Structural and thermal investigations of a high-strength Cu-Zr-Ti-Co bulk metallic glass

Cu 55 Zr 30 Ti 10 Co 5 bulk metallic glass exhibits a high compressive fracture strength of 2.31 GPa and Young's modulus of 130 GPa, values that are higher than those of other Cu- and Zr-based metallic glasses. The addition of Co to the ternary Cu-Zr-Ti alloy stabilizes the supercooled liquid. On heating, the Cu 55 Zr 30 Ti 10 Co 5 metallic glass devitrified and formed an intermediate intermetallic compound prior to reaching equilibrium by diffusion-controlled growth at constant nucleation rate. In the fully annealed state the structure consists of the equilibrium Cu 10 Zr 7 phase with the slightly reduced lattice parameters a = 0.933 nm, b = 0.928 nm and c = 1.254 nm and a small fraction of an unidentified phase.     

High-pressure electrical resistivity behaviour of nanocrystalline perovskite (La,Sr)(Mn,Fe)O3

We report here the electrical resistivity of nanocrystalline perovskite-structured La–Sr manganites as a function of pressures up to 8?GPa, at room temperature. The nanocrystalline perovskite manganites were prepared by the sol–gel technique and found to have crystallite sizes of 12–18?nm. The pressure dependence of the electrical resistivity shows a first-order phase transition at 0.66(2)?GPa and a subtle phase transition between 3.5 and 3.8?GPa. The first-order transition at 0.66?GPa can be related to the transition from localized-electron to band magnetism.     

Effect of aspect ratio on the compressive deformation and fracture behaviour of Zr-based bulk metallic glass

The compressive deformation and fracture features of Zr₅₉Cu₂₀Al₁₀Ni₈Ti₃ bulk metallic glassy samples with aspect ratios in the range of 0.67–2.00 have been investigated. The compressive plastic strain of the glass monotonically increases with decreasing aspect ratio, but the maximum strength almost maintains a constant value of 1.77–1.88?GPa. All the compressive shear-band angles are equal to?～40° if modified by the rotation of the primary shear bands.     

Synthesis of a single phase of high-entropy Laves intermetallics in the Ti–Zr–V–Cr–Ni equiatomic alloy

The high-entropy Ti–Zr–V–Cr–Ni (20 at% each) alloy consisting of all five hydride-forming elements was successfully synthesised by the conventional melting and casting as well as by the melt-spinning technique. The as-cast alloy consists entirely of the micron size hexagonal Laves Phase of C14 type; whereas, the melt-spun ribbon exhibits the evolution of nanocrystalline Laves phase. There was no evidence of any amorphous or any other metastable phases in the present processing condition. This is the first report of synthesising a single phase of high-entropy complex intermetallic compound in the equiatomic quinary alloy system. The detailed characterisation by X-ray diffraction, scanning and transmission electron microscopy and energy-dispersive X-ray spectroscopy confirmed the existence of a single-phase multi-component hexagonal C14-type Laves phase in all the as-cast, melt-spun and annealed alloys. The lattice parameter a = 5.08 Å and c = 8.41 Å was determined from the annealed material (annealing at 1173 K). The thermodynamic calculations following the Miedema’s approach support the stability of the high-entropy multi-component Laves phase compared to that of the solid solution or glassy phases. The high hardness value (8.92 GPa at 25 g load) has been observed in nanocrystalline high-entropy alloy ribbon without any cracking. It implies that high-yield strength (~3.00 GPa) and the reasonable fracture toughness can be achieved in this high-entropy material.     

Pressure dependence of the electrical resistivity of natural cassiterite SnO2 and of undoped and Co-doped nanocrystalline SnO2

The pressure dependence of the electrical resistivity of three different samples of cassiterite, namely natural cassiterite SnO₂, synthetic nanocrystalline SnO₂ (with crystallite size 46?nm) and nanocrystalline Co-doped SnO₂ (with crystallite size 32?nm), has been measured up to 7?GPa at room temperature. The resistivity of natural cassiterite SnO₂ decreases from 2.5?×?10⁴?Ωm at normal pressure and temperature to 1.7?×?10⁴?Ωm at 7.0?GPa. The nanocrystalline SnO₂ has a high resistivity 6.0?×?10⁵?Ωm at normal pressure and temperature and decreases with pressure reaching a value of 2.98?×?10⁵?Ωm at 7?GPa. The activation energy of the electrical conduction of the studied samples were found to be 0.32?eV for the natural SnO₂, 0.40?eV for the nanocrystalline SnO₂ sample and 0.28?eV for the nanocrystalline Co-doped SnO₂. Measurements of the pressure dependence of the electrical resistivity of the Co-doped SnO₂ showed a decrease from 3.60?×?10⁵ to 5.4?×?10⁴?Ωm at 7.0?GPa. We did not observe any pressure-induced phase transition in SnO₂ up to 7?GPa. This study of the high-pressure phase stability of cassiterite corroborates the experimental findings of SnO₂ nanoinclusions in diamonds.     

High-pressure torsion of metastable austenitic stainless steel at moderate temperatures

We subjected samples of a 304 metastable austenitic stainless steel to high-pressure torsion (HPT) in the temperature range of 303–573 K, (i.e. at different austenite stabilities), to examine their microstructures and mechanical properties. HPT processing at room temperature led to the formation of a lamellar microstructure with austenitic and martensitic phases, of which sizes were characterised by prior austenite grains, whereas HPT processing at moderate temperatures produced nanostructured austenite grains through mechanical twinning. The nanostructured 304 steel with an average grain size of ~70 nm exhibited a fine balance between tensile strength (~1.7 GPa) and reduction of area (~55%).     

Novel long-period stacking-ordered structure of martensite in zirconium–cobalt–palladium alloys

A novel long-period stacking-ordered (LPSO) structure of a martensitic phase in a Zr–Co–Pd alloy was discovered and characterized by means of conventional transmission electron microscopy and high-angle annular dark-field scanning transmission electron microscopy. The new phase had a 6O structure and its lattice parameters were estimated to be a = 0.34, b = 0.45 and c = 1.53 nm. The formation mechanism and the space group of the LPSO structure are described.     

Unusual room-temperature compressive plasticity in nanocrystal-toughened bulk copper-zirconium glass

Cast Cu₅₀Zr₅₀ alloy rods with a diameter of 1?mm have been found to consist of a glassy phase containing fine crystalline particles with a size of about 5?nm. They have a glass transition temperature T _g of 675?K, and a large supercooled-liquid region extending 57?K above T _g. The rods exhibit a high yield strength of 1860?MPa and a Young's modulus of 104?GPa. Because they contain a dispersion of embedded nanocrystals, the as-cast bulk metallic glass rods can sustain a compressive plastic strain at room temperature of more than 50%, an exceptional value which is explicable by compensation of any shear softening by nanocrystal coalescence and pinning of shear bands.     

Comparative study of local structure in Zr70Al10Ni20 and quasi-crystal-forming Zr70Al9Ni20Pd1 metallic glasses

The local structure of Zr₇₀Al₉Ni₂₀Pd₁ metallic glass, in which a nano-icosahedral quasi-crystalline phase (I-phase) is formed in the primary stage of crystallization, has been examined and compared with that of Zr₇₀Al₁₀Ni₂₀, the supercooled liquid state of which has a high stability. Since the local environments around the Zr and Ni atoms do not change drastically by the addition of 1 at.% Pd to Zr₇₀Al₁₀Ni₂₀, as evidenced by radial distribution function (RDF) and extended x-ray absorption fine structure (EXAFS) studies, we deduce that the icosahedral phase formed in the Zr₇₀Al₉Ni₂₀Pd₁ metallic glass has a local structure similar to that in Zr₇₀Al₁₀Ni₂₀. Although a very slight rearrangement of Zr–Zr atomic pairs occurs during quasi-crystallization, the I-phase formation is achieved without disturbing the dominant local structure in the glassy state of the Zr₇₀Al₉Ni₂₀Pd₁. An icosahedral local structure is proposed for Zr–Al–Ni metallic glass system as well as for primary quasi-crystal (QC)-forming Zr-based metallic glasses.     

Scale-dependent fracture mode in Cu–Ni laminate composites

Fracture behavior of Cu–Ni laminate composites has been investigated by tensile testing. It was found that as the individual layer thickness decreases from 100 to 20 nm, the resultant fracture angle of the Cu–Ni laminate changes from 72° to 50°. Cross-sectional observations reveal that the fracture of the Ni layers transforms from opening to shear mode as the layer thickness decreases while that of the Cu layers keeps shear mode. Competition mechanisms were proposed to understand the variation in fracture mode of the metallic laminate composites associated with length scale.     

Novel fabrication of bulk Al with gradient grain size distributions via powder metallurgy

We describe a novel approach to synthesize gradient microstructures, defined hereafter as containing a broad but continuous distribution of grain sizes. These microstructures extend the concept of a bimodal grain size distribution and the ability to design with multiple length scales. We demonstrate the proposed approach via experiments involving cryogenic ball milling of Al–4.5Mg–0.4Mn–0.05Fe and Al–50Mg powder followed by subsequent consolidation. Our results reveal that the grains in the consolidated powder present a gradient size distribution ranging from <100 nm to >3 μm. Moreover, phase composition analysis revealed a unique “interfingered” structure where the two starting phases were intermixed in a complex three-dimensional mesh. Hardness studies of this gradient microstructure show average Vickers hardness values of 200 ± 2.6, 204 ± 4.3 and 266 ± 50 for macrohardness, microhardness and nanoindentation, respectively. The standard deviation values highlight that the gradient microstructure is disordered locally, but homogenous macroscopically.     

Synthesis and characterization of nanocrystalline MoBi2Te5 thin films for photoelectrode applications

Molybdenum bismuth telluride thin films have been prepared on clean glass substrate using arrested precipitation technique which is based on self-organized growth process. As deposited MoBi₂Te₅ thin films were dried in constant temperature oven at 110°C and further characterized for their optical, structural, morphological, compositional, and electrical analysis. Optical absorption spectra recorded in the wavelength range 300–800?nm showed band gap (E _g) 1.44?eV. X-ray diffraction pattern and scanning electron microscopic images showed that MoBi₂Te₅ thin films are granular, nanocrystalline having rhombohedral structure. The compositional analysis showed close agreements in theoretical and experimental atomic percentages of Mo⁴⁺, Bi³⁺, and Te^2? suggest that chemical formula MoBi₂Te₅ assigned to as deposited molybdenum bismuth telluride new material is confirmed. The electrical conductivity and thermoelectric power measurement showed that the films are semiconducting with n-type conduction. The fill factor and conversion efficiency was characterized by photoelectrochemical (PEC) technique. In this article, we report the optostructural, morphological, compositional, and electrical characteristics of nanocrystalline MoBi₂Te₅ thin films to check its suitability as photoelectrode in PEC cell.     

High temperature mechanics of nanomoulded amorphous metals

High temperature mechanics of nanomoulded amorphous metals was investigated by in situ nanomechanical testing. Nanopillars of Pd₄₃Cu₂₇Ni₁₀P₂₀ metallic glass were synthesized by thermoplastic forming and their stress–strain response was obtained concurrent with direct observation of their deformation behaviour. This allowed the measurement of mechanical behaviour from nanopillars and the corresponding bulk substrate with identical thermal history. A rise in elastic modulus was seen with increase in temperature for both the nanopillars and substrate, which was explained by diffusive rearrangement of atomic-scale viscoelastic units. The results provide fundamental insights into structural rearrangement in metallic glasses.     

Structural stability of W2B5 under high pressure

High-pressure structural stability studies have been carried out on tungsten boride W₂B₅ up to maximum pressure of 36 GPa using a Mao-Bell diamond-anvil cell at beamline BR-12 of the ELETTRA synchrotron facility (λ = 0.68881 Å). The hexagonal phase (S.G:P6₃/mmc) of W₂B₅ is stable up to the maximum pressure studied. The bulk modulus is estimated to be ~347 GPa using the Birch–Murnaghan equation of state. The variation of lattice parameters and bond lengths B–B and W–B have been studied and the c-axis is seen to be marginally more compressible than the a-axis.     

Effects of annealing temperature on structural,optical, and electrical properties of antimony-doped tin oxide thin films

Antimony-doped tin oxide (ATO) films, approximately 320 nm in thickness, have been prepared by electron beam evaporation onto glass substrates. The films were annealed at temperatures between 400°C and 550°C in air and their structure and surface morphologies were observed by X-ray diffraction (XRD) and atomic force microscopy (AFM) after the different annealing treatments. XRD patterns of the ATO thin films as-deposited and annealed at 400°C showed that they were amorphous, but annealing beyond 400°C caused the films to become polycrystalline with tetragonal structure and orientated in the (1 1 0) direction. The grain size in the annealed films, obtained from the XRD analysis, was in the range 146–256 Å and this increased with the annealing temperature. The dislocation density, cell volume and strain were found to decrease gradually with increasing annealing temperature. Photoluminescence spectra revealed an intensive blue/violet peak at 420 nm, which increased gradually in height with annealing. It is suggested that an increase in the population of Sb⁺⁵ ions might be the reason for the enhancement of the blue/violet emission. The optical properties of the films were also investigated in the UV-visible-NIR region (300–1000 nm). The optical constants, namely the refractive index n and the extinction coefficient k in the visible region were calculated. The optical energy band gap, as determined by the dependence of the absorption coefficient on the photon energy at short wavelengths, was found to increase from 3.59 to 3.76 eV with annealing temperature.     

Unusual stress behaviour of CeO2-doped diamond-like carbon nanofilms

CeO₂-doped diamond-like carbon (DLC) films with thicknesses of 180–200 nm were deposited by unbalanced magnetron sputtering. When the CeO₂ concentration is in the range 5–8%, the residual compressive stress of the deposited films is reduced by 90%, e.g. from about 4.1 GPa to 0.5 GPa, whereas their adhesion strength increases. These effects are attributed to the dissolution of CeO₂ within the DLC amorphous matrix and a widening interface between the DLC film and the Si substrate, respectively.     

Crystallographic texture formation during recrystallization of cold-rolled Fe-3%Si single crystal under high DC magnetic fields

In a flat single crystal of Fe–3%Si alloy with (1 1 0)[0 0 1] orientation, regions with (0 0 1)[1.–1.0] orientation (deformation twins) were created by rolling at a low temperature. After cold rolling at 80% at an angle of 45º to the [0 0 1] direction, a (1 1 2) [1.–1.0] deformation texture was formed. In the recrystallization process during annealing of such a sample, a polycrystalline structure having a nearly cubic texture (0 0 1) [1–1.0] is formed. It is demonstrated that annealing under a high DC magnetic field enhances the cubic texture sharpness as compared to annealing carried out under similar conditions without a magnetic field.     

Microstructure and phase evolution in spark-plasma-sintered Al86Ni6Y4.5Co2La1.5 glassy alloy

Al₈₆Ni₆Y_4.5Co₂La_1.5 amorphous powders synthesized after 200 h of mechanical alloying were spark plasma sintered at 25 and 400 MPa at 400 °C for 15 min. The sample sintered at 25 MPa showed precipitation of FCC-Al grains of sub-micron size attributed to a higher amount of localized high-temperature regions which favoured faster long-range atomic diffusion. On the contrary, the 400-MPa sintered sample showed the presence of nanocrystals (5–20 nm) distributed in an amorphous matrix. This is attributed to higher pressure sintering favouring local and short-range atomic redistributions. The higher amount of retained amorphous phase in the 400-MPa sintered sample could be accounted for by a smaller amount of localized high-temperature regions in comparison to those in 25-MPa sintered sample. High-pressure sintering induces shear fracturing and fragmentation of the brittle amorphous particles and provided better surface contact and packing density. The retention of a larger amount of amorphous phase and a higher relative density (96%) contributes to high microhardness (278 Hv) and nanoindentation hardness (3.7 GPa) of the 400-MPa sintered sample.     

Frequency-temperature dependent dynamics of dielectrics in ferric oxoborate Fe3BO6 of cocktail structure of nanorods

Oxoborates have both dielectric and magnetic properties useful for magnetodielectric devices, sensors, or biological tools. Such compounds Fe₂BO₄, Fe₃BO₅, or Fe₃BO₆ are known to grow easily as single crystals in a liquid flux. A polycrystalline phase forms only on controlled conditions of a solid state reaction of the basic oxides. In this study, we report highly dielectric Fe₃BO₆ when grown in a specific shape of nanorods (～200?nm diameter and 50–100?µm length) from an iron borate glass, which offers devisable shapes of sheets, discs, and fibers. Frequency (f)-temperature reliant dynamics of dielectric constant ε_r is studied over 25–300°C at 0.1–10^3?kHz frequencies. At low frequency such as 100?Hz, a large ε_r -value 40,000, better than most of high ε_r -value ferroelectrics, incurs at room temperature. At f?≥?50?kHz, although only an order of diminished ε_r -value lasts, it increases steadily with temperature, possibly due to increasing electrical conductivity in a specific resistor–capacitor network. Suppressed dielectric relaxation and spin-flops share a merely weak spin-reorientation transition near 160°C. A stable power loss ≤0.5 lasts at f?>?10?kHz useful for possible applications of magnetodielectric materials.     

Kinetic study of static recrystallization in an Fe–Al–O ultra-fine-grained nanocomposite

A nearly abrupt coarsening of grains is observed in a newly developed Fe–Al–O ultra-fine-grained nanocomposite with a significant volume fraction (4%) of alumina nano-precipitates. The microstructure of the alloy was analysed in different states (as-received and annealed) by means of scanning electron microscopy, transmission electron microscopy (TEM) and hardness. The initial grain size 150–200 nm increases up to 50 μm during annealing 1000 °C/8 h and thereafter demonstrates saturation. A linear correlation between volume fraction of coarse grains and hardness was found. It was identified by TEM that alumina nano-precipitates stabilize the dislocation microstructure against recovery very effectively and the grain coarsening is due to fast growth of very few dislocation free grains. Thus, the observed grain coarsening has the attributes of static recrystallization.