13 resultados para (900 1170) °C

em Deakin Research Online - Australia


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A rapid method has been developed to determine recrystallization kinetics of Nb microalloyed steels by interrupted hot torsion test. The softening behaviour was achieved as a function of different processing parameters. The method clearly identified three regions, where the strain dependency of the recrystallization rate varied. Firstly, at large strains the rate of recrystallization was not a function of strain; this is generally ascribed to metadynamic recrystallization. At lower strains the time to 50% recrystallization showed a power low relationship with strain, characteristic of static recrystallization. A further break point exists on the time for 50% softening curve when strain induced precipitation occurs in the material. The onset of strain induced precipitation was at strains below the strain to the peak stress at temperatures below 900&deg;C. The experimental results were used to estimate the time for 50% softening and to anticipate the onset of the strain induced precipitation for the alloy of this study. Grain refinement of the recrystallized austenite continued to strains significantly beyond the peak stress and beyond the static to metadynamic recrystallization rate transition.<br />

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Boron nitride (BN) nanotubes have the same nanostructure as carbon nanotubes but are found to exhibit significant resistance to oxidation at high temperatures. Our systematic study has revealed that BN nanotubes are stable at 700 &deg;C in air and that some thin nanotubes (diameter less than 20 nm) with perfect multiwalled cylindrical structure can survive up to 900 &deg;C. Thermogravimetric analysis reveals an onset temperature for oxidation of BN nanotubes of 800 &deg;C compared with only 400 &deg;C for carbon nanotubes under the same conditions. This more pronounced resistance of BN nanotubes to oxidation is inherited from the hexagonal BN and also depends on the nanocrystalline structure. This high level of resistance to oxidation allows promising BN nanotube applications at<br />high temperatures<br />

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In order to improve the understanding of the dynamic and post-dynamic recrystallization behaviours of AISI 304 austenitic stainless steel, a series of hot torsion test have been performed under a range of deformation conditions. The mechanical and microstructural features of dynamic recrystallization (DRX) were characterized to compare and contrast them with those of the post-dynamic recrystallization. A necklace type of dynamically recrystallized microstructure was observed during hot deformation at 900 &deg;C and at a strain rate of 0.01 s<sup>&minus;1</sup>. Following deformation, the dependency of time for 50% recrystallization, t<sub>50</sub>, changed from &ldquo;strain dependent&rdquo; to &ldquo;strain independent&rdquo; at a transition strain (&epsilon;<sup>*</sup>), which is significantly beyond the peak. This transition strain was clearly linked to the strain for 50% dynamic recrystallization during deformation. The interrelations between the fraction of dynamically recrystallized microstructure, the evolution of post-dynamically recrystallized microstructure and the final grain size have been established. The results also showed an important role of grain growth on softening of deformed austenite.<br />

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The aim of the present work was to undertake a detailed investigation of the softening mechanisms during hot deformation of a 21Cr-10Ni-3Mo (steel A) and a 21Cr-8Ni-3Mo (steel B) austenite/ferrite duplex stainless steels containing about 60% and 30% of austenite, respectively. The steels were subjected to hot deformation in torsion performed at 900 &ordm;C and 1200 &ordm;C using a strain rate of 0.7 s-1 to several strain levels. Quantitative optical and transmission electron microscopy were used in the investigation. Austenite was observed to soften via dynamic recovery (DRV) and dynamic recrystallisation (DRX) accompanied by DRV for the deformation temperatures of 900 &deg;C and 1200 &deg;C, respectively, for the both steels studied. DRX of austenite largely occurred through strain-induced grain boundary migration, complemented by (multiple) twinning, and developed significantly faster in steel A than in steel B, indicating that considerably larger strains partitioned into austenite in the former steel during deformation at 1200 &deg;C. The above softening mechanism was accompanied by the formation of DRX grains from subgrains along the austenite/ferrite interface and by large-scale subgrain coalescence. At 900&deg;C, stressassisted phase transitions between austenite and ferrite were observed, characterised by dissolution of the primary austenite, formation of Widmanst&auml;tten secondary austenite and gradual globularisation of the microstructure with increasing strain. These processes appeared to be significantly more widespread in steel B. The softening mechanism within ferrite for the both steels studied was classified as &ldquo;continuous DRX&rdquo;, characterised by a gradual increase in misorientations between neighbouring subgrains with strain, for the both deformation temperatures.<br />

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Shear bands formed during both cold and hot plastic deformation have been linked with several proposed mechanisms for the formation of ultrafine grains. The aim of the present work was to undertake a detailed investigation of the microstructural and crystallographic characteristics of the shear bands formed during hot deformation of a 22Cr-19Ni-3Mo (mass%) austenitic stainless steel and a Fe-30 mass%Ni based austenitic model alloy. These alloys were subjected to deformation in torsion and plane strain compression (PSC), respectively, at temperatures of 900&deg;C and 950&deg;C and strain rates of 0.7s<sub>-1</sub> and 10s<sub>-1</sub>, respectively. Transmission electron microscopy and electron backscatter diffraction in conjunction with scanning electron microscopy were employed in the investigation. It has been observed that shear bands already started to form at moderate strains in a matrix of pre-existing microbands and were composed of fine, slightly elongated subgrains (fragments). These bands propagated along a similar macroscopic path and the subgrains, present within their substructure, were rotated relative to the surrounding matrix about axes approximately parallel to the sample radial and transverse directions for deformation in torsion and PSC, respectively. The subgrain boundaries were largely observed to be non-crystallographic, suggesting that the subgrains generally formed via multiple slip processes. Shear bands appeared to form through a co-operative nucleation of originally isolated subgrains that gradually interconnected with the others to form long, thin bands that subsequently thickened via the formation of new subgrains. The observed small dimensions of the subgrains present within shear bands and their large misorientations clearly indicate that these subgrains can serve as potent nucleation sites for the formation of ultrafine grain structures during both subsequent recrystallisation, as observed during the present PSC experiments, and phase transformation.<br />

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The evolution of crystallographic texture and deformation substructure was studied in a type 316L austenitic stainless steel, deformed in rolling at 900 &deg;C to true strain levels of about 0.3 and 0.7. Electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used in the investigation and a comparison of the substructural characteristics obtained by these techniques was made. At the lower strain level, the deformation substructure observed by EBSD appeared to be rather poorly developed. There was considerable evidence of a rotation of the pre-existing twin boundaries from their original orientation relationship, as well as the formation of highly distorted grain boundary regions. In TEM, at this strain level, the substructure was more clearly revealed, although it appeared rather inhomogeneously developed from grain to grain. The subgrains were frequently elongated and their boundaries often approximated to traces of {111} slip planes. The corresponding misorientations were small and largely displayed a non-cumulative character. At the larger strain, the substructure within most grains became well developed and the corresponding misorientations increased. This resulted in better detection of sub-boundaries by EBSD, although the percentage of indexing slightly decreased. TEM revealed splitting of some sub-boundaries to form fine microbands, as well as the localized formation of microshear bands. The substructural characteristics observed by EBSD, in particular at the larger strain, generally appeared to compare well with those obtained using TEM. With increased strain level, the mean subgrain size became finer, the corresponding mean misorientation angle increased and both these characteristics became less dependent on a particular grain orientation. The statistically representative data obtained will assist in the development of physically based models of microstructural evolution during thermomechanical processing of austenitic stainless steels.<br />

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&alpha;-Al<sub>2</sub>O<sub>3 </sub>nanowires, with diameter around 10 nm, were synthesized in bulk quantity by heating the mixture of pure aluminum and graphite powders at 900 &deg;C. Scarcity of oxygen is regarded as the reason for the growth of the small diameter &alpha;-Al<sub>2</sub>O<sub>3</sub> nanowires at relatively low temperature. The product was characterized by field emission scanning electron microscopy, high-resolution transmission electron microscopy and photoluminescence. The Oxygen vacancies in the nanowires lead to the strong photoluminescence in the wavelength range of 400&ndash;700 nm with its peak at 527 nm.<br />

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In this work, we investigated the oxygen permeation properties of barium bismuth iron oxide within the family of [Ba<sub>2&minus;3</sub><i><sub>x</sub></i>Bi<sub>3<i>x</i>&minus;1</sub>][Fe<sub>2</sub><i><sub>x</sub></i>Bi<sub>1&minus;2</sub><i><sub>x</sub></i>]O<sub>2+3<i>x</i>/2</sub> for <i>x</i> = 0.17&ndash;0.60. The structure changed progressively from cubic to tetragonal and then to hexagonal as function of x in accordance with the different relative amounts of bismuth on A-site and B-site of ABO<sub>3&minus;&delta;</sub> perovskite lattices. We found that the oxygen flux and electrical conductivity correlated strongly, and it was prevalent for the cubic structure (<i>x</i> = 0.33&ndash;0.40) which conferred the highest oxygen flux of 0.59 ml min<sup>&minus;1</sup> cm<sup>&minus;2</sup> at 950 &deg;C for a disk membrane <i>x</i> = 0.33 with a thickness of 1.2 mm. By reducing the thickness of the disk membrane to 0.8 mm, the oxygen flux increased to 0.77 ml min<sup>&minus;1</sup> cm<sup>&minus;2</sup>, suggesting both surface kinetics and ion diffusion controlled oxygen flux, though the former was more prominent at higher temperatures. For disk membranes <i>x</i> = 0.45&ndash;0.60, the perovskite structure changed to tetragonal and hexagonal, and the oxygen flux was insignificant below 900 &deg;C, clearly indicating electron conduction properties only. However, for two compositions with relatively high bismuth content, e.g. <i>x</i> = 0.55 and 0.60, there was a sudden and significant rise of oxygen permeability above 900 &deg;C, by more than one order of magnitude. These materials changed conduction behavior from metallic to semiconductor at around 900 &deg;C. These results suggest the advent of mixed ionic electronic conducting properties caused by the structure transition as bismuth ions changed their valence states to compensate for the oxygen vacancies formed within the perovskite lattices.<br />

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This study characterizes BaCo0.7Fe0.2Nb0.1O3&minus;&delta; (BCFN) perovskite oxide and evaluates it as a potential cathode material for proton-conducting SOFCs with a BaZr0.1Ce0.7Y0.2O3-&delta; (BZCY) electrolyte. A four-probe DC conductivity measurement demonstrated that BCFN has a modest electrical conductivity of 2&ndash;15 S cm&minus;1 in air with p-type semiconducting behavior. An electrical conductivity relaxation test showed that BCFN has higher Dchem and Kchem than the well-known Ba0.5Sr0.5Co0.8Fe0.2O3&minus;&delta; oxide. In addition, it has relatively low thermal expansion coefficients (TECs) with values of 18.2 &times; 10&minus;6 K&minus;1 and 14.4 &times; 10&minus;6 K&minus;1 at temperature ranges of 30&ndash;900 &deg;C and 30&ndash;500 &deg;C, respectively. The phase reaction between BCFN and BZCY was investigated using powder and pellet reactions. EDX and XRD characterizations demonstrated that BCFN had lower reactivity with the BZCY electrolyte than strontium-containing perovskite oxides such as SrCo0.9Nb0.1O3-&delta; and Ba0.6Sr0.4Co0.9Nb0.1O3&minus;&delta;. The impedance of BCFN was oxygen partial pressure dependent. Introducing water into the cathode atmosphere reduced the size of both the high-frequency and low-frequency arcs of the impedance spectra due to facilitated proton hopping. The cathode polarization resistance and overpotential at a current density of 100 mA cm&minus;2 were 0.85 &Omega; cm&minus;2 and 110 mV in dry air, which decreased to 0.43 &Omega; cm&minus;2 and 52 mV, respectively, in wet air (&sim;3% H2O) at 650 &deg;C. A decrease in impedance was also observed with polarization time; this was possibly caused by polarization-induced microstructure optimization. A promising peak power density of &sim;585 mW cm&minus;2 was demonstrated by an anode-supported cell with a BCFN cathode at 700 &deg;C.<br />

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in situ high-temperature X-ray diffraction and thermal gravimetric- differential thermal analysis on room-temperature powder, as well as X-ray diffraction, Raman spectroscopy, and transmission electron microscopy on quenched powder, were applied to study crystal structure and phase transformations in Ba<sub>2</sub>Bi<sub>0.1</sub>Sc<sub>0.2</sub>Co <sub>1.7</sub>O<sub>6-x</sub> (BBSC). Heating BBSC in air to over 800 &deg;C produces a pure cubic phase with space group Fm3m (no. 225), and cooling down below 800 &deg;C leads to a mixture of three noncubic phases including an unknown phase between 200 and 650 &deg;C, a 2H hexagonal BaCoO3 with space group P63/mmc (no. 194) between 600 and 800 &deg;C, and an intermediate phase at 800 &deg;C. These three phases exist concurrently with the major cubic phase. The weight gain and loss between 300 and 900 &deg;C suggest the occurrence of cobalt reduction, oxidation, and disproportion reactions with dominant reduction reaction at above 600 &deg;C. The thermal expansion of BBSC was also examined by dilatometry. BBSC has a highly temperature-dependent thermal expansion coefficient which relates well with its structure evolution. Furthermore, the oxygen reduction reaction (ORR) of BBSC was probed by symmetrical cell and three-electrode configurations. The presence of hexagonal phase at 700 &deg;C rarely affects the ORR performance of BBSC as evidenced by a slight increase of its area-specific resistance (ASR) value following 48 h of testing in this three-electrode configuration. This observation is in contrast to the commonly held point of view that noncubic phase deteriorates performance of perovskite compounds (especially in oxygen transport applications). Moreover, cathodic polarization treatment, for example, current discharge from BBSC (tested in three-electrode configuration), can be utilized to recover the original ORR performance. The cubic structure seems to be retained on the cathodic polarization - the normal cathode operating mode in fuel cells. Stable 72-h performance of BBSC in cathodic polarization mode further confirms that despite the presence of phase impurities, BBSC still demonstrates good performance between 500 and 700 &deg;C, the desired intermediate operating temperature in solid oxide fuel cells.

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This work compares the oxygen permeation fluxes of five different La0.6Sr0.4Co0.2Fe0.8O3&minus;&delta; membranes (e.g. disk, conventional hollow fiber, modified hollow fiber, Ag- or Pt-deposited hollow fiber membranes) to elucidate the dominance of a particular oxygen transport limiting step (e.g., bulk-diffusion or surface reaction) within each of these membranes. At 900 &deg;C and 100 mL min&ndash;1 helium gas sweep rate, the oxygen fluxes for disk, conventional hollow fiber, modified hollow fiber, Ag-deposited modified hollow fiber, and Pt-deposited modified hollow fiber membranes are 0.10, 0.33, 0.84, 1.42, and 2.62 mL min&ndash;1 cm&ndash;2, respectively, denoting enhanced performance in this sequential order. More than 300% enhancement of fluxes is evidenced by modifying the geometry from disk to conventional hollow fiber. This is attributed to the thickness reduction from 1 mm to 0.3 mm, thus implying bulk-diffusion and surface reaction as the jointly limiting transport step for this disk membrane. In contrast to a conventional hollow fiber that has a sandwich cross-sectional structure (e.g. dense center layer sandwiched by two finger-like layers) as well as dense outer and inner circumference surfaces, the modified hollow fiber has only one dense layer in its outer circumference surface with finger-like porous layer extending all the way from outer cross-sectional part to the inner cross-sectional part. This microstructural difference, in turn, provides substantial reduction of membrane thickness and enlarges surface reaction area for modified hollow fiber (relative to conventional hollow fiber), both of which contributes to the reduced bulk-diffusion and surface reaction resistance; evidenced by almost 250% oxygen flux enhancement. To enhance the performance even further, catalyst (e.g., Ag or Pt) deposition on the outer circumference surface of modified hollow fiber can be utilized to reduce its dominating surface reaction resistance. While both catalysts increase the oxygen fluxes, Pt reveals itself as the better candidate relative to Ag due to melting-induced aggregation and growth of Ag at 950 &deg;C.<br />

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The microstructure evolution and softening processes occurring in 22Cr-19Ni-3Mo austenitic and 21Cr-10Ni-3Mo duplex stainless steels deformed in torsion at 900 and 1200 &deg;C were studied in the present work. Austenite was observed to soften in both steels via dynamic recovery (DRV) and dynamic recrystallisation (DRX) for the low and high deformation temperatures, respectively. At 900 &deg;C, an &quot;organised&quot;, self-screening austenite deformation substructure largely comprising microbands, locally accompanied by micro-shear bands, was formed. By contrast, a &quot;random&quot;, accommodating austenite deformation substructure composed of equiaxed subgrains formed at 1200 &deg;C. In the single-phase steel, DRX of austenite largely occurred through straininduced grain boundary migration accompanied by (multiple) twinning. In the duplex steel, this softening mechanism was complemented by the formation of DRX grains through subgrain growth in the austenite/ferrite interface regions and by large-scale subgrain coalescence. At 900 &deg;C, the duplex steel displayed limited stress-assisted phase transformations between austenite and ferrite, characterised by the dissolution of the primary austenite, formation of Widmanst&auml;tten secondary austenite and gradual globularisation of the transformed regions with strain. The softening process within ferrite was classified as &quot;extended DRV&quot;, characterised by a continuous increase in misorientations across the sub-boundaries with strain, for both deformation temperatures.

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Heterogeneous deformation developed during &quot;static recrystallization (SRX) tests&quot; poses serious questions about the validity of the conventional methods to measure softening fraction. The challenges to measure SRX and verify a proposed kinetic model of SRX are discussed and a least square technique is utilized to quantify the error in a proposed SRX kinetic model. This technique relies on an existing computational-experimental multi-layer formulation to account for the heterogeneity during the post interruption hot torsion deformation. The kinetics of static recrystallization for a type 304 austenitic stainless steel deformed at 900 &deg;C and strain rate of 0.01s<sup>-1</sup> is characterized implementing the formulation. Minimizing the error between the measured and calculated torque-twist data, the parameters of the kinetic model and the flow behavior during the second hit are evaluated and compared with those obtained based on a conventional technique. Typical static recrystallization distributions in the test sample will be presented. It has been found that the major differences between the conventional and the presented technique results are due to the heterogeneous recrystallization in the cylindrical core of the specimen where the material is still partially recrystallized at the onset of the second hit deformation. For the investigated experimental conditions, the core is confined in the first two-thirds of the gauge radius, when the holding time is shorter than 50 s and the maximum pre-strain is about 0.5.