Harald Leitner

Decomposition pathways in age hardening of Ti-Al-N films

The ability to increase the thermal stability of protective coatings under work load gives rise to scientific and industrial interest in age hardening of complex nitride coating systems such as ceramic-like Ti1−xAlxN. However, the decomposition pathway of these systems from single-phase cubic to the thermodynamically stable binary nitrides (cubic TiN and wurtzite AlN), which are essential for age hardening, are not yet fully understood. In particular, the role of decomposition kinetics still requires more detailed investigation. In the present work, the combined effect of annealing time and temperature upon the nano-structural development of Ti0.46Al0.54N thin films is studied, with a thermal exposure of either 1 min or 120 min in 100 °C steps from 500 °C to 1400 °C. The impact of chemical changes at the atomic scale on the development of micro-strain and mechanical properties is studied by post-annealing investigations using X-ray diffraction, nanoindentation, 3D-atom probe tomography and high-resolution...

Atom probe study of the carbon distribution in a hardened martensitic hot-work tool steel X38CrMoV5-1

The microstructure of the hardened common hot-work tool steel X38CrMoV5-1 has been characterized by atom probe tomography with the focus on the carbon distribution. Samples quenched with technically relevant cooling parameters λ from 0.1 (30 K/s) to 12 (0.25 K/s) have been investigated. The parameter λ is an industrially commonly used exponential cooling parameter, representing the cooling time from 800 to 500 °C in seconds divided with hundred. In all samples pronounced carbon segregation to dislocations and cluster formation could be observed after quenching. Carbon enriched interlath films with peak carbon levels of 6-10 at.%, which have been identified to be retained austenite by TEM, show a thickness increase with increasing λ. Therefore, the fraction of total carbon staying in the austenite grows. This carbon is not available for the tempering induced precipitation of secondary carbides in the bulk. Through all samples no segregation of any substitutional elements takes place. Charpy impact testing and fracture surface analysis of the hardened samples reveal the cooling rate induced microstructural distinctions.

Precipitation evolution in a Ti-free and Ti-containing stainless maraging steel.

Stainless maraging steels have a Cr content higher than 12wt% and show a excellent combination of high strength and ductility, which make them attractive for use in machinery fields and aircraft applications. The massive increase of strength during ageing treatment of maraging steels is related to a precipitation sequence of various nm-scaled intermetallic phases. The peak hardness especially in Ti-containing maraging steels can be reached after short-time ageing at temperatures around 500 degrees C. However, precipitation reactions in different stainless maraging steels are not fully understood, especially the evolution from clustering over growing to coarsening. In the present work a commercial maraging steel and a Ti-containing model alloy are investigated and compared to each other. The steels were isothermally heat treated at 525 degrees C for a range of times. Special emphasis was laid on the correlation of hardness to the formation and presence of different kinds of precipitates. The isothermal aged samples were investigated by using two advanced three-dimensional energy compensated atom probes (LEAP and 3DAP) both in voltage mode and in laser mode. The atom probe data were correlated to standard hardness measurements. The results show that the partial substitution of Al by Ti results in a different precipitation behaviour. While the Ti-free maraging steel exhibit only one type of precipitate, the Ti-containing grade shows a change in the type of precipitates during ageing. However, this change leads to an accelerated coarsening and thus to a faster drop in hardness.

The morphology of secondary-hardening carbides in a martensitic steel at the peak hardness by 3DFIM

The morphology and composition of secondary-hardening M(2)C carbides in a complex steel under non-isothermal tempering condition has been investigated with three-dimensional field ion microscopy and atom-probe tomography. The technical set-up and the condition of investigations have been developed. We will reveal for the first time, a virtually non-biased image of the so-called secondary-hardening microstructure, consisting in a very fine dispersion of nanometer-sized needles, idiomorphs and blocky carbides. Needles precipitate with a large number density at the maximum hardness peak. We have found out that this mixture of shape could be explained by the onset of coarsening, but the role of local factors have been evidenced: variation of composition among the carbides and even local strain effects due to the precipitation of a second phase can play a role in changing the growth conditions.

Characterization of δ-phase in superalloy Allvac 718PlusTM

Abstract Nowadays, the trend goes to better and more efficient gas turbine engines with lower emissions, greater durability and lower cycle costs. To this end, new materials such as Allvac 718PlusTM, should enhance the high temperature performance. The appearance, morphology and control of the δ-phase are of special interest because of their critical influence on grain structure, grain size and mechanical properties. In this work, the evolution and the morphology of the δ-phase during heat treatment between 900 and 1000°C for annealing times of up to 8 h are investigated in order to determine the time – temperature – precipitation diagram and to understand the phase morphology. For this, different analysis methods are applied, such as light microscopy analysis with computer-aided quantitative metallography, dual beam focused ion beam and both scanning electron and transmission electron microscopy.

Precipitation behaviour of an Fe–Co–Mo-alloy during non-isothermal ageing

Abstract Fe – Co – Mo alloys show hardening behaviour comparable to that of precipitation hardened Al-alloys, which is characterised by a low hardness after solution annealing and a significant increase in the hardness during subsequent ageing at higher temperatures. In this study, the precipitation behaviour of Fe-25% Co-15% Mo (wt.%) has been studied applying non-isothermal ageing. High sensitivity differential scanning calorimetry and atom probe tomography have been used to characterise the precipitation sequence. Three overlapping exothermic reactions, which are related to precipitation reactions, are observed in the temperature range of 400 to 700°C. The investigations have shown that precipitation starts with diffusion of Mo, followed by the formation of the intermetallic μ-phase which reaches its equilibrium composition at a temperature of about 615°C.

Combining complementary techniques to study precipitates in steels

Abstract Understanding the precipitation reactions is of vital importance for the development of advanced steels. A comprehensive characterization of all phases, however, is still demanding in thes...

Critical consideration of precipitate analysis of Fe-1 at.% Cu using atom probe and small-angle neutron scattering.

An Fe-1 at.% Cu model alloy was examined by atom probe (3DAP) and small-angle neutron scattering (SANS) to verify the accordance of the gained results. The Fe-Cu alloy was heat-treated for various times at 500°C, forming Cu-rich precipitates within the Fe matrix. The chemical compositions of the precipitates and matrix found by 3DAP were used to calculate the magnetic scattering contrast. Additionally, a magnetic moment of the precipitates that contain a significant amount of Fe was taken into account for the calculation of magnetic scattering contrast. This in turn is used for the evaluation of the magnetic scattering curves gained by SANS. Both the 3DAP data as well as the scattering curves were analyzed with regard to radius, number density, and volume fraction of the precipitates as a function of aging time. The results yielded by both techniques are in good agreement and correspond to the development of the hardness of the alloy. Minor differences can be related to the cluster search algorithm used for the analysis of the 3DAP data as well as Fe overestimation based on different field phases.

Residual stresses in forged IN718 turbine discs

Abstract Residual stresses play an important role in the production of forged components like turbine discs. Variations in the processing parameters can lead to different residual stress states, which complicate subsequent processing steps, e.g. turning to the final shape. Therefore, a deeper understanding of the residual stress evolution during thermo-mechanical processing and the resulting distortions during machining is essential in order to optimize the manufacturing process with respect to cost efficiency and quality of the product. Consequently, the development of residual stresses in a forged turbine disc made of nickel-based superalloy IN718 was simulated using a finite element (FE) model. The experimental verification of the model was done by independently performed neutron strain scanning. For the studied forged and subsequently water-quenched disc the obtained residual stresses agree well with the stresses predicted by the used FE.

On the precipitation mechanism in the molybdenum based alloy MHC (Mo–Hf–C)

Abstract The precipitation mechanism of small hafnium carbides in the sintered and thermo-mechanically processed molybdenum based alloy MHC (Mo–0·65Hf– 0·65C (at.-%)) is reported. Light and scanning electron microscopy revealed hafnium oxides, large hafnium carbides and molybdenum carbide layers at the grain boundaries in the as-sintered material. Additionally, atom probe tomography showed a residual dissolved content of 0·12 at.-%Hf, but no carbon in solid solution. After thermo-mechanical processing of the as-sintered material in a deformation dilatometer, transmission electron microscopy revealed small hafnium carbides with diameters of 10–100 nm. These carbides were preferentially located at dislocations and dislocation networks. Without deformation prior to aging, no formation of small hafnium carbides was observed. X-ray diffraction confirmed that decomposition of molybdenum carbides had occurred, which delivered the carbon for the formation of strain induced precipitates.