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.

Can Severe Plastic Deformation Tune Nanocrystallization in Fe-Based Metallic Glasses?

The effects of severe plastic deformation (SPD) by means of high-pressure torsion (HPT) on the structural properties of the two iron-based metallic glasses Fe73.9Cu1Nb3Si15.5B6.6 and Fe81.2Co4Si0.5B9.5P4Cu0.8 have been investigated and compared. While for Fe73.9Cu1Nb3Si15.5B6.6, HPT processing allows us to extend the known consolidation and deformation ranges, HPT processing of Fe81.2Co4Si0.5B9.5P4Cu0.8 for the first time ever achieves consolidation and deformation with a minimum number of cracks. Using numerous analyses such as X-ray diffraction, dynamic mechanical analyses, and differential scanning calorimetry, as well as optical and transmission electron microscopy, clearly reveals that Fe81.2Co4Si0.5B9.5P4Cu0.8 exhibits HPT-induced crystallization phenomena, while Fe73.9Cu1Nb3Si15.5B6.6 does not crystallize even at the highest HPT-deformation degrees applied. The reasons for these findings are discussed in terms of differences in the deformation energies expended, and the number and composition of the individual crystalline phases formed. The results appear promising for obtaining improved magnetic properties of glassy alloys without additional thermal treatment.

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.

Manufacturing of Textured Bulk Fe-SmCo5 Magnets by Severe Plastic Deformation.

Exchange-coupling between soft- and hard-magnetic phases plays an important role in the engineering of novel magnetic materials. To achieve exchange coupling, a two-phase microstructure is necessary. This interface effect is further enhanced if both phase dimensions are reduced to the nanometer scale. At the same time, it is challenging to obtain large sample dimensions. In this study, powder blends and ball-milled powder blends of Fe-SmCo5 are consolidated and are deformed by high-pressure torsion (HPT), as this technique allows us to produce bulk magnetic materials of reasonable sizes. Additionally, the effect of severe deformation by ball-milling and severe plastic deformation by HPT on exchange coupling in Fe-SmCo5 composites is investigated. Due to the applied shear deformation, it is possible to obtain a texture in both phases, resulting in an anisotropic magnetic behavior and an improved magnetic performance.

A Perspective to Control Laser-Induced Periodic Surface Structure Formation at Glancing-Incident Femtosecond Laser-Processed Surfaces.

The favorable combination of high material removal rate and low influence on the material beneath the ultra-short pulsed laser-processed surface are of particular advantage for sample preparation. This is especially true at the micrometer scale or for the pre-preparation for a subsequent focused ion beam milling process. Specific surface features, the laser-induced periodic surface structures, are generated on femtosecond laser-irradiated surfaces in most cases, which pose an issue for surface-sensitive mechanical testing or microstructural investigations. This work strives for an approach to enhance the surface quality of glancing-incident laser-processed surfaces on the model material copper with two distinctly different grain sizes. A new generalized perspective is presented, in which optimized parameter selection serves to counteract the formation of the laser-induced periodic surface structures, enabling, for example, grain orientation mapping directly on femtosecond laser processed surfaces. SUPPLEMENTARY INFORMATION: The online version contains supplementary material available at 10.1007/s11837-021-04963-w.

Microstructural Effects on the Interfacial Adhesion of Nanometer-Thick Cu Films on Glass Substrates: Implications for Microelectronic Devices.

Improving the interface stability for nanosized thin films on brittle substrates is crucial for technological applications such as microelectronics because the so-called brittle-ductile interfaces limit their overall reliability. By tuning the thin film properties, interface adhesion can be improved because of extrinsic toughening mechanisms during delamination. In this work, the influence of the film microstructure on interface adhesion was studied on a model brittle-ductile interface consisting of nanosized Cu films on brittle glass substrates. Therefore, 110 nm thin Cu films were deposited on glass substrates using magnetron sputtering. While film thickness, residual stresses, and texture of the Cu films were maintained comparable in the sputtering processes, the film microstructure was varied during deposition and via isothermal annealing, resulting in four different Cu films with bimodal grain size distributions. The interface adhesion of each Cu film was then determined using stressed Mo overlayers, which triggered Cu film delaminations in the shape of straight, spontaneous buckles. The mixed-mode adhesion energy for each film ranged from 2.35 J/m2 for the films with larger grains to 4.90 J/m2 for the films with the highest amount of nanosized grains. This surprising result could be clarified using an additional study of the buckles using focused ion beam cutting and quantification via confocal laser scanning microscopy to decouple and quantify the amount of elastic and plastic deformation stored in the buckled thin film. It could be shown that the films with smaller grains exhibit the possibility of absorbing a higher amount of energy during delamination, which explains their higher adhesion energy.

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.

Geometrical model for calculating the effect of surface morphology on total x-ray output of medical x-ray tubes.

PURPOSE: Correlation of characteristic surface appearance and surface roughness with measured air kerma (kinetic energy released in air) reduction of tungsten-rhenium (WRe) stationary anode surfaces. METHODS: A stationary anode test system was developed and used to alter nine initially ground sample surfaces through thermal cycling at high temperatures. A geometrical model based on high resolution surface data was implemented to correlate the measured reduction of the air kerma rate with the changing surface appearance of the samples. In addition to the nine thermally cycled samples, three samples received synthetic surface structuring to prove the applicability of the model to nonconventional surface alterations. Representative surface data and surface roughness values were acquired by laser scanning confocal microscopy. RESULTS: After thermal cycling in the stationary anode test system, the samples showed surface features comparable to rotating anodes after long-time operation. The established model enables the appearance of characteristic surface features like crack networks, pitting, and local melting to be linked to the local x-ray output at 100 kV tube voltage ,10° anode take off angle and 2 mm of added Al filtration. The results from the conducted air kerma measurements were compared to the predicted total x-ray output reduction from the geometrical model and show, on average, less than 10 % error within the 12 tested samples. In certain boundaries, the calculated surface roughness Ra showed a linear correlation with the measured air kerma reduction when samples were having comparable damaging characteristics and similar operation parameters. The orientation of the surface features had a strong impact on the measured air kerma rate which was shown by testing synthetically structured surfaces. CONCLUSIONS: The geometrical model used herein considers and describes the effect of individual surface features on the x-ray output. In close boundaries arithmetic surface roughness Ra was found to be a useful characteristic value on estimating the effect of surface damage on total x-ray output.

Hydrogen Trapping in bcc Iron.

Fundamental understanding of H localization in steel is an important step towards theoretical descriptions of hydrogen embrittlement mechanisms at the atomic level. In this paper, we investigate the interaction between atomic H and defects in ferromagnetic body-centered cubic (bcc) iron using density functional theory (DFT) calculations. Hydrogen trapping profiles in the bulk lattice, at vacancies, dislocations and grain boundaries (GBs) are calculated and used to evaluate the concentrations of H at these defects as a function of temperature. The results on H-trapping at GBs enable further investigating H-enhanced decohesion at GBs in Fe. A hierarchy map of trapping energies associated with the most common crystal lattice defects is presented and the most attractive H-trapping sites are identified.

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.

Magnetic Binary Supersaturated Solid Solutions Processed by Severe Plastic Deformation.

Samples consisting of one ferromagnetic and one diamagnetic component which are immiscible at the thermodynamic equilibrium (Co-Cu, Fe-Cu, Fe-Ag) are processed by high-pressure torsion at various compositions. The received microstructures are investigated by electron microscopy and synchrotron X-ray diffraction, showing a microstructural saturation. Results gained from microstructural investigations are correlated to magnetometry data. The Co-Cu samples show mainly ferromagnetic behavior and a decrease in coercivity with increasing Co-content. The saturation microstructure of Fe-Cu samples is found to be dual phase. Results of magnetic measurements also revealed the occurrence of two different magnetic phases in this system. For Fe-Ag, the microstructural and magnetic results indicate that no intermixing between the elemental phases takes place.

In situ atomic-scale observation of oxidation and decomposition processes in nanocrystalline alloys.

Oxygen contamination is a problem which inevitably occurs during severe plastic deformation of metallic powders by exposure to air. Although this contamination can change the morphology and properties of the consolidated materials, there is a lack of detailed information about the behavior of oxygen in nanocrystalline alloys. In this study, aberration-corrected high-resolution transmission electron microscopy and associated techniques are used to investigate the behavior of oxygen during in situ heating of highly strained Cu-Fe alloys. Contrary to expectations, oxide formation occurs prior to the decomposition of the metastable Cu-Fe solid solution. This oxide formation commences at relatively low temperatures, generating nanosized clusters of firstly CuO and later Fe2O3. The orientation relationship between these clusters and the matrix differs from that observed in conventional steels. These findings provide a direct observation of oxide formation in single-phase Cu-Fe composites and offer a pathway for the design of nanocrystalline materials strengthened by oxide dispersions.

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.

From powders to bulk metallic glass composites.

One way to adjust the properties of materials is by changing its microstructure. This concept is not easily applicable on bulk metallic glasses (BMGs), because they do not consist of grains or different phases and so their microstructure is very homogeneous. One obvious way to integrate inhomogeneities is to produce bulk metallic glass composites (BMGCs). Here we show how to generate BMGCs via high-pressure torsion (HPT) starting from powders (amorphous Zr-MG and crystalline Cu). Using this approach, the composition can be varied and by changing the applied shear strains, the refinement of the microstructure is adjustable. This process permits to produce amorphous/crystalline composites where the scale of the phases can be varied from the micro- to the nanometer regime. Even mixing of the two phases and the generation of new metallic glasses can be achieved. The refinement of microstructure increases the hardness and a hardness higher than the initial BMG can be obtained.

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.

On nanostructured molybdenum-copper composites produced by high-pressure torsion.

Nanostructured molybdenum-copper composites have been produced through severe plastic deformation of liquid-metal infiltrated Cu30Mo70 and Cu50Mo50 (wt%) starting materials. Processing was carried out using high-pressure torsion at room temperature with no subsequent sintering treatment, producing a porosity-free, ultrafine-grained composite. Extensive deformation of the Cu50Mo50 composite via two-step high-pressure torsion produced equiaxed nanoscale grains of Mo and Cu with a grain size of 10-15 nm. Identical treatment of Cu30Mo70 produced a ultrafine, lamellar structure, comprised of Cu and Mo layers with thicknesses of ∼ 5 and ∼ 10 - 20 nm , respectively, and an interlamellar spacing of 9 nm. This microstructure differs substantially from that of HPT-deformed Cu-Cr and Cu-W composites, in which the lamellar microstructure breaks down at high strains. The ultrafine-grained structure and absence of porosity resulted in composites with Vickers hardness values of 600 for Cu30Mo70 and 475 for Cu50Mo50. The ability to produce Cu30Mo70 nanocomposites with a combination of high-strength, and a fine, oriented microstructure should be of interest for thermoelectric applications.

Thermally Activated Deformation Behavior of ufg-Au: Environmental Issues During Long-Term and High-Temperature Nanoindentation Testing.

For testing time-dependent material properties by nanoindentation, in particular for long-term creep or relaxation experiments, thermal drift influences on the displacement signal are of prime concern. To address this at room and elevated temperatures, we tested fused quartz at various contact depths at room temperature and ultra-fine grained (ufg) Au at various temperatures. We found that the raw data for fused quartz are strongly affected by thermal drift, but corrected by use of dynamic stiffness measurements all the datasets collapse. The situation for the ufg Au shows again that the data are only useful with drift correction, but with this applied it turns out that there is a significant change of elastic and plastic properties when exceeding 200°C, which is also reflected by an increasing strain rate sensitivity.

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.

The effect of high pressure torsion on structural refinement and mechanical properties of an austenitic stainless steel.

In the present study, the high pressure torsion (HPT) was used to refine the grain structure down to the nanometer scale in an austenitic stainless steel. The principles of HPT lay on torsional deformation under simultaneous high pressure of the specimen, which results in substantial reduction in the grain size. Disks of the 316LVM austenitic stainless steel of 10 mm in diameter were subjected to equivalent strains epsilon of 32 at RT and 450 degrees C under the pressure of 4 GPa. Furthermore, two-stage HPT processes, i.e., deformation at room temperature followed by deformation at 450 degrees C, were performed. The resulting microstructures were investigated in TEM observations. The mechanical properties were measured in terms of the microhardness and in tensile tests. HPT performed at two-stage conditions (firstly at RT next at 450 degrees C) gives similar values of microhardness to the ones obtained after deforming only at 450 degrees C but performed to higher values of the overall equivalent strain epsilon. The effect of high pressure torsion on structural refinement and mechanical properties of an austenitic stainless steel was evaluated.