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Carbon nanotubes (CNTs) with macroscopically ordered structures (e.g., aligned or patterned mats, fibers, and sheets) and associated large surface areas have proven promising as new CNT electroactive polymer materials (CNT-EAPs) for the development of advanced chemical and biological sensors. The functionalization of CNTs with many biological species to gain specific surface characteristics and to facilitate electron transfer to and from them for chemical- and bio-sensing applications is an area of intense research activity.
Mechanical actuation generated by CNT-EAPs is another exciting electroactive function provided by these versatile materials. Controlled mechanical deformation for actuation has been demonstrated in CNT mats, fibers, sheets, and individual nanotubes. This article summarizes the current status and technological challenges for the development of electrochemical sensors and electromechanical actuators based on carbon nanotube electroactive materials.
Dimensional analysis is used to show that the maximum penetration depth and the tip radius affect the β correction factor appearing in the Sneddon relationship between unloading contact stiffness, contact area, and elastic modulus. A simple analytical model based on elasticity theory is derived that predicts the variation of β with penetration depth. This model shows that β increases at low penetration depth and decreases with the tip radius. The β(h) curve given by the model is compared with that calculated by finite element analysis for an elastic material and also with that deduced from experimental measurements performed on fused quartz with two Berkovich indenters: a sharp one and a blunted one. It is also demonstrated that the correction factor can be expressed as two multiplicative contributions, a contribution related to the mechanical properties of the material and a contribution related to the indenter geometry. Implications of these findings on nanoindentation test are also discussed.
Commercially procured single-walled carbon nanotubes were dispersed in 2 wt% solution of sodium cholate and also in 1 wt% solution of sodium dodecyl sulfate. The absorption spectrum of the suspensions was studied in ultraviolet–visible–near-infrared (UV–vis–NIR) range. Two distinct bands, each containing three peaks, were observed in NIR range for both the suspensions. These peaks correspond to transitions between van Hove singularities E11 and E22 in the density of states of the semiconducting nanotubes. Comparing positions of the observed peaks with the empirical Kataura plot, the diameters and chiralities of the nanotubes were estimated. Using tight binding approximations, the diameter of the nanotubes was also estimated theoretically. Discrepancies between the theoretically calculated diameters and those obtained by empirical Kataura plots are found to be higher for E11 peaks. It has been suggested that the reason for this discrepancy is that the observed E11 peaks are blue-shifted due to Coulomb interactions and exciton formation.
Highly porous Ti and TiZrV getter film coatings have been successfully grown on (100) silicon substrates using the glancing-angle direct-current magnetron sputtering method. The evolution of the microstructures of the Ti and the TiZrV films strongly depends on the sputtering flux rate, surface diffusion rate, nucleation rate, compositions, and self-shadowing geometry of the nuclei on the sputtering flux. The larger the glancing angle, the higher the porosity and specific surface area of the Ti and TiZrV films. The weight-gain results strongly depend on several factors, such as specific surface area, the surface structure of the getter film, the diffusion rate of O in the getter film, the reactivity of Ti, Zr, and V on O, and the order of the stabilities of Ti, Zr, and V oxides on the film’s surface. Porous Ti film absorbs oxygen better than porous TiZrV film does due to its higher surface area and the high diffusion rate of O in Ti films.
Compositions of xBiLaO3–(1 − x) PbTiO3 over the range 0 ≤ x ≤ 0.225 were calcined and sintered. The dielectric constant with temperature and differential scanning calorimetry measurements were in excellent agreement with respect to Curie-like tetragonal to cubic transformations starting at 495 °C for pure PbTiO3, shifting to lower temperatures with increasing x. For compositions of x ≥ 0.05, a second higher-temperature (∼600 °C) endotherm, and matching dielectric anomaly, were consistently observed, for which there were no structural changes indicated by hot-stage x-ray diffraction. This transformation was speculated to be based on a thermally induced desegregation of B-site cations.
The desorption–recombination behavior of a mechanically disproportionated, nanostructured Nd12Fe82B6 alloy was investigated by differential scanning calorimetry and thermogravimetric analysis. The microstructure change due to desorption–recombination treatments at various temperatures was characterized by x-ray diffraction, Mössbauer study, and transmission electron microscopy observation. The results show that the hydrogen desorption of the as-disproportionated alloy occurs in two stages: (i) the partial dehydriding of the Nd hydride from Nd2H5 to NdH2, as well as the desorption of the hydrogen absorbed/adsorbed at sites of crystal defects but not in the form of Nd hydride, at temperatures between 180 and 460 °C; and (ii) the complete dehydriding of the Nd hydride from NdH2 to Nd at temperatures between 630 and 780 °C. The recombination of α-Fe with Fe2B and Nd to form Nd2Fe14B occurs following the dehydriding of NdH2 to Nd, and it acts as the controlling step for the whole desorption–recombination process. The kinetics of both the desorption–recombination reaction and the growth of the newly formed Nd2Fe14B grains accelerate with increasing temperature. For a fixed annealing time of 30 min, the optimal processing temperature seems to be 760 °C, which gives rise to a fully recombined Nd2Fe14B–α-Fe nanocomposite microstructure with Nd2Fe14B and α-Fe phases of 25–30 nm in average size.
Glass-forming ability (GFA) in relation to microstructure evolution in the ternary Fe–Nb–B and Fe–Zr–B and quaternary Fe–(Nb,Zr)–B systems was systematically studied in a three-dimensional composition space. Through navigating, it was revealed that alloys with the optimum glass-forming ability (GFA) are coupled with composition regions surrounded by competing crystalline phases. Alloys Fe71Nb6B23, Fe77Zr4B19, and Fe71(Nb0.8Zr0.2)6B23 were illustrated to be the best glass formers in the ternary Fe–Nb–B and Fe–Zr–B systems and the quaternary Fe–(Nb,Zr)–B system, respectively, with a critical size for amorphous formation up to 2 mm. They were compared with the theoretical predictions on the basis of an efficient dense-packing model, and good agreements were obtained.
The kinetics and microstructure of solid-phase crystallization under continuous heating conditions and random distribution of nuclei are analyzed. An Arrhenius temperature dependence is assumed for both nucleation and growth rates. Under these circumstances, the system has a scaling law such that the behavior of the scaled system is independent of the heating rate. Hence, the kinetics and microstructure obtained at different heating rates differ only in time and length scaling factors. Concerning the kinetics, it is shown that the extended volume evolves with time according to αex = [exp(κCt′)]m+1, where t′ is the dimensionless time. This scaled solution not only represents a significant simplification of the system description, it also provides new tools for its analysis. For instance, it has been possible to find an analytical dependence of the final average grain size on kinetic parameters. Concerning the microstructure, the existence of a length scaling factor has allowed the grain-size distribution to be numerically calculated as a function of the kinetic parameters.
Tungsten (W) fiber reinforced Zr47Ti13Cu11Ni10Be16Nb3 bulk metallic glass composite has been prepared by melt infiltration casting. Interfacial characteristics of the composite were analyzed by sessile drop technique, x-ray diffraction (XRD), scanning electron microscopy (SEM), electron probe x-ray microanalysis (EPMA), and nanoindenter. Results indicate that Zr47Ti13Cu11Ni10Be16Nb3 melt wets the W substrate, and the interfacial bond composed of a diffusion–dissolution layer between Zr47Ti13Cu11Ni10Be16Nb3 matrix and W fiber is in good condition. Due to these excellent interfacial characteristics, the mechanical properties of the composite are considerably enhanced with increasing volume fraction of W fiber. It was found that the compressive strength of 70% volume fraction of W fiber composite is 2.6 GPa, which is 58% higher than the value exhibited by the unreinforced matrix. At the same time, the reinforced matrix exhibits 13% plastic deformation when tested under quasi-static compression conditions. Instead of shear mode seen for the unreinforced matrix, the failure mode of the 70% volume fraction W fiber composite is mainly caused by fiber splitting and buckling. Also, the W fiber hinders localized shear bands from propagating and gives rise to multiple shear bands, which results in the enhancement of the compressive strength and plastic deformation.
In situ scanning electron microscope observations have been performed on passivated damascene Cu interconnect segments of different widths during accelerated electromigration tests. In some cases, voids form and grow at the cathode. However, an alternative failure mode is also observed, during which voids form distant from the cathode end of the interconnect segment and drift toward the cathode, where they eventually lead to failure. The number of observations of this failure mode increased with increasing linewidth. During void motion, the shape and the velocity of the drifting voids varied significantly. Postmortem electron backscattered diffraction (EBSD) analysis was performed after in situ testing, and a correlation of EBSD data with the in situ observations reveals that locations at which voids form, their shape evolution, and their motion all strongly depend on the locations of grain boundaries and the crystallographic orientations of neighboring grains.
The influence of the cooling rate on the structure, microhardness, relaxation, and devitrification behavior of Cu44Ag15Zr36Ti5 glassy alloy on heating is studied in the present work. According to transmission electron microscopy investigations, the structures of Cu44Ag15Zr36Ti5 glassy ribbon and bulk samples are somewhat different. The structure of the ribbon samples is amorphous while, the nanoscale clusters of the crystalline phase (highly ordered regions) are formed in the bulk samples. It is reflected in the shift of the x-ray diffraction peak, in the magnitude of the heat of structure relaxation and crystallization, as well as in the change in the Vickers microhardness. An analysis of the cooling curve is also performed.
The formation of 10-nm ZnO nanopyramids using a simple synthetic route has been isolated from the reaction of Zn(OAc)2·2H2O in 1,4-butanediol followed by ripening at 90 °C. This was accomplished by establishing control over the Ostwald ripening process through the use of a carboxylic acid specific adsorbate. Using a variety of analytical methods, it is proposed that the carboxylate groups in the acetate precursor stabilize the {101} habit planes, creating septahedral shapes or nanopyramids. Particle assembly into crystallographically oriented dimers was observed with high specificity, and the association mechanism is suggested to relate to the crystal polarity and the variation in specific adsorption of the carboxylic acid to the surface facets. These materials are a candidate for biological labeling applications in living cells.
There is a wide array of technologically significant materials whose response to electric and magnetic fields can make or break their utility for specific applications. Often, these electrical and magnetic properties are determined by nanoscale features that can be most effectively understood through electron microscopy studies. Here, we present an overview of the capabilities for transmission electron microscopy for uncovering information about electric and magnetic properties of materials in the context of operational devices. When devices are operated during microscope observations, a wealth of information is available about dynamics, including metastable and transitional states. Additionally, because the imaging beam is electrically charged, it can directly capture information about the electric and magnetic fields in and around devices of interest. This is perhaps most relevant to the growing areas of nanomaterials and nanodevice research. Several specific examples are presented of materials systems that have been explored with these techniques. We also provide a view of the future directions for research.
Three different strategies, wet impregnation, in situ reduction, and grafting with silane coupling agents, have been used to introduce CoNi nanoparticles with different existing forms into mesoporous silica. These composites were used as catalysts to grow nanostructured carbons by catalytic chemical vapor deposition using ethene. Carbon nanotubes (CNTs) with different inner diameters can grow out of mesoporous silica particles incorporated with CoNi nanoclusters. Many fewer CNTs could be found in the pore channels of the sample prepared by using silane coupling agents than in those of the sample synthesized via wet impregnation. No CNTs formed in the pore channels of the sample prepared by in situ reduction. After the removal of silica, different carbon nanostructures have been obtained in the pore channels. Ordered graphite carbon mesostructure was obtained from the sample prepared by in situ reduction. Highly dispersed metal catalysts inside mesopore channels are favorable for the formation of graphite carbons with ordered mesostructures.
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.
High-energy synchrotron x-ray diffraction (XRD) has been used to quantify load transfer in bovine plexiform bone. By using both wide-angle and small-angle XRD, strains in the mineral as well as the collagen phase of bone were measured as a function of applied compressive stress. We suggest that a greater proportion of the load is borne by the more mineralized woven bone than the lamellar bone as the applied stress increases. With a further increase in stress, load is shed back to the lamellar regions until macroscopic failure occurs. The reported data fit well with reported mechanisms of microdamage accumulation in bovine plexiform bone.
We review the development of time-resolved, high-resolution environmental scanning/ transmission electron microscopy [E(S)TEM] for directly probing dynamic gas–solid, liquid–solid, and gas–liquid–solid interactions at the atomic level. Unlike a regular TEM, such a microscope allows us to use high gas pressures (up to 40 mbars) in the sample region. The unique information available from experiments performed using E(S)TEM has enabled visualization of the dynamic nature of nanostructures during reactions. Such information can be directly applied to the development of advanced nanomaterials such as carbon nanotubes, silicon nanowires and processes, including the design of novel routes to polymers synthesis, and has aided in the identification of important phenomena during catalysis, chemical vapor deposition, and electrochemical deposition.