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At least 1,621 records · Page 90
All sourcesNASA NTRSDOE OSTI
DOE OSTI2013

Microstructure characterization of the stir zone of submerged friction stir processed aluminum alloy 2219

Aluminum alloy 2219-T6 was friction stir processed using a novel submerged processing technique to facilitate cooling. Processing was conducted at a constant tool traverse speed of 200 mm/min and spindle rotation speeds in the range from 600 to 800 rpm. The microstructural characteristics of the base metal and processed zone, including grain structure and precipitation behavior, were studied using optical microscopy (OM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Microhardness maps were constructed on polished cross sections of as-processed samples. The effect of tool rotation speed on the microstructure and hardness of the stir zone was investigated. The average grain size of the stir zone was much smaller than that of the base metal, but the hardness was also lower due to the formation of equilibrium θ precipitates from the base metal θ′ precipitates. Stir zone hardness was found to decrease with increasing rotation speed (heat input). The effect of processing conditions on strength (hardness) was rationalized based on the competition between grain refinement strengthening and softening due to precipitate overaging. - Highlights: • SZ grain size (∼ 1 μm) is reduced by over one order of magnitude relative to the BM. • Hardness in the SZ is lower than that of the precipitation strengthened BM. • Metastable θ′ in the base metal transforms to equilibrium θ in the stir zone. • Softening in the SZ results from a decrease of precipitation strengthening.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effects of gas to melt ratio on the microstructure of an Al–10.83Zn–3.39Mg–1.22Cu alloy produced by spray atomization and deposition

Various gas to melt ratios (GMR) that govern the cooling rate of spray forming can be achieved through controlling the atomizer form and the atomization pressure. The effect of the GMR on microstructures of an Al–10.83Zn–3.39Mg–1.22Cu alloy produced through spray forming has been studied using electron microscopy. When the GMR is high at 3.5, dendritic structure and quasi-crystalline i-Mg{sub 32}(AlZn){sub 49} particles inherited from the original powders can be observed. Spray forming at medium GMR of 2.3 produces equiaxed α-Al grains and MgZn{sub 2} phase that discontinuously distributes along the grain boundaries and within the grains as small particles. The low GMR of 1.4 corresponds to low cooling rate. Coarse and equiaxed α-Al grains together with eutectic structure consisting of b.c.c.-Mg{sub 32}(AlZn){sub 49} and α-Al phases along the grain boundaries are obtained. - Highlights: • At high GMR, the broken fragments and i-Mg{sub 32}(AlZn){sub 49} quasicrystal are observed. • At medium GMR, microstructure consists of α-Al equiaxed grains and MgZn{sub 2} phase. • At low GMR, the coarsened α-Al grains and bcc-Mg{sub 32}(AlZn){sub 49} eutectic appear.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effect of heat input on the microstructure, residual stresses and corrosion resistance of 304L austenitic stainless steel weldments

Austenitic stainless steels are widely used in high performance pressure vessels, nuclear, chemical, process and medical industry due to their very good corrosion resistance and superior mechanical properties. However, austenitic stainless steels are prone to sensitization when subjected to higher temperatures (673 K to 1173 K) during the manufacturing process (e.g. welding) and/or certain applications (e.g. pressure vessels). During sensitization, chromium in the matrix precipitates out as carbides and intermetallic compounds (sigma, chi and Laves phases) decreasing the corrosion resistance and mechanical properties. In the present investigation, 304L austenitic stainless steel was subjected to different heat inputs by shielded metal arc welding process using a standard 308L electrode. The microstructural developments were characterized by using optical microscopy and electron backscattered diffraction, while the residual stresses were measured by X-ray diffraction using the sin{sup 2}ψ method. It was observed that even at the highest heat input, shielded metal arc welding process does not result in significant precipitation of carbides or intermetallic phases. The ferrite content and grain size increased with increase in heat input. The grain size variation in the fusion zone/heat affected zone was not effectively captured by optical microscopy. This study shows that electron backscattered diffraction is necessary to bring out changes in the grain size quantitatively in the fusion zone/heat affected zone as it can consider twin boundaries as a part of grain in the calculation of grain size. The residual stresses were compressive in nature for the lowest heat input, while they were tensile at the highest heat input near the weld bead. The significant feature of the welded region and the base metal was the presence of a very strong texture. The texture in the heat affected zone was almost random. - Highlights: • Effect of heat input on microstructure, residual stresses and corrosion is studied. • HAZ and width of dendrite in the welded region increase with heat input. • Residual stresses are tensile near the welded region after the highest heat input. • Welded region has the highest pit density after highest heat input. • Dendrites and δ-ferrite were highly oriented in the welded region.

36 MATERIALS SCIENCE↗
DOE OSTI2014

EBSD study on crystallographic texture and microstructure development of cold-rolled FePd alloy

The crystallographic texture and microstructure of FePd alloy after cold-rolling deformation were investigated using electron backscatter diffraction. The major orientations of twin copper and copper after 50% thickness reduction were observed in face-centered cubic-disordered FePd alloy, whereas the main orientation was obtained from brass type after 90% cold rolling. Increase in cold rolling resulted in the change of preferred orientation from copper to brass. Decrease in orientation intensity of copper also increased that of Goss and brass. - Highlights: • The evolution of texture and microstructure in FePd alloy was investigated after cold rolling using EBSD. • Increasing in reduction leads to the change of texture from Copper-type to Brass-type. • The reduction of Copper orientation results in increasing in Goss and Brass orientations.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effect of processing conditions on microstructural features in Mn–Si sintered steels

Sintering of steels containing oxidation sensitive elements is possible if such elements are alloyed with others which present lower affinity for oxygen. In this work, a master alloy powder containing Fe–Mn–Si–C, specifically designed to create a liquid phase during sintering, has been used for such purpose. The effect of processing conditions such as sintering temperature and atmosphere was studied with the aim of describing the microstructural evolution as well as the morphology and distribution of oxides in the sintered material, evaluating the potential detrimental effect of such oxides on mechanical properties. Chemical analyses, metallography and fractography studies combined with X-ray photoelectron spectroscopy analyses on the fracture surfaces were used to reveal the main mechanism of fracture and their correlation with the chemical composition of the different fracture surfaces. The results indicate that the main mechanism of failure in these steels is brittle fracture in the surrounding of the original master alloy particles due to degradation of grain boundaries by the presence of oxide inclusions. Mn–Si oxide inclusions were observed on intergranular decohesive facets. The use of reducing atmospheres and high sintering temperatures reduces the amount and size of such oxide inclusions. Besides, high heating and cooling rates reduce significantly the final oxygen content in the sintered material. A model for microstructure development and oxide evolution during different stages of sintering is proposed, considering the fact that when the master alloy melts, the liquid formed can dissolve some of the oxides as well as the surface of the surrounding iron base particles. - Highlights: • Oxide distribution in steels containing oxidation-sensitive elements • Mn, Si introduced in a master alloy powder, mixed with a base iron powder • Selective oxidation of Mn and Si on iron grain boundaries • Decohesive fracture caused by degradation of grain boundaries by oxide inclusions • Reducing agents efficient at low temperatures critical for avoiding oxide inclusions.

36 MATERIALS SCIENCE↗
DOE OSTI2014

The effect of boron addition on microstructure and mechanical properties of biomedical Ti35Nb6Ta alloy

The beta-titanium alloys are promising materials for bioapplications but their processing via melting is difficult. Coarse grains have been observed in as-cast specimens. Subsequent thermo-mechanical processing seems to be necessary in order to obtain fine-grained microstructure with better mechanical properties. The grain size can be decreased significantly by addition of small boron amount. In this work Ti–35Nb–6Ta alloy with various B additions (0, 0.05, 0.1, 0.3 and 0.5 wt.%) has been studied. Even the smallest amount of B leads to significant grain refinement in Ti–35Nb–6Ta alloy (from 1300 to about 350 μm). Slight grain refinement has been observed also after hot forging and solution treatment. TiB particles emerged in specimens due to B addition. These particles contribute to changes in mechanical properties not only in hot forged and solution treated specimens (hardness increase from 140 to 180 HV10), but also in cold swaged specimens (hardness from 230 to 250 HV10, tensile strength from 800 to 920 MPa). The hardness values can be increased up to 370 HV10 during aging at 400 °C (specimen with 0.5 wt.% B). It has been observed that specimens with low boron addition 0.05 wt.% possess no cytotoxicity. On the other hand in specimens with 0.1 wt.% B or more slight adverse effect on cytotoxicity has been observed. - Highlights: • The influence of boron on microstructure and mechanical properties has been studied. • Beta-transus temperature has been determined. • Cytotoxicity depending on boron content has been evaluated. • Possibility of final heat treatment has been determined.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Quantitative phase analysis and microstructure characterization of magnetite nanocrystals obtained by microwave assisted non-hydrolytic sol–gel synthesis

An innovative preparation procedure, based on microwave assisted non-hydrolytic sol–gel synthesis, to obtain spherical magnetite nanoparticles was reported together with a detailed quantitative phase analysis and microstructure characterization of the synthetic products. The nanoparticle growth was analyzed as a function of the synthesis time and was described in terms of crystallization degree employing the Rietveld method on the magnetic nanostructured system for the determination of the amorphous content using hematite as internal standard. Product crystallinity increases as the microwave thermal treatment is increased and reaches very high percentages for synthesis times longer than 1 h. Microstructural evolution of nanocrystals was followed by the integral breadth methods to obtain information on the crystallite size-strain distribution. The results of diffraction line profile analysis were compared with nanoparticle grain distribution estimated by dimensional analysis of the transmission electron microscopy (TEM) images. A variation both in the average grain size and in the distribution of the coherently diffraction domains is evidenced, allowing to suppose a relationship between the two quantities. The traditional integral breadth methods have proven to be valid for a rapid assessment of the diffraction line broadening effects in the above-mentioned nanostructured systems and the basic assumption for the correct use of these methods are discussed as well. - Highlights: • Fe{sub 3}O{sub 4} nanocrystals were obtained by MW-assisted non-hydrolytic sol–gel synthesis. • Quantitative phase analysis revealed that crystallinity up to 95% was reached. • The strategy of Rietveld refinements was discussed in details. • Dimensional analysis showed nanoparticles ranging from 4 to 8 nm. • Results of integral breadth methods were compared with microscopic analysis.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Microstructural evolution of nanocrystalline Fe–Zr alloys upon annealing treatment

Nanocrystalline Fe–Zr alloys exhibit an extraordinary thermal stability at elevated temperatures, which enables their potential applications in various fields. However, there remain concerns regarding the controlling stabilization mechanisms responsible for their thermal stability. In this work, two nanocrystalline Fe–Zr alloys containing 1 at.% Zr and 5 at.% Zr were annealed at various temperatures (T{sub ann}) up to 900 °C. Microstructural evolution of the alloys upon annealing was investigated by means of an X-ray diffractometer equipped with a 2-dimensional detector and transmission electron microscopy. Below 600 °C, microstructures of the two alloys consist of single nanocrystalline ferrite whose grain size is rather stable upon annealing treatments. Above 600 °C, accompanying the precipitation of Fe{sub 3}Zr phase, an apparent grain coarsening of ferrite is observed, whereas the thermal stability of the alloys is still considerably higher than that of nanocrystalline pure Fe. Based on the experimental results, it was claimed that stabilization of the nanocrystalline Fe–Zr alloys should not be totally ascribed to the thermodynamic stabilization mechanism due to the reduction in grain boundary energy as suggested in earlier investigations [K.A. Darling et al., Scr. Mater. 59 (2008) 530 and K.A. Darling et al., Mater. Sci. Eng. A527 (2010) 3572]; when T{sub ann} is higher than 600 °C, along with the precipitation of Fe{sub 3}Zr, the effect of thermodynamic stabilization is weakened, the kinetic effect arising from Zener pinning of Fe{sub 3}Zr precipitates turns to be an important mechanism contributing to the stabilization of the nanoscale grain size. - Highlights: • We show clear evidence of precipitation of Fe{sub 3}Zr phase above 600 °C. • Stabilization of nanostructure is not solely controlled by thermodynamic mechanism. • Above 600 °C, Zener pinning plays an important role in stabilizing nanostructure.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Nanostructured aluminium titanate (Al{sub 2}TiO{sub 5}) particles and nanofibers: Synthesis and mechanism of microstructural evolution

In this study, aluminium titanate (AT) particles and nanofibers were synthesized through citrate sol gel and sol gel-assisted electrospinning methods in both nanostructured powder and nanofiber forms. The results of X-ray diffraction analysis, field-emission scanning electron microscopy and differential thermal analysis showed that the synthetic products benefit a nanostructured nature with a grain size less than 70 nm. The optimal values for time and temperature at which a roughly pure AT is attained were determined as 2 h and 900 °C, respectively. It was found that the sol gel precursor bears an amorphous structure till 700 °C and begins to be crystallized to alumina, anatase and AT at higher temperatures. Moreover, AT tends to decompose into rutile and alumina at temperatures higher than 900 °C and its degradation rate reaches a maximum at temperatures near to 1100 °C. In this synthesis, citric acid was used as a chelating agent for Al{sup 3} {sup +} and Ti{sup 4} {sup +} ions and it was shown that a low citric acid-to-metal cation ratio leads to larger numbers of nuclei during crystallization and smaller grain size. Finally, a model was suggested to describe the microstructural evolution of AT compound based on a nucleation and growth regime. - Graphical abstract: Display Omitted - Highlights: • We synthesized aluminium titanate ceramic in both powder and nanofiber forms. • The methods in use were citrate sol gel and sol gel-assisted electrospinning. • Powders and nanofibers bear a nanostructured nature with a grain size less than 70 nm. • A model is suggested to describe microstructural evolution of synthetic products.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Thermal stability of bimodal microstructure in magnesium alloy AZ91 processed by ECAP

The changes in microstructure of equal channel angular pressing (ECAP) processed magnesium alloy AZ91 during thermal exposure were studied in this paper. The microstructure stability was investigated by means of electron backscatter diffraction (EBSD), which allowed to measure the changes in grain size, mutual ratio of low-angle boundaries (LABs) to high-angle ones (HABs) and local lattice distortion evaluated by the kernel average misorientation (KAM) parameter. It was found experimentally that the threshold temperature at which significant grain coarsening takes place is 350 °C. No modification to mean grain diameter occurs below this temperature, nonetheless, some changes in LAB and HAB fraction, as well as in local lattice distortion, can be observed. - Highlights: • Thermal stability of bimodal UFG AZ91 alloy was assessed by means of EBSD. • Threshold temperature for pronounced grain coarsening was found at 350 °C. • Below 350 °C increase in LAB fraction and local lattice distortion takes place. • Local lattice distortion (LLD) can be well described using KAM approach. • LLD is influenced by coarsening and precipitation of Mg{sub 17}Al{sub 12} particles.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Microstructure evolution of Ag–8Au–3Pd alloy wire during electromigration

As the continuous shrinkage of the interconnect line width in microelectronics devices, there is a growing concern about the electromigration (EM) failure of bonding wire. In addition, an innovative Ag–8Au–3Pd alloy wire has shown promise as an economical substitute for gold wire interconnects due to the cost pressure of gold in the last decade. In present study of the Ag–8Au–3Pd alloy wire, the surface diffusion occupied the dominant position during EM failure, and the activation energy was found to be 0.61 eV. In order to reveal the failure mechanism, the cross-sections of the Ag–8Au–3Pd alloy wire during EM were prepared by focused ion beam (FIB) micro-machining for electron backscatter diffraction (EBSD) analysis. The microstructure evolution of the Ag–8Au–3Pd alloy wire was characterized by the grain size and grain boundary. As a result, the EM failure originates in the atom transportation, which causes grain size increasing and atom diffusion on the wire surface. - Highlights: • The activation energy of Ag–8Au–3Pd alloy wire was obtained as 0.61 eV. • During EM, the silver atoms diffused from negative to the positive terminal on the wire surface. • The microstructure (grain size and grain boundary) was characterized by FIB-EBSD. • During EM, the atom transportation was found to cause grain size growth and atom diffusion on the wire surface.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructural evolution and grain growth kinetics of GZ31 magnesium alloy

Grain growth behavior of Mg–3Gd–1Zn (GZ31) magnesium alloy was studied in a wide range of annealing time and temperature to clarify the kinetics of grain growth, microstructural evolution and related metallurgical phenomena. This material exhibited typical normal grain growth mode under annealing conditions with annealing temperature of lower than 300 °C and soaking time of lower than 240 min. However, the abnormality in grain growth was also evident at annealing temperature of 400 °C and 500 °C. The dependence of abnormal grain growth (AGG) at mentioned annealing temperatures upon microstructural features such as dispersed precipitates, which were rich in Zn and Gd, was investigated by optical micrographs, X-ray diffraction patterns, scanning electron microscopy images, and energy dispersive X-ray analysis spectra. The bimodality in grain-size distribution histograms also signified the occurrence of AGG. Based on the experimental data on grain growth obtained by annealing treatments, the grain growth exponent and the activation energy were also figured out.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructure of selective laser melted CM247LC nickel-based superalloy and its evolution through heat treatment

The selective laser melting of high temperature alloys is of great interest to the aerospace industry as it offers the prospect of producing more complex geometries than can be achieved with other manufacturing methods. In this study, the microstructure of the nickel-based superalloy, CM247LC, has been characterised following selective laser melting and after a post deposition heat treatment below the γ′ solvus temperature. In the as-deposited state, scanning electron microscopy with electron backscatter diffraction revealed a fine, cellular microstructure with preferential alignment of 〈001〉 along the build direction. A high dislocation density was seen at the periphery of the cells, indicating substantial localised deformation of the material. Fine primary MC carbides were also observed in the inter-cellular regions. High-resolution transmission electron microscopy identified the occurrence of very fine γ′ precipitates, approximately 5 nm in diameter, dispersed within the gamma phase. After heat treatment, the elongated cell colonies were observed to partially coalesce, accompanied by a decrease in dislocation density, producing columnar grains along the build direction. Cuboidal γ′ precipitates approximately 500 nm in diameter were observed to form in the recrystallised grains, accompanied by larger γ′ precipitates on the grain boundaries.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Evolution of microstructure and grain boundary character distribution of a tin bronze annealed at different temperatures

Specimens cut from a rolled tin bronze sheet were annealed at 400–800 °C for 1 h and evolution of their microstructures was then characterized in details by electron channeling contrast imaging and electron backscatter diffraction techniques. Particularly, statistics on special boundaries (SBs) with Σ ≤ 29 and network connectivity of random high angle boundaries (HABs) in the annealed specimens were examined to probe optimization potentials of grain boundary character distribution (GBCD) for this material. Results show that the deformed microstructure in the as-received material begins to be recrystallized when the annealing temperature increase to 500 °C and average grain sizes surge with further increasing temperatures. As a result of the recrystallization, a large number of annealing twins (with Σ3 misorientation) are produced, leading to remarkably increased fractions of SBs (f{sub SBs}). Thanks to preexisting dense low angle boundaries, the majority of SBs in the 500 °C specimen with only partial recrystallization are Σ3{sub ic} (incoherent) boundaries, which effectively disrupt connectivity of random HABs network. Although the f{sub SBs} can be further increased (up to 72.5%) in specimens with full recrystallization (at higher temperatures), the Σ3{sub ic} boundaries would be replaced to some extent by Σ3{sub c} (coherent) boundaries which do not contribute directly to optimizing the GBCD. This work should be able to provide clear suggestions on applying the concept of grain boundary engineering to tin bronze alloys. - Highlights: • The rolled tin bronze begins to be recrystallized as temperature increases to 500 °C. • A lot of SBs are produced after recrystallization and the highest f{sub SBs} is 72.5%. • Partially recrystallized specimen has the optimum GBCD due to more Σ3{sub ic} boundaries. • The Σ3{sub ic} boundaries are replaced by Σ3{sub c} boundaries after full recrystallization.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Elucidating microstructure of spinodal copper alloy through annealing

Improvement in the characteristics of a polycrystalline material is done through engineering of microstructures. Spinodal decomposed copper alloy has been annealed at high temperature with systematic variation in time on multiple specimens. Extensive electron backscatter diffraction experiment was carried out to understand the grain boundary characteristics and morphologies of the alloy as a function of annealing time. The logical variation of annealing time strongly influences diffusion induced grain characteristics such as, shape, size, geometry, inclination, density, types, distribution, misorientations and the nature of subsequently induced twinning morphologies. - Highlights: •Spinodal copper alloy is annealed at high temperature by systematic time variation. •EBSD measurements are performed to quantify grain geometries and morphologies. •Annealing time has a strong influence on grain morphologies, twins and misorientations. •Grain morphologies and geometries are correlated with hardness data. •Elucidating microstructure development through grain boundary engineering.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructure characterization of 316L deformed at high strain rates using EBSD

Specimens from split Hopkinson pressure bar experiments, at strain rates between ~ 1000–9000 s{sup −1} at room temperature and 500 °C, have been studied using electron backscatter diffraction. No significant differences in the microstructures were observed at different strain rates, but were observed for different strains and temperatures. Size distribution for subgrains with boundary misorientations > 2° can be described as a bimodal lognormal area distribution. The distributions were found to change due to deformation. Part of the distribution describing the large subgrains decreased while the distribution for the small subgrains increased. This is in accordance with deformation being heterogeneous and successively spreading into the undeformed part of individual grains. The variation of the average size for the small subgrain distribution varies with strain but not with strain rate in the tested interval. The mean free distance for dislocation slip, interpreted here as the average size of the distribution of small subgrains, displays a variation with plastic strain which is in accordance with the different stages in the stress-strain curves. The rate of deformation hardening in the linear hardening range is accurately calculated using the variation of the small subgrain size with strain. - Highlights: •Only changes in strain, not strain rate, gave differences in the microstructure. •A bimodal lognormal size distribution was found to describe the size distribution. •Variation of the subgrain fraction sizes agrees with models for heterogeneous slip. •Variation of subgrain size with strain describes part of the stress strain curve.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructure evolution and dynamic recrystallization behavior of a powder metallurgy Ti-22Al-25Nb alloy during hot compression

The flow behavior of a powder metallurgy (P/M) Ti-22Al-25Nb alloy during hot compression tests has been investigated at a strain rate of 0.01 s{sup −1} and a temperature range of 980–1100 °C up to various true strains from 0.1 to 0.9. The effects of deformation temperature and strain on microstructure characterization and nucleation mechanisms of dynamic recrystallization (DRX) were assessed by means of Optical microscope (OM), electron backscatter diffraction (EBSD) and transmission electron microscope (TEM) techniques, respectively. The results indicated that the process of DRX was promoted by increasing deformation temperature and strain. By regression analysis, a power exponent relationship between peak stresses and sizes of stable DRX grains was developed. In addition, it is suggested that the discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX) controlled nucleation mechanisms for DRX grains operated simultaneously during the whole hot process, and which played the leading role varied with hot process parameters of temperature and strain. It was further demonstrated that the CDRX featured by progressive subgrain rotation was weakened by elevating deformation temperatures. - Highlights: •Flow behavior of a P/M Ti-22Al-25Nb is studied by hot compression tests. •Microstructure evolution of alloy is affected by deformation temperature and strain. •The relationship between peak stress and stable DRX grain size was developed. •The process of DRX was promoted by increasing deformation temperature and strain. •Nucleation mechanisms of DRX were identified by EBSD analysis and TEM observation.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Experimental study of microstructure changes due to low cycle fatigue of a steel nanocrystallised by Surface Mechanical Attrition Treatment (SMAT)

Electron Backscatter Diffraction technique is used to characterize the microstructure of 316L steel generated by Surface Mechanical Attrition Treatment (SMAT) before and after low cycle fatigue tests. A grain size gradient is generated from the top surface to the interior of the samples after SMAT so that three main regions can be distinguished below the treated surface: (i) the ultra-fine grain area within 5 μm under the top surface with preferably oriented grains, (ii) the intermediate area where the original grains are partially transformed, and (iii) the edge periphery area where the original grains are just mechanically deformed with the presence of plastic slips. Fatigue tests show that cyclic loading does not change the grain orientation spread and does not activate any plastic slip in the ultra-fine grain top surface area induced by SMAT. On the opposite, in the plastically SMAT affected region including the intermediate area and the edge periphery area, new slip systems are activated by low cycle fatigue while the grain orientation spread is increased. These results represent a first very interesting step towards the characterization and understanding of mechanical mechanisms involved during the fatigue of a grain size gradient material. - Highlights: •LCF tests are carried out on specimens processed by SMAT. •EBSD is used to investigate microstructural changes induced by LCF. •A grain size gradient is generated by SMAT from surface to the bulk of the fatigue samples. •New slip systems are activated by LCF and GOS is increased in plastically deformed region. •However, these phenomena are not observed in the top surface ultra-fine grain area.

36 MATERIALS SCIENCE↗