Discrete dislocation plasticity analysis of crack-tip fields in polycrystalline materials

Small scale yielding around a mode I crack is analysed using polycrystalline discrete dislocation plasticity. Plane strain analyses are carried out with the dislocations all of edge character and modelled as line singularities in a linear elastic material. The lattice resistance to dislocation motion, nucleation, interaction with obstacles and annihilation are incorporated through a set of constitutive rules. Grain boundaries are modelled as impenetrable to dislocations. The polycrystalline material is taken to consist of two types of square grains, one of which has a bcc-like orientation and the other an fcc-like orientation. For both orientations there are three active slip systems. Alternating rows, alternating columns and a checker-board-like arrangement of the grains is used to construct the polycrystalline materials. Consistent with the increasing yield strength of the polycrystalline material with decreasing grain size, the calculations predict a decrease in both the plastic zone size and the crack-tip opening displacement for a given applied mode I stress intensity factor. Furthermore, slip-band and kink-band formation is inhibited by all grain arrangements and, with decreasing grain size, the stress and strain distributions more closely resemble the HRR fields with the crack-tip opening approximately inversely proportional to the yield strength of the polycrystalline materials. The calculations predict a reduction in fracture toughness with decreasing grain size associated with the grain boundaries acting as effective barriers to dislocation motion.

The parameter space of graphene chemical vapor deposition on polycrystalline Cu

A systematic study of the parameter space of graphene chemical vapor deposition (CVD) on polycrystalline Cu foils is presented, aiming at a more fundamental process rationale in particular regarding the choice of carbon precursor and mitigation of Cu sublimation. CH 4 as precursor requires H 2 dilution and temperatures ≥1000 °C to keep the Cu surface reduced and yield a high-quality, complete monolayer graphene coverage. The H 2 atmosphere etches as-grown graphene; hence, maintaining a balanced CH 4/H 2 ratio is critical. Such balance is more easily achieved at low-pressure conditions, at which however Cu sublimation reaches deleterious levels. In contrast, C 6H 6 as precursor requires no reactive diluent and consistently gives similar graphene quality at 100-150 °C lower temperatures. The lower process temperature and more robust processing conditions allow the problem of Cu sublimation to be effectively addressed. Graphene formation is not inherently self-limited to a monolayer for any of the precursors. Rather, the higher the supplied carbon chemical potential, the higher the likelihood of film inhomogeneity and primary and secondary multilayer graphene nucleation. For the latter, domain boundaries of the inherently polycrystalline CVD graphene offer pathways for a continued carbon supply to the catalyst. Graphene formation is significantly affected by the Cu crystallography; i.e., the evolution of microstructure and texture of the catalyst template form an integral part of the CVD process. © 2012 American Chemical Society.

Nucleation, growth, and control of ferroelectric-ferroelastic domains in thin polycrystalline films

The unique response of ferroic materials to external excitations facilitates them for diverse technologies, such as nonvolatile memory devices. The primary driving force behind this response is encoded in domain switching. In bulk ferroics, domains switch in a two-step process: nucleation and growth. For ferroelectrics, this can be explained by the Kolmogorov-Avrami-Ishibashi (KAI) model. Nevertheless, it is unclear whether domains remain correlated in finite geometries, as required by the KAI model. Moreover, although ferroelastic domains exist in many ferroelectrics, experimental limitations have hindered the study of their switching mechanisms. This uncertainty limits our understanding of domain switching and controllability, preventing thin-film and polycrystalline ferroelectrics from reaching their full technological potential. Here we used piezoresponse force microscopy to study the switching mechanisms of ferroelectric-ferroelastic domains in thin polycrystalline Pb 0.7Zr0.3TiO3 films at the nanometer scale. We have found that switched biferroic domains can nucleate at multiple sites with a coherence length that may span several grains, and that nucleators merge to form mesoscale domains, in a manner consistent with that expected from the KAI model. © 2012 American Physical Society.

Magnetocaloric effect in nano- and polycrystalline manganite $La_{0.7}Ca_{0.3}MnO_3$

$La_{0.7}Ca_{0.3}MnO_3$ samples were prepared in nano- and polycrystalline forms by sol-gel and solid state reaction methods, respectively, and structurally characterized by synchrotron X-ray diffraction. The magnetic properties determined by ac susceptibility and dc magnetization measurements are discussed. The magnetocaloric effect in this nanocrystalline manganite is spread over a broader temperature interval than in the polycrystalline case. The relative cooling power of the poly- and nanocrystalline manganites is used to evaluate a possible application for magnetic cooling below room temperature.

Magnetocaloric effect in nano- and polycrystalline manganite La 0.7Ca0.3MnO3

La0.7Ca0.3MnO3 samples were prepared in nano- and polycrystalline forms by the sol-gel and solid state reaction methods, respectively, and structurally characterized by synchrotron X-ray diffraction. The magnetic properties determined by ac susceptibility and dc magnetization measurements are discussed. The magnetocaloric effect in this nanocrystalline manganite is spread over a broader temperature interval than in the polycrystalline case. The relative cooling power of the poly- and nanocrystalline manganites is used to evaluate a possible application for magnetic cooling below room temperature. © 2007 Springer-Verlag.

Fabrication, densification, and replica molding of 3D carbon nanotube microstructures

The introduction of new materials and processes to microfabrication has, in large part, enabled many important advances in microsystems, labon- a-chip devices, and their applications. In particular, capabilities for cost-effective fabrication of polymer microstructures were transformed by the advent of soft lithography and other micromolding techniques 1,2, and this led a revolution in applications of microfabrication to biomedical engineering and biology. Nevertheless, it remains challenging to fabricate microstructures with well-defined nanoscale surface textures, and to fabricate arbitrary 3D shapes at the micro-scale. Robustness of master molds and maintenance of shape integrity is especially important to achieve high fidelity replication of complex structures and preserving their nanoscale surface texture. The combination of hierarchical textures, and heterogeneous shapes, is a profound challenge to existing microfabrication methods that largely rely upon top-down etching using fixed mask templates. On the other hand, the bottom-up synthesis of nanostructures such as nanotubes and nanowires can offer new capabilities to microfabrication, in particular by taking advantage of the collective self-organization of nanostructures, and local control of their growth behavior with respect to microfabricated patterns. Our goal is to introduce vertically aligned carbon nanotubes (CNTs), which we refer to as CNT "forests", as a new microfabrication material. We present details of a suite of related methods recently developed by our group: fabrication of CNT forest microstructures by thermal CVD from lithographically patterned catalyst thin films; self-directed elastocapillary densification of CNT microstructures; and replica molding of polymer microstructures using CNT composite master molds. In particular, our work shows that self-directed capillary densification ("capillary forming"), which is performed by condensation of a solvent onto the substrate with CNT microstructures, significantly increases the packing density of CNTs. This process enables directed transformation of vertical CNT microstructures into straight, inclined, and twisted shapes, which have robust mechanical properties exceeding those of typical microfabrication polymers. This in turn enables formation of nanocomposite CNT master molds by capillary-driven infiltration of polymers. The replica structures exhibit the anisotropic nanoscale texture of the aligned CNTs, and can have walls with sub-micron thickness and aspect ratios exceeding 50:1. Integration of CNT microstructures in fabrication offers further opportunity to exploit the electrical and thermal properties of CNTs, and diverse capabilities for chemical and biochemical functionalization 3. © 2012 Journal of Visualized Experiments.

Corrugated carbon nanotube microstructures with geometrically tunable compliance

Deterministic organization of nanostructures into microscale geometries is essential for the development of materials with novel mechanical, optical, and surface properties. We demonstrate scalable fabrication of 3D corrugated carbon nanotube (CNT) microstructures, via an iterative sequence of vertically aligned CNT growth and capillary self-assembly. Vertical microbellows and tilted microcantilevers are created over large areas, and these structures can have thin walls with aspect ratios exceeding 100:1. We show these structures can be used as out-of-plane microsprings with compliance determined by the wall thickness and number of folds. © 2011 American Chemical Society.

Programmable transformation of vertically aligned carbon nanotubes into 3D microstructures

Capillary forming of carbon nanotubes (CNTs) enables the fabrication of unique 3D microstructures over large areas. In this paper we focus on the simulation as well as on the integration of these structures in MEMS devices. We developed finite element models (FEM) that enables qualitative prediction of shape transformations caused by capillary forming; and show how capillary formed CNT structured can be integrated with conventional lithographic processing for patterning of polymers and metals in concert with CNTs. © 2011 IEEE.

Fabrication of high-aspect-ratio polymer microstructures and hierarchical textures using carbon nanotube composite master molds

Scalable and cost effective patterning of polymer structures and their surface textures is essential to engineer material properties such as liquid wetting and dry adhesion, and to design artificial biological interfaces. Further, fabrication of high-aspect-ratio microstructures often requires controlled deep-etching methods or high-intensity exposure. We demonstrate that carbon nanotube (CNT) composites can be used as master molds for fabrication of high-aspect-ratio polymer microstructures having anisotropic nanoscale textures. The master molds are made by growth of vertically aligned CNT patterns, capillary densification of the CNTs using organic solvents, and capillary-driven infiltration of the CNT structures with SU-8. The composite master structures are then replicated in SU-8 using standard PDMS transfer molding methods. By this process, we fabricated a library of replicas including vertical micro-pillars, honeycomb lattices with sub-micron wall thickness and aspect ratios exceeding 50:1, and microwells with sloped sidewalls. This process enables batch manufacturing of polymer features that capture complex nanoscale shapes and textures, while requiring only optical lithography and conventional thermal processing. © 2011 The Royal Society of Chemistry.

Fishtail effects and improved critical current density in polycrystalline bulk MgB2 containing carbon nanotubes

Bulk, polycrystalline MgB2 samples containing 2.5 wt.% multi-walled carbon nanotubes (CNTs) have been prepared by conventional solid state reaction at 800 °C. The effect of Mg precursor powders composed of two different particle sizes on the critical current density (Jc) of the as-sintered samples has been investigated. An enhancement of Jc at high field has been observed in MgB2 samples containing CNTs prepared with fine Mg powders, whereas the values of Jc in the sample prepared using the coarser Mg powders was slightly decreased. These results contrast significantly with measurements on pure, undoped, MgB2 samples prepared from the same Mg precursor powders. They suggest that carbon substitution into the MgB2 lattice, which accounts for increased flux pinning, and therefore Jc, is more effective in precursor Mg powders with a larger surface area. Rather surprisingly, the so-called fishtail effect, observed typically in MgB2 single crystals and in the (RE)BCO family of high temperature superconductors (HTSs), was observed in both sets of CNT-containing polycrystalline samples as a result of lattice defects associated with C substitution. Significantly, analytical fits to the data for each sample suggest that the same flux pinning mechanism accounts for the fishtail effect in polycrystalline MgB2 and (RE)BCO. © 2013 Elsevier B.V. All rights reserved.

Observing graphene grow: catalyst-graphene interactions during scalable graphene growth on polycrystalline copper.

Complementary in situ X-ray photoelectron spectroscopy (XPS), X-ray diffractometry, and environmental scanning electron microscopy are used to fingerprint the entire graphene chemical vapor deposition process on technologically important polycrystalline Cu catalysts to address the current lack of understanding of the underlying fundamental growth mechanisms and catalyst interactions. Graphene forms directly on metallic Cu during the high-temperature hydrocarbon exposure, whereby an upshift in the binding energies of the corresponding C1s XPS core level signatures is indicative of coupling between the Cu catalyst and the growing graphene. Minor carbon uptake into Cu can under certain conditions manifest itself as carbon precipitation upon cooling. Postgrowth, ambient air exposure even at room temperature decouples the graphene from Cu by (reversible) oxygen intercalation. The importance of these dynamic interactions is discussed for graphene growth, processing, and device integration.

A microstructural investigation of deformation in fine SiC particulate- and whisker-reinforced aluminium-matrix composites

Aluminium-based composites, reinforced with low volume fractions of whiskers and small particles, have been formed by a powder route. The materials have been tested in tension, and the microstructures examined using transmission electron microscopy. The whisker composites showed an improvement in flow stress over the particulate composites, and this was linked to an initially enhanced work-hardening rate in the whisker composites. The overall dislocation densities were estimated to be somewhat higher in the whisker composites than the particulate composites, but in the early stages of deformation the distribution was rather different, with deformation in the whisker material being far more localized and inhomogeneous. This factor, together with differences in the internal stress distribution in the materials, is used to explain the difference in mechanical properties.

Fine scale structures from deformation of aluminium containing small alumina particles

Microstructures and mechanical properties have been studied in aluminium containing a fine dispersion of alumina particles, deformed by cold-rolling to strains between 1.4 and 3.5. The microstructure was characterised by TEM. The deformation structures evolved very rapidly, forming a nanostructured material, with fine subgrains about 0.2 μm in diameter and a fraction of high-angle boundaries which was already high at a strain of 1.4, but continued to increase with rolling strain. The yield stress and ductility of the rolled materials were measured in tension, and properties were similar for all materials. Yield stress measurements were correlated with estimates made using microstructural models. The role of small particles in forming and stabilising the deformation structure is discussed. This nanostructured cold-deformed alloy has mechanical properties which are usefully enhanced at comparatively low cost. This gives it, and similar particle-strengthened alloys, good potential for commercial exploitation. © 2002 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.