Diffraction Line Profile Analysis Research Articles

Influence of hydrogen on deformation and embrittlement mechanisms in a high Mn austenitic steel: In-Situ neutron diffraction and diffraction line profile analysis

Austenitic steels have relatively high resistance to hydrogen embrittlement and play a critical role in hydrogen service applications. In particular, high Mn austenitic steels are considered economically viable alloy alternatives for these applications. The current study employed in-situ and ex-situ neutron diffraction techniques combined with diffraction line profile analysis (DLPA) to investigate the influence of hydrogen on deformation and embrittlement mechanisms in a high Mn (approximately 30 wt pct) austenitic steel. Investigation using both neutron diffraction and electron backscatter diffraction revealed the presence of extensive deformation twins and stacking faults within the steel microstructure after tensile deformation in the non-charged condition. These microstructural features suggest planar deformation behavior, which is expected from the relatively low stacking fault energy (SFE) of the alloy (approximately 29 mJ/m2). Hydrogen pre-charging resulted in apparent increases in both dislocations and stacking faults, contributing to macroscopic hardening and embrittlement mechanisms. Overall, numerical parameters obtained through neutron DLPA were used to elucidate the underlying mechanisms associated with hydrogen effects on the mechanical behavior, i.e. macroscopic strengthening, strain hardening rate, and embrittlement.

Nanostructuring and Hardness Evolution in a Medium‐Mn Steel Processed by High‐Pressure Torsion Technique

Severe plastic deformation (SPD) is performed on a newly developed medium‐Mn steel with the composition of Fe–7.66Mn–2Ni–1Si–0.23C–0.05Nb (wt%) to achieve a nanocrystalline microstructure. The SPD process utilizes the high‐pressure torsion (HPT) technique, resulting in a nominal shear strain of approximately 36 000% after processing the disk for 10 turns. In X‐Ray diffraction line profile analysis, an increase in dislocation density to around 230 × 1014 m−2 is observed. In addition, under high strains, a face‐centered cubic (fcc) secondary phase emerges within the body‐centered cubic (bcc) matrix. In analytical transmission electron microscopy, using energy‐dispersive X‐Ray spectroscopy, it is indicated that the secondary‐phase particles are enriched in Al, Mn, and Si. As the strain imposed during HPT increases, the simultaneous rise in dislocation density and nanostructuring lead to material hardening. However, the partial phase transformation from bcc to fcc contributes to material softening. As a result of these two opposite effects, the hardness exhibits a non‐monotonic variation with the shear strain, displaying, for 10 turns of HPT, a lower hardness compared to fewer turns, despite the continuous increase in dislocation density and decrease in crystallite size.

X-ray Diffraction Line Profile Analysis of Natural Calcite Minerals found in Southern Philippines by Williamson-Hall Method

This study employs the Williamson–Hall (W–H) models to examine the microstrains and crystallite sizes of CaCO3 occurring as calcite in limestone samples found in General Santos City and Sarangani Province, Southern Philippines. Using both the Uniform Deformation Model (UDM) and Uniform Stress Deformation (USDM) models, computations for average sizes were established to be identical, implying minimal strain influence. The consistency of resulting measurements extends to the microstrain, revealing uniform results for all samples. Correlation between crystallite sizes and microstrains in the calcite crystals was observed, where high-purity calcites exhibited larger crystallite sizes and microstrains. The crystallite sizes decrease with microstrains for calcites with higher Mg concentration, a finding that can be attributed to lattice distortion and the formation of defects. The release of stress forms these defects, thereby resulting in a reduction of microstrains. Moreover, the distinctly variable responses to strain exhibited by the samples could be influenced by either their anisotropic properties or other additional components. The W–H models, used jointly with UDM and USDM consistently predicted crystallite sizes, and thus offer valuable insights into the uniform stress responses of calcites. These promising results notwithstanding, USDM is shown to be especially relevant for anisotropic samples owing to the display deviations of crystallite sizes, a key feature of anisotropic natural calcites. The microscopic analysis is expected to provide additional understanding regarding the state of the limestone samples.

On some Features of the Grain and Subgrain Size in a Cu-Cr-Zr Alloy After ECAP Processing and Aging

A Cu-1Cr-0.1Zr alloy has been subjected to ECAP processing via route Bc and aging at 250-800°C. Electron BackScatter diffraction (EBSD), Transmission Electron Microscopy (TEM) and X-Ray Diffraction Line Profile Analysis (XRDLPA) techniques have been used to unveil some peculiarities of the grain and subgrain structure with a special emphasis on the comparison of the grain size estimated by the three techniques. For the alloy ECAP processed and aged up to 16 passes, the grain size (from EBSD, 0.2 < d < 5 μm), subgrain size (from TEM, d ~ 0.75 μm) and “apparent” average crystallite size (from XRDLPA, d < 0.25 μm) are manifestly different. The results were compared to the published data and analyzed based on the fundamental aspects of these techniques.

On the stable/metastable nature of the γ-hydride phase in Zircaloy-2: Microstructural characterization by electron diffraction, electron energy-loss spectroscopy, and diffraction line profile analysis

This work investigates the potential metastable versus stable nature of the γ-hydride in Zircaloy-2. Specimens were hydrided, and hydrides were precipitated through water-quenching. Synchrotron X-ray diffraction of the water-quenched sample revealed a diffraction peak with the d-spacing value of ∼2.70 Å. While this peak is conventionally attributed to {111}-γ planes, it could also stem from the (0004)-ζ plane. To clarify this ambiguity, the crystal structure of nano-hydrides was characterized by nano-beam electron diffraction (NBED) and electron energy-loss spectroscopy (EELS). While EELS detected nano-hydrides with plasmon energy (PE) values associated with the ζ-,γ-, and δ-phases, suggesting all three types of phases might be present, complementary NBED analysis revealed that regardless of the measured PE values, the examined nano-hydrides were of only γ- or δ-nature.Repeating the heating/quenching cycles reduced the γ-phase volume fraction until its (almost) complete disappearance after three cycles. δ-phase, however, was observed after each heating/quenching cycle. This observation, in accordance with previous reports, indicates that the γ-phase is metastable in Zircaloy-2, such that even during water-quenching (which is conventionally believed to facilitate the formation of γ-phase) only δ-hydrides form in cases where microstructural conditions are suitable.Diffraction line profile analysis and transmission electron microscopy revealed an increase in dislocation density during the first heating/quenching cycle, with no noticeable variations during subsequent cycles. A mechanism is proposed that links microstructure (i.e., dislocation structure) evolution during heating/quenching cycles to the suppression of the (metastable) γ-phase.

A spatially resolved analysis of dislocation loop and nanohardness evolution in proton irradiated Zircaloys

Proton irradiation is increasingly used as a surrogate for neutron irradiation, providing similar damage structures at significantly lower costs and less time compared to neutron irradiation. However, in contrast to neutrons, protons produce a depth dependent damage profile that incorporates a plateau region and a Bragg peak in the tens of microns region depending on the material and proton energy. Here we demonstrate that this depth dependent damage can be utilised to obtain new understanding about irradiation induced damage at different dose levels from a single sample by combining spatially resolved micro-beam synchrotron X-ray diffraction-based dislocation analysis and nanoindentation. For this purpose, and to study the damage evolution starting from very early stages, we have investigated microstructure evolution and hardening behaviour of Zircaloy-2 and Zircaloy-4 proton irradiated samples between 0.01 dpa and 17 dpa at 350 °C. The results highlight good agreements of SRIM-based damage depth predictions with irradiation-induced dislocation appearance and nanohardness. However, at even relatively low damage levels within the plateau region, dislocation line density and nanohardness profiles appear saturated across the entire irradiated region, even when the dpa levels differed significantly. When relating dislocation loop line densities to nanohardness, it was found that from a certain point hardness increased only very slightly with increasing line densities. This apparent discrepancy can be explained by a decreasing loop size for the highest line densities identified by from the diffraction line profile analysis and the application of a Dispersed Barrier Hardening model that relates obstacle strength to dislocation loop size.

Effect of Sn Addition on the Microstructure and Age-Hardening Response of a Zn-4Cu Alloy

The aim of this research is to assess the influence of Sn inclusion on the microstructure evolution and age-hardening response of a Zn-4Cu alloy. This is the first study to correlate the age-hardening response to the microstructure of Zn-4Cu alloy reinforced with different Sn contents. A series of Zn-4Cu-Sn alloys were successfully fabricated with different Sn concentrations in the range of 0.0–4.0 wt.% using permanent mold casting. The microstructure of Zn-4Cu-Sn alloys was investigated by means of a scanning electron microscope (SEM) attached with an energy dispersive spectroscope (EDS) and X-ray diffraction (XRD) line profile analysis. At room temperature, the Vickers microhardness measurements were used to assess the age-hardening response of alloys. The results show that the microhardness of the Zn-4Cu (ZC) binary alloy increases a little bit from 76 to 80 HV as the aging time increases from 2 to 128 h, respectively. For aging times up to 16 h, the microhardness of all Sn-containing alloys decreases but then increases again. The lowest hardness belongs to the ZC-1.5Sn alloy, and the Sn-Zn-3.0Sn alloy has the highest; the other alloys fall somewhere in between. At high aging times (64 and 128 h), the microhardness of all Sn-containing samples increased continuously with an increasing Sn content from 0.0 to 3.0 wt.%. When the Sn-containing alloys (3.5 and 4.0 wt.% Sn) were aged for 64 and 128 h, the hardness declined by 7.94% and 8.90% compared to their peak aging hardness values, respectively. By considering the structural changes that occur in the Zn-4Cu-Sn alloys, the reasons for the observed variations in microhardness data with increasing Sn content and aging time were elucidated. X-ray diffraction (XRD) data was analyzed to determine the zinc matrix’s lattice parameters, c/a ratio, and unit cell volume variations.

Micro-structural analysis of oxygen irradiated V-4Cr-4Ti by X-ray and electron back scattered diffraction

The effect of O6+ion irradiation on the microstructure of pre-deformed V-4Cr-4Ti alloy has been reported in this study. Changes in the microstructure has been assessed using detail X-ray diffraction line profile analysis in terms of the coherent domain size, rms micro-strain, dislocation density, their nature and their arrangement etc., revealing the importance of pre-deformation in controlling the material response to irradiation. The results are supported by Electron back scattered diffraction and Transmission electron microscopy. Energy Dispersive X-ray analysis has been used to map the micro-chemical changes caused in the sample due to the ion irradiation. Vicker's micro-hardness values were determined to understand the effect of irradiation on the mechanical property of the alloy. The results are explained in terms of the occurrence of vacancy-solute complexes, the formation of which isestablished using Density Functional Theory calculations..

X-Ray Diffraction line profile analysis of defects and precipitates in high displacement damage neutron-irradiated austenitic stainless steels

Irradiation-induced defects and the precipitates in the wrapper material of the Indian Fast Breeder Test Reactor (FBTR), SS 316 are analyzed using the synchrotron source-based Angle Dispersive X-Ray Diffraction (ADXRD) technique with X-rays of energy 17.185 keV (wavelength ∼0.72146 Å). The differences and similarities in the high displacement damage samples as a function of dpa (displacement per atom) and dpa rate in the range of 2.9 × 10−7- 9 × 10−7dpa/s are studied. Ferrite and M23C6 are commonly observed in the present set of high displacement damage 40–74 dpa SS 316 samples irradiated at temperatures in the range of 400–483 °C. Also, the dislocation density has increased as a function of the irradiation dose. The X-ray diffraction peak profile parameters quantified such as peak shift and asymmetry show that the irradiation-induced defects are sensitive to the dpa rate-irradiation temperature combinations. The increase in yield strength as a function of displacement damage is also correlated to the dislocation density.

Tensile strain-hardening behavior and related deformation mechanisms of pure titanium at cryogenic temperature

The tensile strain-hardening behavior of pure Ti at 100 K was investigated using X-ray diffraction line-profile analysis and plasticity simulation. The strain hardening was significantly increased at 100 K, compared with that observed at 298 K. Thus, at 100 K, necking was suppressed during tensile testing, which greatly increased material ductility. The remarkable increase in strain hardening at 100 K was attributed to the dominant activation of prismatic <a> slip and the exceptionally increased rate of its activation stress with tensile strain at 100 K. This finding significantly advances the understanding of the strain-hardening behavior of pure Ti at low temperatures, and it can also guide the development of texture-engineering strategies to increase the low-temperature ductility of pure Ti.

Effect of Si on the evolution of plasticity mechanisms, grain refinement and hardness during high-pressure torsion of a non-equiatomic CoCrMnNi multi-principal element alloy

The present study unraveled the defining role of small silicon (Si) addition (5 atomic %) in dramatically altering the plasticity mechanisms, grain refinement and hardening response of a non-equiatomic CoCrMnNi multi-principal element alloy (MPEA) during high-pressure torsion (HPT) processing. Both the Si-free and the Si-added MPEAs had a face-centered cubic (FCC) structure and were subjected to a quasi-constrained HPT processing at 6 GPa pressure to different number of turns (0.5 and 5). Microstructure evolution was studied at the center and edge of the HPT-processed discs using X-ray diffraction line profile analysis (XLPA) and transmission electron microscopy (TEM). Si addition altered the predominant plasticity mechanism from micro-band formation to extensive occurrence of nano-twinning at the early stage of HPT processing. At later stages of HPT processing, both alloys exhibited deformation twinning but its propensity was considerably higher for the Si-added MPEA, as revealed by ∼50% higher twin fault probability. Additionally, the Si-added MPEA showed ∼30% higher dislocation density at any given stage of HPT processing compared to the Si-free MPEA. A significantly accelerated nano-structuring coupled with a finer saturation grain size was observed in the Si-added MPEA (34 nm for Si-free versus 23 nm for Si-added). These effects can be explained by the influence of Si addition on lowering the stacking fault energy (SFE) (from ∼40 mJ/m2 in Si-free to ∼20 mJ/m2 in Si-added MPEA) and increasing the solute pinning effect of Si on lattice defects. The plasticity mechanisms at nano-scale were also influenced by the presence of Si as confirmed by the formation of nano-twins and stacking faults inside the nano-grains for the Si-added and Si-free MPEAs, respectively. The differences in plasticity mechanisms and microstructure evolution resulted in enhanced hardness in the early stages of HPT processing for the Si-added MPEA, but the difference in hardness between the two alloys tended to be reduced at higher strains.

Effect of Oxygen Ion Irradiation on Nb-1Zr-0.1C Alloy Characterized Using X-Ray Diffraction Line Profile Analysis

One of the proposed materials for structural application in compact high-temperature reactors (CHTRs) is Nb-1Zr-0.1C alloy. Using the Variable Energy Cyclotron at the Variable Energy Cyclotron Centre, Kolkata, Nb-1Zr-0.1C alloy was irradiated with a 160-MeV oxygen (O6+) ion up to three different doses. Emulation of neutron irradiation by ion irradiation could be achieved as the weighted recoil spectra of the oxygen ion are found to be similar to the neutron recoil spectra of CHTRs within recoil energy ranging from 100 eV to 100 keV. The irradiated materials along with one as-received sample were characterized using different X-ray diffraction line profile analyses (XRDLPAs) to systematically evaluate microstructural parameters. A decrease in the domain size with an increase in microstrain and dislocation density is observed at first dose and then found to saturate with further irradiation. An increase in the Wilkens arrangement parameter indicates the formation of less correlated dislocations (clusters) after irradiation. Transmission electron microscopy analysis of as-received and highest-dose samples shows the formation of densely populated defect clusters after irradiation. Nanohardness increased after irradiation due to pinning of the dislocation movement by point defects and defect clusters/loops, as well as carbides in the matrix. The results extracted from the XRDLPAs are compared with our earlier studies of light ion–irradiated (H+) Nb-1Zr-0.1C alloy and oxygen-irradiated pure Nb to understand the effect of the type of ion and the alloying elements, respectively, on the evolution of the microstructure. It may be concluded that changes in dose and dose rate affect the movement of point defects toward sinks. Hence, possible correlated dislocation formation is observed in light ion–irradiated Nb alloy, but correlation is found to decrease with dose for heavy ion–irradiated Nb alloy. On the other hand, the presence of finely dispersed carbides restricts the formation of dislocation loops by making complexes with the defects in heavy ion (O6+)–irradiated Nb-1Zr-0.1C alloy, which is in contrast to pure Nb irradiated using the heavy ion (O6+) in a similar environment.

X-ray diffraction line profile analysis for the detection of the propensity to sensitize

Prior studies have revealed that the sensitization kinetics of 5xxx-series Al-Mg alloys are responsive to the dislocation content, with lower dislocation densities leading to higher rates of sensitization. In this work, X-ray line profile analysis (LPA) was employed to non-destructively assess the dislocation density in 5083 and 5456 alloys samples in various tempers and thermomechanical processing states. Using a conventional laboratory powder diffractometer with a Cu-Kα sealed tube source, it is shown that the approach has the ability to discriminate between samples of disparate tempers (H131, H116, and solutionized and water quenched). Destructive electron backscattered diffraction (EBSD) measurements on select samples confirm the variations, from the perspective of geometrically necessary dislocation density. Experiments were also performed using softer X-rays generated using a Cr Kα sealed tube source, which would render the approach more portable, due to lower shielding requirements. Unfortunately, Cr radiation was not successful due to the limited number of accessible diffraction peaks. Using the dislocations densities measured using LPA together with an established constitutive model permits accurate prediction of the mechanical strength of the alloys of the above disparate tempers. However, the technique does not appear capable of discriminating between samples within a given temper (e.g., H116). Use of a more highly monochromatic X-ray source could render the technique useful for a comprehensive structural health monitoring system for 5xxx alloys prone to sensitization.

X-ray diffraction line profile analysis of defects in neutron-irradiated austenitic stainless steels at low displacement damage levels

Neutron irradiation-induced microstructural changes in variants of austenitic stainless steels were characterized using the Angle Dispersive X-Ray Diffraction (ADXRD) technique with a synchrotron X-ray source of energy 14.968 keV (wavelength ∼0.82833 Å). SS 304 L(N), SS 316 L(N), and SS 316 materials were neutron-irradiated to low displacement damage levels (1–6.75 dpa) in the Fast Breeder Test Reactor at Kalpakkam at temperatures in the range ∼380 °C-400 °C. The effect of the irradiation-induced defects on X-ray diffraction peak profile parameters such as peak broadening, peak shift, and asymmetry were quantified and related to dislocation density. Peak broadening is found to increase as a function of dpa in most of the cases. Considering the highest dpa sample, lattice contraction has been shown by SS 304 L(N) and SS 316 whereas lattice expansion is exhibited by SS 316 L(N). Asymmetry in peak broadening is found to decrease in case of the highest dpa sample. Ferrite volume percent is seen to have increased as a function of dpa in SS 304 L(N) and SS 316 L(N) but not observed in SS 316. SS 304 L(N) has shown a greater propensity towards the austenite to ferrite transformation and 5 dpa sample has about 18 vol% of α-ferrite. However, in case of 5 dpa SS 316 L(N), ferrite content has increased to ∼4 vol% . The increase in yield strength was also related to the dislocation density amongst all three grades of stainless steel. SS 304 L(N) showed saturation in dislocation density and yield strength around 2 dpa whereas SS 316 L(N) showed linear behaviour up to the highest dpa.

Competitive strengthening between dislocation slip and twinning in cast-wrought and additively manufactured CrCoNi medium entropy alloys

In situ neutron diffraction experiments have been performed under loading in cast-wrought (CW) and additively manufactured (AM) equiatomic CoCrNi medium-entropy alloys. The diffraction line profile analysis correlated the faulting-embedded crystal structure to the dislocation density, stacking/twin fault probability, and stacking fault energy as a function of strain. The results showed the initial dislocation density of 1.8 × 1013m−2 in CW and 1.3 × 1014m−2 in AM. It significantly increased up to 1.3 × 1015m−2 in CW and 1.7 × 1015m−2 in AM near fracture. The dislocation density contributed to the flow stress of 470 MPa in CW and 600 MPa in AM, respectively. Meanwhile, the twin fault probability of CW (2.7%) was about two times higher than AM (1.3%) and the stacking fault probability showed the similar tendency. The twinning provided strengthening of 360 MPa in CW and 180 MPa in AM. Such a favorable strengthening via deformation twinning in CW and dislocation slip in AM was attributed to the stacking fault energy. It was estimated as 18.6 mJ/m2 in CW and 37.5 mJ/m2 in AM by the strain field of dislocations incorporated model. Dense dislocations, deformation twinning, and atomic-scale stacking structure were examined by using electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM).

Formation and Microstructural Evolution of Ferritic ODS Steel Powders during Mechanical Alloying.

Ferritic ODS steel elemental powder compositions with various Zr content (0.3-1.0 wt.%), ground in a Pulverisette 6 planetary ball mill, were extensively studied by X-ray diffraction line profile analysis, microscopic observations, microhardness testing and particle size measurements. A characteristic three-stage process of flattening the soft powders, formation of convoluted lamellae and, finally, formation of nanocrystalline grains was observed. In order to quantify the microstructural properties, expressed mainly in terms of crystallite size and dislocation density, a methodology for detailed and accurate microstructure analysis of nanosized and severely deformed materials was proposed by the Whole Powder Pattern Modelling (WPPM) approach. In the case of the proposed ODS alloy composition, the overlapping of Fe and Cr Bragg reflections makes the microstructure analysis certainly more complicated. The results showed that the microstructure of powders evolved towards the nanocrystalline state consisting of fine (diameter of ~15 nm) and narrowly dispersed domains, with extensive dislocation density exceeding 1016 m-2.

Investigation of Quantitative Evaluation of Rolling Contact Fatigue Cracks in Rail Steel by X-Ray Diffraction Line Profile Analysis

Investigation of Quantitative Evaluation of Rolling Contact Fatigue Cracks in Rail Steel by X-Ray Diffraction Line Profile Analysis

Strengthening of high-entropy alloys via modulation of cryo-pre-straining-induced defects

• High entropy alloy was strengthened by cryo-pre-straining-induced defects. • Strengthening mechanism was quantitatively revealed by neutron diffraction method. • Selective recovery of crystal defects assist to optimize the mechanical performance. Owing to their attractive structure and mechanical properties, high-entropy alloys (HEAs) and medium-entropy alloys (MEAs) have attracted considerable research interest. The strength of HEAs/MEAs with a single face-centered cubic (FCC) phase, on the other hand, requires improvement. Therefore, in this study, we demonstrate a strategy for increasing the room-temperature strength of FCC-phase HEAs/MEAs by tuning cryo-pre-straining-induced crystal defects via the temperature-dependent stacking fault energy-regulated plasticity mechanism. Through neutron diffraction line profile analysis and electron microscope observation, the effect of the tuned defects on the tensile strength was clarified. Due to the cryo-rolling-induced high dislocation density, mechanical twins, and stacking faults, the room-temperature yield strength of an equiatomic CoCrFeNi HEA was increased by ∼290%, from 243 MPa (as-recrystallized) to 941.6 MPa (30% cryo-rolled), while maintaining a tensile elongation of 18%. After partial recovery via heat treatment, the yield strength and ultimate tensile strength decreased slightly to 869 and 936 MPa, respectively. Conversely, the elongation increased to 25.6%. The dislocation density and distribution of the dislocations were found to contribute to the strengthening caused by forest dislocations, which warrants further investigation. This study discussed the possibility of developing single-phase high-performance HEAs by tuning pre-straining-induced crystal defects.

Experimental analysis of deformation texture evolutions in pure Cu, Cu-37Zn, Al-6Mg, and −8Mg alloys at cold-rolling processes

Generally, two types of deformation textures of copper-type and brass-type textures are evolved in face-centered cubic (FCC) metals. During deformation, dislocation motion determines which texture will be dominant. The copper-type texture is formed in metals of high stacking fault energy by cross-slip of dislocations and subsequent dislocation cell formation. On the other hand, deformation twinning involves the brass-type texture evolution, whereas some exceptions, such as Al-Mg alloys, also have been reported. This study examined deformation texture evolutions in four cold-rolled FCC alloys of pure Cu, Brass (Cu-37Zn), Al-6Mg, and Al-8Mg alloys. Electron backscattered diffraction and X-ray line profile analysis methods investigated the deformation texture evolution. Three different strains of 0.25, 0.45, and 0.63 were applied to observe the strain effect on texture evolution. In pure Cu, the copper-type texture is developed, as commonly known. The brass-type texture is developed in Brass and Al-Mg alloys. More reduction ratios in those alloys lead to the copper-type texture strengthening in pure Cu, whereas stronger brass-type texture is shown in Brass and Al-Mg alloys by applying more reduction. While the brass-type texture evolution in Brass can be illustrated by deformation twinning, deformation twins are absent in deformed Al-Mg alloys despite their evident brass-type texture formation. Instead, the short-range ordering (SRO) mechanism can explain the brass-texture evolution in Al-Mg alloys. Planar slips by the high Mg content of Al alloys strengthen the rotated Goss orientation with brass-type texture evolution after cold-rolling processes of those alloys.

Dislocation density evolution in cold-rolled Zr-2.5%Nb pressure tubes under thermal treatments by high energy XRD and neutron TOF diffraction peak profile analysis

Diffraction line profile analysis was done to characterize the change in the dislocation density at different stages of the processing route of a Zr-2.5%Nb pressure tube. Two diffraction experiments were carried out: High Energy X-Ray Diffraction (HE-XRD) and Neutron Time of Flight Diffraction (TOF-ND). On samples in the extruded, cold-rolled and post-annealed conditions, the HE-XRD experiment in transmission geometry allows a detailed characterization of the dependence of the line shape on the direction of the scattering vector. Important variations of the FWHM (Full Width at Half Maximum) were observed, which was interpreted as the non-uniform distribution of dislocations among grains with different orientations. Average values of the dislocation density and subgrain size were obtained after applying the Warren-Averbach method.The effect of post deformation annealing for soaking temperatures from 400° to 450°C was studied using TOF-ND. Peak profile analysis was performed on in-situ neutron time-of-flight diffractograms to obtain peak positions and widths to calculate residual stresses and dislocation densities. The results show that the dislocation density decreases largely at early times and it is followed by a slow diminution over time. Dislocation density decreases from ∼8 × 1014 m−2 for the cold-rolled sample to values close or under 2 × 1014 m−2. A remnant dislocation density after long annealing times was detected, with a value that decreases as the soaking temperature increases. Dislocation type was also characterized. It was found that dislocations with 〈a〉 Burgers vectors represent approximately 90% of the population, while the other 10% are 〈c+a〉. An empirical recovery kinetics model was proposed where dislocation mobility is assumed as a thermally activated mechanism. This model can be used as a processing tool to estimate the dislocation density expected for different soaking temperatures and times. The effect of residual stresses on peak broadening was also discussed. It was estimated that this contribution represents around 10–20% to the observed physical line broadening.