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Novel martensitic filler materials with specially adjusted martensite start temperatures (Ms) can counteract the cooling specific shrinkage due to expansion effects of the weld metal associated with phase transformations. That can be exploited to create compressive residual stresses in the weld and adjacent areas, i.e. beneficial for increasing fatigue strength. The Ms temperature is shifted via the chemical composition, mainly by the alloying elements nickel and chromium, resulting as well in different retained austenite contents. Investigations were made using different Low Transformation Temperature (LTT) alloys with varying nickel content. The resulting phase transformation temperatures were – for the first time – detected using high energy synchrotron diffraction and Single Sensor Differential Thermal Analysis (SS-DTA). Compared to angle dispersive diffraction, energy dispersive diffraction offers the possibility to measure residual stresses of the martensite and austenite phase parallel fast in one experiment up to depths of 100 µm. The residual stresses show significant distributions dependent on Ms temperature. The effect on the cold cracking behaviour of these alloys was investigated using the Tekken test. Results show that cold cracking can be avoided when appropriate contents of retained austenite are existent.
The damaging impact of hydrogen on the austenitic stainless steel AISI 304 L was analysed.
To this aim, samples were charged electrochemically with the hydrogen isotope deuterium (2H, D) and examined with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and electron backscatter diffraction (EBSD). The fusion of the obtained chemical and structural information revealed local enrichment of deuterium in austenite, transformation into martensite, crack formation and severe roughening of the specimen surface. The results indicated that martensite was not only formed during charging but also during Desorption and ToF-SIMS examinations. Furthermore, cross-sections of deuterium-charged samples revealed that in preferred deformation bands a g/ε/a 0 evolution is taking place.
By means of microscopic analyses and carrier gas hot extraction (CGHE), it was found that the use of NaAsO2 as recombination poison decreased the uptake of hydrogen significantly and resulted in severe precipitation on the specimen surfaces. This is in contrast to the popular presumption that NaAsO2 enhances the uptake of hydrogen (and
deuterium) during electrochemical charging by hampering its recombination from Atoms to molecules.
The novel heat treatment concept of “Quenching and Partitioning” (Q&P) enables producing low alloyed martensitic steels with high strength and formability. Therefore austenite, retaining from a quenching temperature between Mf and Ms, is stabilised by carbon diffusion. This stabilised austenite transforms in martensite (TRIP effect) under mechanical loading. Current investigations on the Q&P heat treatment of martensitic stainless steels reveal a further enhancement of mechanical properties due to higher amounts of austenite. Thus a tensile strength of 1.800 MPa and a maximum elongation of 20 % are possible, while mechanical properties under compression are much higher due to a distinct SD effect.
The presentation aims to gain a further understanding of the Q&P heat treatment and the resulting mechanical properties for the steel X46Cr13, especially the mechanical behaviour under dynamic mechanical loading condition. Results of drop work and Split Hopkinson Pressure Bar test confirms the findings of quasi static compression test. Furthermore, Charpy impact tests show higher impact toughness compared to the common heat treatment of quenching and tempering (Q&T). Complementary investigations indicate a higher corrosion resistance of Q&P compared to Q&T.
Aircraft main landing gear (MLG) components are commonly manufactured from low-alloyed, martensitic, ultra-high strength steels (UHSS) that have to be coated for corrosion protection, representing an expensive and environmentally harmful production step. To avoid already partly banned corrosion protection plating, the new high-alloyed UHSS, Ferrium S53 (UNS S10500), has been designed to replace lowalloyed legacy materials and has been subjected to a limited field test over five years. As with the legacy alloys, UNS S10500 has a fully hardened martensitic microstructure known to be susceptible to hydrogen assisted cracking, per se. Containing about 10 wt% Cr, steels such as S10500 are at the lower limit for corrosion resistant alloys. Similar to super-martensitic stainless steels used in the oil and gas industry, a common failure sequence in marine environments represents pitting and subsequent hydrogen assisted stress corrosion cracking (HASCC). For addressing such phenomena quantitively, as required for respective lifetime assessments of MLG components and systems, the tolerance of such materials dependent on the absorbed hydrogen concentration must be evaluated quantitatively. However, there is a lack of such valuable materials data, as well as of the fractographic behavior dependent on the hydrogen concentration that might be absorbed during HASCC. To provide an improved understanding of the hydrogen dependent mechanical and fractographic behavior, samples of the legacy AISI 4340 and the new S10500 MLG steels have electrochemically been hydrogen-saturated and subjected to tensile testing. In contrast to a previous study, this contribution for the first time focuses on materials that have been salvaged from real service used landing gear components. In this study, it has been demonstrated that the service-applied S10500 steel has not only a higher strength, but also an improved ductility in comparison to the legacy AISI 4340 steel after similar service durations that provides a higher tolerance against hydrogen concentrations that might be absorbed during potential pitting and HASCC in marine environments. In addition, it has been found that the absorbed hydrogen concentration significantly affects the fracture behavior. Interestingly, hardening of the hydrogen charged low-alloyed AISI 4340 steel changes the fracture topography from trans- toward intergranular, while hardening of the S10500 steel turned the fracture topography from inter- to transgranular at respectively high hydrogen concentrations.
To visualize the varying tetragonal distortions in high carbon martensitic steels by EBSD, two different approaches have been applied on backscattered Kikuchi diffraction (BKD) patterns. A band-edge refinement technique called Refined Accuracy (RA) (Oxford Instruments) is compared with a technique called Pattern Matching (PM), which optimizes the fit to a simulated BKD signal. RA distinguishes between hypothetical phases of different fixed 𝑐∕𝑎, while PM determines a best fitting continuous 𝑐∕𝑎 by projective transformation of a master pattern. Both techniques require stored BKD patterns.
The sensitivity of the 𝑐∕𝑎-determination was tested by investigating the microstructure of a ferritic steel with an expected 𝑐∕𝑎 = 1. The influence of the Kikuchi pattern noise on 𝑐∕𝑎 was compared for a single or 40 averaged frames per measuring point, and turned out to be not significant. The application of RA and PM on the martensitic microstructure delivered qualitatively similar maps of 𝑐∕𝑎. The comparison of RA and PM shows that RA is suitably fast and precise during mapping the martensite 𝑐∕𝑎 ratio in analyses of high carbon martensite, especially for fast initial surveys. As RA leads quantitatively to higher noise in 𝑐∕𝑎, the PM analysis can be used for higher precision results.
Observation of martensite formation by combined use of synchrotron diffraction and dilatometry
(2016)
Welding residual stress engineering by means of an adjusted martensite phase transformation would be highly attractive as detrimental tensile residual stresses may be prevented already during welding without time and cost intensive post processing. The present study shows a synchrotron diffraction analysis of a martensitic steel subjected to thermo-mechanical load cycles. Experiments were conducted regarding the microstructural strain response during the austenite to martensite transformation. The strains are a function of the temperature and the specific loads applied during cooling. The relation between the transformation plasticity of the material, the amount of martensite formed and the arising strains can thus be assessed. The lattice plane specific strains were compared to experimental findings from (macro) dilatation tests. It is shown that the microscopic material behavior differs remarkably from the one observed on the macroscopic scale, what leads to characteristic residual stresses in the material.
Welding residual stress engineering by means of an adjusted martensite phase transformation would be highly attractive as detrimental tensile residual stresses may be prevented already during welding without time and cost intensive post processing. The present study shows a synchrotron diffraction analysis of a martensitic steel subjected to thermo-mechanical load cycles. Experiments were conducted regarding the microstructural strain response during the austenite to martensite transformation. The strains are a function of the temperature and the specific loads applied during cooling. The relation between the transformation plasticity of the material, the amount of martensite formed and the arising strains can thus be assessed. The lattice plane specific strains were compared to experimental findings from (macro) dilatation tests. It is shown that the microscopic material behavior differs remarkably from the one observed on the macroscopic scale, what leads to characteristic residual stresses in the material.
Welding residual stress engineering by means of an adjusted martensite phase transformation would be highly attractive as detrimental tensile residual stresses may be prevented already during welding without time and cost intensive post processing. The present study shows a synchrotron diffraction analysis of a martensitic steel subjected to thermo-mechanical load cycles. Experiments were conducted regarding the microstructural strain response during the austenite to martensite transformation. The strains are a function of the temperature and the specific loads applied during cooling. The relation between the transformation plasticity of the material, the amount of martensite formed and the arising strains can thus be assessed. The lattice plane specific strains were compared to experimental findings from (macro) dilatation tests. It is shown that the microscopic material behavior differs remarkably from the one observed on the macroscopic scale, what leads to characteristic residual stresses in the material.
The novel heat treatment concept, “quenching and partitioning” (Q&P) has been developed for high strength steels with enhanced formability. This heat treatment involves quenching of austenite to a temperature between martensite start and finish, to receive a several amount of retained austenite. During the subsequent annealing treatment, the so called partitioning, the retained austenite is stabilized due to carbon diffusion, which results in enhanced formability and strength regarding strain induced austenite to martensite transformation. In this study a Q&P heat treatment was applied to a Fe-0.45C-0.65Mn-0.34Si-13.95Cr stainless martensite. Thereby the initial quench end temperature and the partitioning time were varied to characterize their influence on microstructural evolution. The microstructural changes were analysed by dilatometer measurements, X-ray diffraction and scanning electron microscopy, including electron back-scatter diffraction. Compression testing was made to examine the mechanical behaviour. It was found that an increasing partitioning time up to 30 min leads to an enhanced formability without loss in strength due to a higher amount of stabilized retained and reversed austenite as well as precipitation hardening.
The quenching and partitioning (Q+P) heat treatment enables a higher deformability of high strength martensitic steels. Therefore, it is necessary to have some metastable austenite in the microstructure, which transforms in martensite during plastic deformation (TRIP-effect). This condition is guaranteed by the quenching and the additional partitioning treatment. Due to local carbon diffusion retained austenite is stabilized and a partial reversion of austenite from martensite occurs. The Q+P heat treatment was investigated for the martensitic stainless steel 1.4034 (X46Cr13) concerning the influence of partitioning time. In line with these efforts metallographic, XRD- and EBSD-measurements were performed to characterize the microstructural evolution. The mechanical experiments included mechanical testing with different strain rates. The reversion of austenite by the partitioning treatment could be detected with EBSD- and XRD-measurements. Further-more the results of the mechanical testing showed improved values of strength and de-formability because of the Q+P heat treatment.
The locally varying tetragonality in martensite grains of a high-carbon steel (1.2 mass percent C) was resolved by electron backscatter diffraction (EBSD) with a spatial resolution in the order of 100 nm. Compared to spatially integrating X-ray diffraction, which yielded an average tetragonality fo c/a=1.05, the EBSD measurements in the scanning electron microscope allowed to image a local variation of the lattice papameter ration c/a in the range of 1.02 ≤ c/a ≤ 1.07. The local variation of tetragonality is confirmed by two different EBSD data analysis approaches based on the fitting of simulated to experimental EBSD patterns. The resulting EBSD-based tetragonality maps are pointing to a complex interaction of carbon concentration and local lattice distortions during the formation process of martensitic structures.