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Gravity has significant effects on alloy solidification, primarily due to thermosolutal convection and solid phase buoyancy. Since 2004, the European Space Agency has been supporting investigation of these effects by promoting in situ X-ray monitoring of the solidification of aluminium alloys on microgravity platforms, on earth, and in periodically varying g conditions. The first microgravity experiment-investigating foaming of liquid metals - was performed on board a sounding rocket, in 2008. In 2012 the first ever X-ray-monitored solidification of a fully dense metallic alloy in space was achieved: the focus was columnar solidification of an Al-Cu alloy. This was followed in 2015 by a similar experiment, investigating equiaxed solidification. Ground reference experiments were completed in all cases. In addition, experiments have been performed on board parabolic flights-where the effects of varying gravity have been studied. We review here the technical and scientific progress to date, and outline future perspectives.
A x-ray radioscopy technique for measuring in situ chemical diffusion coefficients in metallic melts
is presented. The long-capillary diffusion measurement method is combined with imaging
techniques using microfocus tubes and flat panel detectors in order to visualize and quantitatively
analyze diffusive mixing of two melts of different chemical composition. The interdiffusion
coefficient as function of temperature and time is obtained by applying Ficks diffusion laws.
Tracking the time dependence of the mean square penetration depth of the mixing process allows to
detect changes in the mass transport caused by convective flow. The possibility to sort out
convective mass transport contributions from analysis enhances significantly the accuracy compared
to the conventional long-capillary diffusion measurement method with postmortem analysis. The
performance of this novel diffusion measurement method with x-ray radiography technique is
demonstrated by a diffusion experiment in an Al-Ni melt.
The purpose of the present study is to show the feasibility of examining hydrogen desorption in technical iron samples using neutron radiography at the ANTARES facility of the FRM II research reactor, Technische Universität München. It has been shown that this method is appropriate for in situ determination of hydrogen Desorption for concentrations as low as 20 ppmH. Experiments were carried out in the temperature range from room temperature up to 260 °C. Measurement was based on direct comparison between electrochemically hydrogen-loaded iron samples and hydrogen-free reference samples at the same temperature.
This enables the determination of hydrogen concentration as a function of time and temperature. Ex situ carrier gas hot extraction experiments using the same temperature–time profiles as the neutron radiography experiments have been used to calibrate the greyscale values of the radiographs to defined hydrogen concentrations. It can be stated that hydrogen desorption correlates with sample temperature.
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.
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.
MSL compatible isothermal furnace insert for high temperature shear-cell diffusion experiments
(2011)
For long-time diffusion experiments shear-cell techniques offer more favourable terms than the traditional long capillary techniques. Here, we present a further developed shear-cell that enables the measurement of diffusion coefficients up to temperatures of 1600 °C. Hence, diffusion experiments can be carried out at temperatures not accessible until now by conventional capillary or shear-cell techniques. The modified shear-cell, which can contain up to six samples of a total length of 90mm and a diameter of 1.5 mm, is built of 30 shear discs of 3mm thickness each. It is operated in an isothermal furnace insert which can be accommodated in the Materials Science Laboratory of the International Space Station. This provides the opportunity that the shear-cell can be applied to microgravity and to ground-based experiments, respectively. The heater insert with an overall length of 518mm and a diameter of 210mm consists of four heating zones with a total power of 3.5 kW. Temperature homogeneity along the graphite sample compartment is better than 2K at 1600°C. Details of the new design are discussed and results of first successfully performed heating and shearing cycles are presented.
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.
A long list of criteria determining the hot cracking susceptibility already exists. A main influence on solidification cracking can result from the design of the welded construction, i.e. from the influence of external loads. Using the Controlled Tensile Weldability (CTW) test, an external load hot cracking test, the influence of constant pre-load and different extension rates on the solidification cracking behavior of GTA (Gas Tungsten Arc) welds in an austenitic (AISI 309) and a ferritic (AISI 441) steel were investigated. Compared to specimens welded allowing free shrinkage and welded with an applied constant tensile pre-load, the specimens welded during the application of increasing tensile load show solidification cracks. In the weld seams, a characteristic angle α between the predominantly columnar grains and the fusion line can be observed. Specimens showing solidification cracks show a significantly larger angle α compared to the crack-free specimens. Based on these observations, the characteristic angle α is proposed as a new hot cracking criterion.
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.