Characterisation of rosette formation in an aluminium–silicon alloy

Differential thermal analysis has been used to investigate the effect of cooling rate on rosette formation during solidification of a synthetic Al–Fe–Si alloy. Rosettes can be characterised as a very fine multiphase structure within more or less convex areas dispersed in the matrix. Their formation during solidification is related with liquid entrapment and high solidification undercooling associated with the need of independent nucleation events of second phases. It is here shown that their density and internal coarseness depend on cooling rate. Further, metallographic observation of rosettes in contact with large precipitate of β-Al₉Fe₂Si₂ phase allowed to conclude that this latter phase does not help silicon nucleation.     

Interfacial reaction between Co–Cr–Mo alloy and liquid Al

The interfacial reaction between Co–Cr–Mo alloy and liquid Al was investigated using immersion tests. Microstructure characterization indicated that the Co–Cr–Mo alloy was corroded by liquid Al homogeneously, with the formation of a (Co,Cr,Mo)₂Al₉ layer close to alloy matrix and “(Cr,Mo)₇Al₄₅ + Al” layer close to Al. Kinetics analysis showed that the corrosion of the Co–Cr–Mo alloy followed a linear relationship with the immersion duration. Compared with pure Co–liquid Al reaction system, the alloying of Cr and Mo changed the solid–liquid interface structure, but the corrosion of the solid metal was still dominated by the dissolution of an intermetallic layer.     

Ellipsometric and electrochemical studies of oxide films formed on nickel in air at 100–400°C

The properties of oxide film grown on nickel in air at 100–400°C were studied using ellipsometric and electrochemical methods. It was found that during oxidation of nickel at 100–250°C an oxide film is formed which grows according to a logarithmic law. The film formed at higher temperatures is composed of two successive layers. The inner layer exhibits properties identical to the oxide film grown at 100–250°C, while the outer layer, which grows according to a parabolic law, shows different properties. The thickness of the oxide film depends upon both the purity and the pretreatment of the nickel.     

Influence of Mo in the structure of rapidly solidified Fe–Mo–Cr–Mn–Si–C alloy

Abstract

An Fe–Mo–Cr–Mn–Si–C alloy was prepared in an induction furnace and was cast into cylindrical rod in a copper mould in castmatic equipment (low pressure casting). A single phase non-equilibrium featureless (no visible microstructures after deep etching) phase was observed over a certain range of thickness of the rod. In this present work, the extent of the featureless phase was studied with different concentrations of Mo (5–25 wt-%) for 5·5 mm diameter of cylindrical rod at a cooling rate of 1100 K s^–1. Light optical microscopy, scanning electron Microscopy and Vickers hardness tests were used to analyse the samples. The amount of the featureless area varies as the Mo content changes and the maximum featureless area was obtained for 7 wt-% of Mo. This single phase featureless structure exhibits very high hardness (>1350 HV) which can be used in many interesting applications with or without suitable heat treatments.     

Electrodeposition of Ni–Co alloy films onto titanium substrate

Binary bright Ni–Co alloy films were electrodeposited on titanium in the chloride–sulfate electrolytes.The influences of Co2?concentration, current density, and temperature on the Ni–Co alloy films electrodeposition were investigated. The films were analyzed by scanning electron microscope(SEM), energy dispersive spectroscopy(EDS), and X-ray diffraction(XRD). Cathodic polarization for Ni–Co codeposition was performed on Ti working electrodes. With the increase of Co2?concentration, the Ni content in the films decreases and the current efficiency increases slightly. The Ni content increases with the increase of temperature, while it decreases with the increase of current density to a minimum and then increases. The cathodic reduction peak potential is measured to be-1.34 V. Anomalous deposition is found to occur in the Ni–Co codeposition. The SEM of Ni–Co alloy films shows that hydroxide particles are not present on the surface and fine grain, compact, smooth, and bright Ni–Co alloy films are obtained. The XRD result indicates that the deposited Ni–Co alloy film is Ni-solid solution with a facecentered cubic in structure.     

The apparent induction period for γ-Al2O3 development in thermal oxide films on aluminium

A novel technique has been employed to allow ready detection of fine crystallites, probably of -Al₂O₃, of sizes generally less than 10 nm in thermal oxide films on aluminium. Using this approach, the relationship between the average population density of -Al₂O₃ crystals and oxidation time has been obtained for the first time. Importantly, it has been found that oxidation at temperatures of 515 or 490°C results in fine crystal development almost from the onset of thermal oxidation. Thus, the so-called induction period for the growth of the -Al₂O₃ crystals, determined previously from weight gain data, should now be regarded as the oxidation time required for both the population density and sizes of the crystals to become sufficiently large to cause significant deviation in the weight gain data from the initial inverse logarithmic law describing the growth of the amorphous oxide.     

Characterization of oxide films formed on magnesium alloys using bipolar pulse microarc oxidation in phosphate solutions

The surface morphology and chemical composition of the oxide films formed on pure magnesium and AZ91D alloy in aqueous electrolytes which contained sodium hexafluorinealuminate(Na3 AlF6 ), potassium hydroxide (KOH), sodium hexametahposphate ((NaPO3)6 ), and triethanolamine were investigated by X-ray diffraction (XRD), scanning electron microscope(SEM) and energy dispersive spectroscopy(EDX). The results show that the input of the negative pulse has great influences on the quantity and the appearance of the microdischarges. Three types of pores can be distinguished on the surface of the oxide film and their size ranges are 0.5- 1μm, 1 - 2μm and 4- 7μm, respectively. A few microcracks are seen around the large pores. There exists a remarkable fluorideenriched zone of about 4 - 6μm for pure magnesium and 3 - 5μm for AZ91D alloy at the coating/substrate interface.     

The influence of saccharin on the electrodeposition and properties of Co–Ni alloy thin films

Abstract

Co–Ni alloys thin films were electrodeposited on Ru substrates from a chloride-saccharin bath at pH 3.8 and the effects of adding saccharin to the bath on the electrochemical deposition, corrosion resistance, chemical composition, physical and magnetic properties of the deposits were investigated. The analytical techniques of cyclic voltammetry (CV), potentiodynamic polarisation, electrochemical impedance spectroscopy (EIS), atomic absorption spectroscopy (AAS), atomic force microscopy (AFM), X-ray diffraction and hysteresis curves were applied to assess the codeposition process, and determine corrosion resistance, composition, morphology, nanocrystallinity and magnetic properties. Effectively, CV measurements revealed that the addition of saccharin in the electrolytic bath modifies the deposition process and an anomalous codeposition takes place; this enhanced the Co percentage in the Co–Ni deposits. Saccharin addition also increases the double layer capacitance and decreases the charge transfer resistance. On the other hand, the Tafel plots show a higher corrosion resistance for the deposits obtained from a bath with saccharin than those obtained from a bath without it. Furthermore, the presence of the saccharin in the bath also causes notable changes in the morphology and structure characteristics of deposits. In addition, it was found that the additive influences the magnetic properties of Co–Ni alloy thin films. The coercivity and magnetisation saturation are diminished for Co–Ni films prepared from electrolytes with addition of saccharin.     

Electrochemical performance of microarc oxidation films formed on AZ91D alloy in two group electrolytes

The phase composition and electrochemical performances of microarc oxidation（MAO） films prepared on AZ91D alloy by using step-down current method in a phosphate electrolyte（P-film） and silicate electrolyte（Si-film） were studied. The results show that P-film is mainly composed of Mg, MgAl2O4 and MgO, and Si-film is composed of Mg2SiO4 and MgO. There clearly exists a fluoride-enriched zone with the thickness of about 1 - 2 μm for P-film and 0.7 - 1μm for Si-film at the MAO coating/substrate interface. The electrochemical tests show that both P-film and Si-film can enhance the corrosion resistance of AZ91D magnesium alloy significantly. The corrosion failure process of the two films in 5% （mass fraction） NaCl solution is quite different.     

Influence of Gd and B on solidification behaviour and weldability of Ni–Cr–Mo alloy

Abstract

The influence of Gd and B on the solidification behaviour and weldability of Ni–Cr–Mo alloy UNS N06455 has been investigated by Varestraint testing, differential thermal analysis and microstructural characterisation. These alloys are currently being developed as structural materials for nuclear criticality control in applications requiring transportation and disposition of spent nuclear fuel owned by the US Department of Energy. The Gd containing alloys were observed to solidify in a manner similar to a binary eutectic system. Solidification initiated with a primary L→y reaction and terminated at ~1258°C with a eutectic type L→y+Ni₅Gd reaction. The solidification cracking susceptibility of the Gd containing alloys reached a maximum at ~1 wt-%Gd and decreased with both higher and lower Gd additions. Low cracking susceptibility at Gd concentrations below ~1 wt-% was attributed to a relatively small amount of terminal liquid that existed over much of the crack susceptible solid+liquid zone. Low cracking susceptibility at Gd concentrations above ~1 wt-% was attributed to a reduced solidification temperature range and backfilling of solidification cracks. The addition of B above the 230 ppm level leads to the formation of an additional eutectic type reaction at ~1200°C and the secondary phase within the eutectic type constituent was tentatively identified as Mo₃B₂. The B containing alloys exhibited a three step solidification reaction sequence consisting of primary L→y solidification, followed by the eutectic type L→y+Ni₅Gd reaction, followed by the terminal eutectic type L→y+Mo₃B₂ reaction. Boron additions had a strong, deleterious influence on solidification cracking susceptibility. The high cracking susceptibility was attributed to extension of the crack susceptible solid+liquid zone induced by the additional eutectic type L→y+Mo₃B₂ reaction and extensive wetting of the grain boundaries by the solute rich liquid. Simple heat flow equations were combined with solidification theory to develop a relation between the fraction liquid f _L and distance x within the solid+liquid zone. Information on the phenomenology of crack formation in the Varestraint test were coupled with the calculated f _L–x curves and were shown to provide useful insight into composition–solidification–weldability relations.     

Special features of using alloys of the iron–aluminium system for protective coatings of casting moulds

The effect of twin-arc surfacing conditions using aluminium and steel electrode wires on the chemical composition of deposited metal is investigated. The effect of the chemical composition on the mechanical and service properties of deposited layers is described and the efficiency of using intermetallic alloys of the iron–aluminium system as permanent protective coatings of casting moulds is confirmed.     

Electrochemical synthesis of a biomedically important Co–Cr alloy

Co–30 wt.% Cr alloy was prepared by electro-deoxidation in molten calcium chloride at 1123 K. A preliminary study was conducted into the preparation of the mixture of the Co₃O₄ and Cr₂O₃ and the formation of the non-stoichiometric, spinel structured, mixed oxide nominally labeled Co_xCr_yO₄. Constant voltage chronoamperometry was used both to prepare the alloy and to investigate its mechanism of formation. Electro-deoxidation proceeds by the simultaneous rapid reduction of CoO to Co and the slower reduction/substitution of Co_xCr_yO₄ to CaCr₂O₄ and Co metal. The final step of the electro-deoxidation is the reduction of CaCr₂O₄ to Cr metal, which alloys with the Co metal, and release of Ca²⁺ back into the electrolyte.     

FIB-SEM investigation on corrosion propagation of aluminium–lithium alloy in sodium chloride solution

Abstract

Microstructural characterisation of 2A97-T4 aluminium–lithium alloy was carried out using electron probe microanalysis and transmission electron microscopy (TEM). Scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy facilities has been employed to examine localised corrosion sites after immersion in sodium chloride solution. A dual beam microscope, which integrates a focused ion beam and an electron beam in one powerful instrument, has also been employed to investigate the development of intergranular corrosion from both surface and cross-section. It was found that localised corrosion is generally initiated at θ phase particles, which represents only 8.4% of the intermetallic (IM) particles in 2A97-T4 aluminium–lithium alloy. θ phase particles exhibit preferential dissolution of aluminium during corrosion testing, with trench formed at their periphery as well. Initiation of intergranular corrosion is relatively late with respect to the attack of IM particles. Owing to the presence of θ phase particles at intergranular corrosion sites and non-uniform distribution of T1 (Al₂CuLi) grain boundary precipitates, it is supposed that dealloyed θ phase particles and grain boundary precipitates cooperate to provide the driving force for grain boundary attack.     

Structure–property relationship of a spray formed Al–Y–Ni–Co alloy

The structure–property relationship of a spray formed Al–Y–Ni–Co alloy with two sets of processing conditions was investigated. Significant differences in tensile strength, yield strength, and high temperature ductility were observed with respect to the microstructural changes. Fracture toughness values were determined for both sets of specimens and found to be 7.5 and 5.8 MPa·m^1/2, respectively. Three intermetallic phases were observed in the matrix and constitute a volume fraction of approximately 75%. It is believed that the specimens failed during fracture toughness testing by the mechanism of cleavage, observed in the Al₃Y intermetallic particles.     

In-depth profiles of anodic oxide films on FeNi alloy in boric acid-sodium borate solutions

The in-depth profiling of anodic oxide films formed for 1 h on a 55Fe-45Ni alloy in boric acid-sodium borate solutions was made by the simultaneous use of AES (Auger Electron Spectroscopy) and sputter-etching with Ar⁺ ion to determine the thickness and composition of anodic oxide films and to elucidate the experimental variables which affect them. The anodic oxide film was thicker and richer in the Fe component in pH 6.48 solution than in pH 8.45 solution. It was estimated from the in-depth profile of the anodic oxide film that a significant part of the Fe component in the anodic oxide film was in the di-valent state. Enrichment of the Ni component at the oxide/substrate interface and depletion of Ni component in the film were measured as a function of pH and anodic potential. These results are explained in terms of the combination of the following factors: (i) preferential dissolution of the Fe component, (ii) preferential oxidation of the Fe component, and (iii) preferential anodic deposition of the Fe or Ni component.     

Friction welding of Al–Mg–Si alloy to Ni–Cr–Mo low alloy steel

Abstract

It is difficult to weld the dissimilar material combination of aluminium alloys and low alloy steels using fusion welding processes, on account of the formation of a brittle interlayer composed of intermetallic compound phases and the significant difference in physical and mechanical properties. In the present work an attempt has been made to join these materials via the friction welding method, i.e. one of the solid phase joining processes. In particular, the present paper describes the optimisation of friction welding parameters so that the intermetallic layer is narrow and joints of acceptable quality can be produced for a dissimilar joint between Al-Mg-Si alloy (AA6061) and Ni-Cr-Mo low alloy steel, using a design of experiment method. The effect of post-weld heat treatment on the tensile strength of the joints was then clarified. It was concluded that the friction time strongly affected the joint tensile strength, the latter decreasing rapidly with increasing friction time. The highest strength was achieved using the shortest friction time. The highest joint strength was greater than that of the AA6061 substrate in the as welded condition. This is due to the narrow width of the brittle intermetallic layer generated, which progressed from the peripheral (outer surface) region to the centreline region of the joint with increasing friction time. The joints in the as welded condition could be bent without cracking in a bend test. The joint tensile strength in the as welded condition was increased by heat treatment at 423 K (150° C), and then it decreased when the heat treatment temperature exceeded 423 K. All joints fractured in the AA6061 substrate adjacent to the interface except for the joints heated at 773 K (500° C). The joints fractured at the interface because of the occurrence of a brittle intermetallic compound phase.     

Characterization of oxide structures formed on nickel-chromium alloy during low pressure oxidation at 500–600°C

Low pressure oxidation studies of Ni-18%Cr alloy were carried out at temperatures of 500–600°C for very brief periods. Detailed XPS, AES, SEM, and TEM studies identified four stages in the initial oxidation. These are: (1) formation of a mixed nickel-chromium oxide overlayer; (2) growth of submicron-sized oxide nodules; (3) development of dark hole-like patches on the surface; and (4) growth of second generation oxide nodules. Both types of nodules consist primarily of a nickel structure depleted in oxygen. Their formation appears to result from a very rapid outward movement of nickel from localized defects in the metal. The dark patches result from the presence of a chromium oxide-rich underlayer, which appears to form by a lateral migration of chromium from adjacent oxide/metal interface regions and from grain boundaries.