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Showing papers in "Journal of Materials Research in 1999"


Journal ArticleDOI
TL;DR: In this paper, the authors examined the stress associated with crystallite coalescence during the initial stages of growth in thin polycrystalline films with island growth morphology and predicted large tensile stresses in agreement with experimental results.
Abstract: We examined the stress associated with crystallite coalescence during the initial stages of growth in thin polycrystalline films with island growth morphology. As growing crystallites contacted each other at their bases, the side-walls zipped together until a balance was reached between the energy associated with eliminating surface area, creating a grain boundary and straining the film. Our estimate for the resulting strain depends only on interfacial free energies, elastic properties, and grain size and predicts large tensile stresses in agreement with experimental results. We also discuss possible stress relaxation mechanisms that can occur during film growth subsequent to the coalescence event.

554 citations


Journal ArticleDOI
TL;DR: In this paper, a detailed analysis of Sneddon's solution for indentation by a rigid cone reveals several largely ignored features that have important implications for nanoindentation property measurement.
Abstract: Methods for analyzing nanoindentation load-displacement data to determine hardness and elastic modulus are based on analytical solutions for the indentation of an elastic half-space by rigid axisymmetric indenters. Careful examination of Sneddon's solution for indentation by a rigid cone reveals several largely ignored features that have important implications for nanoindentation property measurement. Finite element and analytical results are presented that show corrections to Sneddon's equations are needed if accurate results are to be obtained. Without the corrections, the equations underestimate the load and contact stiffness in a manner that leads to errors in the measured hardness and modulus, with the magnitudes of the errors depending on the angle of the indenter and Poisson's ratio of the half-space. First order corrections are derived, and general implications for the interpretation of nanoindentation data are discussed.

403 citations


Journal ArticleDOI
TL;DR: In this article, Zirconate and titanate pyrochlores were subjected to 1 MeV of Kr+ irradiation and showed a systematic change in the susceptibility to radiation-induced amorphization with increasing Zr content.
Abstract: Zirconate and titanate pyrochlores were subjected to 1 MeV of Kr+ irradiation. Pyrochlores in the Gd2(ZrxTi1-x)2O7 system (x = 0, 0.25, 0.5, 0.75, 1) showed a systematic change in the susceptibility to radiation-induced amorphization with increasing Zr content. Gd2Ti2O7 amorphized at relatively low dose (0.2 displacement per atom at room temperature), and the critical temperature for amorphization was 1100 K. With increasing zirconium content, the pyrochlores became increasingly radiation resistant, as demonstrated by the increasing dose and decreasing critical temperature for amorphization. Pyrochlores highly-enriched in Zr (Gd2Zr2O7, Gd2Zr1.8Mg0.2O6.8, Gd1.9Sr0.1Zr1.9Mg0.1O6.85, and Gd1.9Sr0.1Zr1.8Mg0.2O6.75) could not be amorphized, even at temperature as low as 25 K.

367 citations


Journal ArticleDOI
TL;DR: In this paper, the hardness and elastic modulus of aluminum films with thicknesses of 240, 650, and 1700 nm sputter-deposited on glass were systematically characterized as a function of indenter penetration depth using standard nanoindentation methods.
Abstract: Substrate effects on the measurement of thin film mechanical properties by nanoindentation methods have been studied experimentally using a model soft film on hard substrate system: aluminum on glass. The hardness and elastic modulus of aluminum films with thicknesses of 240, 650, and 1700 nm sputter-deposited on glass were systematically characterized as a function of indenter penetration depth using standard nanoindentation methods. Scanning electron and atomic force microscopy of the hardness impressions revealed that indentation pileup in the aluminum is significantly enhanced by the substrate. The substrate also affects the form of the unloading curve in a manner that has important implications for nanoindentation data analysis procedures. Because of these effects, nanoindentation measurement techniques overestimate the film hardness and elastic modulus by as much as 100% and 50%, respectively, depending on the indentation depth. The largest errors occur at depths approximately equal to the film thickness.

342 citations


Journal ArticleDOI
TL;DR: In this article, the effects of strain gradient on plastic deformation in thermosetting epoxy and polycarbonate thermoplastic were experimentally investigated by nanoindentation and atomic force microscopy.
Abstract: Plasticity in material is typically described as a function of strain, but recent observations from torsion and indentation experiments in metals suggested that plasticity is also dependent on strain gradient. The effects of strain gradient on plastic deformation in thermosetting epoxy and polycarbonate thermoplastic were experimentally investigated by nanoindentation and atomic force microscopy in this study. Both thermosetting and thermoplastic polymers exhibited hardening as a result of imposed strain gradients. Strain gradient plasticity theory developed on the basis of a molecular kinking mechanism has predicted strain gradient hardening in polymers. Comparisons made between indentation data and theoretical predictions correlated well. This suggests that strain gradient plasticity in glassy polymers is determined by molecular kinking mechanisms.

329 citations


Journal ArticleDOI
TL;DR: In this paper, the Scherrer equation (SE), integral breadth analysis (IBA), and single-line approximation (SLA) methods have been employed to extract grain size and microstrain.
Abstract: Measurements of x-ray diffraction (XRD) profiles have been performed on commercially pure Fe and Al powders, cryomilled Fe–3 wt.% Al powders, cold pressed (CP) pure Fe and Al, hot pressed (HP) and hot isostatically pressed (HIP) Fe–3 wt.% Al. Scherrer equation (SE), integral breadth analysis (IBA), and single-line approximation (SLA) methods have been employed to extract grain size and microstrain. The results demonstrate that, in the case of the cryomilled nanocrystalline Fe–3 wt.% Al powders, all these XRD techniques yielded reasonable, consistent grain size results. However, discrepancies were found in cold pressed (CP-Fe), hot pressed (HP-Fe–3 wt.% Al), and hot isostatically pressed (HIP-Fe–3 wt.% Al) samples. TEM imaging revealed the presence of a certain density of dislocations inside the grains in the HP-Fe–3 wt.% Al and HIP-Fe–3 wt.% Al, which is thought to be partly or fully responsible for the observed discrepancies.

255 citations


Journal ArticleDOI
TL;DR: In this paper, a large-scale atomic resolution simulation of nanoindentation into a thin aluminum film using the recently introduced quasicontinuum method is presented to study the initial stages of plastic deformation under the action of an indenter and obtain both macroscopic load versus indentation depth curves, as well as microscopic quantities such as the Peierls stress and density of geometrically necessary dislocations beneath the indenter.
Abstract: This paper presents a large-scale atomic resolution simulation of nanoindentation into a thin aluminum film using the recently introduced quasicontinuum method The purpose of the simulation is to study the initial stages of plastic deformation under the action of an indenter Two different crystallographic orientations of the film and two different indenter geometries (a rectangular prism and a cylinder) are studied We obtain both macroscopic load versus indentation depth curves, as well as microscopic quantities, such as the Peierls stress and density of geometrically necessary dislocations beneath the indenter In addition, we obtain detailed information regarding the atomistic mechanisms responsible for the macroscopic curves A strong dependence on geometry and orientation is observed Two different microscopic mechanisms are observed to accommodate the applied loading: (i) nucleation and subsequent propagation into the bulk of edge dislocation dipoles and (ii) deformation twinning

252 citations


Journal ArticleDOI
TL;DR: This article showed that there can be multiple stress-strain curves for a given set of loading and unloading curves for elastic-plastic solids with work-hardening, and they showed that these curves can be uniquely determined from a conical or pyramidal indenter.
Abstract: Applying the scaling relationships developed recently for conical indentation in elastic-plastic solids with work-hardening, we examine the question of whether stress-strain relationships of such solids can be uniquely determined by matching the calculated loading and unloading curves with that measured experimentally. We show that there can be multiple stress-strain curves for a given set of loading and unloading curves. Consequently, stress-strain relationships may not be uniquely determined from loading and unloading curves alone using a conical or pyramidal indenter.

249 citations


Journal ArticleDOI
TL;DR: In this paper, rare earth aluminates with a rhombohedral structure exhibited larger permittivities than those with an orthorhombic structure, attributed to the difference in ionic size and coordination number.
Abstract: Rare-earth aluminates, LnAlO3 (Ln = Dy, Er, Gd, La, Nd, Pr, Sm, and Y) were prepared using the mixed oxide method, and their microwave dielectric properties were examined at X-band. Most rare-earth aluminates have suitable permittivities and quality factors for applications as dielectric resonators, but a modification of τf is necessary due to the coefficient's large negative value. When considering dielectric properties and lattice matching, YalO3 rather than LaAlO3, was suggested as a promising substrate material for microstrip antennas utilizing high-temperature superconductor thin films. Rare-earth aluminates with a rhombohedral structure exhibited larger permittivities than those with an orthorhombic structure. This difference was attributed to the difference in ionic size and coordination number. It was demonstrated that a nonzero magnetic susceptibility of rare-earth aluminates has an adverse effect on their quality factor. An abrupt variation in the temperature coefficient of permittivity was discussed in terms of oxygen octrahedra tilting.

227 citations


Journal ArticleDOI
TL;DR: In this article, a metallic glass with the nominal composition Zr_(57)Nb_5Al_(10)Cu_(15.4)Ni_(12.6) was used as the matrix in particulate composites reinforced with W, WC, Ta, and SiC.
Abstract: To increase the toughness of a metallic glass with the nominal composition Zr_(57)Nb_5Al_(10)Cu_(15.4)Ni_(12.6), it was used as the matrix in particulate composites reinforced with W, WC, Ta, and SiC. The composites were tested in compression and tension experiments. Compressive strain to failure increased by more than 300% compared with the unreinforced Zr_(57)Nb_5Al_(10)Cu_(15.4)Ni_(12.6), and energy to break of the tensile samples increased by more than 50%. The increase in toughness came from the particles restricting shear band propagation, promoting the generation of multiple shear bands and additional fracture surface area. There was direct evidence of viscous flow of the metallic glass matrix within the confines of the shear bands.

201 citations


Journal ArticleDOI
TL;DR: In this paper, the mechanical properties of vapor-grown carbon fiber (VGCF)/nylon and VGCF/polypropylene composites were discussed, and it was shown that fiber injection can significantly improve the tensile strength and modulus of these composites.
Abstract: This article discusses the mechanical properties of vapor-grown carbon fiber (VGCF)/nylon and VGCF/polypropylene composites. Fibers in the as-produced condition yielded composites with marginally improved mechanical properties. Microscopic examination of these composites clearly showed regions of uninfiltrated fibers, which could account for the unsatisfactory mechanical properties. The infiltration of the fibers by both polymers was improved by carefully ball milling the raw fiber so as to reduce the diameter of the fiber clumps to less than 300 μm. Properties of composites made with ball-milled material were improved in every respect. VGCF reinforcement in nylon slightly improved the tensile strength and doubled the modulus, while VGCF in polypropylene doubled the tensile strength and quadrupled the modulus compared to unreinforced material. Moreover, the composites were sufficiently improved that differences in fiber surface preparation became important. For example, air-etched fibers and fibers covered with low concentrations of aromatics produced polypropylene composites with significantly better mechanical properties than did fibers whose surfaces were heavily coated with aromatics. Both the tensile strength and the modulus of the composites fabricated with clean fibers exceeded theoretical values for composites made with fibers randomly oriented in three dimensions, indicating that the injection-molding process oriented the fibers to some extent.

Journal ArticleDOI
TL;DR: In this paper, the anomalously large expansion on heating and contraction on cooling are attributed to the volume change associated with the allotropic transformation of ZrW2O8 between its high-pressure γ-phase and its low-pressure α-phase.
Abstract: Powder metallurgy was used to fabricate fully dense, unreacted composites consisting of a copper matrix containing 50–60 vol% ZrW2O8 particles with negative thermal expansion. Upon cycling between 25 and 300 °C, the composites showed coefficients of thermal expansion varying rapidly with temperature and significantly larger than predicted from theory. The anomalously large expansion on heating and contraction on cooling are attributed to the volume change associated with the allotropic transformation of ZrW2O8 between its high-pressure γ-phase and its low-pressure α- or β-phases. Based on calorimetry and diffraction experiments and on simple stress estimations, this allotropic transformation is shown to result from the hydrostatic thermal stresses in the particles due to the thermal expansion mismatch between matrix and reinforcement.

Journal ArticleDOI
TL;DR: In this paper, a model of a glass-polymer coating-substrate system indented with hard spheres is investigated, and the morphologies of the cracks and corresponding critical indentation loads for initiation are measured over a broad range of coating thicknesses (20 mm to 5.6 mm).
Abstract: Fracture modes in a model glass–polymer coating–substrate system indented with hard spheres are investigated. The large modulus mismatch between the glass and polymer results in distinctive transverse fracture modes within the brittle coating: exaggerated circumferential (C) ring cracks that initiate at the upper coating surface well outside the contact (as opposed to the near-contact Hertzian cone fractures observed in monolithic brittle materials); median–radial (M) cracks that initiate at the lower surface (i.e., at the substrate interface) on median planes containing the contact axis. Bonding between the coating and substrate is sufficiently strong as to preclude delamination in our system. The transparency of the constituent materials usefully enables in situ identification and quantification of the two transverse fracture modes during contact. The morphologies of the cracks and the corresponding critical indentation loads for initiation are measured over a broad range of coating thicknesses (20 mm to 5.6 mm), on coatings with like surface flaw states, here ensured by a prebonding abrasion treatment. There is a well-defined, broad intermediate range where the indented coating responds more like a flexing plate than a Hertzian contact, and where the M and C cracks initiate in close correspondence with a simple critical stress criterion, i.e., when the maximum tensile stresses exceed the bulk strength of the (abraded) glass. In this intermediate range the M cracks generally form first—only when the flaws on the lower surface are removed (by etching) do the C cracks form first. Finite element modeling is used to evaluate the critical stresses at crack initiation and the surface locations of the crack origins. Departures from the critical stress condition occur at the extremes of very thick coatings (monolith limit) and very thin coatings (thin-film limit), where stress gradients over the flaw dimension are large. Implications of the results concerning practical coating systems are considered.

Journal ArticleDOI
TL;DR: In this article, the effect of low stacking fault energy in pure Cu on microstructural development during ECA pressing at room temperature was examined and it was shown that the low 0stacking fault energy and the consequent low rate of recovery lead to a very slow evolution of the microstructure during pressing.
Abstract: Equal-channel angular (ECA) pressing is a procedure having the capability of introducing an ultrafine grain size into a material. Experiments were conducted to examine the effect of the low stacking fault energy in pure Cu on microstructural development during ECA pressing at room temperature. The results show that the low 0stacking fault energy and the consequent low rate of recovery lead to a very slow evolution of the microstructure during pressing. Ultimately, a stable grain size of −0.27 μm was established in pure Cu but the microstructure was not fully homogeneous even after pressing to a total strain of ∼10. It is shown by static annealing that the as-pressed grains are stable up to ∼400 K, but at higher temperatures there is grain growth. These results lead to the conclusion that a low stacking fault energy is especially favorable for the introduction of an exceptionally small grain size using the ECA pressing procedure.

Journal ArticleDOI
TL;DR: In this paper, the authors presented the mechanics for calculating the quantitative driving force of indentation-induced delamination of thin-film multilayers using standard bending and thin-plate analyses.
Abstract: The mechanics for calculating the quantitative driving force of indentation-induced delamination of thin-film multilayers is presented. The solution is based on the mechanics developed by Marshall and Evans [D.B. Marshall and A.G. Evans, J. Appl. Phys. 56, 2632 (1984).] and extended to the general case of a multilayer by use of standard bending and thin-plate analyses. Presented and discussed are the specific solutions for the bilayer case that show that in the limit of zero thickness of either layer, the solution converges to the single-layer case. In the range of finite thickness, the presence of the superlayer increases the driving force relative to that possible for the original film alone and can be optimized to the experimental situation by proper choice of thickness, elastic constants, and residual stress. The companion paper “Quantitative adhesion measures of multilayer films: Part II. Indentation of W/Cu, W/W, Cr/W” discusses experimental results with copper, tungsten, and chromium thin films.

Journal ArticleDOI
TL;DR: In this paper, the detailed spatially resolved surface temperature increase and subsequent dissipation associated with crack tip plasticity in a Zr-Ti-Ni-Cu-Be bulk metallic glass is characterized for the first time.
Abstract: Deformation in metallic glasses is generally considered to arise from flow in localized shear bands, where adiabatic heating is thought to reduce glass viscosity. Evidence has been inferred from the veined fracture surfaces and molten droplets reported for metallic glasses. In this work, the detailed spatially resolved surface temperature increase and subsequent dissipation associated with crack tip plasticity in a Zr–Ti–Ni–Cu–Be bulk metallic glass is characterized for the first time. Maximum temperatures of up to 54.2 K were estimated from a heat conduction model and shown to be in excellent agreement with a nonhardening plasticity model for the heat generated by a propagating crack. Local cooling was also observed and shown to be consistent with thermoelastic effects.

Journal ArticleDOI
TL;DR: In this article, rare-earth-doped ceria powders with a composition of Ce0.8R0.2O1.9 (R = Yb, Y, Gd, Sm, Nd, and La) were prepared by heating the oxalate coprecipitate when a mixed rare earth/cerium nitrate solution was added to an oxalic solution.
Abstract: Doped ceria, which has a higher oxygen ion conductivity than yttria-stabilized zirconia, is one of the possible electrolytes for solid oxide fuel cell at low temperatures. This study concerns powder preparation and densification of rare-earth-doped ceria. Rare-earth-doped ceria powders with a composition of Ce0.8R0.2O1.9 (R = Yb, Y, Gd, Sm, Nd, and La) were prepared by heating the oxalate coprecipitate when a mixed rare earth/cerium nitrate solution was added to an oxalic solution. The oxalate and derived-oxide powders were characterized by x-ray diffraction (XRD), thermogravimetry differential thermal analysis (TG-DTA), particle size analyzer with laser diffraction, inductively coupled plasma (ICP), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). This method provided the oxalate solid solutions containing Ce and R, which were calcined to form the oxide solid solutions at 600 °C in air. The lattice parameter of oxide powders increased linearly with increasing ionic radius of doped rare earth. The size of platelike particles of oxalates and oxides depended on the concentration of oxalic acid and showed a minimum at 0.4 M oxalic acid. Dry milling of oxide powder with α–Al2O3 ball was effective in reducing the size and aspect ratios of particles with little contamination of Al2O3. These rare-earth-doped ceria powders with various sizes were formed by uniaxial pressing (49 MPa) followed by cold isostatic pressing (294 MPa), and sintered at 900–1600 °C in air for 4 h. The micrometer-sized-doped CeO2 powders were densified above 95% of the theoretical density at 1200 °C. The grain size of rare-earth-doped ceria after sintering at 1600 °C was larger in the samples with the larger rare-earth element.

Journal ArticleDOI
TL;DR: In this paper, the deformation behavior of Knoop indentations made in a soft, porous titanium/aluminum multilayered thin film on a hard silicon substrate was studied through use of the focused-ion-beam milling and imaging technique.
Abstract: The plastic deformation behavior of Knoop indentations made in a soft, porous titanium/aluminum multilayered thin film on a hard silicon substrate is studied through use of the focused-ion-beam milling and imaging technique. Pileup is observed for indentations with depths larger than 30% of the total film thickness. Analysis of the indentation cross sections shows that plastic deformation around the indentation is partly accommodated by the closing of the pores within the multilayers. This densification process reduces the amount of pileup formed below that predicted by finite element simulations. Experimental results show that the pileup is formed by an increase of the titanium layer thickness near the edges of the indentation. The thickness increase is largest near the film/substrate interface and decreases toward the surface of the multilayered film. The amount of normal compression near the center of the indenter is characterized, and it is demonstrated that the deformation becomes more nonuniform with increasing indentation depth.

Journal ArticleDOI
TL;DR: In this paper, the Meyer hardness is defined as the energy consumed to create a residual indentation impression, leading to the concepts of "work of indentation" and "ductility index".
Abstract: The physical insight into the Meyer hardness is given on the basis of the experimental results for indentation load P versus indentation depth h relations and of a simple model for elastoplastic contact deformation. The quadratic relationships of P = k 1 h 2 for loading and P = k 2 ( h − h r ) 2 for unloading with the residual depth of impression h r are essential in the elastoplastic indentation processes and mechanisms. The indentation-induced residual strain energy stored in unloaded impression is properly taken into account. The Meyer hardness is an elastic and plastic parameter that depends not only on the plasticity but also on the elasticity of material indented and significantly depends on the geometry of indenter used. The Meyer hardness is given in terms of the energy consumed to create a residual indentation impression, leading to the concepts of “work of indentation” and “ductility index.”

Journal ArticleDOI
TL;DR: In this article, a strain gradient plasticity modulus with temperature and molecular dependence is proposed and related to indentation hardness, and the physics of the strain-gradient plasticity in glassy polymer is discussed in relation to the modulus.
Abstract: Plastic deformation of metals is generally a function of the strain. Recently, both phenomenological and dislocation-based strain gradient plasticity laws were proposed after strain gradients were experimentally found to affect the plastic deformation of the metal. A strain gradient plasticity law is developed on the basis of molecular theory of yield for glassy polymers. A strain gradient plasticity modulus with temperature and molecular dependence is proposed and related to indentation hardness. The physics of the strain gradient plasticity in glassy polymer is then discussed in relation to the modulus.

Journal ArticleDOI
TL;DR: In this article, the phase equilibria in the Y2O3-Al 2O3 −SiO3 -SiO2 system at 1600, 1400, and 1300 °C were experimentally determined using x-ray diffraction (XRD), scanning electron microscope with attached energy-dispersive detector system (SEM-EDX), and electron probe microanalyzer (EPMA).
Abstract: In order to clarify inconsistencies in the literature and to verify assumed ternary solubilities, the phase equilibria in the Y2O3–Al2O3 –SiO2 system at 1600, 1400, and 1300 °C were experimentally determined using x-ray diffraction (XRD), scanning electron microscope with attached energy-dispersive detector system (SEM-EDX), and electron probe microanalyzer (EPMA). Six quasibinary phases were observed: Y4Al2O9 (YAM), YAlO3 (YAP), Y3Al5O12 (YAG), Y2SiO5, Y2Si2O7 (C and D modifications), and ˜3Al2O3· 2SiO2 (mullite). Y4Al2O9 forms an extended ternary solid solution with the formula Y4Al2(1-x)Si2xO9+x (x = 0 2 ˜0.31). The lowest ternary eutectic temperature was determined at 1371 ± 5 °C by high-temperature differential scanning calorimetry (DSC). The results were compared with previous data available for the Y2O3–Al2O3 –SiO2 system and with data for other RE2O3–Al2O3 –SiO2 (RE = rare earth element) systems.

Journal ArticleDOI
TL;DR: A series of titanium composites, with varying volume fractions of titanium monoboride (TiB) whiskers, were made by mixing various proportions of titanium and titanium diboride powders followed by hot pressing.
Abstract: A series of titanium composites, with varying volume fractions of titanium monoboride (TiB) whiskers, were made by mixing various proportions of titanium (Ti) and titanium diboride (TiB2) powders followed by hot pressing. The phases present were identified by x-ray diffraction. Microstructural examination revealed three different types of TiB whisker morphologies: (i) long and needle-shaped TiB whiskers that are isolated and randomly oriented in the Ti matrix at relatively low volume fractions (0.3), (ii) colonies of refined and densely packed TiB whiskers from intermediatevolume (0.55) to high volume (0.73 and 0.86) fractions, and (iii) coarse and elongated TiB particles with a few needle-shaped whiskers at the highest volume fraction (0.92). In all the composites, TiB was found to be the predominant reinforcement. However, in Ti–TiB composites with 0.86 and 0.92 volume fractions of TiB, a significant amount of TiB2 was also present. The relative volume fractions of Ti, TiB, and TiB2 phases were estimated from the integrated intensities of diffraction peaks by the direct comparison method employing the calculated structure factors and Lorentz polarization factors. The composite microstructure, as well as the evolution of different morphologies, of TiB whiskers is discussed.

Journal ArticleDOI
TL;DR: In this article, a polymerized organic-inorganic complexion route is introduced for the synthesis of yttrium aluminum garnet, YAG (Y3Al5O12) and cordierite (Mg2Al4Si5O18) powders.
Abstract: A polymerized organic–inorganic complexion route is introduced for the synthesis of yttrium aluminum garnet, YAG (Y3Al5O12) and cordierite (Mg2Al4Si5O18) powders. Long-chain polymers such as polyvinyl alcohol (–[CH2–CHOH]-n or PVA) or polyethylene glycol (H[O–CH2–CH2]nOH or PEG) were used as the organic carriers for a precursor ceramic gel. Calcined powders were very porous and homogeneous in distribution of components. Experimental studies by differential thermal analysis and thermogravimetric analysis, x-ray diffraction, solid-state nuclear magnetic resonance, and Fourier transform infrared spectrometry indicated that metal-ion chelation is not the primary mechanism for obtaining molecularly homogeneous precursor powders. Water-soluble cations of mixed oxides in the PVA or PEG process were sterically entrapped in the entangled network and resulted in fine and pure, mixed oxide powders.

Journal ArticleDOI
TL;DR: In this article, the A2M3O12 family of tungstates and molybdates were determined from room temperature to 800 °C, and the observed behavior ranges from strong negative thermal expansion (α = −11 × 10−6 K−1) in Sc2W3O 12 to near zero thermal expansion in Al1.68Sc0.02In0.30W3 O12.
Abstract: Bulk thermal expansion properties of 19 members of the A2M3O12 family of tungstates and molybdates were determined from room temperature to 800 °C. The observed behavior ranges from strong negative thermal expansion (α = −11 × 10−6 K−1) in Sc2W3O12 to near zero thermal expansion in Al1.68Sc0.02In0.30W3O12.

Journal ArticleDOI
TL;DR: In this article, a low-pressure, long-throw sputter deposition with which they have succeeded in fabricating porous titanium thin films possessing “zig-zag,” helical, and “pillar” microstructures, demonstrating microstructural control on a level consistent with evaporated GLAD.
Abstract: Thin films with microstructures controlled on a nanometer scale have been fabricated using a recently developed process called glancing angle deposition (GLAD) which combines oblique angle evaporation with controlled substrate motion. Critical to the production of GLAD thin films is the requirement for a narrow angular flux distribution centered at an oblique incidence angle. We report here recent work with low-pressure, long-throw sputter deposition with which we have succeeded in fabricating porous titanium thin films possessing “zig-zag,” helical, and “pillar” microstructures, demonstrating microstructural control on a level consistent with evaporated GLAD. The use of sputtering for GLAD simplifies process control and should enable deposition of a broader range of thin film materials.

Journal ArticleDOI
TL;DR: In this paper, a new growth mechanism was proposed on the basis of microstructure and different morphologies of the nanowires observed, which is based on the decomposition of semiconductor suboxides and defect structures.
Abstract: Highly pure, ultralong, and uniform-sized semiconductor nanowires in bulk quantity were synthesized by thermal evaporation or laser ablation of semiconductor powders mixed with oxides. Transmission electron microscopy study shows that decomposition of semiconductor suboxides and defect structures play important roles in enhancing the formation and growth of high-quality nanowires. A new growth mechanism is proposed on the basis of microstructure and different morphologies of the nanowires observed.

Journal ArticleDOI
TL;DR: In this paper, the plastic displacements around Knoop indentations made in hard titanium/aluminum multilayered films on soft aluminum alloy substrates have been studied using focused-ion-beam (FIB) milling and high-resolution scanning electron microscopy (SEM), respectively.
Abstract: The plastic displacements around Knoop indentations made in hard titanium/aluminum multilayered films on soft aluminum alloy substrates have been studied. Indentations were cross-sectioned and imaged using focused-ion-beam (FIB) milling and high-resolution scanning electron microscopy (SEM), respectively. The FIB milling method has the advantage of removing material in a localized region without producing mechanical damage to the specimen. The micrographs of the cross-sectioned indentations indicate that most of the plastic deformation around the indentation is dominated by the soft aluminum substrate. There is a very small change in the multilayered film thickness around the indentation—less than 10%. The plastic deformation of the thin film resembles a membrane being deflected by a localized pressure gradient across the membrane. Stress-induced voids are also observed in the multilayered film, especially in the area around the indentation apex. The density and the size of the voids increase with indentation depth. Indentation sink-in effects are observed in all of the indentations inspected. Based on the experimental results, the amount of sink-in of the hard film–soft substrate composite is larger than the bulk substrate and film alone. This is confirmed by the finite element analyses conducted in this work.

Journal ArticleDOI
TL;DR: In this article, a coprecipitation method using various concentrations of NaOH as precipitants was used to extract CaSiO3 powders from an ethanol solution dissolving Ca(NO3)2 · 4H2O and Si(OC2H5)4.
Abstract: CaSiO3 powders were prepared from an ethanol solution dissolving Ca(NO3)2 · 4H2O and Si(OC2H5)4 by the coprecipitation method using various concentrations of NaOH as precipitants. Some Na component remained in the precipitates without washing and strongly affected the characteristics of the resultant powders, but the Na residue was removed by a washing treatment. The precipitate prepared by using 0.33 mol/l of NaOH and twice-washing contained the lowest amount of Na residue. It was calcined at 500 and 900 °C, respectively, to crystallize CaSiO3 phase and ground by a planetary potmill. The ground CaSiO3 powder was sintered to about 89% theoretical density by firing at 1400 °C. By soaking the CaSiO3 sintered bodies in simulated body fluid (SBF) solution for various times, an hydroxylapatite (HAp) layer formed as aggregates of ball-like particles on the surface of the CaSiO3 sintered bodies after soaking for a short period; thereby, the CaSiO3 ceramics is suggested to have very good biocompatibility.

Journal ArticleDOI
TL;DR: In this article, X-ray diffraction was performed on Ln(Mg1/2Ti 1/2)O3 (Ln = Dy, La, Nd, Pr, Sm, Y) compositions and their pertinent properties for use as thin film substrates for YBa2Cu3Ox (YBCO) were measured.
Abstract: 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.

Journal ArticleDOI
TL;DR: In this article, the solid-state phase transition of nanocrystalline maghemite to hematite was investigated by energy dispersive x-ray diffraction (EDXRD).
Abstract: Homogeneous maghemite (γ–Fe2O3) nanoparticles with an average crystal size around 5 nm were synthesized by successive hydrolysis, oxidation, and dehydration of tetrapyridino-ferrous chloride. Morphological, thermal, and structural properties were investigated by transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and x-ray diffraction (XRD) techniques. Rietveld refinement indicated a cubic cell. The superstructure reflections, related to the ordering of cation lattice vacancies, were not detected in the diffraction pattern. Kinetics of the solid-state phase transition of nanocrystalline maghemite to hematite (α–Fe2O3), investigated by energy dispersive x-ray diffraction (EDXRD), indicates that direct transformation from nanocrystalline maghemite to microcrystalline hematite takes place during isothermal treatment at 385 °C. This temperature is lower than that observed both for microcrystalline maghemite and for nanocrystalline maghemite supported on silica.