Crystalline Structures and α → β and γ polymorphs transformation induced by nanoclay in PVDF-based nanocomposite

Poly(vinylidene fluoride) (PVDF) nanocomposites were prepared by melt-mixing. The dispersion of clay platelets and rheology of nanocomposites were analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and rheometric mechanical spectrometer (RMS). The transformation of α to β and γ phase in PVDF was induced by the addition of nanoclay and subsequently the isothermal crystallization kinetics of neat PVDF and its nanocomposite have been investigated. The interaction between clay nanofillers and PVDF macromolecular chains induced the change of conformation from trans-gauche to all-trans crystal structure in PVDF segment. The isothermal crystallization of PVDF/clay nanocomposites was carried out by Differential Scanning Calorimetry (DSC) technique. The influence of clay platelets on nucleation crystallization rate and Avrami exponent were studied. PVDF/clay nanocomposite showed higher crystallization rate indicating that nanoclay has acted as an effective nucleation agent. This nucleation effect of nanoclay increased the Avrami exponent and decreased the degree of crystallinity. © 2014 World Scientific Publishing Company.

Equal-channel angular pressing and annealing of a twinning-induced plasticity steel : microstructure, texture, and mechanical properties

In this work, a high-manganese Fe-23Mn-1.5Al-0.3C Twinning-Induced Plasticity (TWIP) steel was subjected to plastic shear deformation using Equal-Channel Angular Pressing (ECAP) at 300 °C following route BC and additional annealing. The microstructure evolution during both deformation by ECAP and subsequent annealing was investigated and correlated with the mechanical properties. The successive grain refinement during ECAP was promoted by two parallel mechanisms, namely dislocation driven grain fragmentation and twin fragmentation, and accounted for the ultra-high strength. In addition, due to the relatively low volume fraction of deformation twins after ECAP at 300 °C, further contribution of deformation twinning during room temperature deformation allowed additional work-hardening capacity and elongation. During subsequent recovery annealing the ultra-fine grains and deformation twins were thermally stable, which supported retainment of the high yield strength along with regained uniform elongation. For the first time, the texture evolution during ECAP and during the following heat treatment was analyzed. After 1, 2, and 4 ECAP passes a transition texture with the characteristic texture components of both high- and low-SFE materials developed. During the following heat treatment the texture evolution proceeded similar to that observed in the same material after cold rolling. Retaining of the ECAP texture components due to oriented nucleation at grain boundaries and triple junctions as well as annealing twinning accounted for the formation of a weak, retained ECAP texture after recrystallization.

Three-dimensional atom probe analysis of solute distribution in thermomechanically processed TRIP steels

Complex multiphase microstructures were obtained in transformation induced plasticity C–Mn–Si–(Nb–Al–Mo) steels by simulated controlled thermomechanical processing. These microstructures were characterized using transmission electron microscopy, X-ray diffraction and three-dimensional atom probe tomography (APT), which was used to determine the partitioning of elements between different phases and microconstituents. The measured carbon concentration (not, vert, similar0.25 at%) in the ferrite of carbide-free bainite was higher than expected from para-equilibrium between the austenite and ferrite, while the concentrations of substitutional elements were the same as in the parent austenite suggesting that incomplete bainite transformation occurred. In contrast, the distribution of substitutional elements between the ferrite lath and austenite in carbide-containing bainite indicated a complete bainite reaction. The average carbon content in the retained austenite (3.2 ± 1.6 at%) was somewhat higher than the T0 limit. On the basis of the APT measured composition, the calculated Ms temperatures for retained austenite were above room temperature, indicating its low chemical stability.

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%.

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 susceptibility to interfacial fracture on fatigue properties of spot-welded high strength sheet steel

While advanced high strength steels (AHSS) have numerous advantages for the automotive industry, they can be susceptible to interfacial fracture when spot-welded. In this study, the susceptibility of interfacial fracture to spot-weld microstructure and hardness is examined, as well as the corresponding relationships between fatigue, overload performance, and interfacial fracture for a TRIP (transformation induced plasticity) steel. Simple post-weld heat-treatments were used to alter the weld microstructure. The effect on interfacial fracture of diluting the weld pool by welding the TRIP material to non-TRIP steel was examined, along with the effect of altering the base material microstructure. Results show that weld hardness is not a good indicator of either the susceptibility to interfacial fracture, or the strength of the joint, and that interfacial fracture does not necessarily lead to a decrease in strength compared to conventional weld-failure mechanisms, i.e. button pullout. It was also found that while interfacial fracture does affect low cycle to failure behavior, there was no effect on high cycle fatigue.

Microstructure and mechanical properties of C-Si-Mn(-Nb) TRIP steels after simulated thermomechanical processing

Continuous and discontinuous cooling tests were performed using a quench deformation dilatometer to develop a comprehensive understanding of the structural and kinetic aspects of the bainite transformation in low carbon TRIP (transformation induced plasticity) steels as a function of thermomechanical processing and composition. Deformation in the unrecrystallised austenite region refined the ferrite grain size and increased the ferrite and bainite transformation temperatures for cooling rates from 10 to 90 K s^-1. The influence of niobium on the transformation kinetics was also investigated. Niobium increases the ferrite start transformation temperature, refines the ferrite microstructure, and stimulates the formation of acicular ferrite. The effect of the bainite isothermal transformation temperature on the final microstructure of steels with and without a small addition of niobium was studied. Niobium promotes the formation of stable retained austenite, which influences the mechanical properties of TRIP steels. The optimum mechanical properties were obtained after isothermal holding at 400°C in the niobium steel containing the maximum volume fraction of retained austenite with acicular ferrite as the predominant second phase.

Statistical analysis of finite element modeling in sheet metal forming and springback analysis

This work focuses on development of a method to statistically study forming and springback problems of TRansformation Induced Plasticity (TRIP) through an industrial case study. A Design of Experiments (DOE) approach was used to study the sensitivity of predictions to four user input parameters in implicit and explicit sheet metal forming codes. Numerical results were compared to experimental measurements of parts stamped in an industrial production line. The accuracy of forming strain predictions for TRIP steel were comparable with conventional steel, but the springback predictions of TRIP steel were far less accurate. The statistical importance of selected parameters for forming and springback prediction is also discussed. Changes of up to ±10% in Young's modulus and coefficient of friction were found to be insignificant in improving or deteriorating the statistical correlation of springback accuracies.

Multiphase material modelling by multiscale particle-in-cell method

A particle-based method for multiscale modeling of multiphase materials such as Dual Phase (DP) and Transformation Induced Plasticity (TRIP) steels has been developed. The multiscale Particle-In-Cell (PIC) method benefits from the many advantages of the FEM and mesh-free methods, and to bridge the micro and macro scales through homogenization. The conventional mesh-based modeling methods fail to give reasonable and accurate predictions for materials with complex microstructures. Alternatively in the multiscale PIC method, the Lagrangian particles moving in an Eulerian grid represent the material deformation at both the micro and macro scales. The uniaxial tension test of two phase and three-phase materials was simulated and compared with FE based simulations. The predictions using multiscale PIC method showed that accuracy of field variables could be improved by up to 7%. This can lead to more accurate forming and springback predictions for materials with important multiphase microstructural effects.

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.

A study of the strengthening mechanism in the thermomechanically processed TRIP/TWIP steel

The strengthening mechanism responsible for the unique combination of ultimate tensile strength and elongation in a multiphase Fe-0.2C-1.5Mn-1.2Si-0.3Mo-0.6Al-0.02Nb (wt%) steel was studied. The microstructures with different volume fraction of polygonal fenite, bainite and retained austenite were simulated by controlled thermomechanical processing. The interupted tensile test was used to study the bainitic ferrite, retained austenite and polygonal ferrite behavior as a function of plastic strain. X-ray analysis was used to characterize the volume fraction and carbon content of retained austenite. TEM and heat-tinting were utilized to analyze the effect of bainitic fenite morphology on the strain induced transformation of retained austenite and retained austenite twinning as a function of strain in the bulk material. The study has shown that the austenite twinning mechanism is more preferable than the transformation induced plasticity mechanism during the early stages of deformation for a microstructure containing I5% polygonal ferrite, while the transformation induced plasticity effect is the main mechanism in when there is 50% of polygonal ferrite in the microstructure. The baillitic fenite morphology affects the deformation mode of retained austenite during straining. The polygonal fenite behavior during straining depends on dislocation substructure tonned due to the deformation and the additional mobile dislocations caused by the TRIP effect. TRIP and TWIP effects depend not only on the chemical and mechanical stability of retained austenite, but also on the interaction of the phases during straining.

Cyclic deformation of advanced high-strength steels : mechanical behavior and microstructural analysis

The fatigue properties of multiphase steels are an important consideration in the automotive industry. The different microstructural phases present in these steels can influence the strain life and cyclic stabilized strength of the material due to the way in which these phases accommodate the applied cyclic strain. Fully reversed strain-controlled low-cycle fatigue tests have been used to determine the mechanical fatigue performance of a dual-phase (DP) 590 and transformation-induced plasticity (TRIP) 780 steel, with transmission electron microscopy (TEM) used to examine the deformed microstructures. It is shown that the higher strain life and cyclic stabilized strength of the TRIP steel can be attributed to an increased yield strength. Despite the presence of significant levels of retained austenite in the TRIP steel, both steels exhibited similar cyclic softening behavior at a range of strain amplitudes due to comparable ferrite volume fractions and yielding characteristics. Both steels formed low-energy dislocation structures in the ferrite during cyclic straining.

Microstructure and mechanical properties of thermomechanically processed TRIP steel

The strengthening mechanism responsible for the unique combination of ultimate tensile strength and elongation in a multiphase Fe-0.2C-1.5Mn-1.2Si-0.3Mo-0.6Al-0.02Nb (wt%) steel was studied. The microstructures with different volume fractions of polygonal ferrite, bainite and retained austenite were simulated by controlled thermomechanical processing. The interrupted tensile test was used to study the bainitic ferrite, retained austenite and polygonal ferrite behaviour as a function of plastic strain. X-ray analysis was used to characterise the volume fraction and carbon content of retained austenite. Transmission electron microscopy was utilised to analyse the effect of bainitic ferrite morphology on the strain induced transformation of retained austenite and retained austenite twinning as a function of strain in the bulk material. The study has shown that the austenite twinning mechanism is more preferable than the transformation induced plasticity (TRIP) mechanism during the early stages of deformation for a microstructure containing 15% polygonal ferrite, while the transformation induced plasticity effect is the main mechanism when there is 50% of polygonal ferrite in the microstructure. The bainitic ferrite morphology affects the deformation mode of retained austenite during straining. The polygonal ferrite behaviour during straining depends on dislocation substructure formed due to the deformation and the additional mobile dislocations caused by the TRIP effect. Operation of TRIP or twinning mechanisms depends not only on the chemical and mechanical stability of retained austenite, but also on the interaction of the phases during straining.

Effect of bake-hardening on the structure-property relationship of multiphase steels for the automotive industry

The effect of a bake-hardening (BH) treatment on the microstructure and mechanical properties has been studied in C-Mn-Si TRansformation Induced Plasticity (TRIP) and Dual Phase (DP) steels after: (i) thermomechanical processing (TMP) and (ii) intercritical annealing (IA). The steels were characterized using X-ray diffraction, transmission electron microscopy (TEM) and three-dimensional atom probe tomography (APT). All steels showed high BH response. however, the DP and trip steels after IA/BH showed the appearance of upper and lower yield points, while the stress-strain behavior of the trip steel after TMP/BH was still continuous. This was due to the higher volume fraction of bainite and more stable retained austenite in the TMP/BH steel, the formation of plastic deformation zones with high dislocation density around the "as-quenched” martensite and “TRIP” martensite in the IA/BH DP steel and IA/BH TRIP steel, respectively.

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.