Experimental Techniques

• X-ray Powder diffraction
• Two-dimensional X-ray diffraction mapping
• Surface X-ray diffraction (Advanced measurement)
• In-situ X-ray diffraction (Advanced measurement)

Overview

This is a hutch equipped with a general-purpose X-ray diffractometer. Powder diffraction measurements of samples enclosed in capillaries are possible using a capillary spinner for powder diffraction and a two-dimensional detector (standard measurement). You can apply the mail-in measurements.
Furthermore, users may bring their own sample environment to be mounted on the general-purpose sample stage for in-situ measurements.
Usable gases are limited to harmless gases such as N₂ and CO₂. If users bring their own sample cell and set it up themselves, it will be considered a standard measurement. However, if a sample cell is required, we recommend conducting collaborative experiments with Professor Maiko Nishibori of SRIS, Tohoku University as an advanced measurement.

Beam Characteristics

Energy

17.5 keV or 28.5 keV
*Please note that switching energy during beam time is not recommended.

Flux

2.5x10¹¹ cps (calculated value)

Beam size

120 µm(Horizontal)、70 µm(Vertical)

Hutch size

Approx. 3m (optical axis direction) x approx. 2m (width) x approx. 3.3m (height)　

Light Source and Optics

The branchline for XRD measurement provides monochromatized X-rays. A white X-ray beam generated by a 5-pole multipole wiggler light source is monochromatized using Bragg reflection from a Si crystal and is split off-axis from the original beam. The X-ray energy can be selected by choosing either the Si111 or Si220. Focusing is performed by a bent cylindrical mirror.

Experimental Station

Experimental Equipment

[Spinner for powder samples]
Sample-to-detector distance : approx. 240 to 890 mm
Measurement range : 2Θ < 50 degrees

Powder and liquid samples can be sealed in a capillary
【Example of how to prepare a capillary sample】
The sample holder is equivalent to those of SPring-8 BL19B2 and AichiSR BL5S1.
Temperature control and automatic alignment mechanisms are under consideration.

· Regarding the "capillary spinner for powder samples," the rotation axis alignment is currently    manual.
· Analysis software, including that for the "Rietveld method," is not installed.
· Both 17.5 and 28.5 keV energies are available. 17.5 keV is the default, and 28.5 keV can be    accommodated upon request. Please specify your desired energy when requesting beamtime.
· Switching energy during beamtime is not recommended (reason: it takes time for the crystal to    stabilize after switching).
· Measurement of standard samples when switching between the above energies must be    performed within your allocated beamtime. (PhoSIC will not measure standard samples or provide    data after the allocated beamtime)
· Three types of cables (BNC, LAN, USB) are provided for user use, running from the inside to the    outside of the XRD experimental hutch, one of each type. If you wish to use them, please inform us    when requesting beamtime. Please note that in the case of USB cable connection, operation may    not be guaranteed depending on your device, so please understand this in advance and consider    any necessary countermeasures.

Other information

[Large Area IGZO Flat Panel Detector]
Hamamatsu Photonics C14406DK-2918

> Detection area: 430 x 430 mm
Pixel size: 140 µm²
Scintillator: Directly deposited CsI
Frame rate: Maximum 15 fps (full frame)
Dynamic range: 87 dB

Detector

[Sample X-Z Stage for In-situ Experiments]
Optional theta and swivel stages are available.

Sample-to-detector distance: approx. 100-580 mm
Kohzu Seiki XA10A and ZA10A (approx. 100 mm from the stage top surface to the X-ray beam).
Two-dimensional X-ray diffraction mapping is possible (Beam size of horiz. 120 µm and vert. 70 µm).

Layout

With spinner (detector at the closest position)

During in-situ experiments (detector at the furthest position)