73 research outputs found

    An in-depth investigation of the cutting speed impact on the degraded microstructure of worn PCBN cutting tools

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    The impact of an increased cutting speed on the degradation of a low content polycrystalline cubic boron nitride (PCBN) tool material is investigated by advanced microscopy techniques. The locally affected microstructure of worn PCBN cutting tools, after dry hard turning, is studied by high precision in situ lift-out cross sections taken from across the crater, formed on the rake face. The cross sections are studied with scanning electron microscopy, transmission electron microscopy (TEM) with electron energy loss spectroscopy and, primarily, energy filtered TEM. Advanced analysis techniques are crucial to illustrate the degradation mechanisms taking place locally at micro- and nano-metre levels during the machining operation. Results show that a higher cutting speed drastically affects the wear surface of the cutting edge. While an adherent layer, consisting of elements from the workpiece material, covers practically the whole wear surface at a lower cutting speed, it is only partially distributed at a higher cutting speed. Results also show significant differences in the local microstructure of the affected worn zone with an increase in cutting speed. The chemical degradation will go from tool-workpiece interface wear with smooth wear surfaces and almost no interaction with material below the wear surface at lower cutting speed to a severe penetration into the tool material by partially oxidised Fe-rich features at higher cutting speed. The more aggressive degradation behaviour at the higher cutting speed is also more localised. Single chemically worn cBN grains are for example shown. The dominating wear mechanism is shown to be chemical degradation, which accelerates with a higher cutting speed. The cBN phase is more affected than the major matrix phase, Ti(C,N)

    Oxidation induced localized creep deformation in Zircaloy-2

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    Extensive plastic deformation in the metal underneath the oxide scale in autoclave tested Zircaloy-2 was studied using transmission electron microscopy (TEM). It was concluded that the plastic deformation is created by creep during oxidation, and is not caused by surface treatment, sample preparation or cooling from autoclave temperatures. Evidence of large strains was found in the form of dislocation tangles, dis- location patches and sub-grain formation, and also indications of twinning were found. The heavily deformed layer is around a few lm thick and no obvious difference could be seen between alloys with different strength or different oxide thickness

    Tin clustering and precipitation in the oxide during autoclave corrosion of Zircaloy-2

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    Atom probe tomography has been used to study the evolution of tin distribution during the corrosion process in Zircaloy-2. From being completely soluble in the Zr metal matrix, some clustering is evident already in the newly formed oxide close to the metal-oxide interface. Analysis of thicker oxides a few hundred nanometers away from the interface reveals fully developed precipitates of metallic Sn particles of up to 20 nm in size. Although the precipitates contain significant amounts of Zr, it is concluded that they are in the process of being depleted in Zr, which is limited only by the slow diffusion in the oxide scale. The findings are interpreted as being a result of the nobility of the Sn yielding a strong driving force to remain in a metallic state after incorporation in the barrier oxide layer. As Sn occupies substitutional sites in the ZrO2 lattice it is oxidized to a 4+ state when incorporated into the oxide, and in order to remain metallic it must nucleate into precipitates within the inner part of the oxide scale before being re-oxidized to 2+ and eventually to 4+ when the oxygen activity is sufficiently high in the outer parts of the oxide

    Quantitative APT analysis of Ti(C,N)

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    A specially produced Ti(C,N) standard material, with a known nominal composition, was investigated with laser assisted atom probe tomography. The occurrence of molecular ions and single/multiple events was found to be influenced by the laser pulse energy, and especially C related events were affected. Primarily two issues were considered when the composition of Ti(C,N) was determined. The first one is connected to detector efficiency, due to the detector dead-time. The second one is connected to peak overlap in the mass spectrum. A method is proposed for quantification of the C content in order to establish the C/N ratio. A correction was made to the major C peaks, C at 6 and 12 Da, with the 13C isotopes, at 6.5 and 13 Da, according to the known natural abundance. In addition, a correction of the peak at 24 Da, where C and Ti overlap, is proposed based on the occurrence of single/multiple events for respective element. The results were compared to the results from other techniques such as electron energy loss spectroscopy, chemical analysis and X-ray diffraction. After applying the corrections, atom probe tomography results were satisfactory. Furthermore, the content of dissolved O in Ti(C,N) was successfully quantified. \ua9 2011 Elsevier B.V

    Redistribution of alloying elements in Zircaloy-2 after in-reactor exposure

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    An atom probe tomography study of the microstructure of a Zircaloy-2 material subjected to 9 annual cycles of BWR exposure has been conducted. Upon dissolution of secondary phase particles, Fe and Cr are seen to reprecipitate in large numbers of clusters and particles of 1-5 nm sizes throughout the Zr metal matrix. Fe and Sn were observed to segregate to ring-shaped features in the metal that are interpreted to be <c>-component vacancy loops. This implies that these two elements play a major role in the irradiation growth phenomenon in Zr alloys, which is believed to be caused by the formation of <c>-loops. Similarly to autoclave-corroded Zr alloys, the formation of a sub-oxide layer of approximate composition ZrO was observed. On the other hand, no oxygen saturated metal phase was detected underneath the oxide scale

    CrN–NbN nanolayered coatings for enhanced accident tolerant fuels in BWR

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    The accident tolerant fuel (ATF) concept has emerged in the years after the 2011 Fukushima accident as part of a renewed effort in research for light water reactors. The primary focus is to further improve safety measures under and beyond design basis accident conditions, and to improve fuel cladding performance in normal operation. The application of a coating on zirconium claddings can achieve both these aims without extensive changes to the reactor design. Metallic chromium coatings have been profusely studied as solution for pressurized water reactors, but the search for an effective ATF coating able to withstand the environment inside boiling water reactors (BWRs) is still ongoing. In this work, two different versions of a novel nitride coating composition were studied. Zirconium claddings coated with 8 µm thick layers of superlattice CrN–NbN and a nanolayered CrN–NbN were tested in autoclave under BWR operating conditions for 60 days. Scanning electron microscopy, transmission electron microscopy, energy dispersive x-ray spectroscopy, electron back-scattered diffraction, x-ray diffraction, and atom probe tomography were employed to characterize as-deposited and autoclaved samples of these two materials. During exposure, both coating versions formed a stable, dense and passivating oxide scale (200–300 nm thick) on the surface, demonstrating improved oxidation protection under operating conditions. Some differences in the oxide growth mechanism were observed between the superlattice and the nanolayered CrN–NbN coatings, which allowed to glimpse at the effect of the layer thickness on the oxidation protection provided by these coatings. The nano-structured morphology of both coatings remained unaffected by the autoclave test, but a 35 nm thick Zr-Cr-N phase was found at the coating-substrate interface of the superlattice CrN–NbN coated cladding

    Quantitative atom probe analysis of carbides

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    Compared to atom probe analysis of metallic materials, the analysis of carbide phases results in an enhanced formation of molecular ions and multiple events. In addition, many multiple events appear to consist of two or more ions originating from adjacent sites in the material. Due to limitations of the ion detectors measurements generally underestimate the carbon concentration. Analyses using laser-pulsed atom probe tomography have been performed on SiC, WC, Ti(C,N) and Ti 2 AlC grains in different materials as well as on large M 2 3C 6 precipitates in steel. Using standard evaluation methods, the obtained carbon concentration was 6-24% lower than expected from the known stoichiometry. The results improved remarkably by using only the 13 C isotope, and calculating the concentration of 12 C from the natural isotope abundance. This confirms that the main reason for obtaining a too low carbon concentration is the dead time of the detector, mainly affecting carbon since it is more frequently evaporated as multiple ions. In the case of Ti(C,N) andTi 2 AlC an additional difficulty arises from the overlap between C 2 + ,C 2+ 4 and Ti 2+ at the mass-to-charge 24 Da. \ua9 2010 Elsevier B.V

    Selection for Heterozygosity Gives Hope to a Wild Population of Inbred Wolves

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    Recent analyses have questioned the usefulness of heterozygosity estimates as measures of the inbreeding coefficient (f), a finding that may have dramatic consequences for the management of endangered populations. We confirm that f and heterozygosity is poorly correlated in a wild and highly inbred wolf population. Yet, our data show that for each level of f, it was the most heterozygous wolves that established themselves as breeders, a selection process that seems to have decelerated the loss of heterozygosity in the population despite a steady increase of f. The markers contributing to the positive relationship between heterozygosity and breeding success were found to be located on different chromosomes, but there was a substantial amount of linkage disequilibrium in the population, indicating that the markers are reflecting heterozygosity over relatively wide genomic regions. Following our results we recommend that management programs of endangered populations include estimates of both f and heterozygosity, as they may contribute with complementary information about population viability
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