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At least 1,045 records · Page 58
All sourcesNASA NTRSDOE OSTI
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 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

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 OSTI2018

Effect of Final Cooling Temperature on Microstructure and Mechanical Properties of a Cr-Ni-Mo-V Bainite Steel

The microstructural evolution and mechanical properties of a low-carbon high-strength bainitic steel under different final cooling temperatures were studied. The microstructures of the experimental steel at different final cooling temperatures were composed of acicular ferrite and granular bainite. A decrease in final cooling temperature resulted in an increase in volume fraction of granular bainite and a decrease in volume fraction of acicular ferrite. The specimen with the lowest final cooling temperature (459 °C) exhibited the highest yield strength, tensile strength, and yield ratio, and a lower total elongation than the specimens with the highest final cooling temperatures (501 and 535 °C) because of the higher volume fraction of granular bainite and finer bainitic ferrite lath. The specimen with the lowest final cooling temperature had a lower absorbed energy than that of the highest final cooling temperature, because the strip-like martensite–austenite (M-A) constituents that existed between the bainitic ferrite or in prior austenite grain boundaries reduced its toughness. At an intermediate final cooling temperature of 501 °C, the experimental steel exhibited excellent mechanical properties with a yield strength, tensile strength, and absorbed energy of 825 MPa, 1232 MPa, and 102 J, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Hot Rolling on the Microstructure and Mechanical Properties of Nitrogen Alloyed Austenitic Stainless Steel

In the present investigation, the effect of multi-pass hot rolling in the temperature range of 700–1000 °C on the microstructure and mechanical properties of nitrogen alloyed austenitic stainless steel was studied with the aid of optical microscopy, tensile testing and x-ray diffraction measurements. The microstructural changes that occurred in the hot rolled specimens were elongation of grains in rolling direction, nucleation of new grains at the grain boundaries of elongated grains and growth of nucleated grains to form fully recrystallized grains. Elongated grains formed at lower rolling temperature (700–800 °C) due to inadequate strain/temperature for the initiation of dynamic recrystallization. At higher rolling temperature (900–1000 °C), fine grains formed due to dynamic recrystallization. Tensile properties showed strong dependency on the rolling temperature. Tensile strength increased with the decrease in the rolling temperature at the cost of ductility. Maximum strength was observed in samples hot rolled at 700 °C with yield strength of 917 MPa and ductility of 25%. This variation in the tensile properties with the rolling temperature is attributed to changes in the dislocation density and grain structure. The estimated yield strength from the dislocation density, solid solution and grain boundary strengthening closely matched with experimentally determined yield strength confirming the role of dislocation density and grain size in the strengthening.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effects of Stress Ratio and Microstructure on Fatigue Failure Behavior of Polycrystalline Nickel Superalloy

The effects of microstructure and stress ratio on high cycle fatigue of nickel superalloy Nimonic 80A were investigated. The stress ratios of 0.1, 0.5 and 0.8 were chosen to perform fatigue tests in a frequency of 110 Hz. Cleavage failure was observed, and three competing failure crack initiation modes were discovered by a scanning electron microscope, which were classified as surface without facets, surface with facets and subsurface with facets. With increasing the stress ratio from 0.1 to 0.8, the occurrence probability of surface and subsurface with facets also increased and reached the maximum value at R = 0.5, meanwhile the probability of surface initiation without facets decreased. The effect of microstructure on the fatigue fracture behavior at different stress ratios was also observed and discussed. Based on the Goodman diagram, it was concluded that the fatigue strength of 50% probability of failure at R = 0.1, 0.5 and 0.8 is lower than the modified Goodman line.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Current-Assisted Diffusion Bonding of Extruded Ti-22Al-25Nb Alloy by Spark Plasma Sintering: Interfacial Microstructure and Mechanical Properties

Spark plasma sintering (SPS) technology was used to current-assisted bond extruded Ti-22Al-25Nb alloy. The effects of bonding temperature (920-980 °C) and bonding time (10-30 min) on the microstructure evolution and shear strength of this alloy were investigated systematically. The temperature distribution in the specimen during the current-assisted bonding process was also analyzed by numerical simulation. It is noted that the highest temperature was obtained at the bonding interface. As the bonding temperature and bonding time increased, the voids in the interface shrank increasingly until they vanished. A complete metallurgical bonding interface could be produced at 960 °C/20 min/10 MPa, exhibiting the highest shear strength of 269.3 MPa. In addition, the shear strength of the bonded specimen depended on its interfacial microstructure. With increased bonding temperature, the fracture mode transformed from the intergranular fracture at the bonding interface to the cleavage fracture in the substrate.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Study on Microstructures and Mechanical Properties of Foam Titanium Carbide Ceramics Fabricated by Reaction Sintering Process

Foam titanium carbide (TiC) ceramics with a three-dimensional network structure were fabricated by the reaction sintering process, in which polyurethane foam was taken as the template, and TiO{sub 2} and phenolic resin were used as the reactants. Phase, microstructures and fracture morphologies of foam TiC ceramics were characterized by x-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The results show that when the mass ratios of phenolic resin and TiO{sub 2} (F/T) are (0.8-1.2): 1, foam TiC ceramics with pure TiC phase can be formed. As the F/T ratios increase, crystal lattice parameters of fabricated foam TiC ceramics become bigger. When the value of F/T decreases from 1.2 to 0.8, grain size of TiC grows larger and microstructures get denser; meanwhile, the compressive strength increases from 0.10 to 1.05 MPa. Additionally, either raising the sintering temperatures or extending holding time can facilitate the completion of the reaction process and increase the compressive strength.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effects of Chromium Additions upon Microstructure and Mechanical Properties of Cold Drawn Pearlitic Steel Wires

Cr-containing pearlitic steel wires were prepared through cold drawing and simulated galvanization process. Effect of chromium microalloying on microstructural and mechanical properties of the steel wires was investigated. Experimental results show that size of pearlitic colonies of the steel rods decreased as Cr content increased from 0.2 to 0.6 wt.%; meanwhile, interlamellar spacing was little affected because of isothermal phase transition in salt bath. The tensile strength of the pearlitic steel rods was increased from 1480 to 1550 MPa. The tensile strength of the Cr-containing cold drawn wires (ε = 1.58) was increased about 33%, and the torsion circle of the wires were about 15 with cleavage fracture. After annealing at 450 °C for 2 min, tensile strength of the wires increased, but torsion circle was decreased to less than 5. As the annealing time increased, the torsion circle of the steel wires with 0.2 wt.% Cr was improved to about 10 with cleavage fracture, while the torsion performance of the wires having high Cr contents remained low because of delamination fracture. The cementite platelets in Cr-containing wires turned into cementite crystal particles during cold drawing. Microstructure observation and thermal analysis have confirmed that thermal stability of cementite was enhanced with the increase of Cr content.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influence of Welding Combined Plastic Forming on Microstructure Stability and Mechanical Properties of Friction Stir-Welded Al-Cu Alloy

A new tailor-welded process, which combines stages of welding, plastic forming, and heat treatment strengthening, was developed to produce a friction stir-welded (FSW) Al-alloy joint. The Al-Cu sheets were FSW under different welding parameters and then were plastic-deformed. The microstructural evolution and mechanical properties of the FSW joint were investigated by scanning electron microscopy and tensile tests. It was found that high heat input during FSW and low solution temperature suppress the abnormal grain growth (AGG) of the joint due to the differential in grain size and grain boundary energy. The microstructure heterogeneity of the FSW joint is effectively improved, as no AGG occurs. The retention of fine equiaxed grains and the increase in the density of precipitates result in excellent mechanical properties. The increase in the strength and micro-hardness of the joint mainly depends on the plastic deformation prior to aging treatment.

36 MATERIALS SCIENCE↗