The Effect of Excess Aluminum on the Composition and Microstructure of Nb-Al Alloys Produced by Aluminothermic Reduction of Nb2O5

Intermetallic aluminides including those phases of the Nb-Al system are of interest for high-temperature structural applications. Through aluminothermic reduction (ATR) of Nb₂O₅ different alloys of the Nb-Al system can be produced by varying the amount of aluminum (excess aluminum) in the thermit charge. In this work, various Nb-Al alloys were produced by varying Nb₂O₅ and Al powder blends. The resulting alloys were characterized by chemical analysis (Al, O, and C), X-ray diffraction and scanning electron microscopy. The aluminum content of the alloys increased linearly from 14.5 to 50.4 at% as the excess Al was varied from 10 up to 60% over the stoichiometric amount to reduce the Nb₂O₅. The carbon content was lower than 300 wt-ppm. The oxygen content decreases with increasing excess Al, reaching 1300 wt-ppm for the alloy produced with 60% excess Al. The inclusion content (Al₂O₃) decreases significantly as the excess Al is increased. The following metallic phases were identified in the alloys: Nb_ss (niobium solid solution) and Nb₃Al (alloy produced with 10% excess Al); Nb₃Al (alloys produced with 15 and 20% excess Al); Nb₃Al, Nb₂Al, and NbAl₃ (alloy produced with 30% excess Al); and Nb₂Al and NbAl₃ (alloys produced with 40, 50, and 60% excess Al).     

Characterisation of two Al–Fe based high temperature alloy powders

Abstract

Aluminium alloys containing additions of iron and cerium are among the alloys being developed as potential replacements for titanium based alloys for moderately high temperature applications. Development of these alloys is possible using rapid solidification technology, which results in a very fine distribution of dispersoids in the aluminium matrix. The microstructures of two rapidly solidified high temperature alloy powders of composition (wt-%) Al–6·7Fe–5·9Ce (alloy A) and Al–6·2Fe–5·9Ce–1·63Si (alloy B) have been characterised using transmission electron microscopy and the results are explained on the basis of some of the major solidification parameters, such as nucleation undercooling and recalescence. It was observed that most of the powder particles in the +10 to ?20 μm size range contained both microcellular and cellular regions, which could be explained in terms of an initial large undercooling followed by recalescence. The decomposition of the powder microstructure after exposing the powders to temperatures of 350, 420, and 500°C for 1 h was investigated using transmission electron microscopy. This work was complemented by phase identification studies using X-ray diffraction. The equilibrium precipitates Al₁₃Fe₄, Al₈Fe₂Si, and Al₃FeSi were detected in the powder microstructure of alloy B, whereas Al₁₃Fe₄ precipitates were detected in alloy A after high temperature exposure (500°C).

MST/1571     

Effect of Al and C on structure and mechanical properties of Fe–Al–C alloys

Abstract

Effect of aluminium and carbon content on the microstructure and mechanical properties of Fe–Al–C alloys has been investigated. Alloys were prepared by combination of air induction melting with flux cover (AIMFC) and electroslag remelting (ESR). The ESR ingots were hot forged and hot rolled at 1373 K. As rolled alloys were examined using optical microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to understand the microstructure of these alloys. The ternary Fe–Al–C alloys containing 10·5 and 13 wt-%Al showed the presence of three phases: FeAl with disordered bcc structure, Fe₃Al with ordered DO₃ structure and Fe₃AlC_0·5 precipitates with L′1₂ structure. Addition of high concentration of carbon to these alloys resulted in excellent hot workability and superior tensile at room temperature as well as tensile and creep properties at 873 K. An increase in Al content from 9 to 13 wt-% in Fe–Al–C alloys containing the same levels of carbon has no significant influence on strength and creep properties at 873 K, however resulted in significant improvement in room temperature strength accompanied by a reduction in room temperature ductility.     

The chemical behaviour of carbon fibres in magnesium base Mg-Al alloys

The chemical interaction between carbon fibres and Mg-rich Mg-Al alloys was studied at 723–1273 K using optical metallography, scanning electron microscopy and electron probe microanalysis. In a first stage, carbon fibres were heated at 723, 1000 and 1273 K with Mg-Al alloys of different compositions. Two carbide phases were identified at 1000 and 1273 K: an Al₄C₃ type phase with up to 6 wt.%Mg present in solid solution and a new ternary carbide with the chemical formula Al₂MgC₂ existing under two hexagonal crystalline varieties. In a second stage, the solid-liquid phase equilibria in the Al-C-Mg ternary system were experimentally established at 1000 K. At that temperature, all the Mg-Al alloys containing more than 19 ± 2 wt.%Al were observed to be in equilibrium with the Al₄C₃ type phase whereas Mg-Al alloys containing from 0.6 to 19 wt.%Al were found in equilibrium with the ternary carbide Al₂MgC₂. As for the Mg-Al alloys with an Al content lower than or equal to 0.6 ± 0.2 wt.%, they appeared to be in equilibrium with carbon. These thermodynamic principles being established, the extent, morphology and composition of the reaction zones formed in out of equilibrium conditions at the interface between carbon fibres and Mg-rich Mg-Al alloys were characterized. Attempts were made to determine the influence of different factors such as the fibre nature, the alloy composition, the heating time and the heating temperature on the formation and growth of the ternary carbide Al₂MgC₂. The observed changes were interpreted in terms of reaction mechanism and kinetics.     

Development of corrosion resistant magnesium alloys Part 1 Characterisation of splat quenched Mg–10Al and Mg–16Al alloys

Abstract

The surfaces and bulk of splat quenched Mg–10Al and Mg–16Al (wt-%) alloys were investigated. The surfaces were studied using X-ray photoelectron spectroscopy (XPS) , X-ray excited Auger electron spectroscopy (X-AES), Rutherford backscattering spectrometry (RBS) , scanning electron microscopy (SEM), and electron probe microanalysis (EPMA) and the bulk using X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. The solid solubility of Al in Mg was extended to at least 16 wt-%. The quantity of Al ions present on the surfaces of the alloys increased with Al content. Contrary to the suggested layered MgO/Mg–Al–oxide/alloy structure, the surfaces of the alloys consisted of an admixture of magnesium spinel (MgAl₂O₄) in periclase (MgO) and brucite (Mg(OH)₂) of non-uniform thickness varying between 10 and 50 nm, determined via RBS, X-AES, and depth profiling using XPS.

MST/1714a     

Design of powder metallurgy aluminium alloys for applications at elevated temperatures Part 1 Microstructure of high pressure gas atomized powders

Abstract

A method is described for designing powder metallurgy rapidly solidified aluminium alloys using experimental and/or calculated nucleation maps which give the microstructure of gas atomised powders as a function of powder particle size and alloy composition. This method was used to predict the compositions of Al–Cr–Zr–Mn alloys for which the <45 μm sizefraction of the gas atomised powders exhibits a microstructure with or without Al₁₃Cr₂ intermetallic particles. Powders were produced by high pressure gas atomisation and were examined using analytical electron microscopy. The microstructures observed were in excellent agreement with those predicted. The powders exhibited four distinct microstructures with increasing powder particle diameter: (i) segregation free, (ii) cellular α aluminium, (iii) α aluminium plus fine spherical precipitates rich in chromium and manganese, and (iv) α aluminium plus Al₁₃Cr₂ primary intermetallic particles. The solidification of these powders is discussed in terms of solidification front velocity controlled by external heat flow and by the initial undercooling. Particles less than 10 μm in diameter undercool significantly before solidification. Segregation free microstructures occur in the fine <1 μm) particles, where the solidification front velocity exceeds the absolute stability velocity.

MST/1247a     

The morphology of martensite in Fe-C,Fe-Ni-C and Fe-Cr-C alloys

The morphology of martensite in widely varying series of Fe-C, Fe-Ni-C and Fe-Cr-C alloys was investigated using optical microscopy. The effects of formation temperature and alloying elements on the martensite morphology were studied in detail. It was found that in Fe-C alloys, lath martensite forms in alloys with less than 0.8wt% carbon, butterfly martensite forms in alloys with between 0.98 and 1.42wt% carbon and lenticular martensite forms in alloys with more than 1.56wt% carbon. In Fe-Ni-C alloys, four different martensite morphologies form depending upon the formation temperature and composition, and for alloys of a fixed carbon content the martensite morphology changes from lath to butterfly to lenticular to thin plate as the formation temperature is decreased. In Fe-Cr-C alloys, lath martensite forms at high temperature, and below the lath formation temperature mainly {2 2 5}_f plate martensite is formed. Based on the results obtained, the importance of the strength of austenite, and the austenite stacking fault energy to the martensite morphology was discussed.     

Interface microstructures in diffusion bonding of titanium alloys to stainless and low alloy steels

Abstract

Commercial purity Ti and a Ti 6242 alloy have been diffusion bonded to an AISI 316L stainless steel and an AISI 4130 low alloy steel. The microstructures of the as processed products have been analysed using optical metallography, scanning electron microscopy (SEM), and scanning transmission electron microscopy (STEM) techniques. The interdiffusion of the different elements through the interface has been determined using energy dispersive spectroscopy microanalysis in both a SEM and a STEM. For the combinations AISI 316L–commercially pure Ti and AISI 316L–Ti 6242 several regions surrounding the original interface have been observed. Starting from the 316L side, first a α phase is observed, followed by an Fe₂ Ti intermetallic, an FeTi intermetallic, and finally an Fe₂Ti₄O oxide just before the Ti and Ti 6242. Because the diffusion ofTi in Fe is faster than the diffusion of Fe in Ti, a Kirkendall effect is produced. In the AISI 4130–Ti 6242 combination a thin layer of TiC is observed at the interface, limiting the interdiffusion of elements.

MST/1746     

Capability of mechanical alloying and SPS technique to develop nanostructured high Cr,Al alloyed ODS steels

Abstract

Oxide dispersion strengthened (ODS) Fe alloys were produced by mechanical alloying (MA) with the aim of developing a nanostructured powder. The milled powders were consolidated by spark plasma sintering (SPS). Two prealloyed high chromium stainless steels (Fe–14Cr–5Al–3W) and (Fe–20Cr–5Al+3W) with additions of Y₂O₃ and Ti powders are densified to evaluate the influence of the powder composition on mechanical properties. The microstructure was characterised by scanning electron microscope (SEM) and electron backscattering diffraction (EBSD) was used to analyse grain orientation, grain boundary geometries and distribution grain size. Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) equipped with energy dispersive X-ray spectrometer (EDX) were used to observe the nanostructure of ODS alloys and especially to observe and analyse the nanoprecipitates. Vickers microhardness and tensile tests (in situ and ex situ) have been performed on the ODS alloys developed in this work.     

Structural and Phase Transformations in Alloys during Spark Plasma Sintering of Ti + 23.5 at % Al + 21 at % Nb Powder Mixtures

We have studied the effect of sintering temperature on the structural and phase transformations of alloys produced by the spark plasma sintering of Ti + 23.5 at % Al + 21 at % Nb powder mixtures at temperatures in the range 1100–1550°C. The sintered alloys have been characterized by X-ray diffraction, scanning electron microscopy, and energy dispersive X-ray spectroscopy (elemental X-ray mapping). The alloys sintered at temperatures of 1100 and 1200°C have been shown to have a nonuniform microstructure. According to electron microscopy results, the alloys consist of grains of the α₂ and Nb₂Al phases and small precipitates of the O-phase (intermetallic compound Ti₂AlNb). In addition, there are particles of unreacted niobium and titanium. The alloys sintered at a temperature of 1300°C have a uniform lamellar structure.     

A comparative study of Inconel 625 laser cladding by wire and powder feedstock

It has been established that laser cladding technique is useful for enhancing surface performances, hence extending the life of many components in severe corrosive-wear environments. However, a comparative study of the surface performances of laser coatings made via powder and wire feeding systems has not been performed. Inconel 625 powder and wire were deposited on the AISI 304 substrate using similar processing parameters. The microstructure, together with the depth of substrate penetration and the degree of dilution of the deposited tracks, was examined using an optical microscope and a scanning electron microscope (equipped with an energy-dispersive spectrometer). The micro-hardness was measured using a Vickers hardness tester. At optimized parameters, laser tracks of Inconel 625 wire and powder had a strong metallurgical bond at the track–substrate interface and no crack and pore were deposited. Due to the higher laser beam infiltration and a larger depth of substrate penetration, higher substrate dilution was observed in the powder-fed tracks. The tracks comprise continuous ?-matrix and secondary compounds (rich in Nb and Mb). However, finer dendritic microstructure and higher number density of inter-dendritic precipitates were observed in a typical powder laser track compared with the corresponding wire laser track. The typical powder laser track demonstrated higher hardness (245 HV_0.3) compared with the corresponding wire laser track (224 HV_0.3).     

Properties of magnesium alloys reinforced with nanoparticles and carbon nanotubes: a review

Magnesium alloys suffer from only moderate high-temperature strength and creep resistance. Aluminium-free magnesium alloys for sand casting or alloys containing aluminium with expensive additional alloying elements may be in use, but only microparticle or microfibre-reinforced magnesium alloys really exhibit satisfactory creep strengths at temperatures up to 250 °C. Reinforcing magnesium alloys with ceramic nanoparticles could be a solution for preserving a low density while increasing the high-temperature performance. When produced using melting processes, nanoparticle-reinforced magnesium composites are expected to enjoy strengthening due to the grain refinement described in the Hall–Petch relation. When an isotropic distribution of nanoparticles is achieved, the composites are additionally expected to be Orowan-strengthened. In this review, a variety of ceramic materials, such as SiC, Al₂O₃, Y₂O₃, SiO₂ and carbon nanotubes were investigated for reinforcement. Pure magnesium and various magnesium alloys were chosen as the matrix material and both powder metallurgical (PM) and melting processes were used for production of the composites. The mechanical properties of the composites were generally enhanced, compared to an unreinforced alloy; not only at room temperature, but also at elevated temperatures. In some cases an increase in strength in combination with increased ductility was also identified.     

Low temperature specific heat of two stainless steels

Stainless steel is often used as a structural material in ctrygenic systems. For many large-scale, low temperature applications, knowledge of specific heat values for such alloys is essential for proper design. Collings et al¹ have recentky made calorimetric measurements on AISI 310S stainless steel. These measurements indicate the occurence of superparamagnetism, presumably associated with magnetic clusters, by a temperature-independent contribution to the specific heat. Corsan and Mitchen² have recently reported specific heat measurement form 4 K to room temperature on a series of laboratory-produced FeCrNi alloys with chromium contents ranging from 12–24 wt.% and nickel contents int he range 12–20 wt.% Differences of up to 30% were observed in the specific heats as measured at 4 K. However, to the best of our knowledge, no data previously existed on the most common low temperature structural stainless steel—AISI 304. This note describes the results of low temperature specific heat measurements on AISI 304 abd AISI 304L stainless. L designated low carbon content.     

Tribological Studies of a Zr‐Based Glass‐Forming Alloy with Different States

The tribological characteristics of a glass‐forming alloy, Zr_52.5Cu_17.9Ni_14.6Al_10.0Ti_5.0, in atomic percent (at.%, Vit 105), with different microstructural states have been investigated. Friction and wear studies were conducted using a ball‐on‐flat reciprocating sliding apparatus against an AISI E52100 bearing steel under dry condition. The observed wear resistance in an ascending order is: the deformed, creep‐tested, and as‐cast states. Wear analyses suggested that the wear processes of glass‐forming alloys involved abrasion, adhesion, and oxidation. The differences in hardness, free volume, and brittleness in different states significantly affected the friction and wear behaviors of the glass‐forming alloys.     

Mechanism of production of ultra-fine silicon carbide powder by arc plasma irradiation of silicon bulk in methane-based atmospheres

The mechanism of production of ultra-fine SiC powder from a silicon bulk by arc plasma irradiation in either an Ar + CH₄ + H₂ or an Ar + CH₄ atmosphere was studied. Layer and island phases were newly formed in the silicon bulk upon irradiation, and it was revealed from scanning electron and Auger electron spectroscopy that these phases were composed of SiC. The intensity of the X-ray diffraction peaks due to the SiC phase increased with irradiation time almost in parallel to the carbon content involved in the silicon bulk. It is proposed that CH₄ is dissociated in the arc plasma and dissolved in the molten silicon bulk to produce the SiC phase, the sublimation of which is mostly responsible for the production of ultra-fine SiC powder.     

Shape memory characteristics and mechanical properties of high-density powder metal TiNi with post-sintering heat treatment

Through the use of fine titanium and nickel elemental powders and persistent liquid phase sintering, a high density powder metal Ti₅₁Ni₄₉ with a high phase transformation temperature and enthalpy, and narrow transformation hysteresis, which are comparable to those of wrought TiNi alloys, are produced. However, due to the presence of a semi-continuous Ti₂Ni network, the shape recovery and tensile properties in the martensitic state at room temperature, determined using bending tests, are lower than those of cast TiNi counterparts. Through hot isostatic pressing and annealing above the peritectic temperature for sintered specimens, these properties are improved due to the increase in density and spheroidization of the Ti₂Ni compound. The phase transformation temperature and enthalpy are also enhanced due to the continuing carbon absorption by the Ti₄Ni₂X (X = C, O) phase, which decreases the carbon content in the TiNi matrix.     

Development of microstructure in laser surface alloying of steel with chromium

Laser surface alloying (LSA) was used to formin situ Fe-Cr-C alloys on AISI 1018 steel substrates. Chromium powders of different particle sizes were mixed together to obtain optimum packing density of the powder deposited on the substrate. The surface was then melted using a 2kW CW carbon dioxide laser. The processing conditions were related to solute (chromium) content, microstructural refinement of the laser alloyed zone and the heat affected zone (HAZ). The microstructure of the laser surface alloyed region was investigated by optical, scanning and transmission electron microscopy, and X-ray microanalysis techniques. Microstructural study showed a high degree of grain refinement and an increase in solid solubility of alloying element. This process produced a fine distribution of complex type of carbide precipitate in the martensite-ferrite matrix because of the high cooling rate. An alloy of this composition does not show any retained phase. The nature of alloying and chemical diffusion profile as a function of intertrack separation distance affects the final content of alloying element in the surface layer.     

Chemical stability of carbon nanotubes in the 2024Al matrix

Five volume percent of carbon nanotubes and 2024Al alloy powder were mixed with ball milling method, and then the composite was fabricated at 873 K by hot pressing sintering technique. The microstructure of the composite was investigated using optical microscopy, transmission electron microscopy, and X-ray diffraction. The experimental results showed that carbon nanotubes are reacted and changed into Al₄C₃. Nano-Al₄C₃ phases with needle shape are distributed mainly on Al grain boundaries; meanwhile some of them exist within Al grains. The reaction mechanism of carbon nanotubes-Al is discussed.     

Determining of laser surface treatment parameters used for light metal alloying with ceramic powders

There are presented in this paper the investigation results of microstructure as well hardness investigation of the surface layer of cast aluminium alloys in as‐cast state and after laser surface treatment using a high power diode laser (HPDL) with Al₂O₃ ceramic powder. The purpose of this work was to determine the proper laser treatment conditions for surface treatment of the investigated alloys and to describe the structural changes occurred in the surface layer after laser treatment. For investigation of the obtained structure there was used light as well scanning and transmission electron microscopy. The morphology and size of the ceramic powder particles as well the structure of the remelted aluminium surface layer was possible to determine. After the laser surface treatment carried out on the aluminium cast alloys there are visible structural changes concerning the microstructure as well as distribution and morphology of the fed particles occurred in the sample surface. Concerning the laser treatment conditions for surface hardening also the laser power and ceramic powder feed rate was studied. The structure of the surface laser tray changes in a way, that there are zones detected like the remelting zone and the heat influence zone. This investigation with appliance of a high power diode laser for Al alloys makes it possible to obtain or develop an interesting technology very attractive for different industry branches.     

Microwave-assisted synthesis of ceria nanoparticles

Nanocrystalline ceria (CeO₂) particles have been successfully prepared by microwave-assisted heating technique from an aqueous solution containing ammonium Ce(IV) nitrate and sodium hydroxide. Further thermal treatment of the as-prepared powder at 500 °C resulted in the formation of the well-crystallized CeO₂ nanoparticles with an average crystal size of about 8 nm, varying with the heating temperature. The as-prepared powder and the CeO₂ nanoparticles were examined using X-ray diffraction (XRD) and transmission electron microscope (TEM) techniques. It was found that the morphologies of the synthesized powder show from rod-like for the as-prepared sample to sphere-like for the heat-treated nanoparticles. Mechanism of CeO₂ nanocrystallite growth during annealing is primarily investigated.