Effect of Cold Rolling on as–ECAP Interstitial Free Steel

Ti-stabilized interstitial free steel subjected to eight passes, route B_C room temperature equal channel angular pressing (ECAP) additionally was cold rolled (CR) up to 95 pct thickness reduction. Electron back-scattering diffraction and transmission electron microscopy characterized microstructural refinement and microtexture evolution, whereas the mechanical properties were assessed by uniaxial tensile tests. After 95 pct CR, the average high-angle grain boundary spacing reduces to 0.14 μm, whereas the high-angle boundary fraction increases to ~81 pct. The ECAP negative simple shear texture components rotate by ~15 deg around the transverse direction toward the rolling direction for up to 50 pct CR, with typical rolling textures observed at 95 pct CR. The decrease in boundary spacing produces a ~500 MPa gain in 0.2 pct proof stress, a ~600 MPa increase in ultimate tensile strength (UTS), and a ~4 pct loss in total elongation after 95 pct CR. Similar rates of decrease in work hardening correspond to comparable rates of cross and/or multiple slip events irrespective of the processing regime and substructural refinement. The fracture mode of the tensile samples changes from ductile to brittle type between ECAP and 95 pct CR and is attributed to the reduced work hardening capacity of the latter. The modified Hall–Petch equation shows that the convergence of high-angle boundary spacing values with their low-angle counterparts results in an increased contribution via boundary strengthening to the 0.2 pct proof stress and UTS.     

Tensile and Fracture Properties of Cast and Forged Composite Synthesized by Addition of Al-Si Alloy to Magnesium

Cast Mg-Al-Si composites synthesized by addition of Al-Si alloy containing 10, 15, and 20 wt pct of Si, in molten magnesium, to generate particles of Mg₂Si by reaction between silicon and magnesium during stir casting has opened up the possibility to control the size of these particles. The microstructure of the cast composite consists of relatively dark polyhedral phase of Mg₂Si and bright phase of β-Al₁₂Mg₁₇ along the boundary between dendrites of α-Mg solid solution. After hot forging at 350 °C, the microstructure has changed to relatively smaller sizes of β-Al₁₂Mg₁₇ and Mg₂Si particles apart from larger grains surrounded by smaller grains due to dynamic recovery and recrystallization. Some of the Mg₂Si particles crack during forging. In both the cast and forged composite, the Brinell hardness increases rapidly with increasing volume fraction of Mg₂Si, but the hardness is higher in forged composites by about 100 BHN. Yield strength in cast composites improves over that of the cast alloy, but there is a marginal increase in yield strength with increasing Mg₂Si content. In forged composites, there is significant improvement in yield strength with increasing Mg₂Si particles and also over those observed in their cast counterpart. In cast composites, ultimate tensile strength (UTS) decreases with increasing Mg₂Si content possibly due to increased casting defects such as porosity and segregation, which increases with increasing Mg₂Si content and may counteract the strengthening effect of Mg₂Si content. However, in forged composite, UTS increases with increasing Mg₂Si content until 5.25 vol pct due to elimination of segregation and lowering of porosity, but at higher Mg₂Si content of 7 vol pct, UTS decreases, possibly due to extensive cracking of Mg₂Si particles. On forging, the ductility decreases in forged alloy and composites possibly due to the remaining strain and the forged microstructure. The initiation fracture toughness, J _IC , decreases drastically in cast composites from that of Mg-9 wt pct. alloy designated as MA alloy due to the presence Mg₂Si particles. Thereafter, J _IC does not appear to be very sensitive to the increasing presence of Mg₂Si particles. There is drastic reduction of J _IC on forging of the alloy, which was attributed to the remaining strain and forged microstructure, and it is further lowered in the composites because of cracking of Mg₂Si particles. The ratio of the tearing modulus to the elastic modulus in cast composites shows a lower ratio, which decreases with increasing Mg₂Si content. The ratio decreases comparatively more on forging of cast MA alloy than those observed in forged composites.     

Effect of Combined Addition of Cu and Aluminum Oxide Nanoparticles on Mechanical Properties and Microstructure of Al-7Si-0.3Mg Alloy

In this study, an ultrasonic cavitation based dispersion technique was used to fabricate Al-7Si-0.3Mg alloyed with Cu and reinforced with 1 wt pct Al₂O₃ nanoparticles, in order to investigate their influence on the mechanical properties and microstructures of Al-7Si-0.3Mg alloy. The combined addition of 0.5 pct Cu with 1 pct Al₂O₃ nanoparticles increased the yield strength, tensile strength, and ductility of the as-cast Al-7Si-0.3Mg alloy, mostly due to grain refinement and modification of the eutectic Si and θ-CuAl₂ phases. Moreover, Al-7Si-0.3Mg-0.5Cu-1 pct Al₂O₃ nanocomposites after T6 heat treatment showed a significant enhancement of ductility (increased by 512 pct) and tensile strength (by 22 pct). The significant enhancement of properties is attributed to the suppression of pore formation and modification of eutectic Si phases due to the addition of Al₂O₃ nanoparticles. However, the yield strength of the T6 heat-treated nanocomposites was limited in enhancement due to a reaction between Mg and Al₂O₃ nanoparticles.     

Evaluating the Diffusion Coefficient of Sulfur in Low-Silica CaO-SiO<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Slag

The chemical diffusion coefficient of sulfur in the ternary slag of composition 51.5 pct CaO-9.6 pct SiO₂-38.9 pct Al₂O₃ slag was measured at 1680 K, 1700 K, and 1723 K (1403 °C, 1427 °C, and 1450 °C) using the experimental method proposed earlier by the authors. The P_\textS2 P_{{{\text{S}}_{2} }} and P_\textO2 P_{{{\text{O}}_{2} }} pressures were calculated from the Gibbs energy of the equilibrium reaction between CaO in the slag and solid CaS. The density of the slag was obtained from earlier experiments. Initially, the order of magnitude for the diffusion coefficient was taken from the works of Saito and Kawai but later was modified so that the concentration curve for sulfur obtained from the program was in good fit with the experimental results. The diffusion coefficient of sulfur in 51.5 pct CaO-9.6 pct SiO₂-38.9 pct Al₂O₃ slag was estimated to be in the range 3.98 to 4.14 × 10⁻⁶ cm²/s for the temperature range 1680 K to 1723 K (1403 °C to 1450 °C), which is in good agreement with the results available in literature     

Effect of strontium on the microstructure, mechanical properties, and fracture behavior of AZ31 magnesium alloy

The effect of strontium (Sr) on the microstructure, mechanical properties, and fracture behavior of AZ31 magnesium alloy and its sensitivity to cooling rate are investigated. Three phases—blocky-shaped Mg₁₇Al₁₂, acicular Mg₂₀Al₂₀Mn₅Sr, and insular Mg₁₆(Al,Zn)₂Sr—are identified in the Sr-containing AZ31 alloys. With increasing cooling rate, the blocky-shaped Mg₁₇Al₁₂ phase increases, the acicular Mg₂₀Al₂₀Mn₅Sr phase diminishes, and the insular Mg₁₆(Al,Zn)₂Sr phase is refined and granulated. The study suggests that the grain size decreases with increasing cooling rate for a given composition. However, the grain size decreases first, then increases, and finally decreases again with increasing Sr for a given cooling rate. The yield strength (σ _y ) of AZ31 magnesium alloy can be improved by grain refinement and expressed as σ _y =35.88+279.13d ^−1/2 according to the Hall-Petch relationship. The elongation increases when Sr is added up to 0.01 pct and then decreases with increasing Sr addition. Grain refinement changes the fracture behavior from quasicleavage failure for the original AZ31 alloy to mixed features of quasicleavage and microvoid coalescence fracture.     

Effect of Compositional Variation on the Microstructural Evolution and the Castability of Al–Mg–Si Ternary Alloys

This study examined the microstructural evolution and castability of Al–Mg–Si ternary alloys with varying Si contents. Al–6Mg–xSi alloys (where x = 0, 1, 3, 5, and 7; all compositions in mass pct) were examined, with Al–6 mass pct Mg as a base alloy. The results showed that in the ternary alloys with Si ≤ 3 pct, the solidification process ended with the formation of eutectic α-Al–Mg₂Si phases generated by a univariant reaction. However, in the case of ternary alloys with Si > 3 pct, solidification was completed with the formation of α-Al–Mg₂Si–Si ternary eutectic phases generated by a three-phase invariant reaction. In addition to the eutectic Mg₂Si phases, the primary Mg₂Si phases formed in each of the ternary alloys, and the size of both sets of phases increased with increasing Si content. The two-phase eutectic α-Al–Mg₂Si nucleated from the primary Mg₂Si phases. The inoculated Al–6Mg–1Si alloy had the smallest grain size. Moreover, the grain-refining efficacy of the Al–5Ti–B master alloy in the ternary alloys decreased with increasing Si content in the alloys. Despite the poisoning effect of Si on the potency of TiB₂ compounds in the inoculated Al–6Mg–1Si alloy, the grain size of the alloy was slightly smaller than that of the Al–6Mg binary alloy. This resulted from the increasing growth restriction factor (induced by Si addition) of the Al–6Mg–1Si alloy. In terms of the castability, the examined alloys showed different levels of susceptibility to hot tearing. Among the alloys, the ternary Al–6Mg–5Si alloy exhibited the highest susceptibility to hot tearing, whereas the Al–6Mg–7Si exhibited the lowest. The severity of hot tearing initiated by the unraveling of the bifilm was determined by the freezing range, grain size, and the amount of eutectic phases at the end of the solidification process.

     

Separation of Antimony from a Stibnite Concentrate Through a Low-Temperature Smelting Process to Eliminate SO<Subscript>2</Subscript> Emission

The main purpose of this study is to characterize and separate antimony from a stibnite concentrate through a low-temperature sulfur-fixing smelting process. This article reports on a study conducted on the optimization of process parameters, such as flux and zinc oxide weight percentage, in charging, smelting temperature, smelting duration on the antimony yield, resultant crude antimony grade, and sulfur-fixing rate. A maximum antimony recovery of 97.07 pct, crude antimony grade of 96.45 pct, and 98.61 pct sulfur-fixing rate are obtained when a charge (containing 63.20 wt pct of flux and 21.30 wt pct of stibnite, a flux composition of W_\textNaOH /W_{\textNa 2 \textCO3} W_{\text{NaOH}} /W_{{{\text{Na}}_{ 2} {\text{CO}}_{3} }} = 10/147, where W represents weight, and more than 10 pct of the stoichiometric requirement of zinc oxide dosage) is smelted at 1153 K (880 °C) for 120 minutes. This smelting operation is free from atmospheric pollution because zinc oxide is used as the sulfur-fixing agent. The solid residue is subjected to mineral dressing operation to obtain suspension, which is filtered ultimately to produce a cake, representing the solid particles of zinc sulfide. Based on the results of the chemical content analysis of as-resultant zinc sulfide, more than 90 pct zinc sulfide can be recovered, and the recovered zinc sulfide grade can reach 66.70 pct. This material can be sold as zinc sulfide concentrate or roasted to regenerate into zinc oxide.     

Study of the Ni<Subscript>41.3</Subscript>Ti<Subscript>38.7</Subscript>Nb<Subscript>20</Subscript> wide transformation hysteresis shape-memory alloy

The shape-memory characteristics in the Ni_41.3Ti_38.7Nb₂₀ alloy have been investigated by means of cryogenic tensile tests and differential scanning calorimetry measurement. The martensite start temperature M _s could be adjusted to around the liquid nitrogen temperature by controlling the cooling condition. The reverse transformation start temperature A′ _s rose to about 70 °C after the specimens were deformed to 16 pct at different temperatures, where the initial states of the specimens were pure austenite phase, martensite phase, or duplex phase. The shape-memory effect and the reverse transformation temperatures were studied on the specimens deformed at (M _s +30 °C). It was found that once the specimens deformed to 16 pct, a transformation hysteresis width around 200 °C could be attained and the shape recovery ratio could remain at about 50 pct. The Ni_41.3Ti_38.7Nb₂₀ alloy is a promising candidate for the cryogenic engineering applications around the liquid nitrogen temperature. The experimental results also indicated that the transformation temperature interval of the stress-induced martensite is smaller by about one order of magnitude than that of the thermal-induced martensite.     

Microstructure and high-temperature tensile deformation of tiai(si) alloys made from elemental powders

Two ternary TiAl-based alloys with chemical compositions of Ti-46.4 at. pct Al-1.4 at. pct Si (Si poor) and Ti-45 at. pct Al-2.7 at. pct Si (Si rich), which were prepared by reaction powder processing, have been investigated. Both alloys consist of the intermetallic compounds y-TiAl, α₂-Ti₃Al, and ξ-Ti₅(Si, Al)₃. The microstructure can be described as a duplex structure(i.e., lamellar γ/α₂ regions distributed in γ matrix) containing ξ precipitates. The higher Si content leads to a larger amount of ξ precipitates and a finer y grain size in the Si-rich alloy. The tensile properties of both alloys depend on test temperature. At room temperature and 700 °C, the tensile properties of the Si-poor alloy are better than those of the Si-rich alloy. At 900 °C, the opposite is true. Examinations of tensile deformed specimens reveal ξ-Ti₅(Si, Al)₃ particle debonding and particle cracking at lower test temperatures. At 900 °C, nucleation of voids and microcracks along lamellar grain boundaries and evidence for recovery and dynamic recrystallization were observed. Due to these processes, the alloys can tolerate ξ-Ti₅(Si, Al)₃ particles at high temperature, where the positive effect of grain refinement on both strength and ductility can be utilized.     

Preaging effects in Al-Mg-Si alloys

The aging characteristics of aluminum alloy extrusions containing 0.60 to 0.90 wt pct Mg₂Si were determined. At low Mg₂Si levels, preaging treatments at room temperature and at elevated temperatures refined the G.P. zone dispersion and increased the alloy’s hardness after final aging. Preaging had little effect on hardness at the high end of the Mg₂Si range. These results are explained on the basis of current aging theories which invoke the concept of a critical temperature, above which homogeneous nucleation does not take place. This temperature varies from ≃150°C at 0.6 pct Mg2Si to ≃220°C at 1.5 pct Mg₂Si. The apparent activation energy for final aging was estimated to be 21 kcal/mole, a value which is intermediate between the activation energies for vacancy motion and solute (silicon and magnesium) diffusion in aluminum.     

Role of Si in Improving the Shape Recovery of FeMnSiCrNi Shape Memory Alloys

The effect of Si addition on the microstructure and shape recovery of FeMnSiCrNi shape memory alloys has been studied. The microstructural observations revealed that in these alloys the microstructure remains single-phase austenite (γ) up to 6 pct Si and, beyond that, becomes two-phase γ + δ ferrite. The Fe₅Ni₃Si₂ type intermetallic phase starts appearing in the microstructure after 7 pct Si and makes these alloys brittle. Silicon addition does not affect the transformation temperature and mechanical properties of the γ phase until 6 pct, though the amount of shape recovery is observed to increase monotonically. Alloys having more than 6 pct Si show poor recovery due to the formation of δ-ferrite. The shape memory effect (SME) in these alloys is essentially due to the γ to stress-induced ε martensite transformation, and the extent of recovery is proportional to the amount of stress-induced ε martensite. Alloys containing less than 4 pct and more than 6 pct Si exhibit poor recovery due to the formation of stress-induced α′ martensite through γ-ε-α′ transformation and the large volume fraction of δ-ferrite, respectively. Silicon addition decreases the stacking fault energy (SFE) and the shear modulus of these alloys and results in easy nucleation of stress-induced ε martensite; consequently, the amount of shape recovery is enhanced. The amount of athermal ε martensite formed during cooling is also observed to decrease with the increase in Si.     

Desiliconization and decarburization behavior of molten Fe-C-Si(-S) alloy with CO<Subscript>2</Subscript> and O<Subscript>2</Subscript>

One of the most important problems in the steelmaking process is an increase of the disposal slag mainly discharged from the dephosphorization process. In order to reduce the quantity of the disposal slag, the complete removal of silicon from molten pig iron is considered very effective before the dephosphorization in the pretreatment process. From this point of view, the desiliconization and the decarburization behavior of Fe-C-Si alloy with CO₂ and O₂ has been investigated in the present work. It is thermodynamically calculated that silicon should be oxidized in preference to carbon over 0.60 mass pct Si under the condition of s_SiO2=a _C=1 at 1573 K and is experimentally confirmed that silicon is only oxidized under the condition in actual. Even under the competitive region of desiliconizing and decarbonizing, under 0.60 mass pct Si, silicon is found to be oxidized down to about 0.1 mass pct Si in preference. The overall rate constants for the desiliconization and the decarburization are derived, and the value for the desiliconization is one order of magnitude larger than that for the decarburization. The influence of sulfur is also examined, and the retarding effect is not observed on the oxidation reactions.     

Determination of Solid Fraction from Cooling Curve

A new method to determine directly the solid fraction using the cooling curve was proposed for solidification of undercooled melts. Then, to construct three different baselines, a sudden function ξ _α (x) is introduced. In terms of the ξ _α (x) function, accordingly, the solid fractions during solidification of Ni-3.3 wt pct B, Al-7 wt pct Si, Al-14 wt pct Cu, and Fe-4.56 wt pct Ni alloys were predicted. The predictions of the primary, the regular lamellar eutectic, the anomalous eutectic, and the peritectic phases from cooling curves of the solidified samples coincide with the results of measurement or the available methods.     

Thermodynamics on the formation of spinel (MgO·Al<Subscript>2</Subscript>O<Subscript>3</Subscript>) inclusion in liquid iron containing chromium

The stability diagram of MgO, spinel solid solution (MgO·(Al _X Cr_1−X )₂O₃), and sesquioxide solid solution ((Al _Y Cr_1−Y )₂O₃) as a function of Mg, Al, and O contents at a constant chromium content (18 mass pct) in liquid iron is drawn at 1873 K. The interaction parameters between Mg and other solutes (Al, Cr, Ni, Ti, Si, and C) are determined by the experimental method, which assures equilibrium between Mg vapor and liquid iron, were applied to calculate the diagram. Titanium deoxidation is not recommended for the prevention of spinel formation, because Ti accelerates Mg dissolution from refractory or slag due to its high affinity for Mg (e _Mg ^Ti = − 0.64). The standard Gibbs free energies of formation for the three inclusions (periclase, spinel, and sesquioxide solid solutions) and the tielines between two solid solutions were calculated with the aid of the regular solution model and the thermochemical F*A*C*T database computing system, respectively. The phase stability regions and oxygen content in steel for the current Fe-Mg-Al-Cr (18 mass pct)-O system are compared with those of the previous non-Cr system. Detailed information on the spinel composition according to Mg and Al contents is also available from the present stability diagram.     

Observation of the crystallization behavior of a slag containing 46 wt pct CaO, 46 wt pct SiO<Subscript>2</Subscript>, 6 wt pct Al<Subscript>2</Subscript>O<Subscript>3</Subscript>, and 2 wt pct Na<Subscript>2</Subscript>O using the double hot thermocouple technique

In this work, isothermal crystallization of a synthetic slag containing 46 wt pct CaO, 46 wt pct SiO₂, 6 wt pct Al₂O₃, and 2 wt pct Na₂O has been investigated by means of double hot thermocouple technique (DHTT). The effect of Na₂O content on crystallization time was confirmed. Two different types of calcium silicate crystals were observed. Calcium di-silicate forms at temperatures above 1150 °C and calcium tri-silicate precipitate at temperatures below 1050 °C. A mixture of the two types of calcium silicate has been observed between the two temperatures. The tendency of crystals to become richer in calcium at low temperatures that has also been observed in previous published works has been confirmed. No effect of the cooling rate on crystallization start time was confirmed in the range of cooling rates applied in this investigation.     

Oxidation of Fe-V Melts Under CO<Subscript>2</Subscript>-O<Subscript>2</Subscript> Gas Mixtures

The oxidation mechanism of liquid Fe-V alloys with V content from 5 to 20 mass pct under different oxygen partial pressures using CO₂-O₂ mixtures with CO₂ varying from 80 pct to 100 pct was investigated by thermogravimetric analysis between 1823 K and 1923 K (1550 °C and 1650 °C). The products after oxidation were identified by scanning electron microscopy energy-dispersive spectrograph and X-ray diffraction. The results indicate that the oxidation process can be divided into the following steps: an apparent incubation period, followed by a chemical reaction step with a transition step before the reaction, and diffusion as the last stage. At the initial stage, a period of slow mass increase was observed that could be attributed to possible oxygen dissolution in the liquid iron-vanadium coupled with the vaporization of V₂O. The length of this period increased with increasing temperature as well as vanadium content in the melt and decreased with increasing oxygen partial pressure of the oxidant gas. This analysis was followed by a region of chemical oxidation. The oxidation rate increased with the increase of the O₂ ratio in the CO₂-O₂ gas mixtures. During the final stage, the oxidation seemed to proceed with the diffusion of oxygen through the product layer to the reaction front. The Arrhenius activation energies for chemical reaction and diffusion were calculated, and kinetic equations for various steps were setup to describe the experimental results. The transition from one reaction mechanism to the next was described mathematically as mixed-control equations. Thus, uniform kinetic equations have been setup that could simulate the experimental results with good precision.