Papers by Author: Yuichi Ikuhara

Abstract: We systematically investigated the phase transformation and grain-growth behaviors during sintering in 2 and 3 mol% Y₂O₃-stabilized tetragonal ZrO₂ (2Y and 3Y) and 8 mol% Y₂O₃-stabilized cubic ZrO₂ polycrystals (8Y). In particular, grain-boundary segregation and grain-interior distribution of Y³⁺ ions were examined by high-resolution transmission electron microscopy (HRTEM)- and scanning transmission electron microscopy (STEM)-nanoprobe X-ray energy dispersive spectroscopy (EDS) techniques. Above 1200°C, grain growth during sintering in 8Y was much faster than that in 2Y and 3Y. In the grain boundaries in these specimens, amorphous layers did not present; however, Y³⁺ ions segregated at the grain boundaries over a width of about 10 nm. The amount of segregated Y³⁺ ions in 8Y was significantly less than in 2Y and 3Y. This indicates that the amount of segregated Y³⁺ ions is related to grain growth behavior; i.e., an increase in segregated Y³⁺ ions retards grain growth. Therefore, grain-growth behavior during sintering can be reasonably explained by the solute-drag mechanism of Y³⁺ ions segregating along the grain boundary. In 2Y and 3Y, the cubic-phase regions were formed in grain interiors adjacent to the grain boundaries and/or the multiple junctions in which Y³⁺ ions segregated, which can be explained by a grain boundary segregation-induced phase transformation (GBSIPT) mechanism.

Abstract: A threading dislocation (TD) in 4H-SiC, which was currently interpreted as a perfect threading edge dislocation (TED) by synchrotron monochromatic-beam X-ray topography (SMBXT) and molten KOH etching with Na₂O₂ additive, was performed comparative characterization using weak-beam dark-field (WBDF) and large-angle convergent-beam electron diffraction (LACBED) methods. The TD was suggested to be dissociated into a dislocation pair which can be observed in the WBDF image of g=-12-10. The TD, which was identified as b//[-12-10] by SMBXT observation, was unambiguously determined as b=1/3[-12-10] by LACBED analysis. In the case of perfect TED, it was found that the direction of Burgers vector derived from SMBXT observation corresponds to LACBED analysis.

Abstract: Microstructure development during sintering in 3 mol% Y2O3-stabilized tetragonal ZrO2 polycrystal (Y-TZP) was systematically investigated in two sintering conditions: (a) 1100-1650°C for 2 h and (b) 1300°C for 0-50 h. In the sintering condition (a), the density and grain size in Y-TZP increased with the increasing sintering temperature. Scanning transmission electron microscopy (STEM) and nanoprobe X-ray energy dispersive spectroscopy (EDS) measurements revealed that the Y3+ ion distribution was nearly homogeneous up to 1300°C, i.e., most of grains were the tetragonal phase, but cubic-phase regions with high Y3+ ion concentration were clearly formed in grain interiors adjacent to the grain boundaries at 1500°C. High-resolution transmission electron microscopy (HRTEM) and nanoprobe EDS measurements revealed that no amorphous or second phase is present along the grain-boundary faces, and Y3+ ions segregated not only along the tetragonal-tetragonal phase boundaries but also along tetragonal-cubic phase boundaries over a width below about 10 nm, respectively. These results indicate that the cubic-phase regions are formed from the grain boundaries and/or the multiple junctions in which Y3+ ions segregated. We termed this process a “grain boundary segregation-induced phase transformation (GBSIPT)” mechanism. In the sintering condition (b), the density was low and the grain-growth rate was much slow. In the specimen sintered at 1300°C for 50 h, the cubic-phase regions were clearly formed in the grain interiors adjacent to the grain boundaries. This behavior shows that the cubic-phase regions were formed without grain growth, which can be explained by the GBSIPT model.

Abstract: The WC/Co interface structures in WC-Co alloys doped with VC, Cr3C2 or ZrC were examined by high-resolution electron microscopy (HRTEM) and X-ray energy dispersive spectroscopy (EDS) with a special interest in the segregation behavior of respective dopants at the WC/Co interfaces. It was confirmed that the addition of VC or Cr3C2 were effective to reduce WC grain size while that of ZrC was not. In case of VC or Cr3C2-doped alloys, the morphology of WC grains largely changed comparing with undoped and ZrC-doped alloys. The WC/Co interfaces of the two alloys tend to form micro facets with (0001) and {1010} habits. EDS analysis with a sub-nano scale probe revealed that the dopants strongly segregated at the two habits. In contrast, such morphology change, and also dopant segregation, could not be observed in ZrC-doped alloy. In our study, doped ZrC was not found to solute in Co-phase. Doped ZrC distributed in Co-phase to form other grains mainly consisting of ZrC. The interface structures of WC/Co could be considered to be closely related to the inhibition effect to WC grain growth.

Abstract: Dislocation structure of 10º low-angle tilt grain boundary in α-Al2O3 has been observed by high-resolution electron microscopy (HRTEM). It was found that perfect <1120> edge dislocations, which are introduced to compensate the misorientation, dissociated into two mixed partial dislocations with {1120} stacking-fault in between. The distances between the two partials were estimated by the force balances between repulsive forces of periodical dislocations and attractive forces from stacking-fault. The stacking-fault energy for 10o low-angle tilt grain boundary was estimated to be much higher than the previously reported value.

Abstract: In this paper, we characterized atomic structure of a Σ = 3, [110]/{112} grain boundary in a yttria-stabilized cubic zirconia bicrystal. High-resolution transmission electron microscopy (HRTEM) clearly revealed that the grain boundary migrated to form {111}/{115} periodical facets, although the bicrystal was initially joined so as to have the symmetric straight boundary plane of {112}. Atomic-scale process for the facet growth could be modeled by the continuous flippings of atoms at the boundary core.

Abstract: The diffusion behavior of Ti3+ along basal dislocations in sapphire has been investigated by SIMS technique. High-density unidirectional dislocations were introduced by the high-temperature mechanical deformation, and Ti3+ ions were subsequently diffused along the dislocations. The SIMS diffusion profiles clearly showed diffusion tail due to the short circuit diffusion along the dislocations called pipe diffusion. Lattice diffusion coefficient and pipe diffusion coefficient of Ti3+ at 1300°C were measured to be 1.0±0.2×10-19 [m2/sec] and 2.0±0.6× 10-13 [m2/sec], respectively.

Abstract: The microstructures in 3 mol% Y2O3-stabilized tetragonal zirconia polycrystal (Y-TZP) sintered at 1100°-1650°C were investigated to clarify cubic-formation and grain-growth mechanisms. The cubic phase in Y-TZP appeared at 1300°C and its mass fraction increased with increasing sintering temperature. High-resolution transmission electron microscopy (HRTEM) and nanoprobe X-ray energy dispersive spectroscopy (EDS) measurements revealed that no amorphous layer existed along the grain-boundary faces in Y-TZP, and Y3+ ions segregated not only along the tetragonal-tetragonal phase boundaries but also along tetragonal-cubic phase boundaries. Scanning transmission electron microscopy (STEM) and nanoprobe EDS measurements revealed that the Y3+ ion distribution was nearly homogeneous up to 1300°C, but cubic phase regions with high Y3+ ion concentration clearly formed inside grains at 1500°C. These results indicate that cubic phase regions are formed from the grain boundaries and/or the multiple junctions in which Y3+ ions segregated. We termed such a new diffusive transformation phenomenon “grain boundary segregation-induced phase transformation (GBSIPT)”. The grain-growth mechanism is controlled by the solute-drag effect of Y3+ ions segregating along the grain boundary.

Abstract: Bicrystals of Nb-doped SrTiO3, having tilt angles of 4o~18 o with respect to [001], were prepared by joining two single crystals at 1873 K and then investigated to identify the effect of tilt angle on the grain boundary structure. The boundaries consisted of a regular array of dislocations but the positioning of cores along the boundary was found to be changed from a line to a zigzag as a tilt angle was increased up to 10o. The 14° - tilted boundary exhibited two kinds of boundary region exist at the same grain boundary; (1) the discrete cores region as observed in 4° ~ 10° - tilted boundaries and (2) the randomly oriented region as found in the 18° boundary. Thus it was observed that the structure of low-angle tilt boundary changed from the discrete dislocation structure to the randomly oriented structure as a tilt angle increases. These structural changes at the grain boundaries are considered to be related to a minimization of strain due to the high density of dislocations.