Advanced Materials Research Vols. 15-17

Abstract: Supersaturated solid solutions of Cu-44.5at.%Ni-22.5at.%Fe and Cu-37at.%Ni-6at.%Cr alloy were produced by ball milling of a pure chemical elemental mixture for 1080 ks. Two fcc supersaturated solid solutions with a grain size of about 20 and 50 nm, respectively, were obtained after milling. These alloys were subsequently aged at temperatures between 800 and 1003 K for different times. The aging promoted the phase decomposition of the supersaturated solid solution into a mixture of Cu-rich and Ni- phases in both the aged MA alloy powders. The growth kinetics of the modulation wavelength was determined from the X-ray diffraction results and followed the Lifshitz-Slyozov- Wagner theory for a diffusion-controlled coarsening in the mechanically-alloyed Cu-Ni-Fe alloy after aging. However, the sidebands intensity seems to be very low and overlapped with the peaks corresponding to the Cu-rich phase in the aged mechanically-alloyed Cu-Ni-Cr alloy. The growth kinetics of composition modulation wavelength for the aged MA Cu-Ni-Fe alloy was faster at 803 and 898 K than that for the same alloy composition obtained by a conventional processing and then aged at the same temperatures.

Abstract: The thermally aged 10Cr-1Mo-1W-VNbN steels were charged with hydrogen by cathodic electrolysis and then were subjected to the thermal desorption spectroscopic analyses to examine an applicability of hydrogen as a tracer for evaluating the microstructure. The variation in hydrogen desorption characteristics with aging was discussed from the view points of microstructural changes. Experimental results revealed that the amount of hydrogen desorbed, CH, decreased monotonously as the aging proceeded and there was a relatively good correlation between the CH and Vickers hardness. The CH was expected to be a useful indicator for the material degradation. Additionally, the decomposition of the profile was attempted to understand the metallurgical meaning of hydrogen profile and apply the present method to the microstructural evaluation. As the result, it was suggested that the changes in two decomposed profiles with aging might reflect the variation of dislocation density and the precipitation process of M23C6 carbide and/or Laves phase, respectively.

Abstract: The system free energy was estimated for the martensite phase of an Fe-Cr-C ternary alloy, 12Cr2W and 12Cr2W0.5Re steels. The system free energy of the martensite phase is defined as, Gsys = G0 + Estr + Esurf , where G0 is the chemical free energy, Esurf is the interfacial energy for the boundaries in the martensite microstructure, and Estr is the elastic strain energy due to the dislocations in the martensite phase. From the experimental results on SEM/EBSD, the total interfacial energies were estimated to be 0.83J/mol for the ternary alloy and 4.8J/mol for both 12Cr2W and 12Cr2W0.5Re steels in the as-quenched state. Also, the elastic strain energies were estimated to be 7.1J/mol for the ternary alloy, 9.6J/mol for 12Cr2W steel and 9.8J/mol for 12Cr2W0.5Re steel in the as-quenched state. So, the system free energy was about 7.9J/mol for ternary alloy. On the other hand, the system free energy was about 14.4J/mol for 12Cr2W steel and 14.6J/mol for 12Cr2W0.5Re steel. So, these microstructural energies operate as a driving force for the microstructure evolution, e.g., recovery of dislocations and the coarsening of the sub-structures such as martensite-packet, -block and -lath.

Abstract: Oxide-dispersion strengthened (ODS) ferritic stainless steels have been considered as promising high-temperature materials such as interconnects for oxide-fuel cells and nuclear materials for Liquid Metal Fast Reactors or Super-Critical-Water-Cooled Reactors. In the present work, we have prepared Fe-14Cr-2Al-1Si-0.3Ta-1Y2O3 ferritic stainless steels which were dispersion-strengthened by nano-sized Y2O3 via mechanical alloying of elemental powder mixtures and subsequent hot consolidation. A comparison was made with MA 957 and DY-01 alloys. The mechanically alloying behaviour and consolidated mechanical properties of the Fe-14Cr-2Al-1Si- 0.3Ta-1Y2O3 ferritic steels were strongly influenced by processing parameters, especially milling atmosphere. The stability of yttrium oxides and oxidation resistance at high temperatures were examined. The preliminary result shows that the mechanically alloyed Fe-14Cr-2Al-1Si-0.3Ta- 1Y2O3 ferritic stainless steel exhibits interesting properties to be exploited as high temperature materials.

Abstract: Heat-resistant steels of HP series (Fe-25Cr-35Ni) are used as reformer tubes in petrochemical industries. Their composition includes Nb and Ti as strong carbide formers. In the ascast condition, alloys exhibit an austenite matrix with intergranular MC, M23C6 and/or M7C3 eutectic carbides. During exposure at high temperature, phase transformations occur: chromium carbides of M7C3 type transform into the more stable M23C6 type, intragranular M23C6 carbides precipitate, and a silicide, the G-phase (Ni16Nb6Si7), forms due to the instability of MC carbides (NbC). Thermodynamic simulation is of great help for understanding precipitate formation and transformations. Thermo-Calc and Dictra are used to simulate the precipitation of carbides in the austenite matrix during service. However, from an experimental point of view, M23C6 and M7C3 are not easy to distinguish in bulk alloys. Indeed, backscattered scanning electron microscopy does not bring any contrast between the two phases, and energy dispersive spectroscopy (EDS) analysis does not lead to carbon content and consequently to the distinction between M23C6 and M7C3. With transmission electron microscopy (TEM), sample preparation is difficult and the observed area is extremely small. In the present work, HP alloys are investigated by electron backscatter diffraction (EBSD) coupled to EDS. Carbides are identified on the basis of crystal structure, in the bulk, within their microstructural context, and the experimental procedure is both simpler and cheaper than TEM. Precipitates (M23C6, M7C3) could be identified by orientation mapping and single spot analysis.

Abstract: Steels with high amounts of silicon are used in electrical applications due to their low mangectoestriction, high electrical resistivity and reduced energy losses, but they exhibit poor formability. A fundamental study of the workability of such materials using torsion testing may help to understand and to optimise its production. Single deformation torsion tests were carried out on a steel containing 2 wt.-% Si in a temperature range of 800 to 1100°C and strain rates in the range of 0.01 to 2 s-1. A value of 299 kJ/mol was found for the apparent activation energy for hot working after applying the hyperbolic-sine equation to the mean flow stress (MFS) values computed from the test. Multiple deformation torsion tests under continuous cooling conditions were carried out in the same temperature range at strain rates from 0.2 to 1 s-1, the strain per pass and interpass time (determining the cooling rate) were varied. Different critical temperatures, which are of importance for processing this alloy, can be calculated from the dependence of MFS with the inverse absolute temperature; such a method was used to determine the temperature at which recrystallisation stops (Tnr). It was found that this temperature depends on strain rate, pass strain and interpass time. Results of the microstructure analysis of quenched samples are in good agreement with the values of Tnr.

Abstract: Precipitation of carbonitrides has been studied in as-cast slabs of one Nb and one Nb and Ti containing HSLA steel. The precipitates have been quantified using LOM and TEM. The measured size and number distributions was then compared to model calculations of precipitate nucleation and growth using estimates of the cooling rates in the austenitic range (1490oC to 800oC) during casting. Both average size and number distributions could be modelled with good agreement using identical model parameters (except for individual diffusion coefficients for the participating species). The model is based on classic nucleation rate theory and a quasistationary approximation for growth of spherical particles. Local equilibrium is assumed at the phase boundary.

Abstract: Currently new continuous casting processes such as thin slab caster or strip casting are industrialized or under developing in the world steel makers. In these casting processes, cooling rate after solidification becomes much faster compared with thick slab caster, and hot rolling mill connected directly with casting machine tends to be installed. The present study was conducted to investigate variations of austenitic grain size and micro segregation with cooling rate after solidification and also direct hot deformation conditions in austenite immediately after solidification in HSLA steels. HSLA steels were 0.15%C-0.25%Si-1.50%Mn, 0.028%Nb and 0.028%Nb-0.015%Ti with the same basic compositions. A hot working simulator of THERMECMASTER-Z was used, and the center part of tensile specimen set up in this machine was partially or fully levitation-melted by induction heating under argon gas atmosphere. After melting, specimens were cooled at cooling rate from 0.4K/s to 40K/s, and this range covered cooling rates after solidification in heavy thick slab caster and strip casting. Direct hot tensile straining in austenite after solidification was conducted at strain rates from 1.4×10-3s-1 to 2.6s-1, corresponding to an extracting speed in a respective caster. The increase of cooling rate refined continuously as cast austenitic grain size, and it was enhanced in micro alloyed steels. Micro segregation such as Mn was improved by faster cooling. Direct straining after solidification markedly refined austenitic grain size through dynamic or static recrystallization occurring depending on strain rate.

Abstract: Steel strip surface oxidation during hot mill processing represents an industrial and environmental problem: secondary oxide is removed after roughing, but tertiary oxide scales already start to form before entering the finishing stands. Their properties affect the final steel surface quality and its response to further processing. Controlling the oxide layer growth kinetics and mechanical properties can make pickling easier and improve downstream behaviour. A thin wustite-dominated scale layer (<20 μm) is created under controlled conditions in an original laboratory device adequately positioned in a compression test machine to investigate plane strain compression. A first series of oxidation tests were performed on a ULC steel grade to measure the kinetics of oxide scale growth. The samples were first heated up under a protective atmosphere (nitrogen), before being oxidised in air at different temperatures for various oxidation times. These experiments can be considered fair quantitative and qualitative simulations of scale growth as it occurs in a hot strip mill, insofar as the results thus obtained are in good agreement with the literature. After the oxide growth, plane strain compression (PSC) was performed immediately to simulate the hot rolling process. The oxide layers were characterised before and after compression tests by optical and secondary electron microscopy. As expected, the oxide is seen to deform during compression. The obtained oxide layers exhibit good adhesion to the substrate and homogeneity over the thickness, even after compression.