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At least 1,225 records · Page 68
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Low Temperature and Surfactant-Free Hydrothermal Synthesis of CoNi Nanoparticles: Structure, Microstructure, and Magnetic Properties

We report on the synthesis of Co{sub 30}Ni{sub 70} nanoparticles using hydrothermal method at low temperatures and short times (100 °C, 2 h) without any surfactant or external magnetic field. The effect of NaOH concentration on the crystal structure, microstructure, and magnetic properties of CoNi samples has been investigated by x-ray diffraction (XRD), scanning (SEM) and high-resolution transmission (HRTEM) electron microscopy, and vibrating sample magnetometry (VSM). From the Rietveld refinement of x-ray powder diffraction patterns, we have evidenced the coexistence of two phases with face-centered cubic (FCC) and hexagonal (HCP) crystal structures, being 12 nm and 3 nm, respectively, the values for the mean grain size of both phases. SEM images show that the basic microstructure is composed of quasi-spheres and a chain-like morphology appears with increasing the amount of NaOH. HRTEM images evidence the formation of such chains, and confirm the coexistence of FCC and HCP phases. The magnetic hysteresis loops show a clear dependence of the coercivity on the particle morphology indicating the role played by the magnetic shape anisotropy.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2023

Unveiling the microstructural evolution of carbon fibers derived from polyamide-6

Polyacrylonitrile-based carbon fibers have dominated the industry for decades, but the high cost of polyacrylonitrile has prevented the widespread adoption of carbon fiber in high-volume structural applications. As such, a significant amount of research has been dedicated to finding an alternative, low-cost carbon fiber precursor. In this work, carbon fibers were produced from polyamide-6 using metal salt impregnation and a thermo-oxidative stabilization step. To gain further insight into the carbonization process and microstructural transformation, the morphologies, crystallinities, elemental compositions, and thermal stabilities of the fibers were characterized at various stages of processing. The stabilization step resulted in a significant increase in carbon yield, indicating a dramatic increase in thermal stability. This is due to the crosslinking of polyamide-6 chains, which was confirmed by functional group analysis. The crystallinity of the fibers was also significantly altered during processing, as the produced carbon fibers consisted of pseudo-amorphous carbon with two distinct regions of metal salt impregnation. Finally, the findings and microstructural evolution mechanisms provide guidelines for further research into carbon fiber produced from polyamide-6.

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 OSTI2019

Microstructure Development of 308L Stainless Steel During Additive Manufacturing

$In$ $situ$ high-energy X-ray diffraction measurements were completed during deposition of 308L stainless steel wire onto a 304L stainless steel substrate. Attempts were made to extract microstructural features such as phase fraction and internal stress, as well as temperature evolution immediately following the deposition. The limited data that could be collected during deposition and rapid solidification are critically examined. High-energy X-rays coupled with relatively slow detectors were utilized to enable determination of orientation-dependent lattice parameters accurately enough to comment on phase strain evolution between austenite and ferrite. Here, information about the hydrostatic and deviatoric stress states of the constituent phases was determined on time scales that are relevant to their development. However, the time resolution of the technique was insufficient to monitor phase evolution during the solid–solid phase transformation and, more so, during solidification. Moreover, the accurate and absolute determination of inherently statistical parameters, such as phase fraction, depends critically on the ability to sample a statistically significant numbers of grains in the microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructural Characterization of Pure Tin Produced by the Drop-on-Demand Technique of Liquid Metal Jetting

The microstructure–property relationship of a pure tin part built using the drop-on-demand technique of liquid metal jetting, a cost–effective alternative to selective laser-melting or sintering techniques, was determined. Here, the microstructure of the as-built tin is observed to have minimal stored strain, low dislocation density, few to no voids, and the presence of only the β-tin phase; concurrently, mechanical properties are shown to be identical to the traditionally manufactured tin.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Accumulative Roll Bonding of Alloy 2205 Duplex Steel and the Accompanying Impacts on Microstructure, Texture, and Mechanical Properties

The mechanical and microstructural evolution of Alloy 2205 during severe plastic deformation is examined in this study. A combination of accumulative roll bonding (ARB) and cold rolling results in the successful formation of a nanograined dual-phase microstructure of austenite and ferrite with some transformed martensite. Severe deformation to cumulative reductions of 80.5, 92.5, 95, and 97 pct were performed. Microscopy indicates that grain dimensions in the sheet normal direction is less than 100 nm for reductions ≥ 92.5 pct. Shear banding is observed at reductions ≥ 95 pct while twinning is only observed at reductions < 92.5 pct. Neutron diffraction measurements indicated the presence of martensite for reductions ≥ 95 pct at ~ 8 pct volume fraction. Taken in conjunction, it appears that during initial ARB processing, both slip and twinning are active plastic mechanisms. As twinning becomes exhausted, martensitic transformation, slip, and intermittent shear banding account for the active plasticity mechanisms. Material hardness saturates at 92.5 pct reduction, with a maximum hardness of 45 HRC. Sub-sized tensile testing confirms this approximate hardness with measurements indicating a UTS of ~ 1440 MPa. Texture analysis of crystal orientation distributions in the plate normal direction suggest an approximate Kurdjumov–Sachs orientation relationship at all reductions above 80 pct indicating stability of the orientation relationship at high strains. The intragranular structure develops a fine scale sub-grain content with increasing deformation, resulting in a continual evolution of texture up to and including 97 pct reduction. The final structure presents strong components of Goss and rotated cube texture in both the austenite and ferrite. In this body of work we aim to compare ARB of an industrially relevant FCC/BCC system (Alloy 2205) to historical model FCC/BCC systems such as Cu/Nb.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Influence of Molybdenum on Rapid Solidification Microstructure and Microsegregation in Primary Ferrite Solidified Stainless Steel

Due to the widespread use and familiarity of austenitic stainless steels in many industries these alloys are often the first materials used when adapting new processing techniques. The rapid cooling and solidification rates that occur during fusion based additive manufacturing processes like powder bed fusion cause a fundamental shift in the solidification behavior of the material. While the effects that Cr and Ni have on the microstructure have been fairly well documented across a range of solidification conditions, the impact of alloying elements like Mo are not as well understood at rapid solidification rates. For this study, four custom stainless steel alloy feedstocks were made with targeted modification of the Cr and Mo concentrations to maintain a constant Cr/Ni eq ratio of ~1.7. Two-piston splat quenching was used to produce rapidly solidified samples and the solidification mode, phase, and cell size were investigated. Solidification rates were estimated to be between 0.4 and 1.5m/s. A comparison of the microsegregation and partitioning behavior of Cr, Ni and Mo in ferrite solidified material was also performed for the different alloy compositions. Variations of the Mo concentration between each feedstock showed no measurable influence on the solidification/cooling rates, solidification morphology, or the partitioning of Mo. Furthermore, higher concentrations of Mo were found to significantly increase the amount of ferrite phase in the microstructure by suppressing the ferrite to austenite massive transformation.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The Influence of Nominal Composition on the Microstructure, Tensile Properties, and Weldability of Cast Monel Alloys

Cast Monel alloys are used in many industrial applications that require a combination of good mechanical properties and excellent resistance to corrosion. Despite relative widespread use, there has been limited prior research investigating the fundamental composition–structure–property relationships. Here in this work, microstructural characterization, thermal analysis, electron probe microanalysis, tensile testing, and Varestraint testing were used to assess the effects of variations in nominal composition on the solidification path, microstructure, mechanical properties, and solidification cracking susceptibility of cast Monel alloys. It was found that Si segregation caused the formation of silicides at the end of solidification in grades containing at least 3 wt pct Si. While increases to Si content led to significant improvements in strengthening due to the precipitation of β 1 -Ni 3 Si, the silicide eutectics acted as crack nucleation sites during tensile loading which severely reduced ductility. The solidification cracking susceptibility of low-Si Monel alloys was found to be relatively low. However, increases to Si concentration and the onset of associated eutectic reactions increased the solidification temperature range and drastically reduced cracking resistance. Increases in the Cu and Mn concentrations were found to reduce the solubility limit of Si in austenite which promoted additional eutectic formation and exacerbated the reductions in ductility and/or weldability.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Characterization and Rationalization of Microstructural Evolution in GRCop-84 Processed by Laser-Powder Bed Fusion (L-PBF)

In this study, prismatic geometries of GRCop-84 [Cu-8Cr-4Nb (at. pct)] were built with laser-powder bed fusion (L-PBF) process. The samples were sectioned parallel or perpendicular to the build direction and characterized in the as-built and after post-processing with a hot-isostatically pressing (HIP) treatment. The microstructure and phase evolutions were evaluated with optical microscopy, scanning electron microscopy (SEM), electron backscattered diffraction (EBSD), and high-temperature X-ray diffraction (HTXRD) up to 1223 K. The samples in the as-built conditions exhibited predominantly columnar epitaxial and misoriented Cu-FCC grains. The microstructure evolutions are discussed based on locations within the overall build geometry, the dynamics of small melt pool shape and sectioning effects. The above grain structure did not change significantly during post-process HIP treatment. The stability of this FCC grain structure is attributed to the formation of primary stable Cr 2 Nb (Laves phase) during L-PBF, even before the emergence of FCC grains from liquid. The stability of Cr 2 Nb in both as-built and HIPed samples were evaluated using high-temperature X-ray diffraction measurements and compared with that of gas-atomized powder. The significance of these results is discussed with reference to aerospace applications.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural Evolution of Al-1Fe (Weight Percent) Alloy During Accumulative Continuous Extrusion Forming

As a new microstructure refining method, accumulative continuous extrusion forming (ACEF) cannot only refine metal matrix but also refine the phases that exist in it. In order to detect the refinements of grain and second phase during the process, Al-1Fe (wt pct) alloy was processed by ACEF, and the microstructural evolution was analyzed by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Results revealed that the average grain size of Al-1Fe (wt pct) alloy decreased from 13 to 1.2 μm, and blocky Al{sub 3}Fe phase with an average length of 300 nm was granulated to Al{sub 3}Fe particle with an average diameter of 200 nm, after one pass of ACEF. Refinement of grain was attributed to continuous dynamic recrystallization (CDRX), and the granulation of Al{sub 3}Fe phase included the spheroidization resulting from deformation heat and the fragmentation caused by the coupling effects of strain and thermal effect. The spheroidization worked in almost the entire deformation process, while the fragmentation required strain accumulation. However, fragmentation contributed more than spheroidization. Al{sub 3}Fe particle stimulated the formation of substructure and retarded the migration of recrystallized grain boundary, but the effect of Al{sub 3}Fe phase on refinement of grain could only be determined by the contrastive investigation of Al-1Fe (wt pct) alloy and pure Al.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Interfacial Microstructural Evolution and Metallurgical Bonding Mechanisms for IN718 Superalloy Joint Produced by Hot Compressive Bonding

The novel metallurgical joining process for bonding IN718 superalloy was investigated by hot compressive bonding (HCB) process under the deformation temperature range of 1000 °C to 1150 °C and true strains ranging from 0 to 0.5 at a strain rate of 0.001 s{sup −1}. The effect of HCB process parameters on the tensile strength was analyzed. Both the as-deformed and the interfacial microstructures were characterized using the optical microscope, electron backscattered diffraction and transmission electron microscope (TEM) analysis. The results of tensile property revealed that the degree of metallurgical bonding is promoted by increasing deformation temperature and strain. The evolution of the interfacial microstructure showed that the migration of interfacial grain boundary (IGB), which is characterized by discontinuous dynamic recrystallization, is the dominant metallurgical bonding mechanism in the early stages of bonding. TEM analysis indicated that the dislocation density is distributed heterogeneously over both sides of IGB, which is the significant reason for the migration of IGB, during the initial stage of HCB process.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influences of Quench Cooling Rate on Microstructure and Corrosion Resistance of Al-Cu-Mg Alloy Based on the End-Quenching Test

To investigate the effects of the quench cooling rate on corrosion resistance of Al-Cu-Mg alloy, an end-quenching test was conducted and the microstructures at different cooling rates were observed by SEM and TEM. Additionally, the corrosion resistance was characterized by an intergranular corrosion test and electrochemical test. Moreover, the finite element method was applied to simulate the end quenching process. The results indicate that the actual end quenching process can be approximated as one-dimensional heat transfer, and the cooling rate varies at different cooling distances. By affecting the microstructures, decreasing the cooling rate leads to a decline in the corrosion properties. Low cooling rates coarsen the constituent particles and grain boundary particles, resulting in a wide precipitation-free zone and an increase in the intensity of corrosion reactions. A high cooling rate concentrates on the intragranular precipitant, which can reduce the pitting depth and represents a conversion from localized corrosion to general corrosion.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Electron Backscattered Diffraction Study of Microstructural Evolution During Isothermal Deformation of High-N Mn18Cr18 Alloy

In order to understand the dynamic recrystallization (DRX) mechanism of Mn18Cr18N austenitic stainless steel during hot deformation, the investigation of microstructure evolution is significant. Isothermal compression tests were conducted on a Gleeble-3500 thermomechanical simulator in the temperature range of 950 °C to 1150 °C and strain rate range between 0.001 and 1 s{sup −1}. Optical microscopy (OM) and electron backscattered diffraction (EBSD) were employed to study the resultant microstructures. More grain boundary information of hot-deformed specimens was provided by EBSD. It was found that the fraction of low-angle grain boundaries (LAGBs) increases with the decrease of deformation temperature or the increase of strain rate and can be expressed as a function of the Zener–Hollomon parameter. DRX easily occurs at the high deformation temperature and low strain rate. From the flow stress curves, the occurrence of single peak behavior and multiple transient steady-state (MTSS) behavior illustrated the existence of different DRX mechanisms. The EBSD analysis indicated that both continuous dynamic recrystallization (CDRX) and discontinuous dynamic recrystallization (DDRX) existed during hot deformation. For the low fraction of 10 to 15 deg misorientation, CDRX is the minor DRX mechanism while DDRX is the major DRX mechanism for the studied steel.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Fluid Dynamics Effects on Microstructure Prediction in Single-Laser Tracks for Additive Manufacturing of IN625

Single-track laser fusion were simulated using a heat-transfer-solidification-only (HTS) model and its extension with fluid dynamics (HTS_FD) model using a parallel open-source code, which included laminar fluid dynamics, flat-free surface of the molten alloy, heat transfer, phase-change, evaporation, and surface tension phenomena. The results illustrate that the fluid dynamics affects the solidification and ensuing microstructure. For the HTS_FD simulations, thermal gradient, G was found to exhibit a maximum at the extremity of the solidified pool ( i.e. , at the free surface), while for HTS simulations, G exhibited a maximum around the entire edge of the solidified pool. HTS_FD simulations predicted a wider range of cooling rates than the HTS simulations, exhibited an increased spread in the solidification speed, V variation within the melt-pool with respect to the HTS model results. Primary dendrite arm spacing (PDAS) were evaluated based on power law correlations and marginal stability theory models using the ( G , V ) from HTS and HTS_FD simulations to quantify the effect of the fluid dynamics on the microstructure. At low-laser powers and low-scan speeds, the PDAS obtained with the fluid dynamics model (HTS_FD) was larger by more than 30 pct with respect to the PDAS calculated with the simple HTS model. A new PDAS correlation, i.e. , \( \lambda_{1} \left[ {\mu {\text{m}}} \right] = 832\;G\left[ {\text{K/m}} \right]^{ - 0.5} V\left[ {\text{m/s}} \right]^{ - 0.25} \) , which uses the ( G , V ) results from the HTS_FD model was developed and validated against experimental results.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructure and Thermal Stability of A357 Alloy With and Without the Addition of Zr

The principal purpose of this research was to evaluate the effects of Zr on the microstructure and thermal stability of an A357 alloy that has been subjected to an aging treatment (T6) and thermal exposure (250 °C). The results show that the addition of Zr had a significant influence on the refinement of the grain size, which enhanced the hardness and tensile strength of the A357 alloy under the T6 condition. During thermal exposure at 250 °C, the rodlike metastable β’-Mg{sub 2}Si precipitates transformed into coarse equilibrium phase β-Mg{sub 2}Si precipitates, resulting in a significant drop in the hardness and tensile strength of the T6 heat-treated A357 alloy. However, after thermal exposure, coherent, finely dispersed Al{sub 3}Zr precipitates were found to be formed in the T6 heat-treated A357 alloy. The addition of 0.1% Zr played a critical role in improving the high-temperature strength. Consequently, the A357 alloy with the addition of Zr demonstrated better mechanical properties at room temperature and high temperature than the alloy without Zr, in terms of both microstructure and thermal stability.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Post-deformation Annealing Treatment on the Microstructural Evolution of a Cold-Worked Corrosion-Resistant Superalloy (CRSA) Steel

The post-deformation annealing treatments of a commercial cold-worked corrosion-resistant superalloy steel (Sanicro 28 steel) were carried out at different temperatures in the range of 900-1100 °C for different holding durations of 5, 10, and 15 min. The effects of post-deformation annealing time and temperature on the microstructural evolution and subsequent mechanical properties of the processed Sanicro 28 steel were investigated. The observations indicated that twin–twin hardening in cold deformation condition mainly correlates with abundant nucleation of mechanical twins in multiple directions resulting in considerable strain hardening behavior. Microstructural investigations showed that the static recrystallization takes place after isothermal holding at 900 °C for 5 min. Increasing the annealing temperature from 900 to 1050 °C leads to recrystallization development and grain refinement in the as-recrystallized state. In addition, an increase in annealing duration from 5 to 15 min leads to subgrain coarsening and subsequently larger recrystallized grains size. The occurrence of large proportion of the grain refinement, which is achieved in the first annealing stage at 1050 °C after 5 min, is considered as the main factor for the maximum elongation at this stage.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Quenching Process on Microstructures and Mechanical Properties of Fe-0.9Mn-0.5Cr-2.4Ni-0.5Mo-C Steel

To develop an appropriate quenching process to produce Fe-0.9Mn-0.5Cr-2.4Ni-0.5Mo-C steel, the microstructures and mechanical properties of this steel were investigated under the direct quenching and tempering (DQT) and the direct quenching, reheated quenching and tempering (DQQT) heat treatment processes. The microstructure of the DQQT specimen was basically tempered sorbite with spherical precipitates, while quite a bit of tempered martensite was in the DQT specimen with dispersive nanoscaled precipitates. The yield strengths of the DQT and DQQT specimens were 1154 and 955 MPa, respectively. The yield strength of the DQT specimen was higher than that of the DQQT specimen because of its finer grain size, higher density of dislocations and dispersed precipitates. The DQQT specimen had spherical precipitates, which hindered the propagation of the crack. Moreover, the high-angle grain boundaries in the DQQT specimen took a higher proportion. Therefore, the Charpy impact values of DQT and DQQT specimens at − 60 °C were 38 and 75 J, respectively. Consequently, the mechanical properties of the Fe-0.9Mn-0.5Cr-2.4Ni-0.5Mo-C steel, which met the standard of 1000 MPa grade steel plate for hydropower station, were acquired by the DQQT process.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural Evolution and the Precipitation Behavior in X90 Linepipe Steel During Isothermal Processing

Thermomechanical controlled processing of 560-MPa (X90) linepipe steel was simulated in the laboratory using a thermomechanical simulator to study the microstructural evolution and precipitation behavior during isothermal holding. The results indicated that martensite was obtained when the steels were isothermally held for 5 s at 700 °C. Subsequently, granular bainite and acicular ferrite transformation occurred with increased holding time. Different amount of polygonal ferrite formed after isothermally holding for 600-3600 s. Pearlite nucleated after isothermally holding for 3600 s. Precipitation occurred after isothermal holding for 5 s and continuous precipitation occurred at grain boundaries after isothermally holding for 600 s. After isothermally holding for 3600 s, large Nb/Ti carbide precipitated. The presence of MX-type precipitates was confirmed by diffraction pattern. The interphase precipitation (IP) occurred between 5 and 30 s. Maximum hardness was obtained after isothermally holding for 600 s when IP occurred and rapidly decreased to a low value, mainly because polygonal ferrite dominated the microstructure after isothermally holding for 3600 s.

36 MATERIALS SCIENCE↗