Hot deformation and recrystallization of austenitic stainless steel: Part 11. post-deformation recrystallization

The postdeformation recrystallization behavior of a hot-deformed austenitic stainless steel was investigated based on the first part of this study, in which the microstructure development during hot deformation and, in particular, the evolution of dynamic recrystallization (DRX), was studied. The effect of different parameters such as strain, strain rate, and temperature were examined. The dependency of the time for 50 pct softening, t 50, changed from “strain dependent” to “strain independent” at a transition strain (ε*) that was in the steady-state area of the hot deformation flow curve. The fully recrystallized microstructure showed a similar transition in strain sensitivity. However, this occurred at stains greater than ε*. A mathematical model was developed to predict the transition strain under different deformation conditions. Microstructural measurements show that the transition strain corresponds to approximately 50 pct DRX in the deformed structure at the point of unloading.

Mechanisms of dynamic strain induced transformation and post-deformation evolution

In this study, a novel experimental approach was applied to study the mechanism of the equiaxed shape retention in dynamic strain induced ferrite during deformation. The post-deformation ferrite evolution in both static and dynamic transformation was studied. The refinement potential and the origin of their differences in both mechanisms were analysed.

Microstructure evolution and softening processes occurring during annealing of hot deformed Ni-30Fe austenite

The current work investigates the microstructure evolution and softening processes that take place during annealing of an austenitic Ni-30Fe model alloy subjected to hot deformation in the dynamic recrystallization (DRX) regime. The substructure of the deformed matrix grains largely comprised organized microband arrays, though that of the DRX grains consisted of more random, complex subgrain/cell arrangements. This substructure disparity was also reflected by the distinct difference in the mechanism of post-deformation softening taking place during annealing of the deformed matrix and DRX grains. In the former, the recrystallization process took place through nucleation and growth of new grains fully replacing the deformed structure, as expected for the classical static recrystallization (SRX). The corresponding texture was essentially random, in contrast to that of the DRX grains dominated by low Taylor factor components. The microbands originally present within the deformed matrix grains displayed some tendency to disintegrate during annealing, nonetheless, they remained largely preserved even at prolonged holding times. During annealing of the fully DRX microstructure, a novel softening mechanism was revealed. The initial post-dynamic softening stage involved rapid growth of the dynamically formed nuclei and migration of the mobile boundaries in correspondence with the well-established metadynamic recrystallization (MDRX) mechanism. However, in contrast to the deformed matrix, SRX was not observed and the sub-boundaries within DRX grains rapidly disintegrated through dislocation climb and dislocation annihilation, which led to the formation of dislocation-free grains already at short holding times. Consequently, the DRX texture initially became slightly weakened and then remained largely preserved throughout the annealing process.

Microstructural characterization of the austenite behaviour during metadynamic recrystallization

The work discusses the recent findings obtained from the microstructural characterization of an austenitic Ni-30%Fe model alloy during metadynamic recrystallization (MDRX) using both EBSD and TEM techniques. The characterization of the grain structure, texture and dislocation substructure evolution of the fully dynamically recrystallized (DRX) microstructure during post deformation annealing revealed a novel softening mechanism occurring under the current experimental conditions. It is proposed that the initial softening stage involves rapid growth of the dynamically formed nuclei and migration of the mobile boundaries in correspondence with the well-established MDRX mechanism. However, the sub-boundaries within DRX grains progressively disintegrate through dislocation climb and dislocation annihilation, which ultimately leads to the formation of dislocation-free grains. Consequently, the DRX texture largely remains preserved throughout the annealing process.

Evolution of strain-induced precipitates in a model austenitic Fe-30Ni-Nb steel and their effect on the flow behaviour

The present work investigated the evolution of strain-induced NbC precipitates in a model austenitic Fe-30Ni-Nb steel deformed at 925 °C to a strain of 0.2 during post-deformation holding between 3 and 1000 s and their effect on the reloading flow stress. The precipitate particles preferentially nucleated on the nodes of the periodic dislocation networks constituting microband walls. Holding for 10 s resulted in the formation of fine, largely coherent NbC particles with a mean diameter of ∼5 nm, which displayed a cube-on-cube orientation relationship with austenite and caused the maximum increase in the reloading steady-state flow stress. A further increase in the holding time from 30 to 1000 s led to the formation of semi-coherent, gradually coarser and more widely spaced particles with a mean diameter of 8 nm and above, which led to a gradual decrease in the reloading steady-state flow stress. The holding time increase resulted in progressive disintegration of the dislocation substructure and dislocation annihilation through static recovery processes, which was also reflected by the measured softening fractions. The precipitate particle shape changed during post-deformation annealing from elliptical to faceted octahedral and subsequently to tetra-kai-decahedral. © 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Post-growth and in situ annealing on GaInNAs(Sb) and their application in 1.55 mu m lasers

Rapid thermal annealing (RTA) has been demonstrated as an important way to improve the crystal quality of GaInNAs(Sb)/GaAs quantum wells. However little investigation has been made into their application in laser growth, especially at a wavelength of 1.55 mu m. When a GaAs-based laser is grown, AlGaAs is usually used for cladding layers. The growth of the p-cladding layer usually takes 30-45 min at a growth temperature higher than that of the GaInNAs(Sb) active region, which affects the material quality. To investigate this effect, various post-growth annealing processes were performed to simulate this process. Great enhancement of the PL intensity was obtained by a two-step process which consisted of annealing first at 700 degrees C for 60 s and then at 600 degrees C for 45 min. We transferred this post-growth annealing to in situ annealing. Finally, a GaInNAsSb laser was grown with a 700 degrees C in situ annealing process. Continuous operation at room temperature of a GaAs-based dilute nitride laser with a wavelength beyond 1.55 mu m was realized for the first time.

Crack formation due to annealing of Al2O3 films grown on Si(100) by MOCVD

We report crack formation in alumina films grown on Si(100), caused by annealing in a controlled oxidizing ambient. The films were grown in a low-pressure CVD reactor, using aluminium acetylacetonate as precursor. High purity argon and nitrous oxide were employed as carrier and oxidizing gas, respectively. The films were characterized by optical microscopy and SEM/EDAX. The proportion and chemical nature of the heteroatoms, namely C and H, incorporated into the films from the precursor, were characterized by XPS, and FTIR. As-deposited films do not exhibit any cracks, while post-deposition annealing results in cracks. Apart from the delamination of the films, annealing in nitrous oxide ambient leads to an unusual crack geometry, which we term the “railway-track”. These twin cracks are very straight and run parallel to each other for as much as several millimeters. Often, two such linear tracks meet at exactly 90°. Between some of these tracks lie bullet-like structures with very sharp tips, oriented in a specific direction. As cracks are generally activated by residual stress, both thermal and intrinsic, the origins of the stresses that generate these linear cracks are discussed. The redistribution of stress, arising from the removal of C and H during annealing, will also be discussed. An attempt has been made to correlate the formation of cracks with the crystal structure of the film.

Effect of semi-solid heat treatment on elevated temperature plasticity of 304L stainless steel

The present work explores the potential of semi-solid heat treatment technique by elucidating its effect on the plastic behavior of 304L SS in hot working domain. To accomplish this objective, hot isothermal compression tests on 304L SS specimens with semi-solid heat treatment and conventional annealing heat treatment have been carried out within a temperature range of 1273-1473 K and strain rates ranging from 0.01 to 1 s(-1). The dynamic flow behavior of this steel in its conventional heat-treated condition and semi-solid heat-treated condition has been characterized in terms of strain hardening, temperature softening, strain rate hardening, and dynamic flow softening. Extensive microstructural investigation has been carried out to corroborate the results obtained from the analysis of flow behavior. Detailed analysis of the results demonstrates that semi-solid heat treatment moderates work hardening, strain rate hardening, and temperature sensitivity of 304L SS, which is favorable for hot deformation. The post-deformation hardness values of semi-solid heat-treated steel and conventionally heat-treated steel were found to remain similar despite the pre-deformation heat treatment conditions. The results obtained demonstrate the potential of semi-solid heat treatment as a pre-deformation heat treatment step to effectively reduce the strength of the material to facilitate easier deformation without affecting the post-deformation properties of the steel.

Annealing effects on electron-beam evaporated Al2O3 films

The effects of post-deposited annealing on structure and optical properties of electron-beam evaporated Al2O3 single layers were investigated. The films were annealed in air for 1.5 h at different temperatures from 250 to 400 degrees C. The optical constants and cut-off wavelength were deduced. Microstructure of the samples was characterized by X-ray diffraction (XRD). Profile and surface roughness measurement instrument was used to determine the rms surface roughness. It was found that the cut-off wavelength shifted to short wavelength as the annealing temperature increased and the total optical loss decreased. The film structure remained amorphous even after annealing at 400 degrees C temperature and the samples annealed at higher temperature had the higher rms surface roughness. The decreasing total optical loss with annealing temperature was attributed to the reduction of absorption owing to oxidation of the film by annealing. Guidance to reduce the optical loss of excimer laser mirrors was given. (c) 2004 Elsevier B.V. All rights reserved.

Evolution of vertical phase separation in P3HT:PCBM thin films induced by thermal annealing

The achievement of the desirable morphology at the nanometer scale of bulk heterojunctions consisting of a conjugated polymer with fullerene derivatives is a prerequisite in order to optimize the power conversion efficiency of organic solar cells. The various experimental conditions such as the choice of solvent, drying rates and annealing have been found to significantly affect the blend morphology and the final performance of the photovoltaic device. In this work, we focus on the effects of post deposition thermal annealing at 140 °C on the blend morphology, the optical and structural properties of bulk heterojunctions that consist of poly(3-hexylthiophene) (P3HT) and a methanofullerene derivative (PCBM). The post thermal annealing modifies the distribution of the P3HT and the PCBM inside the blend films, as it has been found by Spectroscopic Ellipsometry studies in the visible to far-ultraviolet spectral range. Phase separation was identified by AFM and GIXRD as a result of a slow drying process which took place after the spin coating process. The increase of the annealing time resulted to a significant increase of the P3HT crystallinity at the top regions of the blend films. © 2011 Elsevier B.V. All rights reserved.

Fabrication of Nano-structured VOx Film by Low Temperature Ion Beam Sputtering and Reductive Annealing

VOx thin films have been fabricated by low temperature ion beam sputtering and post reductive annealing process. Semiconductor-metal phase transition is observed for the film annealed at 400 degrees C for 2 hours. The film also shows a polycrystal structure with grain size from 50nm to 150nm. The VOx thin films fabricated by this process have a TCR up to -2.7% at room temperature. Our results indicate a promising fabrication method of the nano-structured VOx film with relatively high TCR and semiconductor-metal phase transition.

Effects of annealing treatment on the formation of CO2 in ZnO thin films grown by metal-organic chemical vapor deposition

Post-growth annealing was carried out on ZnO thin films grown by metal-organic chemical vapor deposition (MOCVD). The grain size of ZnO thin film increases monotonically with annealing temperature. The ZnO thin films were preferential to c-axis oriented after annealing as confirmed by Xray diffraction (XRD) measurements. Fourier transformation infrared transmission measurements showed that ZnO films grown at low temperature contains CO2 molecules after post-growth annealing. A two-step reaction process has been proposed to explain the formation mechanism of CO2, which indicates the possible chemical reaction processes during the metal-organic chemical vapor deposition of ZnO films.

Effects of thermal annealing on polymer photovoltaic cells with buffer layers and in situ formation of interfacial layer for enhancing power conversion efficiency

We have investigated the effects of thermal annealing before and after cathode deposition on poly(3-hexylthiophene)(P3HT)/[6,6]-phenyl C61-butyric acid methyl ester (PCBM) blend photovoltaic cells with different cathode buffer layers. The introduction of cathode buffer layer such as lithium fluoride (LiF) and calcium oxide (CaO) in pre-annealing cells can increase the open-circuit voltage (V-oc) and the power conversion efficiency (PCE). Post thermal annealing after cathode deposition further enhanced the PCE of the cells with LiF/Al cathode.