Accurate determination of the number density of G-phase precipitates in thermally aged duplex stainless steel

G-phase precipitation in the ferrite phase in thermally aged duplex stainless steel (DSS) was investigated. A needle-shaped sample of DSS aged at 673?K for 5000?h was observed by transmission electron microscopy (TEM), and subsequently by atom probe tomography (APT). The precipitates of the G-phase observed by TEM corresponded well to clustering atoms observed by APT. On the other hand, regarding the precipitates of the G-phase that formed in an earlier stage of aging, the present study suggests that not all the precipitates can be detected by TEM. A large area of DSS aged at 673?K for 5000?h containing both the ferrite and austenite phases was observed. The number density of precipitates of the G-phase in the ferrite phase was small in the vicinity of the phase boundary and increased with the distance between the phase boundary and each field of view. The number density reached an almost constant value at a distance of approximately 4?µm from the phase boundary. The suppression of G-phase precipitation in the vicinity of the phase boundary is discussed in terms of the depletion of alloying elements that comprise the G-phase.     

Effects of molybdenum on precipitation behaviours in aged cast stainless steels

The effects of Mo on precipitation behaviours in aged cast stainless steels have been investigated. Mo-free CF3 steel and Mo-bearing CF3M steel, both of which consisted of a duplex structure of ferrite and austenite phases, were prepared. Microstructural evolution in the ferrite phase during ageing at 723 K has been observed by transmission electron microscopy (TEM). Precipitates in CF3 steel were identified to belong to the G-phase and possess lattice coherency with the ferrite phase at interphase boundaries. On the other hand, precipitates in CF3M steel were found to be nanodomains of not only to the G-phase but also to another phase enriched in Mo. Some of the nanodomains containing Mo exhibited diffraction patterns having pseudo five-fold symmetry, but others exhibited regular periodicity in high-resolution TEM images. The atomic structure of the Mo-related nanodomains is proposed to be a distorted χ-phase that retains coherency with the matrix.     

Effects of aging temperature on G-phase precipitation and ferrite-phase decomposition in duplex stainless steel

G-phase precipitation and ferrite-phase decomposition in a cast duplex stainless steel (DSS) aged at 623–723?K for up to 8000?h were investigated using atom probe tomography (APT). Large sample volume was observed in every APT experiment, which yielded significantly statistical results. The number density of G-phase precipitates tended to be high and their sizes were small at lower aging temperatures. G-phase precipitates grew during prolonged isothermal aging. The concentrations of nickel, silicon, manganese and molybdenum in G-phase precipitates tended to increase as the precipitates grew. Heterogeneous distributions of alloying elements within G-phase precipitates were observed. An interesting positional relationship of G-phase precipitates with dislocations was revealed. Regarding the ferrite-phase decomposition, local chromium concentrations in the ferrite phase varied fast at higher aging temperatures. Good correlation between the variation of local chromium concentrations and aging conditions was revealed, which indicates that the variation can be estimated for arbitrary aging conditions. Representative distances between chromium-enriched and chromium-diluted regions were long at higher aging temperatures. Time exponent of the representative distances of ferrite-phase decomposition as well as the size of G-phase precipitates increased with aging temperatures.     

Correlative microscopy of a carbide-free bainitic steel

In this work a carbide-free bainitic steel was examined by a novel correlative microscopy approach using transmission Kikuchi diffraction (TKD) and transmission electron microscopy (TEM). The individual microstructural constituents could be identified by TKD based on their different crystal structure for bainitic ferrite and retained austenite and by image quality for the martensite–austenite (M–A) constituent. Subsequently, the same area was investigated in the TEM and a good match of these two techniques regarding the identification of the area position and crystal orientation could be proven. Additionally, the M–A constituent was examined in the TEM for the first time after preceded unambiguous identification using a correlative microscopy approach. The selected area diffraction pattern showed satellites around the main reflexes which might indicate a structural modulation.     

Correlative atomic scale characterisation of secondary carbides in M50 bearing steel

Correlative atom probe tomography (APT) and transmission electron microscopy (TEM) are used to characterise the microstructure and chemistry of carbide precipitation in M50 bearing steel. This is a prerequisite in establishing relationships between the microstructure and hydrogen embrittlement (HE) resistance. Secondary carbides are the focus of this study, as they play a major role in improving HE-resistance. Secondary carbides are observed in APT, with compositions close to M₄C_3, M₂C and M₃C. Correlative TEM measured orientation relationships between the martensite matrix and carbides, enabling the confirmation of M₃C cementite precipitates in the corresponding APT reconstruction. Additionally, other precipitates observed in TEM were correlated to the M₂C carbides in APT data. The M₄C₃ carbides are found to have a significantly lower volume fraction than the M₂C carbides.     

Formation of fully pearlitic microstructure in medium carbon steel

Pearlitic microstructure can be obtained when austenite of eutectoid composition is slowly cooled from high temperature to below the Ae₃ temperature. It is also possible to induce such structure in hypo-eutectoid composition of austenite through proper heat treatment as well. However, in the current work, one hypo-eutectoid steel during very slow cooling only produced completely pearlitic microstructure which was not expected from a steel with such composition. The calculations carried out considering orthoequilibrium condition actually predicted the presence of about 37% ferrite in the microstructure. Further calculations considering different equilibrium modes and kinetics of transformation indicates that the composition and thermal condition of the steel under consideration was such that proeutectoid ferrite formation could not start before the composition reaches to the Negligible Partitioning Local Equilibrium phase boundary which further coincides with the area described by Hultgren extrapolation and thus, the steel completely transforms to pearlite even with hypo-eutectoid composition during very slow cooling.     

Five-parameter crystallographic characteristics of the interfaces formed during ferrite to austenite transformation in a duplex stainless steel

The crystallography of interfaces in a duplex stainless steel having an equiaxed microstructure produced through the ferrite to austenite diffusive phase transformation has been studied. The five-parameter interface character distribution revealed a high anisotropy in habit planes for the austenite–ferrite and austenite–austenite interfaces for different lattice misorientations. The austenite and ferrite habit planes largely terminated on (1 1 1) and (1 1 0) planes, respectively, for the austenite–ferrite interfaces associated with Kurdjumov–Sachs (K–S) and Nishiyama–Wasserman (N–W) orientation relationships. This was mostly attributed to the crystallographic preference associated with the phase transformation. For the austenite–ferrite interfaces with orientation relationships which are neither K–S nor N–W, both austenite and ferrite habit planes had (1 1 1) orientations. Σ3 twin boundaries comprised the majority of austenite–austenite interfaces, mostly showing a pure twist character and terminating on (1 1 1) planes due to the minimum energy configuration. The second highest populated austenite–austenite boundary was Σ9, which tended to have grain boundary planes in the tilt zone due to the geometrical constraints. Furthermore, the intervariant crystallographic plane distribution associated with the K–S orientation relationship displayed a general tendency for the austenite habit planes to terminate with the (1 1 1) orientation, mainly due to the crystallographic preference associated with the phase transformation.     

Austenite layer and precipitation in high Co–Ni maraging steel

In high Co–Ni maraging steel, austenite has a great effect on the fracture toughness of the steel and the precipitated carbides are the main strengthening phase. In this study, both austenite layers and precipitation were observed and their formation theory was analyzed by Thermo-Calc simulation and several reported results. TEM and HRTEM observation results showed that the thickness of the austenite layers was about 5–10 nm and the length of the needle-like precipitated carbides was less than 10 nm. The carbides maintained coherent or semi-coherent relation with the matrix.     

Effects of N and B on continuous cooling transformation diagrams of Mo–V–Ti micro-alloyed steels

Effects of the single addition of nitrogen (N) and boron (B) and the combined addition of N and B on continuous cooling transformation (CCT) diagrams and properties of the three Mo–V–Ti micro-alloyed steels were investigated by means of a combined method of dilatometry and metallography. Microstructures observed in continuous cooled specimens were composed of pearlite (P), quasi-polygonal ferrite (QPF), granular bainite (GB), acicular ferrite (AF), lath-like bainite (LB) and martensite (M) depending on the cooling rates and transformation temperatures. Single addition of 12?ppm B effectively reduced the formation of QPF and broadened the cooling rate region for LB and M. Added N makes the action of B invalid and the QPF region was prominently broadened, and even though the cooling rate is higher than 50°C?s^?1, it cannot obtain full bainite.     

Phase transformation behavior of the SMA490BW weathering steel

In order to optimize the heat treatment schedule and the welding procedure of the SMA490BW weathering steel, a precise determination of the continuous cooling transformation and simulated heat affected zone continuous cooling transforming diagrams were carried out. Meanwhile, the hardnesses of the specimens with different cooling rates were measured and the microstructures were observed. The microstructures are composed of pearlite, polygonal ferrite, granular structure, acicular ferrite, and lath bainite depending on the cooling rates and transformation temperature. The experiment results provide a useful guide for the heat treatment and welding of this steel.     

Modelling of austenite grain growth kinetics in a microalloyed steel (30MSV6) in the presence of carbonitride precipitates

Austenite grain growth kinetics in the presence of secondary precipitates of a microalloyed steel (30MSV6) was studied employing quantitative metallographic techniques. Austenitizing experiments were carried out at 1,000, 1,100 and 1,200?°C. According to the experimental data, abnormal grain growth behaviour is observed at 1,100?°C while it is normal at 1,000 and 1,200?°C. TEM observation represents multicomponent carbonitride precipitate, (Ti,V)(C,N), in the as-received steel with a mean radius of 35?nm. A mathematical model is proposed considering austenite grain growth along with dissolution and coarsening kinetics of the multicomponent precipitates. The austenite grain growth model for short-term non-isothermal and subsequent long-term isothermal heating stages was developed using a statistical approach. The model includes an algorithm to estimate the size distribution of austenite grains. Precipitate mean field dissolution and Lifshitz–Slyozov–Wagner coarsening models were integrated in the proposed model to calculate the pinning pressure retarding the grain boundary movement. The mean austenite grain size and the grain size distribution (normal and abnormal) calculated by the model are in good agreement with experimental data.     

Hierarchical Cu precipitation in lamellated steel after multistage heat treatment

Abstract

The hierarchical distribution of Cu-rich precipitates (CRPs) and related partitioning and segregation behaviours of solute atoms were investigated in a 1.54 Cu-3.51 Ni (wt.%) low-carbon high-strength low-alloy (HSLA) steel after multistage heat treatment by using the combination of electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and atom probe tomography (APT). Intercritical tempering at 725 °C of as-quenched lathlike martensitic structure leads to the coprecipitation of CRPs at the periphery of a carbide precipitate which is possibly in its paraequilibrium state due to distinct solute segregation at the interface. The alloyed carbide and CRPs provide constituent elements for each other and make the coprecipitation thermodynamically favourable. Meanwhile, austenite reversion occurs to form fresh secondary martensite (FSM) zone where is rich in Cu and pertinent Ni and Mn atoms, which gives rise to a different distributional morphology of CRPs with large size and high density. In addition, conventional tempering at 500 °C leads to the formation of nanoscale Cu-rich clusters in α-Fe matrix. As a consequence, three populations of CRPs are hierarchically formed around carbide precipitate, at FSM zone and in α-Fe matrix. The formation of different precipitated features can be turned by controlling diffusion pathways of related solute atoms and further to tailor mechanical properties via proper multistage heat treatments.     

Structural properties of austenitic stainless steel in the initial state and after rf plasma nitriding

Mössbauer spectroscopy, TEM, electrical resistivity and magnetic measurements are used for investigation of structural changes of X5CrNi189 austenitic stainless steel sheet induced by rf plasma nitriding carried out at 400°C for 24 h. The initial structure formed by small grains of austenite and α′-martensite changes after nitriding into expanded austenite close to the surface and austenite with minor contents of ferrite/CrN in the bulk.     

CO oxidation activity of Cu–CeO2 nano-composite catalysts prepared by laser vaporization and controlled condensation

Ceria supported copper catalysts were synthesized by laser vaporization and controlled condensation method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDAX) and temperature programmed reduction (TPR). The catalytic activity of the nanopowders for CO oxidation reaction was tested in a fixed bed flow tube reactor in Ar–20%O₂–4%CO mixture. Irrespective of the copper content, the catalytic activity of the nanopowders is similar in the initial CO test, and the catalytic activity improves (i.e. the light-off temperature decreases) during a subsequent run. The lowest light-off temperature during the second run is recorded in the material with 20% copper. TEM studies on 20%Cu–CeO₂ sample in the as-prepared condition and after CO test exhibit two types of ceria particles namely, polygonal particles 3–5 nm in size and spherical particles of 15–20 nm in size. Rapid cooling of the nanoparticles formed during the laser ablation results in incorporation of a large amount of copper within the ceria as solid solution. Presence of solid solution of copper is confirmed by EDAX and electron diffraction analyses. In addition, copper-rich surface layer of Cu₂O is found over the spherical particles. The cerium oxide components are essentially identical before and after CO test, except that the polygonal CeO₂ particles contain newly formed fine crystals of CuO. TPR results reveal two reduction peaks, which further supports, the presence of two different copper species in the material. The shift in light-off temperature during the second run is attributed to the synergistic interaction between newly formed CuO crystals with the CeO₂ matrix.     

The feasibility of Al-based oxide precipitation in Fe–10%Cr alloy by ion implantation

This paper reports the feasibility of nano-oxide precipitate formation in Fe–Cr alloy by ion implantation synthesis. High contents of Al⁺ and O⁺ ions were implanted into thin films of high purity Fe–10%Cr alloy at room temperature and were studied by transmission electron microscopy (TEM) and atom probe tomography (APT). In contrast, to the common two-stage implantation/annealing scheme of precipitate ensemble synthesis by ion beams, cluster formation took place at the implantation stage in our study, requiring no subsequent high-temperature annealing. The post-implantation microstructural examination revealed in the as-implanted thin foil an array of precipitates with diameters in the range of 3–30?nm. The precipitate number density distribution was found to depend on the foil thickness. The precipitate enrichment with both Al and O was confirmed by the energy-filtered TEM analysis. Judging from the electron diffraction pattern and high-resolution TEM analysis, the crystal lattice of precipitates corresponds to some cubic modification of aluminium-rich oxide or pure aluminium oxide. The precipitate lattice alignment with the host matrix was revealed for at least a part of precipitates. The analysis of APT data using cluster detection algorithm indicates the presence of local zones enriched in Al and O, even in those areas of as-implanted samples where no clusters were visible by TEM.     

Magnetic-field-induced microstructural features in a high carbon steel during diffusional phase transformation

In this work, a high purity, high carbon steel was heat treated without and with a 12-T magnetic field. The microstructural features induced by magnetic field during its diffusion-controlled austenite decomposition were investigated by means of optical microscopy and SEM/EBSD. It is found that the magnetic field increases the amount of the abnormal structure, which is composed of proeutectoid cementite along the prior austenite boundaries and ferrite around it, because magnetic field increases the austenite grain size and promotes the transformation of carbon-depleted austenite to ferrite. No specific orientation relationship between abnormal ferrite and cementite has been found in the non-field- or the field-treated specimens. Magnetic field evidently promotes the spheroidization of pearlite, due to its effect of enhancing carbon diffusion through raising the transformation temperature and its effect of increasing the relative ferrite/cementite interface energy. As magnetic field favors the nucleation of the high magnetization phase-pearlitic ferrite, the occurrence of the P-P2 OR that corresponds to the situation that ferrite nucleates prior to cementite during pearlitic transformation is enhanced by the magnetic field.     

Development of nitride-layer of AISI 304 austenitic stainless steel during high-temperature ammonia gas-nitriding

Ammonia-gas nitriding of AISI 304 austenitic stainless steel was studied at temperatures higher than 800 °C using SEM and X-ray diffraction. The result showed that S-phase, an expanded austenite, was formed even at such high temperatures due to a high nitriding potential of ammonia gas. The equilibrium phase, CrN was formed through a decomposition of S-layer in two different modes; the one was through continuous precipitation of particles at the surface-side of S-layer due to a higher nitriding potential; the other through a discontinuous(-like) precipitation at the austenite interface-side, producing a fine lamellar structure of austenite and CrN. The γ-phase in the surface-side resulting from the precipitation of CrN particles subsequently transformed into Fe₄N because of a fast enrichment of N atoms and a limited mobility of Cr atoms at the surface-side. A coarse lamellar structure made of austenite and Cr₂N was developed in front of fine lamellae composed of austenite and CrN by the decomposition of supersaturated austenite through a discontinuous precipitation via grain boundary movement.     

Study of diffusive transformations by high energy X-ray diffraction

High energy X-ray diffraction is a powerful tool, able to follow phase transformations during complex thermal or thermo-mechanical treatments. High energy allows one to study volumic specimens of a few mm³ and get successive data within a few seconds or less. The technique is described with different experimental setups (heating devices, detectors for diverse acquisition times) allowing diverse ranges for heating and cooling rates. Three examples are considered to illustrate the results obtained by using high energy X-ray diffraction. The first one corresponds to a simple diffusive phase transformation during an isothermal thermal path for the α–β transformation in a titanium alloy, highlighting the diffusive character considering the cell parameter evolutions of the parent phase. The second one illustrates the precipitation sequences observed during ageing of a β-metastable phase in a titanium alloy that was not obtained by TEM. The last example illustrates the phase evolutions during ageing of a martensitic steel showing the complexity of cell parameters evolution and some evolutions of the stress state.     

Multi-phase transformation kinetics of HSLA steels during continuous cooling: experiments and cellular automaton (CA) simulation

ABSTRACT

Kinetics of multiply ferrite/bainite phase transformation of HSLA steels is investigated by experiments and cellular automaton (CA) simulation. Peak-differentiation method to elucidate the sequential ferrite and bainite phase transformation individually, which is verified by the CA simulation. Such CA modelling executed using classic JMAK theory, but also gives an insight of microstructure evolution of the multi-phase transformation routine on different cooling rate. From that, it enables classic JMAK modelling to capture the detached phase transformation with different growth models and interface-migration mechanisms. Also, we find that the final phase constitution is sensitive to the cooling rate. With increasing the cooling rate, bainite sheaves nucleated at prior austenite boundaries and ferrite/austenite interfaces are significantly facilitated, which seriously inhibits the growth of prior ferrites. The scenario can be interpreted by the CA simulation and the influence of the cooling rate on sequential multi-phase transformation can be also obtained.     

马氏体时效钢的时效结构

本文利用透射电子显微相和电子衍射相对18Ni马氏体时效钢中沉淀强化相和时效结构的结晶学性质进行了研究。利用数个不同晶带的衍射相,一致地鉴别出同时存在Ni₃Mo,Ni₃Ti沉淀相和弥散的逆转变奥氏体,并且确定了它们相对马氏体基体的取向关系。证明了沉淀相、逆转变奥氏体与基体之间,密排面和密排方向都相互平行。指出在透射电子显微相中看到的魏氏型沉淀结构,实际上是由棒状沉淀相构成的三维空间格条结构,其中棒状沉淀相的长度方向平行于基体的四个〈111〉型方向。所观察到的扩张位错和位错塞积的真实性需要更多的实验证实。从结构观点,讨论了沿位错线的沉淀过程,并提出了钴钼交互作用的可能机制。