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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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.

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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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Objectives of the project include: Enable the use of high strength steel hydrogen pipelines, as significant cost savings can result by implementing high strength steels as compared to lower strength pipes. Demonstrate that girth welds in high-strength steel pipe exhibit fatigue performance similar to lower-strength steels in high-pressure hydrogen gas. Identify pathways for developing high-strength pipeline steels by establishing the relationship between microstructure constituents and hydrogen-accelerated fatigue crack growth (HA-FCG)

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The fatigue crack growth behavior of Ti–10V–2Fe–3Al in gaseous hydrogen (H2) was assessed through comparative experiments conducted in laboratory air and 8.3 MPa H2. The measured fatigue crack growth rate (da/dN) versus applied stress intensity factor range (ΔK) relationships and observed fracture morphologies for laboratory air and H2 were comparable up to ΔK ≈ 6.9 MPa√m, when tested at a load ratio of 0.1 and frequency of 10 Hz. At higher ΔK values, significant crack deflection and subsequent catastrophic failure occurred in the specimen tested in H2. This degradation was not observed in a specimen pre-exposed to 8.3 MPa H2 for 96 h and then immediately tested in laboratory air. X-ray diffraction of the failed H2-tested specimen revealed that the material remnants were predominantly composed of TiH2, suggesting that hydride formation was the catalyst for catastrophic failure in H2. The mechanistic implications of these results and their impact on current material compatibility assessments for Ti alloys in hydrogen service are then discussed.

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The effect of hydrogen (H) on the deformation behavior of Monel K-500 in various isothermal heat treatment conditions (non-aged, under-aged, peak-aged, and over-aged) was assessed via uniaxial mechanical testing. H-charged and non-charged specimens were strained to failure to facilitate a comparison of ductility, fracture surface morphology, strength, and work hardening behavior. For all examined heat treatment conditions, H charging leads to a significant reduction in ductility, which is accompanied by a consistent change in fracture surface morphology from ductile microvoid coalescence to brittle intergranular fracture. While H charging led to a systematic enhancement in the yield strength of all heat treatments, the three age-hardened conditions exhibited a more than 2-fold increase relative to the non-aged heat treatment. This suggests that H modifies the dislocation–precipitate interactions, which also manifest themselves through changes in work hardening metrics related to the dislocation storage and recovery rates. In particular, the H-charged peak-aged specimen exhibited a significant increase in initial hardening (dislocation storage) rate relative to the H-charged under-aged specimen. Transmission electron microscopy of these samples revealed the onset of widespread dislocation looping in the H-charged peak-aged sample, in addition to the planar slip bands characteristic of the non-charged condition. This result suggests that hydrogen induces the particle shearing-to-looping transition at smaller particle sizes. Possible mechanistic explanations for this observed behavior are presented.

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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.

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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.

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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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One of the most efficient methods for supplying gaseous hydrogen long distances is by using steel pipelines. However, steel pipelines exhibit accelerated fatigue crack growth rates in gaseous hydrogen relative to air. Despite conventional expectations that higher strength steels would be more susceptible to hydrogen embrittlement, recent testing on a variety of pipeline steel grades has shown a notable independence between strength and hydrogen assisted fatigue crack growth rate. It is thought that microstructure may play a more defining role than strength in determining the hydrogen susceptibility. Among the many factors that could affect hydrogen accelerated fatigue crack growth rates, this study was conducted with an emphasis on orientation dependence. The orientation dependence of toughness in hot rolled steels is a well-researched area; however, few studies have been conducted to reveal the relationship between fatigue crack growth rate in hydrogen and orientation. In this work, fatigue crack growth rates were measured in hydrogen for high strength steel pipeline with different orientations. A significant reduction in fatigue crack growth rates were measured when cracks propagated perpendicular to the rolling direction. A detailed microstructural investigation was performed, in an effort to understand the orientation dependence of fatigue crack growth rate performance of pipeline steels in hydrogen environments.

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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.

Friction stir welded steel pipelines were tested in high pressure hydrogen gas to examine the effects of hydrogen accelerated fatigue crack growth. Fatigue crack growth rate (da/dN) vs. stress-intensity factor range (ΔK) relationships were measured for an X52 friction stir welded pipe tested in 21 MPa hydrogen gas at a frequency of 1 Hz and R = 0.5. Tests were performed on three regions: base metal (BM), center of friction stir weld (FSW), and 15 mm off-center of the weld. For all three material regions, tests in hydrogen exhibited accelerated fatigue crack growth rates that exceeded an order of magnitude compared to companion tests in air. Among tests in hydrogen, fatigue crack growth rates were modestly higher in the FSW than the BM and 15 mm off-center tests. Select regions of the fracture surfaces associated with specified ΔK levels were examined which revealed intergranular fracture in the BM and 15 mm off-center specimens but an absence of intergranular features in the FSW specimens. The X52 friction stir weld and base metal tested in hydrogen exhibited fatigue crack growth rate relationships that are comparable to those for conventional arc welded steel pipeline of similar strength found in the literature.

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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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Fatigue crack growth rate (da/dN) versus stress intensity factor range (AK) relationships were measured for various grades of pipeline steel along with their respective welds in high pressure hydrogen. Tests were conducted in both 21 MPa hydrogen gas and a reference environment (e.g. air) at room temperature. Girth welds fabricated by arc welding and friction stir welding processes were examined in X65 and X52 pipeline grades, respectively. Results showed accelerated fatigue crack growth rates for all tests in hydrogen as compared to tests in air. Modestly higher hydrogen-assisted crack growth rates were observed in the welds as compared to their respective base metals. The arc weld and friction stir weld exhibited similar fatigue crack growth behavior suggesting similar sensitivity to hydrogen. A detailed study of microstructure and fractography was performed to identify relationships between microstructure constituents and hydrogen accelerated fatigue crack growth.

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 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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