The hot working behavior of AISI 1018 steel was studied by hot-compression deformation tests on the Gleeble 1500 thermo-mechanical simulator at true strain values of -0.143 and -0.405, true strain rate values of 0.01 and 0.1, and working temperatures of 900°C and 1000°C. The tests show that a lower working temperature and lower true strain value results in a greater maximum compressive force. The apparent activation energy Qapp was calculated by using the Zener-Hollomon parameter combined with the low stress law. Qapp ­was calculated to be 311 kJ mol-1 K-1.

Nickel based superalloys were developed to withstand the severe thermal and mechanical environment associated with rocket propulsion systems and jet engines. In many alloy systems the strength of a component rapidly deteriorates as the operating temperature increases. Nickel based superalloys, however, retain strength over a range of temperatures which includes the operating range for many propulsion systems. This improved performance is accomplished by a combination of solid-solution strengthening, precipitation strengthening and grain-boundary strengthening. Furthermore, super-alloy systems are designed for ease of fabrication, to include machining, welding and heat treating. Inconel 718 was developed to overcome problems with post-weld cracking that were common in precipitation hardened nickel based superalloys strengthened by γ’. Inconel 718 is strengthened by γ’’ and is less sensitive to cracking during post-weld thermal treatment. However, in some cases, compositional changes which improved the behavior of these alloys during stress relief actually led to greater difficulty during the joining process. Many approaches have been used to determine the hot-cracking sensitivity of Inconel 718. Historically, two approaches have been particularly valuable because of their repeatability, their ability to compare different alloy systems and their verisimilitude to actual fabrication. These are the Gleeble hot-ductility test and the Variable-Restraint (Varestraint) weld test. Varestraint samples were prepared as per standard preparation techniques and tested longitudinally with a GTAW. At a predetermined location a strain was applied perpendicular to weld direction. The applied strain varied from 0.25%, 0.5%, 1.0%, 2.0%, and 4.0%. The Inconel 718 yielded a maximum crack length of 0.6 mm with a saturation strain of 2.0%. Both the total crack length and the number of cracks did not have a saturation strain. Gleeble samples were prepared from rod stock and tested with standard methodology to determine the characteristic temperatures: nil ductility, nil strength, and ductility recovery temperature of Inconel 718. The samples were tested at various pull temperatures on-heating until the nil strength temperature then tested on-cooling with the nil strength temperature acting as the peak temperature. The nil strength temperature was 2273°F, nil ductility temperature was 2182°F, and the ductility recovery temperature was 1925°F. Both the Varestraint and Gleeble results were compared with relevant literature to determine the weldability of the Inconel 718. Four criteria were used to determine the weldability of Inconel 718 and in three of the four tests; the Inconel 718 had equal to or greater weldability than the compared materials. In the fourth test, the Inconel 718 demonstrated lower weldability than the compared alloy systems, however, Inconel 718 operates in different conditions specifically, the high temperature and pressure conditions mentioned above.

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Intercritically annealed medium manganese steels are a promising third-generation advanced high-strength steel candidate, relying on large fractions of Mn-enriched retained austenite for excellent strength-ductility combinations. The present study proposes a novel cyclic intercritical annealing to promote nucleation and efficient stabilization of austenite in a medium Mn microstructure. Design of the heat treatment is driven by the hypothesis that the distribution of ductile austenite is key in mitigating the strain incompatibility that accelerates failure in these steels. Development and preliminary testing of the heat treatment are first detailed and compared with literature results for equivalent isothermal annealing. The effects of cyclic annealing parameters on the amount and stability of retained austenite are also explored through diffraction methods and mechanical testing. Finally, steps are taken towards quantifying austenite formation during the cyclic treatment, and recommendations are made for adapting the designed heat treatment to thicker gauges.

Les aciers renforcés par dispersion d’oxydes (ODS) sont des matériaux candidats pourconstituer les gaines de combustibles des réacteurs nucléaires de IVème génération refroidis au sodium(RNR-Na). Le soudage par résistance en bout de ces gaines est étudié dans ce travail, avec pourobjectif la détermination et la compréhension des effets du procédé sur l’évolution de la microstructuredes aciers ODS à 9 % et 14 % de chrome à l’échelle des grains et des oxydes nanométriques. Uneapproche couplant caractérisations microstructurales sur soudures, simulation numérique et simulationphysique du procédé, à l’aide d’un simulateur thermomécanique Gleeble 3500, est adoptée. Le soudagepar résistance en bout impose localement des conditions de sollicitations sévères en termes dedéformation, vitesse de déformation et température. Ces sollicitations induisent un affinement de lamicrostructure dont l’origine peut être attribuée à un mécanisme de recristallisation dynamique (acier à14 % de chrome) ou à l’association de la recristallisation dynamique et des transformations de phase(acier à 9 % de chrome). Les conditions d’occurrence de la recristallisation dynamique sont étudiéessur ces matériaux. On montre notamment la possibilité d’une transition entre recristallisation dynamiquecontinue et discontinue sur l’acier à 14 % de chrome en fonction des conditions de sollicitation. Il estégalement observé que ces sollicitations thermomécaniques sévères induisent une augmentation de lataille des oxydes nanométriques associée à une diminution de leur fraction volumique. / Oxide dispersion strengthened (ODS) steels are considered as candidate materials for thedevelopment of fuel cladding for sodium-cooled fast reactors (SFR). Resistance upset welding of thecladding is studied in this work. The aim is to determine and to understand the process effects on themicrostructure of ODS steels with 9% and 14% of chromium at the scales of the grains and thenanometric oxides. An approach coupling microstructural characterization of welds, numericalsimulation and physical simulation of the process, using a thermomechanical simulator Gleeble 3500,is proposed. Resistance welding locally imposes severe thermomechanical conditions in terms of strain,strain rate and temperature. Refinement of the microstructure is noted and correspond to a dynamicrecrystallization mechanism (14 % Cr steel) or the combination of dynamic recrystallization and phasetransformations (9 % Cr steel). The conditions of occurrence of dynamic recrystallization are studied.The possibility of a transition between continuous and discontinuous dynamic recrystallization is shownfor the 14 % Cr steel according to the loading conditions. Such severe thermomechanical conditionsinduce an increase in the size of nanoscale oxides associated with a decrease of their volume fraction.

In this thesis, the heat affected zone (HAZ) of Gleeble simulated welds, the weldments and the creep specimens for several types of 9%-12% Cr ferritic steels were studied by focusing on the Type IV cracking in the fine grained zone (FZ). The field emission gun transmission electron microscopy (FEGTEM) and scanning electron microscopy (SEM) were used to measure the phosphorus segregation on the grain boundary (GB) and the creep fracture morphologies respectively. Meanwhile the well-developed grain boundary segregation and precipitation (GBSP) model was applied to simulate the experimental results. The experimental results have showed that the HAZ zone was characterised by softening and Type IV cracking. All the high Cr ferritic steel welds gave a microstructure of mainly tempered martensite and M23C6 precipitates after the post weld heat treatment (PWHT). There was no δ-ferrite observed in the HAZ. The Type IV cracking exhibited a mixed cracking mechanism in which the intergranular grain boundary separation is dominant due to the crack initiation by voids and the faster M23C6 growth with the service time. A new model on the mechanism of the Type IV cracking is established. The FEGTEM research has also showed obvious non-equilibrium phosphorus segregation at the grain boundaries, which is affected significantly by the quenching temperature. The phosphorus GB segregation deteriorates the weak grain boundaries. The experimental results were well in agreement with the GBSP modelling.

This research is aimed at understanding the effect of thermal cycles on the metallurgical and microstructural characteristics of the heat affected zone of a multi-pass pipeline weld. Continuous Cooling Transformation (CCT) diagrams of the pipeline steel grades studied (X65, X70 and X100) were generated using a thermo mechanical simulator (Gleeble 3500) and 10 mm diameter by 100 mm length samples. The volume change during phase transformation was studied by a dilatometer, this is to understand the thermodynamics and kinetics of phase formation when subjected to such varying cooling rates. Samples were heated rapidly at a rate of 400°C/s and the cooling rates were varied between t8/5 of 5.34°C/s to 1000°C/s. The transformation lines were identified using the dilatometric data, metallographic analysis and the micro hardness of the heat treated samples. Two welding processes, submerged arc welding (SAW) and tandem Metal Inert Gas (MIG) Welding, with vastly different heat inputs were studied. An API-5L grades X65, X70 and X100 pipeline steels with a narrow groove bevel were experimented with both welding processes. The welding thermal cycles during multi-pass welding were recorded using thermocouples. The microstructural characteristics and metallurgical phase formation was studied and correlated with the fracture toughness behaviour as determined through the Crack Tip Opening Displacement (CTOD) tests on the welded specimens. It was observed that SAW process is more susceptible to generate undesirable martensite-austenite (M-A) phase which induce formation of localised brittle zones (LBZ) which can adversely affect the CTOD performance. Superimposition of the multiple thermal cycles, measured in-situ from the different welding processes on the derived CCTs, helped in understanding the mechanism of formation of localised brittle zones. Charpy impact samples were machined from the two X65 and X70 grades, for use in thermal simulation experiments using thermo mechanical simulator (Gleeble). The real thermal cycles recorded from the HAZ of the SAW were used for the thermal simulations, in terms of heating and cooling rates. This is to reproduce the microstructures of the welds HAZ in bulk on a charpy impact sample which was used for impact toughness testing, hardness and metallurgical characterisation. The three materials used were showing different response in terms of the applied thermal cycles and the corresponding toughness behaviours. The X65 (a) i.e. the seamless pipe was showing a complete loss of toughness when subjected to the single, double and triple thermal cycles, while the X65 (b), which is a TMCP material was showing excellent toughness in most cases when subjected to the same thermal cycles at different test temperatures. The X70 TMCP as well was showing a loss of toughness as compared to the X65 (b). From the continuous cooling transformation diagrams and the thermally simulated samples results it could be established that different materials subjected to similar thermal cycle can produce different metallurgical phases depending on the composition, processing route and the starting microstructure.

Abstract The blast furnace – basic oxygen furnace route remains the most utilised process route in the production of steel worldwide. Coke is the main fuel of the blast furnace process, however, coke producers and blast furnace operators are facing significant challenges due to increased demands on coke quality and decrease of prime coking coals. The estimation of coke performance in the industrial process through accurate laboratory analyses is of increasing importance. In this doctoral thesis, the aim was to study phenomena related to coke properties and its analysis methods in blast furnace simulating conditions. A new method was introduced to measure the hot strength of coke using a Gleeble 3800 thermomechanical simulator. The hot strengths of industrial cokes were determined at various temperatures and several coke properties, which were believed to affect hot strength, were determined. The effect of H₂ and H₂O in the blast furnace shaft gas were determined in relation to coke reactivity, threshold temperature, and the gasification mechanism. The results obtained by this thesis show that the Gleeble device is suitable for study of coke hot strength. The coke strength was significantly decreased for all three coke grades at temperatures of 1600 °C and 1750 °C when compared to room temperature or 1000 °C. The deformation behaviour of coke was fragile up to 1000 °C, but became at least partially plastic at 1600 °C, and the plasticity further increased at 1750 °C. Notable changes were observed in the deformation behaviour between coke grades at high temperatures. The presence of H₂ and H₂O in the BF shaft gas strongly increased coke reactivity and changed the reaction mechanism of coke to be more surface centric in a specific temperature range. The reactivity of coke in the conditions 100 vol-% CO₂ did not directly correlate with reactivity in a simulated blast furnace shaft gas, which suggest that the widely utilised CRI test does not accurately estimate coke reactivity in the industrial blast furnace process. / Tiivistelmä Masuuni – konvertteri yhdistelmä on edelleen käytetyin prosessireitti teräksen tuotantoon ympäri maailman. Koksi on masuunin tärkein polttoaine. Koksintuottajat ja masuunioperaattorit ovat suurten haasteiden edessä johtuen koksin kasvaneista laatuvaatimuksista ja parhaiden koksautuvien kivihiilten ehtymisestä. Koksin suoriutumisen arviointi masuunin olosuhteissa tarkoilla laboratorioanalyyseillä on yhä merkittävämmässä roolissa. Tässä väitöskirjassa tavoitteena oli tuottaa uutta tietoa koksin ominaisuuksista ja sen analyysimenetelmistä simuloiduissa masuunin olosuhteissa. Uusi metodi esitettiin koksin kuumalujuuden määrittämiseksi Gleeble 3800 termomekaanisella simulaattorilla. Teollisten koksilaatujen kuumalujuuksia määritettiin eri lämpötiloissa ja useita koksin mitattiin, joilla uskottiin olevan vaikutus kuumalujuuteen. Lisäksi työssä tutkittiin masuunin kuilun kaasuatmosfäärissä H2 ja H2O kaasujen vaikutusta koksin kemialliseen reaktiivisuuteen, kaasuuntumisen kynnyslämpötilaan ja reaktiomekanismiin. Tässä työssä esitetyt tulokset osoittavat että Gleeble soveltuu koksin kuumalujuuden määritykseen. Koksin lujuus aleni merkittävästi kaikilla kolmella koksilaadulla kuumennettaessa 1600 ja 1750 °C lämpötiloihin verrattuna huoneenlämpötilaan tai 1000 °C lämpötilaan. Koksin muodonmuutos oli haurasta aina 1000 °C lämpötilassa, mutta muuttui osittain plastiseksi 1600 °C lämpötilassa ja plastisuus kasvoi kun lämpötilaa nostettiin 1750 °C:een. Huomattavia eroja havaittiin eri koksilaatujen muodonmuutoskäyttäytymisessä korkeissa lämpötiloissa. H₂ ja H₂O kaasujen läsnäolo kuilun kaasuatmosfäärissä kasvatti voimakkaasti koksin reaktiivisuutta ja muutti kaasuuntumismekanismia pintakeskisemmäksi rajatulla lämpötila-alueella. Koksin reaktiivisuus 100 % CO₂ kaasussa ei korreloinut suoraan simuloidun masuunin kuilun kaasuatmosfäärin kanssa. Tämä tulos indikoi sitä että maailmalla yleisesti käytetty CRI testi ei ennusta tarkasti koksin reaktiivisuutta masuunissa.