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Inspired by steel forming strategies, this study focuses on the effect of differential cooling on mechanical properties and precipitation kinetics during hot stamping of high strength AA7075 alloy. For this aim, different forming strategies were performed using segmented and differentially heated forming tools to provide locally tailored microstructures. Upon processing, uniaxial tensile tests and hardness measurements were used to characterize the mechanical properties after the aging treatment. Microstructure investigations were conducted to examine the strengthening mechanisms using the electron channeling contrast imaging (ECCI) technique in a scanning electron microscope (SEM). Based on the obtained results, it can be deduced that the tool temperatures play a key role in influencing the mechanical properties. Lower tool temperatures result in higher material strength and higher tool temperatures in lower mechanical properties. By changing the cooling rate with the use of differently heated forming tools, the mechanical properties can be controlled. Microstructure investigations revealed the formation of very fine and homogeneously distributed particles at cooled zones, which were associated with elevated mechanical properties due to the suppression of second phase particle formation during cooling. In contrast, coarse particles were observed at lower cooling rates, explaining the lower material strength found in these zones.

Laser surface remelting can be used to manipulate the microstructure of cast material. Here, we present a detailed analysis of the microstructure of Fe$_2$VAl following laser surface remelting. Within the melt pool, elongated grains grow nearly epitaxially from the heat-affected zone. These grains are separated by low-angle grain boundaries with 1{\deg}-5{\deg} misorientations. Segregation of vanadium, carbon, and nitrogen at grain boundaries and dislocations is observed using atom probe tomography. The local electrical resistivity was measured by an in-situ four-point-probe technique. A smaller increase in electrical resistivity is observed at these low-angle grain boundaries compared to high-angle grain boundaries in a cast sample. This indicates that grain boundary engineering could potentially be used to manipulate thermoelectric properties.

Additive manufacturing processes, such as laser powder bed fusion, require steady powder processing but often exhibit poor flowability and low powder bed densities. Reducing the attractive Van-der-Waals force through nanoparticle coating can enhance initially poor flowability. We investigated the effect of dry-coating nanosized SiO2 on gas-atomized CoCrFeNi powders containing different amounts of particles

Grain refinement tendency of pure Fe and Fe-X (X=5~10at%Al, 2~10at%Ti) alloys produced by laser powder bed fusion (LPBF) process was investigated. Pure Fe, Al, and Ti powders were dry mixed and cubic samples were built from the mixtures. The microstructure analysis revealed that (1) the microstructure of pure Fe consisted of equiaxed grains having an average diameter of 1.7 μm with fine iron oxide particles. (2) Fe-5 and 10at%Al alloys showed coarse columnar grains. (3) Fe-2at%Ti shows a mixture of fine equiaxed and columnar shape grains. (4) the microstructures of Fe-5at%Ti and 10at%Ti alloys are fully equiaxed, and grain refinement tendency was confirmed with increasing Ti content. Ti(N,O) oxi-nitrides are efficient in reducing the grain size because of the low lattice misfit with the ferrite matrix. Additionally, the effectiveness of Ti(N,O) particles as grain refiners was confirmed by building samples using TiN powder mixed with Fe-10at%Al and Fe-2at%Ti. While these alloys alone are coarse grained, a dispersion of Ti(N,O) particles achieved a fine-grained microstructure.

In this work an unexplored method of utilization of gaseous nitriding of Fe-2.3 wt% Al alloy powders was employed to realize a dispersion of nanosized AlN particles in the ferritic matrix. The nitriding treatment was carried out at 580 °C in ammonia atmosphere and the resulting microstructures were characterized by employing light microscopy, scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction and hardness measurements. Nitriding treatment led to the transformation of entire powder particles to iron nitrides (γ'-Fe4N1-x and e-Fe3N1+y) and the surfaces of the particles had a layer of iron-oxides which developed during cooling after nitriding. Al originating from iron-oxide regions partitioned to the iron-oxide/iron-nitride interface and formed an Al-oxide layer. A following hydrogen reduction treatment of the nitrided powders at 600 °C reduced the nitrides and surface oxides of iron to ferrite, leaving Al-oxides and Al-nitrides within the ferrite matrix. A significant increase in hardness after nitriding suggests that this process constitutes a promising new route of producing nitride-dispersion-strengthened steels.

Laser additive manufacturing is attractive for the production of complex, three-dimensional parts from metallic powder using a computer-aided design model1–3. The approach enables the digital control of the processing parameters and thus the resulting alloy’s microstructure, for example, by using high cooling rates and cyclic re-heating4–10. We recently showed that this cyclic re-heating, the so-called intrinsic heat treatment, can trigger nickel-aluminium precipitation in an iron–nickel–aluminium alloy in situ during laser additive manufacturing9. Here we report a Fe19Ni5Ti (weight per cent) steel tailor-designed for laser additive manufacturing. This steel is hardened in situ by nickel-titanium nanoprecipitation, and martensite is also formed in situ, starting at a readily accessible temperature of 200 degrees Celsius. Local control of both the nanoprecipitation and the martensitic transformation during the fabrication leads to complex microstructure hierarchies across multiple length scales, from approximately 100-micrometre-thick layers down to nanoscale precipitates. Inspired by ancient Damascus steels11–14—which have hard and soft layers, originally introduced via the folding and forging techniques of skilled blacksmiths—we produced a material consisting of alternating soft and hard layers. Our material has a tensile strength of 1,300 megapascals and 10 per cent elongation, showing superior mechanical properties to those of ancient Damascus steel12. The principles of in situ precipitation strengthening and local microstructure control used here can be applied to a wide range of precipitation-hardened alloys and different additive manufacturing processes. A Damascus-like steel consisting of alternating hard and soft layers is created by using a laser additive manufacturing technique and digital control of the processing parameters.

Materials, 15 (17), ISSN:1996-1944

The development of strong-scaling computational tools for high-throughput methods with an open-source code and transparent metadata standards has successfully transformed many computational materials science communities. While such tools are mature already in the condensed-matter physics community, the situation is still very different for many experimentalists. Atom probe tomography (APT) is one example. This microscopy and microanalysis technique has matured into a versatile nano-analytical characterization tool with applications that range from materials science to geology and possibly beyond. Here, data science tools are required for extracting chemo-structural spatial correlations from the reconstructed point cloud. For APT and other high-end analysis techniques, post-processing is mostly executed with proprietary software tools, which are opaque in their execution and have often limited performance. Software development by members of the scientific community has improved the situation but compared to the sophistication in the field of computational materials science several gaps remain. This is particularly the case for open-source tools that support scientific computing hardware, tools which enable high-throughput workflows, and open well-documented metadata standards to align experimental research better with the fair data stewardship principles. To this end, we introduce paraprobe, an open-source tool for scientific computing and high-throughput studying of point cloud data, here exemplified with APT. We show how to quantify uncertainties while applying several computational geometry, spatial statistics, and clustering tasks for post-processing APT datasets as large as two billion ions. These tools work well in concert with Python and HDF5 to enable several orders of magnitude performance gain, automation, and reproducibility.

There is growing interest in Laser Powder Bed Fusion (L-PBF) or Selective Laser Melting (SLM) manufacturing of high conductivity metals such as copper and refractory metals. SLM manufacturing of high thermal conductivity metals is particularly difficult. In case of refractory metals, the difficulty is amplified because of their high melting point and brittle behaviour. Rapid process development strategies are essential to identify suitable process parameters for achieving minimum porosities in these alloys, yet current strategies suffer from several limitations. We propose a simple approach for rapid process development using normalized process maps. Using plots of normalized energy density vs. normalized hatch spacing, we identify a wide processability window. This is further refined using analytical heat transfer models to predict melt pool size. Final optimization of the parameters is achieved by experiments based on statistical Design of Experiments concepts. In this article we demonstrate the use of our proposed approach for development of process parameters (hatch spacing, layer thickness, exposure time and point distance) for SLM manufacturing of molybdenum and aluminium. Relative densities of 97.4% and 99.7% are achieved using 200 W pulsed laser and 400 W continuous laser respectively, for molybdenum and aluminium, demonstrating the effectiveness of our approach for SLM processing of high conductivity materials.

Grain structure control is essential in metal additive manufacturing. It is used to avoid anisotropic mechanical properties, hot cracking and to increase the strength via the Hall-Petch effect. Here we demonstrate the use of grain refining particles for grain control in ferritic alloys, specifically Fe-Ti model alloys. We introduce the particles in three different ways, namely (i) by using oxygen-rich raw powders, (ii) by reaction of the molten material with the process gas atmosphere and (iii) by direct addition of the refining ceramic phase in powder form. Samples are produced by Laser Powder Bed Fusion with various concentrations of Ti and under Ar and N2 atmosphere. The resulting microstructures are analyzed using optical and electron microscopy. We demonstrate a transition from a microstructure containing columnar grains >100 μm in length to a strongly grain refined microstructure with equiaxed grains of approx. 1 μm in size. The refining sub-micron-sized particles in all cases are cubic Ti(O,N). We discuss the findings in the light of thermodynamic calculations as well as established grain refinement models.

The 15-5PH (UNS S 15500) stainless steel combines high mechanical strength, ductility, and good corrosion resistance for aircraft and aerospace applications. This set of properties and its high added-value applications make it an excellent choice for additive manufacturing processes such as laser powder-bed fusion (LPBF). However, there is a need to understand the complex microstructure developed in LPBF-processed parts, which may show particularities such as columnar solidification, preferential orientation, different kinds of porosities, chemical segregation along the melt pools, metastable phases, and oxide nanoinclusions. We report the microstructural characterization of LPBF-processed 15-5PH stainless steel in the as-built condition and after aging. Low porosity (

The design of advanced alloys specifically tailored to additive manufacturing processes is a research field that is attracting ever-increasing attention. Laser powder-bed fusion (LPBF) commonly uses pre-alloyed, fine powders (diameter usually 15&ndash, 45 &micro, m) to produce fully dense metallic parts. The availability of such fine, pre-alloyed powders reduces the iteration speed of alloy development for LPBF and renders it quite costly. Here, we overcome these drawbacks by performing in-situ alloying in LPBF starting with pure elemental powder mixtures avoiding the use of costly pre-alloyed powders. Pure iron, chromium, and nickel powder mixtures were used to perform in-situ alloying to manufacture 304 L stainless steel cube-shaped samples. Process parameters including scanning speed, laser power, beam diameter, and layer thickness were varied aiming at obtaining a chemically homogeneous alloy. The scientific questions focused on in this work are: which process parameters are required for producing such samples (in part already known in the state of the art), and why are these parameters conducive to homogeneity? Analytical modelling of the melt pool geometry and temperature field suggests that the residence time in the liquid state is the most important parameter controlling the chemical homogeneity of the parts. Results show that in-situ alloying can be successfully employed to enable faster and cost-efficient rapid alloy development.

High entropy alloys are generally considered to be single phase material. This state is, however, typically a non-equilibrium state after fabrication at high cooling rates. Phase constitution after fabrication or heat treatment is mostly known for isothermal annealing only and for casts as well as rapidly quenched alloys. Knowledge on early phase separation stages of high entropy alloys and their mechanisms are missing so far. Here, we present results on phase separation at intermediate cooling rates, by characterization of gas atomized powder of the AlCoCr0.75Cu0.5FeNi alloy. Although investigation by X-ray diffraction and Electron Backscatter Diffraction indicates a single-phase nature of the powder particles, aberration-corrected scanning transmission electron microscopy and atom probe tomography reveal a nanoscale phase separation into Ni-Al-rich B2 and Fe-Cr-rich A2 regions as well as a high number density of 3.1x1024 Cu-rich clusters per m3 in the B2 matrix. The observed phase separation and cluster formation are linked to spinodal decomposition and nucleation processes, respectively. The study highlights that adequate characterization techniques need to be chosen when making statements about phase stability and structural evolution in compositionally complex alloys., 33 pages, 12 figures

The significant strengthening of selectively laser melted (SLM) 304L stainless steel that occurs due to high-pressure torsion (HPT) is examined by recourse to detailed nanomechanical and microstructural characterization. In the as-built alloy, dislocation hardening is the main strengthening mechanism. After HPT, however, the synergistic combination grain refinement and martensitic transformation dominate the strength of the alloy. In the nanocrystalline regime, the dominance of the grain boundary-mediated plasticity retards the martensite-induced hardening.

Atom probe tomography (APT) is rising in influence across many parts of materials science and engineering thanks to its unique combination of highly sensitive composition measurement and three-dimensional microstructural characterization. In this invited article, we have selected a few recent applications that showcase the unique capacity of APT to measure the local composition at structural defects. Whether we consider dislocations, stacking faults, or grain boundary, the detailed compositional measurements tend to indicate specific partitioning behaviors for the different solutes in both complex engineering and model alloys we investigated.

Mo-Si-B alloys are potential creep resistant materials for accessing harsh loading scenarios beyond Ni-based superalloys due to their excellent mechanical performance at ultra-high temperatures (> 1200 °C). Here, we report on the fabrication through laser additive manufacturing of a Mo rich Mo-Si-B alloy with and without dispersion of oxide (La2O3) particles. The major phase in the solidified material is dendritic α-Mo. The inter-dendritic regions contain a mixture of the Mo5Si3 (T1) + Mo5SiB2 (T2) phases, and not the expected equilibrium Mo3Si + Mo5SiB2 (T2) phases. This combination of phases is shown to yield improved high temperature creep resistance but was only accessible through by addition of Nb, W or Ti that substitute Mo in the intermetallic phases. Whereas here it is attributed to the large undercooling in the small melt pool produced during laser processing. We show that this phase mixture, upon annealing, is stable at 1200 °C for 200 h. We also demonstrate successful dispersion of oxide particles mainly in the inter-dendritic regions leading to a high indentation fracture toughness of ∼18 MPa√m at room temperature. Toughening originates from crack trapping in the ductile α-Mo and the formation of micro-cracks and crack deflection in the vicinity of oxide particles.

The influence of hydrogen on the mechanical behavior of Inconel 718 fabricated by laser powder-bed-fusion was investigated through a series of tensile experiments. Samples subjected to two different post-fabrication heat treatments, viz. direct aging (DA) and homogenization plus aging (HA), were tested. Detailed microstructural characterization showed that a solidification substructure including a high density of dislocations and precipitates prevails in the DA sample while the HA sample is free from such a substructure. The DA sample exhibited a comparatively higher strength, but a lower resistance to hydrogen embrittlement. By recourse to a statistical analysis of the hydrogen-assisted cracks, the severe hydrogen embrittlement of the DA sample was proven to be due to the significant portion of hydrogen-assisted intergranular cracks that occurred without the aid of slip localization. These results are discussed in terms of the changes in microstructure upon heat treatments, and their influences on the hydrogen trapping sites.

Alloys manufactured by laser powder-bed fusion have intrinsic and hierarchical microstructural features inherited from the fast solidification (up to 104 K/s) and subsequent thermal cycles. This creates epitaxed grains, dislocation cell structures, and second-phase oxide nanoparticles. Epitaxed grains follow a pattern where finer grains are found in the melt pool centerline along the laser track. Upon further annealing, this characteristic microstructure has pronounced consequences on the recrystallization mechanisms and thus on grain topology. By changing the scanning strategy, we control the emerging grain patterns in a representative alloy (AISI 316L austenitic stainless steel) by creating linear strings for unidirectional scans, while a chessboard grain pattern arises by applying a 90°-rotation between layers. Upon post-processing annealing (at 1150 °C from 15 min to 8 h), we study the relationship between the as-built and recrystallized microstructures. Recrystallization starts with fine nuclei in regions with high dislocation density along the melt pool centerlines, resulting in early-stage linear impingement (linearly clustered nucleation), as revealed by microstructural path analysis. Recrystallization is sluggish, due to dynamic Zener-Smith pinning. This effect leads to jerky boundary motion due to periodic pinning and depinning from oxide particles, caused by their gradual coarsening. Lower nuclei number density slows kinetics for the case of unidirectional scanning, while twinning aids in the nucleation of grains with mobile grain boundaries. Our findings show that changes in the laser scanning strategy are a suitable design tool for tailoring recrystallization and thus microstructure.

In the development of high-strength aluminium alloys tailored specifically to additive manufacturing (AM), L12-Al3X-forming elements have been proven to be particularly effective alloying additions, reducing the susceptibility of aluminium alloys to solidification cracking by grain refinement and increasing the strength by forming secondary nanoscale precipitates. In the present work, we employ laser powder bed fusion ( L -PBF) to examine the feasibility of using Ti as the main strengthening, L12-forming element for the design of a well-processable, precipitation-strengthened model alloy. Al-1.76Ti and Al-2.51Ti (wt%) alloys with and without ternary additions of Ni and Si are fabricated during processing from powder mixtures. Crack-free microstructures are produced, which display alternating fine- and coarse-grained regions. During heat treatment, one of the investigated alloys, Al-2.51Ti-0.7Si, exhibits an ageing response due to the formation of nanoscale, metastable L12-(Al,Si)3Ti precipitates, reaching a peak hardness of 97 HV. This demonstrates that L -PBF-processed Ti-containing aluminium alloys can exhibit a precipitation hardening response similar to alloys containing Sc or Zr. In the other Al-Ti-based materials tested, no significant hardness increase was found. This discrepancy is ascribed to the effects Si exerts on the precipitation process. First, the addition of Si increases the thermodynamic driving force for homogeneous nucleation of L12-Al3Ti precipitates. Secondly, Si-Ti co-clustering is observed by atom probe tomography, which is expected to enhance the otherwise sluggish diffusion of Ti. The Al-2.51Ti-0.7Si alloy developed in this work can in the future be further strengthened by adding additional alloying elements and by optimising the heat treatment.

By using laser powder bed fusion (LPBF) in the tooling industry, tools with complex geometries and integrated functions, such as adapted cooling channels, can be manufactured with high potential in terms of product lifetimes or cycle times. When processing tool steels with a carbon content > 0.6 wt.-% by means of LPBF, hard and brittle phases are formed as well as soft retained austenite and carbides. Combined with high internal stresses in the part this often leads to crack formation. Using base plate preheating up to 500 °C can enable the production of crack free components, however, to increase the processability of high-speed steel, varying the alloy composition by stabilizing austenite could lead to reduced residual stresses. In this study, we investigate the processability and microstructure of high-speed steel HS6-5-3-8 reference and HS6-5-3-8 with increased carbon content by rapid alloy development (RAD) in the LPBF process. The manufactured specimens are analysed based on part density, hardness, microstructure, and homogeneity of the microstructure. Light-optical and electron microscopic methods (i.e. SEM, EDS, EBSD) are used for microstructure investigations. We found that an increased carbon content in the alloy leads to an increased carbide volume fraction and a fully austenitic matrix. However, contrary to the hypothesized beneficial impact of austenite stabilization on crack formation, we observe a worsening of cracking with C content. Based on these results, we discuss which microstructural features are the deciding factors for cold cracking in LPBF of high-carbon steels. Based on the results, a relationship between alloy composition of high-speed steel and their processability is discussed and the application of RAD by means of LPBF is assessed.

Metallurgical and materials transactions / A 51(11), 5517-5586 (2020). doi:10.1007/s11661-020-05947-2, Published by Springer, Boston

A vital issue during selective laser melting of nonweldable polycrystalline nickel-base superalloys is the formation of microcracks. These are cracks occurring during the last stage of solidification and only at high angle grain boundaries (HAGBs). Solute enrichment to the remaining interdendritic liquid and its partial back-diffusion into the solid contributes to the crack nucleation mechanism. Here we use atom probe tomography coupled with transmission Kikuchi diffraction to determine the misorientation and chemical composition profiles across HAGBs (with and without cracks) and across crack-free low angle grain boundaries (LAGBs). The Gibbsian interfacial excess of solutes (mainly B, C, Si, and Zr) is at least two times higher at the HAGB compared to the LAGB. The chemical profiles show the opposite behavior to established model predictions of the last stage of solidification. Our diffusion calculations elucidate that the chemical profiles are influenced by both microsegregation (of Ti, Nb, and Si) during solidification and solid-state segregation (of B, C, and Zr) during cooling. The chemical profiles in the topmost layer indicate a negligible effect of remelting and reheating. Except for Ti-rich carbides, no secondary phases are found. Additionally, we study an alloy with a reduced content of Zr and Si (by at least 60 wt. %), relative to the standard IN738LC composition. We achieved a 99% reduction in crack length per unit area. However, the grain boundary enrichment of Zr and Si in the modified alloy was similar to the standard alloy. Based on these findings, we critically discuss the contribution of various mechanisms proposed for solidification cracking.

Laser additive manufacturing is attractive for the production of complex, three-dimensional parts from metallic powder using a computer-aided design model

Many alloys produced by Laser Powder Bed Fusion (LPBF) suffer from coarse grains and anisotropic mechanical properties. Here, we investigate how the addition of Ti can cause significant strengthening via grain refinement in a model ferritic stainless steel. We perform LPBF experiments using elemental Fe, Cr, and Ti powders (with significant O impurity in the Fe powder) and perform microstructural analysis by SEM, EDS and EBSD as well as tensile tests on the alloys Fe-19at.%Cr and Fe-19at.%Cr-5at.%Ti. The Fe-Cr alloy displays very large grains after LPBF and a strong cube texture, rendering its mechanical properties similar to a single crystal. In the Fe-Cr-Ti alloy, TiO particle formation in the melt causes strong grain refinement, leading to a texture-free microstructure consisting of equiaxed grains ~1.6 μm in diameter. The 0.2% proof strength of the ternary alloy is more than double that of the binary alloy (281 MPa → 591 MPa), and the work hardening rate is also increased. While the elongation at fracture is reduced for the Fe-Cr-Ti alloy, at ~15 %, it remains sufficient, and samples show ductile fracture surfaces. We estimate that the grain refinement accounts for the majority of the strengthening, however, solid solution strengthening and the effect of the texture are also significant.

The effect of the initial microstructure (recrystallized or cold-rolled) on the nitride precipitation process upon gaseous nitriding of ternary Fe-4.3 at. pct Cr-8.1 at. pct Al alloy was investigated at 723 K (450 °C) employing X-ray diffraction (XRD) analyses, transmission electron microscopy (TEM), atom probe tomography (APT), and electron probe microanalysis (EPMA). In recrystallized Fe-Cr-Al specimens, one type of nitride develops: ternary, cubic, NaCl-type mixed Cr1−x Al x N. In cold-rolled Fe-Cr-Al specimens, precipitation of two types of nitrides occurs: ternary, cubic, NaCl-type mixed Cr1−x Al x N and binary, cubic, NaCl-type AlN. By theoretical analysis, it was shown that for the recrystallized specimens an energy barrier for the nucleation of mixed Cr1−x Al x N exists, whereas in the cold-rolled specimens no such energy barriers for the development of mixed Cr1−x Al x N and of binary, cubic AlN occur. The additional development of the cubic AlN in the cold-rolled microstructure could be ascribed to the preferred heterogeneous nucleation of cubic AlN on dislocations. The nitrogen concentration–depth profile of the cold-rolled specimen shows a stepped nature upon prolonged nitriding as a consequence of instantaneous nucleation of nitride upon arrival of nitrogen and nitride growth rate-limited by nitrogen transport through the thickening nitrided zone.

International audience; One major hindrance that alloy design for additive manufacturing (AM) faces nowadays is hot tearing. Contrary to the previous works which either try to reduce solidification range or introduce grain refinement, the current work presents a new approach of employing segregation engineering to alter the residual stress states at the interdendritic and grain boundary regions and consequently prevent hot tearing. Here, in situ Al alloying is introduced into an existing hot-cracking susceptible high-entropy alloy CoCrFeNi. It is found that within a certain range of compositions, such as Al0.5CoCrFeNi, the hot crack density was drastically decreased. During the solidification of this specific alloy composition, Al is firstly ejected from the primary dendritic face-centred cubic (FCC) phase and segregates into the interdendritic regions. Spinodal decomposition then occurs in these Al-enriched regions to form the ordered B2 NiAl and disordered body-centred cubic (BCC) Cr phases. Due to the higher molar volume and lower homologous temperatures of these B2/BCC phases, the inherent residual strain is accommodated and transformed from a maximum 0.006 tensile strain in CoCrFeNi to a compressive strain of ~0.001 in Al0.5CoCrFeNi. It is believed that this grain boundary segregation engineering method could provide a new pathway to systematically counteract the hot tearing problem in additive manufacturing of metals and alloys, using available thermodynamic and kinetic database information.

Hydrogen embrittlement in 304L austenitic stainless steel fabricated by laser powder-bed-fusion (LPBF) was investigated and compared to conventionally produced 304L samples with two different processing histories; casting plus annealing (CA) and CA plus thermomechanical treatment (CA-TMT). Interestingly, no significant difference in the amount of deformation-induced α′ martensite between the LPBF and CA-TMT samples was observed, suggesting that the solidification substructure in the LPBF sample enhanced the strength without promoting the harmful hydrogen embrittlement effect. These results are discussed in terms of the chemical inhomogeneity, hydrogen-assisted cracking behavior, and hydrogen diffusion and trapping in the present 304L samples.

We report the synthesis of a bulk nanostructured alloy using laser-powder bed fusion. The equiatomic AlCoCrFeMnNi chemically complex alloy forms a nanoscale modulated structure, which is homogeneously distributed in the as-built condition. The nanostructure consists of Al & Ni-rich ordered and Cr & Fe-rich disordered BCC phases. The two phases form an interconnected phase network with coherent interface boundaries. Atom probe tomography and aberration-corrected scanning transmission electron microscopy analysis of the spatial distribution of the modulated structure suggests the occurrence of nano-scale spinodal decomposition. These results introduce a direct synthesis of bulk nanostructured alloys with promising geometric flexibility.

Traditionally, reactive gases such as oxygen (O2) and carbon dioxide (CO2) have been avoided during laser powder bed fusion (L-PBF) of metals and alloys based on the notion that it may lead to defect formation and poor properties. Here we show that instead, these gases can be used to form sub-μm-sized oxide particles in-situ during the L-PBF process in an Fe-Cr-Al-Ti stainless steel and lead to improved room temperature and high-temperature mechanical properties. We manufactured cube samples using pure Ar and various reactive gas atmospheres, namely an O2/Argon (Ar) mixture containing 0.2 % O2 and CO2/Ar mixtures containing up to 100 % CO2. Co-axial measurements of infrared radiation emitted from the melt pool showed correlation to the presence of O2 or CO2 in the gas mixture. Builds produced under CO2-containing atmosphere contained complex oxides with an average diameter of ∼40 nm, an Al-rich core and a Ti-rich shell. Due to the high cooling rates typical to L-PBF, agglomeration of oxides and slag formation on the surface of the samples could almost be entirely avoided. Compression tests at temperatures up to 800 °C showed that the samples produced in 100 % CO2 have about 20 % higher yield stress compared to samples produced in Ar. The paper concludes with a discussion of the formation mechanism of the observed oxides. Our results show that in-situ reactions during additive manufacturing processes are a promising pathway to the synthesis of particle-reinforced alloys.

Ti has a high affinity for hydrogen and is a typical hydride formers. Ti-hydride are brittle phases which probably cause premature failure of Ti-alloys. Here, we used atom probe tomography and electron microscopy to investigate the hydrogen distribution in a set of specimens of commercially pure Ti, model and commercial Ti-alloys. Although likely partly introduced during specimen preparation with the focused-ion beam, we show formation of Ti-hydrides along {\alpha} grain boundaries and {\alpha}/\b{eta} phase boundaries in commercial pure Ti and {\alpha}+\b{eta} binary model alloys. No hydrides are observed in the {\alpha} phase in alloys with Al addition or quenched-in Mo supersaturation., Comment: Published in Acta Materialia in 2018

Laser Additive Manufacturing (LAM) of light metals such as high-strength Al-based alloys offers tremendous potential for e.g. weight reduction and associated reduced fuel consumptions for the transportation industry. Typically, commercial Sc-containing alloys, such as Scalmalloy®, rely on precipitation hardening to increase their strength. Conventional processing involves controlled ageing during which ordered and coherent Al3Sc precipitates form from a Sc-supersaturated solid solution. Here we show how the intrinsic heat treatment (IHT) of directed energy deposition (DED) can be used to trigger the precipitation of Al3Sc already during the LAM process. High number densities of 1023 nano-precipitates per m3 can be realized through solid-state phase transformation from the supersaturated Al-Sc matrix that results from the fast cooling rate in LAM. Yet, the IHT causes precipitates to coarsen, hence reducing their strengthening effect. We implement alternative solidification conditions to exploit the IHT to form a Zr-rich shell around the Al3Sc precipitates that prevents coarsening. Our approach is applicable to a wide range of precipitation-hardened alloys to trigger in-situ precipitation during LAM.

A combination of transmission electron microscopy, atom probe tomography and high-energy X-ray diffraction was employed to investigate the influence of local microstructural changes on strengthening in a commercial Al–Cu–Li–Mg based alloy, AA2198, in the stretched and naturally aged, and overaged states. Strengthening in the stretched and naturally aged temper was shown to be governed by a combination of Cu–Cu clusters, δ′/β′ phase and solution strengthening. This is in contrast to another report which suggests that strength in this temper is only due to Cu-rich clusters [B. Decreus, et al., Acta Mater., 61 (2013) 2207]. On the other hand, although large volume fractions of equilibrium phases such as TB, and θ were present in the overaged temper, its strengthening was largely governed by order hardening, which is the strengthening mechanism associated with the δ′/β′ phase. The δ′/β′ phase remained in the matrix even after extensive overaging.

We study the mechanisms of deformation driven chemical mixing in a metallic nanocomposite model system. More specific, we investigate shear banding at the atomic scale in an amorphous CuZr/ crystalline Cu nanolaminate, deformed by microindentation. Three CuZr/Cu multilayer systems (100 nm Cu/100 nm CuZr, 50 nm Cu/100 nm CuZr, and 10 nm Cu/100 nm CuZr) are fabricated to study the effect of layer thickness on shear band formation and deformation induced alloying. The chemical and structural evolution at different strain levels are traced by atom probe tomography and transmission electron microscopy combined with nano-beam diffraction mapping. The initially pure crystalline Cu and amorphous CuZr layers chemically mix by cross-phase shear banding after reaching a critical layer thickness. The Cu inside the shear bands develops a high dislocation density and can locally undergo transition to an amorphous state when sheared and mixed. We conclude that the severe deformation in the shear bands in the amorphous layer squeeze Zr atoms into the Cu dislocation cores in the Cu layers (thickness

Due to the layer-by-layer build-up of additively manufactured parts, the deposited material experiences a cyclic re-heating in the form of a sequence of temperature pulses. In the current work, this “intrinsic heat treatment (IHT)” was exploited to induce the precipitation of NiAl nanoparticles in an Fe-19Ni-xAl (at%) model maraging steel, a system known for rapid clustering. We used Laser Metal Deposition (LMD) to synthesize compositionally graded specimens. This allowed for the efficient screening of effects associated with varying Al contents ranging from 0 to 25 at% and for identifying promising concentrations for further studies. Based on the existence of the desired martensitic matrix, an upper bound for the Al concentration of 15 at% was defined. Owing to the presence of NiAl precipitates as observed by Atom Probe Tomography (APT), a lower bound of 3–5 at% Al was established. Within this concentration window, increasing the Al concentration gave rise to an increase in hardness by 225 HV due to an exceptionally high number density of 1025 NiAl precipitates per m3, as measured by APT. This work demonstrates the possibility of exploiting the IHT of the LMD process for the production of samples that are precipitation strengthened during the additive manufacturing process without need for any further heat treatment.

Today, a large number of different steels are being processed by Additive Manufacturing (AM) methods. The different matrix microstructure components and phases (austenite, ferrite, martensite) and the various precipitation phases (intermetallic precipitates, carbides) lend a huge variability in microstructure and properties to this class of alloys. This is true for AM-produced steels just as it is for conventionally-produced steels. However, steels are subjected during AM processing to time-temperature profiles which are very different from the ones encountered in conventional process routes, and hence the resulting microstructures differ strongly as well. This includes a very fine and highly morphologically and crystallographically textured microstructure as a result of high solidification rates as well as non-equilibrium phases in the as-processed state. Such a microstructure, in turn, necessitates additional or adapted post-AM heat treatments and alloy design adjustments. In this review, we give an overview over the different kinds of steels in use in fusion-based AM processes and present their microstructures, their mechanical and corrosion properties, their heat treatments and their intended applications. This includes austenitic, duplex, martensitic and precipitation-hardening stainless steels, TRIP/TWIP steels, maraging and carbon-bearing tool steels and ODS steels. We identify areas with missing information in the literature and assess which properties of AM steels exceed those of conventionally-produced ones, or, conversely, which properties fall behind. We close our review with a short summary of iron-base alloys with functional properties and their application perspectives in Additive Manufacturing.

Introducing a soft crystalline phase into an amorphous alloy can promote the compound’s ductility. Here we synthesized multilayered nanolaminates consisting of alternating amorphous Cu54Zr46 and nanocrystalline Cu layers. The Cu layer thickness was systematically varied in different samples. Mechanical loading was imposed by nanoindentation and micropillar compression. Increasing the Cu layer thickness from 10 to 100 nm led to a transition from sharp, cross-phase shear banding to gradual bending and co-deformation of the two layer types (amorphous/nanocrystalline). Specimens with a sequence of 100 nm amorphous Cu54Zr46 and 50 nm Cu layers show a compressive flow stress of 2.57 ± 0.21 GPa, matching the strength of pure CuZr metallic glass, hence exceeding the linear rule of mixtures. In pillar compression, 40% strain without fracture was achieved by the suppression of percolative shear band propagation. The results show that inserting a ductile nanocrystalline phase into a metallic glass prevents catastrophic shear banding. The mechanical response of such nanolaminates can be tuned by adjusting the layer thickness. 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Materials produced by selective laser melting (SLM) experience a thermal history that is markedly different from that encountered by conventionally produced materials. In particular, a very high cooling rate from the melt is combined with cyclical reheating upon deposition of subsequent layers. Using atom-probe tomography (APT), we investigated how this nonconventional thermal history influences the phase-transformation behavior of maraging steels (Fe–18Ni–9Co–3.4Mo–1.2Ti) produced by SLM. We found that despite the “intrinsic heat treatment” and the known propensity of maraging steels for rapid clustering and precipitation, the material does not show any sign of phase transformation in the as-produced state. Upon aging, three different types of precipitates, namely (Fe,Ni,Co)3(Ti,Mo), (Fe,Ni,Co)3(Mo,Ti), and (Fe,Ni,Co)7Mo6 (μ phase), were observed as well as martensite-to-austenite reversion around regions of the retained austenite. The concentration of the newly formed phases as quantified by APT closely matches thermodynamic equilibrium calculations.

The authors uses laser additive manufacturing (LAM) as a combinatorial method for synthesizing microstructurally and compositionally piecewise graded bulk alloys. Authors fabricate blocks consisting of a sequence of ≈500 mm thick tool steel layers, each with different chemical composition, by laser metal deposition where alloy powders are deposited layer-wise on a substrate. The reference materials are a Cr-Mo-V hot working tool steel and a Ni-based maraging steel. The layers between them consist of corresponding blends of the two materials with varying composition from layer to layer (alloy volume fractions 80:20, 60:40, 40:60, and 20:80). The bulk alloy is hot rolled and heat treated. Subsequently each layer is characterized for microstructure, chemical composition and mechanical properties using electron back scatter diffraction, tensile testing, and indentation. The approach is an efficient high-throughput method enabling rapid probing of novel compositional alloy blends. It can be applied for finding new alloys both, by LAM and for LAM. For the tool steel blends synthesized here, authors observe that the Cr-Mo-V tool steel, when mixed with the Ni-base maraging steel, can be continuously tuned for a strength-ductility profile in the range of 800-1650 MPa strength and 15-25% tensile elongation.

Maraging steels are used to produce tools by Additive Manufacturing (AM) methods such as Laser Metal Deposition (LMD) and Selective Laser Melting (SLM). Although it is well established that dense parts can be produced by AM, the influence of the AM process on the microstructure—in particular the content of retained and reversed austenite as well as the nanostructure, especially the precipitate density and chemistry, are not yet explored. Here, we study these features using microhardness measurements, Optical Microscopy, Electron Backscatter Diffraction (EBSD), Energy Dispersive Spectroscopy (EDS), and Atom Probe Tomography (APT) in the as-produced state and during ageing heat treatment. We find that due to microsegregation, retained austenite exists in the as-LMD- and as-SLM-produced states but not in the conventionally-produced material. The hardness in the as-LMD-produced state is higher than in the conventionally and SLM-produced materials, however, not in the uppermost layers. By APT, it is confirmed that this is due to early stages of precipitation induced by the cyclic re-heating upon further deposition—i.e., the intrinsic heat treatment associated with LMD. In the peak-aged state, which is reached after a similar time in all materials, the hardness of SLM- and LMD-produced material is slightly lower than in conventionally-produced material due to the presence of retained austenite and reversed austenite formed during ageing.

The kinetics and microstructure of the static recrystallization of strongly deformed, pure copper were investigated based on a comparison of mesoscopic, cellular automata simulations with experimental data. Physical models for the nucleation rate and the growth rate of recrystallized grains were employed, which required experimentally obtained informations about the deformed state as input. The orientation-distribution function and the misorientation-angle distribution for neighboring grains of deformed specimens were used to set up the microstructure serving as the start configuration for the simulations. The influences of a subgrain-size distribution, of an ongoing nucleation during recrystallization, of an inhomogeneously distributed stored energy in the deformed state, and of a misorientation-dependent interface mobility were investigated. The simulated microstructures after recrystallization exhibit a bimodal grain-size distribution instead of the broad, monomodal grain-size distribution found in the experiments. It is argued that spatially resolved determination of crystal (subgrain) orientation and (deformation) energy is necessary to arrive at realistic descriptions of both the recrystallization kinetics and the microstructure after completed recrystallization.

The kinetics of nucleation-and-growth phase transformations for which nucleation occurs on the parent-phase grain boundaries was studied using mesoscopic microstructure simulations. The influences of the parent microstructure (notably grain size and grain-size distribution) and the parent → product transformation mechanism were determined and discussed. Subsequently, several mesoscopic kinetic models were investigated with respect to their ability to describe the simulated transformation kinetics, namely the classical Johnson–Mehl–Avrami–Kolmogorov (JMAK) model, (i.e., assuming random nucleation), previously proposed empirical extensions of the JMAK model in the framework of the modular kinetic model approach, the Cahn model (assuming nucleation on randomly distributed planes) and a new empirical extension of the Cahn model proposed here. None of the models exactly predicts the real phase transformation kinetics. The classical JMAK model is unable to describe the simulated grain-boundary nucleated transformation kinetics. The Cahn model leads to erroneous results on fitting to simulated transformation curves. It is concluded that the modified Cahn model proposed here is best suited to infer correct values of kinetic material parameters from experimentally obtained data on the kinetics of grain-boundary nucleated phase transformations.

This articles provides a summary of results of recent research on simulations of interface-controlled phase transformations with the aim of better understanding both the kinetics of these transformations and the resulting microstructure. Atomistic (kinetic Monte Carlo) simulations were performed to gain insight into the atomic (jump) processes occurring during interface movement in the massive austenite → ferrite phase transformation in pure iron. Mesoscopic (geometric) simulations were performed to reach an understanding of the formation of the microstructures resulting from phase transformations which obey specified kinetic models. As a special feature, the effect of non-random nucleation on the transformation kinetics was studied.

The kinetics of phase transformations for which nucleation occurs on parent-micro-structure grain boundaries, and the resulting microstructures, were investigated by means ofgeometric simulations. The influences of parent microstructure grain-boundary area density,parent grain-size distribution and parent→product kinetics were analysed. Additionally, thesimulated kinetics were compared with predictions from two kinetic models, namely a modelproposed for spatially random nucleation and a model proposed for grain-boundary nucleation.It was found that the simulated transformed fraction as function of time lies in between the twomodel predictions for all investigated parent microstructures and parent→product kinetics.

The allotropic, martensitic phase transformation (hcp → fcc) in cobalt was investigated by differential scanning calorimetry (DSC) upon isochronal annealing at heating rates in the range from 10 K min−1 to 40 K min−1. The microstructural evolution was traced by optical microscopy and X-ray diffractometry. The kinetics of the phase transformation from hcp to fcc Co upon isochronal annealing was described on the basis of a modular phase transformation model. Appropriate model descriptions for athermal nucleation and thermally activated, anisotropic interface controlled growth tailored to the martensitic phase transformation of Co were implemented into the modular model. Fitting of this model of phase transformation kinetics to simultaneously all isochronal DSC runs yielded values for the energy of the interface separating the hcp and fcc Co phase and the activation energy for growth.

JOM : a publication of the Minerals, Metals & Materials Society (TMS) 68(3), 943-949 (2016). doi:10.1007/s11837-015-1764-2, Published by Springer Science + Business Media, New York, NY

Despite being extremely attractive compounds for strengthening, oxides and nitride particles have found only limited use in metallic materials design, as obtaining appropriate size and dispersion up to now necessitates production by time- and cost-intensive powder metallurgy processes. Here we present an alternative production method, based on the oxide and nitride formation during liquid-metal-deposition procedures in oxygen and/or nitrogen containing atmospheres. Rapid solidification of the small liquid zone suppresses floatation and agglomeration of particles, while subsequent thermo-mechanical treatments densify the material and aids particle dispersion. The in-situ particle formation coupled to the high deposition rates ensures a drastically shortened production chain. The feasibility of the method is exemplarily demonstrated on austenitic stainless steel and commercially available deposition techniques as used in additive manufacturing, performed without shielding gas but instead at air. Even without substantial optimisation of processes and material, >2 vol.% of hard and stable Cr2N particles with sizes down to 80 nm could be evenly dispersed, resulting in pronounced strengthening at both room temperature and 700 °C without significant loss in ductility. Future possibilities for creating novel generations of cost effective and lean high strength materials, especially for high temperature applications, are outlined and discussed. Keywords: ODS steel, Dispersion strengthening, Additive manufacturing