Intergranular Corrosion Behavior of 304LN Stainless Steel Heat Treated at 623 K (350 °C)

Low temperature sensitization of 304LN stainless steel from the two pipes, differing slightly in chemical composition, has been investigated; specimens were aged at 623 K (350 °C) for 20,000 hours and evaluated for intergranular corrosion and degree of sensitization. The base and heat-affected zone (HAZ) of the 304LN-1 appear resistant to sensitization, while 304LN-2 revealed a “dual” type microstructure at the transverse section and HAZ. The microstructure at 5.0-mm distance from the fusion line indicates qualitatively less sensitization as compared to that at 2.0 mm. The 304LN-2 base alloy shows overall lower degree of sensitization values as compared to the 304LN-1. A similar trend of degree of sensitization was observed in the HAZ where it was higher in the 304LN-1 as compared to the 304LN-2. The weld zone of both the stainless steels suffered from cracking during ASTM A262 practice E, while the parent metals and HAZs did not show such fissures. A mottled image within the ferrite lamella showed spinodal decomposition. The practice E test and transmission electron microscopy results indicate that the interdendritic regions may suffer from failure due to carbide precipitation and due to the evolution of brittle phase from spinodal decomposition.     

Evolution of Relationships Between Dislocation Microstructures and Internal Stresses of AISI 316L During Cyclic Loading at 293 K and 573 K (20 °C and 300 °C)

The evolution of dislocation densities and of dislocation microstructures during cyclic loading of AISI 316L is systematically evaluated. In addition, internal stresses are also measured for every cycle and comprehensively analyzed. These observations are made in order to establish relationships between the evolution of dislocation condition and internal stresses, and ultimately to obtain a thorough insight into the complex cyclic response of AISI 316L. Moreover, the dependencies of established relationships on the variation of temperature and strain amplitude are investigated. The back stresses (long-range stresses associated with the presence of collective dislocations over different length scales) are mainly responsible for the cyclic deformation response at high strain amplitudes where dislocations tend to move more quickly in a wavy manner. In contrast, the effective stress, coupling with short-range dislocation interactions, plays an insignificant role on the material cyclic response for wavy slip conditions, but increasingly becomes more important for planar slip conditions. The additionally strong short-range interactions between dislocations and point defects (initially with solute atoms and later in life with corduroy structure) at 573 K (300 °C) cause dislocations to move in more planar ways, resulting in a significant increase in effective stress, leading to their influential role on the material cyclic response.     

The Effect of Nd on the Tension and Compression Deformation Behavior of Extruded Mg-1Mn (wt pct) at Temperatures Between 298 K and 523 K (25 °C and 250 °C)

The tension and compression deformation behavior of extruded magnesium-1 wt pct manganese alloys with nominally 0.3 wt pct (MN10) and 1 wt pct neodymium (MN11) was studied over the temperature range of 298 K to 523 K (25 °C to 250 °C). Nd additions to Mg alloys tend to reduce the strong basal texture exhibited by conventional wrought Mg alloys and this work was intended to study the effect of Nd on the deformation behavior of Mg alloys. In situ tensile and compressive experiments were performed using a scanning electron microscopy, and electron backscatter diffraction was performed both before and after the deformation. A slip trace analysis technique was used to identify the distribution of the deformation systems as a function of strain, and based on this analysis and the texture of the undeformed samples, the critical resolved shear stress ratios between the deformation systems were estimated. In the case of MN11, the deformation behavior under tension at all temperatures was dominated by slip, while in compression, extension twinning was the major deformation mode. In tension at 323 K (50 °C), extension twinning, basal, prismatic 〈a〉, and pyramidal 〈c + a〉 slip were active in MN11. Much less extension twinning was observed at 423 K (150 °C), while basal slip and prismatic 〈a〉 slip were dominant and presented similar relative activities. At 523 K (250 °C), twinning was not observed, and basal slip controlled the deformation. With the reduction of Nd content, less slip deformation and more twinning were observed during the tensile deformation. However, like for MN11, the extent of twinning in MN10 decreased with increasing temperature and basal slip was the primary deformation mode at elevated temperatures. Extension twinning was the major deformation mode under compression for all test temperatures in MN10 and MN11. The tensile strength decreased with increasing temperature for both alloys, where MN10 was slightly stronger than MN11 at 323 K (50 °C), which was expected to be a result of the stronger basal texture exhibited by MN10 due to its lower Nd content. However, MN11 maintained its strength more at elevated temperatures compared with MN10, and this was explained to be a result of the greater Nd content.     

High-Temperature (1023 K to 1273 K [750 °C to 1000 °C]) Plastic Deformation Behavior of B-Modified Ti-6Al-4V Alloys: Temperature and Strain Rate Effects

A minor addition of B to the Ti-6Al-4V alloy, by ~0.1 wt pct, reduces its as-cast prior β grain size by an order of magnitude, whereas higher B content leads to the presence of in situ formed TiB needles in significant amounts. An experimental investigation into the role played by these microstructural modifications on the high-temperature deformation behavior of Ti-6Al-4V-xB alloys, with x varying between 0 wt pct and 0.55 wt pct, was conducted. Uniaxial compression tests were performed in the temperature range of 1023 K to 1273 K (750 °C to 1000 °C) and in the strain rate range of 10^–3 to 10⁺¹ s^–1. True stress–true strain responses of all alloys exhibit flow softening at lower strain rates and oscillations at higher strain rates. The flow softening is aided by the occurrence of dynamic recrystallization through lath globularization in high temperature (1173 K to 1273 K [900 °C to 1000 °C]) and a lower strain rate (10^–2 to 10^–3 s^–1) regime. The grain size refinement with the B addition to Ti64, despite being marked, had no significant effect on this. Oscillations in the flow curve at a higher strain rate (10⁰ to 10⁺¹ s^–1), however, are associated with microstructural instabilities such as bending of laths, breaking of lath boundaries, generation of cavities, and breakage of TiB needles. The presence of TiB needles affected the instability regime. Microstructural evidence suggests that the matrix cavitation is aided by the easy fracture of TiB needles.     

Solid-State Phase Equilibria of the V-Si-Gd System at 973 K (700 °C)

The solid-state phase equilibria of the V-Si-Gd ternary system at 973 K (700 °C) were experimentally evaluated. The existence of nine binary compounds, namely, V₃Si, V₅Si₃, V₆Si₅, VSi₂, Gd₅Si₃, Gd₅Si₄, GdSi, GdSi_1.67, and GdSi_2?x , was confirmed, and no ternary compound was found at 973 K (700 °C). The homogeneity ranges of V₃Si and GdSi_2?x were investigated. It is worth mentioning that the Gd₃Si₄ compound was discovered through changing the experimental conditions, and its crystal structure was discussed.     

Experimentally Determined Phase Diagram for the Barium Sulfide-Copper(I) Sulfide System Above 873 K (600 °C)

The phase diagram of the barium sulfide-copper(I) sulfide system was investigated above 873 K (600 °C) using a custom-built differential thermal analysis (DTA) apparatus. The melting point of barium sulfide was determined utilizing a floating zone furnace. Four new compounds, Ba₂Cu₁₄S₉, Ba₂Cu₂S₃, Ba₅Cu₄S₇, and Ba₉Cu₂S₁₀, were identified through quench experiments analyzed with wavelength dispersive X-ray spectroscopy (WDS) and energy dispersive X-ray analysis (EDS). A miscibility gap was observed between 72 and 92 mol pct BaS using both DTA experiments and in situ melts observation in a floating zone furnace. A monotectic was observed at 94.5 mol pct BaS and 1288 K (1015 °C).     

The Role of Eta Phase Formation on the Creep Strength and Ductility of INCONEL Alloy 740 at 1023 K (750 °C)

INCONEL alloy 740 is an age-hardenable nickel-based superalloy proposed for advanced ultrasupercritical steam boiler applications operating at high stress and long times above 973 K (700 °C), where creep will be the dominate deformation mode. During high-temperature exposure, the alloy can form eta phase platelets that many have suggested may be detrimental to creep strength and ductility. In this study, creep-rupture tests were conducted on smooth and notched bars of INCONEL alloy 740 at 1023 K (750 °C) for times up to 20,000 hours. Examination of the creep-rupture life, creep ductility, failure modes, and microstructure by quantitative electron microscopy shows that a small amount of eta phase does not diminish the creep performance. Applied stress appears to have a minor effect on the precipitation of the eta phase but not its growth rate. Based on the observation that the microstructure after 20,000 hours of creep exposure has reached equilibrium in comparison to thermodynamic calculations, it is concluded that 20,000 hour creep tests are adequate for prediction of long-term creep performance.     

The Effects of Ni-Plating and Prolonged High Temperature Oxidation at 1423 K (1150 °C) on a CMSX-10 Single-Crystal Ni-Based Super-Alloy and Coating System

A hypothesis was investigated, to assess if Ni-plating a 3rd-generation single-crystal alloy could favorably alter the diffusion profile of critical elements such that brittle, deleterious topologically close-packed (TCP) phases did not form or at least the extent to which they did was reduced. In conjunction with delaying the onset of these phases, it was hoped that more favorable alternatives could be promoted, such as martensite (β′). This study showed that Ni-plating did have some positive effects on the super-alloy/coating system. While the coating produced on the Ni-plated alloy was thinner, it retained a higher Al content than its unplated counterpart when subjected to oxidation. The retention of Al within the coating delayed the phase evolution of the coating from a β or β + β′ to a γ′-dominant coating as the Ni-plated system had a greater driving force for Ni and Al diffusion, which helped to establish the Ni-rich diffusion barrier that entrapped Al in the coating. Unfortunately, Ni-plating does not sufficiently alter the diffusion profiles within the alloy to prevent precipitation of the TCP phases. Four pairs of the CMSX-10 alloy were used for this study. While they were all aluminized, only half of them, one in each pair, were Ni plated prior to aluminizing. Three of the four pairs were then oxidized at 1423 K (1150 °C), while the first pair was kept as a standard. X-ray diffraction, scanning electron microscopy, and energy dispersive X-ray spectroscopy were used to characterize each alloy-coating system in an effort to better understand their performance under high temperature oxidation.     

Isothermal Reaction of NiO Powder with Undiluted CH<Subscript>4</Subscript> at 1000 K to 1300 K (727 °C to 1027 °C)

In this study, isothermal reaction behavior of loose NiO powder in a flowing undiluted CH₄ atmosphere at the temperature range 1000 K to 1300 K (727 °C to 1027 °C) is investigated. Thermodynamic analyses at this temperature range revealed that single phase Ni forms at the input \( {{n_{{{\text{CH}}_{ 4} }}^{\text{o}} } \mathord{\left/ {\vphantom {{n_{{{\text{CH}}_{ 4} }}^{\text{o}} } {\left( {n_{{{\text{CH}}_{ 4} }}^{\text{o}} + n_{\text{NiO}}^{\text{o}} } \right)}}} \right. \kern-0pt} {\left( {n_{{{\text{CH}}_{ 4} }}^{\text{o}} + n_{\text{NiO}}^{\text{o}} } \right)}} \) mole fractions (\( X_{{{\text{CH}}_{ 4} }} \)) between ~0.2 and 0.5. It was also predicted that free C co-exists with Ni at \( X_{{{\text{CH}}_{ 4} }} \) values higher than ~0.5. The experiments were carried out as a function of temperature, time, and CH₄ flow rate. Mass measurement, XRD and SEM-EDX were used to characterize the products at various stages of the reaction. At 1200 K and 1300 K (927 °C and 1027 °C), the reaction of NiO with undiluted CH₄ essentially consisted of two successive distinct stages: NiO reduction and pyrolytic C deposition on pre-reduced Ni particles. At 1200 K (927 °C), 1100 K (827 °C), and 1000 K (727 °C), complete oxide reduction was observed within ~7.5, ~17.5, and ~45 minutes, respectively. It was suggested that NiO was essentially reduced to Ni by a CH₄ decomposition product, H₂. Possible reactions leading to NiO reduction were suggested. An attempt was made to describe the NiO reduction kinetics using nucleation-growth and geometrical contraction models. It was observed that the extent of NiO reduction and free C deposition increased with the square root of CH₄ flow rate as predicted by a mass transport theory. A mixed controlling mechanism, partly chemical kinetics and partly external gaseous mass transfer, was responsible for the overall reaction rate. The present study demonstrated that the extent of the reduction can be determined quantitatively using the XRD patterns and also using a formula theoretically derived from the basic XRD data.     

Analysis of the Deformation Behavior in Tension and Tension-Creep of Ti-3Al-2.5V (wt pct) at 296 K and 728 K (23 °C and 455 °C) Using In Situ SEM Experiments

The deformation behavior of a Ti-3Al-2.5V (wt pct) near-α alloy was investigated during in situ deformation inside a scanning electron microscopy (SEM). Two plates with distinct textures were examined. Tensile experiments were performed at 296 K and 728 K (455 °C) (~0.4T _m), while a tensile-creep experiment was performed at 728 K (455 °C) and 180 MPa (σ/σ _ys = 0.72). The active deformation systems were identified in the α phase using electron backscattered diffraction based slip-trace analysis and SEM images of the surface. Prismatic slip deformation was the dominant slip mode observed for all the experiments in both plates, which was supported by a critical resolved shear stress (CRSS) ratio analysis. However, due to the texture of plate 1, which strongly favored the activation of prismatic slip, the percentages of prismatic slip activity for specimens from plate 1 tested at 296 K and 728 K (23 °C and 455 °C) were higher than the specimens from plate 2 under the same testing conditions. T1 twinning was an active deformation mode at both 296 K and 728 K (23 °C and 455 °C), but the extent of twinning activity decreased with increased temperature. T1 twinning was more frequently observed in specimens from plate 2, which exhibited a higher fraction of twinning systems favoring activation at both 296 K and 728 K (23 °C and 455 °C). The tension-creep experiment revealed less slip and more grain boundary sliding than in the higher strain rate tensile experiments. Using a previously demonstrated bootstrapping statistical analysis methodology, the relative CRSS ratios of prismatic, pyramidal 〈a〉, pyramidal 〈c+a〉, and T1 twinning deformation systems compared with basal slip were calculated and discussed in light of similar measurements made on CP Ti and Ti-5Al-2.5Sn (wt pct).     

Tensile, Fatigue, and Creep Properties of Aluminum Heat Exchanger Tube Alloys for Temperatures from 293 K to 573 K (20 °C to 300 °C)

Since automotive heat exchangers are operated at varying temperatures and under varying pressures, both static and dynamic mechanical properties should be known at different temperatures. Tubes are the most critical part of the most heat exchangers made from aluminum brazing sheet. We present tensile test, stress amplitude-fatigue life, and creep–rupture data of six AA3XXX series tube alloys after simulated brazing for temperatures ranging from 293 K to 573 K (20 °C to 300 °C). While correlations between several mechanical properties are strong, ranking of alloys according to one property cannot be safely deduced from the known ranking according to another property. The relative reduction in creep strength with increasing temperature is very similar for all six alloys, but the general trends are also strong with respect to tensile and fatigue properties; an exception is one alloy that exhibits strong Mg-Si precipitation activity during fatigue testing at elevated temperatures. Interrupted fatigue tests indicated that the crack growth time is negligible compared to the crack initiation time. Fatigue lifetimes are reduced by creep processes for temperatures above approximately 423 K (150 °C). When mechanical properties were measured at several temperatures, interpolation to other temperatures within the same temperature range was possible in most cases, using simple and well-established equations.     

Transmission Electron Microscopic Investigations of Grain Boundary Beta Phase Precipitation in Al 5083 Aged at 373 K (100 °C)

The fine-scale microstructure of an Al 5083 alloy sensitized at 373 K (100 °C) for 3, 7, 14, 30, 45, and 90 days has been investigated using transmission electron microscopy (TEM) to study the evolution of the β phase (Al₃Mg₂) at grain boundaries. In fully sensitized Al 5083, the β phase (Al₃Mg₂) mostly forms heterogeneously at grain boundaries. TEM observations showed that the grain boundary precipitation of β phase was discrete up to 14 days of aging, and grain boundaries were fully covered by the β phase after 30 to 45 days of aging. The early stages of β growth on the grain boundaries are consistent with the collector-plate mechanism. We find no evidence of either Mg depletion or segregation at the grain boundaries. The initial growth rates as well as the thicknesses after long aging times are greater than can be accounted for by bulk diffusion of Mg to the grain boundaries. We suggest that dislocation pipe diffusion is necessary to account for the β growth rates.     

Effect of Boron on Carbide Coarsening at 873?K (600?°C) in 9?to 12?pct Chromium Steels

The addition of small amounts of boron to 9 to 12?pct chromium steels has been found to decrease their creep rate at 823?K to 923?K (550?°C to 650?°C). In this article, the behavior of boron during austenitizing, tempering, and isothermal heat treatment at 873?K (600?°C) is studied using high-resolution microscopy and microanalysis as well as using atomistic modeling. It was found that increasing the boron content from 9 to 40?ppm decreased the coarsening constant of M₂₃C₆ by a factor of almost 2. Most of the added boron was incorporated in M₂₃C₆. Atomistic modeling showed that boron diffusion in ferrite is dominated by an interstitial mechanism at 873?K (600?°C). However, the generation of vacancies when carbide precipitates dissolve may promote a distribution with substitutional boron atoms. The absence of a fast mechanism for the transition from substitutional to interstitial occupancy will make the slow substitutional boron diffusion in the matrix rate controlling for the coarsening process.     

Development of Microstructures of Long-Period Stacking Ordered Structures in Mg85Y9Zn6 Alloys Annealed at 673 K (400 °C) Examined by Small-Angle X-Ray Scattering

Development of LPSO structure and in-plane ordering during annealing the Mg85Y9Zn ternary alloy sample at 673 K (400 °C) was examined by synchrotron radiation small-angle scattering/diffraction measurements. By examining the first diffraction peaks for 18R, 10H, and in-plane order spot, the growth kinetics of in-plane order domain and the transition from 10H into 18R were discussed. The domain growth of in-plane order was characterized by small domain with little correlation between neighboring segregation layers.     

Thermodynamic Analysis of the Cu-As-S-(O) System Relevant to Sulfuric Acid Baking of Enargite at 473 K (200 °C)

While the growing demand for copper has compelled the industry to adapt new technologies for the treatment of copper-arsenic (enargite) concentrates, the refractory nature of such concentrates combined with the troublesome presence of arsenic has created a major metallurgical and environmental challenge. Preliminary results of the acid bake-leach process at the University of Utah have shown some potential advantages for the treatment of enargite concentrates. While the transformation of enargite to copper sulfate, arsenolite, and elemental sulfur has already been established experimentally, thermodynamic evaluation of the sulfuric acid baking process provides further understanding which should be useful. In this article, the available thermodynamic data for the species involved in the Cu-As-S-O system are compiled. These data were used to calculate the phase stability (Kellogg) diagrams as well as equilibrium compositions at 473 K (200 °C) using the STABCAL and HSC Chemistry^® 5.1 software packages. The equilibrium composition calculations indicate that enargite can transform to copper sulfate either directly or through chalcocite and/or covellite. The major gaseous species during baking were found to be SO₂ and H₂O. The results of the thermodynamic calculations were further compared with two confirmatory baking experiments involving a high-quality enargite sample. The condensed reaction products from sulfuric acid baking based on XRD results include CuSO₄, As₂O₃, CuO·CuSO₄, and S₈ under both neutral and oxidative conditions. While all these compounds were predicted through equilibrium calculations, some of the predicted compounds were not detected in the sulfuric acid-baked enargite. None of the calculations indicated any appreciable amounts of arsenic-bearing gases at the baking temperature of 473 K (200 °C). Consistent with thermodynamic predictions, no H₂S gas was detected during the sulfuric acid baking experiment. Approximately, 80 pct of the baked enargite samples were leached in water.     

Experimental Investigation of the Ce-Mg-Mn Isothermal Section at 723 K (450 °C) via Diffusion Couples Technique

The isothermal section of the Ce-Mg-Mn phase diagram at 723 K (450 °C) was established experimentally by means of diffusion couples and key alloys. The phase relationships in the complete composition range were determined based on six solid–solid diffusion couples and twelve annealed key alloys. No ternary compounds were found in the Ce-Mg-Mn system at 723 K (450 °C). X-ray diffraction and energy-dispersive X-ray spectroscopy spot analyses were used for phase identification. EDS line-scans, across the diffusion layers, were performed to determine the binary and ternary homogeneity ranges. Mn was observed in the diffusion couples and key alloys microstructures as either a solute element in the Ce-Mg compounds or as a pure element, because it has no tendency to form intermetallic compounds with either Ce or Mg. The fast at. interdiffusion of Ce and Mg produces several binary compounds (Ce _x Mg _y ) during the diffusion process. Thus, the diffusion layers formed in the ternary diffusion couples were similar to those in the Ce-Mg binary diffusion couples, except that the ternary diffusion couples contain layers of Ce-Mg compounds that dissolve certain amount of Mn. Also, the ternary diffusion couples showed layers containing islands of pure Mn distributed in most diffusion zones. As a result, the phase boundary lines were pointing toward Mn-rich corner, which supports the tendency of Mn to be in equilibrium with all the phases in the system.     

Improvement of Creep Resistance at 950 °C and 400 MPa in Ru-Containing Single-Crystal Superalloys with a High Level of Co Addition

Microstructural features, including γ′ volume fraction and size, γ-γ′ lattice misfit, γ channel width, and dislocation substructure, are known to significantly influence the creep performance in Ni-base single-crystal superalloys. In this study, the microstructural characteristics of Ru-containing single-crystal superalloys with different levels of Co, Mo, and Ru additions were quantitatively investigated after ruptured and interrupted creep tests conducted at 1223 K (950 °C) and 400 MPa. The creep lifetime was slightly increased with the high level of Co addition and significantly increased with the coadditions of Mo and Ru. A minor effect of Co content on the γ channel width and γ′ volume fraction was found in experimental alloys. The alloy with high levels of Mo and Ru additions was determined to possess a more negative γ-γ′ lattice misfit, and a high density of stacking faults (SFs) was formed in the γ channels during creep. The combined effects of the SFs in the γ matrix serving as the barriers to dislocation movement, as well as the dense interfacial dislocation networks preventing dislocation to shear the γ′ phase, were considered as the main mechanism responsible for the improvement of creep resistance. Results from this study are helpful to understand the effect of microstructural features on creep performance and contribute to the knowledge of physical metallurgy in Ru-containing single-crystal superalloys.