Photon Factory Activity Report 2005 #23 Part B (2006)
Materials Science

4A/2005C016

Characterization of nanometer-sized metal particles embedded in thin film bymicrobeam grazing incidence small angle x-ray scattering (µGISAXS)techniqueKazuhiro TAKADA1, Taihei MUKAIDE1, Takashi Noma1, Atsuo IIDA2
1CANON Research Center, Shimomaruko, Tokyo 146-8501, Japan
2
KEK-PF, Tsukuba, Ibaraki 305-0801, Japan
Introduction
Recently nanometer-sized metals are interested becauseof their characters. By controlling the characters (size,size distribution etc.) of particles embedded in thin films,
we can obtain the thin films which have various physicalproperties. To produce such a thin film, it is important toknow the detail structures of the films.
Grazing incidence small angle X-ray scattering(GISAXS) technique [1-2] is effective method to evaluate
the structure and morphology of the nanometer-sizedparticles or the nanostructures. So it is ideal to know themetal particles characters. By controlling the incident
angles, we can evaluate the depth-controlled informationof the nanostructures. However under the grazing
incidence condition, the irradiated areas of x-rays becomelarge. Using GISAXS combined with X-ray micro-beam(µGISAXS), it is possible to restrict the irradiated areas
about few micrometer size in lateral direction even under
the grazing incidence condition. So µGISAXS is suitableto evaluate the structures of practical devices. In thisstudy, we have investigated mainly the distribution of themetal particles embedded in thin film.
Experiment
The experiment was done using standard micro-beam
setup at BL-4A. The X-ray energy was 8keV. The X-ray
micro-beam size was set to 4µm×5µm by Kirkpatric-Baez
system. The scattered intensity was measured by animage intensified X-ray CCD camera (C4880-80
Hamamatsu photonics K.K.) or Imaging Plate. Thevacuum path was inserted to reduce air scattering between
the sample stage and detector. The sample to detector
distance was set about 1400mm. The half transmitted
specular beam stop was set in front of the detector.
We confirmed beforehand that µSAXS optics have aresolution about 60nm in transmission mode. The
measurement was done by changing the incident angles.
The incident angles were changing from 0.2°(lower than
the total external reflection angle; αc) to 0.6° (higher thanαc), so we measured the depth information of the metalparticles. The sample was thin film in which nano-meter
sized metal(= gold, silver) embedded.

of Fig1(a) shows that the metal particles are uniformlydistributed. The pattern of Fig1(b) shows the interference
reflections of the film thickness. From these data, it ispossible to estimate of information about the metal byusing the technique of local monodisperse approximation(LMA)[3].

(a)
qz
qy

(b)
qz
qy
Fig.1 Typical µGISAXS patterns of the (a) gold
embedded film obtained with an incident angle α=0.3°.
(b) silver embedded film obtaioned with an incident angle
α=0.3°.

References[1] D.Babonneau et.al., Appl. Phys. Lett. 76,2892(2000).
[2] H.Okuda et.al., Appl.Phys.Lett. 81,2358(2002).
[3] J.S.Pedersen, J.Appl.Cryst. 27,595(1994).
* takada.kazuhiro@canon.co.jp

Results and Discussion
Typical µGISAXS patterns are shown in Fig1. At thesmall angle region, the scattering from the metal particles,
the specular beam which intensity was attenuated andYoneda wing are observed. The X-ray scattered pattern

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