Microstructure-hardness-fretting wear resistance correlation in ultrafine grained Cu-TiB2-Pb composites

The retention of the desired combination of mechanical/tribological properties in ultrafine grained materials presents important challenges in the field of bulk metallic composites. In order to address this aspect, the present work demonstrates how one can achieve a good combination of hardness and wear resistance in Cu-Pb-TiB2 composites, consolidated by spark plasma sintering at low temperatures ( < 500 degrees C). Transmission electron microscope (TEM) studies reveal ultrafine grains of Cu (100-400 nm) with coarser TiB2 particles (1-2 mu m) along with fine scale Pb dispersoid at triple junctions or at the grain boundaries of Cu. Importantly, a high hardness of around 2.2 GPa and relative density of close to 90% relative density (rho(theo)) have been achieved for Cu-15 wt% TiB2-10 wt% Pb composite. Such property theo, combination has never been reported for any Cu-based nanocomposite, by conventional processing route. In reference to the tribological performance, fretting wear tests were conducted on the sintered nanocomposites and a good combination of steady state COF (0.6-0.7) and wear rate (10-4 mm(3)/N m) were measured. An inverse relationship between wear rate and hardness was recorded and this commensurates well with Archard's relationship of abrasive wear. The formation of a wear-resistant delaminated tribolayer consisting of TiB2 particles and ultrafine oxide debris, (Cu, Fe, Ti)(x)O-y as confirmed from subsurface imaging using focused ion beam microscopy has been identified as the key factors for the low wear rate of these composites. (C) 2014 Elsevier B.V. All rights reserved.

Review: Overcoming the paradox of strength and ductility in ultrafine-grained materials at low temperatures

Ultrafine-grained (UFG) materials with grain sizes in the submicrometer or nanometer range may be prepared through the application of severe plastic deformation (SPD) to bulk coarse-grained solids. These materials generally exhibit high strength but only very limited ductility in low-temperature testing, thereby giving rise to the so-called paradox of strength and ductility. This paradox is examined and a new quantitative diagram is presented which permits the easy insertion of experimental data. It is shown that relatively simple procedures are available for achieving both high strength and high ductility in UFG materials including processing the material to a very high strain and/or applying a very short-term anneal immediately after the SPD processing. Significant evidence is now available demonstrating the occurrence of grain boundary sliding in these materials at low temperatures, where this is attributed to the presence of non-equilibrium grain boundaries and the occurrence of enhanced diffusion along these boundaries.

Cyclic Deformation Of Nanocrystalline And Ultrafine-Grained Nickel

The cyclic deformation behavior Of ultrafine-grained (UFG) Ni samples synthesized by the electrodeposition method was studied. Different from those made by severely plastic deformation, the UFG samples used in this study are characterized by large-angle grain boundaries. Behaviors from nanocrystalline Ni and coarse-grained Ni samples were compared with that Of Ultrafine-grained Ni. With in situ neutron diffraction. unusual evolutions of residual lattice strains as well as cyclic hardening and softening behavior were demonstrated during the cyclic deformation. The microstructural changes investigated by TEM are discussed with respect to the unusual lattice strain and cyclic hardening/softening. (C) 2008 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

High-frequency ferromagnetic resonance on ultrafine cobalt particles

We report on high-frequency (300-700 GHz) ferromagnetic resonance (HF-FMR) measurements on cobalt superparamagnetic particles with strong uniaxial effective anisotropy. We derive the dynamical susceptibility of the system on the basis of an independent-grain model by using a rectangular approach. Numerical simulations give typical line shapes depending on the anisotropy, the gyromagnetic ratio, and the damping constant. HF-FMR experiments have been performed on two systems of ultrafine cobalt particles of different sizes with a mean number of atoms per particles of 150 +/- 20 and 310 +/- 20. In both systems, the magnetic anisotropy is found to be enhanced compared to the bulk value, and increases as the particle size decreases, in accordance with previous determinations from magnetization measurements. Although no size effect has been observed on the gyromagnetic ratio, the transverse relaxation time is two orders of magnitude smaller than the bulk value indicating strong damping effects, possibly originating from surface spin disorders.

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.

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 role of recrystallization and coarsening in the formation of ultrafine grained steels through thermomechanical processing.

There is now considerable interest in the development of ultrafine grained steels with an average grain size of the order of 1µm. One of the methods with currently the greatest industrial interest is by dynamic strain induced transformation from austenite to ferrite. This involves deformation below the
equilibrium transformation temperature so that transformation occurs during the deformation. However, large strains are required to completely transform the microstructure during deformation. It is potentially possible to activate transformation during deformation then continue transformation
during subsequent cooling. It is shown that there are two critical strains: the first is where dynamic transformation commences and the second is the minimum strain for a fully ultrafine final microstructure after cooling to room temperature. The deformation and potential role of dynamic
recrystallization of the dynamically formed ferrite is also considered. Overall it is clear that for full industrial exploitation there is a need to understand and exploit the competing issues of nucleation, growth and recrystallization of the ferrite by both dynamic and static processes.

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.

Grain refinement in steels through thermomechanical processing

The development of ultrafine grained microstructures in steels has received considerable attention in recent times. In many cases the aim is to produce high strength structural steels with minimal alloying. It is well established that for an equiaxed ferrite with a uniform dispersion of second phase, both the strength and toughness will be markedly improved if the grain size can be reduced to 1-2 μm, from the typical range of 5-10 μm. Means of achieving this through dynamic strain induced transformation are examined here, following a brief overview of some of the key issues encountered when attempting to refine the austenite in existing mill configurations. A number of deformation microstructure maps are developed to aid the discussion.

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.

The formation of ultrafine ferrite in low C steels through thermomechanical processing

Ultrafine ferrite can be formed in steels through relatively simple thermomechanical processes. The ferrite nucleates intragranularly within the austenite grain on deformation features, which are favoured by heavy shear and large effective strains. It is also possible to produce ultrafine microstructures under multipass deformation conditions, although these may be due to dynamic recovery rather than strain induced transformation.

The effect of multiple deformations on the formation of ultrafine grained steels

A C-Mn-Nb-Ti steel was deformed by hot torsion to study ultrafine ferrite formation through dynamic strain-induced transformation (DSIT) in conjunction with air cooling. A systematic study was carried out first to evaluate the effect of deformation temperature and prior austenite grain size on the critical strain for ultrafine ferrite formation (ε C,UFF) through single-pass deformation. Then, multiple deformations in the nonrecrystallization region were used to study the effect of thermomechanical parameters (i.e., strain, deformation temperature, etc.) on ε C,UFF. The multiple deformations in the nonrecrystallization region significantly reduced ε C,UFF, although the total equivalent strain for a given thermomechanical condition was higher than that required in single-pass deformation. The current study on a Ni-30Fe austenitic model alloy revealed that laminar microband structures were the key intragranular defects in the austenite for nucleation of ferrite during the hot torsion test. The microbands were refined and overall misorientation angle distribution increased with a decrease in the deformation temperature for a given thermomechanical processing condition. For nonisothermal multipass deformation, there was some contribution to the formation of high-angle microband boundaries from strains at higher temperature, although the strains were not completely additive.

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.