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At least 937 records · Page 52

Identifying the microstructural features associated with void nucleation during elevated–temperature deformation of copper

The microstructural-scale mechanisms that produce cracks in metals during deformation at elevated temperatures are relevant to applications that involve thermal exposure. Prior studies of cavitation during high-temperature deformation, for example, creep, suffered from an inability to directly observe the microstructural evolution that occurs during deformation and leads to void nucleation. Here the current study takes advantage of modern high-speed electron backscatter diffraction (EBSD) detectors to observe cavitation in oxygen-free, high-conductivity copper in situ during deformation at 300°C. Most voids formed at the triple junction between a twin boundary and a high-angle grain boundary (HAGB). This finding does not contradict previous studies that suggested that twins are resistant to cracking—it reveals that cracks in HAGBs originate at twin/HAGB triple junctions and that cracks preferentially grow along HAGBs rather than the accompanying twins. Atomistic simulations explored the origins of this observation and suggest that twin/HAGB triple junctions are microstructural weak points.

36 MATERIALS SCIENCE↗

A physically based mechanical model for Mullins effect in thermoplastic polyurethanes

Despite decades of research, connecting the chemical and physical structure of thermoplastic polyurethanes to their mechanical properties remains highly challenging. Of particular note are their large-deformation and rate-dependent behaviors, which vary greatly with molecular chemistry, including the type and relative content of soft and hard segments. In this work, we develop a physically motivated mechanical theory for predicting the behavior of thermoplastic polyurethanes. The theory incorporates a representation of microstructural evolution during mechanical deformation, which captures the signatures of stress softening over cyclic loading (commonly referred to as the Mullins effect). There are only eight physically motivated fitting parameters, including a direct dependence on the hard segment fraction. The model predicts that increasing the hard segment fraction leads to higher stiffness and greater energy dissipation, in quantitative agreement with published experimental data. Furthermore, we provide a comprehensive analysis of the model and validate its predictions across several independent datasets focused on mechanical characterization. Direct comparisons to experimental data demonstrate its predictive capability on the effect of loading rate, cyclic deformations, and applied tension or compression. Altogether, this work establishes a predictive framework that connects polymer chemistry and microstructure to emergent mechanical behaviors.

36 MATERIALS SCIENCE↗

Co-, Ni- and Fe-rich grain-boundary phases enhance creep resistance in θ'-strengthened Al-Cu alloys

Here, microstructural evolution and creep response were investigated in the cast Al-5.0Cu-0.3Mn-0.2Zr (wt.%) alloy with and without addition of slow-diffusing, intermetallic-forming elements Fe, Ni, or Co. Baseline Al-5.0Cu-0.3Mn-0.2Zr alloy exhibits high creep resistance at 300 °C, up to ~75 MPa, which is attributed to high-aspect-ratio, intragranular θ'-Al 2 Cu precipitates that effectively suppress dislocation climb. However, θ'-Al 2 Cu precipitate-free zones form along grain boundaries upon heat treatment, whose extent is amplified during subsequent creep. Such weak regions experience dislocation creep, leading to strain localization and acceleration of grain-boundary sliding. Adding Ni and Co, individually or in combination, leads to the formation of grain-boundary precipitates (Al 9 Co 2 , Al 3 Ni 2 ) which are resistant to coarsening, thus suppressing the formation of θ'-Al 2 Cu precipitate-free zones. This microstructure provides high creep resistance at stresses up to 75–80 MPa, with strain rates much lower than in unmodified Al-5.0Cu-0.3Mn-0.2Zr. Adding Fe, which results in extensive decoration of grain boundaries with coarsening-resistant Al 7 Cu 2 Fe, and then increasing the Cu content to compensate for the Cu loss to this new phase, leads to a new Al-7.4Cu-1.6Fe-0.3Mn-0.2Zr alloy with creep resistance at 300 °C that surpasses known cast aluminum alloys. Adding Fe to improve the creep resistance of Al-Cu alloys is both cost-effective and sustainable. Our findings offer guidelines applicable to various alloy systems on controlling the evolution of precipitate-free zones and its ensuing effects on creep deformation.

36 MATERIALS SCIENCE↗

Microstructure Modeling of 3rd Generation Disk Alloy

The objective of this initiative, funded by NASA's Aviation Safety Program, is to model, validate, and predict, with high fidelity, the microstructural evolution of third-generation high-refractory Ni-based disc superalloys during heat treating and service conditions. This initiative is a natural extension of the DARPA-AIM (Accelerated Insertion of Materials) initiative with GE/Pratt-Whitney and with other process simulation tools. Strong collaboration with the NASA Glenn Research Center (GRC) is a key component of this initiative and the focus of this program is on industrially relevant disk alloys and heat treatment processes identified by GRC. Employing QuesTek s Computational Materials Dynamics technology and PrecipiCalc precipitation simulator, physics-based models are being used to achieve high predictive accuracy and precision. Combining these models with experimental data and probabilistic analysis, "virtual alloy design" can be performed. The predicted microstructures can be optimized to promote desirable features and concurrently eliminate nondesirable phases that can limit the reliability and durability of the alloys. The well-calibrated and well-integrated software tools that are being applied under the proposed program will help gas turbine disk alloy manufacturers, processing facilities, and NASA, to efficiently and effectively improve the performance of current and future disk materials.

Jou, Herng-Jeng↗

Linking microstructure to creep behavior in vertically and horizontally built LPBF Haynes 282 compared with wrought material via θ -projection

Laser Powder Bed Fusion (LPBF) has emerged as a promising route for fabricating intricate geometries in high-performance alloys. Haynes 282 (H282) is a strong candidate for applications such as heat exchangers or engines due to its excellent creep strength and thermal stability; however, the long-term creep behavior of LPBF-processed H282 remains poorly understood. In this study, the θ -projection method is used to analyze and extrapolate the creep behavior of vertically built LPBF, horizontally built LPBF, compared to wrought H282 tested at 816 °C. Vertically built LPBF H282 exhibits the lowest minimum creep rate (MCR), while the horizontally built condition shows a higher MCR comparable to that of wrought H282. Despite these differences, both LPBF conditions exhibit significantly shorter rupture life and reduced rupture strain than the wrought material, with the most severe degradation observed in the horizontal builds, consistent with an earlier onset of tertiary creep and accelerated strain-rate evolution. Microstructural characterization reveals that both LPBF and wrought H282 exhibit abundant twin-related boundary character; however, their grain boundary topologies differ markedly. The wrought alloy contains a higher fraction of low-angle grain boundaries and continuous twin lamellae, whereas the LPBF microstructure is characterized by a suppressed low-angle boundary population and fragmented twin-related boundaries embedded within irregular high-angle grain boundary networks. Fractographic analysis further reveals predominantly intergranular cracking in LPBF H282, accompanied by grain-boundary-decorated carbides, Al 2 O 3 inclusions, and high-aspect-ratio pores. These results demonstrate that grain boundary topology, rather than minimum creep rate alone, plays a critical role in governing creep damage accumulation and rupture behavior in LPBF and wrought H282.

Creep↗

Development of microstructure and texture during single and multiple pass friction stir processing of a strain hardenable aluminium alloy

Highlights: • Development of microstructure and texture during single and multiple pass FSP of a strain hardenable aluminium alloy • Strain induced boundary migration (SIBM) is the dominant nucleation mechanism for recrystallization • Weak crystallographic texture development influenced by SIBM with the relative dominance of shear texture components • Stable microstructure and texture development after multiple pass FSP • FSP is a promising method for the secondary processing of strain hardenable aluminium alloys - Abstract: In the present study, microstructure and texture development during single and multiple pass friction stir processing (FSP) of a strain hardenable wrought AlMg alloy (AA5086) was investigated. Subtle differences were observed while comparing with heat treatable alloys in the nucleation mechanism of the recrystallized microstructure observed in the nugget zone. Strain induced boundary migration was the dominant mechanism of microstructure evolution in the alloy, which influenced the crystallographic texture development by weakening it. Micro-texture measurements reveal variations in the crystallographic texture along the thickness of the sample. Recrystallization texture components were observed in the nugget zone indicative of a pronounced static recrystallization in the alloy as compared to the heat treatable alloys. Bulk texture measurements within the nugget zone of the optimally processed sample reveal a relatively dominant C component of shear texture. Average grain size in the nugget zone remained the same and the bulk crystallographic texture components were retained during multiple-pass FSP. The lower strain energies involved and the enhanced recovery processes due to the high temperature materials processing of the alloy during FSP resulted in a stable microstructure and texture. In summary, FSP could be promoted as a competent and suitable secondary processing technique for the bulk production of ultra-fine-grained materials in strain hardenable aluminium alloys.

36 MATERIALS SCIENCE↗

Exploring the tempering behaviour of additively manufactured high-alloy tool steel using synchrotron X-ray and neutron techniques

Post-processing heat treatment provides a critical pathway toward the commercialisation of additively manufactured (AM) S390 high-speed steel, which is a representative high-alloy tool steel employed in precision manufacturing, offering up to 1.5 times longer tool life and over 20% higher cutting speeds compared to conventional grades. In this study, the phase evolution of AM S390 steel during heat treatment, with particular emphasis on carbide precipitation behaviour, was systematically investigated using a combination of synchrotron X-ray and neutron techniques. The metastable M2C carbides were found to dissolve during austenitisation, while the stable primary carbides MC and M6C experienced coarsening with an average size increase of about 60 nm after just 2 min of tempering. Moreover, the austenite lattice parameters reduced from 3.618 to 3.608 Å within the first 10 min of tempering, suggesting carbon depletion in the steel matrix was likely associated with the formation of secondary carbides. This interpretation was substantiated by small-angle scattering results, which revealed the presence of nanoscale precipitates with a volume fraction of 3.1% after 60 min of tempering. These microstructural evolutions collectively accounted for the observed peak hardness of 921 HV. Furthermore, a comparative analysis of synchrotron and neutron small-angle scattering data highlighted the complementary strengths of each technique, offering critical insight into their suitability for characterising nanoscale features in AM high-alloy steels.

Synchrotron X-ray diffraction↗

Effects of Initial Powder Size on the Mechanical Properties and Microstructure of As-Extruded GRCop-84

GRCop-84 was developed to meet the mechanical and thermal property requirements for advanced regeneratively cooled rocket engine main combustion chamber liners. It is a ternary Cu- Cr-Nb alloy having approximately 8 at% Cr and 4 at% Nb. The chromium and niobium constituents combine to form 14 vol% Cr2Nb, the strengthening phase. The alloy is made by producing GRCop-84 powder through gas atomization and consolidating the powder using extrusion, hot isostatic pressing (HIP) or vacuum plasma spraying (VPS). GRCop-84 has been selected by Rocketdyne, Ratt & Wlutney and Aerojet for use in their next generation of rocket engines. GRCop-84 demonstrates favorable mechanical and thermal properties at elevated temperatures. Compared to NARloy-Z, the currently used inaterial in the Space Shuttle, GRCop-84 has approximately twice the yield strength, 10-1000 times the creep life, and 1.5-2.5 times the low cycle fatigue life. The thermal expansion of GRCop-84 is 7515% less than NARloy-Z which minimizes thermally induced stresses. The thermal conductivity of the two alloys is comparable at low temperature but NARloy-Z has a 20-50 W/mK thermal conductivity advantage at typical rocket engine hot wall temperatures. GRCop-84 is also much more microstructurally stable than NARloy-Z which translates into better long term stability of mechanical properties. Previous research into metal alloys fabricated by means of powder metallurgy (PM), has demonstrated that initial powder size can affect the microstructural development and mechanical properties of such materials. Grain size, strength, ductility, size of second phases, etc., have all been shown to vary with starting powder size in PM-alloys. This work focuses on characterizing the effect of varying starting powder size on the microstructural evolution and mechanical properties of as- extruded GRCop-84. Tensile tests and constant load creep tests were performed on extrusions of four powder meshes: +140 mesh (great3er than l05 micron powder size), -140 mesh (less than or equal to 105 microns), -140 plus or minus 270 (53 - 105 microns), and - 270 mesh (less than or equal to 53 microns). Samples were tested in tension at room temperature and at 500 C (932 F). Creep tests were performed under vacuum at 500 C using a stress of 111 MPa (16.1 ksi). The fracture surfaces of selected samples from both tests were studied using a Scanning Electron Microscope (SEM). The as-extruded materials were also studied, using both optical microscopy and SEM analysis, to characterize changes within the microstructure.

Okoro, Chika L.↗

Constitutive Model for Hot Deformation of the Cu-Zr-Ce Alloy

Hot compressive deformation behavior of the Cu-Zr-Ce alloy has been investigated according to the hot deformation tests in the 550-900 °C temperature range and 0.001-10 s{sup −1} strain rate range. Based on the true stress–true strain curves, the flow stress behavior of the Cu-Zr-Ce alloy was investigated. Microstructure evolution was observed by optical microscopy. Based on the experimental results, a constitutive equation, which reflects the relationships between the stress, strain, strain rate and temperature, has been established. Material constants n, α, Q and ln A were calculated as functions of strain. The equation predicting the flow stress combined with these materials constants has been proposed. The predicted stress is consistent with experimental stress, indicating that developed constitutive equation can adequately predict the flow stress of the Cu-Zr-Ce alloy. Dynamic recrystallization critical strain was determined using the work hardening rate method. According to the dynamic material model, the processing maps for the Cu-Zr and Cu-Zr-Ce alloy were obtained at 0.4 and 0.5 strain. Based on the processing maps and microstructure observations, the optimal processing parameters for the two alloys were determined, and it was found that the addition of Ce can promote the hot workability of the Cu-Zr alloy.

36 MATERIALS SCIENCE↗

Nanocrystalline ZrN thin film development via atomic layer deposition for U-Mo powder

Zirconium nitride (ZrN) thin film deposited via thermal atomic layer deposition (ALD) has been recently chosen as a candidate technology for application of a diffusion barrier coating on the low enriched uranium alloy powder considered in the NNSA research reactor conversion program. Reported here is the first instance of using ALD for coating actinide materials. For this study, a modified ALD system was constructed to produce one micron thick zirconium nitride (ZrN) coating over spherical particulate of natural uranium-molybdenum (U-Mo) based fuel. The ALD system was designed to have a rotating drum system, with provisions for facilitating sequential exposures of chemicals such as tetrakis dimethyl amido zirconium (TDMAZr) and ammonia (NH 3 ) in order to deposit ZrN. The ALD system was successful in developing a highly conformal ZrN coating covering every individual U-7Mo particle. This article describes the ZrN film synthesis details and reports the produced microstructure and composition of the ALD ZrN as deposited on fuel particulates. The as-fabricated coating was determined to have a nanocrystalline structure in the cubic-ZrN (cF8) phase. It exhibited a dense microstructure with adequate interfacial bonding. TEM-EELS characterization demonstrated that the coating contains a very low amount of oxygen impurity. To understand the potential microstructural evolution for ALD ZrN during reactor operation, an in-situ heavy ion (Kr) irradiation experiment was performed at the IVEM-Tandem facility. A total fluence of 7.5 x 10 15 ions/cm 2 (similar to 10 dpa) was achieved, and apart from minor grain coarsening in the ALD ZrN coating, no significant radiation effects were observed.

36 MATERIALS SCIENCE↗

Dynamic Analysis of Recalescence Process and Interface Growth of Eutectic Fe{sub 82}B{sub 17}Si{sub 1} Alloy

By employing the glass fluxing technique in combination with cyclical superheating, the microstructural evolution of the undercooled Fe{sub 82}B{sub 17}Si{sub 1} alloy in the obtained undercooling range was studied. With increase in undercooling, a transition of cooling curves was detected from one recalescence to two recalescences, followed by one recalescence. The two types of cooling curves were fitted by the break equation and the Johnson–Mehl–Avrami–Kolmogorov model. Based on the cooling curves at different undercoolings, the recalescence rate was calculated by the multi-logistic growth model and the Boettinger–Coriel–Trivedi model. Both the recalescence features and the interface growth kinetics of the eutectic Fe{sub 82}B{sub 17}Si{sub 1} alloy were explored. The fitting results that were obtained using TEM (SAED), SEM and XRD were consistent with the changing rule of microstructures. Finally, the relationship between the microstructure and hardness was also investigated.

36 MATERIALS SCIENCE↗

Synergy between phase transformation and domain switching in two morphotropic phase boundary ferroelectrics

We present that many applications of ferroic materials take advantage of the microstructural redistribution under an external stimulus. Despite extensive studies on the microstructural evolution during both domain switching and phase transformations of high-performance ferroelectrics near morphotropic phase boundaries (MPBs), the synergetic interactions between both leading factors remain unclear. Herein, we have illustrated and discerned the correlative response of phase transformation and domain switching in an archetypical piezoceramic of PbTiO 3 -BiScO 3 using a combination of in situ high-energy synchrotron x-ray diffraction and phase-field simulations. The direct structural evidence and domain development from simulations reveal a significant reversible orientation-dependent emerging phase transformation and enhanced domain switching. Increasingly populated polarization variants aligned with the applied electric field owing to this strong synergistic interaction play an important role in enhancing the piezoelectric performances of MPB ferroelectrics. Lastly, in addition to providing further insight into the microstructures of ferroelectrics, the present results have the potential to guide the design of high-performance materials.

36 MATERIALS SCIENCE↗

Characterization of the Hot Deformation Behavior of a Newly Developed Nickel-Based Superalloy

To clarify the microstructural evolution and hot workability of GH4282 during hot forming processes, the hot deformation behavior of this superalloy was investigated by isothermal compression tests in the temperature interval of 950-1210 °C and the strain rate range of 0.01-10 s{sup −1} with a true strain of 0.7. The results show that the flow stresses decrease with an increase in the deformation temperature and a decrease in the strain rate. The characteristic of dynamic recrystallization is revealed by the flow curves. The variation rule of the flow stress can be well described by the hyperbolic sine type equation, and the thermal deformation activation energy is determined to be 498.118 kJ/mol. The optimum hot working parameters are 1100-1180 °C and 0.01-0.1 s{sup −1}, under which the fine and uniform microstructure can be obtained.

36 MATERIALS SCIENCE↗

Sinter-Bonding of AISI 316L and 17-4 PH Stainless Steels

The sinter-bonding method was used to produce AISI 316L/17-4 PH components by conventional powder metallurgy technology. The production process consisted of following steps: the powder layering, co-pressing and co-sintering processes. The co-sintering process was carried out at different sintering temperatures (1200, 1250 and 1300 °C), and times (60, 90 and 120 min) in hydrogen atmosphere. The effect of co-pressing and co-sintering conditions on the ability to create a permanent connection between AISI 316L and 17-4 PH stainless steels was investigated. The densification, dimensional change and microstructural evolution of sintered AISI 316L/17-4 PH components were studied. The increase in co-pressing pressure as well as using of the longer time and the higher temperature of co-sintering process contributed to increase in AISI 316L/17-4 PH component density. The dilatometric study as well as dimensional changes measurements revealed an appropriate sintering compatibility for AISI 316L and 17-4PH steels when the sintering process was carried out at the temperature of 1200 °C for time ranging from 60 to 120 min and at 1250 °C for shorter sintering times. The sintering at temperature of 1300 °C (regardless of other manufacturing conditions) led to a significant deviation from the cylindrical shape of samples, as a result of difference of shrinkage of AISI 316L and 17-4 PH steels. Microstructural study indicated that AISI 316L and 17-4 PH steels creates a good diffusion joint (without any cracks and warpage) during the high-temperature sintering process. Nickel diffusion takes place from the AISI 316L to 17-4 PH stainless steel, and copper and molybdenum diffuse in opposite direction of nickel diffusion. It is possible to achieve a solid connection between two materials exhibiting difference in chemical composition by using sinter-bonding and conventional powder metallurgy technology.

36 MATERIALS SCIENCE↗

Ex-situ Heat Treatment of TEM Foils in a Custom Titanium Fixture: A Case Study on Ni-based Superalloy

The advancement of microstructural characterization at the nanoscale is critical to understanding the microstructural evolution and performance of engineering materials. Transmission electron microscopy (TEM) plays a vital role in such investigations, particularly when coupled with controlled ex- and in-situ experiments. In this study, we introduce a novel method for ex-situ heat treatment (HT) of TEM foils using a custom-designed fixture, made from pure titanium, and vacuum furnace to inhibit oxidation. This approach ensures precise temperature control and minimal sample contamination during HT, critical for substructural characterization and analysis of metallic materials. The fixture consists of a titanium base with three slits, for three sample foils, and a titanium cap for closure. The entire assembly is placed in a vacuum heat treatment furnace with high vacuum capability to prevent oxidation. To validate the effectiveness of the setup, precipitation behavior and microstructural changes were studied in an IN725 variant heat-treated at 500°C for 1 hour and 282 variant heat-treated at 700°C for 1 hour, as case studies.

electron microscopy↗

Ab initio prediction of FeCr sigma (001)/FCC Fe(111) interfacial energy: Effect of interfacial doping of C, B, and N

Interfacial energy plays a crucial role for high-temperature material systems in determining their microstructure evolution and mechanical properties. Optimizing the interfacial energy through doping can improve the stability, performance, and overall functionality of these materials. Here, the present study delivers theoretical investigation on the sigma FeCr (001)//FCC Fe (111) interfacial energy using ab initio methods, focusing on the implications of interfacial doping with important interstitial elements carbon (C), boron (B), and nitrogen (N). The calculated interfacial energy without doping is 0.183J/m 2 . Upon doping, notable reductions in interfacial energy were observed. Doping with B decreased the interfacial energy to 0.046J/m 2 , with single C doping to 0.126J/m 2 , with two C doping to 0.098J/m 2 , and with a single N doping to 0.071J/m 2 . These findings not only shed light on the atomistic origin for the effect of stabilizing the microstructure of stainless steel at elevated temperatures by interstitial doping, but also present a systematic, thorough ab initio approach to predict interfacial doping properties and guide alloy design to enhance the performance and stability.

FeCr sigma phase↗

Anisotropic domains and antiferrodistortive-transition controlled magnetization in epitaxial manganite films on vicinal SrTiO 3 substrates

We studied the microstructural evolution and magnetism of ferroelastic La 0.9 Sr 0.1 MnO 3 (LSMO) epitaxial thin films grown on SrTiO 3 (001) substrates with different miscut angles. The substrate miscut angle plays a critical role in controlling the in-plane magnetic anisotropy. The microscopic origin of such magnetic anisotropy is attributed to the formation of anisotropic stripe domains along the surface step terraces. The magnetization in the LSMO films was found to be selectively modulated by the antiferrodistortive phase transition of the SrTiO 3 substrate. This phenomenon has been qualitatively explained by a strain modified Stoner–Wohlfarth model. We conclude that the magnetization modulation by the SrTiO 3 phase transition depends on h, the ratio of applied magnetic field to the saturation field. Such modulation is only visible with h < 1. The established domain microstructure–anisotropy–magnetism correlation in manganite films can be applied to a variety of complex oxide thin films on vicinal substrates.

36 MATERIALS SCIENCE↗

Temperature and neutron flux dependence of in-reactor creep for cold-worked Zr-2.5Nb - 2016-0042

Over the past 10 years, internally pressurized capsules made from Zr-2.5Nb tubing have been irradiated in the National Research Universal (NRU) reactor at Chalk River Laboratories at temperatures of 280, 320, and 340 deg. C and dose rates between 3 X10{sup 15} n. m{sup -2}. s{sup -1} and 2 X10{sup 17} n. m{sup -2}. s{sup -1} (E>1 MeV). Periodic gaging has been used to assess the primary and secondary (steady-state) creep behavior. The objective of this detailed and controlled experiment was to determine, for the first time, the creep and microstructure evolution in Zr-2.5Nb tubing over a wide range of irradiation conditions for fast neutron fluxes applicable to a CANDU pressure tube. Similar but 'accelerated' creep experiments have been conducted in the Osiris test reactor at fast neutron fluxes of approximately 1.8 X10{sup 18} n. m{sup -2}. s{sup -1} (E>1 MeV), much greater than the neutron fluxes in the NRU reactor. Although accelerated tests in high-flux reactors such as Osiris provide information on irradiation creep, they do not represent the neutron flux conditions applicable to a power reactor. Tests covering power reactor operating conditions are needed to develop models for in-reactor creep of pressure tubes under the appropriate conditions. The data from the NRU reactor are compared with results from creep capsules with similar starting microstructures but irradiated in the Osiris reactor. The results show that the steady-state diametral and axial creep rates have a complex dependence on stress, temperature, and fast neutron flux. Data from out-reactor creep tests on unirradiated and pre-irradiated creep capsules that show the effect of prior irradiation on creep are also reported. The results are discussed in terms of a combination of creep mechanisms involving dislocation glide and mass transport. (authors)

36 MATERIALS SCIENCE↗