The evolution of microbands and their interaction with NbC precipitates during hot deformation of a Fe-30Ni-Nb model austenitic steel

The present work has investigated the evolution of microbands (MBs) and their interaction with strain-induced NbC precipitates during uniaxial compression of a model austenitic Fe-30Ni-Nb steel at 925 °C. The (1 1 0) fibre grains, both without and with copious amounts of precipitates, contained up to large strains crystallographic MBs aligned close to the highly stressed {1 1 1} slip planes having large Schmid factors. The MBs thus maintained their crystallographic character during straining, through continuously rearranging themselves, and did not follow the macroscopically imposed rigid body rotation. During double-pass deformation, fine NbC particles formed at short inter-pass holding remained strongly pinned at small reloading strains and appeared to be dragged by rearranging MB walls. With increasing reloading strain, the fine precipitates became progressively released from the above walls. During reloading after increased holding time, the coarsened particles tended with their increased size to become increasingly detached from the MB walls already at a small strain. The precipitate-free MB wall segments rearranged during straining to maintain their crystallographic alignment, while the detached precipitates followed the sample shape change and rotated towards the compression plane. The MB wall rearrangement generally occurred through cooperative migration of the corresponding dislocation networks.

The role of back stress caused by precipitates on {101-2} twinning in a Mg-6Zn alloy

In the present study, the effect of precipitate characteristics on {101-2} extension twinning have been studied in a Z6 magnesium alloy. A strongly textured Z6 alloy plate was mechanically tested in twinning dominated orientation in solution treated and aged states. Optical microscopy, transmission electron microscopy (TEM) and visco-plastic self consistent (VPSC) modelling are used to examine the effect of precipitate characteristics on twinning. The yield stress was observed to increase by ~80. MPa during ageing and it was estimated that CRSS for twinning increased by ~29. MPa based on VPSC simulations. The increment of twin system strengthening can be attributed to back stress generated by elastically deforming particles.

Size distribution and volume fraction of T1 phase precipitates from TEM images: Direct measurements and related correction

Transmission Electron Microscopy (TEM) can be used to measure the size distribution and volume fraction of fine scale precipitates in metallic systems. However, such measurements suffer from a number of artefacts that need to be accounted for, related to the finite thickness of the TEM foil and to the projected observation in two dimensions of the microstructure. We present a correction procedure to describe the 3D distribution of disc-like particles and apply this method to the plate-like T1 precipitates in an Al-Li-Cu alloy in two ageing conditions showing different particle morphologies. The precipitates were imaged in a High-Angular Annular Dark Field Microscope (HAADF-STEM). The corrected size distribution is further used to determine the precipitate volume fraction. Atom probe tomography (APT) is finally utilised as an alternative way to measure the precipitate volume fraction and test the validity of the electron microscopy results.

Effects of combined silicon and molybdenum alloying on the size and evolution of microalloy precipitates in HSLA steels containing niobium and titanium

The effects of combined silicon and molybdenum alloying additions on microalloy precipitate formation in austenite after single- and double-step deformations below the austenite no-recrystallization temperature were examined in high-strength low-alloy (HSLA) steels microalloyed with titanium and niobium. The precipitation sequence in austenite was evaluated following an interrupted thermomechanical processing simulation using transmission electron microscopy. Large (~ 105 nm), cuboidal titanium-rich nitride precipitates showed no evolution in size during reheating and simulated thermomechanical processing. The average size and size distribution of these precipitates were also not affected by the combined silicon and molybdenum additions or by deformation. Relatively fine (< 20 nm), irregular-shaped niobium-rich carbonitride precipitates formed in austenite during isothermal holding at 1173 K. Based upon analysis that incorporated precipitate growth and coarsening models, the combined silicon and molybdenum additions were considered to increase the diffusivity of niobium in austenite by over 30% and result in coarser precipitates at 1173 K compared to the lower alloyed steel. Deformation decreased the size of the niobium-rich carbonitride precipitates that formed in austenite.

Quantitative examination of carbide and sulphide precipitates in chemically complex steels processed by direct strip casting

A high strength low alloy steel composition has been melted and processed by two different routes: simulated direct strip casting and slow cooled ingot casting. The microstructures were examined with scanning and transmission electron microscopy, atom probe tomography and small angle neutron scattering (SANS). The formation of cementite (Fe3C), manganese sulphides (MnS) and niobium carbo-nitrides (Nb(C,N)) was investigated in both casting conditions. The sulphides were found to be significantly refined by the higher cooling rate, and developed an average diameter of only 100 nm for the fast cooled sample, and a diameter too large to be measured with SANS in the slow cooled condition (> 1.1 μm). Slow cooling resulted in the development of classical Nb(C,N) precipitation, with an average diameter of 7.2 nm. However, after rapid cooling both the SANS and atom probe tomography data indicated that the Nb was retained in the matrix as a random solid solution. There was also some evidence that O, N and S are also retained in solid solution in levels not found during conventional processing.

In-situ X-ray diffraction studies of slip and twinning in the presence of precipitates in AZ91 alloy

The effect of basal plate precipitates on the hardening of basal slip and {101¯2} twinning modes was investigated for a non-aged and aged AZ91 alloy in the twin dominated strain paths. Exploiting in-situ synchrotron and laboratory based X-ray diffraction methodologies, we quantified the critical resolved shear stress (CRSS) for basal slip and twinning modes. The twin volume fraction changes were quantified from the intensity changes with applied load. We observed that the twin volume fraction changes with plastic strain is sensitive to the initial texture, while the relative hardening of different deformation modes are considered as a secondary effect. We also found that the twin interior stresses were significantly smaller and consistent with the high twin back stresses in the presence of precipitates. We propose, based on a simple analytical equation, that the leading edge of the propagating twin have a Burgers vector equivalent to 100 twinning dislocations and when the propagating twin is blocked by a precipitate, relatively high resolved stress is required for bowing the twin dislocation and hence the propagation of the twin occurs by the dissociation of the leading edge of the twinning dislocation.

Interaction between the coating characteristics of galvanneal steel and forming parameters during flat die drawing

Galvanneal steel is considered to be better for automotive applications than its counterpart, galvanized steel, mainly because of its superior coating and surface properties. Galvanneal steel is produced by hot dipping sheet steel in a bath of molten zinc with small, controlled, levels of aluminium, followed by annealing which creates a Fe-Zn intermetallic layer. This intermetallic layer of the coating improves spot weldability and improves subsequent paint appearance. However, if the microstructure of the coating is not properly controlled and forming parameters are not properly selected, wear of the coating could occur during stamping. Frictional sliding of the sheet between the tool surfaces results in considerable amount of coating loss. An Interstitial Free steel with a Galvanneal coating of nominally 60g/m2 was used for the laboratory experiments. Flat Face Friction (FFF) tests were performed with different forming conditions and lubricants to simulate the frictional sliding in stamping. Glow-Discharge Optical Emission Spectrometry (DG-OES) was used to measure the change in the coating thickness during sliding. Optical microscopy was considered for imaging the surfaces as well as an optical method to compare the changes in the coating thickness during the forming. The change to the Galvanneal coating thickness was found to be a function of forming parameters.

Effect of carbon content on the recrystallization kinetics of Nb-steels

A rapid method was used to study the effect of carbon content on the kinetics of post-deformation softening, t50, in Nb-steels. The hot deformation behaviour of austenite was not affected by carbon. However, the t50 was influenced by the carbon with different effects in different temperature regimes. At deformation temperatures above the non-recrystallization temperature, Tnr, carbon produced a small change in the softening behaviour. However, the t50 was significantly retarded with increasing carbon content at deformation temperatures lower than Tnr, due to Nb(C,N) precipitates.

The recrystallization behaviour of Nb microalloyed steels

The deformation and recrystallization behaviour of a range of Nb microalloyed steels has been studied using hot torsion. This work focuses on the change from strain dependent to strain independent recrystallization behaviour as a function of the alloy content, initial microstructure and deformation conditions. It is found that there is a complex interaction between deformation, recrystallization and strain induced precipitation, which has significant implications for controlled rolling in hot strip and plate mills. The data also revealed that the pre-existing precipitates did not influence the behaviour of post deformation softening.

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%.

Biliary intervention augments chemotactic reaction and aggravates cholestatic liver injury in rats

Background
Intervention of the biliary system is frequently done in patients with obstructive jaundice and is associated with significant morbidity and mortality. The pathogenesis is unknown.
Materials and methods
A rat model of bile duct ligation (BDL) for 2 weeks was established in which biliary intervention was feasible by injection of normal saline through an indwelling catheter in the bile ducts. Plasma levels of C-C chemokine MCP-1 and C-X-C chemokine MIP-2 were measured by using ELISA. Blood monocytes, Kupffer cells, and neutrophils in the liver were characterized with antibodies to ED1, ED2, and myeloperoxidase (MPO). Lipid peroxidation was measured by malondialdehyde contents and apoptosis by TUNEL stain of the liver.
Results
Biliary intervention resulted in an increase of plasma MCP-1 and MIP-2 proteins by 1 h, which declined to normal level by 3 h in both sham and BDL rats. The levels in BDL rats were significantly higher than in sham at most points. There was a transient increase of ED1- and ED2-positive cells and MPO-staining cells in sham rat liver by 1 h after intervention. ED2-positive cells increased significantly by 1 h, while ED1- and MPO-positive cells decreased, yet insignificantly after intervention in BDL rats. The cell counts in BDL were constantly higher than in sham. Malondialdehyde increased precipitously in BDL by 3 h and was significantly higher than in sham throughout the study period. Parenchymal liver injury, manifested by elevated ALT, as well as apoptosis and necrosis of liver cells, was significantly increased in BDL rats, but not in sham rats.
Conclusion
Biliary intervention augments chemokine expression, precipitates lipid peroxidation, and aggravates liver injury in cholestatic rats.

Properties of mechanically milled and spark plasma sintered Al–15 at.% MgB2 composite materials

Air-atomized pure aluminium powder with 15 at.% MgB₂ was mechanically milled (MMed) by using a vibrational ball mill, and MMed powders were consolidated by spark plasma sintering (SPS) to produce composite materials with high specific strength. Solid-state reactions of MMed powders have been examined by X-ray diffraction (XRD), and mechanical properties of the SPSed materials have been evaluated by hardness measurements and compression tests. Orientation images of microstructures were obtained via the electron backscatter diffraction (EBSD) technique.

The solid-state reactions in the Al–15 at.% MgB₂ composite materials occurred between the MMed powders and process control agent (PCA) after heating at 773–873 K for 24 h. The products of the solid-state reaction were a combination of AlB₂, Al₃BC and spinel MgAl₂O₄. Mechanical milling (MM) processing time and heating temperatures affect the characteristics of those intermetallic compounds. As the result of the solid-state reactions in MMed powders, a hardness increase was observed in MMed powders after heating at 573–873 K for 24 h. The full density was attained for the SPSed materials from 4 h or 8 h MMed powders in the Al–15 at.% MgB₂ composite materials under an applied pressure of 49 MPa at 873 K for 1 h. The microstructure of the SPSed materials fabricated from the MMed powders presented the bimodal aluminium matrix grain structure with the randomly distributions. The Al–15 at.% MgB₂SPSed material from powder MMed for 8 h exhibited the highest compressive 0.2% proof strength of 846 MPa at room temperature.

Microstructures and bond strengths of the calcium phosphate coatings formed on titanium from different simulated body fluids

Calcium phosphate (Ca-P) coatings were deposited on Ti substrates by a biomimetic method from m-SBF and 10× SBF, respectively. Comparative study of microstructures and bond strengths of the Ca-P coatings deposited from those different SBFs was carried out. Effect of the surface roughness of the substrates on the bond strength of the Ca-P coatings was also studied. Scanning electron microscopy (SEM), X-ray diffractometry (XRD), Fourier transformed infrared spectroscopy (FTIR), inductive coupled plasma spectrometry (ICP) and thermogravimetry (TG) were used to characterize the Ca-P coatings. The bond strengths between the coatings and Ti substrates were measured using an adhesive strength test. Results indicated that the ionic concentrations of the SBFs and the surface roughness of the substrate had a significant influence on the formation, morphology and bond strength of the Ca-P precipitates. The induction period of time to deposit a complete Ca-P layer from the m-SBF is much longer, but the Ca-P coating is denser and has higher bond strength than that formed from the 10× SBF. The Ti with a surface roughness of R_a 0.64 µm and R_z 2.81 µm favoures the formation of a compact Ca-P coating from the m-SBF with the highest bond strength of approximately 15.5 MPa.

The kinetics of two-stage formation of TiAl3 in multilayered Ti/Al foils prepared by accumulative roll bonding

The solid-state reactions of Ti/Al multilayered samples produced by Accumulative Roll Bonding (ARB) have been investigated using differential scanning calorimetry, X-ray diffraction and scanning electron microscopy. The kinetics of the formation of the intermetallic compound TiAl3 was highlighted. Experimental evidence and analysis of the data shows that, there was a two-stage process in the formation of TiAl₃ in the ARB Ti/Al reactive multilayered samples. Calorimetric and microstructural analyses also suggest that the interdiffusion of Al and Ti which led to solid solutions preceded the formation of intermetallic compounds. Despite the apparent chaos in the thickness of the ARB multilayered samples, the distribution of layer spacing did not become broad enough to lose the main features of the double exothermal behaviour. Isothermal DSC shows a larger Avarami constant in ARB Ti/Al multilayered structures than was found in Ti/Al thin films. A modified model based on thin films was set up to describe the kinetic characteristics of the formation of the intermetallic compound TiAl₃ in ARB samples.