Further evidence for room temperature, indentation-induced nanocrystallization in a bulk metallic glass

Room temperature nanoindentation experiments, employing two different pyramidal (Berkovich and cube-corner) indenters, were performed on a Zr-based bulk metallic glass (BMG) to critically examine the possibility of indentation-induced nanocrystallization in BMGs. Cross-sectional transmission electron microscopy images obtained from high angle annular dark field ( HAADF) and high resolution (HR) modes clearly indicate to the occurrence of nanocrystallization. Pronounced nanocrystallite formation in the case of sharper cube-corner indenter suggests that the structural transformation is favored by the high strains introduced during nanoindentation. (c) 2012 Elsevier B.V. All rights reserved.

A study on the formation of crystalline phases during solidification and crystallisation in the bulk metallic glass of Zr53Cu21Al10Ni8Ti8 composition

The present paper considers the formation of crystalline phases during solidification and crystallisation of the Zr53Cu21Al10Ni8Ti8 alloy. Solidification was carried out by a copper mould casting technique, which yielded a partially crystalline microstructure comprising a `big cube phase' in a dendritic morphology and a bct Zr2Ni phase. Detailed high-resolution microscopy was carried out to determine possible mechanisms for the formation of the crystalline phases. Based on microstructural examinations, it was established that the dendrites grew by the attachment of atomistic ledges. The bct Zr2Ni phase, formed during solidification and crystallisation, showed various types of faults depending on the crystallite size, and its crystallography was examined in detail. It has been shown that the presence of these faults could be explained by anti-site occupancy in the bct lattice of the Zr2Ni phase.

On the microstructure-tensile property correlations in bulk metallic glass matrix composites with crystalline dendrites

Bulk metallic glass (BMG) matrix composites with crystalline dendrites as reinforcements exhibit a wide variance in their microstructures (and thus mechanical properties), which in turn can be attributed to the processing route employed, which affects the size and distribution of the dendrites. A critical investigation on the microstructure and tensile properties of Zr/Ti-based BMG composites of the same composition, but produced by different routes, was conducted so as to identify ``structure-property'' connections in these materials. This was accomplished by employing four different processing methods-arc melting, suction casting, semi-solid forging and induction melting on a water-cooled copper boat-on composites with two different dendrite volume fractions, V-d. The change in processing parameters only affects microstructural length scales such as the interdendritic spacing, lambda, and dendrite size, delta, whereas compositions of the matrix and dendrite are unaffected. Broadly, the composite's properties are insensitive to the microstructural length scales when V-d is high (similar to 75%), whereas they become process dependent for relatively lower V-d (similar to 55%). Larger delta in arc-melted and forged specimens result in higher ductility (7-9%) and lower hardening rates, whereas smaller dendrites increase the hardening rate. A bimodal distribution of dendrites offers excellent ductility at a marginal cost of yield strength. Finer lambda result in marked improvements in both ductility and yield strength, due to the confinement of shear band nucleation sites in smaller volumes of the glassy phase. Forging in the semi-solid state imparts such a microstructure. (c) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Indentation size effect and shear transformation zone size in a bulk metallic glass in two different structural states

The existence of an indentation size effect (ISE) in the onset of yield in a Zr-based bulk metallic glass (BMG) is investigated by employing spherical-tip nanoindentation experiments. Statistically significant data on the load at which the first pop-in in the displacement occurs were obtained for three different tip radii and in two different structural states (as-cast and structurally relaxed) of the BMG. Hertzian contact mechanics were employed to convert the pop-in loads to the maximum shear stress underneath the indenter. Results establish the existence of an ISE in the BMG of both structural states, with shear yield stress increasing with decreasing tip radius. Structural relaxation was found to increase the yield stress and decrease the variability in the data, indicating ``structural homogenization'' with annealing. Statistical analysis of the data was employed to estimate the shear transformation zone (STZ) size. Results of this analysis indicate an STZ size of similar to 25 atoms, which increases to similar to 34 atoms upon annealing. These observations are discussed in terms of internal structure changes that occur during structural relaxation and their interaction with the stressed volumes in spherical indentation of a metallic glass. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

On the mechanism and the length scales involved in the ductile fracture of a bulk metallic glass

Some bulk metallic glasses (BMGs) exhibit high crack initiation toughness due to shear band mediated plastic flow at the crack tip and yet do not display additional resistance to crack growth due to the lack of a microstructure. Thus, at crack initiation, the fracture behavior of BMGs transits from that of ductile alloys to that of brittle ceramics. In this paper, we attempt to understand the physics behind the characteristic length from the notch root at which this transition occurs, through testing of four-point bend specimens made of a nominally ductile Zr-based BMG in three different structural states. In the as-cast state, both symmetric (mode I) and asymmetric (mixed mode) bend specimens are tested. The process of shear band mediated plastic flow followed by crack initiation at the notch root was monitored through in situ imaging. Results show that stable crack growth occurs inside a dominant shear band through a distance of, similar to 60 mu m, irrespective of the structural state and mode mixity, before attaining criticality. Detailed finite element simulations show that this length corresponds to the distance from the notch root over which a positive hydrostatic stress gradient prevails. The mean ridge heights on fractured surfaces are found to correlate with the toughness of the BMG. The Argon and Salama model, which is based on the meniscus instability phenomenon at the notch root, is modified to explain the experimentally observed physics of fracture in ductile BMGs. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Wallner lines, crack velocity and mechanisms of crack nucleation and growth in a brittle bulk metallic glass

Mode I fracture experiments were conducted on brittle bulk metallic glass (BMG) samples and the fracture surface features were analyzed in detail to understand the underlying physical processes. Wollner lines, which result from the interaction between the propagating crack front and shear waves emanating from a secondary source, were observed on the fracture surface and geometric analysis of them indicates that the maximum crack velocity is similar to 800 m s(-1), which corresponds to similar to 0.32 times the shear wave speed. Fractography reveals that the sharp crack nucleation at the notch tip occurs at the mid-section of the specimens with the observation of flat and half-penny-shaped cracks. On this basis, we conclude that the crack initiation in brittle BMGs is stress-controlled and occurs through hydrostatic stress-assisted cavity nucleation ahead of the notch tip. High magnification scanning electron and atomic force microscopies of the dynamic crack growth regions reveal highly organized, nanoscale periodic patterns with a spacing of similar to 79 nm. Juxtaposition of the crack velocity with this spacing suggests that the crack takes similar to 10(-10) s for peak-to-peak propagation. This, and the estimated adiabatic temperature rise ahead of the propagating crack tip that suggests local softening, is utilized to critically discuss possible causes for the nanocorrugation formation. Taylor's fluid meniscus instability is unequivocally ruled out. Then, two other possible mechanisms, viz. (a) crack tip blunting and resharpening through nanovoid nucleation and growth ahead of the crack tip and eventual coalescence, and (b) dynamic oscillation of the crack in a thin slab of softened zone ahead of the crack-tip, are critically discussed. (C) 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Structural Evolution and Property Changes in Nd_{60}Al_{10}Fe_{20}Co_{10} Bulk Metallic Glass During Crystallization

The structural evolution and property changes in Nd60Al10Fe20Co10 bulk metallic glass (BMG) upon crystallization are investigated by the ultrasonic method, x-ray diffraction, density measurement, and differential scanning calorimetry. The elastic constants and Debye temperature of the BMG are obtained as a function of annealing temperature. Anomalous changes in ultrasonic velocities, elastic constants, and density are observed between 600–750 K, corresponding to the formation of metastable phases as an intermediate product in the crystallization process. The changes in acoustic velocities, elastic constants, density, and Debye temperature of the BMG relative to its fully crystallized state are much smaller, compared with those of other known BMGs, the differences being attributed to the microstructural feature of the BMG.

Anomalous Thermal Stability of Nd-Fe-Co-Al Bulk Metallic Glass

The thermal stability of Nd60Fe20Co10Al10 bulk metallic glass (BMG) has been studied by differential scanning calorimetry (DSC), dynamic mechanical thermal analysis (DMTA), isochronal dilatation and compression tests. The results show that the glass transition of the BMG takes place quite gradually between about 460 and 650 K at a heating rate of 0.17 K/s. Several transformation processes are observed during continuous heating with the first crystallization process beginning at about 460 K, while massive crystallization takes place near the solidus temperature of the alloy. The positive heat of mixing between the two major constituents, Nd and Fe, and, consequently, a highly inhomogeneous composition of the attained amorphous phase are responsible for the anomalous thermal stability in this system. (C) 2002 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.

Enhanced Plasticity of Zr-Based Bulk Metallic Glass Matrix Composite with Ductile Reinforcement

A composite material containing uniformly distributed micrometer-sized Nb particles in a Zr-based amorphous matrix was prepared by suction cast. The resulting material exhibits high fractured strength over 1550 MPa and enhanced plastic strain of about 29.7% before failure in uniaxial compression test at room temperature. Studies of the serrations on the stress-strain curves and the shear bands on the fractured samples reveal that the amplitude of the stress drop of each serration step corresponds to the extent of the propagation of a single shear band through the materials. The composite exhibits more serration steps and smaller amplitude of stress drop due to the pinning of shear band propagation by ductile Nb particles.

Formation, Thermal Stability and Deformation Behavior of Graphite-Flakes Reinforced Cu-based Bulk Metallic Glass Matrix Composites

Graphite-flake reinforced Cu47Ti34Zr11 Ni-8 bulk metallic glass matrix composite was fabricated by water-cooled copper mould cast. Most of the graphite flakes still keep unreacted and distribute uniformly in the amorphous matrix except that some reactive wetting occurs by the formation of TiC particles around the flakes. It reveals that the presence of graphite flakes does not affect the onset of the glass transition temperature, crystallization reaction and liquidus of the metallic glass. The resulting material shows obvious serrated flow and higher fracture strength under room temperature compressive load, comparing with the monolithic bulk metallic glass (BMG). Three types of interaction between the shear bands and graphite flakes, namely, shear band termination, shear bands branching and new shear bands formation near the graphite flakes can be observed by quasi-static uniaxial compression test and bonded interface technique through Vickers indentation.

Kinetics of Glass Transition and Crystallization in Carbon Nanotube Reinforced Mg-Cu-Gd Bulk Metallic Glass

Mg65 Cu25 Gdlo bulk metallic glass and its carbon nanotube reinforced composite were prepared. Differential scanning calorimeter (DSC) was used to investigate the kinetics of glass transition and crystallization processes. The influence of CNTs addition to the glass matrix on the glass transition and crystallization kinetics was studied. It is shown that the kinetic effect on glass transition and crystallization are preserved for both the monothetic glass and its glass composite. Adding CNTs in to the glass matrix reduces the influence of the heating rate on the crystallization process. In addition, the CNTs increase the energetic barrier for the glass transition. This results in the decrease of GFA . The mechanism of the GFA decrease was also discussed.

Domain structure of hard magnetic NdAlFeCo bulk metallic glass

Magnetic domain structure of hard magnetic Nd60Al10Fe20Co10 bulk metallic glass (BMG) has been studied by using magnetic force microscopy. In the magnetic force images it is shown that the exchange interaction type magnetic domains with a period of about 360 nm do exist in the BMG, which is believed to be associated with the appearance of hard-magnetic properties in this system. As the scale of the magnetic domain is much larger than the size of the short-range ordered atomic clusters existing in the BMG, it is believed that the large areas of magnetic contrast are actually a collection of a group of clusters aligned in parallel by strong exchange coupling interaction. After fully crystallization, the BMG exhibits paramagnetism. No obvious magnetic contrast is observed in the magnetic force images of fully crystallized samples, except for a small quantity of ferromagnetic crystalline phase with low coercivity and an average size of 900 nm.

Serrated Plastic Flow in a Zr-Based Bulk Metallic Glass During Nanoindentation

We investigate plastic deformation of Zr41.2Ti13.8Cu12.5Ni10Be22.5 bulk metallic glass using depth sensing nanoindentation. Numerous serrations in the load-displacement curves during indentation, shear bands and pile-ups around the indent were observed. The results revealed that the serrated plastic flow behaviour in this alloy depends strongly on the indentation strain rate.

Stability of ZrTiCuNiBe Bulk Metallic Glass Upon Isothermal Annealing Near the Glass Transition Temperature

The stability of Zr41Ti14Cu12.5Ni10Be22.5 bulk metallic glass (BMG) upon isothermal annealing near the glass transition temperature has been investigated by using x-ray diffraction, differential scanning calorimetry, and the pulse echo overlap method. The density, elastic constants, and thermodynamic parameters as well as their annealing time dependence have been determined. The microstructural and properties changes of the annealed BMG were checked by acoustic measurement. Obvious structural and property changes were observed with prolonged annealing of the BMG near the glass transition temperature.

Strain Rate-Dependent Compressive Deformation Behavior of Nd-Based Bulk Metallic Glass

Compressive deformation behavior of the Nd60Fe20Co10Al10 bulk metallic glass was characterized over a wide strain rate range (6.0 x 10(-4) to 1.0x10(3) s(-1)) at room temperature. Fracture stress was found to increase and fracture strain decrease with increasing applied strain rate. Serrated flow and a large number of shear bands were observed at the quasi-static strain rate (6.0 x 10(-4)s(-1)). The results suggest that the appearance of a large number of shear bands is probably associated with flow serration observed during compression; and both shear banding and flow serration are a strain accommodation and stress relaxation process. At dynamic strain rates (1.0 x 10(3) s(-1)), the rate of shear band nucleation is not sufficient to accommodate the applied strain rate and thus causes an early fracture of the test sample. The fracture behavior of the Nd60Fe20Co10Al10 bulk metallic glass is sensitive to strain rate.