Materials Science Forum Vols. 706-709

Abstract: Magnetic properties of nanocrystalline Ni and Ni-Fe alloys produced by electrodeposition have been studied at 2K and at 298K. Ni and Ni-15%Fe alloy deposits show nano-grain structure with the average grain size of 23 nm and 12 nm, respectively. Both materials exhibit soft magnetic properties. Nanocrystalline Ni at 2K shows saturation magnetization, coercive force, and remanent magnetization of 57 emu/gr, 101 Oe, and 16 emu/gr respectively. Nanocrystalline Ni-15%Fe alloy exhibits superior soft magnetic properties than Ni with corresponding saturation magnetization, coercive force, and remanent magnetization at 2K of 96 emu/gr, 6 Oe, and 4 emu/gr respectively. The magnetic properties and their dependence upon temperature data are interpreted in terms of the Herzer random anisotropy model for nanocrystalline materials.

Abstract: Three kinds of copper thin films were fabricated by RF-magnetron sputtering. The target power was selected to be 10 and 150 W to change the properties of the films. Thin glass sheet was used as a substrate. For the target power of 150 W, the deposition time was selected to be 7 and 40 min. The thickness was 0.6 μm and 2.9 μm, and the grain size measured was 243 nm and 450 nm, respectively. The grain size of thicker film was larger than that of thinner one. On the other hand, for the target power of 10 W, the thickness and grain size were 2.4 μm and 54 nm, respectively. The grain size depends on the target power. The residual stress distribution in the films was measured by X-ray method. Several methods such as the grazing incidence X-ray diffraction method, the constant penetration depth method and the conventional sin²ψ method were adopted. The measured weighted average stress increased with increasing depth. After taking the maximum value at about 0.3 μm from the surface, the value decreased with increasing depth. The stress distribution near the surface in the films deposited at 150 W was almost identical irrespective of thickness. On the other hand, for the target power of 10 W, the stress distribution shifted to compression side. The reason could be explained by the effect of the thermal residual stress. The real stress distribution was estimated by using the optimization technique. The stress took the maximum value at 0.5 μm from the surface, and was compressive near the substrate. .

Abstract: Residual stresses in welds are of major concern for the structure integrity assessment in industrial components. The stresses in the final weld can be determined relatively simple using well established destructive or non-destructive techniques. However, such measurements reflect only the final condition and it remains unclear how stresses built up during the welding process. In order to optimise the final residual stresses in the weld, it is important to monitor the formation of residual strain and stress during the welding process and as such to gain insight into the mechanisms of stress development. In this work non-destructive high energy dispersive synchrotron X-ray diffraction at a high count rate is applied in order to dissolve the welding process in-situ in time and temperature. However, the achievable time resolution at commonly used instruments is restricted by either a limited photon flux or the read out electronics of the detector system resulting in counting times usually much longer than 1sec. We present an energy dispersive detector and read-out-electronics setup realized at the high flux and energy beam line ID15A at the ESRF. The setup allowed for monitoring the strain evolution in two perpendicular directions simultaneously at a sampling rate of 5Hz, resulting in sufficient time and temperature resolution. The change in detector dead time is accounted for by a correction function, which was specifically determined for the detector setup as used for this in-situ experiment.

Abstract: The aim of the present study was to study the interface implant-bone by synchrotron radiation, the implant has two faces the first one coated with hydroxyapatite and the second uncoated. In orthopaedic surgery, Titanium (Ti-Al-4V) implants are currently coated with hydroxyapatite (HAp), Ca₁₀ (PO₄)₆ (OH)₂, in order to obtain a stable and functional direct connection between the bone and the implant. At the implant-bone interface, the new bone reconstituted after two months of implantation must have the same properties like the natural bone in order to accept the implant. Therefore we studied the texture of the reconstituted bone crystals at the interface applying non destructive x-ray diffraction. The required high spatial resolution was achieved utilizing high-energy synchrotron radiation on ID15 at ESRF in Grenoble, France.

Abstract: In this work, we propose an analytical model, capable of distinguishing the contribution of porosity, pore morphology and solid domain properties to the macroscopic elasticity of a porous ceramic material. A practical method is shown for the evaluation of the dense material elastic properties in porous (and microcracked) polycrystalline materials, making use of in-situ neutron diffraction experiments. By this method, axial and transverse microstrains measurements can reveal the average values for Young’s modulus and Poisson’s ratio of the dense material, as well as the value of pore morphology at known porosity. The approach has been validated on porous SiC. Finite Element Modeling is shown to allow calculating the three-dimensional strain and stress state under applied uniaxial stress, highlighting that small but finite shear stresses arise. Stress-strain curves of porous and microcracked materials have been generated, which correlate qualitatively well with the measured properties and can be used for quantitative numerical simulation of the materials strength. Predictions of FEM coincide very well with analytical calculations, thus corroborating the validity of the analytical method proposed.

Abstract: The residual stress measurement by the conventional X-ray diffraction was formulated on the assumption that a specimen from polycrystalline materials was quasi-isotropic and homogeneous, and the stress was biaxial and almost constant within the X-ray penetration depth. Therefore, it was not available to analyze the stress state of the textured materials by the conventional measurement as a general rule. In resent years, advanced methods have been proposed for the X-ray stress measurement of textured materials. In some methods, it is assumed that the X-ray elastic constant is derived from the crystallite orientation distribution function of textured materials for solving the first anisotropic problem. However, there is a nonlinear problem in the stress analysis from the measured lattice strain. In present study, the X-ray elastic constants were averaged as the expected value around the normal direction of the X-ray diffraction in a similar way. A stress analysis was proposed by differential calculus of the X-ray elastic constant in order to the avoidance of nonlinear problem. The stress analysis was applied to residual stress measurements of a titanium carbide coating film with preferred orientation and a cold-rolled steel with texture. The calculated values of the X-ray elastic constants showed the linearity on some condition for the film. The X-ray stress determination was carried out by the fitting the gradients of the measured lattice strain.

Abstract: In the rolling bearing, the flaking caused by rolling contact fatigue is classified into two types: surface originated flaking and subsurface originated flaking. It has been recognized that marked microstructural change can occur in subsurface originated flaking due to rolling contact fatigue. But there are few reports in surface originated flaking about microstructural change. In this study, surface originated flaking caused by rolling contact fatigue was investigated based on microstructural change. Thrust ball bearing and radial ball bearing was used for fatigue test. Simulation of dent originated flaking was carried out using the bearing with artificial dent. Another fatigue test subjected to surface originated flaking was done under shortage of oil film thickness lubrication condition. Microstructural change was measured by X-ray Diffractmetry (XRD) and Transmission Electron Microscopy (TEM) during fatigue testing. Microstructure of bearing steel used for fatigue test is consisted of martensite with small amount of retained austenite. XRD measurement reveals that the half peak width of martensite and volume fraction of retained austenite decreasing with increasing testing time, and the amount of decrease in these parameter were small in the surface originated flaking compared with subsurface originated flaking when the specimens were flaking. This suggests that surface originated flaking occurs in spite of mild microstructural change. TEM observation about the surface originated flaking shows plastic flow in the surface layer. Especially, it was confirmed that partial recrystallization occurs in the fatigue test under shortage of oil film thickness lubrication condition. But it was also confirmed that degree of recrystallization is lower in the surface originated flaking than subsurface one, and this reasonably explains XRD result. From these results, it was cleared that recrystallizaiton of martensite is differ in degree but not in kind between surface originated flaking and subsurface originated flaking.

Abstract: An analysis of residual stress, one of the contributory factors to the crack tip driving force, is extremely important to probe the fatigue crack growth mechanism and to further develop the life prediction methodology. Since fatigue crack growth is governed by crack-tip plasticity and crack closure in the wake of the crack tip, the investigation of residual stain/stress field in both behind and in front of the crack tip is crucial. In the current work, a 304L stainless steel compact-tension specimen is pre-cracked under constant-amplitude cyclic loading. Neutron diffraction is employed to directly measure the three orthogonal residual strain fields with 1-mm spatial resolution as a function of distance from the crack tip. The mapping results show that the three orthogonal residual-strain distributions around the crack tip depend on the stress multiaxiality, not following a single Poisson relationship to each axis.

Abstract: With the arrival of the third generation of synchrotron sources and/or the introduction of advanced insertion devices (wigglers and undulators), the high energy (E > 50 keV) x-ray diffraction technique has become feasible, leading to new approaches in the quantitative study of the structure of disordered materials than was hither to available. Since we built the SPring-8 bending magnet beamline BL04B2 and two-axis diffractometer for disordered materials in 1999, we have studied on disordered materials from ambient to extreme condition. In this article, the high-energy x-ray diffraction beamline BL04B2 of SPring-8 and recent developments of ancillary equipment (automatic sample changer, conventional high-temperature furnace, aerodynamic levitation furnace) are introduced. Furthermore the structural analysis on the basis of diffraction data with the aid of computer simulations, which we performed in the last 10 years is reviewed.

Abstract: Synchrotron X-ray diffraction is reliable to measure residual stresses and characterize existing phases close to substrate/coating interface. In the present study, we focus on the cobalt-alloys coating deposited on stainless steel forging tools via Plasma Transfer Arc (PTA) process. Forging tools always work in high temperature conditions. Since fatigue crack is often detected near to the interface, we used synchrotron radiation to characterize residual stress profiles both in the substrate and coating sides. Also, we defined phases inside diluted substrate layers and in the stellite coating using a Rietveld refinement.