Publications

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This report serves as the proceedings of the Hydrogen Compatible Materials Workshop held virtually by Sandia National Laboratories on December 2-3, 2020. The purpose of the workshop was to assemble subject matter experts at Sandia and its national laboratory partners within the U.S. Department of Energy's (DOE) Hydrogen Materials Compatibility (H-Mat) Consortium with public and private stakeholders in the research, development and deployment of hydrogen technologies to discuss the topic of hydrogen compatible materials. This workshop was designed to build on past events and current research and development (R&D) efforts to develop a forward-looking vision that identifies gaps and challenges for the next decade. In particular, the workshop organizers sought to expand their understanding of hydrogen compatible materials needs for power, manufacturing and other industrial uses to enable deeper impact and widespread use of hydrogen while continuing to address open questions in hydrogen-powered transportation of concern to Original Equipment Manufacturers, hydrogen producers, materials & component suppliers and other private entities. The workshop was primarily organized as a series of panel-led discussions on the topics of hydrogen-enabled transportation, heating and power, and industrial uses. Each panel consisted of 2-3 subject matter experts who relayed their perspectives on a set of framing questions developed to facilitate discussion by the broader group of workshop participants. By the workshop's conclusion, the participants identified and prioritized a list of technical challenges for each panel topic where further R&D is warranted.

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The effects of internal hydrogen on the deformation microstructures of 304L austenitic stainless steel have been characterized using electron backscattered diffraction (EBSD), transmission Kikuchi diffraction (TKD), high-resolution scanning transmission electron microscopy (HRSTEM), and nanoprobe diffraction. Samples, both thermally precharged with hydrogen and without thermal precharging, were subjected to tensile deformation of 5 and 20 pct true strain followed by multiple microscopic interrogations. Internal hydrogen produced widespread stacking faults within the as-forged initially unstrained material. While planar deformation bands developed with tensile strain in both the hydrogen-precharged and non-precharged material, the character of these bands changed with the presence of internal hydrogen. As shown by nanobeam diffraction and HRSTEM observations, in the absence of internal hydrogen, the bands were predominantly composed of twins, whereas for samples deformed in the presence of internal hydrogen, ε-martensite became more pronounced and the density of deformation bands increased. For the 20 pct strain condition, α′-martensite was observed at the intersection of ε-martensite bands in hydrogen-precharged samples, whereas in non-precharged samples α′-martensite was only observed along grain boundaries. We hypothesize that the increased prevalence of α′-martensite is a secondary effect of increased ε-martensite and deformation band density due to internal hydrogen and is not a signature of internal hydrogen itself.

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Austenitic stainless steels are used extensively in harsh environments, including for high-pressure gaseous hydrogen service. However, the tensile ductility of this class of materials is very sensitive to materials and environmental variables. While tensile ductility is generally insufficient to qualify a material for hydrogen service, ductility is an effective tool to explore microstructural and environmental variables and their effects on hydrogen susceptibility, to inform understanding of the mechanisms of hydrogen effects in metals, and to provide insight to microstructural variables that may improve relative performance. In this study, hydrogen precharging was used to simulate high-pressure hydrogen environments to evaluate hydrogen effects on tensile properties. Several austenitic stainless steels were considered, including both metastable and stable alloys. Room temperature and subambient temperature tensile properties were evaluated with three different internal hydrogen contents for type 304L and 316L austenitic stainless steels and one hydrogen content for XM-11. Significant ductility loss was observed for both metastable and stable alloys, suggesting the stability of the austenitic phase is not sufficient to characterize the effects of hydrogen. Internal hydrogen does influence the character of deformation, which drives local damage accumulation and ultimately fracture for both metastable and stable alloys. While a quantitative description of hydrogen-assisted fracture in austenitic stainless steels remains elusive, these observations underscore the importance of the hydrogen-defect interactions and the accumulation of damage at deformation length scales.

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Fracture resistance of pipeline welds from a range of strength grades and welding techniques was measured in air and 21 MPa hydrogen gas, including electric resistance weld of X52, friction stir weld of X100 and gas metal arc welds (GMAW) of X52, X65 and X100. Welds exhibited a decrease in fracture resistance in hydrogen compared to complementary tests in air. A general trend was observed that fracture resistance in 21 MPa hydrogen gas decreased with increasing yield strength. To accommodate material constraints, two different fracture coupon geometries were used in this study, which were shown to yield similar fracture resistance values in air and 21 MPa hydrogen gas; values using different coupons resulted in less than 15% difference. In addition, fracture coupons were removed from controlled locations in select welds to examine the potential influence of orientation and residual stress. The two orientations examined in the X100 GMAW exhibited negligible differences in fracture resistance in air and, similarly, negligible differences in hydrogen. Residual stress exhibited a modest influence on fracture resistance; however, a consistent trend was not observed between tests in air and hydrogen, suggesting further studies are necessary to better understand the influence of residual stress. A comparison of welds and base metals tested in hydrogen gas showed similar susceptibility to hydrogen-assisted fracture. The overall dominant factor in determining the susceptibility to fracture resistance in hydrogen is the yield strength.

Internal hydrogen can influence the fatigue life, crack growth rate, and crack morphology of austenitic stainless steel, but little is known about the effect of internal hydrogen on fatigue crack initiation sites. To determine the effect of internal hydrogen on the microstructural fatigue crack initiation sites, the location of small fatigue cracks was evaluated with respect to the microstructural features in notched middle tension M(T) 316L specimens both with and without pre-charged hydrogen. The notches of the M(T) specimens were electropolished prior to fatigue testing to facilitate post-test analysis. Fatigue tests were performed with the same constant load amplitude and an R-ratio of 0.1 for specimens with and without internal hydrogen. The fatigue tests were interrupted after a minimal amount of cracking was detected using the direct current potential difference (DCPD) technique. The microstructural locations of the small fatigue cracks were then evaluated with scanning electron microscopy imaging and electron backscatter diffraction (EBSD). Several small transgranular fatigue cracks initiated in the notches of specimens both with and without internal hydrogen. These transgranular cracks always intersected grain boundaries, twin boundaries, and/or triple points indicating that these microstructural features are the critical locations for crack initiation. The transgranular cracks did not propagate along the prominent slip traces. There was no discernible effect of hydrogen on the microstructural sites of fatigue crack initiation in 316L.

Austenitic stainless steel microstructures produced by directed energy deposition (DED) are analogous to those developed during welding, particularly high energy density welding. To better understand microstructural development during DED, theories of microstructural evolution, which have been established to contextualize weld microstructures, are applied in this study to microstructural development in DED austenitic stainless steels. Phenomenological welding models that describe the development of oxide inclusions, compositional microsegregation, ferrite, matrix austenite grains, and dislocation substructures are utilized to clarify microstructural evolution during deposition of austenitic stainless steels. Two different alloys, 304L and 316L, are compared to demonstrate the broad applicability of this framework for understanding microstructural development during the DED process. Despite differences in grain morphology and solidification mode for these two alloys (which can be attributed to compositional differences), similar tensile properties are achieved. It is the fine-scale compositional segregation and dislocation structures that ultimately determine the strength of these materials. The evolution of microsegregation and dislocation structures is shown to be dependent on the rapid solidification and thermomechanical history of the DED processing method and not the composition of the starting material.

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Hydrogen additions to natural gas are being considered around the globe as a means to utilize existing infrastructure to distribute hydrogen. Hydrogen is known to enhance fatigue crack growth and reduce fracture resistance of structural steels used for pressure vessels, piping and pipelines. Most research has focused on high-pressure hydrogen environments for applications of storage (>100 MPa) and delivery (10-20 MPa) in the context of hydrogen fuel cell vehicles, which typically store hydrogen onboard at pressure of 70 MPa. In applications of blending hydrogen into natural gas, a wide range of hydrogen contents are being considered, typically in the range of 2-20%. In natural gas infrastructure, the pressure differs depending on location in the system (i.e., transmission systems are relatively high pressure compared to low-pressure distribution systems), thus the anticipated partial pressure of hydrogen can be less than an atmosphere or more than 10 MPa. In this report, it is shown that low partial pressure hydrogen has a very strong effect on fatigue and fracture behavior of infrastructure steels. While it is acknowledged that materials compatibility with hydrogen will be important for systems operating with high stresses, the effects of hydrogen do not seem to be a significant threat for systems operating at low pressure as in distribution infrastructure. In any case, system operators considering the addition of hydrogen to their network must carefully consider the structural performance of their system and the significant effects of hydrogen on structural integrity, as fatigue and fracture properties of all steels in the natural gas infrastructure will be degraded by hydrogen, even for partial pressure of hydrogen less than 0.1 MPa.

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