Publications
440 results found
Tan Q, Yan Z, Li R, et al., 2022, <i>In</i>-<i>situ</i> synchrotron-based high energy X-ray diffraction study of the deformation mechanism of δ-hydrides in a commercially pure titanium, SCRIPTA MATERIALIA, Vol: 213, ISSN: 1359-6462
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- Citations: 4
da Silva AK, Souza Filho IR, Lu W, et al., 2022, A sustainable ultra-high strength Fe18Mn3Ti maraging steel through controlled solute segregation and alpha-Mn nanoprecipitation, Nature Communications, Vol: 13, Pages: 1-8, ISSN: 2041-1723
The enormous magnitude of 2 billion tons of alloys produced per year demands a change in design philosophy to make materials environmentally, economically, and socially more sustainable. This disqualifies the use of critical elements that are rare or have questionable origin. Amongst the major alloy strengthening mechanisms, a high-dispersion of second-phase precipitates with sizes in the nanometre range is particularly effective for achieving ultra-high strength. Here, we propose an alternative segregation-based strategy for sustainable steels, free of critical elements, which are rendered ultrastrong by second-phase nano-precipitation. We increase the Mn-content in a supersaturated, metastable Fe-Mn solid solution to trigger compositional fluctuations and nano-segregation in the bulk. These fluctuations act as precursors for the nucleation of an unexpected α-Mn phase, which impedes dislocation motion, thus enabling precipitation strengthening. Our steel outperforms most common commercial alloys, yet it is free of critical elements, making it a new platform for sustainable alloy design.
Joseph S, Kontis P, Chang Y, et al., 2022, A cracking oxygen story: a new view of stress corrosion cracking in titanium alloys, Acta Materialia, Vol: 227, Pages: 117687-117687, ISSN: 1359-6454
Titanium alloys can suffer from halide-associated stress corrosion cracking at elevated temperatures e.g., in jet engines, where chlorides and Ti-oxide promote the cracking of water vapour in the gas stream, depositing embrittling species at the crack tip. Here we report, using isotopically-labelled experiments, that crack tips in an industrial Ti-6Al-2Sn-4Zr-6Mo alloy are strongly enriched (>5 at.%) in oxygen from the water vapour, far greater than the amounts (0.25 at.%) required to embrittle the material. Surprisingly, relatively little hydrogen (deuterium) is measured, despite careful preparation and analysis. Therefore, we suggest that a combined effect of O and H leads to cracking, with O playing a vital role, since it is well-known to cause embrittlement of the alloy. In contrast it appears that in α + β Ti alloys, it may be that H may drain away into the bulk owing to its high solubility in β-Ti, rather than being retained in the stress field of the crack tip. Therefore, whilst hydrides may form on the fracture surface, hydrogen ingress might not be the only plausible mechanism of embrittlement of the underlying matrix. This possibility challenges decades of understanding of stress-corrosion cracking as being related solely to the hydrogen enhanced localised plasticity (HELP) mechanism, which explains why H-doped Ti alloys are embrittled. This would change the perspective on stress corrosion embrittlement away from a focus purely on hydrogen to also consider the ingress of O originating from the water vapour, insights critical for designing corrosion resistant materials.
Poplawsky JD, Pillai R, Ren Q-Q, et al., 2022, Measuring oxygen solubility in Ni grains and boundaries after oxidation using atom probe tomography, SCRIPTA MATERIALIA, Vol: 210, ISSN: 1359-6462
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- Citations: 4
Kim S-H, Antonov S, Zhou X, et al., 2022, Atom probe analysis of electrode materials for Li-ion batteries: challenges and ways forward, Journal of Materials Chemistry A, Vol: 10, Pages: 4926-4935, ISSN: 2050-7488
The worldwide development of electric vehicles as well as large-scale or grid-scale energy storage to compensate for the intermittent nature of renewable energy generation has led to a surge of interest in battery technology. Understanding the factors controlling battery capacity and, critically, their degradation mechanisms to ensure long-term, sustainable and safe operation requires detailed knowledge of their microstructure and chemistry, and their evolution under operating conditions, on the nanoscale. Atom probe tomography (APT) provides compositional mapping of materials in three dimensions with sub-nanometre resolution, and is poised to play a key role in battery research. However, APT is underpinned by an intense electric field that can drive lithium migration, and many battery materials are reactive oxides, requiring careful handling and sample transfer. Here, we report on the analysis of both anode and cathode materials and show that electric-field driven migration can be suppressed by using shielding by embedding powder particles in a metallic matrix or by using a thin conducting surface layer. We demonstrate that for a typical cathode material, cryogenic specimen preparation and transport under ultra-high vacuum leads to major delithiation of the specimen during the analysis. In contrast, the transport of specimens through air enables the analysis of the material. Finally, we discuss the possible physical underpinnings and discuss ways forward to enable shielding from the electric field, which helps address the challenges inherent to the APT analysis of battery materials.
Liu C, Lu W, Xia W, et al., 2022, Massive interstitial solid solution alloys achieve near-theoretical strength, Nature Communications, Vol: 13, Pages: 1-9, ISSN: 2041-1723
Interstitials, e.g., C, N, and O, are attractive alloying elements as small atoms on interstitial sites create strong lattice distortions and hence substantially strengthen metals. However, brittle ceramics such as oxides and carbides usually form, instead of solid solutions, when the interstitial content exceeds a critical yet low value (e.g., 2 at.%). Here we introduce a class of massive interstitial solid solution (MISS) alloys by using a highly distorted substitutional host lattice, which enables solution of massive amounts of interstitials as an additional principal element class, without forming ceramic phases. For a TiNbZr-O-C-N MISS model system, the content of interstitial O reaches 12 at.%, with no oxides formed. The alloy reveals an ultrahigh compressive yield strength of 4.2 GPa, approaching the theoretical limit, and large deformability (65% strain) at ambient temperature, without localized shear deformation. The MISS concept thus offers a new avenue in the development of metallic materials with excellent mechanical properties.
Luo T, Mangelinck D, Serrano-Sanchez F, et al., 2022, Grain boundary in NbCo(Pt)Sn half-Heusler compounds: Segregation and solute drag on grain boundary migration, ACTA MATERIALIA, Vol: 226, ISSN: 1359-6454
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- Citations: 4
Zhou X, Wei Y, Kuehbach M, et al., 2022, Revealing in-plane grain boundary composition features through machine learning from atom probe tomography data, ACTA MATERIALIA, Vol: 226, ISSN: 1359-6454
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- Citations: 5
Zhao H, Chakraborty P, Ponge D, et al., 2022, Hydrogen trapping and embrittlement in high-strength Al alloys, Nature, Vol: 602, Pages: 437-441, ISSN: 0028-0836
Ever more stringent regulations on greenhouse gas emissions from transportation motivate efforts to revisit materials used for vehicles1. High-strength aluminium alloys often used in aircrafts could help reduce the weight of automobiles, but are susceptible to environmental degradation2,3. Hydrogen ‘embrittlement’ is often indicated as the main culprit4; however, the exact mechanisms underpinning failure are not precisely known: atomic-scale analysis of H inside an alloy remains a challenge, and this prevents deploying alloy design strategies to enhance the durability of the materials. Here we performed near-atomic-scale analysis of H trapped in second-phase particles and at grain boundaries in a high-strength 7xxx Al alloy. We used these observations to guide atomistic ab initio calculations, which show that the co-segregation of alloying elements and H favours grain boundary decohesion, and the strong partitioning of H into the second-phase particles removes solute H from the matrix, hence preventing H embrittlement. Our insights further advance the mechanistic understanding of H-assisted embrittlement in Al alloys, emphasizing the role of H traps in minimizing cracking and guiding new alloy design.
Peng Z, Meiners T, Lu Y, et al., 2022, Quantitative analysis of grain boundary diffusion, segregation and precipitation at a sub-nanometer scale, ACTA MATERIALIA, Vol: 225, ISSN: 1359-6454
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- Citations: 10
Khanchandani H, El-Zoka AA, Kim S-H, et al., 2022, Laser-equipped gas reaction chamber for probing environmentally sensitive materials at near atomic scale, PLoS One, Vol: 17, Pages: 1-19, ISSN: 1932-6203
Numerous metallurgical and materials science applications depend on quantitative atomic-scale characterizations of environmentally-sensitive materials and their transient states. Studying the effect upon materials subjected to thermochemical treatments in specific gaseous atmospheres is of central importance for specifically studying a material’s resistance to certain oxidative or hydrogen environments. It is also important for investigating catalytic materials, direct reduction of an oxide, particular surface science reactions or nanoparticle fabrication routes. This manuscript realizes such experimental protocols upon a thermochemical reaction chamber called the "Reacthub" and allows for transferring treated materials under cryogenic & ultrahigh vacuum (UHV) workflow conditions for characterisation by either atom probe or scanning Xe+/electron microscopies. Two examples are discussed in the present study. One protocol was in the deuterium gas charging (25 kPa D2 at 200°C) of a high-manganese twinning-induced-plasticity (TWIP) steel and characterization of the ingress and trapping of hydrogen at various features (grain boundaries in particular) in efforts to relate this to the steel’s hydrogen embrittlement susceptibility. Deuterium was successfully detected after gas charging but most contrast originated from the complex ion FeOD+ signal and the feature may be an artefact. The second example considered the direct deuterium reduction (5 kPa D2 at 700°C) of a single crystal wüstite (FeO) sample, demonstrating that under a standard thermochemical treatment causes rapid reduction upon the nanoscale. In each case, further studies are required for complete confidence about these phenomena, but these experiments successfully demonstrate that how an ex-situ thermochemical treatment can be realised that captures environmentally-sensitive transient states that can be analysed by atomic-scale by atom probe microscope.
Kim S-H, Yoo S-H, Chakraborty P, et al., 2022, Understanding alkali contamination in colloidal nanomaterials to unlock grain boundary impurity engineering, Journal of the American Chemical Society, Vol: 144, Pages: 987-994, ISSN: 0002-7863
Metal nanogels combine a large surface area, a high structural stability, and a high catalytic activity toward a variety of chemical reactions. Their performance is underpinned by the atomic-level distribution of their constituents, yet analyzing their subnanoscale structure and composition to guide property optimization remains extremely challenging. Here, we synthesized Pd nanogels using a conventional wet chemistry route, and a near-atomic-scale analysis reveals that impurities from the reactants (Na and K) are integrated into the grain boundaries of the poly crystalline gel, typically loci of high catalytic activity. We demonstrate that the level of impurities is controlled by the reaction condition. Based on ab initio calculations, we provide a detailed mechanism to explain how surface-bound impurities become trapped at grain boundaries that form as the particles coalesce during synthesis, possibly facilitating their decohesion. If controlled, impurity integration into grain boundaries may offer opportunities for designing new nanogels.
Gomell L, Haeger T, Roscher M, et al., 2022, Microstructure manipulation by laser-surface remelting of a full-Heusler compound to enhance thermoelectric properties, ACTA MATERIALIA, Vol: 223, ISSN: 1359-6454
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- Citations: 2
Prithiv TS, Kloenne Z, Li D, et al., 2022, Grain boundary segregation and its implications regarding the formation of the grain boundary α phase in the metastable ,B-Titanium Ti-5Al-5Mo-5V-3Cr alloy, SCRIPTA MATERIALIA, Vol: 207, ISSN: 1359-6462
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- Citations: 17
Varanasi RS, Lipinska-Chwalek M, Mayer J, et al., 2022, Mechanisms of austenite growth during intercritical annealing in medium manganese steels, SCRIPTA MATERIALIA, Vol: 206, ISSN: 1359-6462
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- Citations: 19
Yoo S-H, Kim S-H, Woods E, et al., 2022, Origins of the hydrogen signal in atom probe tomography: case studies of alkali and noble metals, NEW JOURNAL OF PHYSICS, Vol: 24, ISSN: 1367-2630
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- Citations: 9
Agrawal P, Karthikeyan S, Makineni SK, et al., 2022, Dynamic strain aging in the intermediate temperature regime of near-α titanium alloy, IMI 834: Experimental and modeling, ACTA MATERIALIA, Vol: 222, ISSN: 1359-6454
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- Citations: 8
Yoo S-H, Kim S-H, Woods E, et al., 2022, Origins of the hydrogen signal in atom probe tomography, New Journal of Physics, Vol: 24, ISSN: 1367-2630
Atom Probe Tomography (APT) analysis is being actively used to providenear-atomic-scale information on the composition of complex materials inthree-dimensions. In recent years, there has been a surge of interest in thetechnique to investigate the distribution of hydrogen in metals. However, thepresence of hydrogen in the analysis of almost all specimens from nearly allmaterial systems has caused numerous debates as to its origins and impact onthe quantitativeness of the measurement. It is often perceived that most Harises from residual gas ionization, therefore affecting primarily materialswith a relatively low evaporation field. In this work, we perform systematicinvestigations to identify the origin of H residuals in APT experiments bycombining density-functional theory (DFT) calculations and APT measurements onan alkali and a noble metal, namely Na and Pt, respectively. We report that noH residual is found in Na metal samples, but in Pt, which has a higherevaporation field, a relatively high signal of H is detected. These resultscontradict the hypothesis of the H signal being due to direct ionization ofresidual H$_2$ without much interaction with the specimen's surface. Based onDFT, we demonstrate that alkali metals are thermodynamically less likely to besubject to H contamination under APT-operating conditions compared totransition or noble metals. These insights indicate that the detected H-signalis not only from ionization of residual gaseous H$_2$ alone, but is stronglyinfluenced by material-specific physical properties. The origin of H residualsis elucidated by considering different conditions encountered during APTexperiments, specifically, specimen-preparation, transportation, andAPT-operating conditions by taking thermodynamic and kinetic aspects intoaccount.
Johny J, Prymak O, Kamp M, et al., 2022, Multidimensional thermally-induced transformation of nest-structured complex Au-Fe nanoalloys towards equilibrium, Nano Research, Vol: 15, Pages: 581-592, ISSN: 1998-0000
Bimetallic nanoparticles are often superior candidates for a wide range of technological and biomedical applications owing to their enhanced catalytic, optical, and magnetic properties, which are often better than their monometallic counterparts. Most of their properties strongly depend on their chemical composition, crystallographic structure, and phase distribution. However, little is known of how their crystal structure, on the nanoscale, transforms over time at elevated temperatures, even though this knowledge is highly relevant in case nanoparticles are used in, e.g., high-temperature catalysis. Au-Fe is a promising bimetallic system where the low-cost and magnetic Fe is combined with catalytically active and plasmonic Au. Here, we report on the in situ temporal evolution of the crystalline ordering in Au-Fe nanoparticles, obtained from a modern laser ablation in liquids synthesis. Our in-depth analysis, complemented by dedicated atomistic simulations, includes a detailed structural characterization by X-ray diffraction and transmission electron microscopy as well as atom probe tomography to reveal elemental distributions down to a single atom resolution. We show that the Au-Fe nanoparticles initially exhibit highly complex internal nested nanostructures with a wide range of compositions, phase distributions, and size-depended microstrains. The elevated temperature induces a diffusion-controlled recrystallization and phase merging, resulting in the formation of a single face-centered-cubic ultrastructure in contact with a body-centered cubic phase, which demonstrates the metastability of these structures. Uncovering these unique nanostructures with nested features could be highly attractive from a fundamental viewpoint as they could give further insights into the nanoparticle formation mechanism under non-equilibrium conditions. Furthermore, the in situ evaluation of the crystal structure changes upon heating is potentially relevant for high-temperature process
Raabe D, Han L, Fernando F, et al., 2021, A mechanically strong and ductile soft magnet with ultralow coercivity
<jats:title>Abstract</jats:title> <jats:p>Soft magnetic materials (SMMs) are indispensable components in electrified applications and sustainable energy supply, allowing permanent magnetic flux variations in response to high frequency changes of the applied magnetic field, at lowest possible energy loss1. The global trend towards electrification of transport, households and manufacturing leads to a massive increase in energy consumption due to hysteresis losses2. Therefore, minimizing coercivity, which scales the losses in SMMs, is crucial3. Yet, meeting this target alone is not enough: SMMs used for instance in vehicles and planes must withstand severe mechanical loads, i.e., the alloys need high strength and ductility4. This is a fundamental design challenge, as most methods that enhance strength introduce stress fields that can pin magnetic domains, thus increasing coercivity and hysteretic losses5. Here, we introduce a new approach to overcome this dilemma. We have designed a Fe-Co-Ni-Ta-Al multicomponent alloy with ferromagnetic matrix and paramagnetic coherent nanoparticles of well-controlled size (~91 nm) and high volume fraction (55%). They impede dislocation motion, enhancing strength and ductility. Yet, their small size, low coherency stress and small magnetostatic energy create an interaction volume below the magnetic domain wall width, leading to minimal domain wall pinning, thus maintaining the material’s soft magnetic properties. The new material exhibits an excellent combination of mechanical and magnetic properties outperforming other multicomponent alloys and conventional SMMs. It has a tensile strength of ~1336 MPa at 54% tensile elongation, an extremely low coercivity of ~78 A/m (<1 Oe) and a saturation magnetization of ~100 Am2/kg. The work opens new perspectives on developing magnetically soft and mechanically strong and ductile materials for the sustainable electrification of industry and society.</jats:
Rau JS, Balachandran S, Schneider R, et al., 2021, High diffusivity pathways govern massively enhanced oxidation during tribological sliding, ACTA MATERIALIA, Vol: 221, ISSN: 1359-6454
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- Citations: 10
Morgado FF, Katnagallu S, Freysoldt C, et al., 2021, Revealing atomic-scale vacancy-solute interaction in nickel (vol 203, 114036, 2021), SCRIPTA MATERIALIA, Vol: 205, ISSN: 1359-6462
Wu Y, Cao D, Yao Y, et al., 2021, Substantially enhanced plasticity of bulk metallic glasses by densifying local atomic packing, Nature Communications, Vol: 12, Pages: 1-9, ISSN: 2041-1723
Introducing regions of looser atomic packing in bulk metallic glasses (BMGs) was reported to facilitate plastic deformation, rendering BMGs more ductile at room temperature. Here, we present a different alloy design approach, namely, doping the nonmetallic elements to form densely packed motifs. The enhanced structural fluctuations in Ti-, Zr- and Cu-based BMG systems leads to improved strength and renders these solutes’ atomic neighborhoods more prone to plastic deformation at an increased critical stress. As a result, we simultaneously increased the compressive plasticity (from ∼8% to unfractured), strength (from ∼1725 to 1925 MPa) and toughness (from 87 ± 10 to 165 ± 15 MPa√m), as exemplarily demonstrated for the Zr20Cu20Hf20Ti20Ni20 BMG. Our study advances the understanding of the atomic-scale origin of structure-property relationships in amorphous solids and provides a new strategy for ductilizing BMG without sacrificing strength.
Ahmadian A, Scheiber D, Zhou X, et al., 2021, Aluminum depletion induced by co-segregation of carbon and boron in a bcc-iron grain boundary, Nature Communications, Vol: 12, Pages: 1-11, ISSN: 2041-1723
The local variation of grain boundary atomic structure and chemistry caused by segregation of impurities influences the macroscopic properties of polycrystalline materials. Here, the effect of co-segregation of carbon and boron on the depletion of aluminum at a Σ5 (3 1 0 )[0 0 1] tilt grain boundary in a α − Fe-4 at%Al bicrystal is studied by combining atomic resolution scanning transmission electron microscopy, atom probe tomography and density functional theory calculations. The atomic grain boundary structural units mostly resemble kite-type motifs and the structure appears disrupted by atomic scale defects. Atom probe tomography reveals that carbon and boron impurities are co-segregating to the grain boundary reaching levels of >1.5 at%, whereas aluminum is locally depleted by approx. 2 at.%. First-principles calculations indicate that carbon and boron exhibit the strongest segregation tendency and their repulsive interaction with aluminum promotes its depletion from the grain boundary. It is also predicted that substitutional segregation of boron atoms may contribute to local distortions of the kite-type structural units. These results suggest that the co-segregation and interaction of interstitial impurities with substitutional solutes strongly influences grain boundary composition and with this the properties of the interface.
Kuehbach M, Kasemer M, Gault B, et al., 2021, Open and strong-scaling tools for atom-probe crystallography: high-throughput methods for indexing crystal structure and orientation, Journal of Applied Crystallography, Vol: 54, Pages: 1490-1508, ISSN: 0021-8898
Volumetric crystal structure indexing and orientation mapping are key data processing steps for virtually any quantitative study of spatial correlations between the local chemical composition features and the microstructure of a material. For electron and X-ray diffraction methods it is possible to develop indexing tools which compare measured and analytically computed patterns to decode the structure and relative orientation within local regions of interest. Consequently, a number of numerically efficient and automated software tools exist to solve the above characterization tasks. For atom-probe tomography (APT) experiments, however, the strategy of making comparisons between measured and analytically computed patterns is less robust because many APT data sets contain substantial noise. Given that sufficiently general predictive models for such noise remain elusive, crystallography tools for APT face several limitations: their robustness to noise is limited, and therefore so too is their capability to identify and distinguish different crystal structures and orientations. In addition, the tools are sequential and demand substantial manual interaction. In combination, this makes robust uncertainty quantification with automated high-throughput studies of the latent crystallographic information a difficult task with APT data. To improve the situation, the existing methods are reviewed and how they link to the methods currently used by the electron and X-ray diffraction communities is discussed. As a result of this, some of the APT methods are modified to yield more robust descriptors of the atomic arrangement. Also reported is how this enables the development of an open-source software tool for strong scaling and automated identification of a crystal structure, and the mapping of crystal orientation in nanocrystalline APT data sets with multiple phases.
Morgado FF, Katnagallu S, Freysoldt C, et al., 2021, Revealing atomic-scale vacancy-solute interaction in nickel, SCRIPTA MATERIALIA, Vol: 203, ISSN: 1359-6462
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- Citations: 4
Liu C, Li Z, Lu W, et al., 2021, Reactive wear protection through strong and deformable oxide nanocomposite surfaces, Nature Communications, Vol: 12, Pages: 1-8, ISSN: 2041-1723
Wear-related energy and material loss cost over 2500 Billion Euro per year. Traditional wisdom suggests that high-strength materials reveal low wear rates, yet, their plastic deformation mechanisms also influence their wear performance. High strength and homogeneous deformation behavior, which allow accommodating plastic strain without cracking or localized brittle fracture, are crucial for developing wear-resistant metals. Here, we present an approach to achieve superior wear resistance via in-situ formation of a strong and deformable oxide nanocomposite surface during wear, by reaction of the metal surface with its oxidative environment, a principle that we refer to as ‘reactive wear protection’. We design a TiNbZr-Ag alloy that forms an amorphous-crystalline oxidic nanocomposite surface layer upon dry sliding. The strong (2.4 GPa yield strength) and deformable (homogeneous deformation to 20% strain) nanocomposite surface reduces the wear rate of the TiNbZr-Ag alloy by an order of magnitude. The reactive wear protection strategy offers a pathway for designing ultra-wear resistant alloys, where otherwise brittle oxides are turned to be strong and deformable for improving wear resistance.
Kovacs A, Lewis LH, Palanisamy D, et al., 2021, Discovery and implications of hidden atomic-scale structure in a metallic meteorite, Nano Letters: a journal dedicated to nanoscience and nanotechnology, Vol: 21, Pages: 8135-8142, ISSN: 1530-6984
Iron and its alloys have made modern civilization possible, with metallic meteorites providing one of the human’s earliest sources of usable iron as well as providing a window into our solar system’s billion-year history. Here highest-resolution tools reveal the existence of a previously hidden FeNi nanophase within the extremely slowly cooled metallic meteorite NWA 6259. This new nanophase exists alongside Ni-poor and Ni-rich nanoprecipitates within a matrix of tetrataenite, the uniaxial, chemically ordered form of FeNi. The ferromagnetic nature of the nanoprecipitates combined with the antiferromagnetic character of the FeNi nanophases gives rise to a complex magnetic state that evolves dramatically with temperature. These observations extend and possibly alter our understanding of celestial metallurgy, provide new knowledge concerning the archetypal Fe–Ni phase diagram and supply new information for the development of new types of sustainable, technologically critical high-energy magnets.
Liu C, Garner A, Zhao H, et al., 2021, CALPHAD-informed phase-field modeling of grain boundary microchemistry and precipitation in Al-Zn-Mg-Cu alloys, ACTA MATERIALIA, Vol: 214, ISSN: 1359-6454
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- Citations: 19
Ener S, Skokov KP, Palanisamy D, et al., 2021, Twins - A weak link in the magnetic hardening of ThMn<sub>12</sub>-type permanent magnets, ACTA MATERIALIA, Vol: 214, ISSN: 1359-6454
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- Citations: 24
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