The Morphology and Chemistry Evolution of Inclusions in Fe-Si-Al-O Melts

This study aims to elucidate the process of inclusion precipitation in Fe-Si and Fe-Si-Al melts. Deoxidation experiments were carried out in a vacuum induction furnace (VIF) at 1873 K (1600 °C). In the Si-deoxidation experiments, spherical SiO₂ of 1~2 μm diameter was dominant. When 3 wt pct Si and 300 ppm Al were added, such that Al₂O₃ and mullite were thermodynamically stable, the resulting inclusions depended on the addition sequence. When aluminum was added before silicon, spherical aluminum oxides were dominant after the Al addition, but after the Si addition, the number and size of alumina decreased and Al-Si oxides and mullite appeared with increasing time. When silicon was added before aluminum, spherical SiO₂ was dominant after the Si addition, but after the Al addition, spherical and polygonal alumina inclusions were dominant. When Al/Si was added simultaneously, polygonal alumina inclusions were dominant initially, but with time, Al-Si oxide and mullite inclusions increased in numbers. If the Al amount in the Al/Si addition was increased to 600 ppm, only alumina was found. This study shows how, under similar thermodynamic conditions, the transient evolution of inclusions in iron melts in the Si-Al-O system differ depending on the alloy addition sequence.     

Response to Thermal Exposure of Ball-Milled Aluminum-Borax Powder Blends

Aluminum-borax powder mixtures were ball milled and heated above 873 K (600 °C) to produce Al-B master alloys. Ball-milled powder blends reveal interpenetrating layers of deformed aluminum and borax grains that are increasingly refined with increasing milling time. Thermal exposure of the ball-milled powder blends facilitates a series of thermite reactions between these layers. Borax, dehydrated during heating, is reduced by Al, and B thus generated reacts with excess Al to produce AlB₂ particles dispersed across the aluminum grains starting at 873 K (600 °C). AlB₂ particles start to form along the interface of the aluminum and borax layers. Once nucleated, these particles grow readily to become hexagonal-shaped crystals that traverse the aluminum grains with increasing temperatures as evidenced by the increase in the size as well as in the number of the AlB₂ particles. Ball milling for 1 hour suffices to achieve a thermite reaction between borax and aluminum. Ball milling further does not impact the response of the powder blend to thermal exposure. The nucleation-reaction sites are multiplied, however, with increasing milling time and thus insure a higher number of smaller AlB₂ particles. The size of the AlB₂ platelets may be adjusted with the ball milling time.     

Reaction Pathways of Nanocomposite Synthesized in-situ from Mechanical Activated Al–C–TiO<Subscript>2</Subscript> Powder Mixture

In-situ Al matrix composite was synthesized from Al–TiO₂–C powder mixtures using mechanical alloying and heat treatment, subsequently. The effect of ball milling on reaction processes of the resulting nanocomposite was investigated. The evaluation of powder mixture without mechanical activation showed that at 900°C aluminum reduced TiO₂, forming Al₃Ti and Al₂O₃. After 20 h mechanical activation of powder mixture, Al₃Ti and Al₂O₃ were fabricated. After that, by increasing milling time up to 30 h, no new phases formed. The DTA analysis of 30 h milled powder indicated two peaks after aluminum melting at 730 and 900°C. The XRD results confirmed that at 730°C, molten Al reacted with TiO₂ and C, forming Al₃Ti, Al₂O₃ and Al₄C₃. After that, at 900°C, Al₃Ti reacted with Al₄C₃, causing TiC formation. This results proposed that the TiC formation is associated by a series of reactions between intermediate products, Al₃Ti and Al₄C₃ and the resultant nanocomposite was successfully synthesized after 30 h milling and heated by DTA analysis up to 1200°C.     

Carbothermic Reduction of Alumina by Natural Gas to Aluminum and Syngas: A Thermodynamic Study

The carbothermic reduction of alumina to aluminum by methane is analyzed by thermochemical equilibrium calculations in order to determine its thermodynamic constraints. Calculations predict that in the temperature range 2300–2500°C at 1 bar pressure, the reaction Al₂O₃ + 3CH₄ = 2Al +6H₂ + 3CO should occur without significant interference by the formation of unwanted byproducts such as Al₂O, Al₄C₃, and Al-oxycarbides, and with higher yields than by using solid carbonaceous compounds as reducing agent. The reaction was examined for several initial Al₂O₃/CH₄ molar ratios. The proposed process may be carried out in a fluidized bed reactor using concentrated solar energy, induction furnaces, or electric discharges as sources of high-temperature process heat. An important advantage of such a process would be the coproduction of syngas, with the molar ratio H₂/CO = 2, suitable for the synthesis of liquid hydrocarbon fuels and polymeric materials.     

Microstructural evolution at the bonding interface during the early-stage infrared active brazing of alumina

Infrared brazing of Al₂O₃ and alloy 42 using a silver-base active braze alloy was investigated at 900 °C for 0 to 300 seconds, with a heating rate of 3000 °C/min. Experimental results show that Ti₃(Cu, Al)₃O intermetallic with various amounts of Al is observed in the reaction layer and plays an important role in the early stage of reactive wetting. A two-layer structure is observed at the reaction interface brazed at 900 °C for 5 seconds. The reaction layer close to the alumina contains large amounts of Al, so the mass balance of the system is maintained. The growth of the reaction layer is not rate controlled by diffusion within the first 120 seconds. After 120 seconds, the rate controlling mechanism of the reaction layer becomes the diffusion control, satisfying the parabolic law. Dynamic wetting angle measurements using a traditional vacuum furnace at the heating rate of 10 °C/min demonstrate that the wetting angle rapidly decreases within the first 150 seconds, especially 0 to 80 seconds, and eventually stabilizes after 600 seconds.     

A Novel Bonding Method of Pure Aluminum and SUS304 Stainless Steel Using Barrel Nitriding

A great deal of research is being carried out on welding or bonding methods between iron and aluminum. However, it is not so easy to make Fe-Al bonding materials with both high strength and light weight. Recently, a new nitriding process has been proposed to produce aluminum nitride on an aluminum surface using a barrel. This study proposes a new concept in the production of a multilayer which has an AlN and Fe-Al intermetallic compound layer between the aluminum and steel using a barrel nitriding process. The bonding process was carried out from 893 K to 913 K (620 °C to 640 °C) for 18, 25.2, and 36 ks with Al₂O₃ powder and Al-Mg alloy powder. After the process, an aluminum nitride (AlN) layer and a Fe-Al intermetallic compound (Fe₂Al_5.4) layer were formed at the interface between the pure aluminum and SUS304 austenitic stainless steel. The thicknesses of the AlN layer and the intermetallic compound layer increased with increasing treatment temperature and time. The maximum hardnesses of the AlN layer and Fe₂Al_5.4 layers were found to be 377HV and 910HV, respectively, after barrel nitriding at 893 K (620 °C) for 18 ks.     

Solid-state reactions during heating mechanically milled Al/TiO<Subscript>2</Subscript> composite powders

Solid-state reactions between Al and TiO₂ during heating high-energy mechanically milled Al/TiO₂ composite powders have been investigated by using a combination of thermal analysis, X-ray diffraction (XRD), and various microstructural characterization techniques. When the TiO₂ particles and their interparticle spacing in the Al/TiO₂ composite powder particles are sufficiently large, the reaction between Al and TiO₂ proceeds by two steps. The low-temperature step is an interfacial reaction, which starts at a temperature close to 660 °C. The high-temperature step is a reaction facilitated by bulk diffusion and starts at a temperature above 820 °C. The first phase formed from the reaction is always Al₃Ti irrespective of the starting powder composition or milling time. Al₂O₃ is difficult to form at temperatures below 800 °C. The formation of the α-Ti(Al,O) phase proceeds slowly and requires either continuous heating to a temperature above 1000 °C or holding at a temperature close to 1000 °C for a period of time. Mechanical milling of the Al/TiO₂ powder enhances the interfacial reaction between Al and TiO₂. This enhancement is originated from the establishment and refinement of Al/TiO₂ composite microstructure.     

Microwave Heating, Isothermal Sintering, and Mechanical Properties of Powder Metallurgy Titanium and Titanium Alloys

This article presents a detailed assessment of microwave (MW) heating, isothermal sintering, and the resulting tensile properties of commercially pure Ti (CP-Ti), Ti-6Al-4V, and Ti-10V-2Fe-3Al (wt pct), by comparison with those fabricated by conventional vacuum sintering. The potential of MW sintering for titanium fabrication is evaluated accordingly. Pure MW radiation is capable of heating titanium powder to ≥1573 K (1300 °C), but the heating response is erratic and difficult to reproduce. In contrast, the use of SiC MW susceptors ensures rapid, consistent, and controllable MW heating of titanium powder. MW sintering can consolidate CP-Ti and Ti alloys compacted from ?100 mesh hydride-dehydride (HDH) Ti powder to ~95.0 pct theoretical density (TD) at 1573 K (1300 °C), but no accelerated isothermal sintering has been observed over conventional practice. Significant interstitial contamination occurred from the Al₂O₃-SiC insulation–susceptor package, despite the high vacuum used (≤4.0 × 10^?3 Pa). This leads to erratic mechanical properties including poor tensile ductility. The use of Ti sponge as impurity (O, N, C, and Si) absorbers can effectively eliminate this problem and ensure good-to-excellent tensile properties for MW-sintered CP-Ti, Ti-10V-2Fe-3Al, and Ti-6Al-4V. The mechanisms behind various observations are discussed. The prime benefit of MW sintering of Ti powder is rapid heating. MW sintering of Ti powder is suitable for the fabrication of small titanium parts or titanium preforms for subsequent thermomechanical processing.     

A Comprehensive Study of Diffusion Bonding of Mg AZ31 to Al 5754, Al 6061 and Al 7039 Alloys

In the present study, microstructural and mechanical properties of diffusion bonding of AZ31–Mg with Al 5754, Al 6061, and Al 7039 alloys were compared under same conditions. The vacuum diffusion processes were performed at a temperature of 440 °C, the pressure of 29 MPa, and a vacuum of 1?×?10^?4 torr for 60 min. The microstructural characterizations were investigated using optical microscopy and scanning electron microscopy equipped with EDS analysis and linear scanner. The XRD analysis was performed to study phase figures near the interface zone. The results revealed the formation of brittle intermetallic compounds like Al₁₂Mg₁₇, Al₃Mg₂, and their other combinations at bonding interfaces of all samples. Additionally, the hardness of Al alloys seemed to play a key role in increasing diffusion rate of magnesium atoms toward the aluminum atoms, with Al 6061 alloy having the highest diffusion rate. It consequently led to an increase in diffusion rate and thus formation of a strong diffusion bonding between magnesium and aluminum alloys. The highest strength was about 42 MPa for the diffusion bonding between Mg AZ31 and Al 6061. Further investigations on surfaces indicated that the brittle phases especially Al₃Mg₂ caused brittle fracturing.     

Transient liquid phase sintering of high density Fe3Al using Fe and Fe2Al5/FeAl2 powders Part 1: Experimentation and results

Abstract

High density Fe₃Al was produced through transient liquid phase sintering, using rapid heating rates of greater than 150 K min^-1 and a mixture of prealloyed and elemental powders. Prealloyed Fe₂Al₅/FeAl₂ (50Fe/50Al, wt-%) powder was added to elemental iron powder in a ratio appropriate for producing an overall Fe₃Al (13·87 wt-%) ratio. The heating rate, sintering time, sintering temperature, green density and powder particle size were controlled during the study. Heating rate, sintering time and powder particle size had the most significant influence upon the sintered density of the compacts. The highest sintered density of 6·12 Mg m^-3 (92% of the theoretical density for Fe3Al) was achieved after 15 minutes of sintering at 1350°C, using a 250 K min^{- 1} heating rate, 1-6 μm Fe powders and 5·66 μm alloy powders.

SEM microscopy suggests that agglomerated Fe₂Al₅/ FeAl₂ particles, which form a liquid during sintering, are responsible for a significant portion of the remaining porosity in high sintered density compacts, creating stable pores, larger than 100 μm diameter, after melting. High density was achieved by minimising the Kirkendall porosity formed during heating by unbalanced diffusion and solubility between the iron and Fe₂Al₅/FeAl₂ components. The lower diffusion rate of aluminium in the prealloyed powder into the iron compared with elemental aluminium in iron, coupled with a fast heating rate, is expected to permit minimal iron-aluminium interdiffusion during heating so that when a liquid forms the aluminium dissolves in the iron to promote solidification at a lower aluminium content. This leads to a further reduction in porosity.     

Interfacial Molten Reactivity of Aluminum in Contact with (0001) Al2O3 and (111) Al2MgO4 Single Crystal Surfaces

The present work studies (0001) Al₂O₃ and (111) Al₂MgO₄ wetting with pure molten Al by the sessile drop technique from 1073 K to 1473 K (800 °C to 1200 °C) under Ar at PO₂ 10^?15 Pa. Al pure liquid wets a smooth and chemically homogeneous surface of an inert solid, the wetting driving force (t,T) can be readily studied when surface solid roughness increases in the system. Both crystals planes (0001) Al₂O₃ and (111) Al₂MgO₄ have crystallographic surfaces with identical O^?2 crystalline positions however considering Mg²⁺ content in Al₂MgO₄ structure may influence a reactive mode. Kinetic models results under similar experimental conditions show that Al wetting on (0001) Al₂O₃ is less reactive than (111) Al₂MgO₄, however at >1273 K (1000 °C) (0001) Al₂O₃ transformation occurs and a transition of wetting improves. The (111) Al₂MgO₄ and Al system promotes interface formations that slow its wetting process.     

On the interaction between alumina batch and cryolite-alumina melt

The influence produced by the bulk density of alumina powder on the rate of its dissolution in a cryolite-alumina melt of the composition, wt %, 5.5 CaF₂, 1.5 MgF₂, 0.3 Al₂O₃, 2.28 CR is studied. The melt temperature is 950°C; the dissolution rate is determined visually and by changes in the concentration of aluminum oxide in the melt. It is discovered that the dissolution rate of alumina increases in proportion to its bulk density.     

Laser melting treatment by overlapping passes of preheated nickel electrodeposited coatings on Al−Si alloy

Microstructure improvements of a nickel electrodeposited Al−Si alloy were studied after high-power laser melting treatment through a single pass or partially overlapping successive adjacent passes. In some cases, laser melting treatment was preceded by a 5-hour heating of the specimens at 500°C in argon atmosphere furnace. Microstructure observations and microhardness measurements were carried out on the specimens before and after laser melting treatment with and without preheating. Best results concerning microhardness, microstructural homogeneity, and porosity elimination, as well as adhesion of the nickel coating on the Al−Si alloy, were achieved when the specimens were first subjected to heating at 500°C in an argon atmosphere furnace for 5 hours and then submitted to a laser melting treatment through successive adjacent laser passes with an overlapping rate of 70 pct. Microstructure studies were carried out employing X-ray diffraction analysis (XRD) and energy-dispersive spectrometry (EDS). AlNi and Al₃Ni phases were detected in the diffusion area which resulted from the 5-hour heating. AlNi, Al₃Ni, and Al₃Ni₂ phases were identified in the laser melted zones (LMZs). Each one of the above phase was found to be the main phase under different conditions.     

Study on Microstructures of Al-4 wt pct V Master Alloys

Aluminum (Al)-V master alloys have attracted attention, because they can potentially be efficient grain refiners for wrought aluminum alloys. In this paper, the microstructure and factors affecting the microstructure of Al-4 wt pct V master alloys were investigated by means of controlled melting and casting processes followed by structure examination. The results showed that the type and morphology of the V-containing phases in Al-V master alloys were strongly affected by the temperature of the melt, concentration of vanadium in solution in the melt and the cooling conditions. Two main V-containing phases, Al₃V and Al₁₀V, which have different shapes, were found in the alloys prepared by rapid solidification. The Al₃V phase formed when there were both a high temperature (1273 K to 1673 K (1000 °C to 1400 °C)) and a relatively high vanadium content of 3 to 4 wt pct, while the Al₁₀V phase formed at a low temperature (<1373 K (1100 °C)) or a low vanadium content in the range of 1 to 3 wt pct. The results also showed that the type of V-containing phase that formed in the Al-4 wt pct V master alloy was determined by the instantaneous vanadium content.     

The oxidation behavior of Ni-Cr-Al-2ThO2 alloys at 1093° and 1204°C

A pack diffusion process has been developed which permits the introduction of nearly 6 wt pct Al into solid solution in the near surface region of TDNiCr (Ni-20 wt pct Cr-2 vol pct ThO₂) and Ni-20Cr. Alumina scales, adherent under cyclic heating and cooling conditions, were produced on TDNiCr-5.86A1 upon exposure to an environment of 1.33 × 10³N/m² (10 torr) or 1.01 × 10⁵N/m² (760 torr) air at temperatures of 1093° and 1204°C. While the same oxidation kinetics were observed in isothermal tests for Ni-14.6Cr-5.86Al as were obtained for the TDNiCr-5.86A1, the dispersion strengthened alloy exhibited superior oxide scale adhesion during cyclic testing. At 1204°C continuous weight gains were observed under all test conditions for TDNiCr-5.86A1, in contrast to the weight loss with time which occurred several hours after exposure of TDNiCr to an oxidizing environment. TDNiCr with an initial aluminum surface concentration of 4.95 wt pct has nearly comparable oxidation resistance to the TDNiCr-5.86Al alloy. Specimens with 4.3 wt pct Al at the surface have inadequate aluminum to form Al₂O₃ scales, and weight losses are observed after 40 h upon exposure of these specimens to 1.01 × 10⁵N/m² (760 torr) air at 1204°C.     

Peculiarities of the technology and physicomechanical properties of a laminated Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al cermet

A technological approach permitting one to obtain laminated Al₂O₃-Al cermet is considered. The industrial PAP-2 powder with laminated particles served as the starting crude. The powder billets were obtained by compaction under pressure (P) from 100 to 1000 MPa and thermally treated in air by heating in the furnace to 600°C. It is established that either the solid-phase sintering or reaction sintering of the billets in the mode of filtration combustion can be achieved depending on the value of P. In the produced composite, the content of the oxide phase varies from 5 to 40%, while the density and strength upon bending vary in the limits 2.53–2.00 g/cm³ and 330-98 MPa, respectively. The laminated structure of the material is retained after thermal aging in air at t= 600°C for no less than 1000 h.     

Investigation into the Fabrication Possibility of the Boron–Aluminum Sheet Rolling of Increased Strength without Using Homogenization and Quenching

Al–Cu–Mn (Zr) aluminum alloys possess high strength and manufacturability without operations of thermal treatment (TT). In order to investigate the fabrication possibility of the aluminum boron-containing alloy in the form of sheet rolling with an increased strength without TT, Al–2% Cu–1.5% Mn–2% B and Al–2% Cu–1.5% Mn–0.4% Zr–2% B alloys are prepared. To exclude the precipitation of refractory boride particles, smelting is performed in a RELTEK induction furnace providing intense melt stirring. The smelting temperature is 950–1000°C. Pouring is performed into graphite molds 40 × 120 × 200 mm in size. It is established using computational methods (Thermo-Calc) that manganese forms complex borides with aluminum and zirconium at the smelting temperature; herewith, a sufficient amount of manganese remains in liquid, while zirconium is almost absent. The formation of AlB₂Mn₂ complex boride is proven; however, the amount of manganese remaining in the solid solution is sufficient to form the particles of the Al₂₀Cu₂Mn₃ phase in amounts of up to 7 wt %. Boron stimulates the isolation of Al₃Zr primary crystals in the alloy with zirconium; in connection with this, an amount of zirconium insufficient for hardening remains in the aluminum solid solution. The possibility of fabricating thin-sheet rolling with a thickness smaller than 0.3 mm with homogeneously distributed accumulations of the boride phase with a particle size smaller than 10 μm is shown. A high strength level (up to 543 MPa) is attained without using quenching and aging due to the precipitation of dispersoids of the Al₂₀Cu₂Mn₃ phase during hot deformation (t = 450°C).     

Microbial Beneficiation of Salem Iron Ore Using Penicillium purpurogenum

High alumina and silica content in the iron ore affects coke rate, reducibility, and productivity in a blast furnace. Iron ore is being beneficiated all around the world to meet the quality requirement of iron and steel industries. Choosing a beneficiation treatment depends on the nature of the gangue present and its association with the ore structure. The advanced physicochemical methods used for the beneficiation of iron ore are generally unfriendly to the environment. Biobeneficiation is considered to be ecofriendly, promising, and revolutionary solutions to these problems. A characterization study of Salem iron ore indicates that the major iron-bearing minerals are hematite, magnetite, and goethite. Samples on average contains (pct) Fe₂O₃-84.40, Fe (total)-59.02, Al₂O₃-7.18, and SiO₂-7.53. Penicillium purpurogenum (MTCC 7356) was used for the experiment. It removed 35.22 pct alumina and 39.41 pct silica in 30 days in a shake flask at 10 pct pulp density, 308 K (35 °C), and 150 rpm. In a bioreactor experiment at 2 kg scale using the same organism, it removed 23.33 pct alumina and 30.54 pct silica in 30 days at 300 rpm agitation and 2 to 3 l/min aeration. Alumina and silica dissolution follow the shrinking core model for both shake flask and bioreactor experiments.     

Investigation into the Possibility of Fabricating Boraluminum Rolling of Increased Strength without Homogenization and Quenching

Aluminum alloys of the Al–Cu–Mn (Zr) system possess high strength and manufacturability without heat treatment (HT). In order to investigate the possibility of fabricating an aluminum boron-containing alloy in the form of sheet rolling with increased strength without the HT, Al–2% Cu–1.5% Mn–2% B and Al–2% Cu–1.5% Mn–0.4% Zr–2% B alloys are prepared. To exclude the deposition of refractory boride particles, smelting is performed in a RELTEK induction furnace providing intense melt stirring. The smelting temperature is 950–1000°C. Pouring is performed into 40 × 120 × 200 mm graphite molds. It is established using computational methods (Thermo-Calc) that manganese forms complex borides with aluminum and zirconium at the smelting temperature and a sufficient amount of manganese remains in liquid, while zirconium is almost absent in it. The formation of AlB₂Mn₂ complex boride is proved experimentally (scanning electron microscopy and micro X-ray spectral analysis), but the amount of manganese remaining in the solid solution is sufficient to form particles of the Al₂₀Cu₂Mn₃ phase in an amount reaching 7 wt %. Boron in the zirconium-containing alloy stimulates the isolation of primary crystals Al₃Zr, in connection with which an insufficient amount of zirconium remains in the aluminum solid solution for strengthening. The possibility of fabricating thin-sheet rolling smaller than 0.3 mm in thickness with uniformly distributed agglomerations of the boride phase with a particle size smaller than 10 µm is shown. A high level of strength (up to 543 MPa) is attained with no use of quenching or aging due to the isolation of dispersoids of the Al₂₀Cu₂Mn₃ phase during hot deformation (t = 450°C).