Multiple Influences of Molybdenum on the Precipitation Process in a Martensitic PH Stainless Steel

Molybdenum has been found to influence the complex precipitation process in a martensitic precipitation hardening stainless steel during aging at 475 degrees C in several different ways. Three steels with different Mo content (0, 1.2 and 2.3 at.%) were investigated. Studies of the microstructure were performed with atom probe tomography and energy filtered transmission electron microscopy. It is shown that, at the initial stage of aging, a faster nucleation of Cu-rich clusters takes place with increasing Mo content. The Cu-clusters act as precipitation sites for other solute elements and promote the nucleation of Ni-rich phases. During further aging, a higher Mo content in the material instead slows down the growth and coarsening of the Ni-rich phases, because Mo segregates to the interface between precipitate and matrix. Additionally, Mo promotes decomposition of the matrix into alpha and alpha\u27 regions. After longer aging times (>40 h) quasicrystalline Mo-rich R\u27 phase forms (to a greater extent in the material having the highest Mo content). The observations serve to understand the hardness evolution during aging

Crack Growth Studies in a welded Ni-base superalloy

It is well known that the introduction of sustained tensile loads during high-temperature fatigue (dwell-fatigue) significantly increases the crack propagation rates in many superalloys. One such superalloy is the Ni-Fe based Alloy 718, which is a high-strength corrosion resistant alloy used in gas turbines and jet engines. As the problem is typically more pronounced in fine-grained materials, the main body of existing literature is devoted to the characterization of sheets or forgings of Alloy 718. However, as welded components are being used in increasingly demanding applications, there is a need to understand the behavior. The present study is focused on the interaction of the propagating crack with the complex microstructure in Alloy 718 weld metal during cyclic and dwell-fatigue loading at 550 °C and 650 °C

Room temperature plasticity in sub-micrometer thermally grown oxide scales

Thermally grown oxides (TGOs) are generally considered to be brittle, capable of sustaining very limited plastic deformation before fracture. As they are prone to exhibit different forms of defects, the fracture toughness, typically measured to be some 1–2 MPa m1/2 [1], is typically reached well before sufficiently high stresses to induce plasticity can be applied [2]. This is particularly true at room temperature, where possible low-stress thermally activated creep mechanisms are suppressed. However, the occurrence of plasticity in e.g. Al2O3 single crystals at room temperature can occur for samples in the micrometer range [3]. Most measurements of the deformation of TGOs have been made on relatively thick scales, (\u3e1 micrometer), which are limited by the fracture originating from inherent defects. Furthermore, the studies have been limited in resolution and sensitivity, as the scales were adherent to the substrates and tested as a composite. Recently, micro-mechanical testing has been introduced as a method to evaluate mechanical behavior of TGOs on a ferritic/martensitic steel [4], where micro-cantilever bending was used to test specimen extracted from different layers in a 5–10 micrometers thick oxide. Still, the cantilever cross-section was typically several micrometers, and the very similar fracture stresses for notched and un-notched cantilevers seems to indicate that the deformation is still limited by inherent defects. Please click Additional Files below to see the full abstract

Fracture of Cr2O3 single crystals on the microscale

Studying cleavage properties of protective oxide scales is imperative to understand their fracture behaviour, since transgranular fracture is observed in many cases. The small thickness and polycrystalline structure of such scales makes it difficult to identify active cleavage planes directly from mechanical testing. To resolve this issue for Cr2O3, we present an approach to experimentally identify cleavage planes through micro-cantilever bending. Single crystal wafers are used to prepare micro-cantilevers of pentagonal cross-section in different orientations, targeting possible cleavage planes. Fracture surface imaging showed rhombohedral and pyramidal fracture, though surface energy studies predict rhombohedral as the dominant plane. There does exist a preference for rhombohedral fracture over pyramidal, which is also revealed from the experiments

Cold sprayed Cr-coating on Optimized ZIRLO™ claddings: the Cr/Zr interface and its microstructural and chemical evolution after autoclave corrosion testing

Cr-coated Optimized ZIRLO™ cladding material fabricated with the cold-spray deposition process is studied. Microstructure and chemistry of this material are investigated before and after exposure to autoclave corrosion testing with scanning electron microscopy, energy dispersive spectroscopy analysis, electron backscattered diffraction, transmission electron microscopy and atom probe tomography. The results are used to assess what changes have occurred upon autoclave exposure. The formation of a compact, 80 – 100 nm thick Cr2O3 layer is observed on the surface of the exposed samples. Nucleation of ZrCr2 intermetallic phase is discovered at the Cr/Zr interface. This Laves phase nucleates inside the intermixed bonding layer that can be found in both pristine and exposed samples, and decorates the interface in the form of small particles (less than 50 nm in size). Using transmission electron microscopy and atom probe tomography the growth of a Zr-Cr-Fe phase was detected. This phase is found in the region of the Zr-substrate immediately adjacent to the coating, up to a few hundred nanometres distance from the Cr/Zr interface. A small degree of recrystallization occurs upon autoclave exposure in the 1-2 \ub5m thick nanocrystalline layer produced on the Zr-substrate by the cold spray deposition method utilized for the fabrication of the Cr-coating

Microscale fracture of chromia scales

High temperature materials such as superalloys rely on the formation of a protective surface oxide scale for prevention of corrosion. Such materials undergo periods of varying thermal and mechanical loads during operation, which can lead to cracking of the surface oxide. This exposes the material to corrosion, and can also act as stress concentrations, which affects the life of the underlying material. It is therefore necessary to consider the mechanical integrity of these scales while estimating material life. Several models have been developed in which fracture mechanics is utilized to estimate failure. But there is a lack of data such as fracture strains and elastic modulus for oxide scales. Conventional mechanical testing methods such as tensile and bending tests have been modified to obtain mechanical data, but it mainly applies to thick oxide scales (several µm thick). These methods are also limited with respect to isolating substrate and residual stress effects. For advanced materials, where the oxide formation kinetics are low, new methods are required in order to assess the mechanical properties. Please click Additional Files below to see the full abstract

Self-organized nanostructuring in Zr0.69Al0.31N thin films studied by atom probe tomography

We have applied atom probe tomography (APT) to analyze self-organizing structures of wear-resistant Zr0.69Al0.31N thin films grown by magnetron sputtering. Transmission electron microscopy shows that these films grow as a three-dimensional nanocomposite, consisting of interleaved lamellae in a labyrinthine structure, with an in-plane size scale of ~ 5 nm. The structure was recovered in the Al APT signal, while the Zr and N data lacked structural information. The onset of the self-organized labyrinthine growth was observed to occur by surface nucleation, 5–8 nm above the MgO substrate, due to increasing Zr–Al compositional fluctuations during elemental segregation. At a final stage, the labyrinthine growth mode was observed to be interrupted by the formation of larger ZrN grains

Comparing CrN and TiN Coatings for Accident-Tolerant Fuels in PWR and BWR Autoclaves

The development of coatings for accident-tolerant fuels (ATFs) for light water reactor (LWR) applications promises improved corrosion resistance under accident conditions and better performances during operation. CrN and TiN coatings are characterized by high wear resistance coupled with good corrosion resistance properties. They are generally used to protect materials in applications where extreme conditions are involved and represent promising candidates for ATF. Zr cladding tubes coated with 5 \ub5m-thick CrN or TiN, exposed in an autoclave to simulated PWR chemistry and BWR chemistry, were characterized with SEM, EDS, and STEM. The investigation focused on the performance and oxidation mechanisms of the coated claddings under simulated reactor chemistry. Both coatings provided improved oxidation resistance in a simulated PWR environment, where passivating films of Cr2O3\ua0and TiO2, less than 1 \ub5m-thick, formed on the CrN and TiN outer surfaces, respectively. Under the more challenging BWR conditions, any formed Cr2O3\ua0dissolved into the oxidizing water, resulting in the complete dissolution of the CrN coating. For the TiN coating, the formation of a stable TiO2\ua0film was observed under BWR conditions, but the developed oxide film was unable to stop the flux of oxygen to the substrate, causing the oxidation of the substrate