Vacancy clusters in ultrafine grained Al by severe plastic deformation

Bulk nanostructured metals are often formed via severe plastic deformation (SPD). The dislocations generated during SPD evolve into boundaries to decompose the grains. Vacancies are also produced in large numbers during SPD, but have received much less attention. Using transmission electron microscopy, here we demonstrate a high density of unusually large vacancy Frank loops in SPD-processed Al. They are shown to impede moving dislocations and should be a contributor to strength. (C) 2007 American Institute of Physics.

Accommodation of large plastic strains and defect accumulation in nanocrystalline Ni grains

A transmission electron microscopy (TEM) study has been carried out to uncover how dislocations and twins accommodate large plastic strains and accumulate in very small nanocrystalline Ni grains during low-temperature deformation. We illustrate dislocation patterns that suggest preferential deformation and nonuniform defect storage inside the nanocrystalline grain. Dislocations are present in individual and dipole configurations. Most dislocations are of the 60 degrees type and pile up on (111) slip planes. Various deformation responses, in the forms of dislocations and twinning, may simultaneously occur inside a nanocrystalline grain. Evidence for twin boundary migration has been obtained. The rearrangement and organization of dislocations, sometimes interacting with the twins, lead to the formation of subgrain boundaries, subdividing the nanograin into mosaic domain structures. The observation of strain (deformation)-induced refinement contrasts with the recently reported stress-assisted grain growth in nanocrystalline metals and has implications for understanding the stability and deformation behavior of these highly nonequilibrium materials.

Effect of mechanical milling on the structural, magnetic and dielectric properties of coprecipitated ultrafine zinc ferrite

Nanosized ZnFe2O4 particles containing traces of a-Fe2O3 by intent were produced by low temperature chemical coprecipitation methods. These particles were subjected to high-energy ball milling. These were then characterised using X-ray diffraction, magnetisation and dielectric studies. The effect of milling on zinc ferrite particles have been studied with a view to ascertaining the anomalous behaviour of these materials in the nanoregime. X-ray diffraction and magnetisation studies carried out show that these particles are associated with strains and it is the surface effects that contribute to the magnetisation. Hematite percentage, probably due to decomposition of zinc ferrite, increases with milling. Dielectric behaviour of these particles is due to interfacial polarisation as proposed by Koops. Also the defects caused by the milling produce traps in the surface layer contributes to dielectric permittivity via spin polarised electron tunnelling between grains. The ionic mechanism is enhanced in dielectrics with the rise in temperature which results in the increase of dielectric permittivity with temperature.

Microstructural evolution of ultrafine grained structure in plain carbon steels through single pass rolling

In the present study, the effect of nominal equivalent strain (between 0 and 1.2), deformation temperature (790– 750°C) and carbon content (0.06 – 0.35%C) was investigated on ferrite grain refinement through dynamic strain induced transformation (DSIT) in plain carbon steels in single pass rolling. The microstructural evolution of the transformation of austenite to ferrite has been evaluated through the thickness of the strip. The results showed a number of important microstructural features as a function of strain, which could be classified into three regions; no DSIT region, DSIT region, and ultrafine ferrite (UFF) grain region. Hence, two critical strains; dynamic strain induced transformation (εC, DSIT) and ultrafine ferrite formation (εC, UFF) were determined. These strains were increased significantly with an increase in carbon content. The critical strain for UFF formation reduced with decrease in deformation temperature. The UFF microstructure consisted of ultrafine, equiaxed ferrite grains (<2 μm) with very fine cementite particles. In the centre of the rolled strip, there was a conventional ferrite– pearlite microstructure, although ferrite grain refinement and the volume fraction of ferrite increased with increase in the nominal equivalent strain.

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.

Formation of ultrafine grained structure in plain carbon steels through thermomechanical processing

In the present study, wedge-shaped samples were used to determine the effect of nominal equivalent strain (between 0 and 1.2) and carbon content (0.06--0.35%C) on ferrite grain refinement through dynamic strain-induced transformation (DSIT) in plain carbon steels using single-pass rolling. The microstructural evolution of the transformation of austenite to ferrite has been evaluated through the thickness of the strip. The results showed a number of important microstructural features as a function of strain which could be classified into three regions; no DSIT region, DSIT region and the ultrafine ferrite (UFF) grain region. Also, the extent of these regions was strongly influenced by the carbon content. The UFF microstructure consisted of ultrafine, equiaxed ferrite grains (<2 μ$m) with very fine cementite particles. In the centre of the rolled strip, there was a conventional ferrite-pearlite microstructure, although ferrite grain refinement and the volume fraction of ferrite increased with an increase in the nominal equivalent strain.

Formation of ultrafine grained microstructures in steel through strain induced transformation during single pass hot rolling

In the present study, wedge-shape samples were used to study the effect of strain induced transformation on the formation of ultrafine grained structures in steel by single pass rolling. The results showed two different transition strains for bainite formation and ultrafine ferrite (UFF) formation in the surface layer of strip at reductions of 40% and 70%, respectively, in a plain carbon steel. The bainitic microstructure formed by strain induced bainitic transformation during single pass rolling was also very fine. The evolution of UFF formation in the surface layer showed that ferrite coarsening is significantly reduced through strain induced transformation combined with rapid cooling in comparison with the centre of the strip. In the surface, the ferrite coarsening mostly occurred for intragranular nucleated grains (IG) rather than grain boundary (GB) ferrite grains. The results suggest that normal grain growth occurred during overall transformation in the GB ferrite grains. In the centre of the strip, there was significantly more coarsening of ferrite grains nucleated on the prior austenite grain boundaries.

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).

Development of ultrafine grained steels through thermomechanical processing

The formation of ultrafine ferrite by strain induced transformation is assessed using rolling and hot torsion experiments. These experiments are used to examine the impact of thermomechanical processing conditions and steel chemistry on strain induced austenite to ferrite transformation and the formation of ultrafine ferrite. The critical strain for dynamic strain induced transformation increased with increasing carbon equivalence, deformation temperature and austenite grain size. The deformation structure in the austenite grains changes with the thermomechanical processing conditions. Drawing on these results and the current literature, the important factors for the production of ultrafine ferrite are described and a mechanism is proposed.

Nucleation sites for ultrafine ferrite produced by deformation of austenite during single-pass strip rolling

An austenitic Ni-30 wt pct Fe alloy, with a stacking-fault energy and deformation characteristics similar to those of austenitic low-carbon steel at elevated temperatures, has been used to examine the defect substructure within austenite deformed by single-pass strip rolling and to identify those features most likely to provide sites for intragranular nucleation of ultrafine ferrite in steels. Samples of this alloy and a 0.095 wt pct C-1.58Mn-0.22Si-0.27Mo steel have been hot rolled and cooled under similar conditions, and the resulting microstructures were compared using transmission electron microscopy (TEM), electron diffraction, and X-ray diffraction. Following a single rolling pass of ∼40 pct reduction of a 2mm strip at 800 °C, three microstructural zones were identified throughout its thickness. The surface zone (of 0.1 to 0.4 mm in depth) within the steel comprised a uniform microstructure of ultrafine ferrite, while the equivalent zone of a Ni-30Fe alloy contained a network of dislocation cells, with an average diameter of 0.5 to 1.0 µm. The scale and distribution and, thus, nucleation density of the ferrite grains formed in the steel were consistent with the formation of individual ferrite nuclei on cell boundaries within the austenite. In the transition zone, 0.3 to 0.5 mm below the surface of the steel strip, discrete polygonal ferrite grains were observed to form in parallel, and closely spaced “rafts” traversing individual grains of austenite. Based on observations of the equivalent zone of the rolled Ni-30Fe alloy, the ferrite distribution could be correlated with planar defects in the form of intragranular microshear bands formed within the deformed austenite during rolling. Within the central zone of the steel strip, a bainitic microstructure, typical of that observed after conventional hot rolling of this steel, was observed following air cooling. In this region of the rolled Ni-30Fe alloy, a network of microbands was observed, typical of material deformed under plane-strain conditions.

The production of ultrafine ferrite in low-carbon steel by strain-Induced transformation

An investigation into the production of ultrafine (1 µm) equiaxed ferrite (UFF) grains in low-carbon steel was made using laboratory rolling, compression dilatometry, and hot torsion techniques. It was found that the hot rolling of thin strip, with a combination of high shear strain and high undercooling, provided the conditions most suitable for the formation of this type of microstructure. Although high strains could be applied in compression and torsion experiments, large volume fractions of UFF were not observed in those samples, possibly due to the lower level of undercooling achieved. It is thought that ferrite refinement was due to a strain-induced transformation process, and that ferrite grains nucleated on parallel and linear deformation bands that traversed austenite grains. These bands formed during the deformation process, and the undercooling provided by the contact between the strip and the work rolls was sufficient to drive the transformation to homogeneous UFF grains.

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.

Effect of process variables on formation of dynamic strain induced ultrafine ferrite during hot torsion testing

Ultrafine grain sizes were produced using hot torsion testing of a 0.11C-1.68Mn-0.20Si (wt-%) steel, with ultrafine ferrite (<1 µm) nucleating intragranularly during testing by dynamic strain induced transformation. A systematic study was made of the effect of isothermal deformation temperature, strain level, strain rate, and accelerated cooling during deformation on the formation of ultrafine ferrite by this process. Decreasing the isothermal testing temperature below the Ae₃ temperature led to a greater driving force for ferrite nucleation and thus more extensive nucleation during testing; the formation of Widmanstätten ferrite prior to, or early during, deformation imposed a lower temperature limit. Increasing the strain above that where ferrite first began 0.8 at 675C and a strain rate of 3 s¯¹ increased the intragranular nucleation of ferrite. Strain rate appeared to have little effect on the amount of ferrite formed. However, slower strain rates led to extensive polygonisation of the ferrite formed because more time was available for ferrite recovery. Accelerated cooling during deformation followed by air cooling to room temperature led to a uniform microstructure consisting of very fine ferrite grains and fine spherical carbides located in the grain boundaries regions. Air cooling after isothermal testing led to carbide bands and a larger ferrite grain size.

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.

Process for the production of ultrafine powders

A process for the production of ultrafine powders consisting of individual particles with sizes in the range of 1 nm to 200 nm, which is based on the mechanical milling of two or more non-reacting powders. The process includes subjecting a suitable precursor metal compound and a non-reactant diluent phased to mechanical milling which through the process of mechanical activation reduces the microstructure of the mixture of the form of nano-sized grains of the metal compound uniformly dispersed in the diluent phase. Heat treating the milled powder converts the nano-sized grains of the precursor metal compound into a desired metal oxide phase. Alternatively, the precursor metal compound may itself be an oxide phase which has the requisite milling properties to form nanograins when milled with a diluent. An ultrafine powder is produced by removing the diluent phase such that nano-sized grains of the desired metal oxide phase are left behind. The process facilitates a significant degree of control over the particle size and size distribution of the particles in the ultrafine powder by controlling the parameters of mechanical activation and heat treatment.