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All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Chapter 4 - Research Tools: Microstructure, Mechanical Properties, and Computational Thermodynamics

The purpose of this Chapter is to provide an overview of the research tools that are available to evaluate the response of materials that are subject to atomic displacements caused by fast particle irradiation. The major focus is on metals employed in structural components in operating or planned nuclear fission and fusion reactors. Understanding, predicting and characterising the changes in material properties under irradiation requires the ability to characterise the irradiation-induced microstructure at and above the atomic scale, and the ability to relate such changes to the observed degradation in performance sustaining properties. Thus, any discussion of research tools necessarily involves microstructural characterization techniques and mechanical property characterization techniques. In addition, computational thermodynamics (and related multiscale, multiphysics modeling) can also be considered characterization tools since they enable the study of the thermodynamically and kinetically mediated mechanisms (influenced by the irradiation environment) that affect microstructural evolution. Hence, this chapter also contains a brief review of computational thermodynamics.

English, Colin A.↗
DOE OSTI2014

Effects of Sn addition on the microstructure, mechanical properties and corrosion behavior of Ti–Nb–Sn alloys

Ti and Ti alloys are widely used in restorative surgery because of their good biocompatibility, enhanced mechanical behavior and high corrosion resistance in physiological media. The corrosion resistance of Ti-based materials is due to the spontaneous formation of the TiO{sub 2} oxide film on their surface, which exhibits elevated stability in biological fluids. Ti–Nb alloys, depending on the composition and the processing routes to which the alloys are subjected, have high mechanical strength combined with low elastic modulus. The addition of Sn to Ti–Nb alloys allows the phase transformations to be controlled, particularly the precipitation of ω phase. The aim of this study is to discuss the microstructure, mechanical properties and corrosion behavior of cast Ti–Nb alloys to which Sn has been added. Samples were centrifugally cast in a copper mold, and the microstructure was characterized using optical microscopy, scanning electron microscopy and X-ray diffractometry. Mechanical behavior evaluation was performed using Berkovich nanoindentation, Vickers hardness and compression tests. The corrosion behavior was evaluated in Ringer's solution at room temperature using electrochemical techniques. The results obtained suggested that the physical, mechanical and chemical behaviors of the Ti–Nb–Sn alloys are directly dependent on the Sn content. - Graphical abstract: Effects of Sn addition to the Ti–30Nb alloy on the elastic modulus. - Highlights: • Sn addition causes reduction of the ω phase precipitation. • Minimum Vickers hardness and elastic modulus occurred for 6 wt.% Sn content. • Addition of 6 wt.% Sn resulted in maximum ductility and minimum compression strength. • All Ti–30Nb–XSn (X = 0, 2, 4, 6, 8 and 10%) alloys are passive in Ringer's solution. • Highest corrosion resistance was observed for 6 wt.% Sn content.

36 MATERIALS SCIENCE↗
DOE OSTI2017

The effect of carbon on the microstructures, mechanical properties, and deformation mechanisms of thermo-mechanically treated Fe 40.4 Ni 11.3 Mn 34.8 Al 7.5 Cr 6 high entropy alloys

We investigated the effects of cold rolling followed by annealing on the mechanical properties and dislocation substructure evolution of undoped and 1.1 at. % carbon-doped Fe 40.4 Ni 11.3 Mn 34.8 Al 7.5 Cr 6 high entropy alloys (HEAs). X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atom probe tomography (APT) were employed to characterize the microstructures. The as-cast HEAs were coarse-grained and single phase f.c.c., whereas the thermo-mechanical treatment caused recrystallization (to fine grain sizes) and precipitation (a B2 phase for the undoped HEA; and a B2 phase, and M 23 C 6 and M 7 C 3 carbides for the C-doped HEA). Carbon, which was found to have segregated to the grain boundaries using APT, retarded recrystallization. The reduction in grain size resulted in a sharp increase in strength, while the precipitation, which produced only a small increase in strength, probably accounted for the small decrease in ductility for both undoped and C-doped HEAs. For both undoped and C-doped HEAs, the smaller grain-sized material initially exhibited higher strain hardening than the coarse-grained material but showed a much lower strain hardening at large tensile strains. Wavy slip in the undoped HEAs and planar slip in C-doped HEAs were found at the early stages of deformation irrespective of grain size. At higher strains, dislocation cell structures formed in the 19 μm grain-sized undoped HEA, while microbands formed in the 23 μm grain-sized C-doped HEA. Conversely, localized dislocation clusters were found in both HEAs at the finest grain sizes (5 μm). The inhibition of grain subdivision by the grain boundaries and precipitates lead to the transformation from regular dislocation configurations consisting of dislocation-cells and microbands to irregular dislocation configurations consisting of localized dislocation clusters, which further account for the decrease in ductility. Our investigation of the formation mechanism and strain hardening of dislocation cells and microbands could benefit future structural material design.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Mechanical Properties and Microstructure of High-Strength Steel Controlled by Hot Stamping Process

A novel design and manufacturing method, dubbed “precast,” of the cooling system and tools for a hot forming process was proposed in this paper. The integrated structures of the punch and blank holder were determined by analyzing the bending and reverse-bending deformation of the forming parts. The desired crashworthiness performance of an automotive front bumper constructed with this process was obtained by a tailored phase transformation, which generated martensite-bainite in the middle and full martensite transformation in the corner areas. Varying cooling effects in the formed parts caused the highest temperature to be located in the bottom and the lowest on the end of the formed parts. Moreover, the microstructural distributions demonstrated that the bottom possessed a relatively lower content of martensite, while, conversely, the end possessed a higher content. This was precisely the most desired phase distributions for the hot formed parts. For the six-process cycle stamping, the temperatures reached a stable status after an initial rapid increase in the first three process cycles. The microstructural results verified the feasibility of the hot forming tools under multiprocess cycles.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Mechanical property and microstructure evolution of nitrogen-modified Ti-6Al-4V alloy with core-shell structure by hot compression

Highlights: • Core-shell structured Ti-6Al-4 V is composed of α shells and α + β cores. • Nitrogen solution and core-shell structure significantly enhances the strength. • Core-shell structural alloy performs inhomogeneous deformation. - Abstract: Core-shell (CS) structured Ti-6Al-4 V (Ti64) alloy with single α shells and duplex α + β cores was fabricated by powder nitriding and spark plasma sintering. The mechanical property and microstructure evolution of CS-Ti64 alloy was investigated by compression at temperatures of 950–1100 °C and strain rates of 0.001–1 s{sup −1}. The nitrogen-induced solid solution strengthening and the nitrogen-stabilized CS structure significantly enhanced the compressive strength. Microstructure evolution of CS-Ti64, involved inhomogeneous deformation of the core and shell, which was quite different from that of the commercial Ti64. Regions adjacent to shells and central locations of cores suffered large strain and therefore preferentially underwent dynamic recrystallization (DRX). The deformation mechanism of the novel CS-Ti64 alloy was discussed in terms of the α shells, α laths and DRX.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Influence of Indium on Microstructure and Properties of Sn-Pb Binary Alloy Applied in Photovoltaic Ribbon

In this work, the conductivity, melting point, microstructure, spreading behavior, and mechanical properties of three types of Sn-Pb-In(indium) alloys are investigated along with Sn60Pb40 alloy as a reference. The results show that the In element improves the comprehensive properties of the Sn-Pb alloys. The maximum conductivity of the Sn-Pb-In alloys is 7.08 MS/m when the content of the In element is 3 wt.%. With an increasing content of the In element, the melting points of the Sn-Pb-In alloys gradually decrease from 183 to 166 °C. The microstructures of the alloys are refined with the addition of In. The intermetallic compound (IMC) InSn{sub 4} is only found in Sn60Pb34In6, except for the α-Pb and β-Sn phases. A spread test shows that only IMC Cu{sub 6}Sn{sub 5} is present at the Cu/solder interface of the solder joints. The Sn60Pb34In3 solder joint shows the highest ultimate tensile strength of 54 MPa. The microhardness of the alloys slightly increases from 12.76 HV{sub 0.05} to 13.56 HV{sub 0.05} with the In content increasing from 0 to 3 wt.%, while a sharp increase to 15.53 HV{sub 0.05} is observed when the amount of In exceeds 3 wt.%.

36 MATERIALS SCIENCE↗
DOE OSTI2017

High-Speed Friction Stir Welding of AA7075-T6 Sheet: Microstructure, Mechanical Properties, Micro-texture, and Thermal History

Friction-stir-welding (FSW) is a cost-effective and high quality joining process for aluminum alloys (especially heat-treatable allo ys) that has been applied successfully in the aerospace industry. However, the full potential of FSW on more cost-sensitive applications is still limited by the production rate, namely the welding speed of the process. The majority of literature evaluating FSW of aluminum alloys is based on welds made in the range of welding speeds around hundreds of millimeters per minute, and only a handful are at a moderate speed of 1 m/min. In this study we present a microstructural analysis of friction stir welded AA7075-T6 blanks with welding speeds up to 3 m/min. Textures, microstructures, mechanical properties, and weld quality are analyzed using TEM, EBSD, metallographic imaging, and Vickers hardness. Results are coupled with welding parameters to aid in the understanding of the complex material flow and texture gradients within the welds in an effort to optimize welding parameters for high speed processing.

Zhang, Jingyi↗
DOE OSTI2022

Microstructure, compression properties, and oxidation behavior of Hf-25Ta-5Me alloys (Me is Mo, Nb, W, 0.5Mo + 0.5 W, Cr, or Zr)

Hf–Ta based alloys have recently been investigated as potential candidates for high-temperature structural applications. While most attentions have been given to the properties above ~1200 °C where the alloys are mainly single-phase BCC structures and have excellent oxidation performance due to formation of super-oxides, structural properties at lower temperatures are equally important for applications in which an alloy may experience a range of temperatures. In the present work, microstructure, phase composition, mechanical properties and oxidation behavior of six Hf-25Ta-5Me alloys (Me is Mo (HTM alloy), W (HTW), 0.5Mo + 0.5 W (HTMW), Cr (HTC) or Zr (HTZ), the compositions are in at.%) are reported at temperatures below the eutectoid transformation. The alloys were prepared by arc melting followed by hot isostatic pressing for 3 h at 1400 °C and 207 MPa. All the alloys display coarse grains of partially or fully transformed (by a eutectoid reaction) high-temperature BCC phase. The eutectoid regions consist of fine lamellae of Hf-rich HCP and Ta-rich BCC phases. The ternary alloys containing W or Cr also contained small amounts of a cubic Laves phase. At 25 °C, the HTW alloy was the strongest (yield stress σ y = 1966 MPa) but brittle and HTZ was the weakest (σ y = 1120 MPa) but ductile among the studied alloys. Other alloys showed intermediate behaviors. In general, the room temperature ductility of the alloys increased with decreasing σy. All alloys maintained high strength up to 800 °C, but displayed a noticeable strength decrease at 1000 °C. At 1000 °C, HTMW was the strongest alloy (σ y = 468 MPa) and HTC was the weakest alloy (σ y = 368 MPa). All alloys had excellent deformability at 1000 °C. Oxidation behavior of the alloys was studied at 800 °C and 1000 °C and compared with that of Hf–27Ta binary alloy. Although the ternary additions improved oxidation resistance, overall oxidation performance of the studied alloys at 800 °C and 1000 °C was poor.

36 MATERIALS SCIENCE↗
DOE OSTI2015

The effect of postprocessing on tensile property and microstructure evolution of friction stir welding aluminum alloy joint

Friction stir welding is an efficient manufacturing method for joining aluminum alloy and can dramatically reduce grain size conferring excellent plastic deformation properties. Consequently, friction stir welding is used to manufacture tailor welded blanks to optimize weight or performance in the final component. In the study, the microstructural evolution and mechanical properties of friction stir welding joint during plastic forming and subsequent heat treatment were investigated. The microstructural characteristics of the friction stir welding joints were studied by Electron Backscattered Diffraction and Transmission Electron Microscopy. The mechanical properties were evaluated by tensile and microhardness tests. It is found that the tensile and yield strengths of friction stir welding joints are significantly improved after severe plastic deformation due to the grain refinement. Following heat treatment, the strength of the friction stir welding joints significantly decrease due to the obvious abnormal grain growth. Careful attention must be given to the processing route of any friction stir welding joint intended for plastic forming, especially the annealing between forming passes. Severe plastic deforming of the friction stir welding joint leads to a high level of stored energy/dislocation density, which causes the abnormal grain growth during subsequent heat treatment, and consequently reduce the mechanical properties of the friction stir welding joint. - Highlights: • Great changes are observed in the microstructure of FSW joint after postprocessing. • Postprocessing shows great effect on the microstructure stability of FSW joint. • The weld shows more significant decrease in strength than the BM due to the AGG. • Attention must be given to the processing route of FSW joint for plastic forming.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructure, Mechanical Properties and Residual Stress of Selective Laser Melted AlSi10Mg

AlSi10Mg processed by selective laser melting (SLM) is common in various industries because of its complex structure and high performance. The microstructure, residual stress and mechanical properties restrict its application, while they are affected by the scanning path type and preheating temperature. In this work, to investigate the properties of selective laser melted AlSi10Mg alloys and gain better performance results, the microstructure and mechanical tests are performed at several preheating temperatures based on the uniformity and chessboard scanning strategy. It is found that the selective laser melted AlSi10Mg parts fabricated in the chessboard scanning path have better mechanical properties than those fabricated in the uniformity scanning path. Furthermore, a higher preheating temperature can induce less residual stress due to the enhanced Al crystal faces. Finally, analyses of the microstructures, mechanical and residual stress provide a valuable suggestion that the combination of the range of preheating temperature and the scanning path can improve the performance of selective laser melted AlSi10Mg.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Microstructure and properties of a high temperature Al–Ce–Mn alloy produced by additive manufacturing

An Al–10Ce-8Mn (wt%) alloy was designed and fabricated by laser powder bed fusion additive manufacturing (AM). The rapid cooling rates of the AM process produced a refined microstructure with a large fraction of reinforcing intermetallic phases. The tensile properties of the alloy were characterized in the as-fabricated state and following thermal exposure. The properties of the as-fabricated microstructure showed exceptional high-temperature performance and strength retention at elevated temperatures up to 400 °C relative to benchmark wrought Al and AM Al alloy properties. Characterization of the microstructure and thermodynamic modeling of the ternary Al–Ce–Mn system rationalized the solidification and solid-state phase transformations. Finally, analysis of the relevant strengthening mechanisms for both the as-fabricated and thermally exposed conditions was performed.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Solution Treatment on the Microstructure, Micromechanical Properties, and Kinetic Parameters of the β → α Phase Transformation during Continuous Cooling of Ti-6Al-4V Titanium Alloy

The aim of this study is to examine the effect of solution treatment temperature (STT) on the microstructure, the micromechanical properties, and the kinetic parameters of the β → α phase transformation during continuous cooling of the dual phase titanium alloy Ti-6Al-4V. Increasing the STT from 1050 to 1200 °C delays the formation of the α phase during cooling and increases the value of its activation energy. The microstructural analysis reveals the emergence of α{sub W} platelets from protuberances on the α{sub GB}/α{sub W} interface. The investigation of the morphology of the α{sub W} platelets reveals the presence of ledges on their longest side showing a sharp extremity. The micromechanical properties determined by nanoindentation and microhardness tests are almost insensitive to the cooling rate but are strongly affected by the STT; the higher the STT, the lower the overall microhardness of the Ti-6Al-4V alloy. In addition, the STT affects the microhardness and the Young’s modulus of both α and β phases differently; when the STT increases, the microhardness and the Young’s modulus of the α phase decrease, whereas those of the β phase increases.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Nb micro-alloying on microstructure and properties of thermo-mechanically processed high carbon pearlitic steel

Highlights: • Effect of Nb micro-alloying on high carbon steels has been established. • Fine and degenerated pearlite with fine PAGS is achieved due to Nb micro-alloying. • AFM study indicates true interlamellar spacing which conforms well to TEM study. • Hardness and yield strength have been obviously improved with the addition of Nb. - Abstract: Two C-Mn-Si steels with and without Nb micro-alloying are selected in the present study. Both these high carbon steels have been thermo-mechanically processed using Gleeble 3800 simulator. Optical microscope (OM), scanning electron microscope (SEM), transmission electron microscope (TEM), atomic force microscope (AFM) were utilised for microstructural characterisation. The austenitising temperature was varied from 1150 °C to 1200 °C followed by hot compression and subjected to free cooling to evaluate the influence of austenite grain size on transformed microstructure and mechanical properties. It is evident that higher austenite grain size is obtained for both types of steels subjected to higher austenitising temperature. The refinement of pearlite interlamellar spacing (<0.20 μm) with degenerated morphology as well as finer prior austenite grain size (<40 μm) is found to be more prominent for Nb micro-alloyed sample. The average hardness values of both the steels are higher for the specimens, treated at a higher austenitising temperature which is attributed to finer interlamellar spacing. Finally, the correlation between the evolving microstructure and resulting mechanical properties (hardness and yield strength) has been made.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Predicting melt pool depth and grain length using multiple signatures from in-situ single camera two-wavelength imaging pyrometry for laser powder bed fusion

In laser powder bed fusion (LPBF), the in-situ process signatures are known to have a direct correlation with the microstructural properties of the solidified melt pool (MP). It is known that the MP cooling and heating rates, and laser processing parameters can critically determine the grain structure and thereby affect the part properties. The objective of this work is to study the feasibility of using in-process, high-speed imaging pyrometry for evaluating the solidified MP properties “below” the surface, such as depth and microstructural properties. To accomplish this, we employ an in-house single camera-based two-wavelength imaging pyrometry (STWIP) system for monitoring the printing of single-scan tracks with Inconel 718 on a commercial LPBF printer (EOS M290). Further, the lab designed STWIP system is a coaxial high-speed (>10,000 fps) imaging system capable of monitoring MP temperature, morphology, and intensity profiles. The temperature measurements from STWIP are emissivity independent. The STWIP measured MP signatures of the printed tracks are correlated with the ex-situ microscopy characterized MP depth and the average grain lengths. From the data analysis, using support vector machine (SVM)-based regression models, we found that the MP temperature signatures are crucial for an accurate prediction of MP depth and the grain length, thus validating the novelty and necessity of the developed in-situ monitoring methods and analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2019

High-Temperature Properties and Microstructural Stability of the AISI H13 Hot-Work Tool Steel Processed by Selective Laser Melting

The microstructural stabilities, softening resistance, and high-temperature tensile properties of the H13 hot-work tool steel by selective laser melting (SLM) were systematically studied. A series of tempering procedures were performed on the as-SLMed specimens. Afterwards, the mechanism of softening resistance behavior was discussed based on the XRD, SEM, EBSD observations, hardness measurements, and high-temperature tensile tests. It was found that the as-SLMed H13 consisted of α-iron and γ-iron. The carbide-stabilizing elements aggregated as the cell-like substructures for the rapid solidification of the SLM process. After the softening resistance treatment, the retained austenite transformed to ferrite and carbide mixtures. The cell-like substructures dissolved slowly into the matrix when the temperature was below 550 °C. These factors increased the hardness and retarded the softening of the material. When the temperature was 600 °C, the microstructural constituents transformed to soft ferrite and globular carbides, which lead to a considerable decrease of the hardness. Due to the grain refinement, solid solution strengthening, and residual stress, the as-SLMed H13 exhibited better mechanical properties than that of the wrought counterparts.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Tempering Temperature on the Microstructure and Properties of Fe-2Cr-Mo-0.12C Pressure Vessel Steel

To obtain the high-temperature strength and toughness of the medium–high-temperature–pressure steel, the microstructure evolution and mechanical properties of Fe-2Cr-Mo-0.12C steel subjected to three different tempering temperatures after being normalized were investigated. The results show that the microstructure of the sample, tempered in the range 675-725 °C for 50 min, did not change dramatically, yet the martensite/austenite constituents decomposed, and the bainite lath merged together and transformed into polygonal ferrite. At the same time, the precipitate size increased with an increase in tempering temperature. With the increase in the tempering temperature from 675 to 725 °C, the impact absorbed energy of the Fe-2Cr-Mo-0.12C steel at −40 °C increased from 257 to 325 J, and the high-temperature yield strength decreased; however, the high-temperature ultimate tensile strength tempered at 700 °C was outstanding (422-571 MPa) at different tested temperatures. The variations of the properties were attributed to the decomposition of M/A constituents and the coarsening of the precipitates. Fe-2Cr-Mo-0.12C steel normalized at 930 °C and tempered at 700 °C was found to have the best combination of ductility and strength.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effect of loading orientations on the microstructure and property of Al−Cu single crystal during stress aging

The precipitation behavior and property of Al−Cu alloy during stress aging under various loading orientations were investigated using single crystals. The resulting microstructures and the strength property were examined by transmission electron microscope (TEM) and compression test, respectively, and the effect of the distribution of θ′-plates on strength property were discussed. The results show that the precipitation distribution of θ′ was significantly affected by the loading orientation during stress aging of Al−Cu single crystals. Loading along close to 〈011〉{sub Al} directions provided more uniform precipitation distribution of θ′ as compared to loading along close to 〈001〉{sub Al} directions, and therefore provided higher strengthening stress of the θ′-plates for the stress aging sample. The results suggested that regulating the distribution of θ′ and therefore improving strength property are possible via controlling the loading orientation during stress aging. - Highlights: • We studied the effect of loading directions on stress aging of Al−Cu single crystal. • Precipitation distribution of θ′ was noticeably affected by the loading direction. • Loading along close to 〈011〉{sub Al} directions reduced the stress-orienting effect. • The strength property is closely related to the precipitation distribution of θ′. • It is possible to regulate the distribution of θ′ and improve strength property.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Microstructure and Property Evolution in Advanced Cladding and Duct Materials Under Long-Term Irradiation at Elevated Temperature: Critical Experiments

The in-service degradation of reactor core materials is related to underlying changes in the irradiated microstructure. During reactor operation, structural components and cladding experience displacement of atoms by collisions with neutrons at temperatures at which the radiation-induced defects are mobile, leading to microstructure evolution under irradiation that can degrade material properties. At the doses and temperatures relevant to fast reactor operation, the microstructure evolves by microchemistry changes due to radiation-induced segregation, dislocation loop formation and growth, radiation induced precipitation, destabilization of the existing precipitate structure, as well as the possibility for void formation and growth. These processes do not occur independently; rather, their evolution is highly interlinked. Radiation-induced segregation of Cr and existing chromium carbide coverage in irradiated alloy T91 track each other closely. The radiation-induced precipitation of Ni-Si precipitates and RIS of Ni and Si in alloys T91 and HCM12A are likely related. Neither the evolution of these processes nor their coupling is understood under the conditions required for materials performance in fast reactors (temperature range 300-600°C and doses to 200 dpa and beyond). Further, predictive modeling is not yet possible, as models for microstructure evolution must be developed along with experiments to characterize these key processes and provide tools for extrapolation. To extend the range of operation of nuclear fuel cladding and structural materials in advanced nuclear energy and transmutation systems to that required for the fast reactor, the irradiation-induced evolution of the microstructure, microchemistry, and the associated mechanical properties at relevant temperatures and doses must be understood. This project builds upon joint work at the proposing institutions, under a NERI-C program that is scheduled to end in September, to understand the effects of radiation on these important materials. The objective of this project is to conduct critical experiments to understand the evolution of microstructural and microchemical features (loops, voids, precipitates, and segregation) and mechanical properties (hardening and creep) under high temperature and full dose range radiation, including the effect of differences in the initial material composition and microstructure on the microstructural response, including key questions related to saturation of the microstructure at high doses and temperatures.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗