Microstructure mapping of a friction stir welded AA2050 Al–Li–Cu in the T8 state

The heterogeneous precipitate microstructure of a AA2050 Al–Li–Cu in the T8 state after friction stir welding has been mapped by small-angle X-ray scattering (SAXS). 2D resolved maps of the fraction and size of both T₁ platelets precipitates and clusters/GP zones formed at room temperature are provided. TEM micrographs of selected zone confirm the interpretation of SAXS intensities. This microstructure mapping is compared to microhardness mapping and a direct correlation is shown. Short duration heat treatments made in a salt bath help understanding precipitate stability and suggest that the temperature exploration alone explains to a large extent the distribution of the precipitates microstructure across the welded structure.     

Discrete dislocation simulations of precipitation hardening in superalloys

The low-temperature yield stress of a nickel-based superalloy, containing up to 40% Ni₃A1 precipitates (γ′), is calculated by discrete dislocation simulations. A pair of screw or 60°(a/2) ?110? dislocation glides under external stress across a {111} plane of γ phase, intersected by a random distribution of either spherical or cubic γ′ precipitates. The stress is raised until the dislocations can cut or bow round all the obstacles. In this paper the emphasis is on the cutting regime which is prevalent when the precipitates are small and/or have low antiphase-boundary (APB) energies. From a large number of simulations in the cutting regime, the effects of size, shape, volume fraction and APB energy are found to be as follows: The yield stress is proportional to the square root of the volume fraction of γ′. The yield stress depends weakly on the precipitate size in the size range 20–400?nm, for APB energies of 150, 250 and 320?mJ?m^?2. The yield stress depends linearly on the APB energy for APB energies up to 320?mJ?m^?2 in the size range 50–200?nm. At a precipitate size of 100?nm, cubes are weaker obstacles than equivalent spheres by about 25% for an APB energy of 320?mJ?m^?2; however, the shape effect on strengthening decreases with decreasing APB energy and decreasing precipitate size. When a coherency stress (from a lattice parameter mismatch of 0.3%) is added, the yield stress increases by about 10%. When solid-solution strenthening is added, it is potent when the solute is in the γ matrix, but much less potent when the solute is in γ′. When the γ′ precipitates are larger than 400?nm across and the APB energy greater than 250?mJ?m^?2, significant Orowan looping occurs. The yield stress drops inversely as the precipitate size and becomes insensitive to the APB energy but sensitive to the shear modulus. Many of these results from the full simulations differ from the analytical models of strengthening in superalloys but they can be rationalized from the results of simulations on simple homogenized precipitate structures.     

Combining TEM and APFIM techniques to study the microstructure of steels and hardmetals

This paper describes the benefits of combining transmission electron microscopy (TEM) and atom probe field ion microscopy (APFIM) techniques to study the microstructure of steels and hardmetals. In addition to energy dispersive X-ray spectrometry (EDS), recent experience of electron energy loss spectroscopy (EELS) and energy filtered TEM (EFTEM) is treated. Topics covered are: phase composition (APFIM, TEM/EDS and TEM/EELS); precipitate size distribution (EFTEM); precipitate volume fraction (APFIM); and compositional gradients (APFIM, EFTEM and SEM). Examples given include precipitate composition and size distribution in creep resistant 9–12% chromium steels, phase distribution and composition in nitrogen containing hardmetals (cermets) after sintering and heat treatment, and boron grain boundary segregation in austenitic stainless steels.     

Deformation of a nanocube with a single incoherent precipitate: role of precipitate size and dislocation looping

ABSTRACT

Precipitate hardening is a key strengthening mechanism in metallic alloys. Classical models for precipitate hardening are based on the average behaviour of an ensemble of precipitates, and fail to capture the complexity of dislocation-precipitate interactions that have recently been observed at individual precipitates in simulations and in-situ electron microscopy. In order to achieve tailored mechanical properties, detailed deformation mechanisms at specific precipitates that account for precipitate size, crystallography, and defect structure must be understood, but has been challenging to achieve experimentally. Here, in-situ scanning electron microscope mechanical testing is used to obtain the compressive stress–strain behaviour at an individual, incoherent Au precipitate within a Cu nanocube, and determine the influence of precipitate and cube size on yield strength and strain hardening. TEM imaging and strain mapping of the initial structure shows misfit dislocations at the Au precipitate, threading dislocations that traverse the Cu shell, and localised and anisotropic strain near the precipitate and threading dislocation. These nanocubes have yield strengths of 800–1000?MPa and strain hardening rate of 1–4?GPa. Yield strength is found to depend on the distance from the precipitate interface to the cube edge, while strain hardening depends on both cube size and precipitate size. An analytical model is developed to quantify the contribution of Orowan looping, Orowan stress, back stress and image stress to plasticity at the Au precipitate. Orowan stress is found to be the largest contributor, followed by back stress and image stress.     

Quantitative description of the T1 formation kinetics in an Al–Cu–Li alloy using differential scanning calorimetry,small-angle X-ray scattering and transmission electron microscopy

The object of the present study is to design a methodology to follow the kinetics of T₁ precipitation, in an AA2198 alloy, in terms of precipitate size, morphology (thickness, diameter) and volume fraction, during a two-temperature isothermal heat treatment. We used in situ small-angle X-ray scattering (SAXS) as a way to measure the evolution of the T₁ mean thickness and diameter during the heat treatment. Transmission electron microscopy (TEM) was then performed in order to calibrate these evolutions. Furthermore, we demonstrate that the volume fraction evolution can be described successfully using a simple analysis of the differential scanning calorimetry (DSC) thermograms. The latter was calibrated by selected observations in high angular annular dark field scanning transmission electron microscopy (HAADF-STEM). Microstructure evolution during DSC heating ramps was analysed using in situ SAXS: the T₁ phase transformation is found to consist in a two-step thickening process explained by two consecutive diffusion stages. The enthalpy of formation of the T₁ phase is deduced from the DSC measurements.     

Effects of internal stresses and intermediate phases on the coarsening of coherent precipitates: A phase-field study

Phase stability, topology and size evolution of precipitates are important factors in determining the mechanical properties of crystalline materials. In this article, the Cahn-Hilliard type of phase-field model was coupled to elasticity equations within a mixed-order Galerkin finite element framework to study the coarsening morphology of coherent precipitates. The effects of capillarity, particle size and fraction, compositional strain, and inhomogeneous elasticity on the kinetics and kinematics of coherent precipitates in a binary dual phase crystal admitting a third intermediate stable/meta-stable phase were investigated. The results demonstrated the ability of the model to simulate coarsening under the concomitant action of Ostwald ripening and mismatch elastic strain mechanisms. Using a phenomenological coarsening power law, coarsening rates were determined to depend on precipitate size and volume fraction, compositional strain, and strain mismatch between precipitates and the matrix. Results also showed that the necking incubation time between two neighboring precipitates depends inversely on the precipitate’s initial sizes; however, under fixed volume fraction of precipitates, any increase in the initial sizes of the precipitates mitigates the coarsening. Meanwhile, the compositional strain and the growth of the intermediate stable/meta-stable phase leads to substantial enhancements of precipitate coarsening.     

Effect of nitriding time on secondary recrystallization behaviors and magnetic properties of grain-oriented electrical steel

The effect on secondary recrystallization behaviors and magnetic properties of grain-oriented electrical steel of nitriding time from 0 to 240 s in the acquired-inhibitor method has been studied. It was found that the volume fraction of nitride precipitates increased with increasing nitriding time. However, the average diameter of the nitride precipitates decreased with increasing nitriding time. Two kinds of nitride precipitates were found to have formed after primary recrystallization annealing. A fine rod-shaped precipitate was found to be Si₃N₄ and and a coarse, lozenge-shaped precipitate was MnSiN₂. Moreover, primary grain size decreased with increasing nitriding time due to retarding of the grain growth by precipitates. After secondary recrystallization annealing, the specimen that was nitrided for 30 s obtained the largest volume fraction of abnormal growth grains and largest area percentage of Goss grains. Conversely, specimens that were nitrided more or less than 30 s demonstrated poor secondary recrystallization and obtained low area percentage of Goss grains. Furthermore, the optimum nitriding time to obtain the best magnetic properties was 30 s. In addition, the optimum nitrogen content was 150 ppm.     

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.     

Three-dimensional size and orientation of the precipitates in AZ91 magnesium alloys measured by TEM techniques

Knowledge of the microscopic structure, including three-dimensional (3-D) size and orientation of the precipitates, is essential to fully understand the mechanical properties of the magnesium alloys and designing the alloys with better performance. Analytical TEM with high spatial resolution offers the simultaneous measurements of 3-D size, structure, orientation, composition of the precipitates from one typical sample along an established crystallographic axis. Besides popular Burgers orientation relationship (OR), other ORs such as Pitsch--Schrader OR, Crawley OR, Potter OR and a new OR with the form of [0001]_α 1.0° from [311]_γ and (11\bar 20)_α 2.0° from (03\bar 3)_γ between the magnesium matrix and the precipitate γ -Mg₁₇Al₁₂ are identified by TEM imaging and diffraction techniques. As a case study, the thicknesses of the individual precipitates with Burgers OR are further measured to be 100--200~nm through both electron energy-loss spectroscopy and x-ray energy dispersive spectroscopy combining differential x-ray absorption and extrapolation, which are in agreement with the overall 3-D size statistic distribution results obtained through analysing various samples along various directions. Furthermore, the fabricated wedge-shape structure provides a platform on which to study the dependence of the interfacial strain on the variation of the thickness.     

Quantitative analysis of fine nano-sized precipitates in low-carbon steels by small angle neutron scattering

The small angle neutron scattering (SANS) technique was used to determine the nano-sized precipitates in interstitial free (IF) and low-carbon (LC) steels with a hot-rolling temperature. The real-space direct model fitting method was applied to quantitatively analyze the SANS data. The magnetic and chemical properties of precipitates in the samples were also investigated by separation and comparison of nuclear and magnetic SANS scattering data. The size distribution of precipitates in the IF steel is in good agreement with the microstructure observation using transmission electron microscopy. The results revealed that the IF steel had two types of non-magnetic precipitates, Ti₄C₂S₂ and TiC, with the average size of about 30 nm in diameter and little difference in chemical composition. In case of commercial LC steel, the fine and large precipitates are identified as MnS and Fe₃C, respectively. The average size of spherical MnS precipitates was about 4.8 nm in radius and the distribution is isotropic. It is likely that the LC steels have almost the same composition and a similar size as precipitates such as MnS and Fe₃C with different finishing delivery temperatures. Interestingly, the average size and volume fraction of fine precipitates showed no significantly changes under the different finishing delivery temperatures.     

Transmission electron microscopy and X-ray diffraction study of microstructural evolution in magnetoresistive Cu–Fe–Ni ribbons

The evolution of the microstructure of a granular Cu₈₀Fe₁₀Ni₁₀ (at%) melt-spun ribbon is studied by transmission electron microscopy (TEM), energy-filtered transmission electron microscopy (EFTEM) and X-ray diffraction. This system is interesting as large giant magnetoresistance (GMR) values have been measured for this composition. We have shown the presence of two face-centred cubic phases, an (Fe,Ni)-rich phase and a Cu-rich phase. The lattice parameters of these two phases are close and no diffraction or elastic contrast is involved in displaying the two phases in TEM bright-field mode. With EFTEM imaging, we have shown the presence of a fine-scale (Fe,Ni)-rich precipitation inside the Cu-rich fcc matrix. The precipitates are 2–4 nm in the as-spun state and 4–6 nm after annealing for 2 h at 400°C. The lattice parameter of the Cu-rich phase in the as-spun sample is 0.3608 nm and 0.3610 nm for the (Fe,Ni)-rich phase. After a 24-h annealing treatment at 600°C, the mean diameter of the particle is 20 nm and the lattice parameter of the (Fe,Ni)-rich phase has decreased to 0.3600 nm, while that of the Cu-rich phase has increased to 0.3613 nm, which is consistent with a segregation of Fe and Ni in the precipitates. The composition and volume fraction of the two phases measured for this annealed sample are in good agreement with the Thermocalc® predictions.     

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.     

Nanocrystallisation of an Fe44.5Co44.5Zr7B4 amorphous magnetic alloy

The crystallisation of amorphous Fe_44.5Co_44.5Zr₇B₄ was investigated using DSC, electrical resistivity, TEM, HRTEM, CBED and VSM. Melt-spun amorphous Fe_44.5Co_44.5Zr₇B₄ crystallised by the primary crystallisation mode: the DSC results showed two exothermal peaks during heating. The electrical resistivity dropped sharply during the crystallisation event, which was consistent with DSC characterisation. From TEM, HRTEM and CBED results, primary crystallisation products which appeared to be clusters of crystals were found to be single crystal precipitates; these crystals formed in a compact dendritic morphology. Direct measurement of nucleation density and volume fraction was carried out using TEM analysis. The nucleation density was found to be high even in the absence of copper addition. The crystal growth was slow when the average size reached around 30?nm; this resulted in a stable nanocrystalline structure. The soft magnetic properties were improved after nanocrystallisation, the magnetic properties were related to the crystalline volume fraction and the Herzer model.     

A new TEM method for the characterization of the tertiary γ′ nano-precipitates in a PM disk superalloy: influence of ageing

An original method for characterizing the γ′-phase tertiary precipitates in a Ni-based superalloy manufactured by powder metallurgy is described. This investigation is made using post mortem transmission electron microscopy (TEM). It is based on the analysis of sheared areas within crept specimens, which allows the precipitates revealed by the dislocations in their glide plane to be observed. The characteristics of these nano-precipitates, i.e. their size, their volume fraction and the channel width between them, are determined for two different heat treatments (HTs). The results show a wide distribution of the microstructural parameters for a given HT, but only slight differences between the microstructures produced by the two different HTs. This microstructural information allows a better understanding of the wide variety of the deformation micromechanisms observed during creep at high temperature.     

Precipitate characterisation in metallic systems by small-angle X-ray or neutron scattering

Small-angle scattering enables the extraction of precise, quantitative information about nano-scale precipitate microstructures. It can be used with X-rays (SAXS) or neutrons (SANS). This paper presents simple methods for extracting information on the precipitate size and volume fraction from SAS spectra. The various possibilities for obtaining precipitate size are reviewed, and the meaning of their differences is discussed. Examples of applications for complex precipitate microstructure measurements are given in the following areas: kinetic in-situ measurements in Fe–Cu and Fe–Nb–C alloys, non-stoichiometric precipitation in an Al–Zn–Mg–Cu alloy studied by anomalous SAXS (ASAXS), and precipitation mapping in weld cross-sections.     

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.     

SiOx precipitate composition in Si,revisited: Discussion closed?

The composition SiO_x of oxide precipitates in Si has been discussed for the past thirty years with experimentally estimated x ‐values ranging between 1 and 2. It is shown that this spread of x ‐values can be explained by calculating the average composition taking into account temperature and anneal time dependent size and shape of the precipitates and the limitations and probing volumes of the various characterization techniques. Hereby it is assumed that the oxygen‐rich (SiO₂?) core of the precipitates is surrounded by a 2 nm thin SiO layer as revealed by recent electron energy loss spectroscopy analyses. For plate‐like precipitates thinner than and for octahedral precipitates smaller than 6 nm, x ≈ 1. For larger precipitates, the central part of the precipitate consists of SiO_x with x close to 2 and the precipitate has an average x between 1 and 1.3 for plate‐like and up to 1.9 for octahedral precipitates. The predicted x ‐values for different precipitate sizes and morphologies, are compared with published experimental data. SiO_x precipitate nucleation and initial growth should be simulated assuming x = 1 and Fourier transform infrared spectra of precipitates assuming a mixture of SiO₂ and amorphous Si. (© 2015 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)     

A study on the early-stage decomposition in the Al–Mg–Si–Cu alloy AA6111 by electrical resistivity and three-dimensional atom probe

Electrical resistivity measurements and three-dimensional atom probe (3DAP) analysis were employed to investigate early-stage decomposition of the Al alloy AA6111 in the temperature range 60–180°C where electrical resistivity initially increased with ageing time. 3DAP measurements provided information on the shape, number density and solute content of the precipitates, as well as the solute concentration of the matrix, for the ageing conditions corresponding to the resistivity maxima. Using the 3DAP results, the precipitate size distributions for these ageing conditions were determined in terms of the measured number of solute atoms per precipitate. The number density and the Cu content of the precipitates decreased with increasing temperature, whereas the Mg/Si ratio increased. The size distribution of precipitates at the higher ageing temperatures showed the addition of larger size precipitates to the precipitate population. A modification to Matthiessen's law was employed to describe the anomalous resistivity increase by considering the effect of solutes and precipitates on the resistivity evolution. Using the 3DAP results in analysing the resistivity anomaly, it was found that the decrease in the resistivity maxima with increasing temperature was associated with the decrease in the number density of precipitates and not the scattering power of precipitates. The 3DAP results were further used to provide information on the mechanisms of early-stage decomposition and the temperature dependence of the nucleation rate. From this, the nucleation rate appeared to be controlled by the migration of solute atoms, which was assisted by quenched-in vacancies.     

Dislocation structure of plastic relaxation waves in polycrystals and alloys under intense shock wave loading

The influence of the structure factors (sizes of grains and precipitates) on the dislocation structure formed in polycrystals and alloys behind the shock wave front (elastic precursor) has been theoretically discussed in terms of the dislocation kinetic relationships and kinetic equation for the dislocation density. The critical conditions of the transition from the cellular dislocation structure to a uniform dislocation distribution have been formulated. These conditions are used to determine the dependences of the critical pressure, above which the dislocation distribution becomes uniform, on the grain size and precipitate volume density.     

High-resolution transmission electron microscopy and tomographic atom probe studies of the hardening precipitation in an Al–Cu–Mg alloy

The hardening precipitation of an Al–Cu–Mg aluminium alloy designed for aeronautics was investigated using high-resolution transmission electron microscopy (HREM) and tomographic atom probe techniques. The observed precipitates clearly belong either to the Guinier–Preston–Bagaryatskii (GPB) zones type or to the so-called S-Al₂CuMg precipitation. We analysed a large number of precipitates in order to obtain statistical information on the precipitation. We focused on the structural and/or chemical composition of the different precipitates. It was found, in particular, that the very numerous GPB zones do not present a single chemical composition. Evidence is also given for the presence of two different kinds of S-precipitate/matrix orientation relationships, strongly linked to the morphology of the precipitate. The structure of the S precipitates was confirmed by direct comparison with simulated HREM images. Particular attention was paid to the nature of the S-precipitate/matrix interfaces.