Publications

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Additive Manufacturing (AM) offers the opportunity to transform design, manufacturing, and qualification with its unique capabilities. AM is a disruptive technology, allowing the capability to simultaneously create part and material while tightly controlling and monitoring the manufacturing process at the voxel level, with the inherent flexibility and agility in printing layer-by-layer. AM enables the possibility of measuring critical material and part parameters during manufacturing, thus changing the way we collect data, assess performance, and accept or qualify parts. It provides an opportunity to shift from the current iterative design-build-test qualification paradigm using traditional manufacturing processes to design-by-predictivity where requirements are addressed concurrently and rapidly. The new qualification paradigm driven by AM provides the opportunity to predict performance probabilistically, to optimally control the manufacturing process, and to implement accelerated cycles of learning. Exploiting these capabilities to realize a new uncertainty quantification-driven qualification that is rapid, flexible, and practical is the focus of this paper.

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Austenitic stainless steels are used extensively in hydrogen gas containment components due to their known resilience in hydrogen environments. Depending on the conditions, degradation can occur in austenitic stainless steels but typically the materials retain sufficient mechanical properties within such extreme environments. In many hydrogen containment applications, it is necessary or advantageous to join components through welding as it ensures minimal gas leakage, unlike mechanical fittings that can become leak paths that develop over time. Over the years many studies have focused on the mechanical behavior of austenitic stainless steels in hydrogen environments and determined their properties to be sufficient for most applications. However, significantly less data have been generated on austenitic stainless steel welds, which can exhibit more degradation than the base material. In this paper, we assess the trends observed in austenitic stainless steel welds tested in hydrogen. Experiments of welds including tensile and fracture toughness testing are assessed and comparisons to behavior of base metals are discussed.

Additive manufacturing (AM) offers the potential for increased design flexibility in the low volume production of complex engineering components for hydrogen service. However the suitability of AM materials for such extreme service environments remains to be evaluated. This work examines the effects of internal and external hydrogen on AM type 304L austenitic stainless steels fabricated via directed-energy deposition (DED) and powder bed fusion (PBF) processes. Under ambient test conditions, AM materials with minimal manufacturing defects exhibit excellent combinations of tensile strength, tensile ductility, and fatigue resistance. To probe the effects of extreme hydrogen environments on the AM materials, tensile and fatigue tests were performed after thermalprecharging in high pressure gaseous hydrogen (internal H) or in high pressure gaseous hydrogen (external H). Hydrogen appears to have a comparable influence on the AM 304L as in wrought materials, although the micromechanisms of tensile fracture and fatigue crack growth appear distinct. Specifically, microstructural characterization implicates the unique solidification microstructure of AM materials in the propagation of cracks under conditions of tensile fracture with hydrogen. These results highlight the need to establish comprehensive microstructure-property relationships for AM materials to ensure their suitability for use in extreme hydrogen environments.

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This SAND report fulfills the final report requirement for the Born Qualified Grand Challenge LDRD. Born Qualified was funded from FY16-FY18 with a total budget of ~$13M over the 3 years of funding. Overall 70+ staff, Post Docs, and students supported this project over its lifetime. The driver for Born Qualified was using Additive Manufacturing (AM) to change the qualification paradigm for low volume, high value, high consequence, complex parts that are common in high-risk industries such as ND, defense, energy, aerospace, and medical. AM offers the opportunity to transform design, manufacturing, and qualification with its unique capabilities. AM is a disruptive technology, allowing the capability to simultaneously create part and material while tightly controlling and monitoring the manufacturing process at the voxel level, with the inherent flexibility and agility in printing layer-by-layer. AM enables the possibility of measuring critical material and part parameters during manufacturing, thus changing the way we collect data, assess performance, and accept or qualify parts. It provides an opportunity to shift from the current iterative design-build-test qualification paradigm using traditional manufacturing processes to design-by-predictivity where requirements are addressed concurrently and rapidly. The new qualification paradigm driven by AM provides the opportunity to predict performance probabilistically, to optimally control the manufacturing process, and to implement accelerated cycles of learning. Exploiting these capabilities to realize a new uncertainty quantification-driven qualification that is rapid, flexible, and practical is the focus of this effort.

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Additive manufacturing (AM) includes a diverse suite of innovative manufacturing processes for producing near-net shape metallic components, typically from powder or wire. Reported mechanical properties of materials produced by these processes varies significantly and can usually be correlated with the relative porosity in the materials. In this study, relatively simple test components were manufactured from type 304L austenitic stainless steel by powder bed fusion (PBF). The quality of the components depends on a host of manufacturing parameters as well as the characteristics of the feedstock. In this study, the focus is the bulk material response. Tensile properties are reported for PBF type 304L produced in similar build geometries on two different machines with independent operators. Additionally, the effect of hydrogen on the tensile properties of the AM materials is evaluated. The goal of this study is to provide a benchmark for tensile properties of PBF 304L material in the context of wrought type 304L, and to make a preliminary assessment of the effects of hydrogen on tensile properties.

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Austenitic stainless steels are typically used in hydrogen environments due to their resistance to hydrogen embrittlement; however, the behavior of welds is not as well understood and can vary from wrought base materials due to chemical composition differences and the presence of ferrite in the fusion zone of the weld. Applications of welded austenitic stainless steels exposed to hydrogen are not limited to room temperature but also include sub-ambient environments, which can have an additional effect on the degradation. In this study, fracture thresholds were measured of three different austenitic stainless steel welds in the hydrogen-precharged condition. Forged 304L, 316L, and 21Cr-6Ni-9Mn stainless steels were gas tungsten arc welded with 308L filler metal and machined into 3-pt bend bars for fracture testing. Crack growth resistance (J-R) curves were measured of the three welds in the hydrogen-precharged condition at ambient (293 K) and sub-ambient (223 K) temperatures to determine the effects of temperature on fracture threshold. Fracture thresholds were determined using elastic-plastic fracture mechanics through development of J-R curves to determine the stress intensity factor following standard practice for determination of fracture toughness. Fracture threshold tests for the welds revealed significant susceptibility to subcritical cracking when tested in the hydrogen-precharged condition. The 21-6-9/308L and 304L/308L welds exhibited some variability in fracture thresholds that did not appear to trend with temperature, while the 316L/308L weld exhibited a reduction of over 50% in fracture threshold at the lower temperature compared to room temperature. In addition to fracture testing, mini-tensile specimens were extracted from the weld region and tested at 293 K and 223 K in the hydrogen-precharged condition. Hydrogen-precharging slightly increased the yield strength relative to the as-welded condition for all three welds at both temperatures. For all three welds, hydrogen reduced the total elongation by 3-11% at 293 K, whereas reductions in total elongation from 50-64% were observed at 223 K (relative to room temperature without hydrogen). The role of slip planarity on hydrogen-induced degradation of ductility and fracture resistance is discussed as a function of temperature, nickel content, and hydrogen. The fracture surfaces were examined to elucidate the observed differences and similarities in mechanical properties.

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This project was intended to enable SNL-CA to produce appropriate specimens of relevant stainless steels for testing and perform baseline testing of weld heat-affected zone and weld fusion zone. One of the key deliverables in this project was to establish a procedure for fracture testing stainless steel weld fusion zone and heat affected zones that were pre-charged with hydrogen. Following the establishment of the procedure, a round robin was planned between SNL-CA and SRNL to ensure testing consistency between laboratories. SNL-CA and SRNL would then develop a comprehensive test plan, which would include tritium exposures of several years at SRNL on samples delivered by SNL-CA. Testing would follow the procedures developed at SNL-CA. SRNL will also purchase tritium charging vessels to perform the tritium exposures. Although comprehensive understanding of isotope-induced fracture in GTS reservoir materials is a several year effort, the FY15 work would enabled us to jump-start the tests and initiate long-term tritium exposures to aid comprehensive future investigations. Development of a procedure and laboratory testing consistency between SNL-CA and SNRL ensures reliability in results as future evaluations are performed on aluminum alloys and potentially additively-manufactured components.

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Austenitic stainless steels such as 304L are frequently used for hydrogen service applications due to their excellent resistance to hydrogen embrittlement. However, welds in austenitic stainless steels often contain microstructures that are more susceptible to the presence of hydrogen. This study examines the tensile strength and ductility of a multi-pass gas tungsten arc weld made on 304L cross-rolled plate using 308L weld filler wire. Sub-sized tensile specimens were used to ensure the entire gage section of each tensile specimen consisted of weld metal. Specimens were extracted in both axial and transverse orientations, and at three different depths within the weld (root, center, and top). Yield strength decreased and ductility increased moving from the root to the top of the weld. A subset of specimens was precharged with hydrogen at 138 MPa (20,000 psi) and 300oC prior to testing, resulting in a uniform hydrogen concentration of 7700 appm. The presence of hydrogen resulted in a slight increase in yield and tensile strength and a roughly 50% decrease in tensile elongation and reduction in area, compared to the hydrogen-free properties.

Refueling infrastructure for use in gaseous hydrogen powered vehicles requires extensive manifolding for delivering the hydrogen from the stationary fuel storage at the refueling station to the vehicle as well as from the mobile storage on the vehicle to the fuel cell or combustion engine. Manifolds for gas handling often use welded construction (as opposed to compression fittings) to minimize gas leaks. Therefore, it is important to understand the effects of hydrogen on tubing and tubing welds. This paper provides a brief overview of on-going studies on the effects of hydrogen precharging on the tensile properties of austenitic stainless tubing and orbital tube welds.

The wedge geometry is a simple geometry for establishing a relatively constant gradient of strain in a forged part. The geometry is used to establish gradients in microstructure and strength as a function of strain, forging temperature, and quenching time after forging. This geometry has previously been used to benchmark predictions of strength and recrystallization using Sandias materials model for type 304L austenitic stainless steel. In this report, the processing conditions, in particular the times to forge and quench the forged parts, are summarized based on information recorded during forging on June 18, 2013 of the so-called wedge geometry from type 316L and 21Cr-6Ni-9Mn austenitic stainless steels.

Effects of low temperature on hydrogen-assisted cracking in 304L/308L austenitic stainless steel welds were investigated using elastic-plastic fracture mechanics methods. Thermally precharged hydrogen (140. wppm) decreased fracture toughness and altered fracture mechanisms at 293 and 223. K relative to hydrogen-free welds. At 293. K, hydrogen increased planar deformation in austenite, and microcracking of δ-ferrite governed crack paths. At 223. K, low temperature enabled hydrogen to exacerbate localized deformation, and microvoid formation, at austenite deformation band intersections near phase boundaries, dominated damage initiation; microcracking of ferrite did not contribute to crack growth. © 2013 Elsevier Ltd.

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Applications requiring the containment and transportation of hydrogen gas at pressures greater than 70 MPa are anticipated in the evolving hydrogen economy infrastructure. Since hydrogen is known to alter the mechanical properties of materials, data are needed to guide the selection of materials for structural components. The objective of this study is to characterize the role of yield strength, microstructural orientation, and small concentrations of ferrite on hydrogen-assisted fracture in two austenitic stainless steels: 21Cr-6Ni-9Mn (21-6-9) and 22Cr-13Ni-SMn (22-13-5). The testing methodology involves exposure of tensile specimens to high-pressure hydrogen gas at elevated temperature in order to precharge the specimens with hydrogen, and subsequently testing the specimens in laboratory air to measure strength and ductility. In all cases, the alloys remain ductile despite precharging to hydrogen concentrations of ∼1 at. %, as demonstrated by reduction in area values between 30% and 60% and fracture modes dominated by microvoid processes. Low concentrations of ferrite and moderate increases in yield strength do not exacerbate hydrogen-assisted fracture in 21-6-9 and 22-13-5, respectively. Microstructural orientation has a pronounced effect on ductility in 22-13-5 due to the presence of aligned second-phase particles. Copyright © 2008 by ASME.

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Tubular specimens of the nitrogen-strengthened alloy 21Cr-6Ni-9Mn were instrumented with thermocouples and inertia welded using a wide range of axial forces and kinetic energies. It was determined that a linear relationship exists between upset and kinetic energy for a given axial force. Furthermore, the peak temperatures are inversely related to the applied axial force. Microstructural characterization was performed using optical and electron microscopy techniques. Ferrite was observed locally at the weld interface, and it was determined that the width of the ferrite zone could vary widely depending on the process parameters. Electron backscattered diffraction analysis revealed that the ferrite and austenite at the weld interface exhibit the Kurdjumov-Sachs orientation relationship, and suggests that a very large amount of ferrite is present during the welding process that subsequently transforms to austenite during cooling. The fracture toughness of inertia welds thermally charged in gaseous hydrogen was also measured. It was found that the hydrogen-assisted fracture susceptibility of the inertia welds was greater than that of the base metal, but less than that of 21Cr-6Ni-9Mn gas tungsten arc welds. Copyright © 2006 ASM International®.

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The objective of this study was to quantify the hydrogen-assisted fracture susceptibility of gas-tungsten arc (GTA) welds in the nitrogen-strengthened, austenitic stainless steels 21Cr-6Ni-9Mn (21-6-9) and 22Cr-13Ni-5Mn (22-13-5). In addition, mechanisms of hydrogen-assisted fracture in the welds were identified using electron microscopy and finite-element modeling. Elastic-plastic fracture mechanics experiments were conducted on hydrogen-charged GTA welds at 25 C. Results showed that hydrogen dramatically lowered the fracture toughness from 412 kJ/m{sup 2} to 57 kJ/m{sup 2} in 21-6-9 welds and from 91 kJ/m{sup 2} to 26 kJ/m{sup 2} in 22-13-5 welds. Microscopy results suggested that hydrogen served two roles in the fracture of welds: it promoted the nucleation of microcracks along the dendritic structure and accelerated the link-up of microcracks by facilitating localized deformation. A continuum finite-element model was formulated to test the notion that hydrogen could facilitate localized deformation in the ligament between microcracks. On the assumption that hydrogen decreased local flow stress in accordance with the hydrogen-enhanced dislocation mobility argument, the finite-element results showed that deformation was localized in a narrow band between two parallel, overlapping microcracks. In contrast, in the absence of hydrogen, the finite-element results showed that deformation between microcracks was more uniformly distributed.

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