Electron Backscatter Diffraction Research Articles

Effect of grain size on spall fracture of CrCoNi medium-entropy alloy under Taylor-wave loading

The effect of grain size on spall properties of medium-entropy alloy CrCoNi under Taylor-wave loading is investigated. Three different grain sizes, 300 μm, 20 μm, and 3 μm, are explored. The free surface velocity histories are measured to obtain such quantities as dynamic yield strength and spall strength. With decreasing grain size, there is a slight decrease in spall strength, but a significant increase in damage rate. The shock-recovered samples are characterized with scanning electron microscopy and electron backscatter diffraction. In coarse-grained samples, voids tend to nucleate within grain interiors, while in fine-grained samples, voids nucleate preferentially at grain boundaries (GBs). Molecular dynamics simulations show that the nucleation of intergranular or intragranular voids is dominated by GB–slip and slip–slip intersections, respectively. The higher GB density results in more extensive GB–slip intersections, consistent with the experimental results.

Effect of boron on the microstructure and performance of HIP-prepared high boron steels

High boron steels containing 2 wt% and 3.3 wt% boron were fabricated using hot isostatic pressing (HIP). The enhanced shielding performance of the steel with higher boron content was quantitatively evaluated through Monte Carlo simulations using software Fluka. The steels were studied with XRD and the phase ratio were calculated using Rietveld refinement method. The microstructure of the materials was investigated using electron backscatter diffraction (EBSD). Comprehensive thermal property measurements, complemented by Hamilton thermal conductivity model analysis, were conducted on high boron steels. The results revealed that the decreased overall thermal conductivity in these materials is primarily attributed to two factors: the increased volume fraction of the boride phase and the enhanced interconnectivity among boride particles. These findings provide crucial insights into the thermal behavior of high boron steels. Room temperature tensile tests indicate that high boron content can cause the fracture mode of the material to transition from ductile to brittle. This study provides a detailed analysis of the effects of boron content on various properties of high boron steels, which can serve as shielding materials in fusion reactors. Advances were proposed for optimizing the thermal performance of high boron steels in this study.

Breaking the strength-conductivity paradigm in hypoeutectic Al–Si alloy via annealing-induced Si nanoprecipitation

Hypoeutectic Al–Si alloys are increasingly recognized as promising materials for aluminum conductor cables owing to their remarkable combination of high strength and castability. However, the widespread industrial application of these alloys is limited by their moderate electrical conductivities (ECs). In this study, we explored the effects of direct annealing on the EC, mechanical properties, and microstructure of AA4043 rods fabricated via Properzi continuous casting. The AA4043 rods were annealed at different temperatures (200, 250, 300, and 350 °C) for 4 and 24 h. Direct annealing resulted in a significant improvement in the EC of the rods, with all samples exhibiting an EC improvement from 50 to 58% IACS. However, the mechanical strength of the rods was considerably reduced. The sample annealed at 250 °C for 4 h exhibited the best combination of EC (58.8% IACS), microhardness (43 HV), and ultimate tensile strength (141 MPa) among all the as-prepared samples. The sample annealed at 350 °C for 24 h showed the lowest microhardness (31.8 HV) and ultimate tensile strength (113 MPa), with EC of 58.05% IACS. Electron backscatter diffraction (EBSD) results revealed retained fibrous grains structure with partial recrystallization at a lower annealing temperature of 250 °C, whereas a higher annealing temperature of 350 °C resulted in complete recrystallization leading to coarse equiaxed grains. Transmission electron microscopy (TEM) analysis revealed the formation of nano-Si precipitates in the annealed samples. To understand the diverse contributions of the resistivity mechanisms and microstructural characteristics to EC improvement, a constitutive resistivity model was employed. These findings offer valuable insights into improving the EC and maintaining a delicate balance between the EC and strength of novel Al–Si conductor alloys.

Influence of the direction of ferrite-austenite banding on hydrogen embrittlement of 2205 duplex stainless steel

In this study, the fracture behavior of 2205 duplex stainless steel (DSS) under in-situ hydrogen charging is evaluated. For this purpose, fracture toughness tests are performed on single-edge notched bending specimens, in which hydrogen is introduced electrochemically in-situ, using an acid and a saline electrolyte at different current densities. The hydrogen content of both electrochemically and gaseous pre-charged specimens is measured to assess the influence of the aggressiveness of the environment. Three environments are evaluated: realistic, severe and highly severe. As the microstructure of DSS is characterized by the presence of ferrite and austenite bands, the influence of directionality on fracture toughness is also studied. For this purpose, specimens are machined in two directions, being crack growth parallel to the bands in one case, while crack growth is perpendicular to the bands in the other case. Fracture toughness was found to decrease with increasing current density and in a more aggressive environment, and to increase when crack growth was perpendicular to the bands. The fracture surface was also evaluated, revealing splits in the direction of the bands in all in-situ tests. The origin and propagation of these splits were studied using electron backscatter diffraction scans, concluding that splits propagated through the ferrite-austenite interface.

Friction stir processing of AA6061-T6/graphene nanocomposites: Unraveling the influence of tool geometry, rotation, and advancing speed on microstructure and mechanical properties

This research investigated the effect of tool geometry, rotation, and advancing speed on the microstructure and mechanical properties of aluminum AA6061-T6/graphene nanocomposites fabricated by friction stir processing (FSP) using three conical tools with the pin cone angles (PCAs) of 2, 2.5, and 3°. In the first step of the study, the process was performed with and without graphene nanoplatelets (GNPs) at different rotations (710, 1120, and 1400 rpm) and advancing speeds (80, 125, and 160 mm/min). The yield strength, tensile strength, and microhardness of all the samples were lower than those of the base metal. In the second step of the study, the heat input was controlled by reducing rotations (112, 180, and 280 rpm) and advancing speeds (31.5, 25, and 20 mm/min). The mechanical properties of processed samples were studied by tensile tests and microhardness measurements. Microstructural evolution in samples was analyzed by means of a field emission scanning electron microscope (FESEM) equipped with an X-ray energy dispersive spectrometer (EDS) and electron back-scattered diffraction (EBSD) detector. The results indicated that the mechanical properties were improved in the second step with the increase in the advance per revolution (APR) and the PCA. This was linked to the microstructure evolution in the processed samples affected by process parameters and regulated heat input. The effect of each input variable on the mechanical properties was evaluated by statistical analysis and was validated by analysis of variance (ANOVA). The optimal processing was attained by utilization of PCA, tool rotation, and advancing speed.

Unraveling factors affecting the reversibility of martensitic phase transformation in FeNiCoAlTi shape memory alloys: Insights from HR-EBSD and acoustic emission analysis

The reversibility of the martensitic phase transformation is crucial for the functionality of shape memory alloys. The easier the martensite is pinned, the faster occurs the degradation of the shape memory effect during cyclic loading. This study investigates various factors influencing the stabilization of martensite during deformation of single-crystalline states of the FeNiCoAlTi system. In order to investigate early pinning mechanisms in more detail a 〈011〉 single crystal with expected lower reversibility of the martensitic phase transformation and, consequently, lower superelasticity was chosen. Complementary in situ methods, such as digital image correlation and acoustic emission, were used to characterize the evolution of the martensitic phase transformation and the role of dislocations during deformation. Thereby, experimental evidence was elaborated pointing at mechanisms that so far have been underrated in terms of functional degradation. Beside interaction of martensitic variants and dislocation activity, detwinning, associated with high acoustic energy, was identified as an additional significant factor contributing to reduced reversibility and superelasticity. In addition, high-resolution electron backscatter diffraction measurements were applied for the first time to identify residual stresses in the austenitic matrix, which significantly contribute to the reverse transformation. Micro-mechanical experiments using pillar compression tests were carried out to study the influence of residual back stresses of the austenitic matrix on the reversibility of the martensitic phase transformation. A reduced reversibility was found in the case of the absence of back stresses. The findings from this study foster the understanding of pinning mechanisms during loading of the FeNiCoAlTi shape memory alloy eventually enabling targeted optimization for enhanced superelastic material behavior.

The Influence of Sample Thickness on the Bending Fatigue Performance of PBF-Lb 316L Material

Additive manufacturing, specifically Laser Powder Bed Fusion (PBF-LB), has gained prominence for its capability to produce complex near-net-shaped components. While PBF-LB offers advantages such as lightweight construction and cost-effectiveness, post-processing remains crucial to meet specific design requirements. This study investigates the post-processing technique of severe shot peening (SSP) on PBF-LB-manufactured 316L stainless steel, a material widely used for its favorable mechanical properties and corrosion resistance. The research focuses on the enhancement of bending fatigue properties through SSP treatment, examining the influence of material thickness on fatigue behavior. Comparative analysis reveals the effectiveness of SSP in significantly improving fatigue strength irrespective of variations in material thickness. Mechanical properties are explored for different thicknesses subjected to SSP treatment. Electron Backscatter Diffraction (EBSD) is employed to scrutinize the surface properties of the samples, providing knowledge on the microstructural changes induced by SSP. The study contributes to the understanding of the role of material thickness in the context of SSP treatment, offering a comprehensive exploration of the mechanical and fatigue characteristics of PBF-LB-manufactured 316L stainless steel.

Influence of Grain Size and Film Formation Potential on the Diffusivity of Point Defects in the Passive Film of Pure Aluminum in NaCl Solution

The influence of grain size on the corrosion behavior of pure aluminum and the defect density and diffusion coefficient of surface passive films were investigated using electron backscatter diffraction (EBSD) and electrochemical testing techniques, based on the point defect model (PDM). Samples with three different grain sizes (23 ± 11, 134 ± 52, and 462 ± 203 μm) were obtained by annealing at different temperatures and times. The polarization curves and electrochemical impedance spectroscopy results for the pure aluminum in the 3.5% NaCl solution showed that with decreasing grain size, the corrosion current (icorr) decreased monotonously, giving rise to a noble corrosion potential and a large polarization resistance. The Motte–Schottky results showed that the passive films that formed on pure aluminum with fine grains of 23 ± 11 μm had a low density (3.82 × 1020 cm−3) of point defects, such as oxygen vacancies and/or metal interstitials, and a small diffusion coefficient (1.94 × 10−17 cm2/s). The influence of grain size on corrosion resistance was discussed. This work demonstrated that grain refinement could be an effective approach to achieving high corrosion resistance of passive metals.

Resolving the “megacryst paradox”: Feldspar orientation relationships record crystal mobility in granites

K-feldspar megacrysts are common in silicic plutons, but there is a long-running debate around how they form and what their presence tells us about magmatic systems. Field, textural, and geochemical evidence supports growth in a melt-rich environment, but experimental evidence and phase-equilibria modeling indicate that K-feldspar grows late in the crystallization sequence, when the magma is highly crystalline. We provide a new perspective on this problem by examining the arrangement of plagioclase inclusions within megacrysts to test whether they exhibit the systematic low-energy crystallographic relationships expected from attachment by synneusis in melt-rich environments where crystals have space to rotate. We use electron backscatter diffraction to quantify the crystal orientations and find that the megacrysts’ plagioclase inclusions do occupy these preferred orientations and therefore were incorporated in a melt-rich environment. K-feldspar is also present as an interstitial network, but plagioclase crystals hosted within this network have non-systematic orientations. This transition from systematic to non-systematic plagioclase orientations marks the point at which the crystals formed a rigid, interconnected framework that impeded rotation into low-energy orientations. Phase-equilibria modeling indicates that this transition occurred when the magma was ∼55% crystalline. The remaining ∼45% melt crystallized at the eutectic, forming the interstitial phases. Thus, we resolve the “megacryst paradox”; the megacrysts grew freely in melt, and the groundmass K-feldspar formed after crystal lock-up. Megacrysts therefore provide a detailed textural and chemical record of a critical period in the system’s evolution: the transition from a mobile and potentially eruptible magma to an immobile mush.

FEM-Based Conductive Heat Transfer Analytical Description of Solidification Rate and Temperature Gradient during Lateral Laser Beam Oscillation Welding of Aluminum Alloy.

This study investigates the feasibility of utilizing the finite element method (FEM)-based conductive heat transfer (CHT) analysis simulation to determine temperature gradients and solidification rates at the solid-liquid interface during laser beam oscillation welding. By comparing experimental observations with FEM-based CHT analysis, the underlying microstructural evolution and grain formation during welding were examined. FEM-based CHT enables the calculation of temperature gradients (G) and solidification rates (R), offering insights into the formation of equiaxed structures, which are crucial for suppressing hot cracking. Columnar-to-equiaxed structure transition thresholds, such as G/R and G3/R, accurately predict the emergence of fully equiaxed grain structures, validated by electron backscatter diffraction. This research provides valuable insights into temperature gradients and solidification rates in oscillation welding, guiding process design for achieving refined equiaxed structures and minimizing hot cracks.

The effect of prior austenite grain size on crystallography and variant selection in carbide-free nano-structured bainite

Prior austenite grain size (PAGS) significantly affects the microstructure and in turn the mechanical properties of nano-structured bainite. In this study, information about crystallographic variants/blocks as well as packets has been extracted using electron backscattered diffraction (EBSD) technique for two blocks of nano-baintic steels with different PAGS obtained by austenitization at two different temperatures of 900°C and 1000°C respectively. However, the bainitic fraction has been maintained to be similar by choosing the same isothermal temperature of 250°C for transformation to bainite. The child-parent orientation relationship (OR) was determined to be close to Kurdjumov-Sachs (K-S) using EBSD for larger PAGS specimen while smaller PAGS specimen displayed closeness to K-S OR predominantly and Nishiyama-Wassermann (N-W) OR in some regions. It was observed that a higher PAGS leads to finer bainitic lath thickness, packet size and block width size. Stricter variant selection was found in smaller PAGS sample even though variant pairing was observed between variants of higher misorientation. This hints towards small number of nucleation sites for a grain and space constraint, rather than the tendency for pairing as the reason for selection.

Microstructural modification and enhanced mechanical properties in Zr50-Ti50 alloy via low temperature electron wind force annealing

This study investigates the microstructural transformations and associated property enhancements in a Zr50-Ti50 alloy annealed at only 120 °C with low duty cycle current pulses. Microanalysis with electron backscatter diffraction (EBSD) and X-ray diffraction (XRD) show the formation of alpha lath structure, typically observed in much higher thermal annealing temperatures. EBSD and XRD analyses revealed the formation and/or growth of the lath structure, with notable changes in pole distributions and the appearance of a distinct peak at 52.5° in the XRD spectrum. The lath structure is quantified using FiJi weka segmentation machine learning technique. Nanoindentation data showed an increase in the average hardness from ~7 to ~8 GPa and a corresponding increment in the reduced modulus from 127 to 148 GPa. The observed increase in low-angle grain boundaries (LAGBs) from 4% to 12% further complements the findings, suggesting a complex interplay of microstructural features contributing to the overall improvement in the mechanical properties. The proposed low temperature annealing technique demonstrates the predominant role of the electron wind force for tailoring the microstructure and mechanical performance of ZrTi alloys, providing insights that could have implications for the broader field of materials engineering.

Heuristic determination of parent β matrix orientation from burgers oriented α precipitates in Ti alloys

A heuristic stereographic tool has been developed supporting identification of un-measurable parent β grain orientations in Ti alloys from electron back scattered diffraction (EBSD) without computation. The method involves the use of inverse pole figure (IPF) Euler angle color patterns of α laths in Burgers oriented α/β crystals. The approach employs the use of composite stereographic projections of two fundamental α/β variants of the Burgers orientation relationship (BOR), overlaid with a commonly used IPF Euler angle color scheme for α lath orientations. Use of the heuristic tool associates many α lath orientations via EBSD-IPF derived Euler angle color patterns with the required, but usually un-measurable parent β grain orientation. Results from use of the heuristic tool are compared with observations from EBSD-IPF scans that directly measured α lath and parent β grain orientations. A reference look-up table associating characteristic α lath color patterns with orientation of their underlying parent β grain is provided. It is shown that the use of the heuristic tool to determine orientations of interest enables identification of un-measurable parent β grain orientations rather than obtaining an approximate answer using complicated computational methods. The new tool yields fairly accurate results avoiding post-processing, and often does not require the presence of more than two or three variants.

Effect of surface high-density twinned structure on the fatigue crack initiation of Ti–6Al–4V

Fatigue crack initiation sites would transfer from surface to subsurface of metal specimens through shot peening (SP) or laser shock surface strengthening. This phenomenon is typically attributed to the introduction of compressive residual stress on the surface of the specimen during the surface strengthening process. In this study, Ti–6Al–4V specimens featuring a high-density twinned structure on their surfaces, which eliminated compressive residual stress, were fabricated. Fatigue test result revealed that fatigue crack initiation sites in specimens with twinned structures were predominantly located in the subsurface, near the junction area between the twinned structure and the matrix. This phenomenon was accompanied by an increase in fatigue life. The microstructural features in the fatigue crack source were analyzed using focused ion beam (FIB) coupled with electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM). It was observed that primary crack formed in badly oriented grains that are difficult to initiate dislocation slip according to the Schmid factor (SF). Nonetheless, TEM observations revealed the activation of basal <a> dislocations in these grains, potentially leading to crack nucleation along basal slip bands and subsequent propagation along the basal plane. Our results suggest that a high-density twin structure on the surface can enhance the fatigue strength of Ti–6Al–4V by transferring the fatigue crack source to the subsurface.

Study on mechanical properties of nickel-based alloy N06625 at low to intermediate temperatures

Due to its excellent mechanical properties and good corrosion resistance at low to intermediate temperatures, nickel-based alloy N06625 has gradually become an ideal material for high-temperature gas-cooled reactor evaporators in nuclear power plants. It is currently receiving more and more attention. In this work, the tensile test of nickel-based alloy N06625 was carried out at room temperature to 900℃. The dynamic strain aging (DSA) process and microstructure evolution were studied by electron back-scatter diffraction (EBSD). The dynamic strain aging and intermediate temperature embrittlement of nickel-based alloy N06625 in the temperature range 25-900℃ were systematically studied. The results show that the stress-strain curve exhibits a serrated shape at 200-700℃, and with the increase in temperature, the serrated type changes from type A to type A+B and type C. The type A and type A+B serrations are related to the diffusion of interstitial carbon atoms. The interaction between substitutional elements Cr and Mo and movable dislocations causes the type C serration. As the temperature increases, high-density dislocations accumulate at the grain boundaries, and the proportion of substructural grains increases. A brittle fracture occurs at 600-800℃. The fracture mechanism may be due to the stress concentration at the grain boundary caused by the appearance of micropore, which weakens the grain boundary's strength and promotes the grain boundary's early failure. The continuous increase of strain makes the micropore fuse and grow to form a crack source.

Oriented growth of 5-inch optical polycrystalline diamond films by suppressing dark features

Optical diamond materials are essential for infrared optical windows, microwave windows, and laser windows due to their exceptional properties. However, dark features inside the diamond are significant factors limiting optical properties, particularly at high deposition rates. This work focuses on adjusting crystallographic parameters to prepare (110) oriented optical-grade polycrystalline diamond films, aiming to mitigate dark features. Diamond films deposited via microwave plasma chemical vapor deposition (MPCVD) exhibit discernible quality stratification. Characterization analysis of diamond film samples with varying levels of black defects reveals a correlation: films with higher dark feature content tend to exhibit a preference for the (111) orientation, accompanied by a significant presence of penetration twins and interstitial voids. Conversely, transparent diamond films demonstrate a prominent (110) orientation, featuring numerous contact twins that alleviate competition from penetration twins and original grains during growth. Electron backscatter diffraction (EBSD) and scanning electron microscope (SEM) results reveal that transparent diamond films cultivated with a pronounced preference for the (110) orientation manifest consistent and seamless contact twins, leading to fewer dark features and improved optical transmittance. In contrast, (111) oriented diamond film exhibits numerous penetration twins, and holes form between them. Based on the analysis, 5-inch optical polycrystalline diamond films with (110) orientation were achieved successfully by suppressing dark features.

Microstructure evolution and grain growth characteristics of IN625 in laser surface melting: Effects of laser power and scanning speed

This study investigated the effects of laser power and scanning speed on the microstructure evolution and grain growth characteristics of IN625 in laser surface melting. Laser powers of 400W, 600W and 800W at scanning speeds from 200mm/min to 800mm/min were employed to melt the surface of as-cast IN625 using a continuous Yb-doped fibre laser. The microstructure from the surface to the melt pool boundary was characterised by scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD). It was shown that a cellular structure was developed at low energy densities (≤ 240J/mm2), since low energy densities resulted in more rapid solidification. A coarse grain region was found near the surface after melting and a columnar grain growth region was formed close to the melt pool boundary at increasing laser power. Large angle grain boundaries were eliminated and medium angle grain boundaries exhibited an area fraction of 90% after laser surface melting. This was due to the fact that the twinned grains were fully melted in the melt pool and no twins were formed after solidification. An analytical approach was proposed to the estimate the melt pool depth and good agreement between experimental and calculated melt pool depth was obtained at laser power of 400W and 600W.

Influence of heating temperature and time on mechanical-degradation, microstructures and corrosion performances of Teflon/granite coated aluminum alloys used for non-stick cookware

This study explores the functional characteristics (erosion, corrosion, mechanical damage, and microstructural features) of non-stick cookware made from aluminum alloys. Typically coated with polytetrafluoroethylene (PTFE-Teflon) or ceramic for non-stick properties, we conducted a systematic investigation using corrosion, abrasion, and mechanical tests on six types of cookware from different manufacturers (Manuf-1-6). The cookware was heated at various temperatures [Room temperature (RT), 100, 175, 250, & 350 °C] and times (45 & 120 min). Tests included Taber wear, Adhesive Pull-off, hot & RT corrosion, and surface roughness measurements. Characterization involved optical microscopy, scanning electron microscope (SEM) with electron backscattered diffraction (EBSD), and x-ray diffraction (XRD). Ceramic-coated cookware from Manuf-4 demonstrated superior mechanical strength, wear, and corrosion resistance due to refined microstructures. Manuf-1's PTFE-coated cookware also performed well. Optimal results were observed when heating below 250 °C for up to 45 min. Prolonged heating and temperatures beyond 250 °C adversely affected internal structures of all cookware. Thus, it is advisable to use Al-based non-stick cookware below 250 °C for a maximum of 45 min.

Effect of prior austenite grain size on austenite reversion, bainite transformation and mechanical properties of Fe-2Mn-0.2C steel

To elucidate the response of austenite reversion and subsequent bainite transformation behavior to the prior austenite grain (PAG) size, the transformation kinetics and amount of reverted austenite in the intercritical region, the subsequent bainite transformation kinetics, and the tensile properties were investigated by dilatometers, scanning electron microscopy, electron backscatter diffraction, transmission electron microscopy, and the mechanical tests. The results show that, when annealed at 730 °C, fine-grained specimens exhibit faster reverted austenite transformation rate than coarse-grained specimens due to the presence of more PAG boundaries. As the intercritical temperature rises to 760 °C, more intragranular globular austenite forms in the coarse-grained specimen, which accelerates the reverted austenite transformation rate. Compared to fine-grained specimens, coarse-grained specimens exhibit faster bainite transformation and higher amount of bainitic ferrite. The microstructure after austempering consists of intercritical ferrite, bainitic ferrite, RA and fresh martensite. With increasing the austempering time, more bainitic ferrite is formed and the amount of RA and fresh martensite decreases. With increasing the austempering time, the increase in the amount of bainitic ferrite leads to an increase in the yield strength, while the decrease in the amount of RA leads to a decrease in the elongation. Moreover, compared with coarse-grained specimens, the finer microstructure in fine-grained specimens improves yield and tensile strengths, while higher amount of RA contributes to larger uniform and total elongations.

Effect of grain size on spall fracture of CrCoNi medium-entropy alloy under Taylor-wave loading

The effect of grain size on spall properties of medium-entropy alloy CrCoNi under Taylor-wave loading is investigated. Three different grain sizes, 300 μm, 20 μm, and 3 μm, are explored. The free surface velocity histories are measured to obtain such quantities as dynamic yield strength and spall strength. With decreasing grain size, there is a slight decrease in spall strength, but a significant increase in damage rate. The shock-recovered samples are characterized with scanning electron microscopy and electron backscatter diffraction. In coarse-grained samples, voids tend to nucleate within grain interiors, while in fine-grained samples, voids nucleate preferentially at grain boundaries (GBs). Molecular dynamics simulations show that the nucleation of intergranular or intragranular voids is dominated by GB–slip and slip–slip intersections, respectively. The higher GB density results in more extensive GB–slip intersections, consistent with the experimental results.