Photoluminescence properties of trace amounts of Pr and Tb in yttria-stabilized zirconia

We have investigated the photoluminescence (PL) properties of trace amounts of Pr and Tb in single-crystal samples of yttria-stabilized zironia (YSZ), and found that Pr of the order of 10⁻⁶ mass% and Tb of the order of 10⁻⁵ mass% in YSZ can be detected by the PL spectroscopy. The PL spectra of the YSZ samples for the 280 nm excitation were comprised of several peaks and a broad emission. The peaks were attributed to transitions of Pr³⁺ and Tb³⁺ in the YSZ samples, whereas the broad emission seemed to be attributed to the yttria-associated oxygen vacancies. The peak intensities corresponded to the amounts of Pr and Tb in the YSZ samples, the amounts of which were analyzed by glow discharge mass spectrometry. In the PL excitation spectra, but not in the photoabsorption spectra, small peaks at 376 and 381 nm were observed, and were attributed to the transitions of Tb³⁺ in the YSZ samples. The results of the PL excitation spectra corresponding to the Pr³⁺ line emissions suggest that the charge transfer occurs between the YSZ and Pr ion in it. The trace amounts of these lanthanoids in YSZ would disturb the decay process of the photoinduced electrons to the yttria-associated oxygen vacancies.     

Local structure analysis of smoky and colorless topaz using single crystal Al NMR

The angular dependence of the ²⁷Al NMR spectrum was measured for single crystals of smoky and colorless topaz, Al₂SiO₄(F,OH)₂. Smoky topaz was obtained by irradiating high energy neutrons to colorless topaz. The quadrupole coupling constant e²Qq/h and the asymmetry parameter η were obtained from the analysis of the angular dependences of quadrupole splitting of the ²⁷Al NMR spectrum. The local structures around the aluminum atoms in smoky and colorless topaz were discussed from the magnitude and the direction of the electric field gradient. The directions of principal axes of the EFG tensor of ²⁷Al were close to the directions of Al-O and Al-F bonds. The difference in the bond lengths between Al(1)-F(1) and Al(1)-F(2) was found to affect the x and y components of the EFG tensor.     

统计优化迭代法测量质子交换波导折射率分布

提出了一种用于拟合测量渐变波导的折射率分布的新的理论处理。该方法把统计优化手段导入循环迭代法 ,可适用于费米函数这一类曲线变化范围大、且有多个自变量的函数。实验上用焦磷酸质子交换制备了LiNbO3波导样品 ,用该方法对退火后的折射率分布作了测量拟合 ,折射率拟合值与实验值的均方差为± 8.2× 10 - 4。     

Evaluation of fine structure of tubular zeolite NaA membrane by FTIR-ATR and FIB-TEM.

A zeolite NaA (LTA) membrane supported by an alumina porous support tube for pervaporation (PV) dehydration of ethanol was characterized by transmission electron microscopy (TEM) using a focused ion beam (FIB) thin-layer specimen preparation technique and by Fourier transform infrared attenuated total reflectance method (FTIR-ATR) using a diamond prism as the waveguide. FIB-TEM clearly presented cross-section images up to about 15 microm depth from the membrane surface. FTIR-ATR monitored the Si-O asymmetric stretching vibration spectrum. The Si-O spectrum was compared with the TEM image and their relationships were discussed. By combining the two methods, we could study the thickness of surface LTA crystals, the grain boundary, the LTA/alumina interface structure and the crystallinity and density of materials inside of the alumina porous support. Consequently, fine structure changes of the LTA membrane corresponding to the hydrothermal synthesis condition could be sensitively detected.     

Phase Measurement Algorithm in Wavelength Scanned Fizeau Interferometer

Wavelength scanned interferometry allows the simultaneous measurement of top surface shape and optical thickness variation of a transparent object consisting of several parallel surfaces. Interference signals from these surfaces can be separated in frequency space, and their phases are detected by discrete Fourier analysis. However, these signal frequencies are shifted from the detection frequency by the refractive index dispersion of the object and a nonlinearity of the wavelength scanning. The Fourier analysis is sensitive to the detuning of the signal frequency and suffers from the multiple-beam interference noise. Conventional error-compensating algorithms cannot be applied to an object consisting of more than three reflecting surfaces. We derive a new 2N-1 sample error-compensating algorithm, which allows the phase detection of any order of harmonic frequency among the interference signals. The new algorithm suppresses the effect of signal frequency detuning as well as the multiple-beam interference noise and can be applied to the measurement of complex objects consisting of more than three reflecting surfaces.     

Structural and electrical properties of crystalline (1−x)Ta2O5−xTiO2 thin films fabricated by metalorganic decomposition

Polycrystalline (1−x)Ta₂O₅−xTiO₂ thin films were formed on Si by metalorganic decomposition (MOD) and annealed at various temperatures. As-deposited films were in the amorphous state and were completely transformed to crystalline after annealing above 600 °C. During crystallization, a thin interfacial SiO₂ layer was formed at the (1−x)Ta₂O₅−xTiO₂/Si interface. Thin films with 0.92Ta₂O₅–0.08TiO₂ composition exhibited superior insulating properties. The measured dielectric constant and dissipation factor at 1 MHz were 9 and 0.015, respectively, for films annealed at 900 °C. The interface trap density was 2.5×10¹¹ cm⁻² eV⁻¹, and flatband voltage was −0.38 V. A charge storage density of 22.8 fC/μm² was obtained at an applied electric field of 3 MV/cm. The leakage current density was lower than 4×10⁻⁹ A/cm² up to an applied electric field of 6 MV/cm.     

Preparation and certification of the new reference materials; plastics (disk form, JSAC 0621-0625) for determination of mercury using x-ray fluorescent analysis.

The Japan Society for Analytical Chemistry has developed some new plastic certified reference materials (CRMs) for the analysis of mercury in polyester disks using XRF analysis. These CRMs (named as JSAC 0621-0625) were prepared by casting polyesters including a toluene solution of organometallic compounds as a standard. Concentrations of the five levels of mercury ranged from 0 to 250 mg/kg. Homogeneity tests of prepared disks had shown excellent results. Interlaboratory comparison study for the certification was performed by 15 laboratory participants. The z-scores in robust statistical method was applied for the evaluation of outliers. The certified values were assigned after discarding outliers. The uncertainties of certified values were determined as the confidence levels of 95%.