Hydrogen-assisted damage in austenite/martensite dual-phase steel

For understanding the underlying hydrogen embrittlement mechanism in transformation-induced plasticity steels, the process of damage evolution in a model austenite/martensite dual-phase microstructure following hydrogenation was investigated through multi-scale electron channelling contrast imaging and in situ optical microscopy. Localized diffusible hydrogen in martensite causes cracking through two mechanisms: (1) interaction between {1?1?0}_M localized slip and {1?1?2}_M twin and (2) cracking of martensite–martensite grain interfaces. The former resulted in nanovoids along the {1?1?2}_M twin. The coalescence of the nanovoids generated plate-like microvoids. The latter caused shear localization on the specific plane where the crack along the martensite/martensite boundary exists, which led to additional martensite/martensite boundary cracking.     

Evolution of a sharp {110} texture in microcrystalline Fe78Si9B13 during magnetic crystallization from the amorphous phase

The effect of magnetic crystallization on texture evolution and control in nanocrystalline materials has been studied using a melt-spun amorphous Fe₇₈Si₉B₁₃ alloy. The magnetic crystallization was conducted at temperatures ranging from 653 to 853?K in a magnetic field up to 6?T. The temperatures used for magnetic crystallization were chosen on the basis of the Curie and crystallization temperatures of the amorphous phase, and the Curie temperature of the crystallized phase. The resultant microstructure was characterized by X-ray diffraction and FE-SEM/EBSP/OIM techniques. It was found that a sharp {110} texture developed when the amorphous precursor was crystallized at 853?K in a magnetic field of 6?T applied in a direction parallel to the ribbon surface.     

Effect of heat treatment on the NO2-sensing properties of sputter-deposited indium tin oxide thin films

Transparent conducting indium tin oxide (ITO) films were deposited onto glass substrates by radio-frequency magnetron sputtering at 648?K, under an oxygen partial pressure of 1?Pa. The effect of annealing on the electrical properties of the films was studied. Characterization of the coatings revealed an electrical resistivity below 6.5?×?10^??3?Ω?cm. The ITO films deposited at 648?K were amorphous, while the crystallinity improved after annealing at 700?K. The surface morphology examined by scanning electron microscopy appears to be uniform over the entire surface area after annealing. The NO₂-sensing properties of the ITO films were investigated and showed sensitivity at concentrations lower than 50?ppm, at a working temperature of 600?K.     

Effect of cooling rate on size-dependent atomic ordering of CoPt nanoparticles

We report on the effect of cooling rate on the size-dependent atomic ordering of CoPt nanoparticles using aberration corrected high-resolution transmission electron microscopy. It was found that cooling rate plays a crucial role in promoting atomic ordering during the cooling process after annealing. Nanoparticles of ≈3?nm in diameter show the A1-disordered phase after annealing at 873?K for 1?h followed by rapid cooling (110?K/min), while the L1₀-ordered phase is obtained when the cooling rate is slow (1.5?K/min). The disordered phase is also obtained by rapid cooling after annealing at 973?K for 1?h. These results unambiguously indicate that the order–disorder transformation temperature is reduced to a temperature at least lower than 873?K for CoPt nanoparticles smaller than 3?nm in diameter. The slow cooling process promotes the atomic ordering, which resulted in an enhancement of magnetic coercivity as high as 2200?Oe. This study demonstrates that hard magnetic properties of the CoPt nanoparticles can be improved by controlling the cooling rate after heat treatments.     

Influence of interface migration during annealing of martensite/austenite mixtures

Tempering of martensite in the absence of carbide precipitation leads to carbon partitioning into retained austenite. If the martensite/austenite interface is assumed to remain stationary during this process, the phase compositions reach a condition that has recently been called constrained carbon equilibrium. If iron atoms are sufficiently mobile at the interface, longer partitioning times may lead to migration of the ferrite/austenite interface. The interface may be expected to move in either direction, depending on the specific details of the phase fractions and compositions controlling the chemical potential of iron at the interface. If interface migration occurs during carbon partitioning, the situation is more complicated and conditions could exist where the interface moves first in one direction and then the other.     

Giant electrocaloric effect of highly (1 0 0)-oriented 0.68PbMg1/3Nb2/3O3–0.32PbTiO3 thin film

PbZr_0.95Ti_0.05O₃ thin film has the highest electrocaloric properties of all the oxide thin films (0.48?K?V^?1). Here, it is shown giant electrocaloric properties in 200?nm (1?0?0)-oriented PMN–PT 68/32 film near the ferroelectric Curie temperature of 146?°C. The results indicate the significance of this system to achieve electrocaloric entropy change and temperature change, up to 32.21?J/kg?°C and 14?K, respectively, in 12?V (i.e. 1.155?K?V^?1) near the Curie point. This exceeds the previous best results obtained in PbZr_0.95Ti_0.05O₃ thin film.     

After-effects induced by interactions between hydrogen and the martensite transformation in Ni–Ti superelastic alloy

The effects of dynamic interactions between hydrogen and a stress-induced martensite transformation on the recovery of deteriorated tensile properties by ageing in air at room temperature have been investigated for a Ni–Ti superelastic alloy. A specimen is subjected to single stress-induced martensite and reverse transformations immediately after hydrogen charging. Upon tensile testing, brittle fracture occurs in the latter half of the elastic deformation region of the martensite phase after the stress-induced martensite transformation. Upon ageing before the tensile test, fracture occurs during the stress-induced martensite transformation. In addition, the nano- and micro-morphologies of the brittle outer part of the fracture surface of the specimen are changed by ageing. Thus, the tensile properties markedly deteriorate, rather than recover, by ageing. The present results clearly indicate that dynamic interactions between hydrogen and the stress-induced martensite transformation have serious after-effects on hydrogen embrittlement of Ni–Ti superelastic alloy.     

Recrystallization of amorphous ion-implanted silicon carbide after thermal annealing

Single crystals of 6H–SiC were implanted at room temperature with 4-MeV Au ions to a fluence of 10^15?cm^?2. Raman spectra showed that full amorphization was achieved. The recrystallization process was studied by micro-Raman spectrometry after isochronal thermal annealing between 700 and 1500°C. The spectra permitted the evolution upon annealing of Si–C bonds, and also of Si–Si and C–C bonds, to be followed. Amorphous phase relaxation takes place below 700°C; then recrystallization of the 6H polytype sets in at 700°C. At 900°C crystallites with different crystalline states are formed. Moreover, Raman spectra provide evidence of graphitic nanocluster formation at 1500°C.     

Microstructures and tensile properties of 304 steel with dual nanocrystalline and microcrystalline austenite content prepared by aluminothermic reaction casting

The microstructures of 304 stainless steels with different amounts of nanocrystalline and microcrystalline austenite prepared by an aluminothermic reaction casting, without and with annealing at 1073?K for 8?h, have been investigated by X-ray diffraction, an electron probe micro-analyser, a transmission electron microscope and a scanning electron microscope. The steels, both without and with annealing, consisted of different dual nanocrystalline and microcrystalline austenite combinations and a little nanocrystalline δ ferrite, while the average grain size of the nanocrystalline austenite increased from 19 to 26?nm and volume fraction of the microcrystalline austenite increased from 17 to 30% after annealing. The tensile strength of the steel was dramatically increased from 500 to 1000?MPa and the tensile elongation ratio increased from 8 to 12% after annealing. However, the tensile strength was decreased to 600?MPa and the tensile elongation ratio increased from 12 to 22% after an annealing at 1273?K. The combination of dual nanocrystalline and microcrystalline austenite obtained after the annealing at 1073?K results in the best tensile properties.     

Recrystallization in a low-density low-alloy Fe–Mn–Al–C duplex-phase alloy

The recrystallization behaviour of a cold-rolled, low-density, low-alloy duplex-phase alloy (Fe–6.57Al–3.34Mn–0.18C, wt.%) has been studied. Temperature-resolved X-ray diffraction and dilatometry showed that the alloy recrystallizes at 850?°C during continuous heating. However, electron back-scattered diffraction investigations using Kernel average misorientation revealed that during annealing ferrite recrystallizes at lower temperatures while austenite remains strained up to 1200?°C. This study underlines the complexity of recrystallization of a microstructure comprising of constituents with high and low stacking fault energy.     

Effect of crystallization on the surface area of porous Ni-based metallic glass foams

The change of the specific surface area in porous Ni₅₉Zr₂₀Ti₁₆Si₂Sn₃ metallic glass (MG) upon partial crystallization was investigated. The observed increase in the surface area of the annealed Ni-based MG foams is due to the formation of homogeneously distributed Ni₁₀(Zr,Ti)₇ rod-shape intermetallic phases with nominal diameters around 250?nm and ～800?nm length on the surface of MG struts during the crystallization. For longer annealing, the specific surface area decreases again due to a change of the morphology of the crystals from rod-like to disc-like appearance, thus suggesting an optimum regime for increasing the specific surface area upon isothermal annealing at a given temperature.     

Thermomagnetic study of devitrification in Fe-Si-B-Cu-Nb(-X) alloys

Thermomagnetic measurements have been used to study the magnetic and structural changes occurring at the two steps of the crystallization process of Fe_73.5Si_13.5B₉Cu₁Nb₁X₂ (X = Zr, Nb, Mo and V) alloys. Alloying raises the thermal stability of the amorphous phase against nanocrystallization in the order V < Mo < Nb < Zr and some differences in the final crystalline phases are found. The Curie temperature of the amorphous phase increases (about 15K) during structural relaxation. In the course of nanocrystallization a further increase of about 30K in the Curie temperature of the amorphous intergranular is observed for samples with X = Zr, Nb and Mo, but only of about 15K for samples containing V. The observed increase in the Curie temperature of the Fe-Si phase between the end of the first crystallization process and the end of the second crystallization process is associated with a reduction in the Si content, in agreement with X-ray diffraction results.     

Application of the stagnant stage concept for monitoring Mn partitioning at the austenite-ferrite interface in the intercritical region for Fe–Mn–C alloys

The length of the stagnant stage during the new ferrite growth starting from a mixture of austenite and ferrite has been investigated for a Fe-0.17Mn-0.023C (wt%) alloy. It was found that the stagnant stage depends on the thermal path followed to create the mixture, and deduce that the tie-lines for austenite to ferrite transformation are quite different from those for ferrite to austenite transformation. The length of the stagnant stage is determined by the very local partitioning effect at the interface, and it can be used as a tool to monitor the Mn partitioning.     

A study of thermal vacancies and dislocation structure in Fe–40 at.% Al

The densities of thermal vacancies and residual dislocations in bulk specimens of Fe–40?at.%?Al have been investigated using differential dilatometry and X-ray diffraction. A large quenched-in vacancy concentration at temperatures above about 873?K was apparent from the decrease in average lattice parameter. This was correlated to a lowering of the effective enthalpy of vacancy formation from about 91 to 42?kJ mol^?1, possibly caused by the presence of different types of point defect in lower- and higher- temperature regimes. The residual dislocations were found to have a major concentration on {100} planes at any given temperature. An increase in the dislocation density and a concurrent fall in the vacancy concentration was observed with a lowering of the quenching temperature from 1223 to 1073?K, indicating the possibility of vacancy annihilation at 1073?K.     

First interactions between hydrogen and stress-induced reverse transformation of Ni–Ti superelastic alloy

The first dynamic interactions between hydrogen and the stress-induced reverse transformation have been investigated by performing an unloading test on a Ni–Ti superelastic alloy subjected to hydrogen charging under a constant applied strain in the elastic deformation region of the martensite phase. Upon unloading the specimen, charged with a small amount of hydrogen, no change in the behaviour of the stress-induced reverse transformation is observed in the stress-strain curve, although the behaviour of the stress-induced martensite transformation changes. With increasing amount of hydrogen charging, the critical stress for the reverse transformation markedly decreases. Eventually, for a larger amount of hydrogen charging, the reverse transformation does not occur, i.e. there is no recovery of the superelastic strain. The residual martensite phase on the side surface of the unloaded specimen is confirmed by X-ray diffraction. Upon training before the unloading test, the properties of the reverse transformation slightly recover after ageing in air at room temperature. The present study indicates that to change the behaviour of the reverse transformation a larger amount of hydrogen than that for the martensite transformation is necessary. In addition, it is likely that a substantial amount of hydrogen in solid solution more strongly suppresses the reverse transformation than hydrogen trapped at defects, thereby stabilising the martensite phase.     

Nucleation of He bubbles in amorphous FeBSi alloy irradiated with He ions

It is interesting to investigate the formation of He bubbles in amorphous alloys because point defects do not exist in amorphous materials. In the present study, the microstructural evolution of amorphous Fe₇₉B₁₆Si₅ alloy, either irradiated with 5?keV He⁺ ions or implanted with 150?eV He⁺ ions without causing displacement damage, and then annealed at a high temperature, was investigated using transmission electron microscopy (TEM). Vacancy-type defects were formed in the amorphous alloy after irradiation with 5?keV He⁺ ions, and He bubbles formed during annealing the irradiated samples at high temperature. On the other hand, for samples implanted with 150?eV He⁺ ions, although He atoms are also trapped in the free volume, no He bubbles were observed during annealing the samples even up to 873?K. In conclusion, the formation of He bubbles is related to the formation and migration of vacancy-type defects even in amorphous alloys.     

PbO compensation in the growth of PbWO4: Y3+ crystals

The light yield of Y³⁺-doped PbWO₄ crystals increases after low-dose-rate irradiation with?γ?rays, and the radiation hardness is sensitive to annealing temperature. In the PWO growth procedure, an excess of PbO in the starting materials is a convenient method of compensating for PbO volatility. The relationship between the excess of PbO and the abnormal radiation behaviour has been investigated. The mechanism of the normal excess of PbO in the growth of PWO: Y³⁺ is discussed.     

A novel lattice correspondence of B19 → B19′ transformation in Ti–Ni–Cu shape memory alloy thin film

In this study, we found a novel lattice correspondence of the B19–B19′ transformation in a Ti–Ni–Cu thin film: (1?1?1)_B19′//(0?0?1)_B19, [0, 1, 1]_B19′//[1?0?0]_B19. Near the coarse precipitate and the grain boundaries, the B19′ martensite forms with the novel lattice correspondence to product the (1?1?1) type I twinning instead of the usual (0?0?1) compound twinning. Crystallographic analyses show that the novel lattice correspondence results from the local stress concentration.     

Static and dynamical ageing processes at room temperature in a Fe25Ni0.4C virgin martensite: effect of C redistribution at the nanoscale

The work-hardening behaviour of virgin martensitic steel has been investigated in a strictly un-aged state and after various ageing conditions. At room temperature (RT), the un-aged alloy shows astonishing tensile performances (ultimate tensile stress?=?1600?MPa/uniform elongation?=?15%) but unexpected serrations. These serrations can be suppressed by static ageing (at RT or higher) while maintaining the initial work-hardening rate (ageing at RT). Parallel investigations using atom probe tomography reveal that the distribution of carbon at the atomic scale evolves from purely homogeneous for virgin martensite to partly segregated at a very fine scale (5–10?nm) after static ageing. This particular mechanical behaviour can therefore be associated with a very local decrease in available carbon in solid solution due to redistribution and segregations on defects (nanotwins) that occurs rapidly, even after few days at RT.     

Specific heat and low-field magnetocaloric effect in A-site ordered PrBaMn2O6 manganite

The specific heat and magnetocaloric effect (MCE) of A-site ordered PrBaMn₂O₆ manganite have been studied. The anomalies caused by the ferromagnetic (FM) and antiferromagnetic (AFM) phase transitions are revealed in the specific heat curve. Direct and inverse MCE are observed at the Curie and Néel points correspondingly. A value of the inverse MCE in the heating run is smaller than in the cooling regime. We attribute this effect to the competition between FM and AFM interactions. A significant advantage of PrBaMn₂O₆ as a magnetocaloric material is an MCE spanning a broad range of temperature with a maximum at room temperature.