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- Neutron radiography (15)
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Eingeladener Vortrag
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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.
Hydrogen assisted cracking of metals limits the durability of welds and constructions. Still
the failure mechanisms are not fully understood, for instance the role of hydrogen mass
transport during crack initiation. Measuring the hydrogen concentration as a function of
time (and space) would allow to determine diffusion coefficients helping to enlighten this
lack of understanding. Therefore, neutron radiography is a valuable tool for measuring in
situ hydrogen transport in iron and steels [1].
The influence of grain boundaries on the hydrogen diffusion behaviour can be determined
by comparing the diffusion behaviour of samples with e.g. different microstructure. In a
first study we investigated in situ the simplest case, the hydrogen effusion out of pure iron
(ARMCO) using neutron radiography at ANTARES [2]. Samples were charged electrochemically
ex situ with a well defined amount of hydrogen, stored in liquid nitrogen and were then
heat treated during a neutron radiography measurement whilst the change of neutron transmission
was recorded. For analysis the gray values in the pictures were transformed into
concentrations with help of an ex post calibration. Therefore, the experimental temperaturetime
profile of the heat treatment has been repeated with identical samples in the home lab
and the amount of effusing hydrogen was measured by carrier gas hot extraction. In a first
approximation the concentration of hydrogen in the sample can be calculated by subtracting
the hydrogen concentration in the atmosphere from the initial one in the sample. We
were able to measure hydrogen concentrations as low as 65 wt.ppm.
Simultaneously monitoring of hydrogenous
sample and hydrogen-free reference allowed
for in situ measurement of hydrogen effusion.
Sample heating was done by infrared radiation.
Diffusion coefficients for hydrogen effusion
from iron have been calculated. They coincide
fairly with literature data.
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.
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.
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.
We report about diffusion measurements and molecular dynamic simulations
in Al-Ni and Al-Cu melts. Capillary methods were used to measure Ni and
Cu self diffusion and to measure interdiffusion. The combination of the
capillary set-up with X-ray radiography allowed in-situ detecting of
convective contributions to the interdiffusion transport by tracking the
time dependence of diffusion. Thus, the determination of the
interdiffusion coefficient can
be restricted to convection-free experiment times resulting in an
increased accuracy of the measured interdiffusion coefficient.
Additionally, quasielastic neutron scattering was used to measure
convection-free Ni and Cu self diffusion. Molecular dynamics simulations
were used to determine all diffusion coefficients and the thermodynamic
factor. The comparison between experiment and simulation shows an
excellent agreement of the interdiffusion coefficients as a function of
temperature. It was found that interdiffusion is enhanced by
thermodynamic forces with a maximum around the stoichiometric composition.