Deformation Induced Structure and Property Changes in a Nanostructured Multiphase CrMnFeCoNi High-Entropy Alloy.

A nanocrystalline CrMnFeCoNi high-entropy alloy produced using severe plastic deformation using high-pressure torsion was annealed at selected temperatures and times (450 °C for 1 h and 15 h and at 600 °C for 1 h), causing a phase decomposition into a multi-phase structure. The samples were subsequently deformed again by high-pressure torsion to investigate the possibility of tailoring a favorable composite architecture by re-distributing, fragmenting, or partially dissolving the additional intermetallic phases. While the second phase in the 450 °C annealing states had high stability against mechanical mixing, a partial dissolution could be achieved in the samples subjected to 600 °C for 1 h.

Phase Transformation Induced by High Pressure Torsion in the High-Entropy Alloy CrMnFeCoNi.

The forward and reverse phase transformation from face-centered cubic (fcc) to hexagonal close-packed (hcp) in the equiatomic high-entropy alloy (HEA) CrMnFeCoNi has been investigated with diffraction of high-energy synchrotron radiation. The forward transformation has been induced by high pressure torsion at room and liquid nitrogen temperature by applying different hydrostatic pressures and large shear strains. The volume fraction of hcp phase has been determined by Rietveld analysis after pressure release and heating-up to room temperature as a function of hydrostatic pressure. It increases with pressure and decreasing temperature. Depending on temperature, a certain pressure is necessary to induce the phase transformation. In addition, the onset pressure depends on hydrostaticity; it is lowered by shear stresses. The reverse transformation evolves over a long period of time at ambient conditions due to the destabilization of the hcp phase. The effect of the phase transformation on the microstructure and texture development and corresponding microhardness of the HEA at room temperature is demonstrated. The phase transformation leads to an inhomogeneous microstructure, weakening of the shear texture, and a surprising hardness anomaly. Reasons for the hardness anomaly are discussed in detail.

Micro-mechanisms of failure in nano-structured maraging steels characterised throughin situmechanical tests.

High-pressure-torsion (HPT) processing introduces a large density of dislocations that form sub-grain boundaries within the refined nano-scale structure, leading to changes in precipitate morphology compared to hot-rolled maraging steels. The impact of such nanostructuring on the deformation and fracture micro-mechanisms is being reported for the first time usingin situcharacterization techniques along with transmission electron microscopy and atom probe tomography analysis, in this study. Digital image correlation has been used to quantify the full field strain maps in regions of severe strain localization as well as to determine the fracture toughness through critical crack tip opening displacements. It is seen that the phenomenon of planar slip leads to strain softening under uniaxial deformation and to crack branching under a triaxial stress state in hot rolled maraging steels. On the other hand, nano-structuring after HPT processing creates a large number of high angle grain boundaries as dislocation barriers, leading to strain hardening under uniaxial tension and nearly straight crack path with catastrophic fracture under triaxial stress state. Upon overaging, the hot-rolled sample shows signature of transformation induced plasticity under uniaxial tension, which is absent in the HPT processed overaged samples, owing to the finer reverted austenite grains containing higher Ni concentration in the latter. In the overaged fracture test samples of both the hot-rolled and HPT conditions, crack tips show a signature of strain induced transformation of the reverted austenite to martensite, due to the accompanying severe strain gradients. This leads to a higher fracture toughness even while achieving high strengths in the overaged conditions of the nanocrystalline HPT overaged samples. The results presented here will aid in design of suitable heat treatment or microstructure engineering of interface dominated nano-scale maraging steels with improved damage tolerance.

Soft Magnetic Properties of Ultra-Strong and Nanocrystalline Pearlitic Wires.

The paper describes the capability of magnetic softening of a coarse-grained bulk material by a severe deformation technique. Connecting the microstructure with magnetic properties, the coercive field decreases dramatically for grains smaller than the magnetic exchange length. This makes the investigation of soft magnetic properties of severely drawn pearlitic wires very interesting. With the help of the starting two-phase microstructure, it is possible to substantially refine the material, which allows the investigation of magnetic properties for nanocrystalline bulk material. Compared to the coarse-grained initial, pearlitic state, the coercivities of the highly deformed wires decrease while the saturation magnetization values increase-even beyond the value expectable from the individual constituents. The lowest coercivity in the drawn state is found to be 520 A m-1 for a wire of 24-µm thickness and an annealing treatment has a further positive effect on it. The decreasing coercivity is discussed in the framework of two opposing models: grain refinement on the one hand and dissolution of cementite on the other hand. Auxiliary measurements give a clear indication for the latter model, delivering a sufficient description of the observed evolution of magnetic properties.

Electron Irradiation Effects on Strength and Ductility of Polymer Foils Studied by Femtosecond Laser-Processed Micro-Tensile Specimens.

The influence of irradiation on mechanical properties of polymer foils used in spacecraft applications has widely been studied via macroscopic tensile samples. An increase in the local resolution of this investigation can be achieved by reducing the sample's dimensions. A femtosecond laser enables a fast fabrication of micro-samples with dimensions from tens of µ m to the mm range, with ideally no influence on the material. Tensile experiments using such micro-tensile samples were conducted on FEP, Upilex-S and PET foils. The influence of the laser processing on the polymer foils was evaluated. Additionally an investigation of degradation due to electron irradiation was performed. Furthermore an outlook to extend this technique to depth-resolved measurements by preparing samples from locally thinned foils is presented. The study demonstrates the feasibility of femtosecond laser processing for rapid fabrication of micro-samples, enabling insights into the effect of electron irradiation on local mechanical properties of polymers.

Optimizing mechanical properties of Fe26.7Co26.7Ni26.7Si8.9B11 high entropy alloy by inducing hypoeutectic to quasi-duplex microstructural transition.

High-entropy alloys (HEAs) have inspired considerable interest due to their attractive physical and mechanical properties. In this work, the microstructural evolution induced by different heat treatments on rapidly solidified hypoeutectic precursors of a Fe26.7Co26.7Ni26.7Si8.9B11 HEA is investigated and correlated with the corresponding mechanical properties. The microstructures of the rapidly solidified precursors are composed of primary fcc solid solution dendrites embedded in a eutectic matrix. When the samples are annealed at different temperatures after furnace cooling or quenching, respectively, the eutectic structure gradually decomposes into fcc, tetragonal (Fe,Co)2B, and hexagonal Ni31Si12 crystals with increasing annealing temperature, leading to a gradual increase of the content of the fcc crystals and both their aggregation and coarsening. Then the dominant structural framework gradually transforms from eutectic structures to fcc dendrites and ultimately the (Fe,Co)2B crystals become isolated as dominant reinforcement particles distributed in the interdendritic regions. This gradual microstructural transition from hypoeutectic to quasi-duplex structures leads to the change of the dominant deformation mechanism from crack-controlled to dislocation-dominated deformation, which allows to control both ductility and strength in a wide range. Hence, this study provides some guideline for how to tune the microstructure and mechanical properties of HEAs.

Influence of Annealing on Microstructure and Mechanical Properties of a Nanocrystalline CrCoNi Medium-Entropy Alloy.

An equiatomic CrCoNi medium-entropy alloy was subjected to high-pressure torsion. This process led to a refinement of the microstructure to a grain size of about 50 nm, combined with a strong increase in the materials hardness. Subsequently, the thermodynamic stability of the medium entropy alloy was evaluated by isothermal and isochronal heat treatments. Annealed samples were investigated by scanning and transmission electron microscopy as well as X-ray diffraction, and were subjected to tensile tests to establish microstructure-property relationships. Furthermore, a comparison of mechanical properties with a grade 316L stainless steel was performed in order to evaluate if the CrCoNi alloy is competitive with commercially available structural materials in the nanocrystalline state. A minority phase embedded in the face-centered cubic matrix of the CrCoNi alloy could be observed in multiple annealed states, as well as the as-received and high-pressure torsion processed material. For 200 h of annealing at 500 °C, it was determined that the minority phase has a hexagonal-closed-packed crystal structure. A possible explanation for the formation of the phase is a preferential segregation of Co to stacking faults.

Electrochemical and biocompatibility examinations of high-pressure torsion processed titanium and Ti-13Nb-13Zr alloy.

The purpose of this study was to estimate the electrochemical behavior and biocompatibility of ultrafine-grained (UFG) commercially pure titanium (CPTi) and Ti-13Nb-13Zr (TNZ) alloy obtained by high-pressure torsion process. Electrochemical behavior of materials in artificial saliva at 37°C was evaluated by potentiodynamic polarization tests and electrochemical impedance spectroscopy (EIS), and the obtained results indicated that UFG TNZ alloy showed corrosion current density (jcorr  = 53 ± 5 nA cm-2 ) which was 2 times lower compared to coarse-grained (CG) TNZ alloy (jcorr  = 110 ± 12 nA cm-2 ) and higher corrosion resistance, while UFG CPTi and CPTi showed approximately the same corrosion rate (mean jcorr ∼ 38-40 nA cm-2 ). Static immersion test in artificial saliva, performed in this study, showed that the released ion concentrations from UFG materials were more than 10 times lower than the permitted concentration (the highest released Ti ion concentration from UFG CPTi and UFG TNZ alloy was 1.12 and 1.28 ppb, respectively, while permitted concentration was 15.5 ppb). The in vitro cytotoxicity tests, as the initial phase of the biocompatibility evaluation, showed that the fraction of surviving cells in all examined materials was much higher compared to the control sample and hence demonstrated absence of cytotoxicity and an increase of fibroblast cells adhesion on UFG materials surfaces. UFG CPTi and UFG TNZ alloy can be considered as promising materials for applications in dentistry due to high corrosion resistance and outstanding biocompatibility which were shown in this study. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 106B: 1097-1107, 2018.

Femtosecond laser machining for characterization of local mechanical properties of biomaterials: a case study on wood.

The standard preparation technique for micro-sized samples is focused ion beam milling, most frequently using Ga+ ions. The main drawbacks are the required processing time and the possibility and risks of ion implantation. In contrast, ultrashort pulsed laser ablation can process any type of material with ideally negligible damage to the surrounding volume and provides 4 to 6 orders of magnitude higher ablation rates than the ion beam technique. In this work, a femtosecond laser was used to prepare wood samples from spruce for mechanical testing at the micrometre level. After optimization of the different laser parameters, tensile and compressive specimens were produced from microtomed radial-tangential and longitudinal-tangential sections. Additionally, laser-processed samples were exposed to an electron beam prior to testing to study possible beam damage. The specimens originating from these different preparation conditions were mechanically tested. Advantages and limitations of the femtosecond laser preparation technique and the deformation and fracture behaviour of the samples are discussed. The results prove that femtosecond laser processing is a fast and precise preparation technique, which enables the fabrication of pristine biological samples with dimensions at the microscale.

The effect of severe grain refinement on the damage tolerance of a superelastic NiTi shape memory alloy.

Nickel-titanium (NiTi) shape memory alloys are widely used for medical components, as they can accommodate large strains in their superelastic state. In order to further improve the mechanical properties of NiTi, grain refinement by severe plastic deformation is applied to generate an ultrafine-grained microstructure with increased strength. In this work comprehensive fracture and fatigue crack growth experiments were performed on ultrafine-grained NiTi to assess its damage tolerance, which is essential for the safe use of this material in medical applications. It was found, that equal channel angular pressing of NiTi for 8 passes route BC increases the transformation stress by a factor of 1.5 and the yield stress of the martensite by a factor of 2.6, without significantly deteriorating its fracture and fatigue crack growth behavior. The fatigue crack growth behavior at high mean stresses is even improved, with lower fatigue crack growth rates and higher threshold stress intensity factor ranges, however, beneficial contributions from crack closure are slightly reduced.

Exceptional damage-tolerance of a medium-entropy alloy CrCoNi at cryogenic temperatures.

High-entropy alloys are an intriguing new class of metallic materials that derive their properties from being multi-element systems that can crystallize as a single phase, despite containing high concentrations of five or more elements with different crystal structures. Here we examine an equiatomic medium-entropy alloy containing only three elements, CrCoNi, as a single-phase face-centred cubic solid solution, which displays strength-toughness properties that exceed those of all high-entropy alloys and most multi-phase alloys. At room temperature, the alloy shows tensile strengths of almost 1 GPa, failure strains of ∼70% and KJIc fracture-toughness values above 200 MPa m(1/2); at cryogenic temperatures strength, ductility and toughness of the CrCoNi alloy improve to strength levels above 1.3 GPa, failure strains up to 90% and KJIc values of 275 MPa m(1/2). Such properties appear to result from continuous steady strain hardening, which acts to suppress plastic instability, resulting from pronounced dislocation activity and deformation-induced nano-twinning.

A fracture-resistant high-entropy alloy for cryogenic applications.

High-entropy alloys are equiatomic, multi-element systems that can crystallize as a single phase, despite containing multiple elements with different crystal structures. A rationale for this is that the configurational entropy contribution to the total free energy in alloys with five or more major elements may stabilize the solid-solution state relative to multiphase microstructures. We examined a five-element high-entropy alloy, CrMnFeCoNi, which forms a single-phase face-centered cubic solid solution, and found it to have exceptional damage tolerance with tensile strengths above 1 GPa and fracture toughness values exceeding 200 MPa·m(1/2). Furthermore, its mechanical properties actually improve at cryogenic temperatures; we attribute this to a transition from planar-slip dislocation activity at room temperature to deformation by mechanical nanotwinning with decreasing temperature, which results in continuous steady strain hardening.

Grain boundary excess volume and defect annealing of copper after high-pressure torsion.

The release of excess volume upon recrystallization of ultrafine-grained Cu deformed by high-pressure torsion (HPT) was studied by means of the direct technique of high-precision difference dilatometry in combination with differential scanning calorimetry (DSC) and scanning electron microscopy. From the length change associated with the removal of grain boundaries in the wake of crystallite growth, a structural key quantity of grain boundaries, the grain boundary excess volume or expansion [Formula: see text] m was directly determined. The value is quite similar to that measured by dilatometry for grain boundaries in HPT-deformed Ni. Activation energies for crystallite growth of [Formula: see text] and [Formula: see text] are derived by Kissinger analysis from dilatometry and DSC data, respectively. In contrast to Ni, substantial length change proceeds in Cu at elevated temperatures beyond the regime of dominant crystallite growth. In the light of recent findings from tracer diffusion and permeation experiments, this is associated with the shrinkage of nanovoids at high temperatures.

Enhanced fatigue endurance of metallic glasses through a staircase-like fracture mechanism.

Bulk-metallic glasses (BMGs) are now candidate materials for structural applications due to their exceptional strength and toughness. However, their fatigue resistance can be poor and inconsistent, severely limiting their potential as reliable structural materials. As fatigue limits are invariably governed by the local arrest of microscopically small cracks at microstructural features, the lack of microstructure in monolithic glasses, often coupled with other factors, such as the ease of crack formation in shear bands or a high susceptibility to corrosion, can lead to low fatigue limits (some ~1/20 of their tensile strengths) and highly variable fatigue lives. BMG-matrix composites can provide a solution here as their duplex microstructures can arrest shear bands at a second phase to prevent cracks from exceeding critical size; under these conditions, fatigue limits become comparable with those of crystalline alloys. Here, we report on a Pd-based glass that similarly has high fatigue resistance but without a second phase. This monolithic glass displays high intrinsic toughness from extensive shear-band proliferation with cavitation and cracking effectively obstructed. We find that this property can further promote fatigue resistance through extrinsic crack-tip shielding, a mechanism well known in crystalline metals but not previously reported in BMGs, whereby cyclically loaded cracks propagate in a highly "zig-zag" manner, creating a rough "staircase-like" profile. The resulting crack-surface contact (roughness-induced crack closure) elevates fatigue properties to those comparable to crystalline alloys, and the accompanying plasticity helps to reduce flaw sensitivity in the glass, thereby promoting structural reliability.

Influence of grain shape and orientation on the mechanical properties of high pressure torsion deformed nickel.

Severely plastically deformed (SPD) materials, for example those produced by high pressure torsion (HPT), are reported to possess outstanding mechanical properties. A typical HPT microstructure consists of elongated grains, usually of grain size well below 1 µm, which are aligned parallel to the shear plane and showing typical shear texture components. To answer the question of how these single features of a SPD microstructure affect the mechanical properties individually, such as the yield strength, the ultimate tensile strength, the uniform elongation and the reduction in area, uniaxial tensile tests have been conducted. The samples were tested in two different orientations. Within the same testing orientation the average grain aspect ratio was also varied. The variation in grain aspect ratio within a sample was achieved through a slight back rotation of the already deformed material and selective radius-dependent specimen extraction. The main results are as follows: the ductility (in terms of the reduction in area) is influenced by the grain aspect ratio. In contrast, the ultimate tensile strength is independent of the grain aspect ratio but shows an explicit dependency on the specimen orientation.