Combined atom probe tomography and density functional theory investigation of the Al off-stoichiometry of κ-carbides in an austenitic Fe-Mn-Al-C low density steel

We report on the investigation of the off-stoichiometry and site-occupancy of κ-carbide precipitates within an austenitic (γ), Fe-29.8Mn-7.7Al-1.3C (wt.%) alloy using a combination of atom probe tomography and density functional theory. The chemical composition of the κ-carbides as measured by atom probe tomography indicates depletion of both interstitial C and substitutional Al, in comparison to the ideal stoichiometric L′12 bulk perovskite. In this work we demonstrate that both these effects are coupled. The off-stoichiometric concentration of Al can, to a certain extent, be explained by strain caused by the κ/γ mismatch, which facilitates occupation of Al sites in κ-carbide by Mn atoms (MnγAl anti-site defects). The large anti-site concentrations observed by our experiments, however, can only be stabilized if there are C vacancies in the vicinity of the anti-site.

Formation of nanoscale titanium carbides in ferrite: an atomic study

The formation and evolution of nanoscale titanium carbide in ferrite during the early isothermal annealing process were investigated via molecular dynamics simulation. The atomic interactions of titanium and carbon atoms during the initial formation process explained the atoms aggregation and carbides formation. It was found that the aggregation and dissociation of titanium carbide occurred simultaneously, and the composition of carbide clusters varied in a wide range. A mechanism for the formation of titanium carbide clusters in ferrite was disclosed.

In-situ synthesis of titanium carbides in iron alloys using plasma transferred arc welding

The synthesis of Fe-TiC metal matrix composite during metal deposition with laser and arc welding techniques is of technical and economic interest for hard surfacing of engineering components. Recent studies linked the resistance to abrasive wear with the size and morphology of TiC precipitates, which are strongly dependent on the deposition conditions and, more importantly, on the alloy chemistry. In this study, the effect of silicon and manganese on the TiC precipitates was explored and different processing conditions were assessed. The characterisation included optical and scanning electron microscopy, X-ray diffraction and microhardness testing. The results indicate that silicon and manganese can have a significant effect on TiC size and morphology. Therefore, the composition of the matrix alloy offers an effective pathway to modify the microstructure of in-situ precipitated Fe-TiC metal matrix composites. © 2013 Elsevier B.V.

Effect of the thermomechanical processing parameters on the microstructure-property relationships in C-Mn-Si TRIP steel

In this work a wide range of roughing (deformation in the austenite recrystallised region) and finishing (deformation in the non-recrystallised region) strains and isothermal holding times were used to clarify the effect of processing parameters on the transformation kinetics and mechanical properties of 0.2C-1.55Mn-1.55Si (wt%) TRIP steel. The results have highlighted the complex relationships between multi-phase microstructure and mechanical properties of TRIP steel. The presence of the triclinic carbides, formed during isothermal holding, deteriorated the mechanical properties of steel studied.

Precipitate characterisation of an advanced high-strength low-alloy (HSLA) steel using atom probe tomography

Increased fuel economy, combined with the need for the improved safety has generated the development of new hot-rolled high-strength low-alloy (HSLA) and multiphase steels such as dual-phase or transformation-induced plasticity steels with improved ductility without sacrificing strength and crash resistance. However, the modern multiphase steels with good strength-ductility balance showed deteriorated stretch-flangeability due to the stress concentration region between the soft ferrite and hard martensite phases [1]. Ferritic, hot-rolled steels can provide good local elongation and, in turn, good stretch-flangeability [2]. However, conventional HSLA ferritic steels only have a tensile strength of not, vert, similar600 MPa, while steels for the automotive industry are now required to have a high tensile strength of not, vert, similar780 MPa, with excellent elongation and stretch-flangeability [1]. This level of strength and stretch-flangeability can only be achieved by precipitation hardening of the ferrite matrix with very fine precipitates and by ferrite grain refinement. It has been suggested that Mo [3] and Ti [4] should be added to form carbides and decrease the coiling temperature to 650 °C since only a low precipitation temperature can provide the precipitation refinement [4]. These particles appeared to be (Ti, Mo)C, with a cubic lattice and a parameter of 0.433 nm, and they were aligned in rows [4]. It was reported [4] that the formation of these very fine carbides led to an increase in strength of not, vert, similar300 MPa. However, the detailed analysis of these particles has not been performed to date due to their nanoscale size. The aim of this work was to carry out a detailed investigation using atom probe tomography (APT) of precipitates formed in hot-rolled low-carbon steel containing additions Ti and Mo.

The investigated low-carbon steel, containing Fe–0.1C–1.24Mn–0.03Si–0.11Cr–0.11Mo–0.09Ti–0.091Al at.%, was produced by hot rolling. The processing route has been described in detail elsewhere [5] European Patent Application, 1616970 A1, 18.01.2006.[5]. The microstructure was characterised by transmission electron microscopy (TEM) on a Philips CM 20, operated at 200 kV using thin foil and carbon replica techniques. Qualitative energy dispersive X-ray spectroscopy (EDXS) was used to analyse the chemical composition of particles. The atomic level of particle characterisation was performed at the University of Sydney using a local electrode atom probe [6]. APT was carried out using a pulse repetition rate of 200 kHz and a 20% pulse fraction on the sample with temperature of 80 K. The extent of solute-enriched regions (radius of gyration) and the local solute concentrations in these regions were estimated using the maximum separation envelope method with a grid spacing of 0.1 nm [7]. A maximum separation distance between the atoms of interest of dmax = 1 nm was used.

The microstructure of the steel consisted of two types of fine ferrite grains: (i) small recrystallised grains with an average grain size of 1.4 ± 0.2 μm; and (ii) grains with a high dislocation density (5.8 ± 1.4 × 1014 m−2) and an average grain size of 1.9 ± 0.1 μm in thickness and 2.7 ± 0.1 μm in length (Fig. 1a). Some grains with high dislocation density displayed an elongated shape with Widmanstätten side plates and also the formation of cells and subgrains (Fig. 1a). The volume fraction of recrystallised grains was 34 ± 8%.

Characterization of nano-scale particles in hot-rolled, high strength low alloy steels (HSLA)

The contribution of nano-scale particles observed using Atom Probe Tomography in an increase of yield strength of conventional and advanced HSLA steels was studied. The advanced HSLA steel showed higher yield strength than conventional HSLA steel. There were two types of carbides, which primarily contribute to an increase in yield strength of conventional HSLA steel: (i) coarse TiC with average size of 25±5nm and (ii) fine TiC with average radius of 3±1.2nm. The presence of two types of carbides was found in the microstructure of advanced HSLA steel: (i)
nano-scale Ti0.98Mo0.02C0.6 carbides with average radius of 2.2±0.5nm, and (ii) C19Cr7Mo24 particles with an average radius of 1.5±0.3nm. The contribution of precipitation hardening in the yield strength of advanced HSLA steel due to the nano-scale particles was 174MPa, while this value in the conventional HSLA steel was 128MPa.

Effect of initial processing on the microstructure-property relationships in bake-hardened C-Mn-Si TRIP steels

The effect of pre-straining (PS) and bake-hardening (BH) on the microstructure and mechanical properties has been studied in C-Mn-Si TRansformation Induced Plasticity (TRIP) steels after: (i) thermomechanically processing (TMP) and (ii) intercritical annealing. The steels were characterised before and after PS/BH by transmission electron microscopy (TEM), X-ray diffraction (XRD), and tensile tests. The main microstructural differences were the higher volume fraction of bainite and more stable retained austenite in the TMP steel. This led to a difference in the strain-hardening behavior before and after BH treatment. The higher dislocation density in ferrite and formation of microbands in the TMP steel after PS and the formation of Fe3C carbides between the bainitic ferrite laths during BH for both steels also affected the strain-hardening behavior. However, both steels after PS/BH treatment demonstrated an increase in the yield and tensile strength.

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.

Effect of pre-straining and bake hardening on the microstructure and mechanical properties of CMnSi trip steels

The effects of pre-straining and bake hardening on the mechanical behaviour and microstructural changes were studied in two CMnSi TRansformation-Induced Plasticity (TRIP) steels with different microstructures after intercritical annealing. The TRIP steels before and after pre-straining and bake hardening were characterised by X-ray diffraction, optical microscopy, transmission electron microscopy, three dimensional atom probe and tensile tests. Both steels exhibited discontinuous yielding behaviour and a significant strength increase with some reduction in ductility after pre-straining and bake hardening treatment. The following main microstructural changes are responsible for the observed mechanical behaviours: a decrease in the volume fl:action of retained austenite, a increase in the dislocation density and the formation of cell substructure in the polygonal ferrite, higher localized dislocation density in the polygonal ferrite regions adjacent to martensite or retained austenite, and the precipitation of fine iron carbides in bainite and martensite. The mechanism for the observed yield point phenomenon in both steels after treatment was analysed.

Electron backscattering diffraction analysis of an ancient wootz steel blade from central India

The electron backscattering diffraction technique was used to analyse the nature of carbides present in an ancient wootz steel blade. Bulky carbides, pro-eutectoid carbide along the prior austenite grain boundaries and fine spheroidized carbides were detected. Electron backscattering diffraction was employed to understand the texture of these carbides. The orientations of the cementite frequently occur in clusters, which points to a common origin of the members of the cluster. For the bands of coarse cementite, the origin is probably large coarse particles formed during the original cooling of the wootz cake. Pearlite formed earlier in the forging process has led to groups of similarly oriented fine cementite particles. The crystallographic texture of the cementite is sharp whereas that of the ferrite is weak. The sharp cementite textures point to the longevity of the coarse cementite throughout the repeated forging steps and to the influence of existing textured cementite on the nucleation of new cementite during cooling.

Effect of pre-straining and bake hardening on the microstructure and mechanical properties of CMnSi trip steels

The effects of pre-straining and bake hardening on the mechanical behaviour and microstructural changes were studied in two CMnSi TRansformation-Induced Plasticity (TRIP) steels with different microstructures after intercritical annealing. The TRIP steels before and after pre-straining and bake hardening were characterised by X-ray diffraction, optical microscopy, transmission electron microscopy, three dimensional atom probe and tensile tests. Both steels exhibited discontinuous yielding behaviour and a significant strength increase with some reduction in ductility after pre-straining and bake hardening treatment. The following main microstructural changes are responsible for the observed mechanical behaviours: a decrease in the volume fraction of retained austenite, an increase in the dislocation density and the formation of cell substructure in the polygonal ferrite, higher localized dislocation density in the polygonal ferrite regions adjacent to martensite or retained austenite, and the precipitation of fine iron carbides in bainite and martensite. The mechanism for the observed yield point phenomenon in both steels after treatment was analysed.

Effect of NbC and TiC precipitation on shape memory in an iron-based alloy

This paper examines the effects of TiC and NbC precipitation and prior cold rolling on the shape memory behaviour of an iron-based alloy. A precipitate-free alloy was used as a reference to investigate the relative contributions of prior-deformation and precipitation on shape memory. Heat treatment of the Nb- and Ti-containing alloys at 700 °C and 800 °C resulted in carbide precipitates between 120 nm and 220 nm in diameter. Bend testing of these samples showed a marginal increase in shape memory compared to the precipitate-free alloy. Under these conditions TiC precipitation exhibited slightly better shape memory than for NbC. However, this small increase was over-shadowed by the marked increase in shape memory that can be produced by subjecting the alloys to cold rolling followed by recovery annealing. When processed in this way, fine carbides are formed in the Ti- and Nb-containing alloys during the heat treatment. For particles >25 nm in diameter the shape memory is unaffected, but, it was found that small <5 nm particles have a detrimental effect on shape memory due to pinning of the martensite plates, thereby inhibiting their reversion to austenite. The optimum shape memory was observed in the precipitate-free alloy after cold rolling and recovery annealing.

Characterization of the bake-hardening behavior of transformation induced plasticity and dual-phase steels using advanced analytical techniques

The bake-hardening (BH) behavior of TRansformation Induced Plasticity (TRIP) and Dual-Phase (DP) steels after intercritical annealing (IA) has been studied using transmission electron microscopy, X-ray diffraction and three dimensional atom probe tomography. It was found for the DP steel that carbon can segregate to dislocations in the ferrite plastic deformation zones where there is a high dislocation density around the "asquenched" martensite. The carbon pinning of these dislocations, in turn, increases the yield strength after aging. It was shown that bake-hardening also leads to rearrangement of carbon in the martensite leading to the formation of rod-like low temperature carbides in the DP steel. Segregation of carbon to microtwins in retained austenite of the TRIP steel was also evident. These factors, in combination with the dislocation rearrangement in ferrite through the formation of cells and microbands in the TRIP steel after pre-straining, lead to the different bake-hardening responses of the two steels.

Understanding of the bainite transformation in a nano-structured bainitic steel

A 0.79C-1.5Si-1.98Mn-0.98Cr-0.24Mo-1.06Al-1.58Co (wt%) steel was isothermally heat treated at 200°C for 10 days to form a nano-scale bainitic microstructure consisting of nanobainitic ferrite laths with high dislocation density and retained austenite films. The crystallographic analysis using TEM and EBSD revealed that the bainitic ferrite laths are close to the Nishiyama-Wassermann orientation relationship with the parent austenite. There was only one type of packet identified in a given transformed austenite grain. Each packet consisted of two different blocks having variants with the same habit plane, but different crystallographic orientations. The presence of fine C-rich clusters and Fe-C carbides with a wide range of compositions in bainitic ferrite was revealed by Three-dimensional Atom Probe Tomography (APT). The high carbon content of bainitic ferrite compared to the para-equilibrium level of carbon in ferrite, absence of segregation of carbon to the austenite/bainitic ferrite interface and absence of partitioning of substitutional elements between the retained austenite and bainitic ferrite were also found using APT.