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- Hydrogen (4)
- Hydrogen diffusion (4)
- Hydrogen embrittlement (4)
- Diffusion (3)
- Blister (2)
- Energy dispersive diffraction (2)
- In situ (2)
- Iron (2)
- Neutron radiography (2)
- Neutron tomography (2)
Neutron radiography and tomography have been used for a time resolved in situ analysis and a 3D mapping of hydrogen diffusion in iron and steel. Samples were electrochemically charged with hydrogen and afterwards neutron transmission images were taken. Hydrogen diffusion coefficients in duplex stainless steel were determined at 623 K by measuring and comparing the sample's mean intensity with a hydrogen-free reference sample and subsequent normalisation to standards with known hydrogen content. In technical iron and in supermartensitic stainless steel the hydrogen distributions have been investigated. The radiographic images in iron show blisters, cracks and the distribution of molecular hydrogen inside cracks. The analysis of the diffusion behaviour of hydrogen out of a blister illustrates the capabilities of the method with respect to time and spatial resolution. The neutron tomography of supermartensitic tensile stressed samples illustrates the capability to visualise hydrogen distributions three-dimensionally. -------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
On a utilisé la radiographie neutronique et la tomographie pour une analyse in situ à résolution temporelle et une cartographie 3D de la diffusion de l'hydrogène dans le fer et l'acier. On a chargé des échantillons par électrochimie avec de l'hydrogène et ensuite on a pris des images par émission de neutrons. On a déterminé les coefficients de diffusion de lhydrogène dans l'acier inoxydable duplex à 623 K en mesurant et en comparant l'intensité moyenne de l'échantillon avec un échantillon de référence sans hydrogène et une normalisation subséquente à des échantillons références à teneur connue en hydrogène. On a examiné la distribution d'hydrogène dans le fer technique et dans l'acier inoxydable supermartensitique. Les images radiographiques du fer montrent des soufflures, des fissures, et la distribution de l'hydrogène moléculaire à l'intérieur des fissures. L'analyse du comportement de diffusion de l'hydrogène hors d'une soufflure illustre les possibilités de la méthode par rapport à la résolution temporelle et spatiale. La tomographie neutronique des échantillons supermartensitiques chargés en traction illustre la capacité de visualiser les distributions d'hydrogène en trois dimensions.
Modern methods like carrier gas hot extraction enable the quantification of dissolved hydrogen as well as the determination of the hydrogen trapping and diffusion behavior. This method was applied in order to compare for the first time the hydrogen diffusion and trapping behavior in electrochemically charged and welded duplex stainless steel (1.4462). Characteristic extraction temperatures (400, 650, and 900 °C) were used to quantify the amounts of diffusible hydrogen and trapped hydrogen for the base material and the weld metal, and in order to calculate the effective diffusion coefficients corresponding to the specific temperature. The comparison of the charging methods showed that electrochemically charged samples have a higher content of diffusible hydrogen than the welded samples. In addition, the effusion times increase in welded samples, which indicate a higher amount of trapped hydrogen. In electrochemically charged weld samples, a significant lower concentration of hydrogen was determined than in the base material. In addition, the effective diffusion coefficients were calculated for every microstructure and charging method. It was found that the base material has a higher effective hydrogen diffusion coefficient than that of the weld metal. This effect is due to the tortuous path of hydrogen diffusion in the weld metal.
Neutron Bragg-edge imaging was applied for the visualization of a γ-Austenite to α'-martensite phase transformation. In the present study, a super martensitic
stainless steel sample was heated until complete austenitization and was subsequently cooled down to room temperature. The martensitic phase Transformation started at Ms = 190 °C. Using a monochromatic neutron beam with λ = 0.390 nm, the transmitted intensity was significantly reduced during cooling below Ms, since the emerging martensitic phase has a higher attenuation coefficient than the austenitic phase at this wavelength. The phase Transformation process was visualized by filming the transmission images from a scintillator screen with a CCD camera with a temporal resolution of 30 s and a spatial
resolution of 100 µm.
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.
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.
TRIP-steels offer a good combination between strength and ductility. Therefore TRIP-steels are widely used in the automobile industries. The aim of this work is to study the stability of involved phases during heating and to identify the kinetics of the occuring phase transformations. For that purpose, in-situ diffraction measurements, using high energy synchrotron radiation were conducted. The analysis revealed the decomposition of the metastable austenitic phase into carbide and ferrite along the heating process and the regeneration of the austenite by further heating of the sample.
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.
Neutron tomography has been applied to investigate the mechanism of hydrogen assisted cracking in technical iron and supermartensitic steel. Rectangular technical iron block samples showed blistering due to intense hydrogen charging and the tomographic method revealed in situ the spatial distribution of hydrogen and cracks. Hydrogen accumulated in a small region around cracks and the cracks are filled with hydrogen gas. Cracks close to the surface contained no hydrogen. Hydrogenous tensile test samples of supermartensitic steel were pulled until rupture and showed hydrogen accumulations at the notch base and in the plastically deformed region around the fracture surface.