High-Throughput X-Ray Powder Diffractometer

◆Equipment overview

It is possible to obtain powder diffraction measurements of materials such as polycrystals. Data can be obtained with a small amount of trace mg powder samples. In addition, a feature of the industrial use BLs is a robot that is available to make fully automated measurements, and the device configurating is compatible with many sample environments desired by the user.

◆Features of the Equipment

A high-throughput powder diffractometer is installed in the BL19B2 beamline’s first experimental hatch. MYTHEN, an original photon counting, 1-dimensional semiconductor detector, is arranged in 12 pieces in the angle equal to the diffraction angle. One exposure covers a 2θ diffraction angle of a range of 80°, and a resolution angle of 0.005°. To control the device, an original GUI has been developed for the input language SPEC, and is straight forward to allow first-time users to immediately understand the experimental methods. Almost all data collection operations, such as sample exchanges and sample positioning, are automatically completed using robots. While the sample is being irradiated by the X-rays, the beam size has a length of 0.3mm and a width of 3mm, and through a thin, glass capillary, the powder samples can be measured. The available X-ray energy is 7-37keV.

◆Equipment accessories

By spraying a glass capillary with low or high temperature Nitrogen gas, the temperature of the sample changes and can be measured while changing.
The low temperature devices cover 100 to 500K, and the high-temperature devices cover everything from room temperature to 1000K. The temperature change devices are linked with the sample exchange robot, and once the sample is prepared, the temperature change measurement data can be obtained fully automatically.
In addition, for samples that are difficult to powder, a special sample stage with a three-axis simultaneous shake mechanism is available. This can be used for difficult to powder samples, such as bulk metal samples with large crystal grains, to obtain powder diffraction profiles that can be used to analyze the crystal structure.
In addition, for reflection arrangement measurements on flat plate samples that cannot be tested with transmission arrangements, a multi-solar slit system can collect data with very high angular resolution.
This such robot is designed to be used for various purposes other than fully automated measurements. Please ask the person in charge of the beamline for more information.

◆Experiment / sample preparation

During the experiment, the glass capillary and the sample are both irradiated with X-rays, and the background scattering is observed.
It is necessary to use different materials and size depending on the objective of the experiment.
First, it is recommended that the material be made of “Lindeman Glass”, which is thin and limits X-ray scattering.
However, Lineman glass becomes soft at high temperatures so for experiments above 500℃, please use “borosilicate glass”, “soda glass” or “quartz glass”.
Quartz glass has the highest temperature resistance, but the disadvantage is that the shape of the background is complex, so its use should be contemplated carefully.
The standard inner diameter of the capillary is 0.3mm, but increases and decreases under the influence of X-ray absorption.
In addition, since most of the experiment is completed by a robot, the progress of sample preparation is done quickly.
Therefore, it is recommended that the preparation work for filling the glass capillaries with powder be completed before coming to the office. Consequently, it is recommended that the preparation work of filling the glass capillary with powder be completed before entering the office. Also, if there is a concern about sample oxidation or deterioration while taking temperature change measurements, the capillary should be filled with inert gas or sealed.
For information on powder filling and operation of the sample holder, please refer to the first half of the video in the URL below.
https://support.spring8.or.jp/powder/jukebox.html

◆Experimental procedure / precautions

With fully automated measurements using the robot, first fill the capillary with powder, then attach to the sample holder dedicated to the device.
Easy-to-handle mounting jigs are available, which can each be assembled within 1-2 minutes.
Up to 100 sample holders can be mounted to a single robot.
Sample selection and exposure conditions are entered into a Microsoft Excel spreadsheet.
It is recommended that screening measurements of 1 minute per 1 sample is used to obtain high precision data with high statistical accuracy.
By looking at this result, you can determine the exposure conditions (exposure time) to obtain sufficient statistical accuracy for the data analysis you wish to perform.
Also, if necessary, glass capillary data (empty) should be measured.
When measuring temperature changes due to gas spraying, exposure time, the sample’s temperature stability and the time for the gas to change temperature should all be accounted for.
Temperature change measurements take at least 2 times longer than room temperature measurements, since they rely on several points to determine the rate of change.
In addition, for temperature changes, if overcooling or overheating affects the condition of the sample, it is possible to set a change rate so overshooting does not occur.
The conditions of these devices can also be controlled by entering them in a Microsoft Excel sheet.

◆Contact

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◆List of representative treatises

“New perovskite-related structure family of oxide-ion conducting materials NdBaInO4”
K. Fujii, Y. Esaki, K. Omoto, M. Yashima, A. Hoshikawa, T. Ishigaki, and J. R. Hester
Chem. Mater., 26, 8, (2014) 2488?2491
DOI：10.1021/cm500776x

“Quantitative analysis of heavy elements and semi-quantitative evaluation of heavy mineral compositions of sediments in Japan for construction of a forensic soil database using synchrotron radiation X-ray analyses”
I. Nakai, S. Furuya, W. Bong, Y. Abe, K. Osaka, T. Matsumoto, M. Itou, A. Ohta and T. Ninomiya
X-ray spectrometry 43, (2014) 38-48
DOI : 10.1002/xrs.2496

"Effect of Annealing on Crystal and Local Structures of Doped Zirconia Using Experimental and Computational Methods"
T. Itoh, M. Mori, M. Inukai, H. Nitani, T. Yamamoto, T. Miyanaga, N. Igawa, N. Kitamura, N. Ishida, and Y. Idemoto
The Journal of Physical Chemistry C 119 (16), (2015) 8447-8458
DOI：10.1021/jp5117118

"Crystalline-Amorphous-Crystalline Transformation in a Highly Brilliant Luminescent System with Trigonal-Planar Gold(l) Centers"
K. Igawa, N. Yoshinari, M. Okumura, H. Ohtsu, M. Kawano and T. Konno
Scientific Reports 6, (2916) 26002
DOI：10.1038/srep26002

"Versatile High-Throughput Diffractometer for Industrial Use at BL19B2 in SPring-8"
K. Osaka, Y. Yokozawa, Y. Torizuka, Y. Yamada, M. Manota, N. Harada, Y. Chou, H. Sasaki, A. Bergamaschi, and Masugu Sato
AIP Conference Proceedings 2054, (2019) 050008
DOI : 10.1063/1.5084626