Julien Deleume

Kinetic Study of the Low Temperature Internal Oxidation of Nickel Based Model Alloys Exposed to PWR Primary Water

Two Ni-Fe-Cr ternary alloys have been oxidized in simulated pressurized water reactor primary water at 360°C for 1000 h. The chemical composition of those alloys were chosen in order to be representative of the one of chromium depleted areas under the oxide scale of industrial alloys (e.g. alloy 600) exposed in the same conditions. The resulting oxidized structures (corrosion scale and underlying metal) were characterized using complementary analytical methods (FEG-SEM, TEM, SIMS, optical microscopy). On the one hand, the characterized external oxide layer is very close to the one observed on industrial nickel-base alloys, hence validating the use of such model alloys. On the other hand, both free oxygen and oxides have been detected at grain boundaries several micrometers under the metal/oxide interface. Implications of such a finding on the involved transport mechanisms for oxygen and the intergranular stress corrosion cracking resistance of nickel-base alloys are then discussed.

Influence of Interstitials Content on the Sensitivity of Alloy 718 to Oxidation Assisted Intergranular Fracture

Alloy 718 is known to be sensitive to oxidation assisted intergranular cracking. It is also demonstrated that the occurrence of jerky flow (also called Portevin-Le Châtelier effect) stops the intergranular damaging mechanism. As dynamic strain ageing is known to be linked with the alloy content of interstitial species, the aim of the present work is to study the effect of carbon, nitrogen and oxygen concentrations on the mechanical behaviour of thin tensile specimens tested under oxidation conditions close to those encountered industrially for turbo machine disks. Thanks to heat treatments performed under reducing atmosphere, the content of interstitial species in tested alloy 718 samples is gradually curbed. Tensile specimens were then tested between 550 and 700°C for the strain rate range [10-5, 10-1] s-1. The key point of this work is that, for a given testing temperature, the tensile tests clearly demonstrated that the transition from an intergranular fragile fracture mode to a transgranular ductile one was always linked with the occurrence of Portevin-Le Châtelier phenomenon but for slower strain rates in comparison with what was observed on the as received aged material tested in the same conditions. This shift of the transition of fracture mode through the lower strain rates remained true until a threshold value of the heat treatment time under reducing atmosphere. Specimens heat treated over this value systematically exhibited a fully transgranular ductile fracture mode, whatever the plastic flow regime was. Implication of such a finding on the intergranular embrittlement of alloy 718 by high temperature oxidation is then discussed.

Influence of Interstitials Content on the Diffusion of Niobium in Alloy 718

Many studies have emphasized the beneficial effect of niobium on the physical metallurgy of Ni-Cr-Fe alloy 718. Among the different strengthening actions of niobium, such as solid solution hardening and carbide precipitation, the precipitation of niobium with nickel in a strengthening phase γ” (Ni3Nb) during the aging heat treatment has the largest influence on the mechanical properties of alloy 718. The improvement of the niobium distribution and diffusion in the Ni-matrix may allow a more homogenized repartition of γ” precipitates and seems then to be an effective way to upgrade the mechanical properties. As γ” precipitates decompose to the stable δ phase at very long aging times, the study of the effect of carbon, nitrogen and oxygen concentrations on precipitation and dissolution of the δ phase may give information on γ” precipitation and on niobium distribution. It is the purpose of the present work to examine the role that the alloy content of interstitial species plays with the niobium-rich δ phase evolution in alloy 718. Alloy 718 samples were heat treated under hydrogenated argon at 980°C for 0 to 96 hours in order to gradually curb the content of interstitial species by reaction with the reducing atmosphere. Chemical analyses realized by glow discharge mass spectrometry (GDMS) confirmed the reduction of the concentration of these species. Specimens were solution-treated for 1h at 1050°C in an inert atmosphere and furnace cooled. Some of the samples were then aged at 920°C for times ranging from 10 min to 1 hour. The precipitation was measured quantitatively in terms of volume fraction and the morphology of the precipitates was appreciated using scanning electron microscopy (SEM). The differences in the precipitation kinetics and in the microstructure evolution for each interstitial concentration are then discussed.