Dependence of fracture toughness of austempered ductile iron on austempering temperature

Ductile cast iron samples were austenitized at 927 °C and subsequently austempered for 30 minutes, 1 hour, and 2 hours at 260 °C, 288 °C, 316 °C, 343 °C, 371 °C, and 399 °C. These were subjected to a plane strain fracture toughness test. Fracture toughness was found to initially increase with austempering temperature, reach a maximum, and then decrease with further rise in temperature. The results of the fracture toughness study and fractographic examination were correlated with microstructural features such as bainite morphology, the volume fraction of retained austenite, and its carbon content. It was found that fracture toughness was maximized when the microstructure consisted of lower bainite with about 30 vol pct retained austenite containing more than 1.8 wt pct carbon. A theoretical model was developed, which could explain the observed variation in fracture toughness with austempering temperature in terms of microstructural features such as the width of the ferrite blades and retained austenite content. A plot of K _IC ² against σ _y (X _γ, C _γ)^1/2 resulted in a straight line, as predicted by the model.     

Microstructural development and austempering kinetics of ductile iron during thermomechanical processing

A new method of refining the microstructure of austempered ductile iron (ADI) by thermome chanical processing is investigated. Refinement of microstructure is effected by grain refinement of parent austenite by hot deformation in the austenitizing temperature range, before the austempering treatment. The effects of austenite deformation on the kinetics of austempering reaction and the microstructure development were studied using metallography and X-ray diffraction (XRD), at different austempering temperatures and deformations. The process window for optimum microstructure was determined in terms of the parameters involved. Deformation of 40 to 60 pct could be imparted in the temperature range 900 °C to 1025 °C, resulting in a reduction in the prior austenite grain size by 35 to 50 pct and ferrite size in ausferrite by 70 to 75 pct. The effects of austenitization temperature on the austempered microstructure were also studied.     

Microstructure and mechanical properties of Al-alloyed ductile iron upon casting and austempering

In the current study, Al was added to ductile iron (DI) in the range of 0·68–2·70 wt-% and its influence on the mechanical properties and on the microstructure at different section thicknesses was investigated. It was observed that increasing Al addition up to 2·70 wt-% improves the hardness and strength in the as-cast condition. However, this effect was completely reversed after austempering, where the mechanical properties decreased gradually with increasing Al content. In conclusion, Al reduced the strength of DI after austenitising at 900°C. Higher austempering temperatures may be required to achieve the desired properties depending on the Al content of the as-cast DI.     

Influence of stepped austempering process on the fracture toughness of austempered ductile iron

This research studied the effect of a two-step austempering process on the fracture toughness of ductile iron and compared it to that of the conventional upper- and lower-ausferrite austempered ductile irons (ADIs). The results showed that such a two-step austempering heat-treatment process yielded a fracture-toughness value equivalent to that of the upper-ausferrite ADI, while the hardness was maintained at the level of lower-ausferrite ADI. This provided a unique combination of high toughness with good hardness (strength) properties for the ADI with a two-step austempering. Optical microscopy, scanning electron microscopy (SEM), and X-ray diffraction analysis were performed to correlate the properties attained to the microstructural features.     

In-situ microstructural evolutions of 5Mn steel at elevated temperature in a transmission electron microscope

The microstructural evolutions of 5 Mn steel during various heat treatments have been investigated by in-situ transmission electron microscopy(TEM).The specimen of 5 Mn steel was prepared using focused ion beam(FIB)milling,which allowed the selection of specific morphology of interest prior to the in-situ observation.The complete austenization at 800°C was verified at the atomic scale by minimizing thermal expansion and sample drift in a heating holder based on micro-electro-mechanical-systems.During annealing at 650°C,the formation of reverted austenite was dynamically observed,while the morphologies of austenite laths of 5 Mn steel after in-situ heating were quite similar to that after ex-situ intercritical annealing.During annealing at 500°C,the morphological evolution of cementite and associated Mn diffusion were investigated.It was demonstrated that a combination of FIB sampling and high temperature in-situ TEM enables us to probe the morphological evolution and elemental diffusion of specific areas of interest in steel at high spatial resolution.     

Chemical composition and structural identification of eutectic carbide in 1 pct Mn ductile iron

Manganese, which may be used in ductile cast iron as a potent hardenability promoter, segregates in the intercellular region. This segregation becomes more severe as a consequence of poor inoculation, low cooling rate, or increasing of nominal Mn content in the alloy. In severely Mn-segregated regions, Mn eutectic carbide may be formed, which has a deteriorating effect on the mechanical properties of casting. In this study, a 1 Pct Mn ductile iron was used to investigate the chemical composition and crystal structure of the Mn eutectic carbide by electron microscopy (scanning and transmission), X-ray, and an electron probe microanalyzer (EPMA). Transmission electron microscope (TEM) and X-ray studies show that the crystal structure of carbide is orthorhombic with lattice parameters ofa = 14.825,b = 11.415, andc = 8.880 (Å). The concentrations of Mn, Si, and Cr in carbide, analyzed by scanning electron microscope-energy-dispersive X-ray spectrometer (SEM-EDX) and transmission electron microscope-energy-dispersive X-ray spectrometer (TEM-EDX), were 5.0 to 7.0, 0.5 to 2.8 and 1.5 to 2.2 (wt Pct), respectively. The ratio of Fe plus other metal atoms to C was calculated from EPMA experiments to be 2.5-2.9. It was shown that by diminishing Mn segregation, precipitated eutectic carbide can be reduced. It is expected that this can be achieved by reducing nominal content of Mn or by increasing nodule count.     

A high resolution transmission electron microscope study of early stage precipitation on dislocation lines in Al-Zn-Mg

The weak beam transmission electron microscopy technique was employed to study the early stages of precipitation on dislocation lines in Al-3.87 wt pct Zn-1.79 wt pct Mg. The heterogeneous precipitation sequence was found to follow the homogeneous sequence in this alloy. The interaction between the initial coherent precipitate particles and the strain fields of the catalyzing dislocations produced “gaps” of background intensity at precipitate locations along the otherwise continuous weak beam images of the dislocation lines. A simple model was developed to relate a distribution of measured weak beam gap lengths to a particle size distribution at a given aging treatment. In this manner the growth kinetics of the initial precipitate phase was observed; it was found that the precipitation followed the Cottrell-Bilbyt ^2/3law, suggesting that matrix dislocations may assist the growth of heterogeneous precipitates in a manner analogous to grain boundary “collector plates.” Weak beam microscopy was found to be superior to standard bright field microscopy for the current study. Particles too small to be visible in bright field were revealed in weak beam. Weak beam observations also indicated that the coherent precipitate particles were positioned asymmetrically about the dislocation cores.     

Neutron diffraction study of austempered ductile iron

Crystallographic properties of an austempered ductile iron (ADI) were studied by using neutron diffraction. A quantitative phase analysis based on Rietveld refinements revealed three component phases, α-Fe (ferrite), γ-Fe (austenite), and graphite precipitate, with weight fractions of 66.0, 31.5, and 2.5 pct, respectively. The ferrite phases of the samples were found to be tetragonal,14/mmm, with ac/a ratio of about 0.993, which is very close to the body-centered cubic (bcc) structure. The austenite phase had C atoms occupying the octahedral site of the face-centered cubic (fcc) unit cell with about 8 pct occupancy ratio. A strong microstrain broadening was observed for the two Fe phases of the samples. The particle sizes of the acicular ferrite phase were studied by using small angle neutron scattering. The analysis suggested a mean rod diameter of 700 A. The scattering invariant predicts a ferrite volume fraction consistent with the powder diffraction analysis. A textbook case of nodular graphite segregation, with average diameters ranging from 10 to 20 μm, was observed by optical micrography.     

Influence of the Mn content on the kinetics of austempering transformation in compacted graphite cast iron

Mossbauer spectroscopy has been used to monitor the kinetics of austempering transformation in two compacted graphite (CG) cast irons alloyed with 0.11 and 0.58 wt pct of Mn, respectively. The phase relations were analyzed in terms of the Johnson-Mehl’s equation, determining the kinetics parameters n (time exponent) and k (constant rate of the transformation). The values obtained were n=1.4 and k=7.47 × 10⁻³ s⁻¹ for the low-Mn alloy, and n=2.2 and k=3.9×10⁻³ s⁻¹ for the high-Mn alloy. These results, which reveal a faster kinetics for the low-Mn alloy, are coherent with metallographic observations, and the driving force obtained through the determination of the austenite carbon concentration that was determined from the Mossbauer data using the Genins model for the Fe-C configurations in the fcc lattice. The kinetics parameters are further compared to those obtained in austempered ductile iron (ADI), by analyzing the graphite morphology influence on the austempering transformation.     

AnIn Situ transmission electron microscope deformation study of the slip transfer mechanisms in metals

The slip transfer mechanisms across grain boundaries in 310 stainless steel, high-purity aluminum, and a Ni-S alloy have been studied by using thein situ transmission electron microscope (TEM) deformation technique. Several interactions between mobile lattice dislocations and grain boundaries have been observed, including the transfer and generation of dislocations at grain boundaries and the nucleation and propagation of a grain boundary crack. Quantitative conditions have been established to correctly predict the slip transfer mechanism. This paper is based on a presentation made in the symposium “Interface Science and Engineering” presented during the 1988 World Materials Congress and the TMS Fall Meeting, Chicago, IL, September 26–29, 1988, under the auspices of the ASM-MSD Surfaces and Interfaces Committee and the TMS Electronic Device Materials Committee.     

Photochemically induced focal cochlear lesions in the guinea pig: II. A transmission electron microscope study

We report the characterization of a de novo unbalanced chromosome rearrangement by comparative genomic hybridization (CGH) in a 15-day-old child with hypotonia and dysmorphia. We describe the combined use of CGH and fluorescence in situ hybridization (FISH) to identify the origin of the additional chromosomal material on the short arm of chromosome 6. Investigation with FISH revealed that the excess material was not derived from chromosome 6. Identification of unknown unbalanced aberrations that could not be identified by traditional cytogenetics procedures is possible by CGH analysis. Visual analysis of digital images from CGH-metaphase spreads revealed a predominantly green signal on the telomeric region of chromosome 10p. After quantitative digital ratio imaging of 10 CGH-metaphase spreads, a region of gain was found in the chromosome band 10p14-pter. The CGH finding was confirmed by FISH analysis, using a whole chromosome 10 paint probe. These results show the usefulness of CGH for a rapid characterization of de novo unbalanced translocation, unidentifiable by karyotype alone.     

In-situ straining of Ni3Al in a transmission electron microscope

TEM in-situ straining experiments have been performed on thin foils of Ni₃Al and Ni₃Al containing 750 ppm (0.35 at.%) boron. During the straining, gliding APB-coupled dislocations were observed to leave superlattice intrinsic stacking faults (S-ISF's) as debris in their wake confirming a mechanism for S-ISF formation first suggested by Pak et al. [Scripta metall.19, 1081 (1976)]. The APB-coupled dislocations (i) pile-up at grain boundaries, (ii) become extrinsic grain boundary dislocations and (iii) initiate slip in adjacent grains. The characteristics of the crack propagation process indicated that plastic flow, albeit localised, precedes fracture.     

Thy-1 immunolabeled thymocyte microdomains studied with the atomic force microscope and the electron microscope

The atomic force microscope (AFM) and the transmission electron microscope (TEM) have been used to study the morphology of isolated mouse thymocyte microdomains and Thy-1 antigen distribution at the surface of these structures. AFM images were recorded in air in the contact mode on membrane vesicles deposited on previously heated tissue culture plastic sheets and indirectly immunolabeled for Thy-1 expression with colloidal gold-conjugated secondary antibodies. AFM images of untreated plastic plates showed a very characteristic network of streaks 20-200 nm wide. Heating the plastic removed the streaks and provided flat surfaces (r.m.s. 1 nm). This substrate allowed strong adsorption and homogeneous spreading of the vesicles and easy manipulations during immunolabeling experiments. Vesicles flattened on the substrate without losing their morphology. The 10-nm membrane-bound gold beads were reproducibly imaged without degradation by repeated tip scanning. The observed microdomains had a mean diameter of 184 +/- 76 nm, and 65% of them were specifically labeled. Images obtained with the TEM on the same vesicles, deposited on carbon-coated grids and negatively stained, confirmed the AFM observations. The size distribution of the microdomains was quite similar, but the number of beads per vesicle was significantly higher, and 76% of the vesicles were labeled. The difference may be explained 1) by removal of beads from the vesicles in the additional washing step with water, which was necessary for the AFM; 2) by tip-sample convolution; and 3) by statistical fluctuations.     

An analytical electron microscope study of the kinetics

The detection and quantification of the segregation of Bi to grain boundaries in Cu using Analytical Electron Microscopy is demonstrated and the effects of time and temperature are observed. The experimental data are compared with the theoretical prediction of McLean’s segregation isotherm. Special grain boundaries are also considered. The analysis shows that the detection of the variation of segregation with time and temperature as well as grain boundary characteristics is possible using analytical electron microscopy and that the quantification techniques used here agree well with theoretical calculations of the segregant levels.     

A scanning electron microscope study of the interstitial tissue of the canine testis

Scanning electron microscopy (SEM) is a potent tool that is especially valuable in interpreting the three-dimensional relationships of cells within tissues. This type of information is obtainable from thin sections in transmission electron microscopy (TEM) only by reconstructions of serial sections. The arrangement of the interstitial cells of the testis in relation to the capillaries and lymphatic channels, in particular, is easier to visualize in SEM than in TEM. Cytoplasmic constituents, as well as cell surface modifications, are demonstrable by this technique. The presence of droplets, presumably lipid droplets, both within and on the Leydig cells and the lymphatic endothelial cells, is quite evident. Other cytoplasmic structures are also apparent. For example, the possible functional significance of "openings" that are seen by SEM on the septa that surround lipid droplets is discussed relative to the appearance of the same area as seen in thin sections or in freeze-fracture replicas. SEM should become a very useful method for studying cytological and morphological alterations that occur in testicular tissue that is subjected to physical or chemical manipulation.