Evolution of the residual stress state in a duplex stainless steel during loading

The evolution of micro- and macrostresses in a duplex stainless steel during loading has been investigated in situ by X-ray diffraction. A 1.5 mm cold-rolled sheet of alloy SAF 2304 solution treated at 1050°C was studied. Owing to differences in the coefficient of thermal expansion between the two phases, compressive residual microstresses were found in the ferritic phase and balancing tensile microstresses in the austenitic phase. The initial microstresses were almost two times higher in the transverse direction compared to the rolling direction. During loading the microstresses increase in the macroscopic elastic regime but start to decrease slightly with increasing load in the macroscopic plastic regime. For instance, the microstresses along the rolling direction in the austenite increase from 60 MPa, at zero applied load, to 110 MPa, at an applied load of 530 MPa. At the applied load of 620 MPa a decrease of the microstress to 90 MPa was observed. During unloading from the plastic regime the microstresses increase by approximately 35 MPa in the direction of applied load but remain constant in the other directions. The initial stress state influences the stress evolution and even after 2.5% plastic strain the main contribution to the microstresses originates from the initial thermal stresses. Finite element simulations show stress variations within one phase and a strong influence of both the elastic and plastic anisotropy of the individual phases on the simulated stress state.     

Austenite–ferrite transformation kinetics under uniaxial compressive stress in Fe–2.96 at.% Ni alloy

The effect of an applied constant uniaxial compressive stress on the kinetics of the austenite (γ) → ferrite (α) massive transformation in the substitutional Fe–2.96 at.% Ni alloy upon isochronal cooling has been studied by differential dilatometry. All imposed stress levels are below the yield stress of austenite and ferrite in the temperature range of the transformation. An increase in compressive stress results in a small but significant increase of the onset temperature of the γ → α transformation and a decrease of the overall transformation time. A phase transformation model, involving site saturation, interface-controlled growth and incorporation of an appropriate impingement correction, has been employed to extract the interface-migration velocity of the γ/α interface. The interface-migration velocity for the γ → α transformation is approximately constant at fixed uniaxial compressive stress and increases with increasing applied uniaxial compressive stress. Furthermore, the value obtained for the energy corresponding with the elastic and plastic deformation associated with the accommodation of the γ/α volume misfit depends on the transformed fraction and decreases significantly as the applied uniaxial compressive stress increases. An understanding of the observed effects is obtained, recognizing the constraints imposed on the phase transformation due to the applied stress.     

Press for hydrostatic extrusion with back-pressure and the properties of thus extruded materials

A press for hydrostatic extrusion within the extrusion pressure range up to 2 GPa with back-pressure up to 0.7 GPa was designed and constructed. The press is equipped with an integrated pressure intensifier, and a control and recording system which permits recording the process parameters, such as extrusion pressure, back-pressure and its stability, time and speed of the extrusion, and enables monitoring the process on-line. The double-layer high-pressure chamber and the monobloc back-pressure chamber were analyzed using the finite element method with allowance made for the self-strain-hardening effect known as autofrettage. The maximum permissible load imposed on chambers and the resulting balance pressure established in the case of the two chambers being accidentally connected were also evaluated. Several cold extrusion processes assisted with back-pressure from 400 MPa to 700 MPa were conducted, experimenting with low or non-ductile materials, such as the ZW3 magnesium alloy, GJL250 grey cast iron, GJS500 nodular cast iron, bismuth of 99.999% purity, and molybdenum of 99.9% purity. The bulk, non-defected products with diameters ranging from 4 to 7 mm were obtained. The use of back-pressure permitted the materials to be plastically deformed during a single cold operation with the percent deformation from 36% in grey cast iron to more than 80% in Bi. Thanks to the strain-hardening due to the severe plastic deformation, the materials acquired excellent properties (YS = 392 MPa in the magnesium alloy, σ_d0.2 = 709 MPa in molybdenum, σ_dM = 1140 MPa in grey cast iron, and σ_d0.2 = 643 MPa in nodular cast iron) impossible to achieve by classical plastic deformation processes. The hardness of the materials was also increased adequately, and the refinement of their microstructure resulted in an increase of ductility. These advantageous results obtained by using the press indicate that hydrostatic extrusion with back-pressure has a great applicative potential.     

Effect of strain rate on deformation behavior of TRIP steels

Tensile deformation behavior of Si–Mn TRIP (TRansformation Induced Plasticity) steel with vanadium and without vanadium and the DP (Dual Phase) steel of the same composition were studied in a large range of strain rate (0.001–2000 s^?1) by routine material testing machine, rotation disk bar–bar tensile impact apparatus and high-speed material testing machine of servo-hydraulic type. In situ measurement of the transformation of retained austenite was performed by means of X-ray stress apparatus in order to have detailed knowledge about the transformation of retained austenite at quasi-static tensile. Microstructure of steels before and after tensile were observed by means of optical microscope (OM), scanning electron microscope (SEM) and transmission electron microscope (TEM). It is shown that there is no yield plateau observed on the stress–strain curve at quasi-static condition for TRIP steel containing vanadium because the vanadium carbide suppress the formation of Cottrell atmosphere in matrix. Retained austenite of Si–Mn TRIP steel containing vanadium transforms to martensite at loading stress of 502 MPa (its yielding strength is 486 MPa), while the transformation of retained austenite in matrix of Si–Mn TRIP steel without vanadium happens when its yielding process is finished at quasi-static tensile. It is confirmed that phase transformation of retained austenite in TRIP steel is strain induced phase transformation. It is noted that tensile elongation of TRIP steel at dynamic tensile is always lower than that at quasi-static tensile. That is because gradually strain induced phase transformation of retained austenite in TRIP steel is suppressed by deformation localization at dynamic tensile.     

The growth of PANI films at 450 MPa

A series of polyaniline (PANI) films were prepared on quartz substrates by in situ polymerization with different reaction time under 450 MPa of hydrostatic high pressure. For investigating the effect of high pressure on the growth of the films, two additional series of samples with comparable conditions under ambient pressure were synthesize. The aniline cation radicals nucleated within 2 min and the polyaniline films grew within 10 min at 450 MPa of pressure. This compared with about 10 min for nucleation and 60 min for growth of polyaniline films under comparable ambient conditions. The process of PANI film growth under high pressure was obviously different from that in ambient pressure case. The high pressure used in polymerization affected directly the electrical property, the morphology, and growth of the films. A formation model of polyaniline film growth in high pressure case was proposed.     

On thermal and vibrational properties of LaGaO3 single crystals

The thermal expansion and vibrational properties of [1 0 0] and [0 0 1] LaGaO₃ single crystals have been studied by thermal mechanical analysis and micro-Raman spectroscopy. A first-order orthorhombic to rhombohedral phase transition has been confirmed by both techniques, as well as by in situ heating using optical microscopy. The appearance of a metastable intermediate phase, tentatively assigned as monoclinic, has been detected both by optical microscopy and Raman spectroscopy upon heating of the [1 0 0] and [0 0 1] LaGaO₃ single crystals. Not only temperature, but the stress-induced orthorhombic to rhombohedral phase transition has also been detected by Raman mapping of the residual impression made by Vickers indentation. The position map of bands belonging to the lower-temperature/pressure orthorhombic and the higher-temperature/pressure rhombohedral phase show that the rhombohedral phase is located inside the impression, where the applied indentation stresses are the highest, whereas no rhombohedral phase is detected outside the impression, where the surface has not been altered by contact stresses.     

Double twinning in Ni–Mn–Ga–Co

Magnetic shape-memory alloys tend to deform via magnetic-field-induced and stress-induced twin-boundary motion. The rather low martensite transformation temperature of ternary Ni–Mn–Ga limits the operating temperature for potential applications. By alloying 5 at.% cobalt, the martensite transformation temperature and the Curie temperature was increased from 70 and 110 °C respectively up to 160 °C. In the single crystalline samples two non-modulated structures with tetragonal and orthorhombic lattices were found. The non-modulated orthorhombic structure has similar lattice parameters to the pseudo-orthorhombic 14M Ni–Mn–Ga phase. The single crystal specimen with the non-modulated orthorhombic structure exhibited a cyclic permutation of all three crystallographic axes in response to uniaxial loading. The parallelepiped-shaped sample was compressed repeatedly in all three directions. While maximizing work done by the load during deformation required three different martensite variants to result from deformation in three different directions, only two different martensite variants were found. The analysis of the sample shape revealed two variants mutually related through cyclic permutation of the lattice parameters, which cannot result from a single twinning event. The cyclic permutation is discussed in the light of Crocker’s double twinning mechanism.     

In situ observation of syntactic foams under hydrostatic pressure using X-ray tomography

Syntactic foams (hollow glass microspheres embedded in a polymeric matrix) are being used increasingly for the purpose of thermal insulation in ultradeep water. A better understanding of the damage mechanisms of these materials at the microsphere scale under such a hydrostatic loading condition is of prior importance in determining actual material limits, improving phenomenological modelling and developing novel formulations in the future. To achieve this goal, a study based on X-ray microtomography was performed on two syntactic foam materials (polypropylene and polyurethane matrix) and a standard foamed PP. A special set up has been designed in order to allow the X-ray microtomographic observation of the material during hydrostatic pressure loading using ethanol as the pressure fluid. Spatial resolution of (3.5 μm)³ and in situ non-destructive scanning allowed a unique qualitative and quantitative analysis of the composite microstructure during stepwise isotropic compression by hydrostatic pressure up to 50 MPa. The collapse of weaker microspheres were observed during pressure increase and the damage parameters could be estimated. It is shown that the microspheres which are broken or the porosities which are close to the surface in the foamed PP are filled by a fluid (either the ethanol or the polymeric matrix itself). The hydrostatic pressure decreases the volume of the foam only slightly. In the PU matrix, ethanol diffusion is seen to induce swelling of the matrix, which is an unexpected phenomenon but reveals the high potential of X-ray microtomographic observation to improve diffusion analysis in complex media.     

Shape memory properties of Ti–Nb–Mo biomedical alloys

Mo is added to Ti–Nb alloys in order to enhance their superelasticity. The shape memory properties of Ti–(12–28)Nb–(0–4)Mo alloys are investigated in this paper. The Ti–27Nb, Ti–24Nb–1Mo, Ti–21Nb–2Mo and Ti–18Nb–3Mo alloys exhibit the most stable superelasticity with a narrow stress hysteresis among Ti–Nb–Mo alloys with Mo contents of 0, 1, 2 and 3 at.%, respectively. The ternary alloys reveal better superelasticity due to a higher critical stress for slip deformation and a larger transformation strain. A Ti–15Nb–4Mo alloy heat-treated at 973 K undergoes (2 1 1)〈1 1 1〉-type twinning during tensile testing. Twinning is suppressed in the alloy heat-treated at 923 K due to the precipitation of the α phase, allowing the alloy to deform via a martensitic transformation process. The Ti–15Nb–4Mo alloy exhibits stable superelasticity with a critical stress for slip deformation of 582 MPa and a total recovery strain of 3.5%.     

A TEM study on the crystallization behavior of an yttrium-doped Zr-based bulk metallic glass

Transmission electron microscopy (TEM) is used to conduct the systematic study of the annealing induced crystallization, both continuously and isothermally, of a Zr-based metallic glass. Through detailed microstructure analysis, it is found that the crystallization of this metallic glass is initialized by a nano-scaled primary crystallization process with a tetragonal structured crystal (a = 0.96 nm and c = 2.82 nm) as the primary phase. A eutectic crystallization is followed afterwards with two types of crystalline phases as the crystallization products, one of which is determined to be a metastable orthorhombic phase (a = 0.69 nm, b = 0.75 nm and c = 0.74 nm). Upon annealing at a raised temperature or isothermal treatments, a solid state phase transformation takes place and the orthorhombic metastable phase transforms into two types of tetragonal crystalline phases. The whole crystallization process of this metallic glass is in turn realized, and the thermal stability and nano-crystallization mechanism are discussed based on the microstructure and thermal analyses.     

Deformation mechanisms of a 20Mn TWIP steel investigated by in situ neutron diffraction and TEM

The deformation mechanisms and associated microstructure changes during tensile loading of an annealed twinning-induced plasticity steel with chemical composition Fe–20Mn–3Si–3Al–0.045C (wt.%) were systematically investigated using in situ time-of-flight neutron diffraction in combination with post mortem transmission electron microscopy (TEM). The initial microstructure of the investigated alloy consists of equiaxed γ grains with the initial α′-phase of ～7% in volume. In addition to dislocation slip, twinning and two types of martensitic transformations from the austenite to α′- and ε-martensites were observed as the main deformation modes during the tensile deformation. In situ neutron diffraction provides a powerful tool for establishing the deformation mode map for elucidating the role of different deformation modes in different strain regions. The critical stress is 520 MPa for the martensitic transformation from austenite to α′-martensite, whereas a higher stress (>600 MPa) is required for actuating the deformation twin and/or the martensitic transformation from austenite to ε-martensite. Both ε- and α′-martensites act as hard phases, whereas mechanical twinning contributes to both the strength and the ductility of the studied steel. TEM observations confirmed that the twinning process was facilitated by the parent grains oriented with 〈1 1 1〉 or 〈1 1 0〉 parallel to the loading direction. The nucleation and growth of twins are attributed to the pole and self-generation formation mechanisms, as well as the stair-rod cross-slip mechanism.     

A distributed step-like switching model of the continuous field-driven phase transformations observed in PMN–xPT relaxor ferroelectric single crystals

The field-driven phase transformation behavior of relaxor ferroelectric single crystal PZN–xPT is discontinuous and displays well-defined forward and reverse coercive fields, whereas the same transformation in PMN–xPT is nearly continuous and occurs over a range of field levels. In analogy to the broad Curie range in relaxor ferroelectrics arising from property fluctuations at the nanometer length scale, the continuous field-driven phase transformations in PMN–xPT are modeled as a step-like series of discontinuous transformations associated with similar spatial property fluctuations. An increase in the applied field gradually increases the volume fraction of the new phase at the expense of the old phase, resulting in a continuous transition between phases. The model simulation produces excellent agreement with the measured material response of 〈0 1 1〉 cut PMN–0.32PT single crystals under conditions of cooperative stress and electric field loading.     

Controlling Al/Cu composite diffusion layer during hydrostatic extrusion by using colloidal Ag

In this study, intermetallic compound formation at the interface between aluminum and copper during hydrostatic extrusion was simulated by performing a solid state diffusion bonding experiment with various processing parameters, including bonding temperature and pressure and holding time, and by inserting an Ag colloid layer between the aluminum and copper. Regression equations were developed to predict thickness of diffusion layer and interface hardness.An intermetallic compound formed at the interface between the Al and Cu during diffusion bonding at 420 °C and 240 MPa for 60 min, and it was effectively controlled by inserting an Ag colloid. These experimental data will be useful for setting up processing parameters to prepare Al/Cu matrix composite materials by using hydrostatic extrusion.     

Atomistic study of hydrogen distribution and diffusion around a {1 1 2}<1 1 1> edge dislocation in alpha iron

Despite extensive investigations, the distribution of hydrogen around a stress singularity field is still not well understood. In this study, we conducted molecular statics (MS) analyses of the hydrogen-trap energy around a {1 1 2}<1 1 1> edge dislocation in alpha iron. The distribution of hydrogen in crystals is generally assumed to be dominated by hydrostatic stress. However, the MS results indicate that the hydrogen-trap energy is sensitive to shear stress as well as hydrostatic stress, thus indicating that strong trap sites are distributed across a wide range on the slip plane around the dislocation core. We also performed molecular dynamics simulation of hydrogen diffusion, and revealed the anisotropic diffusion behaviour of hydrogen around the dislocation core.     

Inter-martensitic transitions in Ni–Fe–Ga single crystals

The strain–temperature response of Ni–Fe–Ga single crystals underscores the role of the inter-martensitic transformation in creating intersecting heating and cooling segments; the separation of these segments occurs due to irreversibilities at high stresses and at high temperatures. An ultra-narrow tensile (1 °C) and compressive (<10 °C) thermal hysteresis are observed for the A ⇌ 10M ⇌ 14M case, accompanied by a small stress hysteresis (<30 MPa) in compressive and tensile stress–strain responses. The hysteresis levels increase and the intersecting segments disappear at high stresses and at high temperatures. This paper reports the use of a thermo-mechanical formulation to rationalize the role of inter-martensitic transformations. Plotting the transformation stress as a function of temperature indicates that inter-martensitic transformations enable a very wide pseudoelastic temperature range, as high as 425 °C. The measured Clausius–Clapeyron curve slope in compression (2.75 MPa °C⁻¹) is eight times the tensile slope (0.36 MPa °C⁻¹); the higher slope is attributed to the predominance of A ⇌ L1₀ at high temperatures.     

An in situ bulk Zr58Al9Ni9Cu14Nb10 quasicrystal-glass composite with superior room temperature mechanical properties

An in situ bulk Zr₅₈Al₉Ni₉Cu₁₄Nb₁₀ quasicrystal-glass composite has been fabricated by means of copper mould casting. The microstructure and constituent phases of the alloy composite have been analyzed by using X-ray diffraction, transmission electron microscopy and high-resolution transmission electron microscopy. Icosahedral quasicrystals were found to be the majority phase and the grain size is in half-μm scale. In between the I-phase grains is a glassy phase. Optical microscopy and scanning electron microscopy revealed that the as-cast alloys were pore-free. The microhardness of the composite is about 5.90 ± 0.30 GPa. The room temperature compression stress–true strain curve exhibits a 2% elastic deformation up to failure, and a maximum fracture stress of 1850 MPa at a quasi-static loading rate of 4.4 × 10⁻⁴ s⁻¹. The mechanical property is superior to the early developed quasicrystal alloys, and is comparable to Zr-based bulk metallic glasses and their nanocomposites. The quasicrystal-glass composite exhibits basically a brittle fracture mode at room temperature.     

Processing and dry sliding wear performance of spray deposited hyper-eutectic aluminum–silicon alloys

The influence of spray deposition process on the refinement of silicon phase and the tribological performance of hyper-eutectic Al–Si alloys is reported in this work. Due to the rapid solidification conditions that prevail during the spray deposition process, both primary and eutectic silicon were found to be refined resulting in equi-axed morphology of the silicon phase across the matrix. The average silicon particle size increased from 7 μm to 17 μm with increase in the silicon content of the spray deposited alloys used for the present study. Transmission electron microscopy of the spray deposited samples exhibited sub-micron sized silicon particles of both equi-axed and acicular morphology in the aluminum matrix. Pin-on-disc wear tests were performed on the spray deposited samples, by sliding samples against hardened steel counterface for about 1000 m at a speed of 0.3 m/s under varied loading conditions ranging from 0.17 MPa to 1 MPa. Scanning electron microscopy of the wear tracks and wear debris was carried out to understand the wear mechanism. The wear performance was improved with increase in the silicon content of the alloy. The wear performance of the alloys was compared with similar alloys produced through various processing routes reported in the literature. The spray deposited alloys were observed to exhibit relatively better wear performance for the range of composition and loading conditions employed.     

CRSS of γ/γ′ phases from in situ neutron diffraction of a directionally solidified superalloy tension tested at 900 °C

Neutron diffraction was used to monitor elastic strains during in situ tension testing of a directionally solidified (DS) superalloy at 900 °C. Changes in misfit and thermal expansion coefficients of individual phases were obtained. In the γ phase, it is demonstrated that elastic strains saturate at 350 MPa, which is well below the yield strength of the alloy. This is interpreted as the onset of dislocation glide through less stressed vertical channels. The critical resolved shear stress (CRSS) of γ is found to be 143 ± 11 MPa, in agreement with a calculated CRSS that is dominated by Orowan bowing of dislocations through nanoscale-wide γ channels. This provides confirmation of Orowan bowing in plasticity/creep of the γ phase. Implications of CRSS and misfit in a “threshold stress” for creep and rafting are discussed. The CRSS of γ′ is found to be consistent with pairwise penetration of dislocations into γ′.     

Mechanical behavior of cellular borosilicate glass with pressurized Ar-filled closed pores

High strength borosilicate foams were fabricated by melting glass powder under high-pressure argon gas and subsequent heat treatment of the glass bulk at atmospheric pressure. In the first step, borosilicate glass powder was melted at 1100 °C for 1 h by capsule-free hot isostatic pressing (HIPing) under a high gas pressure of 10–70 MPa. Pressurized Ar-filled spherical pores were introduced into the glass, and argon atoms were dissolved in the glass network structure. The expansion of argon-filled pores and the release of the dissolved Ar gas resulted in the formation of pressurized Ar-filled closed pores by isothermal heat treatment at 800 °C for 10 min. A high porosity of up to 80% with a bimodal distribution of micro-size cells was obtained for the resultant cellular borosilicate glass. By increasing the total gas pressure from 10 to 70 MPa, the compressive strength and the Young’s modulus were increased considerably from 15 to 52 MPa and from 4.1 to 12.6 GPa, respectively, which can be substantially attributed to the high collapse stress from the high enclosed gas pressure. The cellular glass with a high porosity showed a large failure strain under uniaxial compression.