Papers by Keyword: Synchrotron X-Ray

Abstract: Residual stress relaxation in sputtered ZnO films has been studied in-situ by synchrotron x-ray diffraction. The films deposited on (001) Si substrates were thermally treated from 25°C to 700°C. X-ray diffraction 2D patterns were captured continuously during the heating, plateau and cooling ramps. The corrections carried out for compensating the furnace drift are discussed. We first observe an increase of the intrinsic compressive stresses before stress relaxation starts to operate around 370°C. Then, thermal contraction upon cooling dominates so that overall, the large initial compressive film stresses turn to tensile after thermal treatment. The overall behaviour is discussed in terms of structural changes induced by the heat treatment.

Abstract: We investigated dislocation behavior in the crystal grown on 6H-SiC (0001) by solution method using synchrotron X-ray topography and thermal chlorine etching. It was confirmed that basal plane dislocation was not newly formed in the grown layer. In addition, the positions of threading screw dislocations (TSDs) were displaced and some of them disappeared in the grown layer. This displacement was caused by the bending of the TSDs during growth.

Abstract: A motorcycle transmission gear of chromium-molybdenum steel with 0.2%C was carburized in carrier gas. Carburizing process including heating, carburizing, diffusing and quenching was simulated using elastoplastic finite element method. The carbon content, hardness, residual strain and residual stress fields of gear were analyzed. The unstressed lattice plane spacing and residual strains of the interior near the internal spline of gear were experimentally measured by synchrotron x-ray and neutron diffraction methods. As a result, the analyzed carbon content and hardness gradients of gear accorded with the experimental results. The radial, hoop and axial directions of cylindrical gear were found to be not always principal axes of residual stress field. On the other hand, the analyzed residual strains in the radial, hoop and axial directions of gear slightly discorded with the experimental results. Although correlation between the measured three strains was similar to that of the weighted average of analyzed strains, residual strain and stress fields of motorcycle transmission gear could not be accurately predicted at the present finite element analysis. It was concluded that carbon diffusion phenomenon and resultant hardening could be analyzed by the finite element method, and the actual interior residual strain and stress fields should be nondestructively measured by neutron diffraction method.

Abstract: The residual strain field around the scratches of 125µm depth and 5µm root radius have been measured from the Synchrotron X-ray diffraction. Scratches were produced using different tools in fine-grained aluminium alloy AA 5091. Residual stresses up to +1700 micro-strains were measured at the scratch tip for one tool but remained up to only +1000 micro-strains for the other tool scratch. The load-displacement curves obtained from nanoindentation were used to determine the residual stresses around the scratches. It was found that the load-displacement curves are sensitive to any local residual stress field present and behave according to the type of residual stresses. This combination of nanoindentation and synchrotron X-rays has been proved highly effective for the study of small-scale residual stresses around the features such as scratches.

Abstract: Material of the specimen was austenitic stainless steel (SUS316L). The specimens were given tensile plastic strains from 0% to 55%. The Vickers hardness of the specimen corresponded to the plastic strain. The residual macrostress was measured by Mn-Kα radiations. The residual macrostress of the annealed specimen had a small compression and changed into a tension after ten- sile plastic deformation. The specimen with 1% plastic strain showed the maximum tensile residual stress. To examine the dependency of the residual stress on the lattice plane, the residual microstress for each lattice plane was measured by hard synchrotron X-rays. The residual microstress was related with Young’s modulus which was calculated by Kro¨ ner model. A new method, 2θ-cos2 χ method, was proposed to solve the problem of coarse grains and it was excellent in comparison with the sin2 ψ method.

Abstract: The internal stress in solid-oxide fuel cells (SOFCs) was evaluated during the thermal, reduction and re-oxidation cycles by using high-energy X-ray synchrotron radiation of about 70 keV at Beam line BL02B1 of SPring-8. The oxidized cell has a compression of about 400 MPa in the c-ScSZ electrolyte and a tension of 50-100 MPa in the NiO-YSZ anode at room temperature. In-situ measurement during the thermal cycle in an air atmosphere, the internal stress decreased with increasing temperature, becoming approximately zero at 1000 K. After the thermal cycle, the internal stress returned to its initial value. In the measurement during the reduction cycle, the internal stress was smaller than that measured during the cooling cycle after the anode was reduced from NiO-YSZ to Ni-YSZ. In the re-oxidation cycle of a reduced cell, the internal stress in the electrolyte went into tension above 800 K when the anode was re-oxidized from Ni-YSZ to NiO-YSZ. This tensile stress is responsible for possible fracture of unit cells in SOFCs.

Abstract: In order to understand an effect of crack-face bridging stress field of alumina ceramics on its fracture toughness, local residual stress distribution due to crack face grain bridging behind the crack tip was measured using synchrotron x-ray beam at SPring-8 in Japan. The SEPB (Single Edge Precracked Beam) specimens of two types of polycrystalline Al2O3 were used for stress measurement; one was pressureless sintered Al2O3 (AL1) and the other was hot-press sintered Al2O3 (TAL). Pop-in precracks were introduced by bridge-indentation method. Before residual stress mapping, the SEPB specimens were unloaded from a constant applied load to zero using four points bending device. Two-dimensional residual stress field was mapped by scanning a micro X-ray beam of 50×50 μm2 with the scanning interval of 12.5 or 25 μm. As a result, in the case of AL1 having conventional fracture toughness and strength, the compressive residual stresses due to crack-face bridging were only observed in the close vicinity of crack tip. On the other hand, in the case of TAL having higher fracture toughness and strength, the compressive residual stresses were widely distributed behind the crack tip. Larger compressive stress was locally generated along the crack path at interlocked grains. The compressive bridging stresses distributed behind the crack tip were found to enlarge with a decrease in the crack opening displacement against a constant applied stress intensity factor, Kapp. It was concluded that the difference in residual stress fields behind crack tip was attributed to the differences in its microstructure and microcrack propagation behavior, such as deflections and interlocked grains.

Abstract: In order to clarify the effect of alloying elements on the axial ratio of magnesium binary solid solutions, the solid solutions of Mg-Al, Mg-Zn, and Mg-Li with various concentrations were casted and homogenized. Synchrotron X-ray diffraction patterns were then obtained from annealed powder samples and analyzed using the Rietveld method. The effects of solutes concentration on lattice parameters were explained on the basis of atomic size difference and valence electron effect, which changes electron overlap of magnesium. It has been found in this study that Al and Li raise and reduce the c/a ratio, respectively, while Zn has no effect on the c/a ratio.

Abstract: Most of the advanced Zr-based alloys contain Nb for improving the corrosion resistance. However, the Nb effect on the corrosion behavior of Zr alloys has not been established. For developing fuel cladding materials, it is essential to investigate the effect of the Nb-content and annealing conditions after beta quenching on the microstructure and the corrosion of Zr-xNb alloys. In this study, a systematic investigation to obtain the optimized annealing condition and Nb content were performed for Zr-xNb alloys (x = 0.1~2.0 wt.%). The corrosion resistance of 0.1 and 0.2 wt.% Nb alloys where Nb existed in an equilibrium soluble state in the matrix was excellent in the quenched and annealed conditions. For the high Nb-containing alloys, the corrosion rates were very sensitive to the annealing condition, and it took about 50 hours at 570
to reach the corrosion rates comparable to those of the low Nb wt.% alloys. The corrosion resistance was closely related to the stabilization of the tetragonal ZrO2 and the columnar oxide structure when the Nb concentration in the matrix was reduced to the equilibrium soluble limit.