Yasuko Terada

Construction and Commissioning of BL37XU at SPring-8

Trace element analysis beamline (BL37XU) at SPring‐8 was designed for application to various X‐ray fluorescence analyses such as XRF imaging, XAFS, TXRF and XRF holography. The beamline has of two branches, one being a SPring‐8 standard undulator‐beamline optics branch (Branch A) and the other a high‐energy branch (Branch B). In the experimental hutches, several kinds of experimental device are equipped. The end‐stations have been opened to public use since November 2002, and various experiments have been carried out.

Kozoite-(Nd), Nd(CO3)(OH), a new mineral in an alkali olivine basalt from Hizen-cho, Saga Prefecture, Japan

Abstract Kozoite-(Nd), Nd(CO3)(OH), occurs in cavities and fissures of alkali olivine basalt exposed at Niikoba, Hizen-cho, Higashi Matsuura-gun, Saga Prefecture, Japan, in association with lanthanite- (Nd) and kimuraite-(Y). The crystal structure was refined by the Rietveld method in space group Pmcn; a = 4.9829(1), b = 8.5188(2), c = 7.2570(2) Å, Z = 4 using powder diffraction data obtained by a combination of a Gandolfi camera and monochromatic synchrotron radiation. Kozoite-(Nd) is pale pinkish-purple to white with a vitreous to powdery luster. The calculated density is 4.77 g/cm3. It has high birefringence, α = 1.698(2), γ = 1.780(5). The four strongest lines in the X-ray powder patterns [d(Å), I/I0, hkl] are (4.29, 100, 110); (2.93, 89, 102); (2.33, 78, 131) and (2.06, 78, 221). Kozoite-(Nd) is the first naturally occurring RE(CO3)(OH) end-member in the ancylite group.

Emulsion drying preparation of layered LiMnxCr1−xO2 solid solution and its application to Li-ion battery cathode material

Abstract Lithium–chromium–manganese oxides, LiMn x Cr 1− x O 2 (0≤ x ≤0.6), were synthesized as solid solutions by simple calcination of emulsion-dried powder precursor. The product was well crystallized to an α-NaFeO 2 structure (space group: R 3 m ). By combination of Rietveld analysis of X-ray diffraction data and X-ray absorption near edge structure (XANES) techniques, the final product is considered to be [Li I ] 3 a oct [Mn x III Cr 1− x III ] 3 b oct [O 2 ] 6 c (0≤ x ≤0.6). The prepared oxides were electrochemically active, and capacity as cathode materials for lithium-ion battery was improved with increasing Mn substitution amount.

OBSERVATION OF SURFACE DISTRIBUTION OF PRODUCTS BY X-RAY FLUORESCENCE SPECTROMETRY DURING D2 GAS PERMEATION THROUGH Pd COMPLEXES

In-situ measurement of transmutation of Cs into Pr was performed, and the surface distribution of Pr was investigated using XRF (X-Ray Fluorescence spectrometry) at SPring-8, a large synchrotron x-ray facility. The in-situ measurement indicated that Pr emerged and Cs decreased at some points after D2 gas permeation, though any Pr cannot be observed before D2 gas permeation at all the points on the Pd complex surface. Using small size X-ray beam in 100and 500-micrometer squares, we obtained 2 dimensional XRF spectra for three permeated samples, from which we detected Pr. Pr was detected again by the two small x-ray beams as expected. The amount of Pr varied greatly at different locations of the Pd surface, however, a clear correlation between surface structures and distribution of Pr has not seen up to now. Experimental results suggest that nuclear transmutations do not occur uniformly but some uncertain factors, presumably condensed matter effects in the present Pd/D/CaO system, have a large effect on the rate or the process of the reactions.

OBSERVATION OF NUCLEAR TRANSMUTATION REACTIONS INDUCED BY D2 GAS PERMEATION THROUGH Pd COMPLEXES

We have been studying low energy nuclear transmutations induced by D2 gas permeation through Pd complexes (Pd/CaO/Pd). We presented experimental results at ICCF9 and ICCF10 . In this paper, we report recent progress. Transmutations of Ba into Sm were observed in two cases: with natural Ba on Pd complex samples (a definite result), and with mass 137-enriched Ba (probable). In these experiments, the atomic mass increase was 12 and atomic number increase was 6. One of our experimental apparatuses was carried to SPring-8, which is the world’s largest synchrotron radiation facility, located at Hyogo prefecture in Japan. Pr was confirmed several times by XRF at SPring-8. Some experiments were done to explore physical structure of the CaO layer. According to a D ion beam bombardment experiment performed at Tohoku University, the deuterium density of our Pd complex is one order larger than normal Pd. When we replaced CaO with MgO, we did not obtain any positive results. These results shed light on the role of the CaO layer in the Pd complex.

Relationship between the Li ionic conduction and the local structures in B-site substituted perovskite compounds, (Li0.1La0.3)1+xMxNb1−xO3 (M=Zr, Ti; x=0, 0.05)

Generally, it is known that the activation energy for the Li+ conduction in the perovskite-type oxides such as (Li,La)NbO3 decreases with the expansion of the lattice. However, our previous results showed an increase in the activation energy with Zr doping at B site in spite of lattice expansion. In the present study, the local structure of B site substituted perovskite oxides, (Li0.1La0.3)1+xMxNb1−xO3 (M=Zr, Ti; x=0, 0.05), has been investigated using the extended x-ray absorption fine structure (EXAFS) technique with a view to explore the divergence exerted by Zr-doped perovskites. The EXAFS measurement revealed that the Li+ migration pathway in the Zr-doped samples is subjected to contract due to the local lattice distortion around the Zr-doped site.

Development and application of multi‐purpose x‐ray fluorescence analyzer using synchrotron and conventional x‐ray sources

A multi-purpose analyzer was developed to carry out x-ray fluorescence (XRF) analysis of micro-samples and total reflection x-ray fluorescence (TXRF) analysis of environmental samples using either conventional x-ray or synchrotron radiation as an excitation source. Cosmic dust samples collected in Antarctica were successfully analyzed using a conventional x-ray source. XRF spectra of 36 cosmic dust samples were measured automatically using a combination of specially designed software and a sample holder, and trace amounts of heavy elements (10 ppm level in the sample) were detected. The potential ability of the XRF analyzer in TXRF mode using synchrotron x-rays from a third-generation light source, SPring-8, was tested using a standard river water and arsenic-containing water as samples. Satisfactory linearity of concentration versus net intensity of As was obtained in the concentration range 100 fg–100 ng with a detection limit of 10 fg. Copyright

Stable delivery of nano-beams for advanced nano-scale analyses

Advanced nano-scale analyses such as x-ray absorption fine structure (XAFS), x-ray magnetic circular dichroism (XMCD) spectroscopy and x-ray fluorescence (XRF) with a ~100 nm spatial resolution have been routinely conducted by upgrading two x-ray beamlines BL37XU and BL39XU at SPring-8. The focusing beam size can be varied from 50 nm to 2 μm and high flux achieved at 1012 photons/s/0.01% b.w. with the beam size of 300 × 300 nm2 (full width at half maximum) at 12 keV.

X-ray reflection from a water surface investigated by a new liquid interface reflectometer at SPring-8

X-ray reflection measurement of a water surface was demonstrated using recently developed liquid interface reflectometer at SPring-8. The reflectometer equipped with two-dimensional hybrid pixel array detector, PILATUS, achieved x-ray reflectivity towards 10-9 with the integration time at each angle of only 1 sec, having enormous potential for quick measurements.