Energy dispersive synchrotron diffraction for in-situ analyses of hydrogen behavior in steels
(2013)
The extent of hydrogen embrittlement phenomenon is dependent on the interaction of hydrogen with the material i.e. diffusion behavior, lattice distortions, phase transformations and residual stresses developments. For the better understanding of the hydrogen interaction with the metal, possibilities of performing in-situ observations of the mentioned factors has to be accomplished. The EDDI (Energy Dispersive Diffraction) beamline at the BESSY II facility in Berlin provides this possibility and was used in order to investigate the aspects of this phenomenon in in-situ scale.
The energy dispersive method entails a synchrotron X-ray white beam with a wide energy range (20–120 keV) which allows a fixed position of the sample and the detector, and combined with the high photons flux it allows a very short measurement time for obtaining a full scale X-Ray Diffraction patterns.
In this contribution, the successful usage of high energy X-rays, applied for the first time for hydrogen behavior observations, provided the ability for evaluating in-situ the hydrogen diffusion behavior and the hydrogen interaction with stresses fields in the material.
Steel samples were charged with hydrogen and examined by Synchrotron radiation.
Two different methods were used in this research; the first is diffusible hydrogen concentration evaluation extracted from the lattice distortions, i.e. changes of the lattice parameter. The second is calculation of the residual stresses present in the sample and the interaction of hydrogen with them, using the known sin2ψ method.
Hydrogen interaction with residual stresses in steel studied by synchrotron X-ray diffraction
(2014)
The residual stress state in a material has an important role in the mechanism of cracking, induced or assisted by hydrogen. In this contribution, the beamline EDDI in BESSY II instrument in Berlin was used in order to investigate the influence of hydrogen upon the residual stresses state existing in a Supermartensitic stainless steel sample. The method used for investigating the residual stresses is the sinus square ψ method. This method involves the usage of high energy X-ray diffraction in order to measure the residual stress state and magnitude. It was found that hydrogen presence has a significant influence upon the magnitude of the residual stresses, as its value decreases with high hydrogen content. This effect is reversible, as hydrogen desorbs from the sample the residual stress magnitude gains its initial value before hydrogen charging.
Hydrogen embrittlement (HE) is a widely known phenomenon and under investigation already for more than a century. This phenomenon, though thoroughly studied, is not yet completely understood, and so far, there are several suggested mechanisms that try to explain the occurrence of HE. One important factor of understanding the HE phenomenon and predicting hydrogen-assisted failure is the descent knowledge about the hydrogen transport behaviour in the material. Neutron radiography is a proven method for tracking hydrogen diffusion and it was applied successfully in various research studies. In the presented study, we examined the hydrogen effusion behaviour in duplex stainless steel by means of neutron radiography and calculated the effective diffusion coefficient from the obtained transmission images.
We investigated the hydrogen distribution spatially and temporally in technical iron at room temperature. Samples were charged electrochemically and subsequently analysed by means of neutron radiography and tomography. The radiographic images allowed for a time-resolved analysis of hydrogen fluxes. The three-dimensional distribution of hydrogen measured by neutron tomography delivered valuable information for the damage analysis of hydrogen-induced cracks. For the first time hydrogen concentration gradients inside the material could be detect directly together with the cracks. The neutron radiography and tomography results were gained at the Research Reactor BER II of the HZB in Berlin.
We investigated hydrogen embrittlement and blistering in electrochemically hydrogen-charged technical iron samples at room temperature. Hydrogen-stimulated cracks and blisters and the corresponding hydrogen distributions were observed by neutron tomography. Cold neutrons were provided by the research reactor BER II to picture the sample with a spatial resolution in the reconstructed three-dimensional model of ~25 µm. We made the unique observation that cracks were filled with molecular hydrogen and that cracks were surrounded by a 50 µm wide zone with a high hydrogen concentration. The zone contains up to ten times more hydrogen than the bulk material. The hydrogen enriched zone can be ascribed to a region of increased local defect density. Hydrogen also accumulated at the sample surface having the highest concentration at blistered areas. The surfaces of the brittle fractured cracks showed micropores visualized by scanning electron microscopy. The micropores were located at grain boundaries and were surrounded by stress fields detected by electron backscattered diffraction. The cracks clearly originated from the micropores.