Formation of icosahedral quasicrystals in an annealed Zr65Al7.5Ni10Cu12.5Ag5 metallic glass

The formation and thermal stability of an icosahedral quasicrystalline phase in an annealed Zr₆₅Al_7.5Ni₁₀Cu_12.5Ag₅ metallic glass have been investigated by X-ray diffraction and transmission electron microscopy analyses. It was found that the quasicrystalline phase can precipitate from the glassy state and the supercooled liquid of the alloy over a wide range of annealing temperatures. After optimizing the heat-treatment conditions, the volume fraction of the quasicrystalline phase in the alloy can reach as high as about 80%. Investigation of the thermal stability of the quasicrystalline phase demonstrates that it is very stable when the annealing temperature is below the glass transformation temperature T _g of the alloy.     

Structure of a cubic phase related to Cd?Mg?rare-earth quasicrystals

The structure of a Cd₆₈Mg₁₂Dy₂₀ crystalline phase denoted as the φ-phase, which has a composition close to that of the Cd₆₆Mg₂₁Dy₁₃ icosahedral quasicrystalline phase, has been investigated by electron diffraction and scanning transmission electron microscopy (STEM). The φ phase has a fcc lattice with a = 21.6Å. High-angle annular dark-field STEM with Z contrast confirms that the phase has the Cd₄₅Sm₁₁-type structure. The atomic cluster in the structure is shown to be characterized by a Friauf polyhedron with tetrahedral symmetry.     

Use of electron channelling contrast imaging to assess near-surface mechanical damage

The crystal structure of a cubic phase in the system Zn-Mg-Er has been solved by a combination of high-resolution electron microscopy and X-ray powder diffraction. This phase is considered to be related to that of the quasicrystalline phase. The structure consists of 448 atoms in the unit cell with lattice constant of a ₀ = 20.20Å and the space group is F43m. Important structural elements in the cubic structure are interpenetrating icosahedral units around Zn and Mg atoms and Frank-Kasper polyhedra around the Mg atoms. No giant icosahedral atomic cluster, such as the 136-atom Bergman cluster, was found in the stucture.     

Structural study of a superlattice Al-Ni-Ru decagonal quasicrystal using high-resolution electron microscopy and a high-angle annular dark-field technique

A high-quality superlattice Al-Ni-Ru decagonal quasicrystal with 0.4nm periodicity, formed in the conventionally solidified Al₇₀Ni₂₀Ru₁₀ alloy, has been studied by high-resolution electron microscopy and a high-angle annular dark-field (Z-contrast) technique. It has been clearly revealed that its structure is characterized as an aperiodically ordered arrangement of decagon-shaped atomic columnar clusters which have a diameter of 2nm and show pentagonal symmetry. On the basis of high-resolution electron microscopy structure images, and the atom-resolution Z-contrast observations which highlight the transition-metal sites, the arrangement of atoms in the superlattice decagonal quasicrystal are proposed.     

Structural characteristics of a high-quality Al?Ni?Ru decagonal quasicrystal with 1.6nm periodicity,studied by atomic-scale electron microscopy observations

We report the structural characteristics of a high-quality stable decagonal quasicrystal (D phase) with 1.6nm periodicity, formed in Al₇₅Ni₁₅Ru₁₀ alloy annealed at 890°C for 24h. The tiling structure and the arrangement of transition-metal atoms (Ru and Ni) in this Al-Ni-Ru D phase have been clearly revealed by high-resolution electron microscopy (HREM) and by highangle annular detector dark-field (HAADF) scanning transmission electron microscopy (STM) respectively. On the basis of the HREM and HAADF STM observations, the relationship between the arrangement of local structural units and the formation of the long-range quasiperiodic tiling structure is discussed.     

Transformation of the decagonal quasicrystalline phase to a B2 crystalline phase in the Al-Cu-Co system by high-energy ball milling

Samples of a decagonal quasicrystalline phase, located in the Al-Cu-Co system and synthesized by a slow cooling technique, have been mechanically milled in a high-energy planetary ball mill for 10, 20 and 30h. The milled powders, as well as powders that had been annealed (after milling) for times ranging from 30 to 150min at 600C, were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. A phase transformation from the decagonal phase to a B2 crystalline phase during highenergy ball milling is reported here for the first time. Powders milled for more than 10h contained predominantly the B2-type crystalline phase with a lattice parameter of 0.29nm. This crystalline phase was found to be quite stable after milling for 30h and also on subsequent annealing at 600C. These experimental results lend support to an earlier suggestion that the decagonal phase in Al-Cu-Co is actually less stable than the B2 phase at low temperatures.     

Effects of ball milling and annealing of an alloy in the Al-Fe-Cu system: Implications for phase equilibria

An icosahedral quasicrystalline alloy in the Al-Fe-Cu system has been mechanically milled in a high-energy ball mill (Szegvari attritor) for 1, 3, 6 and 10 h. Samples were characterized by X-ray diffraction and transmission electron microscopy. The evolution of nanosize crystallites of the disordered B2 phase (bcc; a = 0.29 nm), coexisting with either the parent icosahedral phase or an amorphous phase, occurs during milling. Isothermal heat treatment of milled powder at various temperatures (200, 500, 600, 700, 800 and 850°C) leads in all cases, except at 200°C, to the transformation from disordered B2 and amorphous phases to an ordered B2 phase with a high degree of long-range ordering. The maximum degree of superlattice ordering was found after isothermal treatment at 800^oC. The implications of these results are discussed with reference to phase equilibria existing between crystalline and quasicrystalline phases in the Al-Fe-Cu system.     

Debonding criterion for the piezoelectric fibre push-out test

An Al-Ni-Co pentagonal quasicrystal, showing electron diffraction patterns with pentagonal symmetry and including so-called superlattice reflections, has been examined by the high-angle annular detector dark-field technique with scanning transmission electron microscopy. Columnar clusters with a pentagonal arrangement of transition-metal atoms around their centres are arrayed in a rhombic tiling with a bond length of 2nm, all the clusters having the same orientation of pentagonal symmetry.     

Dislocations in quasicrystals and their interaction with cluster-like obstacles

A dislocation moving through a quasicrystal leaves in its wake a fault denoted a phason wall. For a two-dimensional model quasicrystal the disregistry energy of this phason wall is studied to determine possible Burgers vectors of the quasicrystalline structure. Unlike periodic crystals, the disregistry energy is an average quantity with large fluctuations on the atomic scale. Therefore the dislocation core structure and mobility cannot be linked to this quantity, e.g. by a Peierls-Nabarro model. Atomistic simulations show that dislocation motion is controlled by local obstacles inherent to the atomic structure of the quasicrystal.     

Onset of plasticity in a Σ = 5 GaAs compliant structure

Compliant structures have been fabricated in which a thin GaAs layer (thickness between 10 and 20nm) was bonded on top of a GaAs substrate with a large twist angle (about 37). This twist angle value was chosen so that the energy of the boundary (coincident boundary of type =5 (001)) was minimized. The structure of the interface was characterized and the onset of plasticity in such a compliant substructure was investigated using nanoindentation that allowed the low-load deformation regime to be observed. The results are compared with those obtained under the same conditions on a GaAs bulk substrate alone. No plastic zone was observed by transmission electron microscopy in the compliant structure under loads below 0.25mN while, under the same loads, plastic deformation was observed in the bulk substrate. For higher loads (2mN), plastic-flow enhancement was observed in the compliant structure. The results are discussed in the light of the arrangement of dislocations observed in the plastic zones.     

New 1/1 cubic approximant phases in the Al-Cu-Ru-Si system studied by electron diffraction and high-resolution electron microscopy

Two types of new Al-Cu-Ru-Si 1/1 cubic approximant phases, both of which have cell parameters a=12.68A have been found in an as-cast Al_58.5Cu₁₈Ru_13.5Si₁₀ alloy. The two phases have sc and bcc structures respectively and are finely mixed in transmission electron microscopy observations. It is proposed that the sc structure is caused by ordering of atoms in the bcc structure.     

Atomic structure and solute segregation of a Σ = 3, [110]/{111} grain boundary in an yttria-stabilized cubic zirconia bicrystal

The atomic structure and chemical composition of a =3, [110]/{111} symmetric tilt grain boundary in an yttria-stabilized cubic zirconia bicrystal has been investigated by high-resolution transmission electron microscopy (HRTEM) and nanoprobe energy-dispersive X-ray spectroscopy. The experimental HRTEM images are compared with simulated images for a model obtained by lattice statics calculations. It is found that the grain boundary has two individual mirror symmetrical planes in cation and anion sublattices. In this case, the cations are forced to form sevenfold coordination in the vicinity of the boundary owing to the restraint of the boundary structure, while the cations in the cubic fluorite structure have eightfold coordination. The segregation of yttrium ions was experimentally detected at the = 3 boundary, a finding that is considered to be closely related to the change in the local coordination at the boundary.     

A cubic approximant in the Zn-Mg-Er alloy

A cubic approximant for the icosahedral phase is found in the Zn-Mg-Er system. The preparation of the Zn-Mg-Er ternary phase (the so-called R phase) through quenching and annealing is described in detail. The R phase was found by means of scanning electron microscopy in combination with wavelength-dispersive X-ray analysis. The composition of the R phase varies around Zn₆₃Mg₂₃Er₁₄ in different samples depending on the initial composition. The structure has been studied by a combination of high-resolution transmission electron microscopy (HRTEM) and X-ray powder diffraction. The R phase is cubic with a ₀ = 2.02 nm and crystallizes in the space group F 43m. The close relationship of this phase to the icosahedral phase in the Zn-Mg-Y, RE system (RE = rare earth) is demonstrated through electron diffraction features and HRTEM images.     

A new orthorhombic approximant of the icosahedral Al–Cu–Fe quasicrystal

We report on the formation of a new crystalline approximant phase of the icosahedral (i-)Al–Cu–Fe quasicrystal. This phase is formed during sintering of Al-based composites reinforced with i-AlCuFeB quasicrystalline particles. The structure of this phase has been characterized by transmission electron microscopy (TEM) and high-resolution electron microscopy (HREM). TEM revealed that it is a B-centred orthorhombic phase with lattice parameters a = 1.166 nm, b = 1.195 nm and c = 3.44 nm. Its chemical composition, as determined by electron energy loss spectroscopy (EELS), is close to Al_76.9Cu_2.7Fe_20.4, with an average number of valence electrons per atom e/a of 1.92, similar to the value in all other approximants of the i-phase discovered thus far. Initial results on local atomic arrangements along one of its pseudo-5-fold axes are also presented.     

Local translational order in the icosahedral quasicrystalline phase of V41Ni36Si23

Abstract

The local translational order of the icosahedral quasicrystalline phase in rapidly solidified V₄₁Ni₃₆Si₂₃ has been investigated by means of selected-area electron diffraction and high-resolution electron microscopy. Experimental results show that translational order always occurs in the twofold direction and can be observed when the quasicrystal is examined along its fivefold and threefold as well as twofold axes. Sometimes it occurs in two or three coplanar twofold directions simultaneously. In these cases some crystalline islands exist in the icosahedral quasicrystal and this corresponds to the initial stage of transformation from a quasicrystal to the stable crystalline phase.     

Quasicrystalline Al-Fe phase formed by ion mixing

Abstract

A quasicrystalline Al-Fe phase has been formed by room-temperature ion mixing of AI-Fe multiple layers with no additional postannealing. The quasicrystalline phase was dispersed as grain in an amorphous matrix. The size of the grains was about 10-30nm, and the composition was determined to be Al₈₀Fe₂₀. The structure of the quasicrystalline phase was identified by calculating some 20 sharp diffraction rings in the selected-area diffraction pattern and found to be similar to that of the rapidly quenched AI-Mn quasicrystalline phase.     

Evidence for structural disorder in the icosahedral phase

Abstract

We report transmission electron microscopy results on quasicrystalline samples of Al–25 wt% Mn and Al-38 wt% Mn-5 wt% Si melt-spun flakes. The selected-area diffraction patterns (SADPs) from ‘off-axis’ orientations show not only sharp diffraction maxima but also a diffuse ring, invariant of sample thickness, indicating that it does not arise from amorphous surface oxide. Over-exposed SADPs taken from axial orientations also showed the weak diffuse ring. We suggest that our results indicate the presence of disordered material within the icosahedral phase. Models for the icosahedral phase which involve an assembly of icosahedral clusters inherently contain interstitial voids, which may contain disordered material. Thus our results support these models rather than those derived from space-filling filings, or multiple twinning.     

Transmission electron microscopy study of a new silicon nitride phase

An abnormally large phase, which was found in the precursor-derived Si 3.0 B 1.1 C 5.3 N 3.0 ceramics after crystallization under a nitrogen pressure of 100bar at 1800C for 3h, has been characterized by means of transmission electron microscopy and electron-energy-loss spectroscopy (EELS). EELS analysis shows that this phase consists of only silicon and nitrogen, no other elements being detected. The analysis of selected-area diffraction and convergent-beam electron diffraction in conjunction with EELS reveals that the unknown phase is a variant of silicon nitride. It has a hexagonal structure with lattice parameters a =0.737nm and c =0.536nm, and the space group P62c. .     

Reply to the comments on “Room-temperature precipitation in quenched Al–Cu–Mg alloys: a model for the reaction kinetics and yield-strength development”

We present transmission electron microscopy observations and a crystallographic analysis that show that the only significant report on the observation of {112} pseudotwins in B2 structures by Goo et al. (1985, Acta metall., 3, 1725) is a misidentification of the {114} true twins.     

Microstructural evolution of single-walled carbon nanotubes under electron irradiation

A sample containing single-wall carbon nanotubes (SWCNTs) has been annealed at 900°C and then irradiated by high-energy electrons in an ultrahigh-vacuum transmission electron microscope. Sequential high-resolution images showed that the structures of SWCNT bundles and individual SWCNT segments first collapsed into disordered and fullerene-like carbon materials and then reorganized into graphitic particles under continuous electron irradiation. The speed of structural evolution is dependent on the flux density of the electron irradiation.