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Revealing hydrogen embrittlement mechanisms in steels is of great interest to scientists and engineers. Neutron radiography makes it possible to measure in-situ hydrogen diffusion with high spatial and temporal resolution at concentrations as low as 20 ppm. We compare hydrogen-charged specimens with hydrogen-free reference specimens and use calibration standards to normalize the hydrogen concentrations. This allows quantitative tracking of the hydrogen concentration evolution as a function of time, space and temperature. Furthermore, a view into the material with 'neutron eyes' facilitates the detection of cavities that contain molecular hydrogen.
Cold neutrons are predominantly scattered at hydrogen when penetrating hydrogen-charged samples, resulting in a high image contrast between hydrogen and e.g. iron. The used radiographic set-ups consist of a neutron source, state-of-the-art scintillator screens and digital cameras. This allows monitoring diffusive hydrogen fluxes two-dimensionally with 20s temporal resolution. Such hydrogen fluxes can be quantified by using standards with known hydrogen content and similar sample thickness.
Neutron tomography generates three-dimensional models of the hydrogen distribution in steel. Such models gain new insight for damage analysis by showing the hydrogen accumulations around cracks and by enabling the hydrogen gas pressure estimation inside cracks.
The capabilities and limitations, as well as perspectives of this method will be discussed and illustrated with help of selected examples.
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.
When in situ techniques became available in recent years this led to a breakthrough in accurately determining diffusion coefficients for liquid alloys. Here we discuss how neutron radiography can be used to measure chemical diffusion in a ternary AlCuAg alloy. Neutron radiography hereby gives complementary information to x-ray radiography used for measuring chemical diffusion and to quasielastic neutron scattering used mainly for determining self-diffusion. A novel Al2O3 based furnace that enables one to study diffusion processes by means of neutron radiography is discussed. A chemical diffusion coefficient of Ag against Al around the eutectic composition Al68.6Cu13.8Ag17.6 at.% was obtained. It is demonstrated that the in situ technique of neutron radiography is a powerful means to study mass transport properties in situ in binary and ternary alloys that show poor x-ray contrast.
In recent years, the optimization of the imaging stations at research reactors and especially the further development of the neutron detectors allowed the measurement of hydrogen distributions with increasing spatial and temporal resolution at lower detection limits at the same time. Hydrogen has compared to iron a high total neutron cross section, which allows with basic radiographic methods the visualization of hydrogen in two and three dimensions inside the microstructure of components. This enables the in situ measuring of hydrogen mass flows inside cm thick steel samples with a temporal resolution of 20 s as well as the quantitative measurement of hydrogen accumulations at the crack’s inner surfaces in hydrogen embrittled iron samples. For the first time, we detected directly gaseous hydrogen in the crack cavities and we could measure the gas pressure. This new quality of the information on a micrometer scale allows new insights for the analysis of damage mechanisms, e.g. of hydrogen embrittlement. Further, this method is non-destructive and provides local information in situ and in three dimensions with a spatial resolution of 20-30 µm, which is not accessible with common methods as e.g. thermal desorption spectroscopy.
In this contribution, we show examples that demonstrate the spatial and temporal resolution of the neutron radiography and tomography method in order to visualize and quantify hydrogen accumulations at cracks. The measurements were performed at the research reactor BER II of HZB in Berlin and at the FRM II reactor of the neutron source Heinz Maier-Leibnitz in Garching.
Neutron imaging has become a valuable tool for measuring hydrogen distributions qualitatively and quantitatively in metals. Hydrogen mass flow can be measured inside cm thick Steel samples with 10 s temporal resolution. Hydrogen accumulations around craclcs in embrittled iron samples can be visualized three-dimensionally. The gas pressure of hydrogen in crack cavities has been measured to be in the ränge of 5 MPa to 15 MPa. This quality of information allows new insights for the analysis of damage mechanisms on a micrometer scale, e.g., of hydrogen blistering. Further, this method is nondestructive and provides local information in situ and in three dimensions with a spatial resolution of 20 µm - 30 µm.
Neutron imaging is a valuable tool for measuring hydrogen distributions qualitatively and quantitatively in metals. Time-resolved neutron radiography allows to measure hydrogen mass flow inside cm thick steel samples with ~10 s temporal resolution. Hydrogen accumulations around cracks in embrittled iron samples can be visualized three-dimensionally by neutron tomography. This quality of information allows new insights for the analysis of damage mechanisms on a micrometer scale, e.g. of hydrogen blistering. Even the gas pressure of molecular hydrogen in crack cavities has been measured from tomographic reconstructions to be in the range of 5 MPa to 15 MPa for technical iron. Further, this method is non-destructive and provides local information in situ and in all three dimensions with a spatial resolution of 20 - 30 µm. The combination with other methods gives a new quality of information, e.g. of the hydrogen allocation on fractured surfaces.
Neutron imaging
(2016)
Neutron imaging methods are appropriate to investigate hydrogen distributions in several metallic systems. The large total neutron cross section of hydrogen compared to those of elements or isotopes, respectively, in usual structural materials like steels or zirconium alloys allows the detection even of small amounts of hydrogen in such materials. The dependence of the total macroscopic neutron cross section of the sample or component on the hydrogen concentration can be determined experimentally by means of calibration specimens with known hydrogen concentrations. Such a calibration allows for a full quantitative determination of the local hydrogen concentration with a spatial resolution better than 20 μm. Because neutron radiography is fast and non-destructive, in situ investigations of time-dependent processes like hydrogen absorption and release or hydrogen bulk diffusion can be performed. This chapter gives an introduction into the main neutron imaging methods, radiography and tomography, and gives as examples results of neutron imaging investigations of hydrogen in different steels and in zirconium alloys,respectively.
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.