arXiv subjects

Reinhard Pippan

Publications and source records attributed to Reinhard Pippan.

At least 19 recordsLinked to original sources

arXiv2023

Synthesis of hard magnetic α-MnBi phase by high pressure torsion and field assisted annealing

Bulk composites using powder blends of Mn and Bi with equal atomic ratios are consolidated and severely deformed by high-pressure torsion (HPT). Subsequent annealing treatments lead to the formation of the ferromagnetic and rare-earth free hard magnetic α-MnBi phase. The initial phase formation is studied by in-situ high-energy XRD annealing experiments showing a beneficial influence of HPT-deformation on the amount of α-MnBi. The nucleation sites are strongly increased, thus the volumetric α-MnBi phase content exceeds 50 vol.%. A lower HPT-pressure of 2 GPa is found to be preferred over 5 GPa to obtain high α-MnBi contents. Annealing is done with or without applying an external magnetic field. Additionally, influences of the HPT-induced shear deformation are discussed and correlated with preferred diffusion path ways fostering the formation of anisotropic α-MnBi phase.

cond-mat.mtrl-sci↗

arXiv2023

Deformation-induced homogenization of the multi-phase senary high-entropy alloy MoNbTaTiVZr processed by high-pressure torsion

Dendritic microstructures are frequently observed in as-solidified refractory high-entropy alloys (RHEAs), and their homogenization typically requires a long-term heat treatment at extremely high temperatures. High-pressure torsion (HPT) has been shown to be capable of mixing immiscible systems at room temperature, and therefore represents a promising technique for homogenizing dendritic RHEAs. In this work, the as-solidified RHEA MoNbTaTiVZr was processed up to 40 revolutions by HPT. It was found that the dendritic microstructure was eliminated, resulting in a chemical homogeneity at a von Mises equivalent shear strain of about 400. The study of deformation mechanism showed an initial strain localization, followed by a co-deformation of the dendritic and interdendritic regions. In the co-deformation step, the Zr-rich interdendritic region gradually disappeared. The deformation-induced mixing also led to the formation of an ultra-fine grained (UFG) microstructure, exhibiting a grain size of approximately 50 nm. The microhardness increased from 500 HV in the as-solidified to 675 HV in the homogenized UFG state. The underlying mechanisms responsible for the microhardness enhancement, such as grain refinement and solid solution strengthening, were also discussed.

cond-mat.mtrl-sci↗

arXiv2022

Manufacturing of Textured Bulk Fe-SmCo$_{5}$ 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-SmCo$_{5}$ 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-SmCo$_{5}$ 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.

cond-mat.mtrl-sci↗

arXiv2022

Oxide-stabilized microstructure of severe plastically deformed CuCo alloys

Nanocrystalline materials are well known for their beneficial mechanical and physical properties. However, it is of utmost importance to stabilize the microstructure at elevated temperatures to broaden the window of application e.g. by pinning grain boundaries through impurities or oxides. CuCo alloys, severe plastically deformed using high-pressure torsion, were used to investigate the evolution of oxides upon annealing. These investigations were performed using electron microscopy, synchrotron high-energy X-ray scattering and atom probe tomography. Monitoring the evolution of oxides by in-situ small angle scattering investigations indicates the growth of primary oxides as well as the formation of another species of oxide at elevated temperatures. Slightly different coarsening can be observed in heat-treated samples, which can be traced back to the influence of different oxide amounts. The initially supersaturated CuCo matrix changes by the decomposition process as well as Co- and Cu-based oxides formation and growth. It has been found that the major number of oxides which are present after annealing, can already be found in the starting materials.

cond-mat.mtrl-sci↗

arXiv2022

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 for a wire of 24 um 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.

cond-mat.mtrl-sci↗

arXiv2021

Nanocrystalline FeCr alloys synthesised by severe plastic deformation -- a potential material for exchange bias and enhanced magnetostriction

This work gives insights into processing and characterisation of bulk nanocrystalline FeCr materials. The investigated FeCr alloys, consisting of 30, 50 and 70 at.% ferromagnetic Fe and remaining anti-ferromagnetic Cr, are processed by arc melting and subsequent severe plastic deformation by high pressure torsion. The physical similarities between elemental Fe and Cr in combination with the nanocrystalline structure of the as-deformed alloys, necessitates advanced characterisation techniques for the as-deformed state: In-situ annealing synchrotron X-ray diffraction measurements as well as electron microscopy experiments are linked to magnetostrictive measurements and reveal a single phase microstructure. Surprisingly, the nanocrystalline FeCr alloys remain supersaturated solid solutions upon annealing above 500°C, meaning a decomposition in a FeCr nanocomposite is suppressed. For the chosen annealing conditions grain growth is faster than decomposition and enhanced magnetostrictive values are found compared to materials in the as-deformed state.

cond-mat.mtrl-sci↗

arXiv2021

Sampling the Cu-Fe-Co phase diagram by severe plastic deformation for enhanced soft magnetic properties

Initial powder mixtures of Cu, Fe and Co are exposed to severe plastic deformation by high-pressure torsion to prepare solid solutions. A broad range of compositions is investigated, whereas this study aims at the synthesis of soft magnetic materials and therefore at the formation of a homogeneous and nanocrystalline microstructure. For intermediate ferromagnetic contents, high-pressure torsion at room temperature yields single-phase supersaturated solid solutions. For higher ferromagnetic contents, two consecutive steps of high-pressure torsion deformation at different temperatures yield the desired nanocrystalline microstructure. Depending on the Co-to-Fe-ratio, either a single-phase supersaturated solid solution or a nanocomposite forms. The composite exhibits an enhanced magnetic moment, indicating the formation of a (Fe,Co)-alloy upon severe plastic deformation. Soft magnetic properties are verified for large Co-to-Fe-ratios and this microstructure is found to remain stable up to 400 °C.

cond-mat.mtrl-sci↗

arXiv2021

Spinodal decomposition stabilizes plastic flow in a nanocrystalline Cu-Ti alloy

A combination of high strength and reasonable ductility has been achieved in a copper-1.7 at.%titanium alloy deformed by high-pressure torsion. Grain refinement and a spinodal microstructure provided a hardness of 254 +/- 2 HV , yield strength of 800 MPa and elongation of 10%. The spinodal structure persisted during isothermal ageing, further increasing the yield strength to 890MPa while retaining an elongation of 7%. This work demonstrates the potential for spinodal microstructures to overcome the difficulties in retaining ductility in ultra-fine grained or nanocrystalline alloys, especially upon post-deformation heating where strain softening normally results in brittle behavior.

cond-mat.mtrl-sci↗

arXiv2021

On the magnetic nanostructure of a Co-Cu alloy processed by high-pressure torsion

In this study, a preparation route of Co-Cu alloys with soft magnetic properties by high-pressure torsion deformation is introduced. Nanocrystalline, supersaturated single-phase microstructures are obtained after deformation of Co-Cu alloys, which are prepared from an initial powder mixture with Co-contents above 70 wt.%. Isochronal annealing treatments up to 400°C further reveal a remarkable microstructural stability. Only at 600°C, the supersaturated phase decomposes into two fcc-phases. The coercivity, measured by SQUID as a function of annealing temperature, remains significantly below the value for bulk-Co in all states investigated. In order to understand the measured magnetic properties in detail, a quantitative analysis of the magnetic microstructure is carried out by magnetic force microscopy and correlated to the observed changes in coercivity. Our results show that the rising coercivity can be explained by a magnetic hardening effect occurring in context with spinodal decomposition.

cond-mat.mtrl-sci↗

arXiv2021

Strain Induced Anisotropic Magnetic Behaviour and Exchange Coupling Effect in Fe-SmCo$_{5}$ Permanent Magnets Generated by High Pressure Torsion

High-pressure torsion (HPT), a technique of severe plastic deformation (SPD), is shown as a promising processing method for exchange-spring magnetic materials in bulk form. Powder mixtures of Fe and SmCo$_{5}$ are consolidated and deformed by HPT exhibiting sample dimensions of several millimetres, being essential for bulky magnetic applications. The structural evolution during HPT deformation of Fe-SmCo$_{5}$ compounds at room- and elevated- temperatures of chemical compositions consisting of 87, 47, 24 and 10 wt.% Fe is studied and microstructurally analysed. Electron microscopy and synchrotron X-ray diffraction reveal a dual-phase nanostructured composite for the as-deformed samples with grain refinement after HPT deformation. SQUID magnetometry measurements show hysteresis curves of an exchange coupled nanocomposite at room temperature, while for low temperatures a decoupling of Fe and SmCo$_{5}$ is observed. Furthermore, exchange interactions between the hard- and soft-magnetic phase can explain a shift of the hysteresis curve. Strong emphasis is devoted to the correlation between the magnetic properties and the evolving nano-structure during HPT deformation, which is conducted for a 1:1 composition ratio of Fe to SmCo$_{5}$. SQUID magnetometry measurements show an increasing saturation magnetisation for increasing strain $γ$ and a maximum of the coercive field strength at a shear strain of $γ$ = 75.

cond-mat.mtrl-sci↗

arXiv2021

In situ AC-hysteresis measurements of SPD-processed Cu20(Fe15Co85)80

The changes of magnetic properties upon heat treatment of a metastable supersaturated solid solution processed by severe plastic deformation are investigated by in-situ AC-hysteresis measurements. Data are analyzed in the framework of dynamic loss theory, with correlative investigations of the microstructural properties. The evolution of hysteresis upon annealing points out that the single-phase supersaturated solid solution remains stable up to 400°C, then hindering of domain wall motion sets in at this temperature. At 600°C, a multi phase microstructure is present, causing a significant increase in coercivity.

cond-mat.mtrl-sci↗

arXiv2021

Processing of nanostructured bulk Fe-Cr alloys by severe plastic deformation

The processing of binary alloys consisting of ferromagnetic Fe and antiferromagnetic Cr by severe plastic deformation (SPD) with different chemical compositions has been investigated. Although the phase diagram exhibits a large gap in the thermodynamical equilibrium at lower temperatures, it is shown that techniques based on SPD help to overcome common processing limits. Different processing routes including initial ball milling (BM) and arc melting (AM) and a concatenation with annealing treatments prior to high-pressure torsion (HPT) deformation are compared in this work. Investigation of the deformed microstructures by electron microscopy and synchrotron X-ray diffraction reveal homogeneous, nanocrystalline microstructures for HPT deformed AM alloys. HPT deformation of powder blends and BM powders leads to an exorbitant increase in hardness or an unusual fast formation of a $σ$-phase and therefore impede successful processing.

cond-mat.mtrl-sci↗

arXiv2020

Effect of Carbon in Severe Plastically Deformed Metals

In the last decades severe plastic deformation techniques have gained increasing interest as they allow the production of bulk nanostructured materials with superior mechanical and functional properties. However, because of mechanically induced grain boundary migration, the achievable grain size reduction is not indefinite but tends to stagnate once sufficient strain has been applied. Consequently, addition of solute elements or second phase particles offers the possibility to access the true nanocrystalline regime. Due to their low solubility and high mobility, interstitial elements are extremely effective at subduing boundary migration. Herein the effect of carbon on grain refinement and the resulting mechanical properties are summarized. As carbon may not only be added as graphite but could also be introduced in other forms or as allotropes such as nanotubes, nanodiamonds, or carbides, the respective advantages and problems associated with it are the center of discussion. Independent of the strategy used, strength levels hardly achievable with other alloying elements can be obtained. Moreover, as carbon does not have a negative effect on grain boundary cohesion, despite the enormous strength levels even ductility and toughness can be widely maintained.

cond-mat.mtrl-sci↗

arXiv2020

Influence of Processing Parameters on the Mechanical Properties of HPT-Deformed Nickel Carbon Nanotube Composites

Nickel carbon nanotube composites with varying amounts of carbon nanotubes are deformed by high pressure torsion at different deformation temperatures to high strains, where no further refinement of the Nickel matrix microstructure is observed. Mean Nickel grain sizes increase with increasing HPT deformation temperature, while the size of the carbon nanotube agglomerates is significantly reduced. Additionally, the distribution of the agglomerates in the metal matrix becomes more homogenous. To investigate the mechanical performance of the HPT deformed composites, uniaxial tensile and compression tests are conducted. Depending on the HPT deformation temperature and the resulting microstructure, either brittle or ductile fracture occurs. Increased HPT deformation temperatures induce a decrease in the anisotropy of the mechanical properties, mainly caused by a shrinking of the carbon nanotube agglomerates. It is shown, that tuning the HPT deformation temperature is the key for optimizing both the microstructure and the mechanical performance.

cond-mat.mtrl-sci↗

arXiv2020

High-Pressure Torsion Deformation Induced Phase Transformations and Formations: New Material Combinations and Advanced Properties

Heavy plastic shear deformation at relatively low homologous temperatures is called high-pressure torsion (HPT) deformation, which is one method of severe plastic deformation (SPD). The aim of the paper is to give an overview of a new processing approach which permits the generation of innovative metastable materials and novel nanocomposites by HPT deformation. Starting materials can be either coarse-grained multi-phase alloys, a mixture of different elemental powders or any other combination of multiphase solid starting materials. After HPT processing, the achievable microstructures are similar to the ones generated by mechanical alloying. Nevertheless, one advantage of the HPT process is that bulk samples of the different types of metastable materials and nanocomposites are obtained directly during HPT deformation. It will be shown that different material combinations can be selected and materials with tailored properties, or in other words, materials designed for specific applications and the thus required properties, can be synthesized. Areas of application for these new materials range from hydrogen storage to materials resistant to harsh radiation environments.

cond-mat.mtrl-sci↗

arXiv2020

Intermixing of Fe and Cu on the atomic scale by high-pressure torsion as revealed by DC- and AC-SQUID susceptometry and atom probe tomography

The capability of high-pressure torsion on the preparation of supersaturated solid solutions, consisting of Cu-14Fe (wt.%), is studied. From microstructural investigations a steady state is obtained with nanocrystalline grains. The as-deformed state is analyzed with atom probe tomography, revealing an enhanced solubility and the presence of Fe-rich particles. The DC-hysteresis loop shows suppressed long range interactions in the as-deformed state and evolves towards a typical bulk hysteresis loop when annealed at 500°C. AC-susceptometry measurements of the as-deformed state reveal the presence of a superparamagnetic blocking peak, as well as a magnetic frustrated phase, whereas the transition of the latter follows the Almeida-Thouless line, coinciding with the microstructural investigations by atom probe tomography. AC-susceptometry shows that the frustrated state vanishes for annealing at 250°C.

cond-mat.mtrl-sci↗

arXiv2020

Magnetic dilution by severe plastic deformation

Mixtures of Fe and Cu powders are cold-compacted and subsequently deformed with severe plastic deformation by high-pressure torsion, leading to bulk samples. The dilution of Fe in the Cu matrix is investigated with SQUID-magnetometry, whereas the magnetic properties change as a function of Fe-content from a frustrated regime to a thermal activated behaviour. The magnetic properties are correlated with the microstructure, investigated by synchrotron X-ray diffraction and atom probe tomography. Annealing of the as-deformed states leads to demixing and grain growth, with the coercivity as a function of annealing temperature obeying the random anisotropy model. The presented results show that high-pressure torsion is a technique capable to affect the microstructure even on atomic length scales.

cond-mat.mtrl-sci↗

arXiv2020

Tuneable Magneto-Resistance by Severe Plastic Deformation

Bulk metallic samples were synthesized from different binary powder mixtures consisting of elemental Cu, Co, and Fe using severe plastic deformation. Small particles of the ferromagnetic phase originate in the conductive Cu phase, either by incomplete dissolution or by segregation phenomena during the deformation process. These small particles are known to give rise to granular giant magnetoresistance. Taking advantage of the simple production process, it is possible to perform a systematic study on the influence of processing parameters and material compositions on the magneto-resistance. Furthermore, it is feasible to tune the magnetoresistive behavior as a function of the specimens chemical composition. It was found that specimens of low ferromagnetic content show an almost isotropic drop in resistance in a magnetic field. With increasing ferromagnetic content, percolating ferromagnetic phases cause an anisotropy of the magnetoresistance. By changing the parameters of the high pressure torsion process, i.e., sample size, deformation temperature, and strain rate, it is possible to tailor the magnitude of giant magneto-resistance. A decrease in room temperature resistivity of approx. 3.5% was found for a bulk specimen containing an approximately equiatomic fraction of Co and Cu.

cond-mat.mtrl-sci↗