Publications

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Numerous projects are looking into distributing blends of natural gas and different amounts of gaseous hydrogen through the existing natural gas distribution system, which is widely composed of medium density polyethylene (MDPE) line pipes. The mechanical behavior of MDPE with hydrogen is not well understood; therefore, the effect of gaseous H2 on the mechanical properties of MDPE needs to be examined. In the current study, we investigate the effects of gaseous H2 on fatigue life and fracture resistance of MDPE in the presence of 3.4 MPa gaseous H2. Fatigue life tests were also conducted at a pressure of 21 MPa to investigate the effect of gas pressure on the fatigue behavior of MDPE. Results showed that the presence of gaseous H2 did not degrade the fatigue life nor the fracture resistance of MDPE. Additionally, based on the value of fracture resistance calculated, a failure assessment diagram was constructed to determine the applicability of using MDPE pipeline for distribution of gaseous H2. Even in the presence of a large internal crack, the failure assessment evaluation indicated that the MDPE pipes lie within the safe region under typical service conditions of natural gas distribution pipeline system.

Despite their susceptibility to hydrogen-assisted fracture, ferritic steels make up a large portion of the hydrogen infrastructure. It is impractical and too costly to build large scale components such as pipelines and pressure vessels out of more hydrogen-resistant materials such as austenitic stainless steels. Therefore, it is necessary to understand the fracture behavior of ferritic steels in high-pressure hydrogen environments to manage design margins and reduce costs. Quenched and tempered (Q&T) martensite is the predominant microstructure of high-pressure hydrogen pressure vessels, and higher strength grades of this steel type are more susceptible to hydrogen degradation than lower strength grades. In this study, a single heat of 4340 alloy was heat treated to develop alternative microstructures for evaluation of fracture resistance in hydrogen gas. Fracture tests of several microstructures, such as lower bainite and upper bainite with similar strength to the baseline Q&T martensite, were tested at 21 and 105 MPa H2. Despite a higher MnS inclusion content in the tested 4340 alloy which reduced the fracture toughness in air, the fracture behavior in hydrogen gas fit a similar trend to other previously tested Q&T martensitic steels. The lower bainite microstructure performed similar to the Q&T martensite, whereas the upper bainite microstructure performed slightly worse. In this paper, we extend the range of high-strength microstructures evaluated for hydrogen-assisted fracture beyond conventional Q&T martensitic steels.

Type 2 high-pressure hydrogen vessels for storage at hydrogen refueling stations are designed assuming a predefined operational pressure cycle and targeted autofrettage conditions. However, the resulting finite life depends significantly on variables associated with the autofrettage process and the pressure cycles actually realized during service, which many times are not to the full range of the design. Clear guidance for cycle counting is lacking, therefore industry often defaults to counting every repressurization as a full range pressure cycle, which is an overly conservative approach. In-service pressure cycles used to predict the growth of cracks in operational pressure vessels results in significantly longer life, since most in-service pressure cycles are only a fraction of the full design pressure range. Fatigue crack growth rates can vary widely for a given pressure range depending on the details of the residual strains imparted during the autofrettage process because of their influence on crack driving forces. Small changes in variables associated with the autofrettage process, e.g., the target autofrettage overburden pressure, can result in large changes in the residual stress profile leading to possibly degraded fatigue life. In this paper, computational simulation was used for sensitivity studies to evaluate the effect of both operating conditions and autofrettage conditions on fatigue life for Type 2 highpressure hydrogen vessels. The analysis in this paper explores these sensitivities, and the results are used to provide guidance on cycle counting. In particular, we identify the pressure cycle ranges that can be ignored over the life of the vessel as having negligible effect on fatigue life. This study also examines the sensitivity of design life to the autofrettage process and the impact on life if the targeted residual strain is not achieved during manufacturing.

High pressure hydrogen storage vessels are frequently retired upon reaching their designed number of pressure cycles, even in cases where the in-use pressure cycles are significantly less severe than the design pressure cycle. One method for extending the life of hydrogen vessels is recertification through non-destructive evaluation (NDE); however, NDE techniques are frequently evaluated with machined defects in test samples rather than fatigue cracks which occur during pressure cycling and may be more difficult to detect. In this paper, 50 mm wide ring sections (called C-rings, since they represent slightly more than half the circumference) were extracted from pressure vessels and mechanically cycled to establish fatigue cracks. Sub-millimeter starter notches were machined, via plunge electrical discharge machining (EDM), to control the location of crack initiation. Crack growth was monitored via direct current potential difference (DCPD) and backface strain gauges, both of which were shown to be good indicators for crack propagation. The C-ring geometry and fatigue crack growth were modeled to demonstrate the ability to monitor/control the crack length and area, which can be used to develop calibration samples of varying crack depth for NDE techniques. Additionally, this sample is intended to evaluate the influence of residual stresses on the sensitivity of NDE techniques, such as the design stresses in autofrettaged vessels.

High strength austenite-ferrite duplex stainless steels are a potential alternative to austenitic stainless steels for components in hydrogen gas storage systems. Since these components experience cyclic loading from frequent pressurization and depressurization, the effect of hydrogen on the fatigue behavior of duplex stainless steel must be understood. To determine the influence of hydrogen on fatigue crack initiation and fatigue life of a 255 super duplex stainless steel, circumferentially notched tensile (CNT) specimens were fatigue tested in the as-received condition in air, with pre-charged internal hydrogen in air, and in the as-received condition in high pressure hydrogen gas. The direct current potential difference (DCPD) method was used to detect crack initiation so that S-N curves could be produced for both (i) cycles to crack initiation and (ii) cycles to failure. An electropolished CNT specimen was also cycled in the as-received and hydrogen pre-charged conditions but interrupted just after crack initiation. The microstructural locations of small fatigue cracks were then identified with scanning electron microscopy and electron backscatter diffraction (EBSD). High pressure hydrogen gas and pre-charged hydrogen decreased the fatigue life of 255 duplex stainless steel by a nearly identical amount. The effects of hydrogen on fatigue crack initiation and fatigue life of 255 duplex stainless steel are discussed and compared to austenitic stainless steels.

Decarbonizing natural gas networks is a challenging enterprise. Replacing natural gas with renewable hydrogen is one option under global consideration to decarbonize heating, power and residential uses of natural gas. Hydrogen is known to degrade fatigue and fracture properties of structural steels, including pipeline steels. In this study, we describe environmental testing strategies aimed at generating baseline fatigue and fracture trends with efficient use of testing resources. For example, by controlling the stress intensity factor (K) in both K-increasing and K-decreasing modes, fatigue crack growth can be measured for multiple load ratios with a single specimen. Additionally, tests can be designed such that fracture tests can be performed at the conclusion of the fatigue crack growth test, further reducing the resources needed to evaluate the fracture mechanics parameters utilized in design. These testing strategies are employed to establish the fatigue crack growth behavior and fracture resistance of API grade steels in gaseous hydrogen environments. In particular, we explore the effects of load ratio and hydrogen partial pressure on the baseline fatigue and fracture trends of line pipe steels in gaseous hydrogen. These data are then used to test the applicability of a simple, universal fatigue crack growth model that accounts for both load ratio and hydrogen partial pressure. The appropriateness of this model for use as an upper bound fatigue crack growth is discussed.

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Austenitic stainless steels are the standard materials for containment of hydrogen and tritium because of their resistance to mechanical property degradation in those environments. The mechanical performance of the primary containment material is critical for tritium handling, processing, and storage, thus comprehensive understanding of the processes of tritium embrittlement is an enabling capability for fusion energy. This work describes the investigation of the effects of low levels of tritium-decay-helium ingrowth on 304 L tubes. Long-term aging with tritium leads to high helium contents in austenitic stainless steels and can reduce fracture toughness by 95 %, but the details of behavior at low helium contents are not as well characterized. Here, we present results from tensile testing of tritium pre-charged 304 L tube specimens with a variety of starting microstructures that all contain a low level of helium. The results of the tritium exposed-and-aged materials are compared to previously reported results on similar specimens tested in an unexposed condition as well as the hydrogen precharged condition. Tritium precharging and aging for a short duration resulted in increased yield strengths, ultimate tensile strengths and slightly increased elongation to failure, comparable to higher concentrations of hydrogen precharging.

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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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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.

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.

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.

High pressure Type 2 hoop-wrapped, thick-walled vessels are commonly used at hydrogen refueling stations. Vessels installed at stations circa 2010 are now reaching their design cycle limit and are being retired, which is the motivation for exploring life extension opportunities. The number of design cycles is based on a fatigue life calculation using a fracture mechanics assessment according to ASME Section VIII, Division 3, which assumes each cycle is the full pressure range identified in the User's Design Specification for a given pressure vessel design; however, assessment of service data reveals that the actual pressure cycles are more conservative than the design specification. A case study was performed in which in-service pressure cycles were used to re-calculate the design cycles. It was found that less than 1% of the allowable crack extension was consumed when crack growth was assessed using in-service design pressures compared to the original design fatigue life from 2010. Additionally, design cycles were assessed on the 2010 era vessels based on design curves from the recently approved ASME Code Case 2938, which were based on fatigue crack growth rate relationships over a broader range of K. Using the Code Case 2938 design curves yielded nearly 2.7 times greater design cycles compared to the 2010 vessel original design basis. The benefits of using inservice pressure cycles to assess the design life and the implications of using the design curves in Code Case 2938 are discussed in detail in this paper.

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