Satoshi Koizumi

Beyond simple small-angle X-ray scattering: developments in online complementary techniques and sample environments

Possibilities in auxiliary technique combinations with small- and wide-angle X ray scattering are described, as well as more complicated sample environments used in X-ray and neutron scattering.

Contrast variation by dynamic nuclear polarization and time-of-flight small-angle neutron scattering. I. Application to industrial multi-component nanocomposites

Contrast variation small-angle neutron scattering by dynamic nuclear polarization is applied to industrial multi-component nanocomposites.

Multi-tube area detector developed for reactor small-angle neutron scattering spectrometer SANS-J-II

A newly developed multi-tube area detector for a small-angle neutron scattering (SANS) spectrometer (SANS-J-II) at the research reactor JRR-3 in Tokai, Japan, has been implemented via the use of one-dimensional position-sensitive 3He detectors (tubes). Ninety-six active tubes of 8u2005mm in diameter and 650 and 580u2005mm in length were filled with 15u2005atm (1.52u2005MPa) of 3He and aligned vertically parallel in order to cover a sufficiently large area for small-angle scattering measurement. These tubes are enclosed in an air chamber together with neutron encode and GATENET modules (VME boards), which compose a standard data acquisition system for the spallation neutron source of the Japan Proton Accelerator Research Complex. This system facilitates the acquisition of time-of-flight neutron event data. The multi-tube detector is mounted on a truck moving in a vacuum chamber of the SANS spectrometer. After discriminating noise originating from γ-rays, and calibrating the positions and sensitivities of individual tubes, the resolution was determined (i.e. channel widths along parallel and vertical directions along a tube). The counting rate of one tube was determined to be 1.4 × 103 counts per second with a counting loss of 1%. This implies that the new detector, composed of 96 tubes, can detect more than 105 neutrons per second with a counting loss of 1%. To demonstrate its use, small-angle scattering originating from a diblock copolymer film with a highly oriented lamellar microdomain was observed. The data acquisition in event mode has a great advantage in time-resolved measurements that are synchronized with external stimuli imposed on a sample.

Preparation of Robust Metal‐Free Magnetic Nanoemulsions Encapsulating Low‐Molecular‐Weight Nitroxide Radicals and Hydrophobic Drugs Directed Toward MRI‐Visible Targeted Delivery

With a view to developing a theranostic nanomedicine for targeted drug delivery systems visible by magnetic resonance (MR) imaging, robust metal-free magnetic nanoemulsions (mean particle size less than 20u2005nm) consisting of a biocompatible surfactant and hydrophobic, low molecular weight 2,2,5-trimethyl-5-(4-alkoxy)phenylpyrrolidine-N-oxyl radicals were prepared in pHu20057.4 phosphate-buffered saline (PBS). The structure of the nanoemulsions was characterized by electron paramagnetic resonance spectroscopy, and dynamic light scattering and small-angle neutron-scattering measurements. The nanoemulsions showed high colloidal stability, low cytotoxicity, enough reduction resistance to excess ascorbic acid, and sufficient contrast enhancement in the proton longitudinal relaxation time (T1 ) weighted MR images in PBS in vitro (and preliminarily in vivo). Furthermore, the hydrophobic anticancer drug paclitaxel could be encapsulated inside the nanoparticles, and the resulting paclitaxel-loaded nanoemulsions were efficiently incorporated into HeLa cells to suppress cell growth.

Small angle neutron scattering data of polymer electrolyte membranes partially swollen in water.

In this article, we show the small-angle neutron scattering (SANS) data obtained from the polymer electrolyte membranes (PEMs) equilibrated at a given relative humidity. We apply Hard-Sphere (HS) structure model with Percus–Yervick interference interactions to analyze the dataset. The molecular structure of these PEMs and the morphologies of the fully water-swollen membranes have been elucidated by Zhao et al. “Elucidation of the morphology of the hydrocarbon multi-block copolymer electrolyte membranes for proton exchange fuel cells” [1].

In situ observation of water in a fuel cell catalyst using scanning electron microscopy

To visualize water in the catalyst of polymer electrolyte fuel cells (PEFCs), backscattered electron (BSE) imaging by means of scanning electron microscopy was employed. To confine a wet specimen of catalyst, an environmental wet cell was manufactured with a silicon nitride thin film (∼100 nm) as the beam window. By supplying humidified gas into the cell, a change in BSE brightness was detected in the catalyst attached to the silicon nitride window. As humidification proceeded, the BSE image became darker and returned brighter by switching to a dry gas. Monte Carlo simulations were performed to evaluate the energy and number of BSE obtained after passing through water with thickness d. Combining the results of the Monte Carlo simulation successfully converted the change in brightness to the change in thickness from d = 100 nm to d = 3 μm. This established method of evaluating water with a thickness resolution of the order of Δd = 100 nm can be applied to in situ observations of the catalyst in a PEFC during operation.