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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