Electron Backscatter Diffraction Technique Research Articles

Effect of cold-rolling and annealing temperature on microstructure, texture evolution and mechanical properties of FeCoCrNiMn high-entropy alloy

This study investigates the effects of cold rolling and annealing on the microstructure, texture, and mechanical properties of FeCoCrNiMn high-entropy alloys. Utilizing vacuum induction melting, the alloy was initially cast into ingots and hot-rolled into plates, which were subsequently cold-rolled to various thicknesses and annealed at different temperatures. Microstructural analyses were conducted using X-ray diffraction and electron backscatter diffraction techniques, revealing a persistent face-centered cubic structure across all conditions. The texture evolution demonstrated a shift from Copper and S components to dominant Goss and Brass components as cold rolling intensified, suggesting the formation of Brass-type texture in FeCoCrNiMn at high deformation. Mechanical testing showed that the alloy's yield and tensile strengths significantly increased with cold rolling, reaching optimum values at ∼66 % reduction. Annealing at 750 °C enhanced both strength and ductility, primarily through grain refinement and the formation of Σ3 annealing twin boundaries, which dominated the microstructure of recrystallized grains. The study confirms that the low stacking fault energy of the alloy facilitates the activation of twinning and transformation-induced plasticity mechanisms, crucial for the observed enhancements in mechanical properties.

Comparison on Hysteresis Loops and Dislocation Configurations in Fatigued Face-Centered Cubic Single Crystals

The aggregation and evolution of dislocations form different configurations, which are the preferred locations for fatigue crack initiation. To analyze the spatial distribution of the same dislocation configuration and the resulting configuration morphologies on different observation planes, several typical hysteresis loops and dislocation configurations in fatigued face-centered cubic single crystals with various orientations were compared. The crystal orientations of these specimens were determined by the electron back-scattering diffraction technique in a Cambridge S360 Scanning Electron Microscope. It is well known that dislocation ladder and wall structures, as well as patch and vein structures, are distributed on their respective observation planes, (12¯1) and (111). These correspond to the point defect direction and line defect direction of dislocations, respectively. Therefore, the wall structures on the (12¯1) and (111) planes consist of point defects and line defects, which can be defined as point walls and line walls, respectively. Furthermore, the walls on the (12¯1) plane consist of Persistent Slip Band ladders connected with each other, corresponding to the formation of deformation bands. The evolution of dislocation patterns follows a process from patch to ladder and from vein to wall. The formation of labyrinths and dislocation cells originates from the activation of different secondary slip systems. In one word, it can help us better understand the physical nature of metal fatigue and failure by studying the distribution and evolution of different configurations.

Sequential stable (δ18O and δ13C) isotopic analysis of ammonite aptychi from Upper Cretaceous eastern Gulf Coastal Plain

This study reports sequential δ18O and δ13C values measured in ammonite aptychi (n=8) and assesses their preservation via scanning electron microscopy and electron backscatter diffraction techniques. The samples were collected from the Late Cretaceous Mooreville Chalk in Greene and Dallas Counties, Alabama, USA. These ontogenetic data profiles may provide insight into possible migration patterns, potentially including both short-term and long-term movements between cooler and warmer water. The δ18O variations appear primarily caused by temperature variation because it is unlikely that fresh water influenced these samples so far offshore. Estimated age of all species indicate these animals analyzed here did not live >3.5–13 years. Calculated paleotemperature values based on δ18O data vary between 15 °C and 28 °C, similar to other estimates from the Upper Cretaceous eastern Gulf Coastal Plain. While some systematic patterns were observed in the data, no definitive seasonal cyclicity was observed.

Low temperature tensile behavior and microstructure analysis of copper containing antibacterial stainless steel

Using Shimadzu AGS-100KN universal tensile testing machine, tensile tests were conducted on copper containing antibacterial stainless steel at 25 °C, −20 °C, −60 °C, −100 °C, and −140 °C. The fracture morphology and microstructure evolution of the material were then analyzed using various techniques including scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), X-ray diffraction (XRD), and transmission electron microscopy (TEM) techniques. The experimental findings showed that with the decrease of deformation temperature, the ultimate tensile strength(UTS) increased by about 49.7 %, the yield strength (YS) increased by about 35.5 %, and the elongation(EI) decreased by about 27.3 %, showed obvious low temperature strengthening effect. The High-angle grain boundaries (HAGBs) increased with decreasing temperature, while low-angle grain boundaries (LAGBs) decreased. The plasticity gradually decreased and the strength gradually increased, resulting in an increase in its ability to resist deformation. The number of precipitated phases gradually increased, and the size also gradually becomes larger, and the interaction between the diffusely distributed precipitated phases and dislocations led to precipitation strengthening. With the decrease of temperature, the stacking fault energy gradually decreased, the SFE was 21.26 mJ/m2 at the temperature of −140 °C. The main plastic deformation mechanism of copper-containing austenitic stainless steel in the low-temperature tensile process was transformed from deformation twins to strain-induced martensitic phase transformation.

Electropulsing-induced recrystallization of cold-rolled SUS304 and effects of duration on mechanical properties

A cold rolled SUS304 stainless steel was treated by electropulsing treatment (EPT) with different time and duration, and then, microstructural evolution and texture development was studied by electron backscattering diffraction (EBSD) technique. EPT enhances the recrystallization process of cold rolled SUS304 stainless steel and the completed recrystallization state of sample can be obtained at low temperature below 530 K for a short time of 100 s. The best strength-ductility combination can be obtained when 210 μs of pulse duration applying. Pulse duration has been found to have a significant impact on the microstructure and tensile properties of SUS304. EPT is not a simple heat treatment process and electrical effects should be responsible for the recrystallization of the EPT samples.

Investigating the microstructure and mechanical properties of Al–Ag-Sc ultra-fine grain alloy processed by accumulative rolling bonding method

The aim of the present study is to investigate the effect of accumulative roll bonding (ARB) and precipitation hardening on the microstructure development and there of mechanical properties of ultrafine grained Al–Ag-Sc alloy. For this purpose, the samples were heated to a temperature of 600 °C for 24 h, and then they were quenched in water. In order to carry out the two-stage precipitation hardening process, the samples were placed in the furnace at a temperature of 350 °C for 5000 s in the first stage, which was followed by quenching in water. In the second stage, they were heated to 250 °C for 5000 s following by water quenching too. Following, the samples were subjected to the ARB for up to 8 cycles. Scanning Electron Microscope (SEM) equipped with Electron Backscatter Diffraction (EBSD) and energy dispersive spectroscopy (EDS) techniques, and X-Ray Diffraction (XRD) was used to verify the microstructure and phase analysis of the prepared samples. Also, tensile and microhardness tests were conducted to confirm the mechanical properties, and pin-on-disk tests were done to check wear behavior. Microstructural parameters such as crystallite size, microstrain, and density of dislocations in rolled sheets were estimated using the Rietveld method. The Results have shown that applying various cycles of the ARB process leads to the development of ultra/nano grain structure. In that sense, performing 8-cycle of the ARB transformed the low angle grain boundaries (LAGBs) of the 4-cycle ARB condition to high angle grain boundaries (HAGBs). Results showed that there is proper welding between different layers, except for the layers created in the last cycle. Similarly, the obtained size of the crystallites demonstrates that the samples become finer when ARB cycles are increased. The results of the mechanical tests indicated that after 8 cycles, there is approximately 3.5-fold and 2.5-fold increase in the tensile strength and hardness compared to the original (annealed) sample, respectively. While the elongation decreased slowly and reached 1.5% in the 8th cycle. A fractography of the fracture surface of the original sample included deep and coaxial dimples, indicating a ductile fracture. Analysis of wear surface degradation showed that scratch wear occurred for all samples.

Application of the EBSD Technique in the Study of Porosity and Permeability in Deformation Bands in Sandstone.

Deformation bands are common constituents of porous clastic fluid reservoirs. Various techniques have been used to study deformation band structure and the associated changes in porosity and permeability. However, the use of electron backscatter diffraction technique is limited. Thus, more information is needed regarding the crystallographic relationships between detrital crystals, which can significantly impact reservoir rock quality. We employ microscopic and microstructural investigation techniques to analyze the influence of cataclastic deformation bands on pore space. Porosity measurements of the Cretaceous Ilhas Group sandstone in NE Brazil, obtained through computerized microtomography, indicate that the undeformed domains exhibit a total porosity of up to 13%. In contrast, this porosity is slightly over 1% in the deformation bands. Scanning electron microscopy analyses revealed the presence of grain fragmentation and dissolution microstructures, along with cement-filling pre-existing pores. The electron backscatter diffraction analyses indicated extensive grain fragmentation and minimal contribution from intracrystalline plasticity as a deformation mechanism. However, the c axes of quartz crystals roughly align parallel to the orientation of the deformation band. In summary, we have confirmed and quantified the internal changes in a deformation band cluster, with grain size reduction and associated compaction as the main mechanism supported by quartz cementation.

Unveiling the formation of nanotwin-mediated metastable ζ-hydrides in fatigued Zr-1Nb-0.01Cu cladding tube

The impact of internal pressure fatigue treatment on the α-Zr matrix and hydride precipitates in Zr-1Nb-0.01Cu cladding tube has been systematically investigated using synchrotron-based high-energy X-ray diffraction, electron backscatter diffraction and transmission electron microscopy techniques. The evolution in d-spacings of the basal plane (0002), the pyramidal plane {101¯1} and the prismatic plane {101¯0} at azimuths from 0° to 360° indicates that the internal pressure fatigue treatment has imparted a degree of plastic deformation upon the α-Zr phase, which is further confirmed by the presence of {101¯2} deformation twins within the α-Zr phase. Concurrently, the prior internal pressure fatigue treatment at 400 °C significantly increased nucleation sites for zirconium hydrides during the subsequent furnace cooling process. High-density dislocations can be seen in both the δ-hydride precipitate ({111}<110> type) and the α-Zr matrix ({101¯0}<a> type) near the hydride-matrix interface. Additionally, δ-hydride {111}<112¯> nanotwins were observed within the micro-sized δ-hydrides in the fatigued cladding tube, resulting from the nucleation and growth of intra-granular δ-hydrides at different regions of the same parent α-Zr grain. Furthermore, the HCP-structured ζ-hydride phase was detected at the δ-hydride nanotwin forefront along the growth direction and at the curved δ-hydride nanotwin boundaries, providing direct experimental evidence to the notion that the metastable ζ-hydride serves as the precursor to the stable δ-hydride phase during the precipitation process. The current experimental findings contribute to the fundamental understanding of microscopic mechanisms underlying the delayed hydride cracking and the stress-induced hydride reorientation in Zr alloys.

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.

Construction of meta-dynamic recrystallization dynamic model of 316L stainless steel based on grain orientation spread during continuous variable rate thermal deformation

Because the deformation parameters (temperature, strain rate) in the actual manufacturing process are non-constant. We investigate meta-dynamic recrystallization behavior under the transient mutation state. First, based on a single-pass thermal deformation experiment and electron backscatter diffraction (EBSD) technique, this study establishes a quantitative calculation method for the volume fraction of meta-dynamic recrystallization under different deformation conditions, and find the GOS threshold basis for judging the occurrence of meta-dynamic recrystallization. Comparing the experimental results with the numerical simulation results, it is found that the MDRX behavior of the material could be accurately described. The meta-dynamic recrystallization evolution law of the material in the thermal deformation insulation stage under the variable strain rate state is investigated by continuous variable rate thermal deformation experiment and numerical simulation. It is observed that an increase of the average strain rate in the continuous variable strain rate state would promote the meta-dynamic recrystallization softening behavior of the material in comparison with the steady state deformation stage, and vice versa.

An investigation to microstructural and texture evolution during the cold rolling of Al0.3CoCrFeNi high entropy alloy

In the present study, Al0.3CoCrFeNi high entropy alloy (HEA) was subjected to thickness reductions through cold rolling process in order to thoroughly investigate the evolution of microstructure and deformation texture. Important aspects of deformed microstructures such as the formation of twinning bundles and shear bands in the specimens were monitored. The evolution of texture during the cold rolling process was measured by X-Ray Diffraction (XRD) and Electron Back Scatter Diffraction (EBSD) technique which revealed the formation of Copper type texture at the initial stages of rolling due to slip deformation mechanism. Originated from twinning and followed by shear banding, the texture was subsequently developed toward predominantly Brass type. Microstructural features and texture evolution behavior of the investigated single phase FCC alloy was attributed to its low SFE level. Visco Plastic Self Consistent (VPSC) technique was coupled in the research to simulate the material behavior and to examine the contribution of slip and twinning systems. Benefiting VPSC justifications, the texture transition from Copper type to Brass type was related to lower CRSS value of slip in comparison to twinning at the small strains which was then grows faster at the later stages of rolling facilitating the onset of twinning and providing the texture transition basement.

Developing Ultra‐High Strength Bainitic Steel by Hot Stamping Process and Anisothermal Holding

Hot stamping is a well‐established process in the automotive industry for structural parts to decrease the weight of a vehicle without reducing the safety and stiffness of components. In this work, a bainitic approach during the hot stamping process is studied by anisothermal annealing. The effect of different strategies on the microstructure and mechanical properties of the hot‐stamped parts is investigated. The microstructure is analyzed using light microscopy (LM), scanning electron microscopy (SEM), and electron backscatter diffraction (EBSD) techniques. Tensile and hardness tests are applied to analyze mechanical properties. A microstructure consisting of a carbide‐free bainite matrix containing martensite, fine‐grained ferrite, and retained austenite is obtained. SEM analysis of fracture surfaces from tensile samples reveals that the bainitic microstructure showed mainly a ductile fracture by dimples and voids along with some quasi‐cleavage fracture.

Cold Metal Transfer Welding of Ferritic and Austenitic Stainless Steel: Microstructural, Mechanical, and Electrochemical Studies

AbstractIn the present study, cold metal transfer arc welding was employed to weld the 304L austenitic stainless steel (ASS) and Ti-stabilized 439 ferritic stainless steel (FSS) using a 309L filler electrode. Dissimilar joints were prepared using low heat input (HI; W1 ~ 247 J/mm) and high HI (W2 ~ 282 J/mm). The solidification mode for both weldments were the ferritic-austenitic mode and the weld zone (WZ) regions of both the weldments consists of columnar austenites, lathy and skeletal ferrite phases. The interfaces between WZ and ASS base metal showed the unmixed zone, whereas a conventional heat-affected zone (HAZ) was formed between the WZ and FSS base metals. The formation of ferrite stringers were observed in the unmixed zone, whereas peppery features of chromium-rich carbides were observed in HAZ. Moreover, electron backscattered diffraction technique was used to distinguish the microstructural differences between W1 and W2 weldments. Increase in the HIs resulted in decreased ferrite fraction in WZ as well as decrease in the mechanical strength of the joints. The W1 weldment depicted higher values of average micro-hardness (WZ ≈ 334.32 HV) than W2 (WZ ≈ 310.92 HV)) weldment. The electrochemical behaviour of the weldments was analysed for both the base metals and WZ of weldments. The higher degree of sensitization (DOS ~ 9.24%) of W1-WZ showed lower intergranular corrosion resistance than W2-WZ (DOS ~ 7.77%), however, the opposite trend was observed for impedance and pitting resistance.

Contrastive learning based on hierarchical graph of microstructures through directed energy deposition process to establish process-structure–property relationship via autoencoder

n this study, an innovative algorithm is developed to transform microstructures to hierarchical graphs without manual feature engineering. The hierarchical graph comprises two layers. Initially, pixel data, which includes Euler angles, phase, and position, forms the pixel-wise graphs within individual grains. Following this foundation, the grains serve as nodes, constituting the second layer. Importantly, the hierarchical graph preserves essential measurement data and structural details for training machine learning models. After that, a contrastive learning model based on hierarchical graph is designed to capture representations of microstructures obtained by the electron backscatter diffraction (EBSD) technique. This model can be directly extended for other microscopy techniques, such as Scanning Electron Microscopy (SEM), Energy-Dispersive X-ray spectroscopy (EDX), and Transmission Electron Microscopy (TEM). Using the learned microstructure representations, an autoencoder model for the directed energy deposition (DED) is developed to establish the relationship among process parameters, microstructures, and material properties, completing the process-structure–property cycle quantitatively. The performance of the present model is naturally benchmarked against two other models: a contrastive learning model based on pixel-wise graph (without manual feature engineering) and a contrastive learning model based on grain-wise graph (employing manual feature engineering). The results of the present model highlight the potential in decoding the process-structure–property relationships in the DED process.

Effect of HIP Treatment on the Evolution of Texture and Microstructure of LBPF Fabricated Pure Ni

Microstructure and texture analysis were conducted employing electron backscatter diffraction (EBSD) technique on laser powder bed fusion (LPBF) fabricated pure Ni. The texture analysis of the hot isostatic pressed (HIP) and as-printed (AP) samples were done utilizing orientation distribution function (ODF) maps. The AP sample comprises mostly of &amp;lt;110&amp;gt;||BD fiber texture with insignificant presence of twins. In contrast, the HIP sample has &amp;lt;111&amp;gt;||BD grains. It was found that the development of the texture &amp;lt;111&amp;gt;||BD was due to the deformation linked to the HIP process. In addition, HIP generated a substantial fraction of Σ3 coincident site lattice boundaries (CSL) because of pure Ni which is a medium stacking fault energy (SFE) element.

Microstructure and properties of the as-cast alumina-forming austenitic steel during cold-rolling

An as-cast alumina-forming austenitic (AFA) steel was directly cold rolled. The microstructure was characterized by electron backscatter imaging and electron backscatter diffraction techniques. Results show that the as-cast AFA steel exhibits excellent cold-rolling deformation ability. With increasing rolling deformation, the content of δ-ferrite/α′-martensite increases, and the proportion of low-angle boundaries (LABs) in δ-ferrite/α′-martensite and austenite increases greatly. In contrast, the number of twins in the austenite matrix decreases significantly. The microhardness and tensile strength of the AFA steel increase significantly. The increase in hardness and tensile strength is mainly attributed to the increase of martensite, the grain refinement of austenite, and the increase of LABs content in austenite and δ-ferrite/α′-martensite.

Monitoring the phase evolution and fracture behavior of advanced multiphase QP steel using EBSD technique and digital image correlation

A novel multiphase 0.17C-5Mn-0.88Si-0.76Al-0.22Mo-0.06Nb steel was subjected to complex thermomechanical processing schedules to produce quenching and partitioning (Q&P) microstructures. The tests were performed in the Gleeble 3800 simulator applying multiple deformations in a plane state of strain and final deformation was applied at 850 °C. The samples were controlled cooled to 240 °C and 260 °C to produce some martensite fraction and subsequently partitioned at a temperature of 450 °C to enrich austenite in carbon from the supersaturated martensite. Different primary/secondary martensite microstructures containing retained austenite were produced, which were subjected to detailed microstructural and fracture studies using scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD). The mechanical behaviour of the samples was investigated in static tensile tests using sub-sized flat samples. Digital image correlation (DIC) measurements were performed to monitor the strain distribution in a micro scale. Relationships between processing conditions and fracture behaviour were assessed in fractographic tests.

Study on hot deformation behavior and recrystallization mechanism of an Al-6.3Zn-2.5Mg-2.6Cu-0.11Zr alloy based on machine learning

The data from thermal simulation plays a significant role in understanding the deformation behavior and deformation mechanisms of materials, and provides guidance for the design of hot deformation processes. In this paper, thermal simulation experiments were performed on an Al-6.3Zn-2.5Mg-2.6Cu-0.11Zr alloy, and the microstructure after hot deformation were characterized by Electron Backscatter Diffraction (EBSD) technique. The thermal simulation data and microstructural characteristics were analyzed and studied using machine learning technique: the Backpropagation Artificial Neural Network (BP-ANN) method, correlation analysis and K-means clustering analysis. A model for predicting not only flow stress but also dislocation density was established using the BP-ANN method, which exhibits good prediction accuracy. The R² and AARE values are 90.19 % and 6.87 % for the prediction of dislocation density, and are 98.67 % and 6.96 % for the prediction of flow stress. Subsequently, correlation analysis was performed to investigate the relationship between energy dissipation efficiency η and deformation parameters as well as microstructural characteristics, revealing that energy dissipation rate is correlated positively with the content of dynamical recrystallization (DRX) and high angle grain boundary (coefficients of 0.90 and 0.82) and negatively with the dislocation density and the Zener-Hollomon parameter (coefficients of −0.98 and −0.97). Additionally, K-means clustering analysis was applied to study the relationship between the energy dissipation efficiency and softening mechanisms, it was found that the softening mechanisms changed with the variation of η value, dynamic recovery (DV), geometric DRX (GDRX) and continuous DRX (CDRX) dominated when η>0.38; DV, CDRX and discontinuous DRX(DDRX) dominated when 0.28<η<0.38; DV dominated when η<0.28. The results show that machine learning techniques are useful tools in mining thermal simulation data, and more information can be obtained than traditional data mining methods.

Electrochemical behavior and microstructural characterization of nano-SiC particles reinforced aluminum matrix composites prepared via friction stir processing

The present work aims to elucidate the mechanism of microstructural evolution in different regions of nano-SiC particles reinforced aluminum matrix composites prepared by friction stir processing (FSP) on its electrochemical behavior. Electron backscatter diffraction technique (EBSD) and transmission electron microscopy (TEM) were employed to characterize the microstructure evolution of stir zone (SZ), advancing side thermomechanically affected zone (AS-TMAZ), retreating side thermomechanically affected zone (RS-TMAZ) and base metal (BM). The electrochemical behaviors of the above zones were investigated using electrochemical tests. A homogeneous and fine microstructure is formed in SZ, not only the nano-SiC is homogeneously distributed within the grains with an average grain size of 3.5 μm, but also the recrystallized grains account for the highest percentage of 85 %. The potentiodynamic polarization curve indicates that the corrosion current densities of the BM, RS-TMAZ, AS-TMAZ and SZ are 0.89, 0.39, 0.85 and 0.36 μA/cm2, respectively, while the polarization impedances are 33.40, 51.42, 48.72 and 73.79 kΩ cm2, respectively. Combining the Nyquist and Bode plots analysis, the optimal electrochemical corrosion resistance is in SZ. The fine and homogeneous recrystallized grains in SZ significantly improve its electrochemical corrosion resistance. This is mainly ascribed to the increase in crystal defects as a result of the increase in grain boundaries, elevating the electron scattering. Simultaneously, the increase in high-energy state grain boundaries is beneficial to the rapid formation of a thicker passivation film.

Quasi-in-situ observation of fatigue crack growth behavior of friction stir welded 2024-T4 joint

This study presents a quasi-in situ observation of the fatigue crack growth behavior in a friction stir welded 2024-T4 joint. The microstructure and fatigue properties of the joint were investigated using electron backscatter diffraction (EBSD) technique, scanning electron microscopy (SEM), and fatigue crack growth tests. The fatigue crack growth behavior of the joint was examined by conducting fatigue crack growth tests with different notch locations. The results show that the sample with the notch in the stir zone (SZ) exhibited the highest resistance to fatigue crack growth, followed by the notched samples of the Advancing side (AS) and Retreating side (RS) weldments. Microstructural observations showed a homogeneous microstructure with a fine grain size in SZ and it was observed that this fine-grained structure significantly enhanced the material’s resistance to fatigue crack growth. The experimental results were further analyzed using the Paris model to provide a quantitative understanding of the crack growth behavior. The study underlines the impact of microstructural characteristics and notch location on the fatigue performance of the weldment. Overall, the quasi-in situ observations and experimental findings contribute to a comprehensive understanding of the fatigue crack growth behavior in friction stir welded 2024-T4 joints.