We have studied the onset of plasticity in coherently-strained semiconductor superlattices, using nano-indentation with spherical indenter tips to observe the full stress-strain curve. The yield pressure is reduced by as much as a factor of two by the presence of the coherency strain. By varying the thicknesses and strains of the superlattice layers, we provide a proof that yield commences over a finite volume. It is properties averaged or summed over this volume which determine the yield pressure. We show that the relevant yield criterion for our experimental data is the rate of change of elastic strain energy with plastic relaxation, integrated over a volume of the order of a micron across. This result is expected to be valid for other systems with highly inhomogenous strain fields, and hence to be applicable to modelling of point contact, and to the design and understanding of structural materials which have coherently-strained microstructure.

Nanostructured WC-Co powders obtained by mechanical milling were investigated by combination of X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) techniques. HRTEM image analysis shows that in the as-milled nanostructured powder, many WC grains contain stacking faults lying on the plane{10.0}. Analysis of phase images showed that these defects were nearly periodically ordered along the [10.0] direction. Based on these observations, a structural model is proposed for the WC grains with ordered stacking faults, which is in fact equivalent to a superstructure of WC with space group Amm2. When this model is introduced together with the normal WC structure (space group P6m2) into the Rietveld refinement, a much better agreement between the calculated and experimental XRD profiles is obtained. This study allowed obtaining the lattice parameters, grain size, microstrain and other structural information on the as-milled powders.

In this review, some general conclusions based on studies performed to date on fatigued materials of ultrafine grain (UFG) size produced by equal channel angular pressing (ECAP) are drawn, and open issues of current interest are defined. Important aspects addressed include the apparent discrepancy between improved fatigue strengths in Wöhler (S-N) plots as opposed to inferior fatigue strengths in Manson-Coffin plots, the clarification of the microstructural mechanisms of severe cyclic softening in conjunction with dynamic (local) grain/subgrain coarsening and damaging large-scale catastrophic shear banding. The important roles of the cyclic slip mode, the friction stress, the crystal structure and the temperature of cyclic deformation with respect to stable cyclic deformation behaviour are emphasized. Based on such considerations, criteria are formulated that must be observed, when designing ECAP-processed UFG-materials of superior fatigue strength.

An NTP ensemble molecular dynamics simulation was carried out to investigate the mechanism of nano-sized crystallization during plastic deformation in an amorphous metal. The atomic system used in this study was Ni single component. The total number of Ni atoms was 1372. The Morse type inter-atomic potential was employed. An amorphous model was prepared by a quenching process from the liquid state. Pure shear stresses were applied to the amorphous model at a temperature of 50 K. At applied stresses of less than 2.4GPa, a linear relation between shear stress and shear strain was observed. However, at an applied shear stress of 2.8 GPa, the amorphous model started to deform significantly until shear strain reached to 0.78. During this deformation process, phase transformation from amorphous into crystalline structure (fcc) was observed. Furthermore, an orientation relationship between shear directions and crystalline phase was obtained, that is, two shear directions are parallel to a (111) of the fcc structure. This crystallographic orientation relationship agreed well with our experimental result of Ni-P amorphous alloy. Mechanisms of phase transformation from amorphous into crystalline structure were discussed.

The properties of elemental and bimetallic free, supported and assembled nanoclusters are modeled at the atomic scale and the models are discussed on the basis of experimental observations. This way, the memory of some free cluster properties in nanostructured materials may be evaluated.

The combination of molecular statics with High Resolution Transmission Electron Microscopy (HRTEM) allows to predict fine detail of the lattice relaxation of a truncated octahedral gold cluster deposited on MgO. Metropolis Monte Carlo (MC) predicts that a lattice mismatch may contribute to disordering in deposited Cu3Au nanoclusters. In both Cu-Au and Ni-Al free clusters, offset of equilibrium stoichiometry may result in segregation of Au or Al at the cluster surface. An ordered stoichiometric core is surrounded by a disordered mantle where the excess species resides. Different modeling methods predict different nanometer scale textures.

Therefore, cluster assembled Ni3Al alloys formed by condensation and pressing are modeled in two different ways. Both make use of a combination of Molecular Dynamics and MC. Whatever the model nanostructure, the segregation properties of free clusters remain in the nanostructured material. This segregation is one possible cause that can inhibit the formation of a metastable martensitic phase as observed in bulk Ni-Al alloys.

The occurrence of vacancy clusters and voids is hardly identified by HRTEM. On the other hand, their distribution and sizes are sensitive to the nanostructure modeling. Therefore, a new characterization method is developed, which combines positron lifetime spectroscopy with the calculation of positron lifetimes from selected areas of the model samples.

Mechanisms responsible for the formation of a misfit dislocation in a lattice-mismatched system have been studied using Molecular Dynamics simulations of a two-dimensional Lennard-Jones system. Results show clearly how the strain due to the lattice-mismatched interface acts as a driving force for migration of dislocations in the substrate and the overlayer and nucleation of dislocations in the overlayer edges. Moreover, we observe dislocation reactions in which the gliding planes of dislocations change such that they can migrate to the interface.

Molecular dynamics simulation for the morphology and the defect structure in nanoparticles has been performed. The nanoparticles are consisted of 1300 – 5000 atoms and the EAM potential developed by the present authors is adopted to calculate the interactions between atoms. The atom consisting the surfaces or defects are selected thorough the potential energy of individual atoms and structure is investigated by calculating the local crystalline order. A relation between the cooling rate and the particle morphology is also investigated.

Different structural configurations of nanoparticles have been investigated by advanced transmission electron microscopy (TEM) techniques. The cluster-surface interaction of Au clusters, produced in a laser vaporization source and deposited with low energy on MgO cubes, is investigated by high-resolution transmission electron microscopy (HRTEM). A dilation of the Au lattice that perfectly accommodates the misfit with the MgO lattice is measured and modeled with Molecular Dynamics (MD). To study the chemical ordering in bimetallic clusters, Au-Cu alloy clusters with different stoichiometries are produced and deposited in the same way as the Au clusters. Electron diffraction (ED) ring patterns obtained from these alloy clusters lying on amorphous carbon, are indexed as face-centered cubic, which is confirmed by HRTEM. This indicates that clusters of Au-Cu alloys are solid solutions, i.e. no ordering takes place in these clusters. Assembled nanoclusters of Ni3Al, produced by the inert gas condensation (IGC) technique and pressed under high pressure (2 GPa), are investigated by HRTEM. These studies indicate that nanocrystalline Ni3Al consists of small crystallites of random crystallographic orientations separated by grain boundaries, with the presence of several nanoscaled voids. From the selected area electron diffraction (SAED) ring pattern, an incomplete L12 ordering is concluded.

The theoretical calculations of the position response to different types of defects can be very helpful in order to interpret properly positron measurements. In this contribution a new computational technique to determine position properties in nanocrystalline materials is presented. In such calculations we employ the realistic models of n-materials obtained using molecular dynamics. The new technique is based on the so-called atomic superposition method where atomic densities are superimposed in a selected region of the model (virtual) sample to approxiamte the electron density of the system. We study the virtual samples of n-Cu, n-NiAl, and n-Ni3Al, for which we calculate position lifetime and position binding energies corresponding to defects located in selected regions of the samples. The regions of interest for position calculations comprise grain boundaries inculding triple points, nano-voids, and bulk-like regions.

Mechanical properties of nanocrystalline Ni made by Inert Gas Condensation and Electrodeposition are presented in relation to their microstructure. Significant plasticity is only observed at elevated temperatures for both types of nanocrystalline Ni. However, a higher temperature is needed in the Inert gas condensated material. Careful analysis of the microstructure by means of X-ray diffraction and conventional electron microscopy reveal initial differences in as-prepared samples. The change in microstructure during deformation at elevated temperatures and during heat treatment without external load is investigated and information about the deformation mechanisms is reported.

New high temperature ceramic eutectic composites have been obtained. The composite is self-assembled in one quick step by rapid supercooling of the multioxide alumina-YAG-zirconia eutectic in an arc-image lamp furnace. The new material will find applications as in-situ coating and component for use at ultra-high temperature. Periodic self-assembled layered structures kinetically forced to solidify with interspacing in the submicron range will result in very interesting properties and applications for high temperature multioxide oxide eutectic composites, offering the challenge of design of layered nanostructures tailored to specific applications by kinetic control during solidification.

We have developed a novel processing technique to fabricate “artifact free” tungsten carbide (WC) nanocomposites. In this method, pulsed laser deposition of WC in conjunction with a few monolayers of nickel aluminide (NiAl) is used to control the grain size of nanocrystalline composites. The grain size of WC was controlled by the thickness of tungsten carbide and the substrate temperature. The role of NiAl is to ensure the nucleation of tungsten carbide islands, and it is also insoluble in WC. Using this approach, we have fabricated nanocomposites of grain sizes ranging from 6 nm to 35 nm. The hardness of the composite increases with the decrease in grain size, following approximately Hall-Petch relationship. The role of NiAl in grain boundary deformation is of particular interest in strengthening the nanocrystalline composites. The potential of this technique to go to even lower grain sizes is discussed.

A new fatigue strengthening method which is applicable for both the micro-sized materials and ordinary-sized materials have been proposed. Dislocations are pinned at their intersections by the formation of nano-crystals after cold work in this strengthening method.

Nano-sized α'-martensite particles, the diameter of which was approximately 5 nm, were formed by a cryogenic treatment at a certain temperature above (martensite burst starting temperature) in a commercially available 316-type austenitic stainless steel. These nano-particles are considered to be formed at intersections of dislocations. Fatigue life tests using ordinary-sized specimens revealed that high cycle fatigue life of the 316-type austenitic stainless steel was extended by the cryogenic treatment and this is considered to be due to the pinning of dislocations by the formation of nano-sized α'-martensite particles.

Variable-charge molecular dynamics simulation of 32 TiO2-nanoparticles with diameter 60Å is performed for 40 ps at 1 GPa and 1,400 K for both rutile and anatase phases, to investigate their phase-dependent sintering mechanisms. In the rutile case, the nanoparticles rotate around their centers during the first 20 ps. Varying degrees of neck formation between neighboring rutile-nanoparticles are found at ∼ 40 ps. In the anatase case, the nanoparticles maintain their original orientations. Similar degrees of neck formation are observed at contacting regions of the anatase nanoparticles.

The advent of nanocrystalline materials has provided new opportunities to explore grain size dependent phenomenon. Superplasticity is such a grain size dependent phenomenon defined by the ability to attain tensile elongation of 200% or more. Superplasticity in microcrystalline materials has been well characterized. The constitutive equations that describe microcrystalline superplasticity predict enhanced properties for nanocrystalline materials. Enhanced properties in such nanocrystalline material include lower superplastic temperature at constant strain rate, higher superplastic strain rate at constant temperature, and lower flow stresses. Investigations with nanocrystalline Ni3Al and ultra-fine grained Ti-6Al-4V alloy have shown a reduction in the superplastic temperature. However, the flow stresses in these materials are significantly higher than expected. The high flow stresses are accompanied by strong strain hardening.

Transmission electron microscopy in situ straining of nanocrystalline Ni3Al has shown that grain boundary sliding and grain rotation occurred during straining. The sliding and rotation decreased with strain. Dislocation activity was observed but was not extensive. There was no observable dislocation storage. The parameters of the generalized constitutive equation for superplasticity for nanocrystalline Ni3Al and Ti-6Al-4V are in reasonable agreement with the parameters for microcrystalline material. The rate parameters suggest that nanocrystalline superplasticity shares common features with microcrystalline superplasticity. In contrast, the observed flow stresses and strong strain hardening indicate that nanocrystalline superplasticity is not a simple extension of microcrystalline behavior scaled to finer grain size.

Using the dislocation model of strain anisotropy in X-ray diffraction peak profile analysis it is shown that in nanocrystalline copper produced by inert gas condensation dislocations are present, at least, down to average grain sizes of the order of 20 nm. Based on the analysis of the dislocation contrast factors it is suggested that with decreasing grain size the proportion of Lomer-Cottrell type dislocations increases.

The microstructure and tensile properties were investigated for pulse-plated nanocrystalline nickel electrodeposits prepared from an additive-free sulfamate-based solution. Square-wave cathodic current densities were varied from 25 to 75 mA/cm2. The samples deposited at 25 mA/cm2 showed the smallest grain size (d ∼ 12 nm), and the grain size was found to increase with increasing current densities. The grain size of the electrodeposits ranged from approximately 27 to 12 nm. Tensile results indicated that the yield strength of the specimens increased with decreasing grain size. Scanning electron microscopy revealed that all electrodeposits fractured through a ductile mechanism.

Coatings of Be1−xCux are prepared by magnetron sputter deposition onto spherical polymer mandrels. The application of an applied bias during deposition refines the columnar morphology of the coating and surface finish to the nanoscale. A mechanical testing technique is developed to load the thin-walled spherical capsules under uniaxial tension at constant strain to fracture. The bias-deposited material exhibits an increase in strength by a factor of three or more following a Hall-Petch type relationship with surface roughness.

Nanocrystalline samples of copper were prepared using inert gas condensation and an optimized sequence of powder outgassing and compaction. TEM specimens were cut, electropolished, and mounted in a straining stage. In situ TEM observations including real-time video were captured during straining in the microscope. Areas of presumed increased stress concentration were identified near small cracks around the perimeter of the electropolished hole. Such locations were observed in the TEM while the specimen was pulled in tension. Several microstructural changes were captured during deformation including numerous sudden shifts in contrast of grains and parts of grains, occasional dislocation motion, opening and propagation of the crack. Relationships between grain size and deformation are described.

Nanocrystalline metallic powders and coatings have been synthesized using a millimeter wave driven polyol process. We have been able to prepare powders of single elements, alloys, metastable alloys, composites and coatings. Examples of a few of the metals processed in this study include Fe, Co, Ni, Cu, Ru, Rh, Pt, Au, FePt, FexCo100−x, NiAg and Cu-Ni. The polyol experiment was set up in the millimeter wave processing chamber, the beam was directed into the center of the solution and it was brought to reflux, using the millimeter wave beam as a heat source. Varying the power input easily controlled the rate of reflux.