SPring-8, the large synchrotron radiation facility

Inquiry number

SOL-0000001008

Beamline

BL20XU (Medical and Imaging II)

Scientific keywords

A. Sample category	inorganic material, research on method, instrumentation
B. Sample category (detail)	ferroelectric material, insulator, ceramics, solid-state crystal
C. Technique	fluorescent X-rays
D. Technique (detail)	trace-element, diffraction, scattering
E. Particular condition	microbeam (1-10 µm), 2D imaging
F. Photon energy	X-ray (4-40 keV)
G. Target information	dislocation, strain, function and structure, function, elemental composition

Industrial keywords

level 1---Application area	electric component, cell (battery)
level 2---Target	condenser, fuel cell
level 3---Target (detail)	electric rod
level 4---Obtainable information	crack, crevice, structure, molphology
level 5---Technique	imaging

Classification

A80.10 electronics, A80.12 semiconductor, A80.30 inorganic material, A80.36 electrochemistry

Body text

A hard x-ray scanning microscope opens the possibility of combining x-ray imaging and the chemical species analysis. We have performed an element (Sr) mapping of dielectric ceramics BaTiO₃/SrTiO₃ with fluorescent x-ray using microbeam being developed. The microscope experiment was performed at the end station of beamline 20XU using the sputtered-sliced zone plate as a focusing element.
Two kinds of samples (composite ceramics of BaTiO₃/SrTiO₃ = 9 : 1 were prepared. One was prepared using the spark plasma sintering (SPS) or pulse electric current sintering. SPS is make use of microscopic electrical discharge between particles under pressure of 30-50 MPa and electric current of 4000A. This process enables a compact powder to be sintered to a high density in much shorter sintering periods, 3 minutes compared with the conventional sintering process. The short sintering periods is advantageous in suppressing exaggerated grain and chemical reaction between the grains. The other was the conventional sintering (CS) method. For CS process the mixed BaTiO₃/SrTiO₃ = 9 : 1 powder was pressed into a pellet and sintering in air at pressure 190 MPa and at a temperature 1300C for two hours.
Two dimensional mapping of Sr atom for the SPS and the CS were made. Fig.1 shows the scanning micrographs of the SPS and the CS respectively, where white area denotes high Sr content. In the SPS the area boundaries are clear, and SrTiO₃ particles seem to be more localized. In the CS the boundary among white, gray and black are not clear, and SrTiO₃ particles seem to be distributed homogeneously.

Source of the figure

Bulletin from SPring-8

Bulletin title

ユーザーレポート2003B

Page

118

Technique

The BL20XU is suitable for microbeam experiment because of spatially coherent X-ray beam using long (248 m) beam transport path. In this experiment, a sputtered-sliced Fresnel zone plate is used as a beam focusing element, and micrometer-resolution mapping in high energy X-ray region becomes possible.

Source of the figure

No figure

Required time for experimental setup

2 shift(s)

Instruments

Instrument	Purpose	Performance
Multi-purpose high-precision diffractometer	micro-focusing
Beam-monitor 2	alignment of optics	4.3 µm pixel size
Sputtered-sliced zone plate	beam focusing element

References

Related experimental techniques

Questionnaire

The measurement was possible only in SPring-8. Impossible or very difficult in other facilities.

Ease of measurement

Middle

Ease of analysis

Easy

How many shifts were needed for taking whole data in the figure?

Two-three shifts