Microstructure, mechanical properties and fractography of heat-treated manganese steel

A Fe-8.46%Mn-0.24%Nb-0.038%C (wt.%) manganese steel was investigated. The steel has a 100% bcc structure after heat treatment at 850°C for 1.5 h, water quenching or air cooling. Martensite interlocked microstructure consisting of fine martensite plates/needles with different spatial orientations was found. Austenite forms, in small amounts, after a 600°C reheating treatment. Scanning electron microscopy images and energy dispersive spectrometry of the fracture surfaces revealed both ductile and brittle types of failure and precipitates. Deep quenching after the heat treatments does not change the phase composition or the hardness. NbC is formed in the steel, in high number densities. It plays a role in the impact fracture process, by acting as void nucleation sites, facilitating ductile fracture with dimples appearing on the fracture surface.

Melt Processing and Properties of Polyamide 6/Graphene Nanoplatelet Composites

Graphene, due to its outstanding properties, has become the topic of much research activity in recent years. Much of that work has been on a laboratory scale however, if we are to introduce graphene into real product applications it is necessary to examine how the material behaves under industrial processing conditions. In this paper the melt processing of polyamide 6/graphene nanoplatelet composites via twin screw extrusion is investigated and structure–property relationships are examined for mechanical and electrical properties. Graphene nanoplatelets (GNPs) with two aspect ratios (700 and 1000) were used in order to examine the influence of particle dimensions on composite properties. It was found that the introduction of GNPs had a nucleating effect on polyamide 6 (PA6) crystallization and substantially increased crystallinity by up to 120% for a 20% loading in PA6. A small increase in crystallinity was observed when extruder screw speed increased from 50 rpm to 200 rpm which could be attributed to better dispersion and more nucleation sites for crystallization. A maximum enhancement of 412% in Young's modulus was achieved at 20 wt% loading of GNPs. This is the highest reported enhancement in modulus achieved to date for a melt mixed thermoplastic/GNPs composite. A further result of importance here is that the modulus continued to increase as the loading of GNPs increased even at 20 wt% loading and results are in excellent agreement with theoretical predictions for modulus enhancement. Electrical percolation was achieved between 10–15 wt% loading for both aspect ratios of GNPs with an increase in conductivity of approximately 6 orders of magnitude compared to the unfilled PA6.

Fate of organo-mineral particles in streams: Microbial degradation by streamwater & biofilm assemblages

Inland waters are of global biogeochemical importance. They receive carbon inputs of ~ 4.8 Pg C/ y of which, 12 % is buried, 18 % transported to the oceans, and 70 % supports aquatic secondary production. However, the mechanisms that determine the fate of organic matter (OM) in these systems are poorly defined. One aspect of this is the formation of organo-mineral complexes in aquatic systems and their potential as a route for OM transport and burial vs. their use as carbon (C) and nitrogen (N) sources within aquatic systems. Organo-mineral particles form by sorption of dissolved OM to freshly eroded mineral surfaces and may contribute to ecosystem-scale particulate OM fluxes. We experimentally tested the availability of mineral-sorbed OM as a C & N source for streamwater microbial assemblages and streambed biofilms. Organo-mineral particles were constructed in vitro by sorption of ¹³C:¹⁵N-labelled amino acids to hydrated kaolin particles, and microbial degradation of these particles compared with equivalent doses of ¹³C:¹⁵N-labelled free amino acids. Experiments were conducted in 120 ml mesocosms over 7 days using biofilms and water sampled from the Oberer Seebach stream (Austria). Each incubation experienced a 16:8 light:dark regime, with metabolism monitored via changes in oxygen concentrations between photoperiods. The relative fate of the organo-mineral particles was quantified by tracing the mineralization of the ¹³C and ¹⁵N labels and their incorporation into microbial biomass. Here we present the initial results of ¹³C-label mineralization, incorporation and retention within dissolved organic carbon pool. The results indicate that 514 (± 219) μmol/ mmol of the ¹³:¹⁵N labeled free amino acids were mineralized over the 7-day incubations. By contrast, 186 (± 97) μmol/ mmol of the mineral-sorbed amino acids were mineralized over a similar period. Thus, organo-mineral complexation reduced amino acid mineralization by ~ 60 %, with no differences observed between the streamwater and biofilm assemblages. Throughout the incubations, biofilms were observed to leach dissolved organic carbon (DOC). However, within the streamwater assemblage the presence of both organo-mineral particles and kaolin particles was associated with significant DOC removal (-1.7 % and -7.5 % respectively). Consequently, the study demonstrates that mineral and organo-mineral particles can limit the availability of DOC in aquatic systems, providing nucleation sites for flocculation and fresh mineral surfaces, which facilitate OM-sorption. The formation of these organo-mineral particles subsequently restricts microbial OM degradation, potentially altering the transport and facilitating the burial of OM within streams.

Earthworms produce granules of intricately zoned calcite

Earthworms of the family Lumbricidae, which includes many common species, produce and secrete up to millimeter-sized calcite granules, and the intricate fine-scale zoning of their constituent crystals is unique for a biomineral. Granule calcite is produced by crystallization of amorphous calcium carbonate (ACC) that initially precipitates within the earthworm calciferous glands, then forms protogranules by accretion on quartz grain cores. Crystallization of ACC is mediated by migrating fluid films and is largely complete within 24 11 of ACC production and before granules leave the earthworm. Variations in the density of defects formed as a byproduct of trace element incorporation during calcite crystall growth have generated zoning that can be resolved by cathodoluminescence imaging at ultraviolet to blue wavelengths and using the novel technique of scanning electron microscope charge contrast imaging. Mapping of calcite crystal orientations by electron backscatter diffraction reveals an approximate radial fabric to the granules that reflects crystal growth from internal nucleation sites toward their margins. The survival within granules of ACC inclusions for months after they enter soils indicates that they crystallize only within the earthworm and in the presence of fluids containing biochemical catalysts. The earthworm probably promotes crystallization of ACC in order to prevent remobilization of the calcium carbonate by dissolution. Calcite granules vividly illustrate the role of transient precursors in biomineralization, but the underlying question of why earth-worms produce granules in volumes sufficient to have a measurable impact on soil carbon cycling remains to be answered.

Fragmentation of orientation within grains of a cold-rolled interstitial-free steel

The formation of a favourable recrystallization texture in interstitial-free (IF) steels depends on the availability and activation of particular nucleation sites in the deformed microstructure. This paper presents a description of the deformed microstructure of a commercially cold-rolled IF steel, with particular emphasis on the microstructural inhomogeneities and short-range orientational variation that provide suitable nucleation sites during recrystallization. RD-fibre regions deform relatively homogeneously and exhibit little short-range orientational variation. ND-fibre regions are heavily banded and exhibit considerable short-range orientational variation associated with the bands. While the overall orientational spread of ND-fibre grains frequently is about the ND-axis, the short-range orientational variation often involves rotation about axes in the TD-ND plane that are nearer to the TD than the ND.

The evolution of ultrafine ferrite formation through dynamic strain-induced transformation

Hot torsion testing of a C–Mn–V steel was used to study the evolution of  ultrafine ferrite (UFF) formation by dynamic strain-induced transformation (DSIT) in conjunction with air-cooling for two prior austenite grain sizes. This study evaluated not only the evolution of DSIT ferrite during straining, but also the grain growth behaviour of DSIT ferrite grains during post-deformation cooling. For both austenite grain sizes, the DSIT ferrite initially nucleated on/or near prior austenite grain boundaries at an early stage of transformation followed by the grain interiors. The prior austenite grain size affected the distribution of DSIT ferrite nucleation sites at an early stage of transformation and the subsequent coarsening behaviour of the grain boundary (GB) and the intragranular ferrite (IG) grains during post-deformation cooling. For the fine prior austenite grain size, the distribution of DSIT ferrite grains was more homogenous compared with the coarse austenite and the coarsening occurred not only in the GB ferrite grains but also in the IG ferrite grains. However, the ferrite coarsening mostly occurred for the IG ferrite rather than the GB ferrite grains in the coarse austenite. The result suggests that normal grain growth occurred during the overall transformation in the GB ferrite grains for the coarse initial austenite grain size.

Effect of thermomechanical parameters on the critical strain for ultrafine ferrite formation through hot torsion testing

A C–Mn–V steel was used to study ultrafine ferrite formation (1–3 μm) through dynamic strain-induced transformation (DSIT) using hot torsion experiments. A systematic study determined the critical strain for the start of DSIT (C,DSIT), although this may not lead to a fully ultrafine microstructure. Therefore, the strain to produce an ultrafine ferrite (UFF) as final microstructure (C,UFF) during deformation was also determined. In addition, the effect of thermomechanical parameters such as deformation temperature, prior austenite grain size, strain rate and cooling rate on C,DSIT and C,UFF has been evaluated. DSIT ferrite nucleated on prior austenite grain boundaries at an early stage of straining followed by intragranular nucleation at higher strains. The prior austenite grain size affected the distribution of DSIT ferrite nucleation sites at an early stage of transformation and the subsequent coarsening behaviour of the grain boundary and intragranular ferrite grains during post-deformation cooling. Also, C,DSIT and C,UFF increased with an increase in the prior austenite grain size and deformation temperature. The post-deformation cooling had a strong effect not only on C,UFF but also the UFF microstructure (i.e. final ferrite grain size and second phase characteristics).

The formation of ultrafine grained steel microstructures through thermomechanical processing.

The formation of ultrafine grained steels is an area of intense research around the World. There are a number of methods to produce grain sizes of approximately 1 µm, ranging from extreme thermal and deformation cycles to more typical thermomechanical processes. This paper reviews the status of the production of ultrafine grained steels through relatively simple thermomechanical processing. It is shown that this requires deformation within the Ae3 to Ar3 temperature range for a given alloy. The formation of ultrafine ferrite involves a dynamic transformation of a significant volume fraction of the austenite to ferrite. This dynamic strain induced transformation arises from the introduction of additional intragranular nucleation sites. It is possible that the deformation also hinders the growth or coarsening of the ferrite and may also lead to dynamic recrystallization of the ferrite. The most likely commercial exploitation of ultrafine ferrite would appear to rely on the formation of a critical volume fraction of dynamic strain induced ferrite followed by controlled cooling to ensure this is maintained to room temperature and to also form other secondary phases, such as martensite, bainite and/or retained austenite to improve the formability.

Ultrafine grained structure formation in steels using dynamic strain induced transformation processing

The refinement of ferrite grain size is the most generally accepted approach to simultaneously improve the strength and toughness in steels. Historically, the level of ferrite refinement is limited to 5-10 μm using conventional industrial approaches. Nowadays, though, several thermomechanical processes have been developed to produce ferrite grain sizes of 1-3 μm or less, ranging from extreme thermal and deformation cycles to more typical thermomechanical processes. The present paper reviews the status of the production of ultrafine grained steels through relatively simple thermomechanical processing. This requires deformation within the Ae3 to Ar3 temperature range for a given alloy. Here, the formation of ultrafine ferrite (UFF) involves the dynamic transformation of a significant volume fraction of the austenite to ferrite. This dynamic strain induced transformation (DSIT) arises from the introduction of extensive intragranular nucleation sites that are not present in conventional controlled rolling. The DSIT route has the potential to be adjusted to suit current industrial infrastructure. However, there are a number of significant issues that have been raised, both as gaps in our understanding and as obstacles to industrial implementation. One of the critical issues is that it appears that very large strains are required. Combined with this concern is the issue of whether a combination of dynamic and static transformation can be used to achieve an adequate level of refinement. Another issue that has also become apparent is that grain sizes of 1 μm can lead to low levels of ductility and hence many workers are attempting to obtain 2-3 μm grains, or to introduce a second phase to provide the required ductility. There are also a number of areas of disagreement between authors including the role of dynamic recrystallisation of ferrite in the production of UFF by DSIT, the reasons for the low coarsening rate of UFF grains, the role of microalloying elements and the effects of austenite grain size and strain rate. The present review discusses these areas of controversy and highlights cases where experimental results do not agree.

The production of ultrafine ferrite during hot torsion testing of a 0.11 Wt Pct C steel

Ultrafine ferrite grain sizes were produced in a 0.11C-1.6Mn-0.2Si steel by torsion testing isothermally at 675 °C after air cooling from 1250 °C. The ferrite was observed to form intragranularly beyond a von Mises equivalent tensile strain of approximately 0.7 to 0.8 and the number fraction of intragranular ferrite grains continued to increase as the strain level increased. Ferrite nucleated to form parallel and closely spaced linear arrays or “rafts” of many discrete ultrafine ferrite grains. It is shown that ferrite nucleates during deformation on defects developed within the austenite parallel to the macroscopic shear direction (i.e., dynamic strain-induced transformation). A model austenitic Ni-30Fe alloy was used to study the substructure developed in the austenite under similar test conditions as that used to induce intragranular ferrite in the steel. It is shown that the most prevalent features developed during testing are microbands. It is proposed that high-energy jogged regions surrounding intersecting microbands provide potential sites for ferrite nucleation at lower strains, while at higher strains, the walls of the microbands may also act as nucleation sites.

Patterned growth of carbon nanotubes on Si substrates without predeposition of metal catalysts

Aligned carbon nanotubes (CNTs) can be readily synthesized on quartz or silicon-oxide-coated Si substrates using a chemical vapor deposition method, but it is difficult to grow them on pure Si substrates without predeposition of metal catalysts. We report that aligned CNTs were grown by pyrolysis of iron phthalocyanine at 1000 °C on the templates created on Si substrates with simple mechanical scratching. Scanning electron microscopy and x-ray energy spectroscopy analysis revealed that the trenches and patterns created on the surface of Si substrates were preferred nucleation sites for nanotube growth due to a high surface energy, metastable surface structure, and possible capillarity effect. A two-step pyrolysis process maintained Fe as an active catalyst.

Dynamic recrystallization of austenite in Ni-30 Pct Fe model alloy : microstructure and texture evolution

The microstructure and crystallographic texture development in an austenitic Ni-30 pct Fe model alloy was investigated within the dynamic recrystallization (DRX) regime using hot torsion testing. The prominent DRX nucleation mechanism was strain-induced grain boundary migration accompanied by the formation of large-angle sub-boundaries and annealing twins. The increase in DRX volume fraction occurred through the formation of multiple twinning chains. With increasing strain, the pre-existing Σ3 twin boundaries became gradually converted to general boundaries capable of acting as potent DRX nucleation sites. The texture characteristics of deformed grains resulted from the preferred consumption of high Taylor factor components by new recrystallized grains. Similarly, the texture of DRX grains was dominated by low Taylor factor components as a result of their lower consumption rate during the DRX process. The substructure of deformed grains was characterized by “organized,” banded subgrain arrangements, while that of the DRX grains displayed “random,” more equiaxed subgrain/cell configurations.

Fine structure of shear bands formed during hot deformation of two austenitic steels

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°C and 950°C and strain rates of 0.7s_-1 and 10s_-1, 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.

Thermo-mechanical processing and the shape memory effect in an Fe–Mn–Si-based shape memory alloy

The effect of cold rolling and annealing on the shape memory effect (SME) in an Fe–Mn–Si-based alloy has been studied. It has been found
that the SME in these alloys can be significantly increased by the appropriate thermo-mechanical processing (TMP). The optimum conditions
were found to be 15% cold rolling followed by annealing at 800 ◦C for 15 min. This produced a total strain recovery of 4.5%. TEM showed that
this processing schedule produces a microstructure of evenly spaced, and well defined stacking faults throughout the parent phase. It is shown for
the first time that samples processed in this way produce a larger fraction of martensite compared to samples in the as-austenitized condition. It
is concluded that the stacking faults induced by TMP act as nucleation sites for martensite formation during deformation. The SME is improved
primarily as a result of the increased amount of martensite that is formed in this condition.

Martensite/particle interactions and the shape memory effect in an Fe–Mn–Si-based alloy

The effect of carbide precipitates with a size range of 30–300 nm on the austenite to martensite transformation has been studied. Such particles are known to enhance shape memory, and it was the aim of this work to clarify how the particles exert a favourable effect on shape memory. Differential scanning calorimetry revealed that the presence of particles increases the amount of thermally induced martensite. X-ray diffraction showed that the presence of particles increases the amount of stress-induced martensite also. Surface-relief produced on a pre-polished surface by bending deformation showed that the particle-containing samples exhibited a more complex and highly tilted surface-relief indicative of the formation of a larger volume fraction of martensite. The reversion characteristics of the particle-containing and solution-treated samples were similar: both showed co-reversion of multiple variants of martensite within the same volume of microstructure. However, a higher volume fraction of martensite reverted for the particle-containing sample on recovery annealing. The increased density of nucleation sites for martensite formation and a higher volume fraction of stress-induced martensite for a given strain are therefore considered to be the main contributions of relatively coarse carbide particles to the improvement of shape memory performance.