Atom probe tomography as a tool to advance steels design and performance

Development of modern steels consisting of complex or nano-scale microstructures with advanced properties requires in-depth understanding of the mechanisms responsible for their microstructure/property relationships. The evolution of microstructure during processing is often associated with various changes taking place at atomic level. These include solute distribution between phases as a result of phase transformations, formation of atmospheres at dislocations, clustering and precipitation phenomena due to various thermo-mechanical processing schedules and/or heat treatments. Atom probe tomography (APT) is invaluable tool for gaining insight into events at atomic scale determining the steel properties. This technique also contributes to the fundamental understanding of phase transformations, which is essential for nano-scale engineering of modern steels and optimization of their performance. In this work application of APT to study solute segregation, clustering and precipitation in TRIP steels and nanostructured bainitic steels after isothermal heat-treatment and after thermomechanical processing will be discussed.

Application of advanced experimental techniques for the microstructural characterization of nanobainitic steels

A 0.79C-1.5Si-1.98Mn-0.98Cr-0.24Mo-1.06Al-1.58Co (wt%) steel was isothermally heat treated at 350°C bainitic transformation temperature for 1 day to form fully bainitic structure with nano-layers of bainitic ferrite and retained austenite, while a 0.26C-1.96Si-2Mn-0.31Mo (wt%) steel was subjected to a successive isothermal heat treatment at 700°C for 300 min followed by 350°C for 120 min to form a hybrid microstructure consisting of ductile ferrite and fine scale bainite. The dislocation density and morphology of bainitic ferrite, and retained austenite characteristics such as size, and volume fraction were studied using Transmission Electron Microscopy. It was found that bainitic ferrite has high dislocation density for both steels. The retained austenite characteristics and bainite morphology were affected by composition of steels. Atom Probe Tomography (APT) has the high spatial resolution required for accurate determination of the carbon content of the bainitic ferrite and retained austenite, the solute distribution between these phases and calculation of the local composition of fine clusters and particles that allows to provide detailed insight into the bainite transformation of the steels. The carbon content of bainitic ferrite in both steels was found to be higher compared to the para-equilibrium level of carbon in ferrite. APT also revealed the presence of fine C-rich clusters and Fe-C carbides in bainitic ferrite of both steels.

Effect of composition and processing parameters on the formation of nano-bainite in advanced high strength steels

The nano-bainitic microstructures were compared in a 0.79C-1.5Si-1.98Mn-0.24Mo-1.06Al (wt%) steel after isothermal heat-treatment and a Fe-0.2C-1.5Mn-1.2Si-0.3M0-0.6Al-0.02Nb (wt%) steel after controlled thermo-mechanical processing. The microstructure for both steels consisted of bainite. The microstructural characteristics of bainite, such as the morphology of the nano-bainite and thicknesses of bainitic ferrite and retained austenite layers, as a function of steel composition and processing was studied using transmission electron microscopy (TEM). It was found that the nano-bainitic structure can be formed in the low alloy steel through thermomechanical processing. Atom probe tomography (APT) was employed as a powerful technique to determine local composition distributions in three dimensions with atomic resolution. The important conclusions from the APT research were that the carbon content of bainitic ferrite is higher than expected from paraequilibrium level of carbon in ferrite for both steels and that Fe-C clusters and fine particles are formed in the bainitic ferrite in both steels despite the high level of Si.

In vitro behavior of human osteoblast-like cells (SaOS2) cultured on surface modified titanium and titanium–zirconium alloy

In this study, titanium (Ti) and titanium-zirconium (TiZr) alloy samples fabricated through powder metallurgy were surface modified by alkali-heat treatment and calcium (Ca)-ion-deposition. The alteration of the surface morphology and the chemistry of the Ti and TiZr after surface modification were examined. The bioactivity of the Ti and TiZr alloys after the surface modification was demonstrated. Subsequently, the cytocompatibility of the surface modified Ti and TiZr was evaluated via in vitro cell culture using human osteoblast-like cells (SaOS2). The cellular attachment, adhesion and proliferation after cell culture for 14 days were characterized by scanning electron microscopy (SEM) and MTT assay. The relationship between surface morphology and chemical composition of the surface modified Ti and TiZr and cellular responses was investigated. Results indicated that the surface-modified Ti and TiZr alloys exhibited excellent in vitro cytocompatibility together with satisfactory bioactivity. Since osteoblast adhesion and proliferation are essential prerequisites for a successful implant in vivo, these results provide evidence that Ti and TiZr alloys after appropriate surface modification are promising biomaterials for hard tissue replacement.

Wear characteristics of ultra-hard cutting tools when machining austempered ductile iron

Nodularised Ductile Cast Iron, when subjected to heat treatment processes - austenitising and austempering produces Austempered Ductile Iron (ADI). The microstructure of ADI also known as "ausferrite" consists of ferrite, austenite and graphite nodules. Machining ADI using conventional techniques is often a problematic issue due to the microstructural phase transformation from austenite to martensite during machining. This paper evaluates the wear characteristics of ultra hard cutting tools when machining ADI and its effect on machinability. Machining trials consist of turning ADI (ASTMGrade3) using two sets of PCBN tools with 90% and 50% CBN content and two sets of ceramics tools; Aluminium Oxide Titanium Carbide and Silicon Carbide - whisker reinforced Ceramic. The cutting parameters chosen are categorized as roughing and finishing conditions; the roughing condition comprises of constant cutting speed (425 m/min) and depth of cut (2mm) combined with variable feed rates of 0.1, 0.2, 0.3 and 0.4mm/rev. The finishing condition comprises of constant cutting speed (700 m/min) and depth of cut (0.5mm) combined with variable feed rates of 0.1, 0.2, 0.3 and 0.4mm/rev. The benchmark condition to evaluate the performance of the cutting tools was tool wear evaluation, surface texture analysis and cutting force analysis. The paper analyses thermal softening of the workpiece by the tool and its effect on the shearing mechanism under rough and finish machining conditions in term of lower cutting forces and enhanced surface texture of the machined part.

Influence of grain size and training temperature on strain of polycrystalline Ni50Mn29Ga21 samples

The alloy Ni-Mn-Ga aroused great interest for application as a magnetic shape memory (MSM) material. This effect is caused by reorientation of twin variants by an external magnetic field. So far, most of the experiments were concentrated on single crystals. But, the MSM effect can also be realised in polycrystals which can be prepared much more efficiently. Here, polycrystalline samples were prepared by directional solidification with a <100> fibre texture of the high temperature cubic austenitic phase parallel to the heat flow. Afterwards, a heat treatment was applied for chemical homogenisation and stress relaxation in the austenitic state. Then the samples were heated up to the austenitic state and cooled down under load. The microstructure was analysed by Electron Back Scatter Diffraction (EBSD) before and after that treatment. Mechanical training at room temperature and 40°C was tracked by recording stress-strain curves. By increasing the number of training cycles the strain also increases. The influence of different training temperatures was investigated on samples with different grain sizes.

Characterization of 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 produce a nano-structured bainitic steel. The microstructure consisted of nanobainitic ferrite laths with a high dislocation density and retained austenite films having extensive twins. The crystallographic analysis using TEM and EBSD revealed that the bainitic ferrite laths are close to the Nishiyama-Wassermann orientation relationship with their 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. Atom Probe Tomography (APT) revealed that the carbon content of nanobainitic ferrite laths was much higher than expected from the para-equilibrium level. This was explained due to the long heat treatment time, which led to the formation of fine Fe-C clusters on areas with high dislocation densities in bainitic ferrite laths.

Imparting sensitization resistance to an Al-5Mg alloy via Nd addition

Low-level Nd additions, up to 0.17 wt%, were added to Al-5Mg to explore the impact on the subsequent degree of sensitization. Following heat treatment at 150°C for 1 day and 7 days, nitric acid mass loss (NAMLT) tests revealed that additions of >0.11% Nd were effective at decreasing the amount of subsequent intergranular attack.

The effect of microstructure on the decrease of the apparent Young's Modulus in DP 780 steel

Currently, there is a significant effort into developing novel multiphase microstructures to further improve the strength/ductility combination of advanced high-strength steels. To achieve this, the effect of the microstructure on sheet formability needs to be further understood. In this study, the effect of the microstructure on the variation of the elastic modulus in loading and unloading of DP 780 steel has been investigated. Five microstructures with varying volume fractions of ferrite and martensite were generated using different heat treatment cycles. Tension tests were performed to different strain values and the Young’s Modulus during loading and unloading was determined. The test results show that the reduction in unloading modulus with prestrain depends on the volume fraction and hardness of the martensitic phase.

Cryo-rolling and formability of 2024 aluminium

Sheets of precipitate hardenable 2024 aluminium have been processed by rolling at liquid nitrogen temperature in order to refine the microstructure. A number of different aging/heat treating procedures have been utilised that have resulted in significantly different mechanical properties. The cryo-rolled material was heat treated at 150 °C for varying times and the resulting mechanical properties evaluated as a function of this holding time. The resulting properties were found to be strongly influenced by precipitates that formed either during the aging step, rolling process or the subsequent heat treatment. The formability of the cryo-rolled and heat treated material has been investigated using a limiting dome height test (Erichsen cupping test).

Phase-structure effects of electrospun TiO2 nanofiber membranes on As(III) adsorption

TiO2 nanofibers (NFs) with different phases such as amorphous, anatase, mixed anatase?rutile, and rutile have been prepared by combining the electrospinning technique with the subsequent process of heat treatment or acidic-dissolution method. The obtained NFs are characterized by a Fourier transform infrared spectrometer (FT-IR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and N2 adsorption?desorption isotherm measurements. Phase structure effects of electrospun TiO2 NFs on As(III) adsorption behaviors have been investigated. The results showed a significant effect of the phase structures of TiO2 NFs on As(III) adsorption rates and capacities. Amorphous TiO2 NFs have the highest As(III) adsorption rate and capacity in the investigated samples, which can be attributed to its higher surface area and porous volume. This research provides a simple and low-cost method for phasecontrolled fabrication of TiO2 NFs and application for effective removal of arsenic from aqueous solution.

A case study on effect of feed rate on machinability of austempered ductile iron

Austempered Ductile Iron (ADI) is a type of nodular, ductile cast iron subjected to heat treatments - austenitising and austempering. Whilst machining is conducted prior to heat treatment and offers no significant difficulty, machining post heat treatment is demanding and often avoided. Phase transformation of retained austenite to martensite leading to poor machinability characteristics is a common problem experienced during machining. This case study explains the effect of feed rate on machinability of ADI using cutting force analysis and tool failure analysis. The experimental design consists of conducting drilling trials on grade 1200 and 1400 at constant depth of cut, 25mm; constant speed, 45m/min; no coolant and variable feed rates from 0.2 to 0.35 mm/rev (increment of 0.025mm/rev). Metallography and X-ray diffraction technique was carried out in order to identify and quantify the microstructural phases before and after drilling. The results from the trial infer that the best way to machine ADI efficiently without tool failure is using low feeds and high speeds and without coolant.