Publications

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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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The Enhanced Surveillance Sub-program has an annual NNSA requirement to submit a comprehensive report on all our fiscal year activities right after the start of the next calendar year. As most of you know, we collate all of our PI task submissions into a single volume that we send to NNSA, our customers, and use for other programmatic purposes. The functional objective of this report is to formally document the purpose, status, and accomplishments and impacts of all our work. For your specific submission, please follow the instructions described below and use the template provided. These are essentially the same as was used last year. We recognize this report may also include information on specific age-related findings that you will provide again in a few months as input to the Stockpile Annual Assessment process (e.g., in the submittal of your Component Assessment Report). However, the related content of your ES AR input should provide an excellent foundation that can simply be updated as needed for your Annual Assessment input.

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.

The objective of this work was twofold: (1) measure reliable fatigue crack growth relationships for X65 steel and its girth weld in high-pressure hydrogen gas to enable structural integrity assessments of hydrogen pipelines, and (2) evaluate the hydrogen accelerated fatigue crack growth susceptibility of the weld fusion zone and heat-affected zone relative to the base metal. Fatigue crack growth relationships (da/dN versus ΔK) were measured for girth welded X65 pipeline steel in high pressure hydrogen gas (21 MPa) and in air. Hydrogen assisted fatigue crack growth was observed for the base metal (BM), fusion zone (FZ), and heat-affected zone (HAZ), and was manifested through crack growth rates reaching nearly an order of magnitude acceleration over rates in air. At higher ΔK values, crack growth rates of BM, FZ, and HAZ were coincident; however, at lower ΔK, the fatigue crack growth relationships exhibited some divergence with the fusion zone having the highest crack growth rates. These relative fatigue crack growth rates in the BM, FZ, and HAZ were provisional, however, since both crack closure and residual stress contributed to the crack-tip driving force in specimens extracted from the HAZ. Despite the relatively high applied R-ratio (R = 0.5), crack closure was detected in the heat affected zone tests, in contrast to the absence of crack closure in the base metal tests. Crack closure corrections were performed using the adjusted compliance ratio method and the effect of residual stress on Kmax was determined by the crack-compliance method. Crack-tip driving forces that account for closure and residual stress effects were quantified as a weighted function of ΔK and Kmax (i.e., Knorm), and the resulting da/dN versus Knorm relationships showed that the HAZ exhibited higher hydrogen accelerated fatigue crack growth rates than the BM at lower Knorm values.

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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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The objective of this study was to explore an approach for measuring fatigue crack growth rates (da/dN) for Cr-Mo pressure vessel steels in high-pressure hydrogen gas over a broad cyclic stress intensity factor (ΔK) range while limiting test duration, which could serve as an alternative to the method prescribed in ASME BPVC VIII-3, Article KD-10. Fatigue crack growth rates were measured for SA-372 Grade J and 34CrMo4 steels in hydrogen gas as a function of ΔK, loadcycle frequency (f), and gas pressure. The da/dN vs. ΔK relationships measured for the Cr-Mo steels in hydrogen gas at 10 Hz indicate that capturing data at lower ΔK is valuable when these relationships serve as inputs into design-life analyses of hydrogen pressure vessels, since in this ΔK range crack growth rates in hydrogen gas approach rates in air. The da/dN vs. f data measured for the Cr-Mo steels in hydrogen gas at selected constant-ΔK levels demonstrate that crack growth rates at 10 Hz do not represent upper-bound behavior, since da/dN generally increases as f decreases. Consequently, although fatigue crack growth testing at 10 Hz can efficiently measure da/dN over a wide ΔK range, these da/dN vs. ΔK relationships at 10 Hz cannot be considered reliable inputs into design-life analyses. A possible hybrid approach to efficiently establishing the fatigue crack growth rate relationship in hydrogen gas without compromising data quality is to measure the da/dN vs. ΔK relationship at 10 Hz and then apply a correction based on the da/dN vs. f data. The reliability of such a hybrid approach depends on adequacy of the da/dN vs. f data, i.e., the data are measured at appropriate constant-ΔK levels and the data include upper-bound crack growth rates.

We measured the hydrogen-assisted fatigue crack growth rates (da/dN) for SA516 Grade 70 steel as a function of stress-intensity factor range (ΔK) and load-cycle frequency to provide life-prediction data relevant to pressure swing adsorber (PSA) vessels. For ΔK values up to 18.5 MPa m^1/2, the baseline da/dN versus ΔK relationship measured at 1Hz in 2.8 MPa hydrogen gas represents an upper bound with respect to crack growth rates measured at lower frequency. However, at higher ΔK values, we found that the baseline da/dN data had to be corrected to account for modestly higher crack growth rates at the lower frequencies relevant to PSA vessel operation.

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.

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Carbon-manganese steels are candidates for the structural materials in hydrogen gas pipelines; however, it is well known that these steels are susceptible to hydrogen embrittlement. Decades of research and industrial experience have established that hydrogen embrittlement compromises the structural integrity of steel components. This experience has also helped identify the failure modes that can operate in hydrogen containment structures. As a result, there are tangible ideas for managing hydrogen embrittlement in steels and quantifying safety margins for steel hydrogen containment structures. For example, fatigue crack growth aided by hydrogen embrittlement is a well-established failure mode for steel hydrogen containment structures subjected to pressure cycling. This pressure cycling represents one of the key differences in operating conditions between current hydrogen pipelines and those anticipated in a hydrogen delivery infrastructure. Applying structural integrity models in design codes coupled with measurement of relevant material properties allows quantification of the reliability/integrity of steel hydrogen pipelines subjected to pressure cycling. Furthermore, application of these structural integrity models is aided by the development of physics-based predictive models, which provide important insights such as the effects of microstructure on hydrogen-assisted fatigue crack growth. Successful implementation of these structural integrity and physics-based models enhances confidence in the design codes and enables decisions about materials selection and operating conditions for reliable and efficient steel hydrogen pipelines.

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The US Department of Energy (DOE) Energy Efficiency and Renewable Energy (EERE) Office of Fuel Cell Technologies Office (FCTO) is establishing the Hydrogen Fueling Infrastructure Research and Station Technology (H2FIRST) partnership, led by the National Renewable Energy Laboratory (NREL) and Sandia National Laboratories (SNL). FCTO is establishing this partnership and the associated capabilities in support of H2USA, the public/private partnership launched in 2013. The H2FIRST partnership provides the research and technology acceleration support to enable the widespread deployment of hydrogen infrastructure for the robust fueling of light-duty fuel cell electric vehicles (FCEV). H2FIRST will focus on improving private-sector economics, safety, availability and reliability, and consumer confidence for hydrogen fueling. This whitepaper outlines the goals, scope, activities associated with the H2FIRST partnership.

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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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Austenitic stainless steels have been extensively tested in hydrogen environments. These studies have identified the relative effects of numerous materials and environmental variables on hydrogen-assisted fracture. While there is concern that welds are more sensitive to environmental effects than the non-welded base material, in general, there have been relatively few studies of the effects of gaseous hydrogen on the fracture and fatigue resistance of welded microstructures. The majority of published studies have considered welds with geometries significantly different from the welds produced in assembling pressure manifolds. In this study, conventional, uniaxial tensile testing was used to characterize tubing of type 316L austenitic stainless steel with an outside diameter of 6.35 mm. Additionally, orbital tube welds were produced and tested to compare to the non-welded tubing. The effects of internal hydrogen were studied after saturating the tubes and orbital welds with hydrogen by exposure to high-pressure gaseous hydrogen at elevated temperature. The effects of hydrogen on the ductility of the tubing and the orbital tube welds were found to be similar to the effects observed in previous studies of type 316L austenitic stainless steels. Copyright © 2013 by ASME.

The objective of this work is to enable the safe design of hydrogen pressure vessels by measuring the fatigue crack growth rates of ASME code-qualified steels in high-pressure hydrogen gas. While a design-life calculation framework has recently been established for high-pressure hydrogen vessels, a material property database does not exist to support the analysis. This study addresses such voids in the database by measuring the fatigue crack growth rates for three heats of ASME SA-372 Grade J steel in 100 MPa hydrogen gas at two different load ratios (R). Results show that fatigue crack growth rates are similar for all three steel heats and are only a mild function of R. Hydrogen accelerates the fatigue crack growth rates of the steels by at least an order of magnitude relative to crack growth rates in inert environments. Despite such dramatic effects of hydrogen on the fatigue crack growth rates, measurement of these properties enables reliable definition of the design life of steel hydrogen containment vessels. Copyright © 2013 by ASME.

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Threshold stress intensity factors were measured in high-pressure hydrogen gas for a variety of low alloy ferritic steels using both constant crack opening displacement and rising crack opening displacement procedures. Thresholds for crack extension under rising displacement, K THi, for crack extension under constant displacement, KTHi*, and for crack arrest under constant displacement K THa, were identified. These values were not found to be equivalent, i.e. K THi < K THa < K THi*. The hydrogen assisted fracture mechanism was determined to be strain controlled for all of the alloys in this study, and the micromechanics of strain controlled fracture are used to explain the observed disparities between the different threshold measurements. K THa and K THi differ because the strain singularity of a stationary crack is stronger than that of a propagating crack; K THa must be larger than K THi to achieve equivalent crack tip strain at the same distance from the crack tip. Hydrogen interacts with deformation mechanisms, enhancing strain localization and consequently altering both the nucleation and growth stages of strain controlled fracture mechanisms. The timing of load application and hydrogen exposure, i.e., sequential for constant displacement tests and concurrent for rising displacement tests, leads to differences in the strain history relative to the environmental exposure history and promotes the disparity between K THi* and K THi. K THi is the only conservative measurement of fracture threshold among the methods presented here. © 2012 The Minerals, Metals & Materials Society and ASM International.

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Gaseous hydrogen is an alternative to petroleum-based fuels, but it is known to significantly reduce the fatigue and fracture resistance of steels. Steels are commonly used for containment and distribution of gaseous hydrogen, albeit under conservative operating conditions (i.e., large safety factors) to mitigate so-called gaseous hydrogen embrittlement. Economical methods of distributing gaseous hydrogen (such as using existing pipeline infrastructure) are necessary to make hydrogen fuel competitive with alternatives. the effects of gaseous hydrogen on fracture resistance and fatigue resistance of pipeline steels, however, has not been comprehensively evaluated and this data is necessary for structural integrity assessment in gaseous hydrogen environments. In addition, existing standardized test methods for environment assisted cracking under sustained load appear to be inadequate to characterize low-strength steels (such as pipeline steels) exposed to relevant gaseous hydrogen environments. In this study, the principles of fracture mechanics are used to compare the fracture and fatigue performance of two pipeline steels in high-purity gaseous hydrogen at two pressures: 5.5 MPa and 21 MPa. In particular, elastic-plastic fracture toughness and fatigue crack growth rates were measured using the compact tension geometry and a pressure vessel designed for testing materials while exposed to gaseous hydrogen. Copyright © 2010 by ASME.

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Fatigue crack growth rates and rising displacement fracture thresholds have been measured for a 4130X steel in 45 MPa hydrogen gas. the ratio of minimum to maximum load (R-ratio) and cyclic frequency was varied to assess the effects of these variables on fatigue crack growth rates. Decreasing frequency and increasing R were both found to increase crack growth rate, however, these variables are not independent of each other. Changing frequency from 0.1 Hz to 1 Hz reduced crack growth rates at R = 0.5, but had no effect at R = 0.1. When applied to a design life calculation for a steel pressure vessel consistent with a typical hydrogen trailer tube, the measured fatigue and fracture data predicted a re-inspection interval of nearly 29 years, consistent with the excellent service history of such vessels which have been in use for many years. Copyright © 2010 by ASME.

No concerns for Hydrogen-Enriched Compressed Natural gas (HCNG) in steel storage tanks if material strength is < 950 MPa. Recommend evaluating H{sub 2}-assisted fatigue cracking in higher strength steels at H{sub 2} partial pressure in blend. Limited fatigue testing on higher strength steel cylinders in H{sub 2} shows promising results. Impurities in Compressed Natural Gas (CNG) (e.g., CO) may provide extrinsic mechanism for mitigating H{sub 2}-assisted fatigue cracking in steel tanks.

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Threshold stress intensity factors were measured in high-pressure hydrogen gas for a variety of low alloy ferritic steels using both constant crack opening displacement and rising crack opening displacement procedures. The sustained load cracking procedures are generally consistent with those in ASME Article KD-10 of Section VIII Division 3 of the Boiler and Pressure Vessel Code, which was recently published to guide design of high-pressure hydrogen vessels. Three definitions of threshold were established for the two test methods: K{sub THi}* is the maximum applied stress intensity factor for which no crack extension was observed under constant displacement; K{sub THa} is the stress intensity factor at the arrest position for a crack that extended under constant displacement; and K{sub JH} is the stress intensity factor at the onset of crack extension under rising displacement. The apparent crack initiation threshold under constant displacement, K{sub THi}*, and the crack arrest threshold, K{sub THa}, were both found to be non-conservative due to the hydrogen exposure and crack-tip deformation histories associated with typical procedures for sustained-load cracking tests under constant displacement. In contrast, K{sub JH}, which is measured under concurrent rising displacement and hydrogen gas exposure, provides a more conservative hydrogen-assisted fracture threshold that is relevant to structural components in which sub-critical crack extension is driven by internal hydrogen gas pressure.

Carbon-manganese steels are candidates for the structural materials in hydrogen gas pipelines, however it is well known that these steels are susceptible to hydrogen embrittlement. Decades of research and industrial experience have established that hydrogen embrittlement compromises the structural integrity of steel components. This experience has also helped identify the failure modes that can operate in hydrogen containment structures. As a result, there are tangible ideas for managing hydrogen embrittement in steels and quantifying safety margins for steel hydrogen containment structures. For example, fatigue crack growth aided by hydrogen embrittlement is a key failure mode for steel hydrogen containment structures subjected to pressure cycling. Applying appropriate structural integrity models coupled with measurement of relevant material properties allows quantification of safety margins against fatigue crack growth in hydrogen containment structures. Furthermore, application of these structural integrity models is aided by the development of micromechanics models, which provide important insights such as the hydrogen distribution near defects in steel structures. The principal objective of this project is to enable application of structural integrity models to steel hydrogen pipelines. The new American Society of Mechanical Engineers (ASME) B31.12 design code for hydrogen pipelines includes a fracture mechanics-based design option, which requires material property inputs such as the threshold for rapid cracking and fatigue crack growth rate under cyclic loading. Thus, one focus of this project is to measure the rapid-cracking thresholds and fatigue crack growth rates of line pipe steels in high-pressure hydrogen gas. These properties must be measured for the base materials but more importantly for the welds, which are likely to be most vulnerable to hydrogen embrittlement. The measured properties can be evaluated by predicting the performance of the pipeline using a relevant structural integrity model, such as that in ASME B31.12. A second objective of this project is to enable development of micromechanics models of hydrogen embrittlement in pipeline steels. The focus of this effort is to establish physical models of hydrogen embrittlement in line pipe steels using evidence from analytical techniques such as electron microscopy. These physical models then serve as the framework for developing sophisticated finite-element models, which can provide quantitative insight into the micromechanical state near defects. Understanding the micromechanics of defects can ensure that structural integrity models are applied accurately and conservatively.

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Objectives are to enable development and implementation of codes and standards for H{sub 2} containment components: (1) Evaluate data on mechanical properties of materials in H{sub 2} gas - Technical Reference on Hydrogen Compatibility of Materials; (2) Generate new benchmark data on high-priority materials - Pressure vessel steels, stainless steels; and (3) Establish procedures for reliable materials testing - Sustained-load cracking, fatigue crack propagation. Summary of this presentation are: (1) Completed measurement of cracking thresholds (K{sub TH}) for Ni-Cr-Mo pressure vessel steels in high-pressure H{sub 2} gas - K{sub TH} measurements required in ASME Article KD-10 (2) Crack arrest test methods appear to yield non-conservative results compared to crack initiation test methods - (a) Proposal to insert crack initiation test methods in Article KD-10 will be presented to ASME Project Team on Hydrogen Tanks, and (b) Crack initiation methods require test apparatus designed for dynamic loading of specimens in H{sub 2} gas; and (3) Demonstrated ability to measure fatigue crack growth of pressure vessel steels in high-pressure H{sub 2} gas - (a) Fatigue crack growth data in H{sub 2} required in ASME Article KD-10, and (b) Test apparatus is one of few in U.S. or abroad for measuring fatigue crack growth in >100 MPa H{sub 2} gas.

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AISI 316 austenitic stainless steel is a preferred material of construction for valves, fittings, and other fluid system components for high-pressure gaseous hydrogen service. The interaction of hydrogen with stainless steel depends on the prevailing stress-state and the microstructural characteristics of a component's material of construction, among other variables. To evaluate the effects of geometrical stress-risers and two-phase microstructures on hydrogen-assisted fracture of AISI 316 stainless steel, smooth and notched tensile properties were measured for annealed material as well as for autogenously welded specimens after thermal precharging with hydrogen. The tensile ductility of welded microstructures is significantly reduced by hydrogen precharging, and the addition of a notch further degrades ductility. These observations are rationalized in terms of hydrogen-enhanced localized plasticity. Copyright © 2009 ASM International® All rights reserved.

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Non-destructive detection methods can reliably certify that gas transfer system (GTS) reservoirs do not have cracks larger than 5%-10% of the wall thickness. To determine the acceptability of a reservoir design, analysis must show that short cracks will not adversely affect the reservoir behavior. This is commonly done via calculation of the J-Integral, which represents the energetic driving force acting to propagate an existing crack in a continuous medium. J is then compared against a material's fracture toughness (J{sub c}) to determine whether crack propagation will occur. While the quantification of the J-Integral is well established for long cracks, its validity for short cracks is uncertain. This report presents the results from a Sandia National Laboratories project to evaluate a methodology for performing J-Integral evaluations in conjunction with its finite element analysis capabilities. Simulations were performed to verify the operation of a post-processing code (J3D) and to assess the accuracy of this code and our analysis tools against companion fracture experiments for 2- and 3-dimensional geometry specimens. Evaluation is done for specimens composed of 21-6-9 stainless steel, some of which were exposed to a hydrogen environment, for both long and short cracks.

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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