deposition of highly diluted solutions of pure and Ca-modified lead titanates to prepare ultrathin ferroelectric films, the thickness of which is controlled by the concentration of the precursor solution. The results show that we are able to obtain single crystalline phase continuous films down to 18 nm thickness, one of the lowest reported using these methods. Below that thickness, the films start to be discontinuous, which is attributed to a microstructural instability that can be controlled by an adequate tailoring of the processing conditions. The effect of the reduction of thickness on the piezoelectric behavior is studied by piezoresponse force microscopy. The results indicate that films retain a significant piezoelectric activity regardless of their low thickness, which is promising for their eventual integration in nanodevices, for example, as transducer elements in nanoelectromechanical systems.

We investigated the polishing rate and selectivity of nitrogen-doped Ge2Sb2Te5 (NGST) to SiO2 film for different abrasive materials (colloidal silica, fumed silica, and ceria abrasives). They both were strongly dependant on abrasive material properties. The polishing rate of nitrogen-doped NGST decreased in the order ceria, fumed silica, and colloidal silica abrasives, which was determined by abrasive material properties, such as abrasive hardness, crystal structure, and primary and secondary abrasive sizes. In addition, the polishing rate slope of NGST film was not significantly different for different abrasive materials, indicating that the polishing of NGST film is mechanical dominant polishing. In contrast, the polishing rate slope of SiO2 film decreased in the order ceria, fumed silica, and colloidal silica abrasives, indicating that the polishing of SiO2 film is chemical dominant polishing. Furthermore, the difference in polishing rate slopes between NGST and SiO2 film gave a polishing rate selectivity of NGST to SiO2 film higher than 100:1 with colloidal silica abrasive.

We investigated structural and characteristic changes in thin HfO2 films (<10 nm) by varying their thicknesses and also examined their influence on the properties of Pt/SrBi2Ta2O9/HfO2/Si metal/ferroelectric/insulator/semiconductor (MFIS) structures. HfO2 films with different thicknesses were found to exhibit rather distinct characteristics and to profoundly affect the properties of the fabricated MFIS capacitor. We found that, when employing 3.2-nm-thick HfO2 as the buffer layer, the MFIS capacitor showed good memory performance at low operation voltage. However, this study demonstrated that some of the HfO2 limited its application in MFIS memory, even though it is the most promising alternative gate dielectric material.

We obtained Ba3Yb(BO3)3 single crystals by the flux method with solutions of the BaB2O4–Na2O–Yb2O3 system. The evolution of the cell parameters with temperature shows a slope change at temperatures near 873 K, which may indicate a phase transition that is not observed by changes appearing in the x-ray powder patterns or by differential thermal analysis (DTA). The evolution of the diffraction patterns with the temperature shows incongruent melting at temperatures higher than 1473 K. DTA indicates that there is incongruent melting and this process is irreversible. Ba3Yb(BO3)3 has a wide transparency window from 247 to 3900 nm. We recorded optical absorption and emission spectra at room and low temperature, and we determined the splitting of Yb3+ ions. We used the reciprocity method to calculate the maximum emission cross section of 0.28 × 10−20 cm2 at 966 nm. The calculated lifetime of Yb3+ in Ba3Yb(BO3)3 is τrad = 2.62 ms, while the measured lifetime is τ = 3.80 ms.

A polymer, which by pyrolysis transforms into Al–C–N–(O) ceramics, was synthesized from trimethylamine alane and cyan amide, and its applicability as a sintering additive for Si3N4 was investigated. Si3N4 powders were mixed with the precursor by treatment with organic slurries of the precursor to induce the homogeneous distribution of the additive. The green-bodies were pretreated in air or NH3 at 800 °C to control the chemical composition of the additive, through which the densification of Si3N4 could be improved. Dense samples with very fine grains (<2 μm) were obtained after sintering at 1600 °C in 0.1 MPa N2. Besides silicon nitride, submicrometer silicon carbide particles were observed in the samples, indicating that this procedure (i.e., the use of this novel sintering additive) also allows for the fabrication of SiC–Si3N4 composites.

Accurate determination of the “zero point,” the first contact between an indenter tip and sample surface, has to date remained elusive. In this article, we outline a relatively simple, objective procedure by which an effective zero point can be determined accurately and reproducibly using a nanoindenter equipped with a continuous stiffness measurement option and a spherical tip. The method relies on applying a data shift, which ensures that curves of stiffness versus contact radius are linear and go through the origin. The method was applied to fused silica, sapphire single crystals, and polycrystalline iron with various indenter sizes to a zero-point resolution of ≈2 nm. Errors of even a few nanometers can drastically alter plots and calculations that use the data, including curves of stress versus strain.

A multiscale modeling approach applied to the stiffness prediction of polymers with high cross-link density is discussed. The material of focus in this work is the ionic polymer Nafion®. The approach applies rotational isomeric state theory in combination with a Monte Carlo methodology to develop a simulation model for polymer chain conformation. From this a large number of end-to-end chain lengths between cross links are generated; the probability density function of these lengths is estimated with the most appropriate Johnson family method. This estimation is used in a Boltzmann statistical thermodynamics approach to the multiscale prediction of stiffness. This work addresses the importance of the simulated polymer chain length in the generation of stable predictions. The multiscale prediction is found to be physically reasonable; the approach has the potential of serving as a first-order prediction tool for properties that are experimentally difficult or impossible to measure.

Oxyfluoride aluminosilicate glasses with compositions of 50SiO2–20Al2O3–20BaF2–10GdF3–0.5PrF3–xYbF3(x = 0, 1.0, 2.5, 5, 7.5, 10, 15, 20, 25, and 30 mol%) have been prepared to study their thermal and optical properties. From the differential thermal analysis (DTA) measurement, glass-transition temperatures and onset crystallization temperatures have been evaluated and from them, glass-stability factors against crystallization were calculated. Glass stabilities were decreased gradually with fluoride content increment in all the studied glasses. The photoluminescence and decay measurements have also been carried out for these glasses. In these glasses, an efficient near-infrared (NIR) quantum cutting with optimal quantum efficiency approaching 160% have been demonstrated, by exploring the cooperative downconversion mechanism from Pr3+ to Yb3+ with 481 nm (3P0 → 3H4) excitation wave length. These glasses are promising materials to achieve high-efficiency silicon-base solar cells by means of downconversion in the visible part of the solar spectrum.

We have studied grain coupling and critical current density (Jc) in ex situ processed Fe-sheathed MgB2 tapes fabricated by a powder-in-tube (PIT) technique, using MgB2 powder soaked in various chemical solutions. The grain coupling and the Jc are strongly influenced by the chemical solutions. Compared with the chemical treatment in a benzene solution of benzoic acid, the use of a cyclohexane solution of benzoic acid doubles the Jc value. Cyclohexane is less stable and hence effectively removed from the surface of MgB2 grains, bringing about the improved coupling of grains and the Jc enhancement.

Oligomerically modified reactive montmorillonite clay was used in the preparation of aramid-layered silicate nanocomposites. The dispersion behavior of organoclay was monitored in the aramid matrix synthesized from 4-aminophenylsulfone and isophthaloyl chloride in dimethylacetamide. These polyamide chains were end-capped with carbonyl chloride groups to interact chemically with oligomerically modified layered silicate. Thin composite films containing 2 to 20 wt% of organoclay were probed for x-ray diffraction (XRD), transmission electron microscopy (TEM), mechanical testing, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and water absorption measurements. XRD and TEM results described the distribution level of clay platelets and morphology of hybrid materials. Mechanical measurements revealed that modulus and strength improved up to 6 wt% clay loading, while toughness of nanocomposites increased with the addition of 2 wt% clay content in the matrix. The elongation showed a decreasing trend with increasing clay content in the hybrids. Thermal-decomposition temperatures of the nanocomposites were in the range 225 to 450 °C. The glass-transition temperature increased up to 12 wt% addition of organoclay in the matrix relative to pristine aramid depicting interfacial interactions among the phases. Water absorption of the nanocomposites reduced with augmenting organoclay loading, indicating decreased permeability.

A modified casting Al–Cu alloy with ultrahigh tensile strength and ductility of about 520 MPa and 13.5% was obtained by PrxOy addition. PrxOy was decomposed to form AlPrO3, which acted as the effective heterogeneous nuclei for the crystallization of the primary α–Al phase. The main reason for the simultaneous increase in the strength and ductility of the modified alloy may be attributed to the effect of a large number of regular, network, and homogeneous nanoscale θ′ phase precipitates and more crystal grain and dendrite boundaries formed by their refinement on restricting and impeding the dislocation actuation and movement.

Fe-encapsulating carbon nano onionlike fullerenes (NOLFs) were obtained by chemical vapor deposition (CVD) using heavy oil residue as carbon source and ferrocene as catalyst precursor in an argon flow of 150 mL/min at 900 °C for 30 min. Field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive spectroscopy (EDS), x-ray diffraction (XRD), and Raman spectroscopy were used to characterize morphology and microstructure of the products. The results show that Fe-encapsulating NOLFs collected at the outlet zone of quartz tube had core/shell structures with sizes ranging from 3 to 6 nm and outer shells composed of poorly crystallized graphitic layers. Their growth followed particle self-assembling growth mechanism, and all atoms in the graphite sheets primarily arose from Fe-carbide nanoparticles.

A facile one-pot synthetic approach, using oleic acid and oleylamine as composite stabilizers combined with high-temperature treatment in 1-octadecene, has been developed for the preparation of monodisperse and uniform lanthanum phosphate and europium-doped lanthanum phosphate nanocrystals. In particular, with the present synthetic approach, the size of the resulting nanocrystals could be tuned precisely and continuously from 3.5 to 6.5 nm by seed-mediated epitaxial growth. The as-obtained uniform nanocrystals with hydrophobic surfaces, which show efficient photoluminescence, could be easily dispersed in nonpolar solvents. More importantly, these nanocrystals can also be easily modified to water-dispersed ones with hydrophilic surfaces for potential use in in vitro imaging in bioanalysis. In addition, a synthetic mechanism for these monodisperse nanocrystals is presented and discussed.

The microstructures, interfacial reactions, and bonding strength properties of the Ti–Cu dissimilar joints using a commercially available Ag–28Cu–2Ti filler were studied, particularly as they relate to the role of an Ag barrier layer at the Ti interface. A joint microstructure and interfacial reactions closely related to the formation of brittle interfacial Ti–Cu intermetallics were fully dominated by the presence of the Ag layer at the Ti interface. Reliable Ti(base)/TiAg/Ag/Ag–Cu eutectic/Cu(base) joints without any detrimental Ti–Cu intermetallics were achieved at low brazing temperatures below 810 °C by applying an Ag interlayer of suitable thickness. It was notable that their bonding strengths were strong enough to exceed the strength of a Cu bulk base metal. This research demonstrates the potential application of an Ag interlayer for the reliable Ti–Cu dissimilar joints.

Results of an investigation of the interaction potential of synthetic and pre-treated calcium silicate hydrate (C-S-H) [with hexadecyltrimethylammonium (HDTMA)] are reported. The effective and strong interaction of these molecules with the C-S-H surface was shown using 13C and 29Si cross polarization magic angle spinning (CP MAS) nuclear magnetic resonance, x-ray diffraction, thermogravimetric analysis, scanning electron microscopy, and Fourier transform infrared spectroscopy analysis. The HDTMA–C-S-H interaction is influenced by the poorly crystallized layered structure of C-S-H. An indefinite number of layers and an irregular arrangement are confirmed by the SEM images. The position and shape of the 002 reflection of C-S-H are affected by drying procedures, chemical pre-treatment, and reaction temperature. Recovery of the initial 002 peak position after severe drying and rewetting with distilled water or interaction with HDTMA is incomplete but accompanied by an increase in intensity. It is inferred that the stability of C-S-H binders in concrete can be affected by a variation in nanostructure resulting from engineering variables such as curing temperature and use of chemical admixtures.

The oxidation behavior of Zr2[Al(Si)]4C5 and Zr3[Al(Si)]4C6 in air has been investigated. The oxidation kinetics of bulk Zr2[Al(Si)]4C5 and Zr3[Al(Si)]4C6 at 900–1300 °C generally follow a parabolic law at a very short initial stage and then a linear law for a long period with the activation energy of 237.9 and 226.8 kJ/mol, respectively. The oxide scales have a duplex structure, consisting of mainly an outer porous layer of ZrO2, Al2O3, and aluminosilicate/mullite, and a thin inner compact layer of these oxides plus remaining carbon. The oxidation resistance of Zr2[Al(Si)]4C5 and Zr3[Al(Si)]4C6 has been improved compared with Zr2Al3C4, and is much better than ZrC due to larger fraction of protective oxidation products, Al2O3 and aluminosilicate/mullite.

An in situ surface-reaction approach has been developed for the synthesis of microcrystals Cu4I4(C6H5N)4, Cu4I4(C9H7N)4, and Cu2I2(C8H6N2) in solid films. Microcrystals of Cu4I4(C6H5N)4, Cu4I4(C9H7N)4, and Cu2I2(C8H6N2) were easily formed on a copper substrate at the solid Cu–liquid pyridine (C6H5N),–quinoline (C9H7N), and–quinoxaline (C8H6N2) interfaces. The resulting microcrystal films were characterized by photoluminescence spectroscopy, scanning electron microscopy, transmission electron microscopy, energy dispersive x-ray spectroscopy, x-ray diffraction, and electrochemical impedance spectroscopy. The effect of ligands on the morphology of the film materials and their chemical properties were also discussed. These microcrystal films possessing reversible photocurrent and photovoltage properties were studied in detail. The photoactive and mechanically stable complex films described here may provide new strategies for fabricating photoluminescence solid films, photomodulation potential, and current films. The potential applications of the microcrystal films are for small light-induced electronic junction and photoluminescence sensors.

This work reports for the first time the synthesis of γ-(Al1-xFex)2O3 solid solutions with a high specific surface area (200-230 m2/g) by the decomposition of metal oxinate [(Al1-xFex)(C9H6ON)3] and investigated the potential of these materials as catalysts for the synthesis of carbon nanotubes by catalytic chemical vapor deposition using methane or ethylene as carbon the source. The nanocomposite powders prepared by reduction in H2-CH4 contain carbon nanotubes (CNTs), which are mostly double-walled but also contain a fair amount of undesirable carbon nanofibers, hollow carbon particles, and metal particles covered by carbon layers. Moreover, abundant metallic particles are observed to cover the surfaces of the matrix grains. By contrast, the nanocomposite powders prepared by reduction in N2-C2H4 are not fully reduced, and the CNTs are much more abundant and homogeneous. However, they are multiwalled CNTs with a significant proportion of defects. The powders were studied by several techniques including Mössbauer spectroscopy and electron microscopy.