Photon Factory Activity Report 2005 #23 Part B (2006)
Materials Science15A/2005G222

Development of in-situ DSC-SWAXS system for metallic alloys- a preliminary test
Hiroshi OKUDA1*, Isao MURASE2 Shojiro OCHIAI1, Mikio OHTAKA2
1
IIC Kyoto University, Sakyo-ku, Kyoto 606-8501, Japan
2
Grad. School of Mater.Sci. Kyoto University, Sakyo-ku Kyoto 606-8501, Japan
Introduction
Diffusional phase transformation process in multicomponent alloy systems is one of the major researchsubjects in the development and control ofmicrostructures in metallic or oxide materials. In order toexamine microstructural stability of glass materials,
understanding crystallization process of the glassy
materials and supercooled liquids is quite important.
However, the stability of these glasses or liquids dependon the thermal hysteresis or environments such as trace
impurity of oxygen etc. Therefore, we need an in-situ andsimultaneous measurements of thermal properties andstructural properties in order to obtain reliable
relationship between relaxation / glass transition/
crystallization or precipitation processes. For lower
temperatures with moderate sensitivity, commercial
DSC/SAXS cell is readily available. However, theseproducts are not suitable for the phase transition of
metallic glass where the change in heat capacity is rather
small and the temperature should be higher. Therefore, wehave attempted to develop an in-situ DSC/SWAXS
system applicable to experiments on phase transformation
processes in metallic materials.
Experimental
The in-situ DSC/SWAXS apparatus developed in thepresent proposal has several points that are different fromordinary commercial DSC-SAXS cells. One is that theDSC cell part is a modified version of commercial highsensitivity DSC, originally designed for inorganic
materials up to about 800 K with enough sensitivity toevaluate glass transition temperature of bulk metallic
glasses. To maintain sensitivity and high-temperature use,the DSC cell was designed to be used in the verticalalignment. Therefore, it requires that the X ray should beintroduced from bottom window, goes through thethermopile units and DSC pan, then the direct /scatteredand diffracted beams go out of the upper window. Two
one-dimensional PSPCs are to be used in the presentsystem, one for SAXS and the other for WAXS. The DSC
unit is leak-tight and can be evacuated during the scan. At
the beam-line 15A, the incident beam was diffracted
upward with a Ge 111 flat single crystal wafer. Diffraction
condition of Ge 333 was used to orient the beam upwards.
Since the wavelength of the incident X-ray is 0.15 nm at
BL15A, the diffracted beam, along with the offset angle
given by a front mirror, is ideally vertical in the present
condition.

150

Users' Report

Figure1 gives a photograph of the DSC/SWAXS
system used in the present test. The stage was installed
close to the focal point of the incident beam to produce asmall diffracted beam.
Present test revealed that some improvement on theDSC cell structure was necessary for quick setup of theapparatus in this crowded beamline. For this purpose, a
new configuration of thermocouples with larger angle ofacceptance in DSC cell is now under fabrication, andplanned to be used for the in-situ experiment in thesecond term of 2006.

References[1]H.Okuda et al., Mater. Sci. Forum, in press.
*okuda@iic.kyoto-u.ac.jp

Fig.1 Photograph of the in-situ DSC-SWAXS
apparatus installed at the back end of BL-15A.
The incident beam is diffracted verticallyupwards, goes through the DSC cell and thenenter the SWAXS chamber.