Electron Backscatter Diffraction Technique Research Articles

Microstructure, precipitates and mechanical properties of Cu-3Ni-1Ti alloy by two-stage cold rolling and aging treatment

The effects of two-stage cold rolling and aging treatment on the mechanical and electrical properties of Cu-Ni-Ti alloy were investigated. The microstructure evolution, precipitation behavior, and strengthening mechanism of the alloy after two-stage cold rolling and aging treatment were analyzed using microhardness, tensile strength, and electrical performance tests, combined with transmission electron microscopy (TEM) and electron backscatter diffraction (EBSD) techniques. The research results show that the alloy after two-stage cold rolling and aging treatment exhibits excellent comprehensive properties, tensile strength reaches 635 MPa, yield strength is 597 MPa, hardness is 182 HV, conductivity is 62.1 % IACS, and elongation is 14.5 %. This processing method facilitates the precipitation of more nanoscale Ni3Ti phases and the formation of smaller cellular substructures. Consequently, the alloy maintains its exceptional mechanical properties through the combined effects of dislocation and precipitation strengthening. This study provides a novel preparation process and a solid theoretical foundation for enhancing the mechanical and electrical properties of Cu-Ni-Ti alloys.

Restoring Plasticity in Nickel‐Based Superalloy Using High‐Density Pulsed Electric Current

This study explores the efficacy of high‐density pulsed electric current (HDPEC) in healing plastic deformation damage in single‐crystal Ni‐based superalloys. Single‐crystal specimens are prepared from directionally solidified nickel‐based superalloy to assess the potential of electric current treatment in restoring plastic deformation capability. Experiments involving various current densities and pulse durations reveal that a pulsed electric current of 17 ms at 400 A mm−2 yields optimal results, enhancing fracture elongation from 7.8% to 12.3% without compromising strength. The study conducts a comprehensive analysis of microstructural changes induced by pulsed electric current, employing quasi‐in‐situ electron backscatter diffraction and transmission electron microscopy techniques. The results demonstrate that HDPEC disrupts the planar dislocation network, homogenizes dislocation distribution, and promotes dislocation entanglement. Consequently, microdefects in the alloy are eliminated, restoring the material's ductility. The findings suggest that this technology holds significant promise for repairing fatigued components and underscore the potential for further research in this domain.

Analysis of stress corrosion cracking failure of 316L stainless steel flow promoter string in the aggressive oilfield environment

This paper analyzes the failure mechanisms of stress corrosion cracking (SCC) in 316L stainless steel flow promoter strings in corrosive oilfield environments. Electrochemical tests and passive film analysis techniques were employed to elucidate the degradation behavior of the 316L stainless steel passive film. The fracture characteristics were analyzed using slow strain rate tensile tests, scanning electron microscopy, and electron backscatter diffraction techniques to clarify the SCC mechanisms. The results indicate that the SCC of 316L stainless steel is controlled by anodic dissolution due to passive film breakdown in the oilfield environment. The degradation of the passive film, induced by Cl- and CO2, promotes SCC in 316L stainless steel, with cracks propagating in a trans granular manner.

Study of microstructural evolution during operation of electrically connected components and analysis of failure mechanism

Abstract As a key current-carrying structure of high-voltage bushings, the reliability of electrical connection components is crucial to the safe and stable operation of power equipment. To obtain the microstructural evolution of electrical connection components with different deterioration states, CUD strap contactors were deteriorated in different ways, and electron backscatter diffraction technique was used to test the microstructure of strap contactors with different deterioration states. The results showed that compared to the unused contactors, the contact resistance of the contactors under the combined effect of friction and high temperature increased 203.12 times and was in a failed state. During the process from unused state to wear deterioration, high temperature deterioration, and then to eventual failure of the contactors, the average grain size gradually grows from 8.15 μm to 25 μm, the dislocation density gradually decreases from 2.38 × 1014 m−2 to 1.04 × 1014 m−2, and there are a significant proportion of the recrystallized organization. These changes are detrimental to the mechanical properties of the contactors. In addition, the distribution of grain boundaries in the contact area proves the occurrence of over-temperature phenomenon in this area, which will accelerate the deterioration of the contactors and eventually lead to the failure of the component. The relevant conclusions can provide a theoretical basis for the design of electrical connection structure of strap contacts as well as the study of deterioration mechanism.

Dependency of mechanical properties in Ti-7Mo-3Al-3Cr-3Nb alloy on the β phase stability: Regulating primary α phase

In this study, the modification of the β-phase stability of Ti-7Mo-3Al-3Cr-3Nb alloy has been achieved by heat treatment at different temperatures. The synergy effects of primary α-phase and β-phase stability on the deformation behavior and mechanical properties were systematically studied based on these samples, combining the electron backscattering diffraction and transmission electron microscopy techniques. The content of the primary α-phase and stability of the β-phase increase when the heat treatment temperature is lowered from 860°C to 770°C, which increases the yield strength of the alloys. When the content of primary α-phase is less than 9%, high strength and ultra-high work-hardening rates can be simultaneously achieved, with maximum work-hardening reaching 12.75GPa and the ultimate tensile strengths reaching 846MPa. Stress-induced α′′ martensitic (SIM α′′) transformation is observed in all experimental samples during tensile deformation, and the trigger stress of martensitic transformation decreases with the decrease of β-phase stability. When the stability of the β-phase decreases, the quantity of SIM α′′ increases, while martensitic variants and twinned martensite increase to coordinate local strains. Meanwhile, as the strain increases, the martensite laths grow into martensite domains, which trigger martensite twins during deformation, and the interaction of the primary α-phase and β-phase deformation products will achieve different work-hardening rates. This study provides a possible strategy for the design and modification of new high-strength and 、work-hardening rate titanium alloys.

Towards measuring absolute residual stress by HR-EBSD with simulated reference patterns

The High-Resolution Electron Backscatter Diffraction (HR-EBSD) technique has drawn attention in recent years, mainly thanks to its ability to assess the elastic strain/stress state with a sub-micron spatial resolution. Each diffraction pattern is correlated with a reference one, and the strain level relative to the reference is retrieved in the procedure. Several studies have attempted to use dynamically simulated diffraction patterns as references to access absolute strain/stress states to circumvent the difficulty of finding a strain-free reference pattern, which is often inaccessible. Numerous factors need to be considered and corrected to register better experimental and simulated diffraction patterns, such as the accurate positioning of the projection center, Kikuchi band (K-band) brightness asymmetry, K-band gray level reversal, optical distortion, or non-uniform electron energy. Here, an integrated digital image correlation method is proposed to register experimental patterns to a master pattern defined on a sphere, where the difficulties with experimental patterns are, for the most part, corrected efficiently. Due to the shallow inspection depth of EBSD, the free-surface property (vanishing stress vector at the observation surface) is also adopted to reduce the degrees of freedom and enhance precision. Through several tests on high-quality experimental patterns, the proposed method proves robust and precise. Both the systematic and random errors of the residual strain results are several 10−4. The method also allows the simultaneous determination of residual stress and the projection center coordinates.

Effect of Mg on Plasticity and Microstructure of Al-Mg-Ga-Sn-In Soluble Aluminum Alloy.

Soluble aluminum alloy materials used in underground operational tools are synthesized via a high-temperature smelting process. The microstructure and composition distribution of the alloy were analyzed using X-ray diffraction, metallographic microscopy, and scanning electron microscopy with energy-dispersive X-ray and electron backscatter diffraction techniques. The mechanical properties were evaluated using a universal testing machine and hardness tester, while solubility assessments were conducted in a constant-temperature water bath. This study focuses on the plasticity and dissolution characteristics of Al-Mg-Ga-Sn-In alloys with varying Mg contents. The tensile strength (σb) of the alloy was 181.99 MPa, with an elongation (δ) of 27.49% and cross-sectional shrinkage (φ) of 11.67% at a magnesium content of 3.0 wt.%. Additionally, in the compressive test, the compressive yield strength (σsc) was recorded at 188.32 MPa, while the compression rate (δ) was 27.06% and the section expansion rate (φ) was 138.66%. Furthermore, the alloy demonstrated the ability to dissolve spontaneously in water at 90 °C, exhibiting an average dissolution rate of 1.0 g·h-1cm-2 and a maximum dissolution rate of 3.25 g·h-1cm-2 after 12.0 h. Consequently, this alloy composition not only satisfies the requirements for rapid solubility but also exhibits favorable plasticity, providing a novel reference for the selection of soluble aluminum alloy materials.

Two-Dimensional X-Ray Diffraction (2D-XRD) and Micro-Computed Tomography (Micro-CT) Characterization of Additively Manufactured 316L Stainless Steel

In-depth quality assessment of 3D-printed parts is vital in determining their overall characteristics. This study focuses on the use of 2D X-Ray diffraction (2D-XRD) and X-Ray micro-computed tomography (micro-CT) techniques to evaluate the crystallography and internal defects of 316L SS parts fabricated by the powder-based direct energy deposition (DED) technique. The test samples were printed in a controlled argon environment with variable laser power and print speeds, using a customized deposition pattern to achieve a high-density print (>99%). Multiple features, including hardness, elastic modulus, porosity, crystallographic orientation, and grain morphology and size were evaluated as a function of print parameters. Micro-CT was used for in-depth internal defect analysis, revealing lack-of-fusion and gas-induced (keyhole) pores and no observable micro-cracks or inclusions in most of the printed body. Some porosity was found mostly concentrated in the initial layers of print and decreased along the build direction. 2D-XRD was used for phase analysis and grain size determination. The phase analysis revealed single phase γ-austenitic FCC phase without any detectable presence of the δ-ferrite phase. A close correlation was found between Electron Backscatter Diffraction (EBSD) and 2D-XRD results on the average size distribution and the crystallographic orientation of grains in the sample. This work demonstrates the fast and reliable as-printed crystallography analysis using 2D-XRD compared to the EBSD technique, with potential for in-line integration.

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.