Publications

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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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Current models for hydrogen embrittlement rely on adjustable parameters to correct for uncertainties in crack tip stress fields and subsequent H₂-concentrations. Techniques are needed to quantify these concentrations ahead of crack tips in mechanically loaded materials, providing data for model calibration and validation. The goal of this work was to establish advanced analytical techniques to detect and quantitatively measure hydrogen ahead of cracks in stressed solids. Two advanced analytical techniques, kelvin probe force microscopy (KPFM) and nuclear reaction analysis (NRA), were explored to evaluate the feasibility to provide qualitative and quantitative H₂-concentration fields in geometries designed to be 'loaded' while under observation. The feasibility of the KPFM technique at detecting hydrogen was evaluated using electrochemically precharged hydrogen as well as a mixed hydrogen gas atmosphere. The KPFM technique was able to detect the presence of elevated stress and hydrogen concentrations ahead of a tensile loaded crack tip. The results suggest that KPFM is a viable technique for qualitatively imaging changes in stress and hydrogen concentrations on the scale needed to inform predictive models. KPFM could be used to provide local stress and hydrogen variations associated with hydrogen traps or different phases which require sensitive measurements on the micron scale. NRA provided quantitative measurements of the hydrogen-isotope deuterium ahead of a tensile loaded notch, however, the vacancy formation due to the incident high energy He 3 beam overwhelmed stress-assisted enhancement of deuterium concentrations such that the effect of stress was overshadowed in this analysis. Modeling of the chemo- mechanical hydrogen concentration change was used to verify this observation.

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The objective of this project is to measure the hydrogen-affected fracture properties of structural welded metals exposed to hydrogen isotopes. The main goal of FY16 was to evaluate low-temperature effects on fracture properties of stainless steel welds pre-charged with hydrogen. Forged stainless steels consisting of 316L, 304L, and 21-6-9 welded with 308L filler metal were pre-charged and tested at 223 K at select displacement rates to evaluate fracture behavior over the lower STS temperature range. Reductions in fracture thresholds were observed for all stainless steel welds when samples were precharged with hydrogen; however, temperature effects were not observed in the 304L and 21-6-9 welds. Only 316L exhibited enhanced degradation at 223 K. In addition to fracture testing, tensile specimens were extracted from the weld region and tested at 296 K and 223 K in the hydrogen pre-charged condition. A slight increase in yield strength was measured in the pre-charged condition at 296K and 223 K for the three different welds. A reduction in total elongation of 3-11% was observed at 296 K, whereas reductions in total elongation from 50-64% were observed at 223 K. Microhardness and ferrite numbers were measured in the weld regions to try to elucidate the factors affecting fracture. Lastly, in collaboration with Savannah River National Laboratory (SRNL), weld and heat-affected zone bend specimens extracted from forged 304L and 21-6-9 stainless steel were supplied to SRNL and are in the final stages of sample preparation for subsequent tritium exposure, aging, and fracture testing. The collection of testing completed and planned between Sandia and SRNL contributes to the development of a comprehensive database of properties for materials as a function of hydrogen-isotope concentrations.

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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. In conclusion, 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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