Electron Channeling Contrast Research Articles

Hydrogen-assisted failure in Ni-based superalloy 718 studied under in situ hydrogen charging: The role of localized deformation in crack propagation

We investigated hydrogen embrittlement in Ni-based superalloy 718 by tensile testing at slow strain rate (10−4 s−1) under continuous electrochemical hydrogen charging. Hydrogen-assisted cracking mechanisms were studied via electron backscatter diffraction (EBSD) analysis and electron channeling contrast imaging (ECCI). In order to elucidate the effects of stress or strain in the cracking mechanisms, material conditions with different strength levels were investigated, including samples in solution annealed (as water quenched) and 780 °C age-hardened states. The microstructure observations in the vicinity of the cracks enabled us to establish correlations between the microstructure, crack initiation sites, and crack propagation pathways. Fracture in the hydrogen-charged samples was dominated by localized plastic deformation. Strain-controlled transgranular cracking was caused by shear localization due to hydrogen-enhanced localized plasticity (HELP) and void nucleation and coalescence along {111} slip planes in both, the solution annealed and age-hardened materials. Stress-assisted intergranular cracking in the presence of hydrogen was only observed in the high strength age-hardened material, due to slip localization at grain boundaries, grain boundary triple junction cracking, and δ/γ-matrix interface cracking. To investigate the effect of δ-phase in crack propagation along grain boundaries, the over-aged state (aged at 870 °C) with different precipitation conditions for the δ-phase was also investigated. Observations confirmed that presence of δ-phase promotes hydrogen-induced intergranular failure by initializing micro-cracks from δ/γ interfaces.

EBSD and electron channeling study of anomalous slip in oligocrystals of high chromium ferritic stainless steel

In the present study, electron backscatter diffraction (EBSD) and electron channeling contrast imaging (ECCI) techniques were applied to investigate the deformation pattern of coarse ferrite grains after being subjected to 3%, 6%, and 10% tensile deformation. Oligocrystals of Crofer® 22H ferritic steel were obtained as experimental material at 1075°C for 22min annealing. Using kernel average misorientation (KAM) mapping obtained from EBSD, possible slip planes are (110), (101), (12–1) and (32-1) in grain A; (0–11), (−101), (−112), (1–21) in grain B; and (0–11), (1–21) and (11–2) in grain C. Combining ECCI and EBSD techniques enables us to identify two a0[11¯1]/2 edge dislocations that occur on the (110)[1–11] and (32–1)[1–11] slip systems for grain A, thereby breaking down Schmid’s law.

Toughening Behavior in Alloy 617 with Long Term Ageing

The influence of ageing at temperature 700°C for up to 20 000 hours on the deformation, damage and fracture behavior of Alloy 617 has been investigated by two toughness tests. Dense nano γ` phase and carbides are the main precipitates. However, the long-term aged material still shows high toughness. The mechanism has been studied using electron backscatter diffraction (EBSD) and electron channeling contrast imaging (ECCI). The results show that dense nano/micro-twins have been formed in the adjacent of the fracture front during the impact toughness or CTOD testing. Increase of ageing time reduces the number of nano/micro-twins, but they can be observed in all aged materials in spite of different strain rates. This indicates that besides dislocation slip, twinning is another deformation mechanism in long term aged material during the toughness tests. Formation of nano/micro-twins may be one of contributions to high toughness in the aged material, which is termed as twin induced toughening.

Electron channelling contrast imaging of dislocations in a conventional SEM

Dislocations in shock loaded tantalum single crystals were imaged using both transmission electron microscope (TEM) and electron channelling contrast image (ECCI) in a scanning electron microscope with a conventional backscattered electron detector. The results were compared with backscattered electron intensity profiles across dislocations calculated via the dynamic theory of electron diffraction. A one-to-one correspondence between ECCI and TEM is established. High voltage and low index reflections should be used to obtain the highest dislocation contrast and greatest imaging depth.

Cross-correlation based high resolution electron backscatter diffraction and electron channelling contrast imaging for strain mapping and dislocation distributions in InAlN thin films

We describe the development of cross-correlation based high resolution electron backscatter diffraction (HR-EBSD) and electron channelling contrast imaging (ECCI), in the scanning electron microscope (SEM), to quantitatively map the strain variation and lattice rotation and determine the density and identify dislocations in nitride semiconductor thin films. These techniques can provide quantitative, rapid, non-destructive analysis of the structural properties of materials with a spatial resolution of order of tens of nanometers. HR-EBSD has a sensitivity to changes of strain and rotation of the order of 10−4 and 0.01° respectively, while ECCI can be used to image single dislocations up to a dislocation density of order 1010 cm−2. In the present work, we report the application of the cross-correlation based HR-EBSD approach to determine the tilt, twist, elastic strain and the distribution and type of threading dislocations in InAlN/AlN/GaN high electron mobility transistor (HEMT) structures grown on two different substrates, namely SiC and sapphire. We describe our procedure to estimate the distribution of geometrically necessary dislocations (GND) based on Nye-Kroner analysis and compare them with the direct imaging of threading dislocations (TDs) by ECCI. Combining data from HR-EBSD and ECCI observations allowed the densities of pure edge, mixed and pure screw threading dislocations to be fully separated.

Effects of microstructure on mechanical properties of CuNiSi alloys

There is an increasing demand for precipitation-hardened Cu-Ni-Si alloys in the industry, where the high strength and moderate electrical conductivity are required. The main objective of this study was to apply a combination of microstructure refinement using swaging (SW) to generate an ultrafine-grained (UFG) microstructure in Cu-2.5 wt%Ni-0.5 wt%Si-0.06 wt%Mg (Cu-2.5Ni-0.5Si-0.06Mg), along with an optimized precipitation hardening. As a result, a substantial improvement of mechanical properties of the swaged samples (UFG condition) after precipitation hardening is apparent as compared to the precipitation-hardened non-swaged samples (coarse-grained (CG) condition). The mechanical properties of the UFG state are significantly superior to those of the CG state, i.e., a sharp increase in the elongation to fracture of 14% and a tensile strength of 800–900 MPa can be achieved. This study summarizes a detailed description of the microstructure after different processing steps using optical microscope (OM), electron channeling contrast imaging (ECCI) methods, and transmission electron microscopy (TEM), and presents the consequences on the most important mechanical properties such as the strength and ductility.

Damage Initiation in Dual-Phase Steels: Influence of Crystallographic and Morphological Parameters

Typical microstructures of dual-phase (DP) steels consist of hard martensite particles dispersed within a ductile ferritic matrix. These microstructures possess a complex network of grain and interphase boundaries, which, together with the mechanical contrast of their phase composition, control micro-damage initiation mechanisms, induced by deformation. Accordingly, in this study we analyze the influence of individual microstructural features and interfaces on damage nucleation and progression in DP steels with respect to applied tensile strain. Prominent micro-damage mechanisms include cracking of martensite and damage initiation at interphase boundaries. Influence of martensite morphology is discussed based on a statistical analysis of the damage features as observed by electron channeling contrast imaging (ECCI) and electron backscatter diffraction (EBSD) maps. Prior austenite grain boundaries (PAGbs) in martensite show a brittle behavior and are highly susceptible to crack propagation.

Influence of Dynamic Strain Ageing and Long Term Ageing on Deformation and Fracture Behaviors of Alloy 617

Influences of dynamic strain ageing and long term ageing on deformation, damage and fracture behaviors of Alloy 617 material have been studied. Dynamic strain ageing can occur in this alloy at temperature from 400 to 700°C, which leads to a strain hardening and also an increase in fracture strain due to plastic deformation caused by twinning. Long term ageing at 700°C for up to 20 000 hours can cause different precipitation such as γ ́, M6C (Mo-rich) and M23C6 (Cr-rich) carbides. These carbides are both inter-and intra-granular particles. The long term ageing reduces the fracture toughness of the material, but the alloy can still have rather high impact toughness and fracture toughness even with an ageing at 700°C for 20 000 hour. The mechanisms have been studied using electron backscatter detection and electron channeling contrast imaging. It shows that besides dislocation slip, twinning is another main deformation mechanism in these aged Alloy 617 materials. At the crack front, plenty of micro or nanotwins can be observed. The formation of these twins leads to a high ductility and toughness which is a new observation or a new concept for this type of material.

Nanoscale fissure formation in AlxGa1–xN/GaN heterostructures and their influence on Ohmic contact formation

Nanoscale surface fissures on AlxGa1–xN/GaN (15 nm/1 µm) heterostructures grown by metalorganic vapour phase epitaxy (MOVPE) were imaged using tapping‐mode atomic force microscopy (AFM) and electron channelling contrast imaging (ECCI). Fissure formation was linked to threading dislocations, and was only observed in samples cooled under H2 and NH3, developing with increasing barrier layer Al content. No strain relaxation was detected regardless of fissure formation up to barrier layer Al composition fractions of x = 0.37. A reduction of measured channel carrier density was found in fissured samples at low temperature. This instability is attributed to shallow trap formation associated with fissure boundaries. For Ti/Al/Ni/Au Ohmic contact formation to high Al content barrier layers, fissures were found to offer conduction routes to the 2DEG that allow for low resistance contacts, with fissure‐free samples requiring additional optimisation of the metal stack and anneal conditions to achieve contact resistivity of order those measured in fissured samples. In addition, the effects of fissures were found to be detrimental to thermal stability of sheet and contact resistance, suggesting that fissure formation compromises the integrity of the 2DEG.

Analysis of dislocation configurations in a [0 0 1] fcc single crystal by electron channeling contrast imaging in the SEM.

We have investigated the dislocation configurations in a [0 0 1] single crystal of a face-centered alloy (316L stainless steel) by the electron channeling contrast imaging (ECCI) technique in the scanning electron microscope under controlled diffraction conditions. Specific dislocations such as piled-up dislocations and Lomer-Cottrell dislocations were characterized by the analysis of dislocation contrast and dislocation line trace analysis. The ECCI technique also allows the sound estimation of the local resolved stress acting on gliding dislocations by the analysis of the radius of curvature following a transmission electron microscopy-based geometrical approach.

Concurrent inheritance of microstructure and texture after slow β→α cooling of commercially pure Zr

A rolled and recrystallized commercially pure Zr sheet was β-solution treated and then cooled at two rates, i.e. air cooling (AC) and furnace cooling (FC). Microstructures and textures of original and β-cooled specimens were characterized by use of electron channeling contrast imaging, electron backscatter diffraction and X-ray diffraction techniques. Results reveal a novel phenomenon, i.e. the concurrent inheritance of microstructure and texture in the FC specimen cooled at a very slow rate. In contrast, for the AC specimen with faster cooling, typical lamellar α phases are obtained with relatively scattered texture. Based on comparatively crystallographic and thermodynamic analyses, reasons accounting for microstructure and texture differences in both cases are discussed, highlighting the significant role played by the variant selection behavior. It is postulated that increasing cooling rates should be more feasible to change the transformed texture in Zr materials.

Reprint of: Electron channelling contrast imaging for III-nitride thin film structures

Electron channelling contrast imaging (ECCI) performed in a scanning electron microscope (SEM) is a rapid and non-destructive structural characterisation technique for imaging, identifying and quantifying extended defects in crystalline materials. In this review, we will demonstrate the application of ECCI to the characterisation of III-nitride semiconductor thin films grown on different substrates and with different crystal orientations. We will briefly describe the history and the theory behind electron channelling and the experimental setup and conditions required to perform ECCI. We will discuss the advantages of using ECCI, especially in combination with other SEM based techniques, such as cathodoluminescence imaging. The challenges in using ECCI are also briefly discussed.

Characterization of Amorphous Oxide Nano-Thick Layers on 316L Stainless Steel by Electron Channeling Contrast Imaging and Electron Backscatter Diffraction.

Characterization of the topmost surface of biomaterials is crucial to understanding their properties and interactions with the local environment. In this study, the oxide layer microstructure of plasma-modified 316L stainless steel (SS316L) samples was analyzed by a combination of electron backscatter diffraction and electron channeling contrast imaging using low-energy incident electrons. Both techniques allowed clear identification of a nano-thick amorphous oxide layer, on top of the polycrystalline substrate, for the plasma-modified samples. A methodology was developed using Monte Carlo simulations combined with the experimental results to estimate thickness of the amorphous layer for different surface conditions. X-ray photoelectron spectroscopy depth profiles were used to validate these estimations.

Two-dimensional grain boundary sliding and mantle dislocation accommodation in ODS ferritic steel

The mechanism governing grain boundary sliding (GBS) accommodated by dislocation and microstructural evolution in regions II/III and III was studied to understand superplasticity. Two-dimensional GBS that occurred during high-temperature shear in oxide dispersion strengthened ferritic steel exhibiting an elongated and aligned grain structure was analyzed using surface markers drawn by focused ion beams. In addition, the accommodating dislocation structure was evaluated by electron back-scattered diffraction and electron channeling contrast imaging. In the initial stage of deformation, GBS triggered dislocation slippage in “mantle” areas near grain boundaries. These mantles tended to appear around GBS-resistant areas such as curved boundaries and grain protrusions. Next, the mantle dislocations generated dislocation walls before forming low-angle boundaries (LABs) along {110} crystallographic planes via dynamic recovery at the core/mantle boundaries. Finally, secondary GBS or rigid rotation occurred at the newly formed LABs to compensate for the initial GBS and resulted in continuous dynamic recrystallization. These mantle dislocation activities and substructural evolution mechanisms were graphically modeled and validated by comparison with previous studies.

Analysis of FIB-induced damage by electron channelling contrast imaging in the SEM.

We have investigated the Ga+ ion-damage effect induced by focused ion beam (FIB) milling in a [001] single crystal of a 316 L stainless steel by the electron channelling contrast imaging (ECCI) technique. The influence of FIB milling on the characteristic electron channelling contrast of surface dislocations was analysed. The ECCI approach provides sound estimation of the damage depth produced by FIB milling. For comparison purposes, we have also studied the same milled surface by a conventional electron backscatter diffraction (EBSD) approach. We observe that the ECCI approach provides further insight into the Ga+ ion-damage phenomenon than the EBSD technique by direct imaging of FIB artefacts in the scanning electron microscope. We envisage that the ECCI technique may be a convenient tool to optimize the FIB milling settings in applications where the surface crystal defect content is relevant.

Texture evolution and microstructural thermal stability of as-extruded AA2099 during hot deformation

Two thermal-mechanical regimes were selected to investigate the recrystallization process of an as-extruded AA2099 alloy. Specimens were deformed to strains of 0.4, 0.7 and 0.9 at 520°C and strain rates of 0.001s−1 and 0.1s−1, respectively. Electron backscatter diffraction (EBSD) and electron channeling contrast (ECC) imaging were performed for all specimens to characterize their textures and microstructures. The texture evolution is reflected by variation of deviation angle between <111> and extrusion directions, which appears to progressively approach ~35° (<110>//ED) due to lattice rotation in both regimes before ε=0.7. The reconstruction maps indicate that the nucleation of recrystallization is related to strain incompatibility near grain boundaries. The textures of specimens deformed to strain of 0.9 exhibit significant difference between the two regimes, i.e the <110>//ED fiber texture is comparatively weakened by recrystallization nuclei growth at the lower strain rate (0.001s−1). ECC images for specimen deformed at 0.001s−1 reveal significant differences in size and volume fraction of Al3Zr particles between recrystallized and unrecrystallized regions, suggesting remarkable influence of boundary migration on the thermal stability of Al3Zr particles.

Threading dislocation density characterization in III–V photovoltaic materials by electron channeling contrast imaging

Accurate and rapid threading dislocation density (TDD) characterization of III–V photovoltaic materials using electron channeling contrast imaging (ECCI) is demonstrated. TDDs measured using ECCI showed close agreement with those from electron beam-induced current mapping (EBIC) and defect selective etching (DSE). ECCI is shown to be well-suited for measuring TDD values over a range of ~5×106–5×108cm−2. ECCI can distinguish individual dislocations in clusters closer than 0.2µm, highlighting its excellent spatial resolution compared to DSE and EBIC. Taken together, ECCI is shown to be a versatile and complementary method to rapidly quantify TDD in III–V solar cells.

Characterization of encapsulated quantum dots via electron channeling contrast imaging

A method for characterization of encapsulated epitaxial quantum dots (QD) in plan-view geometry using electron channeling contrast imaging (ECCI) is presented. The efficacy of the method, which requires minimal sample preparation, is demonstrated with proof-of-concept data from encapsulated (sub-surface) epitaxial InAs QDs within a GaAs matrix. Imaging of the QDs under multiple diffraction conditions is presented, establishing that ECCI can provide effectively identical visualization capabilities as conventional two-beam transmission electron microscopy. This method facilitates rapid, non-destructive characterization of sub-surface QDs giving immediate access to valuable nanostructural information.

A Study on the Effect of Strain Rate on the Dynamic Recrystallization Mechanism of Alloy 617B

The effect of strain rate on dynamic recrystallization (DRX) behavior and mechanism of alloy 617B was investigated by isothermal compression test in a temperature range of 1393 K to 1483 K (1120 °C to 1210 °C) with a wide strain rate scope of 0.01 to 20 s−1. The microstructure evolution was investigated comprehensively by optical microscopy, electron backscatter diffraction (EBSD), electron channeling contrast imaging (ECCI), and transmission electron microscopy (TEM) to provide detailed insight into the effect of strain rate on DRX mechanism. The study shows that DRX is accelerated at both low strain rate and high strain rate conditions with an apparent sluggish kinetics at the intermediate strain rate of 1 s−1. In the low strain rate condition (i.e., <1 s−1), DRX is mainly controlled by the growth of DRX nuclei due to the sufficient time. When the strain rate is higher than 1 s−1, besides the commonly accepted reason of adiabatic heat generated by high strain rate, enhanced DRX nucleation mechanism is crucial for the promotion of DRX at high strain rate. High strain rate could lead to enhanced pile-up of dislocation and higher stored energy, which can facilitate the process of DRX. In addition, distortion or subdivision of twins and “grain fragment” are detected when the strain rate is higher than 1 s−1, which provide additional DRX nucleation mechanism. As a result, the combined effect leads to the higher DRX nucleation rate to promote DRX at high strain rate. The effect of strain rate on DRX is the completion result between sufficiency of time on the one hand and adiabatic heat and enhanced nucleation mechanism on the other.

Deformation mechanisms in a fine-grained Udimet 720LI nickel-base superalloy with high volume fractions of γ′ phases

Hot-deformation behaviors and mechanisms below γ′ solvus of U720LI with fine-grained microstructure and high volume fractions of γ′ phases were studied. MTS hot-compressed samples under hot-deformation parameters (Temperatures of 1040°C, 1070°C, 1100°C, 1130°C, strain rates of 0.01s−1, 0.1s−1, 0.5s−1 and strains of 0.11, 0.36, 0.69 and 1.2) were investigated by using multiple microstructural analysis methods, such as transmission electron microscopy (TEM), electron channeling contrast image (ECCI), et al.. Rare recovery and recrystallization were observed indicating that other deformation mechanisms might be enhanced during the deformation process. Except for the pinning effect, deformation happened within γ′ phases and also γ′ phase promoted the deformation of the matrix. When the slipping was inhibited by γ′ phases, twinning acted as a deformation mechanism in fine-grained U720LI. Due to the retardation effect of γ′ phases in the early stage of the deformation process, local grain boundary migration took effect. Once grain boundaries crossed γ′ phases, it made recrystallization by strain induced boundary motion(SIBM) easier.