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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Following the ASME codes, the design of pipelines and pressure vessels for transportation or storage of high-pressure hydrogen gas requires measurements of fatigue crack growth rates at design pressure. However, performing tests in high pressure hydrogen gas can be very costly as only a few laboratories have the unique capabilities. Recently, Code Case 2938 was accepted in ASME Boiler and Pressure Vessel Code (BPVC) VIII-3 allowing for design curves to be used in lieu of performing fatigue crack growth rate (da/dN vs. ?K) and fracture threshold (KIH) testing in hydrogen gas. The design curves were based on data generated at 100 MPa H2 on SA-372 and SA-723 grade steels; however, the data used to generate the design curves are limited to measurements of ?K values greater than 6 MPa m1/2. The design curves can be extrapolated to lower ?K (<6 MPa m1/2), but the threshold stress intensity factor (?Kth) has not been measured in hydrogen gas. In this work, decreasing ?K tests were performed at select hydrogen pressures to explore threshold (?Kth) for ferritic-based structural steels (e.g. pipelines and pressure vessels). The results were compared to decreasing ?K tests in air, showing that the fatigue crack growth rates in hydrogen gas appear to yield similar or even slightly lower da/dN values compared to the curves in air at low ?K values when tests were performed at stress ratios of 0.5 and 0.7. Correction for crack closure was implemented, which resulted in better agreement with the design curves and provide an upper bound throughout the entire ?K range, even as the crack growth rates approach ?Kth. This work gives further evidence of the utility of the design curves described in Code Case 2938 of the ASME BPVC VIII-3 for construction of high pressure hydrogen vessels.

Limited fatigue data exists for small-volume welded austenitic stainless steel components typically employed in hydrogen infrastructure due to the difficulty of testing these components with conventional specimen designs. To assess the fatigue performance of orbital tube welds of austenitic stainless steels, a hole-drilled tubular specimen was designed to produce a stress concentration in the center of the orbital weld. Fatigue life testing was performed on welded and non-welded 316L stainless steel hole-drilled tubular specimens, and the effects of hydrogen were evaluated by testing specimens with no added hydrogen and with internal hydrogen introduced through gaseous precharging. When accounting for the differences in flow stress caused by microstructural variations and the presence of internal hydrogen, the total fatigue life and fatigue crack initiation life of the welded and non-welded tubes were comparable and were reduced by internal hydrogen. In addition, the fatigue life results produced with the hole drilled tubular specimens were consistent with fatigue life data from circumferentially notched stainless steel specimens that have a similar elastic stress concentration factor. To better understand the mechanics of this specimen geometry, mechanics modeling was performed to compare the stress and strain distributions that develop at the stress concentration in the hole-drilled tubular and circumferentially notched specimens during fatigue cycling.

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Tensile properties, fatigue crack initiation, fatigue crack growth rate, and fatigue life are evaluated in 304L austenitic stainless steel fabricated by directed energy deposition (DED). Large lack of fusion (LoF) defects (often >1 mm in length) significantly reduce ultimate tensile strength and ductility, as well as accelerate fatigue crack initiation and reduce fatigue life. In comparison, small spherical defects (<100 μm in diameter) have less effect on tensile and fatigue properties. Fatigue crack growth rate is less severely affected by defects than other properties, showing only local acceleration in the proximity of LoF defects. Therefore, shorter fatigue life is attributed to the role of LoF defects on facilitating fatigue crack initiation and to a lesser extent fatigue crack propagation. Additionally, the fatigue life can be normalized for defects by considering their effect on ultimate tensile strength, suggesting that in the limit of low defect population, the fatigue strength of additively manufactured stainless steel is similar to conventional wrought materials.

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Microstructures and mechanical properties are evaluated in austenitic stainless steel structures fabricated by directed energy deposition (DED) considering the effects of applied loading orientation, build geometry, and distance from the deposition baseplate. Locations within an as-deposited build with different thermomechanical history display different yield strength, while those locations with similar history have approximately the same yield strength, regardless of test specimen orientation. Thermal expansion of deposited material near the baseplate is inhibited by the mechanical constraint imposed by the baseplate, promoting plastic deformation and producing a high density of dislocations. Concurrently, high initial cooling rates decrease away from the baseplate as the build is heated, causing an increased spacing of cellular solidification features. An analysis of strengthening mechanisms quantitatively established for the first time the important strengthening contribution of high dislocation densities in the materials (166–191 MPa) to yield strength that ranged from 438 to 553 MPa in the present DED fabricated structures. A newly adopted mechanistic relationship for microsegregation strengthening from the literature indicated an additional important contribution to strengthening (123–135 MPa) due to the cellular solidification features. These findings are corroborated by the measured evolution of microstructure and hardness caused by annealing the DED material. These results suggest that the mechanical properties of deposited austenitic stainless steels can be influenced by controlling thermomechanical history during the manufacturing process to alter the character of compositional microsegregation and the amount of induced plastic deformation.

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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.

The design of pressure vessels for high-pressure gaseous hydrogen service per ASME Boiler and Pressure Vessel Code Section VIII Division 3 requires measurement of fatigue crack growth rates in situ in gaseous hydrogen at the design pressure. These measurements are challenging and only a few laboratories in the world are equipped to make these measurements, especially in gaseous hydrogen at pressure in excess of 100 MPa. However, sufficient data is now available to show that common pressure vessel steels (e.g., SA-372 and SA-723) show similar fatigue crack growth rates when the maximum applied stress intensity factor is significantly less than the elastic-plastic fracture toughness. Indeed, the measured rates are sufficiently consistent that a master curve for fatigue crack growth in gaseous hydrogen can be established for steels with tensile strength less than 915 MPa. In this overview, published reports of fatigue crack growth rate data in gaseous hydrogen are reviewed. These data are used to formulate a two-part master curve for fatigue crack growth in high-pressure (106 MPa) gaseous hydrogen, following the classic power-law formulation for fatigue crack growth and a term that accounts for the loading ratio (R). The bounds on applicability of the master curve are discussed, including the relationship between hydrogen-assisted fracture and tensile strength of these steels. These data have been used in developing ASME VIII-3 Code Case 2938. Additionally, a phenomenological term for pressure can be added to the master curve and it is shown that the same master curve formulation captures the behavior of pressure vessel and pipeline steels at significantly lower pressure.

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This work proposes a finite element (FE) analysis workflow to simulate directed energy deposition (DED) additive manufacturing at a macroscopic length scale (i.e. part length scale) and to predict thermal conditions during manufacturing, as well as distortions, strength and residual stresses at the completion of manufacturing. The proposed analysis method incorporates a multi-step FE workflow to elucidate the thermal and mechanical responses in laser engineered net shaping (LENS) manufacturing. For each time step, a thermal element activation scheme captures the material deposition process. Then, activated elements and their associated geometry are analyzed first thermally for heat flow due to radiation, convection, and conduction, and then mechanically for the resulting stresses, displacements, and material property evolution. Simulations agree with experimentally measured in situ thermal measurements for simple cylindrical build geometries, as well as general trends of local hardness distribution and plastic strain accumulation (represented by relative distribution of geometrically necessary dislocations).

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Directed energy deposited (DED) and forged austenitic stainless steels possess dissimilar microstructures but can exhibit similar mechanical properties. In this study, annealing was used to evolve the microstructure of both conventional wrought and DED type 304L austenitic stainless steels, and significant differences were observed. In particular, the density of geometrically necessary dislocations and hardness were used to probe the evolution of the microstructure and properties. Forged type 304L exhibited the expected decrease in measured dislocation density and hardness as a function of annealing temperature. The more complex microstructure–property relationship observed in the DED type 304L material is attributed to compositional heterogeneities in the solidification microstructure.

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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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The capabilities in the Hydrogen Effects on Materials Laboratory (HEML) at Sandia National Laboratories and the related materials testing activities that support standards development and technology deployment are reviewed. The specialized systems in the HEML allow testing of structural materials under in-service conditions, such as hydrogen gas pressures up to 138 MPa, temperatures from ambient to 203 K, and cyclic mechanical loading. Examples of materials testing under hydrogen gas exposure featured in the HEML include stainless steels for fuel cell vehicle balance of plant components and Cr[sbnd]Mo steels for stationary seamless pressure vessels.

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Direct energy deposition (DED) is an additive manufacturing process that can produce complex near-net shape metallic components in a single manufacturing step. DED additive manufacturing has the potential to reduce feedstock material waste, streamline manufacturing chains, and enhance design flexibility. A major impediment to broader acceptance of DED technology is limited understanding of defect populations in the novel microstructures produced by DED and their relationship to process parameters and resultant mechanical properties. A design choice as simple as changing the build orientation has been observed to result in differences as great as ∼25% in yield strength for type 304L austenitic stainless steel deposited with otherwise identical deposition parameters. To better understand the role of build orientation and resultant defect populations on fatigue behavior in DED 304L, tension-tension fatigue testing has been performed on circumferentially notched cylindrical test specimens extracted from both vertical and horizontal orientations relative to the build direction. Notched fatigue behavior was found to be strongly influenced by the manufacturing defect populations of the material for different build orientations.

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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.

Circumferentially notched specimens of several austenitic stainless steel alloys subjected to positive load ratio, load-controlled fatigue have been cycled to failure in high pressure hydrogen gas. The number of cycles to failure for a given applied stress amplitude varies among the alloys tested indicating that control of fatigue life in hydrogen environments may be attained through informed alloy selection. The number of cycles to initiate a crack does not vary significantly among the alloys tested, however the total life to failure varied by over an order of magnitude. This difference in life is attributed to variations of the stress and strain fields ahead of the blunt notch. These fields are influenced by the strength and strain hardening characteristics of each alloy and they dictate the driving force for fatigue crack growth while the crack is small.

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Banded ferrite-pearlite X65 pipeline steel was tested in high pressure hydrogen gas to evaluate the effects of oriented pearlite on hydrogen assisted fatigue crack growth. Test specimens were oriented in the steel pipe such that cracks propagated either parallel or perpendicular to the banded pearlite. The ferrite-pearlite microstructure exhibited orientation dependent behavior in which fatigue crack growth rates were significantly lower for cracks oriented perpendicular to the banded pearlite compared to cracks oriented parallel to the bands. The reduction of hydrogen assisted fatigue crack growth across the banded pearlite is attributed to a combination of crack-tip branching and impeded hydrogen diffusion across the banded pearlite.

Polymeric materials have played a significant role in the adoption of a multi-materials approach towards the development of a safe and cost-effective solution for hydrogen fuel storage in Fuel Cell Vehicles (FCVs). Numerous studies exist with regards to the exposure of polymeric materials to gaseous hydrogen as applicable to the hydrogen infrastructure and related compression, storage, delivery, and dispensing operations of hydrogen at fueling stations. However, the behavior of these soft materials under high pressure hydrogen environments has not been well understood. This study involves exposure of select thermoplastic and elastomeric polymers to high pressure hydrogen (70-100 MPa) under static, isothermal, and isobaric conditions followed by characterization of physical properties and mechanical performance. Special attempt has been made to explain hydrogen effects on polymer properties in terms of polymer structure-property relationships, and also understand the influential role played by additives such as fillers, plasticizers, and processing AIDS in polymers exposed to hydrogen. Efforts have also been focused on deriving suitable conditions of static testing in high pressure hydrogen environments as a valuable part of developing a suitable test methodology for such systems. Understanding the relationships between polymer composition and microstructure, time of exposure, rate of depressurization, purge and exposure conditions, etc. in this simple study will help better define the test parameters for upcoming high pressure cycling experiments in hydrogen.

The degradation of stress-controlled fatigue-life (stress-life) of notched specimens was measured in the presence of internal and in external hydrogen for two strain-hardened austenitic stainless steels: 316L and 21Cr-6Ni-9Mn. To assess the sensitivity of fatigue performance to various hydrogen conditions fatigue tests were performed in four environments: (1) in air with no added hydrogen, (2) in air after hydrogen pre-charging to saturate the steel with internal hydrogen, and in external gaseous hydrogen at pressure of (3)10 MPa (1.45 ksi), or (4) 103 MPa (15 ksi). The fatigue performance of the strain-hardened 316L and 21Cr-6Ni-9Mn steels in air was indistinguishable for the tested conditions. Decreases in the fatigue-life at a given stress level were measured in the presence of hydrogen and depended on the hydrogen environment. Testing in 103 MPa (15 ksi) external gaseous hydrogen always resulted in a clear decrease in the fatigue-life at a given maximum stress. Alloy dependent reductions in the observed life at a given maximum stress were observed in the presence of internal hydrogen or in gaseous hydrogen at a pressure of 10 MPa (1.45 ksi). The measured fatigue-life of hydrogen pre-charged specimens was comparable to the life with no intentional hydrogen additions. Accounting for the increased flow stress resulting from the supersaturation of hydrogen after pre-charging results in consistency between the measured fatigue-life of the pre-charged condition and measurements in 103 MPa (15 ksi) external hydrogen. The current results indicate that internal hydrogen may be an efficient method to infer hydrogen-assisted fatigue degradation of stainless steels in high-pressure gaseous hydrogen.

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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This project addresses the following technical barriers from the Safety, Codes and Standards section of the 2012 Fuel Cell Technologies Office Multi-Year Research, Development and Demonstration Plan (section 3.8): (A) Safety data and information: limited access and availability (F) Enabling national and international markets requires consistent RCS (G) Insufficient technical data to revise standards.

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