実験報告書様式（一般利用課題・成果公開利用）（ ※本報告書は英語で記述してください。ただし、産業利用課題として採択されている方は日本語で記述していただいても結構です。 ）提出日 Date of Report

Experimental Report

2013/1/7

課題番号 Project No.

装置責任者 Name of responsible person

2012A0091

武田 全康

実験課題名 Title of experiment

装置名 Name of Instrument/（BL No.）

Combined assessment of polymer - magnetic nanoparticle films by

写楽（１７）

diffuse scattering/GISANS and GISAXS

実施日 Date of Experiment

実験責任者名 Name of principal investigator2012.11.6-8

奥田浩司 Hiroshi Okuda
所属 Affiliation
京大工 Dept.Mater.Sci.Eng, Kyoto University
試料、実験方法、利用の結果得られた主なデータ、考察、結論等を、記述して下さい。（適宜、図表添付のこと）
Please report your samples, experimental method and results, discussion and conclusions. Please add figures andtables for better explanation.
1. 試料 Name of sample(s) and chemical formula, or compositions including physical form.
Fe3O4 nanoparticle dispersed Polystylene film cast on Si substrate

2. 実験方法及び結果 （実験がうまくいかなかった場合、その理由を記述してください。）
Experimental method and results.

If you failed to conduct experiment as planned, please describe reasons.

Experimental:
Sample was made from Fe3O4 magnetic nanoparticle having 15 nm of diameter and toluene solution ofpolystylene spin-cast on a 2inchi Si substrate. To measure the scattering intensity along qy directions aroundthe Yoneda peak, the sample alignments was set with 90 degree rotation from standard reflectivity
measurement setting, i.e., the sample normal is set parallel to the vertical direction.
From the intensity assessment check made at the first beamtime in July, the slit in the qz direction was kept
open for upper bound to gain as much neutrons available, since we are interested in the in-plane nanostucturein the present measurements. The second measurements were made for two days.
Owing to the scan direction necessary for the present one, alignment of the sample took more timecompared to the standard reflectivity. One major point is that X-ray does not penetrate through the substrate,
but neutron easily does, so that the alignment procedure was found to be quite differenct from what we usually
do at synchrotron facilities. The above two points made us use much time to fix the measurement condition

12. 実験方法及び結果（つづき） Experimental method and results (continued)
than we first anticipated.
Preliminary measurement with X-rays
Figure 1 shows the prelinary GISAXS measurements made at Phoron Factory, BL06A station before the first
beamtime of neutron. It shows a well defined interparticle
intereference peak at about qy=0.5 nm-1 along the
Yoneda peak and a strong diffuse scattering in the qz
direction at qy=0. With a II-CCD, with high sensitivity andless dynamic range the exposure time was about a coupleof seconds, and with Pilatus, it can be extended to 20
seconds for better statistics. To confirm that the film
structure is uniform over the substrate, the X-ray wasscanned across the sample with a beamsize of about 0.8
mm. The pattern was confirmed to agree well in thecentral area that we scanned in the present measurement, forFig.1 GISAXS profile with IICCD

about 1.5 inches. The magnetization curve obtained with SQUID

obtained at Photon factory for theshowed that the magnatization almost saturated at the field ofsame

samplemeasuredinthepresent beamtime.
about 1kOe(80%), although the signal is very
weak and diamagnetic component from Si
substrate was dominantly strong..
Figure 2 gives the present results with neutrons,
averaged over the wavelength between 0.5 and 8
angstroms. A well-defined peak at the qy
corresponding to the interparticle interference in
the GISAXS pattern was recognized in thepresent GISANS measurements. The intensity
increase at lower qy observed in the GISAXS,
corresponding to the larger heterogeneity of thefilm, yet much smaller than the scale checkedwith scanning GISAXS, was not observed in the present

Fig.2 GISANS profile in the qy

condition. As seen in the figure, the present profile suggests

direction

thewavelengththat the scattering intensity is strongly enhanced at some of

between 0.5 and 8 A.

Vertical and

the

the

in-plane denotes the direction ofenhancement depends on the films structure of the sample

magnetic field applied to the sample.

that gives dynamical effects, requiring reflectivity data.

The intensity was summed with the

Further analysis is under way on this viewpoint.

wavelength resolution of about 10%

wavelengths.

The

energydependence

of

2

using