In laser additive manufacturing (AM) of hot work tool steels, direct tempering (DT) of the tool from as-built (AB) condition without prior conventional austenitization and quenching results in enhanced tempering resistance. To date, intercellular retained austenite (RA) decomposition, leading to a shift in secondary hardening peak temperature, and finer martensite substructure are reported to be responsible for such a behavior. In this work, authors aimed at studying the strengthening contributions by performing isothermal tempering tests for long times (up to 40 hours) at elevated temperatures (up to 650 degrees C) on DT and quenched and tempered (QT) specimens. The thermal softening kinetics and the microstructural evolution were evaluated with the support of computational thermodynamics. The results suggest that the main contributor to enhanced temper resistance in DT condition is the larger fraction of thermally stable and extremely fine (similar to 20 nm) secondary (tempering) V(C,N) compared with QT. This could be explained by the reduction of available V and C in austenitized and quenched martensite for a later secondary V(C,N) precipitation during tempering, because of equilibrium precipitation of relatively large (up to 500 nm) vanadium-rich carbonitrides during the austenitization process. A complementary effect of the substructure refinement (i.e., martensite block width) in rapidly solidified highly supersaturated martensite was also quantified in terms of Hall-Petch strengthening mechanism. The significant effect of secondary V(C,N) was successfully validated by assessing a laser AM processed vanadium-free hot work tool steel in QT and DT condition, where no significant differences in strength and temper resistance between the two conditions were evident. [GRAPHICS] .

Electron beam-powder bed fusion (PBF-EB) is an additive manufacturing process that utilizes an electron beam as the heat source to enable material fusion. However, the use of a charge-carrying heat source can sometimes result in sudden powder explosions, usually referred to as "Smoke", which can lead to process instability or termination. This experimental study investigated the initiation and propagation of Smoke using in situ high-speed synchrotron radiography. The results reveal two key mechanisms for Smoke evolution. In the first step, the beam-powder bed interaction creates electrically isolated particles in the atmosphere. Subsequently, these isolated particles get charged either by direct irradiation by the beam or indirectly by back-scattered electrons. These particles are accelerated by electric repulsion, and new particles in the atmosphere are produced when they impinge on the powder bed. This is the onset of the avalanche process known as Smoke. Based on this understanding, the dependence of Smoke on process parameters such as beam returning time, beam diameter, etc., can be rationalized.

As a potent grain refiner for steel casting, TiN is now widely used to refine γ-austenite in steel additive manufacturing (AM). However, the refining mechanism of TiN during AM remains unclear despite intensive research in recent years. This work aims to boost our understanding on the mechanism of TiN in refining the γ-austenite in AM-fabricated 316 stainless steel and its corresponding effect on the mechanical behaviour. Experimental results show that addition of 1 wt.% TiN nanoparticles led to complete columnar-to-equiaxed transition and significant refinement of the austenite grains to ∼2 µm in the 316 steel. Thermodynamic and kinetic simulations confirmed that, despite the rapid AM solidification, δ-ferrite is the primary solid phase during AM of the 316 steel and γ-austenite forms through subsequent peritectic reaction or direct transformation from the δ-ferrite. This implies that the TiN nanoparticles actually refined the δ-ferrite through promoting its heterogenous nucleation, which in turn refined the γ-austenite. This assumption is verified by the high grain refining efficiency of TiN nanoparticles in an AM-fabricated Fe-4 wt.%Si δ-ferrite alloy, in which δ-ferrite forms directly from the melt and is retained at room temperature. The grain refinement is attributed to the good atomic matching between δ-ferrite and TiN. Grain refinement in the 316 steel through 1 wt.% TiN inoculation not only eliminated the property anisotropy but also led to a high strain-hardening rate upon plastic deformation and thereby a superior strength-ductility synergy with yield strength of 561 MPa, tensile strength of 860 MPa and elongation of 48%.

A high-energy white synchrotron X-ray beam enables penetration of relatively thick and highly absorbing samples. At the P61A White Beam Engineering Materials Science Beamline, operated by Helmholtz-Zentrum Hereon at the PETRA III ring of the Deutsches Elektronen-Synchrotron (DESY), a tailored X-ray radiography system has been developed to perform in-situ X-ray imaging experiments at high temporal resolution, taking advantage of the unprecedented X-ray beam flux delivered by ten successive damping wigglers. The imaging system is equipped with an ultrahigh-speed camera (Phantom v2640) enabling acquisition rates up to 25 kHz at maximal resolution and binned mode. The camera is coupled with optical magnification (5x, 10x) and focusing lenses to enable imaging with a pixel size of 1,35 micrometre. The scintillator screens are housed in a special nitrogen gas cooling environment to withstand the heat load induced by the beam, allowing spatial resolution to be optimized down to few micrometres. We present the current state of the system development, implementation and first results of in situ investigations, especially of the electron beam powder bed fusion (PBF-EB) process, where the details of the mechanism of crack and pore formation during processing of different powder materials, e.g. steels and Ni-based alloys, is not yet known.

An electron beam powder bed fusion (EPBF) printability study of a medium-C hot-work tool steel with focus on part density and surface roughness was performed using three different powder particle size distributions (PSDs) of 45–105 μm (typical for EPBF), 20–60 μm (typical for laser beam powder bed fusion), and a 50–50 wt.% mixture of these two powders. First, acceptable process parameter windows were generated based on as-printed density for each PSD. Full density parts (at least 99.5% dense according to NIST) were produced using the 20–60 μm PSD and the mix PSD. Fifteen different contouring strategies were also tested for potential improvement of the as-printed side surface roughnesses, which ranged from 23.3 to 25.7 μm among the three PSDs. Side surface roughness as low as 13.8 μm was attained by using contouring strategies employing two contouring lines, which were typically observed to be more effective than one-line strategies. Overall, the 20–60 μm PSD was determined to convey a better as-printed build quality over a wider range of parameters without sacrificing process productivity.

The development of a sample environment for in situ x-ray characterization during metal Electron Beam Powder Bed Fusion (PBF-EB), called MiniMelt, is presented. The design considerations, the features of the equipment, and its implementation at the synchrotron facility PETRA III at Deutsches Elektronen-Synchrotron, Hamburg, Germany, are described. The equipment is based on the commercially available Freemelt ONE PBF-EB system but has been customized with a unique process chamber to enable real-time synchrotron measurements during the additive manufacturing process. Furthermore, a new unconfined powder bed design to replicate the conditions of the full-scale PBF-EB process is introduced. The first radiography (15 kHz) and diffraction (1 kHz) measurements of PBF-EB with a hot-work tool steel and a Ni-base superalloy, as well as bulk metal melting with the CMSX-4 alloy, using the sample environment are presented. MiniMelt enables time-resolved investigations of the dynamic phenomena taking place during multi-layer PBF-EB, facilitating process understanding and development of advanced process strategies and materials for PBF-EB.<br />

During fusion-based metal additive manufacturing, there is an inherent directionality in heat transfer, which leads to columnar grain growth. This may result in cracking and anisotropic mechanical properties in many alloy systems. Therefore, it is important to study the conditions under which columnar-to-equiaxed transition in grain structure occurs. The grain morphology is determined by several factors such as process conditions, local alloy composition, and number density of nucleating sites. In the present work, a model for simulating columnar-to-equiaxed transition is formulated, considering nucleating site size distribution, rapid solidification and constitutional undercooling in multicomponent alloys. Furthermore, the model is coupled with multicomponent Calphad-based thermodynamic and diffusion mobility descriptions. It is demonstrated that including the above aspects is important in accurately predicting the columnar-to-equiaxed transition by comparing with experimental data for an additively manufactured TiB2-reinforced AlSi10Mg alloy. The framework developed in this work may be used to predict columnar-to-equiaxed transition in additively manufactured technical alloys consisting of multiple elements.

One generic challenge in powder bed fusion - laser beam (PBF-LB) is the formation of epitaxially grown columnar grains, which lead to the undesirable anisotropy of mechanical properties. This anisotropy could be rectified by ex-situ or in-situ inoculation in some particular alloy systems. Understanding the grain refinement mechanism caused by in-situ inoculation is, however, complicated by remelting caused by the overlapping between neighboring scan tracks, when printing bulk samples using multiple tracks. Here in this work, a series of single tracks using ferritic stainless steels feedstock powder with and without pre-alloyed inoculant-forming elements, were printed at different scanning speeds to gain refreshed understanding on the mechanism of the observed grain refinement. Interestingly, the grain refinement in single tracks and bulk samples printed from the powder with and without inoculant-forming elements showed an opposite tendency. When using the powder without inoculant-forming elements, the single tracks showed large columnar grains, while the bulk samples showed even larger grain sizes; when using the powder with pre-alloyed inoculant-forming elements, fine equiaxed grains are found at the centers of the melt pools, surrounded by slightly coarser columnar grains at melt pool boundaries, in both single tracks and bulk samples. Noticeably, the mean grain sizes in the bulk samples are however smaller compared to those for single tracks because of remelting. Our work provides new insights on the grain refinement via in-situ inoculation during the PBF-LB process and highlights the importance of studying single tracks to better understand the melting and solidification behavior.

Solidification during fusion-based additive manufacturing (AM) is characterized by high solidification velocities and large thermal gradients, two factors that control the solidification mode of metals and alloys. Using two synchrotron-based, in situ setups, we perform high-speed X-ray diffraction measurements to investigate the impact of the solidification velocities and thermal gradients on the solidification mode of a hot-work tool steel over a wide range of thermal conditions of relevance to AM of metals. The solidification mode of primary delta-ferrite is observed at a cooling rate of 2.12 x 104 K/s, and at a higher cooling rate of 1.5 x 106 K/s, delta-ferrite is sup-pressed, and primary austenite is observed. The experimental thermal conditions are evaluated and linked to a Kurz-Giovanola-Trivedi (KGT) based solidification model. The modelling results show that the predictions from the multicomponent KGT model agree with the experimental observations. This work highlights the role of in situ XRD measurements for a fundamental understanding of the microstructure evolution during AM and for vali-dation of computational thermodynamics and kinetics models, facilitating parameter and alloy development for AM processes.