Evolution of rapidly solidified NiAlCu(B) alloy microstructure

This study concerned phase transformations observed after rapid solidification and annealing at 500, 700 and 800 °C in 56.3 Ni‐39.9 Al‐3.8 Cu‐0.06 B (E1) and 59.8 Ni‐36.0 Al‐4.3 Cu‐0.06 B (E2) alloys (composition in at.%). Injection casting led to a homogeneous structure of very small, one‐phase grains (2–4 µm in size). In both alloys, the phase observed at room temperature was martensite of L1₀ structure. The process of the formation of the Ni₅Al₃ phase by atomic reordering proceeded at 285–394 °C in the case of E1 alloy and 450–550 °C in the case of E2 alloy. Further decomposition into NiAl (β) and Ni₃Al (γ′) phases, the microstructure and crystallography of the phases depended on the path of transformations, proceeding in the investigated case through the transformation of martensite crystallographic variants. This preserved precise crystallographic orientation between the subsequent phases, very stable plate‐like morphology and very small β + γ′ grains after annealing at 800 °C.     

The Third International Conference on Scanning Tunnelling Electron Microscopy

The transition quasi-crystalline→crystalline is found to be very sluggish in the ternary alloy Al₆₀Mn₁₁Ni₄. This makes it possible to study in detail the relationship between the decagonal phase, obtained after furnace cooling, and two different crystalline phases, which result after long annealing at 400°C. Use is made of electron diffraction, high resolution electron microscopy and optical diffraction. The crystalline phases still exhibit features which are closely related to those of the decagonal phase. This can be concluded from a comparison of the electron diffraction patterns of the quasi-crystalline phase along a number of zones, with those of the crystalline phases along corresponding zones. The crystalline phases contain different types of defects which are analysed in detail using high resolution images and diffuse scattering in the electron diffraction patterns. The close relationship between the electron diffraction patterns of the crystalline and quasi-crystalline phases is explained in terms of general optical principles. Some characteristic features of a model of the quasi-crystalline phase are tentatively proposed.     

Dislocations in nanostructured two‐phase Fe30Ni20Mn20Al30

In a previous study, the dislocations in Fe₃₀Ni₂₀Mn₂₅Al₂₅ (at. %), which consist of 50 nm wide alternating b.c.c. and B2 phases, were shown to have a/2<111> Burgers vectors after room temperature deformation. The dislocations were found to glide in pairs on both {110} and {112} slip planes and were relatively widely separated in the b.c.c. phase, where the dislocations were uncoupled, and closely spaced in the B2 phase, where the dislocations were connected by an anti‐phase boundary. In this article, we analyze the dislocations in the two ～5 nm‐wide B2 phases in a related two‐phase alloy Fe₃₀Ni₂₀Mn₂₀Al₃₀, with compositions Fe‐23Ni‐21Mn‐24Al and Fe‐39Ni‐12Mn‐34Al, compressed to ～3% strain at a strain rate 5 × 10^?4 s^?1 at 873 K (the lowest temperature at which substantial plastic flow was observed). It is shown that slip occursby the glide of a<100> dislocations. A review of the literature suggests that the differences in the observed slip vector between these B2 phases could be due to the differences in composition, differences in deformation temperature, or possibly both. Microsc. Res. Tech. 76:263–267, 2013. © 2013 Wiley Periodicals, Inc.     

The substructure of quasicrystalline Al-Mn alloy observed by TEM

The morphology of the icosahedral phase in Al₈₆Mn₁₄ alloy has been observed as flower-like and of granular shape by TEM. These two kinds of morphologies may be regarded as the different sections of a three-dimensional flower-like grain. Inside these grains, a fine substructure of a few nm in size has been found. A dendritic morphology with a diffraction pattern showing five-fold symmetry have also been observed in the Al₈₆Mn₁₄ alloy. On the basis of these observations, a model based on nucleation, growth and aggregation has been proposed to explain the formation process of the quasicrystalline state.     

Crystalline phases found in rapidly quenched Ni–Nb–Zr alloys

The properties of metallic alloys can be significantly improved by developing non‐equilibrium phases in the microstructures through rapid solidification techniques, thus the characterisation of these unusual structures is extremely important. In this research, the microstructures of three rapidly quenched alloys, namely Ni_65.2Nb_33.8Zr_1.0, Ni_54.8Nb_31.1Zr_14.1 and Ni_54.8Nb_21.6Zr_23.6 (at. %) were investigated in greater detail in order to determine the structures and compositions of their crystalline phases. These crystalline phases were characterised using a combination of scanning electron microscopy, energy dispersive x‐ray spectroscopy, x‐ray diffraction and transmission electron microscopy techniques. The phases were compared to the crystalline structures reported in the literature. Our results indicate some agreement with the Ni–Nb phase diagram and an isothermal section of the Ni–Nb–Zr phase diagram; however, it is detected zirconium solubility in the Ni₃Nb phase, as well as, the absence of expected crystalline phases.     

Modification of Mo-Si alloy microstructure by small additions of Zr

Molybdenum and its alloys are potential materials for high-temperature applications. However, molybdenum is susceptible to embrittlement because of oxygen segregation at the grain boundaries. In order to alleviate the embrittlement small amounts of zirconium were alloyed to a solid solution of Mo-1.5Si alloy. Two Mo-based alloys, namely Mo-1.5Si and Mo-1.5Si-1Zr, were investigated by the complementary high-resolution methods transmission electron microscopy and atom probe tomography. The Mo-1.5Si alloy shows a polycrystalline structure with two silicon-rich intermetallic phases Mo₅Si₃ and Mo₃Si located at the grain boundaries and within the grains. In addition, small clusters with up to 10 at% Si were found within the molybdenum solid solution. Addition of a small amount of zirconium to Mo-1.5Si leads to the formation of two intermetallic phases Mo₂Zr and MoZr₂, which are located at the grain boundaries as well as within the interior of the grain. Transmission electron microscopy shows that small spherical Mo-Zr-rich precipitates (<10 nm) decorate the grain boundaries. The stoichiometry of the small precipitates was identified as Mo₂Zr by atom probe tomography. No Si-enriched small precipitates were detected in the Mo-1.5Si-1Zr alloy. It is concluded that the presence of zirconium hinders their formation.     

A study of phase separated Ni66Nb17Y17 metallic glass using atom probe tomography

Microstructural characterization of Ni₆₆Nb₁₇Y₁₇ as spun metallic glass ribbon was carried out using atom probe tomography. A comparison of different experimental conditions for pulsed laser and pulsed voltage field evaporation reveal that the laser pulsing can be optimized to avoid preferential evaporation of yttrium. Atom probe tomography measurements illustrate that the sample undergoes phase separation resulting in two interconnected phases during the process of vitrification. The yttrium-enriched phase was depleted in niobium and yttrium-depleted phase was enriched in niobium. Moreover, detailed analyses of the roller-contact and non-contact sides of the melt-spun ribbon show different wavelength of phase separated regions revealing that the degree of phase separation is directly associated with the cooling rate.     

Synthesis and characterization of permalloy-reinforced Al2O3 nanocomposite powders by mechanical alloying

Intermetallics of Fe and Ni, which are known as permalloy, are under attention due to their excellent magnetic performance. Besides, mechanical properties of the materials can be improved by decreasing crystallite size of FeNi intermetallics or by reinforcing them with hard secondary phases such as Al₂O₃. In this study, FeNi–Al₂O₃ nanocomposite powders with three different compositions were successfully synthesized through mechanical alloying of Fe₂O₃, Ni, and Al powders mixture. Characterization of the samples was accomplished by scanning electron microscopy, transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy and X-ray diffraction. Effects of various parameters such as chemical composition of received materials, milling time, and annealing on the phase evolution, morphology, and microhardness of samples were investigated. It was found that by the addition of Fe as diluent, the required milling time for formation of FeNi intermetallic increased. By increasing milling time, mean crystallite size of FeNi decreased and reach to about 28 nm for FeNi-30 wt% Al₂O₃ nanocomposite powder sample. TEM observations also showed that in situ-formed Al₂O₃ particles, with particle size of about 65 nm, were uniformly dispersed within FeNi matrix.     

The influence of voxel size on atom probe tomography data

A methodology for determining the optimal voxel size for phase thresholding in nanostructured materials was developed using an atom simulator and a model system of a fixed two-phase composition and volume fraction. The voxel size range was banded by the atom count within each voxel. Some voxel edge lengths were found to be too large, resulting in an averaging of compositional fluctuations; others were too small with concomitant decreases in the signal-to-noise ratio for phase identification. The simulated methodology was then applied to the more complex experimentally determined data set collected from a (Co_0.95Fe_0.05)₈₈Zr₆Hf₁B₄Cu₁ two-phase nanocomposite alloy to validate the approach. In this alloy, Zr and Hf segregated to an intergranular amorphous phase while Fe preferentially segregated to a crystalline phase during the isothermal annealing step that promoted primary crystallization. The atom probe data analysis of the volume fraction was compared to transmission electron microscopy (TEM) dark-field imaging analysis and a lever rule analysis of the volume fraction within the amorphous and crystalline phases of the ribbon.     

Subsurface damage during dry sliding wear of Al-Al3Ni eutectic alloy

Cylindrical Al-Al₃Ni eutectic alloy wear pins (10 mm in diameter) were slid against a polished steel surface in a pin-on-disc rotating machine under unlubricated conditions with bearing pressures of 6–60 kPa and a constant sliding speed of 70 m min^?1. Metallographic changes in the subsurface region of contact were examined by optical microscopy and microhardness measurements. In the bearing pressure range investigated the alloy exhibited “mild” wear in two linear regions identified as pure “oxidative” wear at low bearing pressures and oxidative with superimposed “metallic” wear at higher bearing pressures. Plastic deformation and fragmentation of the Al₃Ni phase occurred under all bearing pressures. However, in composites prepared by unidirectional solidification containing large Al₃Ni particles fragmentation was insignificant. In all other specimens the size of the fragmented particles in the subsurface region of contact was about 5 μm irrespective of the bearing pressure.     

Influence of structural parameters on magnetoresistive properties of CuFeNi melt spun ribbons

The microstructure of Cu₈₀Fe₁₀Ni₁₀ (at%) granular ribbon was investigated by means of atom probe tomography (APT). A granular system is composed of magnetic precipitates embedded in a non-magnetic matrix. In this ribbon, the magnetic precipitates have a diameter smaller than 5 nm in the as-spun state, and their crystallographic structure is very similar to the one of the matrix, which makes it difficult to characterize them using conventional techniques. Those data are of great importance to understand the magnetic and the transport behaviour of these ribbons. Using atom probe tomography, a 3D reconstruction of the microstructure of the as-spun and annealed ribbons was achieved and a precise characterization of the compositions of the two phases and of the composition profile at interfaces was carried out. In the as-spun state the composition of the matrix is Cu₈₉Fe₃Ni₈, the one of the precipitates is Cu₃₀Fe₄₀Ni₃₀. Upon annealing, the precipitates get enriched in iron. After annealing at 600 °C for 24 h, the measured compositions are close to the one predicted by Thermocalc, with Cu₉₄Fe₁Ni₅ for the matrix and Cu₅Fe₆₄Ni₃₁ for the precipitates.     

Characterisation of the early stages of solute clustering in 1Ni–1.3Mn welds containing Cu

Microstructural characterisation of neutron irradiated low alloy steels is important for developing mechanistic understanding of irradiation embrittlement. This work is focused on the early stages of irradiation-induced clustering in a low Cu (0.03 wt%), high Ni (∼1 wt%) weld. The weld was irradiated at a very high dose rate and then examined by atom probe (energy-compensated position-sensitive atom probe (ECOPoSAP) and local electrode atom probe (LEAP)) with supporting microstructural information obtained by small angle neutron scattering (SANS) and positron annihilation (PALA).     

Effect of microstructure and mechanical properties on the seizure resistance of cast aluminium alloys

Seizure resistance of several cast aluminium base alloys has been examined using a standard Hohman Wear Tester. Disks of aluminium base alloys were run against a standard aluminium 12% silicon base alloy. The seizure resistance of the alloys (as measured by the lowest bearing parameter reached before seizure) increased with hardness, yield and tensile strength. In Al-Si-Ni alloys where silicon and nickel have little solid solubility in α-aluminium and Si and Ni Al₃ hard phases are formed, the minimum bearing parameter decreased with the parameter V (The product of vol. % of hard phases in the disk and the shoe). Apparently the silicon and NiAl₃ particles provided discontinuities in the matrix and reduced the probability (1 ? V) of the α-aluminium phase in the disk coming into contact with the α-aluminium phase in the shoe. The copper and magnesium containing Al-Si-Ni alloys with lesser volumes of hard phases exhibit considerably better seizure resistance indicating that a slight increase in the solute content or the hardness of the primary α-phase leads to a considerable increase in seizure resistance. Deformation during wear and seizure leads to fragmentation of the original hard particles into considerably smaller particles uniformly dispersed in the deformed α-aluminium matrix.     

Influence of plastic deformation and prolonged ageing time on microstructure of a Haynes 242 alloy

The material used in this study was a commercial HAYNES® alloy 242? with a nominal composition of Ni‐25% Mo‐8% Cr (in wt.%). In the standard heat treatment, the 242 alloy is annealed at a temperature between 1065 and 1095 °C and then water quenched. The ageing treatment is carried out at 650 °C for 24 h in order to develop the long‐range‐order strengthening. The alloy in the conventionally aged condition was additionally cold rolled to 50% reduction in thickness and subsequently subjected to prolonged ageing at 650 °C for 4000 h. The enhanced diffusion resulted in the decomposition of the Ni₂(Mo,Cr) metastable phase into the stable Ni₃Mo‐based phase. The presence of the new stable phase increased the yield and tensile strengths but deteriorated the ductility of the alloy at both room and 650 °C temperatures.     

Wear behavior and mechanisms of alumina-based ceramic tools in machining of ferrous and non-ferrous alloys

In this paper, the machining performance and wear mechanisms of two alumina-based ceramic cutting tools (Al₂O₃/TiB₂ and Al₂O₃/TiB₂/SiC_w) in continuous turning of hardened steel and nickel based alloy (Inconel 718) were examined. Results showed that in turning of hardened steel performed under identical conditions, Al₂O₃/TiB₂/SiC_w tool exhibited lower flank wear resistance than that of Al₂O₃/TiB₂ tool, the mechanisms responsible for this were determined to be the strong atom bonding between SiC and Fe, and the whisker pullout from the matrix for Al₂O₃/TiB₂/SiC_w ceramic tool. In continuous turning of Inconel 718, the Al₂O₃/TiB₂/SiC_w tool showed greatly improved flank wear resistance compared to Al₂O₃/TiB₂ tool, adhesion and abrasion wear were found to be the dominant wear mechanisms, the adhesion and diffusion of Ni, and Cr of Inconel 718 to the tool rake face may accelerate the tool wear rates.     

Novel investigation on tribological properties of Ni–P–Ag–Al2O3 hybrid nanocomposite coatings

In this research, silver and alumina particles were co-deposited within Ni–P matrix to obtain Ni–P–Ag–Al₂O₃ hybrid coating. The structure of coatings was analyzed by X-ray diffraction and the tribological properties of deposits were evaluated by pin on disc tribometer. 3D optical profiler and scanning electron microscopy were used to study wear rate and worn surfaces. The results showed that Ni–P–Ag and Ni–P–Ag–Al₂O₃ coatings have the self-lubrication property and maximum hardness (∼1310 HV) and wear resistance were obtained for Ni–P–Al₂O₃ coating. Also, Ni–P–Ag–Al₂O₃ hybrid nanocomposite coating had higher wear resistance than Ni–P and Ni–P–Ag coatings. Moreover, the best conditions was achieved for heat treated hybrid coating in the concentration of 30 mg/L silver and 150 mg/L alumina in the plating solution.     

An ion microprobe study of the microchemistry of Ni-base superalloy-Al2O3 metal-matrix composites

The chemical microstructure of Ni-base superalloy/Al₂O₃ metal-matrix composites (MMCs) has been studied by scanning ion microprobe microanalysis, using the secondary ion mass spectrometry (SIMS) technique. The MMCs were fabricated using the transient-liquid-phase bonding (TLP) process, with B-doped superalloy powder as an interlayer. Boron was found to diffuse rapidly throughout the matrix to form boride phases, mostly at the grain boundaries in the matrix. These borides contain excess Cr (also Mo, Si, W) in comparison with the Ni alloy-matrix, but are depleted in Ni (also in Al and Co). Carbides form at the grain boundaries as thin platelets and inside the grains as fine particles. Chemical reaction occurs between the sapphire fibre and the matrix; formation of NiAl₂O₄ spinel at the interface is suggested. This interface reaction layer is friable and parts of it peel off during consolidation to become inclusions in the matrix near the fibre/matrix interface.     

Crystal orientation mapping of NiO grown on cube textured Ni tapes

Samples of cube textured Ni tapes were oxidized in flowing oxygen at different temperatures. Crystal orientation maps (COMs) of the resulting oxide layers were produced by electron backscatter diffraction. The oxide layers were also analysed by X‐ray diffraction (XRD), scanning electron microscopy and atomic force microscopy (AFM). The oxide grain size of a sample oxidized at 600 °C was similar to that of the substrate and the oxide was highly textured, both indicating epitaxial growth. The orientation relationship between the substrate and the oxide was directly observed from XRD to be (111)_NiO//(001)_Ni, [01]_NiO//[110]_Ni with four, equivalent, in‐plane variants. In each variant, the oxide has both <110>‐ and <211>‐type directions parallel to the Ni <110> directions. Differences in oxide thickness and surface roughness on neighbouring grains were revealed by AFM and these were attributed to the existence of a range of oxide growth conditions resulting from small differences in the orientation of each substrate grain. Similar macrotexture and microstructure were observed on a sample oxidized at 1300 °C, but additional, facetted oxide crystals had formed at the oxide grain boundaries. COMs showed that these crystals were either cube or 45° rotated cube orientated, a texture different to that of the large oxide grains. The grain boundary crystals were thought to form by inward diffusion of oxygen at defects in the growing oxide scale.     

Pawley and Rietveld refinements using electron diffraction from L1₂-type intermetallic Au₃Fe₁-x nanocrystals during their in-situ order-disorder transition

During the in-situ order-disorder transition of intermetallic L1₂-type Au₃Fe_1−x nanocrystals, structural information has been retrieved from their electron diffraction patterns based on the Pawley refinement that is unrelated to the electron kinematical or dynamical scattering nature as well as the Rietveld refinement using a kinematical approximation. At room temperature, it was found that the nanocrystals contain approximately x=40% vacancies at the Fe site. Based on in-situ heating this phase displayed an irreversible order-disorder transition, with the transition temperature between 553 and 593 K. A sudden increase in lattice parameter was detected during the first heating from the ordered phase, while the second heating of the disordered phase showed only a linear relationship with temperature. From the lattice parameter measurement of the disordered phase, the coefficient of thermal expansion was estimated as 1.462×10⁻⁵ K⁻¹. The long-range order parameter S was determined by the refined site occupancies, as well as the integrated intensities of the superlattice (1 0 0) and fundamental (2 2 0) reflections using the Pawley and Rietveld refinements during the order-disorder transition. Considering the dynamical scattering effect, Blackman two-beam approximation theory was applied to corrected S, which slightly attenuated after the correction. A comparison of the electron diffraction with X-ray diffraction data was made. It was demonstrated that elemental and structural information could be retrieved through quantitative electron diffraction studies of the nanomaterials. Since the Pawley refinement algorithm does not include the electron scattering event, it is especially useful to refine the electron diffraction data regardless of the sample thickness.