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- Neutron radiography (15)
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Eingeladener Vortrag
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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.
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.
We report about investigations of typical material problems in steels. First, residual stresses in and around weld seams with low martensite transition temperature filler material were analyzed w/ and w/o additional transverse tensile load. The investigation was accompanied by x-ray diffraction measurements to track stress-induced phase transitions. Martensite formation during welding under external load yield strain gradients near the surface that improve the integrity of the weld. Further, the residual stress distribution close to laser-treated steel surfaces was analyzed. The method could be improved to reduce analysis artifacts. Finally, hydrogen diffusion in different steels was measured using neutron radiography and subsequent image analysis. Diffusion coefficients were derived by analyzing the time-dependent mass flux. In an outlook we describe the optimal ESS instrumentation from a metallurgists point of view.
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.
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.