Dirk Ponge

Chemical gradients across phase boundaries between martensite and austenite in steel studied by atom probe tomography and simulation

Partitioning at phase boundaries of complex steels is important for their properties. We present atom probe tomography results across martensite/austenite interfaces in a precipitation-hardened maraging-TRIP steel (12.2 Mn, 1.9 Ni, 0.6 Mo, 1.2 Ti, 0.3 Al; at.%). The system reveals compositional changes at the phase boundaries: Mn and Ni are enriched while Ti, Al, Mo and Fe are depleted. More specific, we observe up to 27 at.% Mn in a 20 nm layer at the phase boundary. This is explained by the large difference in diffusivity between martensite and austenite. The high diffusivity in martensite leads to a Mn flux towards the retained austenite. The low diffusivity in the austenite does not allow accommodation of this flux. Consequently, the austenite grows with a Mn composition given by local equilibrium. The interpretation is based on DICTRA and mixed-mode diffusion calculations (using a finite interface mobility).

Ultrastrong steel via minimal lattice misfit and high-density nanoprecipitation

Next-generation high-performance structural materials are required for lightweight design strategies and advanced energy applications. Maraging steels, combining a martensite matrix with nanoprecipitates, are a class of high-strength materials with the potential for matching these demands. Their outstanding strength originates from semi-coherent precipitates, which unavoidably exhibit a heterogeneous distribution that creates large coherency strains, which in turn may promote crack initiation under load. Here we report a counterintuitive strategy for the design of ultrastrong steel alloys by high-density nanoprecipitation with minimal lattice misfit. We found that these highly dispersed, fully coherent precipitates (that is, the crystal lattice of the precipitates is almost the same as that of the surrounding matrix), showing very low lattice misfit with the matrix and high anti-phase boundary energy, strengthen alloys without sacrificing ductility. Such low lattice misfit (0.03 ± 0.04 per cent) decreases the nucleation barrier for precipitation, thus enabling and stabilizing nanoprecipitates with an extremely high number density (more than 1024 per cubic metre) and small size (about 2.7 ± 0.2 nanometres). The minimized elastic misfit strain around the particles does not contribute much to the dislocation interaction, which is typically needed for strength increase. Instead, our strengthening mechanism exploits the chemical ordering effect that creates backstresses (the forces opposing deformation) when precipitates are cut by dislocations. We create a class of steels, strengthened by Ni(Al,Fe) precipitates, with a strength of up to 2.2 gigapascals and good ductility (about 8.2 per cent). The chemical composition of the precipitates enables a substantial reduction in cost compared to conventional maraging steels owing to the replacement of the essential but high-cost alloying elements cobalt and titanium with inexpensive and lightweight aluminium. Strengthening of this class of steel alloy is based on minimal lattice misfit to achieve maximal precipitate dispersion and high cutting stress (the stress required for dislocations to cut through coherent precipitates and thus produce plastic deformation), and we envisage that this lattice misfit design concept may be applied to many other metallic alloys.

Linear complexions: Confined chemical and structural states at dislocations.

Welcoming steels new complexion Metals have a number of famous properties, including good strength and ductility. Controlling these properties frequently requires modifying the number and type of structural defects in a metal alloy. Kuzmina et al. produced a new type of defect, called a linear complexion, in magnesium-rich steel (see the Perspective by Kaplan). These complexions are chemically and structurally distinct regions located inside a linear defect and are isolated from the bulk by a layer of dislocations. The discovery suggests a new path for targeting defects and improving alloy development. Science, this issue p. 1080; see also p. 1059 Targeted magnesium segregation in steel allows for confined chemical and structural states inside linear defects. [Also see Perspective by Kaplan] For 5000 years, metals have been mankind’s most essential materials owing to their ductility and strength. Linear defects called dislocations carry atomic shear steps, enabling their formability. We report chemical and structural states confined at dislocations. In a body-centered cubic Fe–9 atomic percent Mn alloy, we found Mn segregation at dislocation cores during heating, followed by formation of face-centered cubic regions but no further growth. The regions are in equilibrium with the matrix and remain confined to the dislocation cores with coherent interfaces. The phenomenon resembles interface-stabilized structural states called complexions. A cubic meter of strained alloy contains up to a light year of dislocation length, suggesting that linear complexions could provide opportunities to nanostructure alloys via segregation and confined structural states.

Nanoscale austenite reversion through partitioning, segregation and kinetic freezing: Example of a ductile 2 GPa Fe–Cr–C steel

Austenite reversion during tempering of a Fe–13.6 Cr–0.44 C (wt.%) martensite results in an ultra-high-strength ferritic stainless steel with excellent ductility. The austenite reversion mechanism is coupled to the kinetic freezing of carbon during low-temperature partitioning at the interfaces between martensite and retained austenite and to carbon segregation at martensite–martensite grain boundaries. An advantage of austenite reversion is its scalability, i.e. changing tempering time and temperature tailors the desired strength–ductility profiles (e.g. tempering at 400 C for 1 min produces a 2 GPa ultimate tensile strength (UTS) and 14% elongation while 30 min at 400 C results in a UTS of � 1.75 GPa with an elongation of 23%). The austenite reversion process, carbide precipitation and carbon segregation have been characterized by X-ray diffraction, electron back-scatter diffraction, transmission electron microscopy and atom probe tomography in order to develop the structure–property relationships that control the material’s strength and ductility.

Bone-like crack resistance in hierarchical metastable nanolaminate steels

Bone-inspired steel Load cycling of metal components leads to fatigue and ultimately failure through the propagation of cracks. Koyama et al. took inspiration from bone to develop a steel with a laminated substructure that arrests cracks. The resulting hierarchical material has much better fatigue resistance properties than other iron alloys. The strategy need not be limited to steel; other metal alloys should also benefit from this type of microstructural engineering. Science, this issue p. 1055 A multiphase nanolaminate microstructured steel shows greatly improved fatigue resistance. Fatigue failures create enormous risks for all engineered structures, as well as for human lives, motivating large safety factors in design and, thus, inefficient use of resources. Inspired by the excellent fracture toughness of bone, we explored the fatigue resistance in metastability-assisted multiphase steels. We show here that when steel microstructures are hierarchical and laminated, similar to the substructure of bone, superior crack resistance can be realized. Our results reveal that tuning the interface structure, distribution, and phase stability to simultaneously activate multiple micromechanisms that resist crack propagation is key for the observed leap in mechanical response. The exceptional properties enabled by this strategy provide guidance for all fatigue-resistant alloy design efforts.

Enhancing Hydrogen Embrittlement Resistance of Lath Martensite by Introducing Nano-Films of Interlath Austenite

Partial reversion of interlath austenite nano-films is investigated as a potential remedy for hydrogen embrittlement susceptibility of martensitic steels. We conducted uniaxial tensile tests on hydrogen-free and pre-charged medium-Mn transformation-induced plasticity-maraging steels with different austenite film thicknesses. Mechanisms of crack propagation and microstructure interaction are quantitatively analyzed using electron channelling contrast imaging and electron backscatter diffraction, revealing a promising strategy to utilize austenite reversion for hydrogen-resistant martensitic steel design.

Pulsed-laser atom probe studies of a precipitation hardened maraging TRIP steel

A precipitation hardened maraging TRIP steel was analyzed using a pulsed laser atom probe. The laser pulse energy was varied from 0.3 to 1.9 nJ to study its effect on the measured chemical compositions and spatial resolution. Compositional analyses using proximity histograms did not show any significant variations in the average matrix and precipitate compositions. The only remarkable change in the atom probe data was a decrease in the ++/+ charge state ratios of the elements. The values of the evaporation field used for the reconstructions exhibit a linear dependence on the laser pulse energy. The adjustment of the evaporation fields used in the reconstructions for different laser pulse energies was based on the correlation of the obtained cluster shapes to the TEM observations. No influence of laser pulse energy on chemical composition of the precipitates and on the chemical sharpness of their interfaces was detected.

Grain boundary characterization and grain size measurement in an ultrafine-grained steel

Abstract Ultrafine ferrite grains in a plain C–Mn steel (0.3 mass% C) were produced by large-strain warm compression and subsequent annealing treatment in a temperature range between 773 K and 1003 K. The samples were investigated by means of high-resolution electron back-scatter diffraction. The resulting microstructures showed very fine ferrite grains and homogeneously distributed cementite particles. The majority of the grain boundaries (55–70 %) were classified as high-angle ones (≥ 15° misorientation). When considering only these high-angle grain boundaries, the average grain size changed from 0.9 mm at a deformation temperature of 773 K to 2.2 mm at a deformation temperature of 1003 K. For the same range the average subgrain sizes increased from 0.6 mm to 1.5 mm. The basic result of this study is that the grain size characterization of polycrystalline microstructures with ultrafine grains requires the use of the high-resolution electron back-scatter diffraction method in conjunction with a careful a...

Atomic scale investigation of non-equilibrium segregation of boron in a quenched Mo-free martensitic steel

B-added low carbon steels exhibit excellent hardenability. The reason has been frequently attributed to B segregation at prior austenite grain boundaries, which prevents the austenite to ferrite transformation and favors the formation of martensite. The segregation behavior of B at prior austenite grain boundaries is strongly influenced by processing conditions such as austenitization temperatures and cooling rates and by alloying elements such as Mo, Cr, and Nb. Here an local electrode atom probe was employed to investigate the segregation behavior of B and other alloying elements (C, Mn, Si, and Cr) in a Cr-added Mo-free martensitic steel. Similar to our previous results on a Mo-added steel, we found that in both steels B is segregated at prior austenite grain boundaries with similar excess values, whereas B is neither detected in the martensitic matrix nor at martensite-martensite boundaries at the given cooling rate of 30K/s. These results are in agreement with the literature reporting that Cr has the same effect on hardenability of steels as Mo in the case of high cooling rates. The absence of B at martensite-martensite boundaries suggests that B segregates to prior austenite grain boundaries via a non-equilibrium mechanism. Segregation of C at all boundaries such as prior austenite grain boundaries and martensite-martensite boundaries may occur by an equilibrium mechanism.

Recrystallization during Annealing of a Cold Rolled Lean Duplex Stainless Steel

Duplex stainless steels (DSSs) are based on the Fe-Cr-Ni system and formed by ferrite (30-70%) and austenite. They have high tensile strength, good toughness and weldability and excellent corrosion resistance including stress-corrosion cracking and resistance to localized corrosion. The increase of the raw materials of the last years, there has been a motivation to develop new stainless steels with lower contents of nickel and molybdenum. Lean duplex stainless steels (LDSSs) are almost Mo free and nickel content lower than 4%. The lean duplex grades are expected to substitute not only 304/316 grades but also other duplex stainless steel grades. LDSSs are used for structural applications and for the less corrosion conditions such as liquor tanks and suction rolls. The aim of the present work was to study the kinetics of recovery and recrystallization of the lean duplex stainless steel 1.4362 during annealing treatment. The material was subjected to hot rolling and cold rolling of 70%, annealing treatment for different times at temperatures from 1000 to 1100°C and subsequently water quenched. Optical microscopy and electron back scattering diffraction (EBSD) were employed to study the evolution of the microstructure during the annealing treatment. After cold rolling austenite exhibited more strain hardening than ferrite. Consequently, the driving force of the austenite for recrystallization is higher. During annealing, recovery took place in ferrite, while the austenite remained nearly unrecovered until beginning of recrystallization. The layered grain morphology produced during cold rolling remained after the annealing treatment. The volume fraction of the phases did not show significant changes with the annealing time. Nevertheless, the volume fraction of austenite decline with an increasing of annealing temperature. After 60 seconds at 1100°C, annealing primary recrystallization had progressed in both phases, which show a bamboo-structure where the grain boundaries ran perpendicular to the phase boundaries. Grain growth progressed for longer annealing times. After 600 seconds, the bamboo-structure started to change for a more globular grain structure, pearl-structure. It continued and became more pronounced at longer annealing times. At lower temperatures, the recrystallization behavior is similar; however, the structure was refined. Recovery is favored by the high stacking fault energy of ferrite and the layered grain morphology. The lean duplex stainless steel 1.4362 shows a similar recrystallization kinetics compare with standard duplex stainless steels.