Interaction of Hydrogen and Deformation in 316L Stainless Steel

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1 Proceedings of the SEM Annual Conference June 1-4, 2009 Albuquerque New Mexico USA 2009 Society for Experimental Mechanics Inc. Interaction of Hydrogen and Deformation in 316L Stainless Steel Bonnie R. Antoun and Bo Song Sandia National Laboratories, Livermore, CA, , USA ABSTRACT The presence of hydrogen in stainless steel materials has a significant embrittlement effect on the mechanical properties, resulting in severe reduction in the material s resistance to crack growth and fracture. A predictive capability to quantitatively assess hydrogen embrittlement effects on stainless steel materials is sought, but requires experimental discovery and determination of the interactions of hydrogen presence and mechanical deformation. INTRODUCTION Hydrogen and a surrounding stress field have complex interactions in stainless steel materials. Hydrogen affects the material plasticity, notch sensitivity and fracture characteristics [1,2]. To develop a mechanistic understanding of hydrogen embrittlement effects in stainless steels, 316L stainless steel specimens were charged in a high pressure hydrogen charging facility shown in Fig. 1. Identical specimens were also prepared that were not hydrogen charged to enable direct comparisons. Experiments were designed to determine specific theoretical parameters of a coupled hydrogen-dislocation plasticity model [3] and to determine the effect of hydrogen on yield and hardening behavior. Specimens were subjected to several types of mechanical experiments with variable loading parameters to fully characterize the materials and elucidate hydrogen effects through differences observed and measured in the material response as a function of hydrogen level. Additionally, we plan to correlate material microstructure with material properties as a function of hydrogen level. The experimental methods and results for the various experiments employed are described in this paper. Fig. 1 High pressure hydrogen charging facility showing pressurized vessels that 316L stainless steel specimens were contained in during long-term charging.

2 EXPERIMENTAL METHODS Over two hundred 3.8 mm (0.15 in.) diameter tensile specimens were machined for this study from 63.5 mm (2.5 in.) diameter 316L stainless steel bar. A portion of the specimens are shown in Fig. 2. The specimens were annealed at 1000 ºC and divided into three groups: annealed, low hydrogen level and high hydrogen level. The low and high hydrogen level specimens were charged in the hydrogen facility for a period of several weeks at 44.8 MPa (6500 psi) and 138 MPa (20,000 psi), respectively. This paper describes the first set of planned experiments used in determining the interaction of hydrogen level and mechanical deformation: tensile and stress relaxation experiments. Experiments were conducted as a function of hydrogen level as well as a function of several mechanical and thermal parameters including strain rate, strain level prior to relaxation and temperature. All experiments were conducted on an 89 kn (20 Kip) MTS servo-hydraulic test frame in true strain control using a 12.7 mm (0.5 in.) gage length extensometer. Experiments were conducted in a temperature-controlled environmental chamber at room temperature or at 54 ºC ( 65 ºF) using a solenoid-controlled supply of liquid nitrogen gas. Photographs during testing at the two temperatures are shown in Fig. 3. The strain rates studied were: 1x10-5 /s, 1x10-3 /s, 0.01/s and 0.1/s. Experiments were either conducted to failure, in the case of a tensile test, or were interrupted at a pre-determined Fig. 2 Photograph of some of the 3.8 mm (0.15 in.) diameter 316L stainless steel specimens. Fig. 3 Photographs of experiments conducted at room temperature and 54 ºC. strain level at which point stress relaxation was commenced, where the strain rate was set to zero. The pre-set strain levels chosen were the proportional limit, 0.2% yield offset and 10% strain. EXPERIMENTAL RESULTS The results for a room temperature tensile test of annealed material (no hydrogen charging) at 0.001/s strain rate are shown in Fig. 4 in terms of engineering stress versus engineering strain. Figure 5 shows the determination of the 0.2% yield offset strain value and the proportional limit strain value that is a parameter for the stress relaxation experiments. Figure 6 shows experiments conducted over the full range of strain rates, from 1x10-5 /s to 0.1/s, for annealed material. There is some test-to-test scatter related to the variation in grain size in the specimens. This was discovered as the data was being analyzed and was found to be related to a radial dependence of grain size in the 316L stainless steel bar stock, the tensile specimens were removed from two radii in the bar. However, the strain rate dependence of the material is still obvious. Figure 7 shows strain rate effects in the low hydrogen level material. Figure 8 shows a summary of the strain rate dependence for the two temperatures and material states. The material at both temperatures and hydrogen levels exhibits strain rate effects, the flow stress increases linearly with logarithm of strain rate and is dependent on the temperature and hydrogen level. However, the strain rate sensitivity is only slightly dependent on the hydrogen level or the temperature.

3 Fig. 4 Stress-strain curve for annealed, room temperature 316L stainless steel at 0.001/s strain rate. Fig. 5 Determination of 0.2% yield offset and proportional limit strain levels. Fig. 6 Stress-strain curves for annealed, room temperature 316L stainless steel. Fig. 7 Stress-strain curves for low hydrogen level, room temperature 316L stainless steel. Fig. 8 Flow stress versus logarithmic strain rate for 316L stainless steel.

4 The stress relaxation experiments were performed by conducting a tensile test at a given strain rate to one of the pre-determined strain levels, then changing the strain rate to zero and allowing the stress to relax. The specimen was allowed to relax until it reached its asymptotic limit. An example of stress relaxation experimental results for the annealed material is shown in Figs. 9 (stress versus strain) and 10 (stress versus time) for an initial strain rate of 0.01/s, conducted to a strain level of 10%. A summary of the relaxation time versus the logarithm of the strain rate is shown in Fig. 11. The stress relaxation time was significantly lower for the low hydrogen level material than the annealed material. The stress relaxation time also showed a significant strain rate and temperature effects. As expected, the effects of hydrogen level are much better indicated through the stress relaxation experiments than through the more common tensile experiments. Experimental work continues on the high hydrogen level material as well as other experiments and correlation with microstructure. Fig. 9 Stress relaxation experiment: room temperature, 0.01/s strain rate to 10% strain. Fig. 10 Stress relaxation time for room temperature, 0.01/s strain rate to 10% strain. Fig. 11 Relaxation time versus logarithmic strain rate for 316L stainless steel.

5 CONCLUSIONS Experimental methods have been developed that allow us to start understanding the complex interactions of hydrogen presence and deformation in stainless steels from a mechanics viewpoint. This brings us closer to developing a predictive capability to quantitatively assess hydrogen effects on materials of interest. We have been able to discover some key parameters that are very sensitive to hydrogen level and can be studied in a systematic manner. This work is continuing with future planned experiments that include small temperature excursion tests, thermal cycling tests, and a series of strain rate change tests. ACKNOWLEDGEMENTS Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy under Contract DE-ACO4-94AL REFERENCES 1. Antoun, B., Hong, S., Ohashi, Y., Brown, A., and Connelly, K., Experiments for Validation of Elastic- Plastic Fracture Modeling of Hydrogen Affected Materials, 2009 SEM Annual Conference and Exposition on Experimental and Applied Mechanics, Albuquerque, NM, June Nibur, K.A., Bahr, D.F., and Somerday, B.P., Hydrogen Effects on Dislocation Activity in Austenitic Stainless Steel, Acta Materialia, Vol. 54, Issue 10, June 2006, pp Bammann, D., Novak, P., Sofronis, P., and Somerday, B., A Coupled Dislocation-Hydrogen Based Model of Inelastic Deformation of Metals and Alloys, Proceedings ECF16, July 2006.

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