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Microstructural modification of additively manufactured metals by electropulsing

Additive Manufacturing

Noell, Philip N.; Rodelas, Jeffrey R.; Ghanbari, Zahra G.; Laursen, Christopher M.

Additive manufacturing (AM) promises rapid development cycles and fabrication of ready-to-use, geometrically-complex parts. The metallic parts produced by AM often contain highly non-equilibrium microstructures, e.g. chemical microsegregation and residual dislocation networks. While such microstructures can enhance some material properties, they are often undesirable. Many AM parts are thus heat-treated after fabrication, a process that significantly slows production. This study investigated if electropulsing, the process of sending high-current-density electrical pulses through a metallic part, could be used to modify the microstructures of AM 316 L stainless steel (SS) and AlSi10Mg parts fabricated by selective laser melting (SLM) more rapidly than thermal annealing. Electropulsing has shown promise as a rapid postprocessing method for materials fabricated using conventional methods, e.g. casting and rolling, but has never been applied to AM materials. For both the materials used in this study, as-fabricated SLM parts contained significant chemical heterogeneity, either chemical microsegregation (316 L SS) or a cellular interdendritic phase (AlSi10Mg). In both cases, annealing times on the order of hours at high homologous temperatures are necessary for homogenization. Using electropulsing, chemical microsegregation was eliminated in 316 L SS samples after 10, 16 ms electrical pulses. In AlSi10Mg parts, electropulsing produced spheroidized Si-rich particles after as few as 15, 16 ms electrical pulses with a corresponding increase in ductility. This study demonstrated that electropulsing can be used to modify the microstructures of AM metals.

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Automated high-throughput tensile testing reveals stochastic process parameter sensitivity

Materials Science and Engineering: A

Heckman, Nathan H.; Ivanoff, Thomas I.; Roach, Ashley M.; Jared, Bradley H.; Tung, Daniel J.; Brown-Shaklee, Harlan J.; Huber, Todd H.; Saiz, David J.; Koepke, Joshua R.; Rodelas, Jeffrey R.; Madison, Jonathan D.; Salzbrenner, Bradley S.; Swiler, Laura P.; Jones, Reese E.; Boyce, Brad B.

The mechanical properties of additively manufactured metals tend to show high variability, due largely to the stochastic nature of defect formation during the printing process. This study seeks to understand how automated high throughput testing can be utilized to understand the variable nature of additively manufactured metals at different print conditions, and to allow for statistically meaningful analysis. This is demonstrated by analyzing how different processing parameters, including laser power, scan velocity, and scan pattern, influence the tensile behavior of additively manufactured stainless steel 316L utilizing a newly developed automated test methodology. Microstructural characterization through computed tomography and electron backscatter diffraction is used to understand some of the observed trends in mechanical behavior. Specifically, grain size and morphology are shown to depend on processing parameters and influence the observed mechanical behavior. In the current study, laser-powder bed fusion, also known as selective laser melting or direct metal laser sintering, is shown to produce 316L over a wide processing range without substantial detrimental effect on the tensile properties. Ultimate tensile strengths above 600 MPa, which are greater than that for typical wrought annealed 316L with similar grain sizes, and elongations to failure greater than 40% were observed. It is demonstrated that this process has little sensitivity to minor intentional or unintentional variations in laser velocity and power.

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Achieving high strength and ductility in traditionally brittle soft magnetic intermetallics via additive manufacturing

Acta Materialia

Babuska, Tomas F.; Wilson, Mark A.; Johnson, Kyle J.; Whetten, Shaun R.; Curry, John C.; Rodelas, Jeffrey R.; Atkinson, Cooper; Lu, Ping L.; Chandross, M.; Krick, Brandon A.; Michael, Joseph R.; Argibay, Nicolas A.; Susan, D.F.; Kustas, Andrew K.

Intermetallic alloys possess exceptional soft magnetic properties, including high permeability, low coercivity, and high saturation induction, but exhibit poor mechanical properties that make them impractical to bulk process and use at ideal compositions. We used laser-based Additive Manufacturing to process traditionally brittle Fe–Co and Fe–Si alloys in bulk form without macroscopic defects and at near-ideal compositions for electromagnetic applications. The binary Fe–50Co, as a model material, demonstrated simultaneous high strength (600–700 MPa) and high ductility (35%) in tension, corresponding to a ∼300% increase in strength and an order-of-magnitude improvement in ductility relative to conventionally processed material. Atomic-scale toughening and strengthening mechanisms, based on engineered multiscale microstructures, are proposed to explain the unusual combination of mechanical properties. This work presents an instance in which metal Additive Manufacturing processes are enabling, rather than limiting, the development of higher-performance alloys.

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Microstructural Modification and Healing of Additively Manufactured Parts by Electropulsing

Noell, Philip N.; Rodelas, Jeffrey R.; Ghanbari, Zahra G.; Laursen, Christopher M.

For many applications, the promises of additive manufacturing (AM) of rapid development cycles and fabrication of ready-to-use, geometrically-complex parts cannot be realized because of cumbersome thermal postprocessing. This postprocessing is necessary when the non- equilibrium microstructures produced by AM lead to poor material properties. This study investigated if electropulsing, the process of sending high-current-density electrical pulses through a metallic part, could be used to modify the material properties of AM parts. This process has been used to modify conventional wrought materials but has never been applied to AM materials. Two representative AM materials were examined: 316L stainless steel and A1Si10Mg. Two hours of annealing are needed to remove chemical microsegregation in AM 316L; using electropulsing, this was accomplished in 200 seconds. The ductility of AlSil0Mg parts was increased above that of the as-built material using electropulsing. This study demonstrated that electropulsing can be used to modify the microstructures of AM metals. ACKNOWLEDGEMENTS The authors would like to acknowledge Jay Carroll for beneficial discussions and supplying material. Also, the authors would like to acknowledge Zachary Casias, Peter Duran, John Laing, Sara Dickens, Celedonio Jaramillo, Renae Hickman, and Christina Profazi for their exceptional experimental support.

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Evolution of 316L stainless steel feedstock due to laser powder bed fusion process

Additive Manufacturing

Heiden, Michael J.; Deibler, Lisa A.; Rodelas, Jeffrey R.; Koepke, Joshua R.; Tung, Daniel J.; Saiz, David J.; Jared, Bradley H.

Some of the primary barriers to widespread adoption of metal additive manufacturing (AM) are persistent defect formation in built components, high material costs, and lack of consistency in powder feedstock. To generate more reliable, complex-shaped metal parts, it is crucial to understand how feedstock properties change with reuse and how that affects build mechanical performance. Powder particles interacting with the energy source, yet not consolidated into an AM part can undergo a range of dynamic thermal interactions, resulting in variable particle behavior if reused. In this work, we present a systematic study of 316L powder properties from the virgin state through thirty powder reuses in the laser powder bed fusion process. Thirteen powder characteristics and the resulting AM build mechanical properties were investigated for both powder states. Results show greater variability in part ductility for the virgin state. The feedstock exhibited minor changes to size distribution, bulk composition, and hardness with reuse, but significant changes to particle morphology, microstructure, magnetic properties, surface composition, and oxide thickness. Additionally, sieved powder, along with resulting fume/condensate and recoil ejecta (spatter) properties were characterized. Formation mechanisms are proposed. It was discovered that spatter leads to formation of single crystal ferrite through large degrees of supercooling and massive solidification. Ferrite content and consequently magnetic susceptibility of the powder also increases with reuse, suggesting potential for magnetic separation as a refining technique for altered feedstock.

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The role of microstructure and surface finish on the corrosion of selective laser melted 304L

Journal of the Electrochemical Society

Schaller, Rebecca F.; Mishra, Ajit; Rodelas, Jeffrey R.; Taylor, Jason M.; Schindelholz, Eric J.

The corrosion behavior of selective laser melted (SLM) 304L was investigated and compared to conventional wrought 304L in aqueous chloride and acidic solutions. Through immersed electrochemical testing and exposure in acidic solutions, the SLM 304L exhibited superior pitting resistance in the polished state compared to wrought 304L. However, the surface condition of the SLM material had a great impact on its corrosion resistance, with the grit-blasted condition exhibiting severely diminished pitting resistance. Local scale, capillary micro-electrochemical and scanning electrochemical microscopy investigations, identified porosity as a contributing factor to decreased corrosion resistance. Preferential corrosion attack was not observed to be related to the characteristic underlying cellular microstructure produced through SLM processing. This study highlights the effects of SLM microstructural features on corrosion resistance, specifically the substantial influence of surface finish on SLM corrosion behavior and the need for development and optimization of processing techniques to improve surface finish.

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Extreme-Value Statistics Reveal Rare Failure-Critical Defects in Additive Manufacturing

Advanced Engineering Materials

Boyce, Brad B.; Salzbrenner, Bradley S.; Rodelas, Jeffrey R.; Swiler, Laura P.; Madison, Jonathan D.; Jared, Bradley H.; Shen, Yu L.

Additive manufacturing enables the rapid, cost effective production of customized structural components. To fully capitalize on the agility of additive manufacturing, it is necessary to develop complementary high-throughput materials evaluation techniques. In this study, over 1000 nominally identical tensile tests are used to explore the effect of process variability on the mechanical property distributions of a precipitation hardened stainless steel produced by a laser powder bed fusion process, also known as direct metal laser sintering or selective laser melting. With this large dataset, rare defects are revealed that affect only ≈2% of the population, stemming from a single build lot of material. The rare defects cause a substantial loss in ductility and are associated with an interconnected network of porosity. The adoption of streamlined test methods will be paramount to diagnosing and mitigating such dangerous anomalies in future structural components.

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Corrosion properties of powder bed fusion additively manufactured 17-4 PH stainless steel

Corrosion

Schaller, Rebecca S.; Taylor, Jason M.; Rodelas, Jeffrey R.; Schindelholz, Eric J.

The corrosion susceptibility of a laser powder bed fusion (LPBF) additively manufactured alloy, UNS S17400 (17-4 PH), was explored compared to conventional wrought material. Microstructural characteristics were characterized and related to corrosion behavior in quiescent, aqueous 0.6 M NaCl solutions. Electrochemical measurements demonstrated that the LPBF 17-4 PH alloy exhibited a reduced passivity range and active corrosion compared to its conventional wrought counterpart. A microelectrochemical cell was used to further understand the effects of the local scale and attributed the reduced corrosion resistance of the LPBF material to pores with diameters ≥50 μm.

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High-throughput stochastic tensile performance of additively manufactured stainless steel

Journal of Materials Processing Technology

Salzbrenner, Bradley S.; Rodelas, Jeffrey R.; Madison, Jonathan D.; Jared, Bradley H.; Swiler, Laura P.; Shen, Yu L.; Boyce, Brad B.

An adage within the Additive Manufacturing (AM) community is that “complexity is free”. Complicated geometric features that normally drive manufacturing cost and limit design options are not typically problematic in AM. While geometric complexity is usually viewed from the perspective of part design, this advantage of AM also opens up new options in rapid, efficient material property evaluation and qualification. In the current work, an array of 100 miniature tensile bars are produced and tested for a comparable cost and in comparable time to a few conventional tensile bars. With this technique, it is possible to evaluate the stochastic nature of mechanical behavior. The current study focuses on stochastic yield strength, ultimate strength, and ductility as measured by strain at failure (elongation). However, this method can be used to capture the statistical nature of many mechanical properties including the full stress-strain constitutive response, elastic modulus, work hardening, and fracture toughness. Moreover, the technique could extend to strain-rate and temperature dependent behavior. As a proof of concept, the technique is demonstrated on a precipitation hardened stainless steel alloy, commonly known as 17-4PH, produced by two commercial AM vendors using a laser powder bed fusion process, also commonly known as selective laser melting. Using two different commercial powder bed platforms, the vendors produced material that exhibited slightly lower strength and markedly lower ductility compared to wrought sheet. Moreover, the properties were much less repeatable in the AM materials as analyzed in the context of a Weibull distribution, and the properties did not consistently meet minimum allowable requirements for the alloy as established by AMS. The diminished, stochastic properties were examined in the context of major contributing factors such as surface roughness and internal lack-of-fusion porosity. This high-throughput capability is expected to be useful for follow-on extensive parametric studies of factors that affect the statistical reliability of AM components.

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Corrosion properties of powder bed fusion additively manufactured stainless steels

Materials Science and Technology Conference and Exhibition 2017, MS and T 2017

Schaller, Rebecca S.; Taylor, Jason M.; Rodelas, Jeffrey R.; Mishra, Ajit; Schindelholz, Eric J.

Metal additive manufacturing (AM) has recently become a desirable process for complex parts across a broad range of applications. However, AM materials often have a varied microstructure due to non-equilibrium solidification conditions. While some adjustments have been made in manufacturing to enhance mechanical traits, very little attention has been directed at understanding the corrosion properties of these materials. The microstructural characteristics of the AM materials may lead to reduction in the corrosion resistance of the AM alloys compared to their conventional counterparts. This presentation explores the corrosion susceptibility of AM stainless steels in aqueous sodium chloride environments as well as industry relevant solutions. Further detailed corrosion studies combined with microstructural characterization provide insight into the microstructural influences on corrosion.

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Laser Rewelding of 304L Stainless Steel

Maguire, Michael C.; Rodelas, Jeffrey R.

Laser welding of 304L stainless steel during component fabrication has been found to alter the chemical composition of the steel due to material evaporation. During repair or rework, or during potential reuse/ rewelding of certain components, the potential exists to alter the composition to the extent that the material becomes prone to solidification cracking. This work aims to characterize the extent of this susceptibility in order to make informed decisions regarding rewelding practice and base metal chemistry allowances.

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Defect Characterization for Material Assurance in Metal Additive Manufacturing (FY15-0664)

Salzbrenner, Bradley S.; Boyce, Brad B.; Jared, Bradley H.; Rodelas, Jeffrey R.; Laing, John R.

No industry-wide standards yet exist for minimum properties in additively manufactured (AM) metals. While AM alloys such as 17-4 precipitation hardened stainless steel have been shown to have average properties that can be comparable to wrought or cast product, they suffer from inconsistent performance. Variability in the feedstock powder, feature sizes, thermal history, and laser performance can lead to unpredictable surface finish, chemistry, phase content, and defects. To address this issue, rapid, efficient, high-throughput mechanical testing and data analysis was developed, providing profound statistical insight into the stochastic variability in properties. With this new approach, 1000’s of comprehensive tensile tests can be performed for the cost of 10’s of conventional tests. This new high-throughput approach provides a material qualification pathway that is commensurate with the quick turn-around benefit of AM.

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129 Results
129 Results