Measurements of single asperity wear on oxidized silicon surface in aqueous potassium hydroxide (KOH) using atomic force microscopy (AFM), where the single crystal silicon tip was used both to tribologically load and image the surface, is presented. AFM was also operating in the lateral (frictional) force mode to investigate the pH dependence of kinetic friction between the tip and the SiO2 surface. It was shown that the Si tip wear amount strongly depended on the solution pH value and was at a maximum at around pH 10. It was also found that the Si removal volume in mol was approximately equal to that of SiO2 irrespective of the solution pH value. This equality implies that the formation of the Si–O–Si bridge between one Si atom of the tip and one SiO2 molecule of the specimen at the wear interface. The surface of the Si tip is then oxidized. Finally, the bond rupture by the tip movement will occur, the dimeric silica (OH)3Si–O–Si(OH)3, including the Si–O–Si bridge, is dissolved in the KOH solution. The frictional signal is also sensitive to the pH values of the solution and peaked at around pH 10. These results indicate that the removal behavior of the Si tip and SiO2 surface would be affected by the frictional force between the Si and the SiO2, because of an increased liquid temperature and a compressive stress in Si and SiO2 networks. Strong influence is observed by the pH of the ambient solution confirming the important role of the OH− in the wear mechanism. Pressure dependence of the microwear behavior under aqueous electrolyte solutions has also been investigated. A microscopic removal mechanism, which is determined by interplay of the diffusion of water in Si and SiO2, is presented.

Spherical particles of ferrite (intermediate between Fe3O4 and γ-Fe2O3) were grown on seed crystals (∼9 nm) via the green rust route in an aqueous solution added with sucrose, which promotes spherical growth. By highly dispersing the seed crystals in an HNO3 solution, we could control the diameter of the particles over a wide range of 20–200 nm (geometric standard deviation: 1.1–1.4) by changing the amount of the seed crystals. At the beginning of the seed growth, clusters of the seed crystals were resolved into smaller clusters, each composed of a few seed crystals.

In situ devitrification and consolidation of gas atomized Al87Ni8La5 glassy powders into highly dense bulk specimens was carried out by spark plasma sintering. Room temperature compression tests of the consolidated bulk material reveal remarkable mechanical properties, namely, high compression strength of 930 MPa combined with plastic strain exceeding 25%. These findings demonstrate that the combined devitrification and consolidation of glassy precursors by spark plasma sintering is a suitable method for the production of Al-based materials characterized by high strength and considerable plastic deformation.

Zn-0.7 wt.% Cu-hypoperitectic alloy was prepared in a graphite crucible under a vacuum atmosphere. Unidirectional solidification of the Zn-0.7 wt.% Cu-hypoperitectic alloy was carried out by using a Bridgman-type directional solidification apparatus under two different conditions: (i) with different temperature gradients (G = 3.85–9.95 K/mm) at a constant growth rate (41.63 μm/s) and (ii) with different growth rate ranges (G = 8.33–435.67 μm/s) at a constant temperature gradient (3.85 K/mm). The microstructures of the directionally solidified Zn-0.7 wt.% Cu-hypoperitectic samples were observed to be a cellular structure. From both transverse and longitudinal sections of the samples, cellular spacing (λ) and cell-tip radius (R) were measured. The effects of solidification-processing parameters (G and V) on the microstructure parameters (λ and R) were obtained by using a linear regression analysis. The present experimental results were also compared with the current theoretical and numerical models and similar previous experimental results.

To investigate the microwave (MW) processing of Fe3O4, for which occurrence of decrystallization has been reported, the micro/nanostructures of MW-heated Fe3O4 powder were observed in this study. The specimens were irradiated by 2.45 GHz MW at the position of magnetic (H)-field maximum in a TE10 single mode applicator. The specimen was heated well above the Curie temperature in H-field. The heated specimen above 1000 °C revealed the glass-like surface with the diminished x-ray diffraction (XRD) peak intensities. They resemble the reported features of decrystallization in an earlier work performed at Penn State University. According to the XRD profiles of the MW-heated specimens, formation of FeO and shift of Fe3O4 peaks to the lower angle with the broadened width were observed. To account for the findings, a model is presented that phase separation occurred into FeO and Fe3O4 resulting in an increased lattice parameter due to the increased oxygen content. This activity is caused by local transport of oxygen in nanoscale. Considering the shape of the main XRD Fe3O4 peak with a shoulder and the existence of halo in nanobeam diffraction (NBD), amorphous phase areas exist. As a result of transmission electron microscopy observation, it was shown that they were in nanoscaled localized regions, and it was not confirmed that the glass-like morphologies (or decrystallized morphologies) are totally amorphous. The observed micro/nanostructures and mechanism of the amorphous phase formation were discussed considering the Fe-O phase diagram.

La2Zr2O7 (LZO) films have been grown by metalorganic decomposition (MOD) to be used as buffer layers for coated conductors. LZO can crystallize into two similar structures: fluorite or pyrochlore. Coated conductor application focuses on pyrochlore structure because it is a good barrier against oxygen diffusion. Classical x-ray diffraction is not able to separate the contribution of these two structures. Transmission electron microscopy and high-resolution transmission electron microscopy were used to determine the local distribution of these two phases in epitaxial LZO layers grown on LaAlO3. A characteristic feature of LZO thin films deposited by MOD is the formation of nanovoids in an almost single-crystal structure of LZO pyrochlore phase. For comparison, LZO layers deposited by metalorganic chemical vapor deposition were also studied. In this last case, the film is compact without voids and the structure corresponds to pyrochlore phase. Thus, the formation of nanovoids is a characteristic feature of MOD grown films.

Self-organized nanotubular layers are electrochemically fabricated on Ti–4Zr–22Nb–2Sn alloys in water/glycerol (volume ratio 1:1) mixtures containing 0.3 M NH4F. Highly ordered nanotubes with two distinct diameters of ∼203 ± 5 (large size) and 113 ± 5 nm (small size) were observed at the bottom of the layer, which may be ascribed to the different microstructure and composition in this alloy. On extended anodization, the small-size tubes gradually disappeared because of the increasing H+. After annealing for 1 h at 500 °C, the nanotube layer on the Ti–4Zr–22Nb–2Sn alloy was transformed from the amorphous phase to anatase. The nanotubes were connected to each other by spaced rings at the sidewalls, whereas the distance between neighboring rings increased with the amplitude of applied current density.

The microstructural evolution inside adiabatic shear bands in Fe–Cr–Ni alloys dynamically deformed (strain rates > 104 s−1) by the collapse of an explosively driven, thick-walled cylinder under prescribed strain conditions was examined by electron backscatter diffraction. The observed structure within the bands consisted of both equiaxed and elongated grains with a size of ∼200 nm. These fine microstructures can be attributed to recrystallization; it is proposed that the elongated grains may be developed simultaneously with localized deformation (dynamic recrystallization), and the equiaxed grains may be formed subsequently to deformation (static recrystallization). These recrystallized structures can be explained by a rotational recrystallization mechanism.

Thin films of Ga-doped ZnO (GZO) were prepared on glass and Al2O3 (0001) substrates by using RF magnetron sputtering at a substrate temperature of 350 °C, RF power of 175 W, and working pressure of 6 mTorr. The effect of film thickness and substrate type on the structural and electrical properties of the thin films was investigated. X-ray diffraction study showed that GZO thin films on glass substrates were grown as a polycrystalline hexagonal wurtzite phase with a c-axis preferred, out-of-plane orientation and random in-plane orientation. However, GZO thin films on Al2O3 (0001) substrates were epitaxially grown with an orientation relationship of . The structural images from scanning electron microscopy and atomic force microscopy showed that the GZO thin films on glass substrates had a rougher surface morphology than those on Al2O3 (0001) substrates. The electrical resistivity of 1000 nm-thick GZO thin films grown on glass and Al2O3 (0001) substrates was 3.04 × 10−4 Ωcm and 1.50 × 10−4 Ωcm, respectively. It was also found that the electrical resistivity difference between the films on the two substrates decreased from 9.48 × 10−4 Ωcm to 1.45 × 10−4 Ωcm with increasing the film thickness from 100 nm to 1000 nm.

This study is concerned with the investigation of the structural evolution occurring during isothermal annealing of an Mn-89.7 wt%Sb alloy in a high magnetic field in the semisolid state. The alloy specimens were isothermally annealed without and with an 11.5-T magnetic field for various annealing times. With the application of the magnetic field, the average characteristic radius of the primary MnSb particles increased with increasing annealing time. The primary MnSb particles were oriented with their c-plane parallel to the imposed field direction. Furthermore, the primary MnSb particles were found to align along the field direction and form chainlike structures eventually. These phenomena were attributed to the attraction and coalescence of the particles induced by the dipole–dipole interactions among them.

The constitution of the ternary system Al–Cu–Fe in the region above 40 at.% Al at 600 °C is investigated by means of x-ray diffraction, metallography, scanning electron microanalysis, energy dispersive x-ray spectroscopy, and differential thermal analysis. The phase equilibria in the Al-rich corner are clarified by the valuable experimental evidence for the four-phase reaction L + λFe4Al13 ↔ (Al) + ω at 600.7 °C and experimental findings that the phase αFe4CuAl23 was not detected. A thermodynamic model of the Al–Cu–Fe system was then performed over the entire composition range by taking into account the phase diagram data above 560 °C from the literature and the present work. This work challenged the modeling of the considerably complex order–disorder phase transition between bcc_A2 and bcc_B2 phases and the miscibility gap of bcc_B2 phase using the modified sublattice model.

Nix and Gao [J. Mech. Phys. Solids46, 411 (1998)] established an important relation between the microindentation hardness and indentation depth for axisymmetric indenters. We use the conventional theory of mechanism-based strain gradient plasticity [Huang et al., Int. J. Plast.20, 753 (2004)] established from the Taylor dislocation model [Taylor, Proc. R. Soc. London A145, 362 (1934); Taylor, J. Inst. Met.62, 307 (1938)] to study the Berkovich and other triangular pyramid indenters. The three-dimensional finite element analysis shows that the widely used equivalence of equal base area leads to significant errors, particularly in microindentation. A new equivalence of equal angle is proposed for triangular pyramid indenters, and it has been validated for a large range of indenter angles and indentation depths.

Indentation is widely used to extract material elastoplastic properties from measured force-displacement curves. Many previous studies argued or implied that such a measurement is unique and the whole material stress-strain curve can be measured. Here we show that first, for a given indenter geometry, the indentation test cannot effectively probe material plastic behavior beyond a critical strain, and thus the solution of the reverse analysis of the indentation force-displacement curve is nonunique beyond such a critical strain. Secondly, even within the critical strain, pairs of mystical materials can exist that have essentially identical indentation responses (with differences below the resolution of published indentation techniques) even when the indenter angle is varied over a large range. Thus, fundamental elastoplastic behaviors, such as the yield stress and work hardening properties (functions), cannot be uniquely determined from the force-displacement curves of indentation analyses (including both plural sharp indentation and deep spherical indentation). Explicit algorithms of deriving the mystical materials are established, and we qualitatively correlate the sharp and spherical indentation analyses through the use of critical strain. The theoretical study in this paper addresses important questions of the application range, limitations, and uniqueness of the indentation test, as well as providing useful guidelines to properly use the indentation technique to measure material constitutive properties.

Instrumented indentation tests have been widely adopted for elastic modulus determination. Recently, a number of indentation-based methods for plastic properties characterization have been proposed, and rigorous verification is absolutely necessary for their wide application. In view of the advantages of spherical indentation compared with conical indentation in determining plastic properties, this study mainly concerns verification of spherical indentation methods. Five convenient and simple models were selected for this purpose, and numerical experiments for a wide range of materials are carried out to identify their accuracy and sensitivity characteristics. The verification results show that four of these five methods can give relatively accurate and stable results within a certain material domain, which is defined as their validity range and has been summarized for each method.

Nb can improve the oxidation resistance of TiAl; however, the reported concomitant effects on the mechanical properties are controversial. Therefore, the effect of different Nb additions (0∼20.83 at.% Nb) on the lattice distortion as well as dislocation nucleation and mobility of TiAl were examined by density-functional theory calculations to solve the puzzle. The calculation of the formation energy and c/a ratio showed that Nb slightly decreases the phase stability and enhances the anisotropy. The variation of shearing energy barrier demonstrates an interesting staged strengthening effect of Nb on TiAl. Further analyses of the charge density difference and the partial density of states reveal that the physical origination is the electronic anisotropy, which is correlated with the Nb content and distribution.

Mn-90.8 wt%Sb alloys were solidified without and with high magnetic fields to investigate the effects of high magnetic fields on the structure evolution of the alloys. It was found that there were only MnSb/Sb eutectics without any primary phase in the alloy at 0 T, whereas a small amount of primary MnSb dendrites appeared in the MnSb/Sb eutectic matrix when the magnetic flux density was 4.4 T. In magnetic fields of 6.6, 8.8, and 11.5 T, both of two primary phases, i.e., MnSb and Sb, occurred in the matrix. In addition, the volume fraction of these two primary phases increased with increasing magnetic flux density. In magnetic fields of 8.8 and 11.5 T, primary MnSb dendrites aligned parallel to the magnetic field direction and gathered at the edge of the specimens. In contrast, primary Sb dendrites gathered in the center region of the specimens.

Titanium nitride nanopowders were synthesized through a chemical reduction of titanium tetrachloride by sodium in liquid ammonia. The products of the reaction were the mixture of sodium chloride and titanium nitride nanopowders. The mixture was then separated by ammonia extraction. The nanopowders were heated under vacuum up to 1200 °C and were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), Brunauer-Emmet-Teller (BET) surface area measurement, and chemical analysis. The results show that the product is nanocrystalline cubic phase TiN with Ti/N atomic ratio performed 1:1, and the surface area is from 20 to 50 m2 ·g−1 depending on the heating temperature. The particle sizes estimated by the TEM analysis correspond well with the results of the surface area measurements. The XRD pattern indicates that the crystal size grows with an increase in heating temperature.

The morphology of nanocolumns grown by glancing angle deposition is studied for molecular materials forming amorphous and crystalline solids. Amorphous tris(8-hydroxyquinoline)aluminum nanocolumn arrays were obtained at sample rotation speeds varying from 0.3 rpm (revolutions per minute) to 30 rpm. For crystalline pentacene, an array of regular nanocolumns formed at a rotation speed of 3 rpm, while higher and lower rotation speeds led to a wide distribution of column heights and shapes. The incoming molecular flux and the molecular diffusion length on column surfaces, both dependent on rotation speed, were found to govern the resulting morphology of crystalline pentacene nanocolumns.

Fully dense HfC and TaC-based composites containing 15 vol% TaSi2 or MoSi2 were produced by hot pressing at 1750–1900 °C. TaSi2 enhanced the sinterability of the composites and nearly fully dense materials were obtained at lower temperatures than in the case of MoSi2-containing ones. The TaC-based composites performed better than HfC composites at room temperature, showing values of mechanical strength up to 900 MPa and a fracture toughness of 4.7 MPa·m1/2. However, preliminary oxidation tests carried out in air at 1600 °C revealed that HfC-based composites have a superior high temperature stability compared to TaC-based materials.

Spark plasma sintering (SPS) of a codoped α-alumina powder has been investigated at temperatures between 850 and 1200 °C. The “grain size versus relative density” trajectory showed a significant grain growth as soon as the residual porosity closed. The densification mechanism was determined by anisothermal (investigation of the heating part of a SPS run) and isothermal methods. It was proposed that grain-boundary sliding, accommodated by oxygen grain-boundary diffusion, governed densification.