問い合わせ番号

INS-0000000352

ABSTRACT

  Beamline BL10XU is dedicated to high-pressure research using diamond anvil cells (DACs). We can perform high-pressure powder x-ray diffraction under the conditions of high-pressure and a wide range of temperature from cryogenic region to thousands of kelvins. A major feature of this beamline is high-brilliance and high-energy X-rays produced from synchrotron radiation source of the in-vacuum type undulator. The monochromatic and focused X-ray beam (6∼61 keV) irradiates a sample enclosed to samples in DACs which enables to generate high-pressures over 300 GPa. The XRD Debye-Sheller rings from sample are collected on an image plate (IP) area detector or an X-ray flat panel detector (FPD), and high speed CdTe hybrid pixel array detector. In experimental stations, cryostats and a double-sided laser heating system (1500∼6000 K) have been prepared to provide the extreme temperature conditions. Combined high pressure generation using DAC and to use the high energy and high brilliance X-ray of SPring-8, users cover a wide range of scientific research fields such as high-pressure condensed matter physics, materials sciences, mineral physics, and Earth and planetary sciences, and specializes in in-situ measurements of material properties under the extreme conditions: determination of crystal structure, pressure-induced structural phase transitions, and equation of state, and the analysis of phase diagram.

X-RAY SOURCE AND OPTICS

  A high-intensity, high-energy, and quasi-monochromatic X-rays beam is supplied from a short-period hybrid in-vacuum type undulator. The undulator beam is monochronized by a Spring-8 standard type double crystal monochromator (DCM) with liquid-nitrogen-cooled, resulting in intense X-rays (>10¹³ photons/s) with a sufficient energy resolution (ΔE/E ∼ 10^-4). The DCM is equipped with Si 111 crystal and Si 220 crystal, which covers X-rays energy to 37 keV and 61 keV, respectively.
The stacked compound X-ray refractive lens (CRL), which are made from glassy carbon or aluminum, are installed at downstream position of 4.3 m from the DCM. The CRL device provides high spatial and angular resolutions (about 10 arcseconds) suitable for X-ray diffraction experiments at sample position.　Using CRL in optics hutch, the X -ray spot size is 0.05 mm (V) × 0.15 mm (H) at sample position (FWHM). About 7 times intensity gain is obtained by CRL when X-rays energy is tuned at 30 keV. Multi-step focusing in combination with a refractive lens installed in the experimental hutch, we can finally provide a micro-beam with a minimum diameter of 0.8 µm (V) × 0.9 µm (H) at the sample position.

Fig. 1. Schematic view of BL10XU optics hutch

• MAJOR FEATURE OF BL10XU

  Available x-ray energy	6 - 61 keV
  Energy resolution	ΔE/E ∼10-4
  X-ray beam size	φ 0.001 - 1.0 mm
  Flux	∼1.0 × 1013 photons/sec (30 keV), ∼1.0 × 1012 photons/sec (61 keV)

EXPERIMENTAL STATIONS

  The equipment for high-pressure x-ray diffraction experiments are installed in a tandem-type experimental hutch in BL10XU. High-pressure study with DACs is conducted utilizing x-ray energies from 6 to 61 keV.

Fig. 2. Integration system of X-ray diffractometer and Raman
scattering for high pressure and low temperature experiments in experimental hutch 1

EXPERIMENTAL HUTCH1

  A low vibration closes cycle GM cryostat and each sample stages designed for the cryostat have been installed to perform high pressure and low temperature XRD measurements with oscillations. A helium gas driven membrane system for a DAC mounted in the cryostat can be used to compress sample in DAC remotely. An on-line Raman spectroscopy system is equipped for pressure measurements at cryogenic temperature. The system consists of a microscope unit with long working distance objective lens and a silver-coated glassy carbon mirror (Fig. 2). The glassy carbon mirror is employed as laser delivery optics and is transparent to high energy x-rays. The Raman system was used with diode laser operating at 532 nm. X-ray diffraction images are collected on an image plate area detector (IP, Rigaku. Co., R-AXIS IV⁺⁺; 300×300 mm²; pixel size 0.1 mm) or a Perkin Elmer digital X-ray flat panel detector (FPD, XRD0822 CP23; 1024×1024 pixels; 0.2 mm pixel pitch). The camera distance between a sample and the detector is tunable between 220 and 540 mm and between 200 and 450 mm, depending on a measuring range of diffraction angle and an angular resolution.

EXPERIMENTAL HUTCH2

  High-pressure X-ray diffraction study can be carried out using laser-heating system and micro X-ray beam. Incident x-ray optics, a diffractometer for DACs, a stage for X-ray detectors, and laser heating optics have been installed, which are mounted on independent optical tables (Fig. 3). The optical tables on which the incident x-ray optics and laser heating optics are mounted have Y-Z translation stages (X axis is along the X-ray beam), allowing to precisely aligning these optics to X-ray beam position. The sample stage system, which consists of high-precision and high-load X-Y-Z translation and rotation stages, is designed for mounting the variable DACs (e.g., a cube type DAC for ultra-high- pressure experiments and a symmetric piston-cylinder type DAC for laser heating).

Fig. 3. High-precision diffractometer system for high-pressure x-ray
diffraction experiments equipped in the experimental hutch 2.

  The XRD Debye rings are collected on the Rigaku image plate area detector (IP, R-AXIS IV⁺⁺; 300×300 mm²; pixel size 0.1 mm), the Perkin Elmer digital x-ray flat panel detector (FPD, XRD0822 CP23; 1024×1024 pixels; 0.2 mm pixel pitch). Depending on experimental situations, two kinds of detectors can be selected: IP and FPD are used for collecting accurate diffraction data with high-resolution and for high-speed X-ray data collection, respectively. The sample-to-detector distance for IP and FPD can be shifted between 200 and 450 mm and between 200 and 430 mm, respectively. High speed CdTe hybrid pixel array detector (LABMDA CdTe 750k, X-Spectrum GmbH; pixel size 55 µm×55 µm, detector pixels 512×1528) is also prepared. On the detector stage, a microscope unit is equipped to observe samples in DACs and to align the sample to X-ray beam. The microscope unit can also be used as Raman probe head for on-line pressure measurements and Raman spectroscopy measurement.
　A double-sided laser heating system with near-infrared fiber lasers is installed for high-pressure and high-temperature X-ray diffraction experiments to understand mineral physics of deep Earth materials and to synthesize new high-pressure materials. Fig. 4 shows the laser heating system for DACs installed in the BL10XU. The glassy carbon mirror with Ag-coated is employed to deliver the laser to the sample in the DAC and is transparent over 90% for high-energy x-ray above 30 keV. For the purpose of generating high temperature above 5000 K at high pressure, double 100 W SPI fiber lasers have been installed since 2008. The laser spot size at the sample is tunable in the range of 10 to 50 µm.

Fig. 4. The optics of double-sided laser heating and temperature
measurements in the experimental hutch 2

　Also in hutch 2, the low-vibration helium closes cycle GM cryostat have been installed to low temperature X-ray diffraction experiments using micro focused beam. A helium gas driven membrane system for the DAC mounted in the cryostat can be used for remotely applying pressure on a sample in the DAC.

DATA EVALUATION SOFTWARE

The IP detector, R-AXIS IV⁺⁺, and the FPD are operated using an X-ray diffraction data acquisition software designed by Rigaku Co. and a programming software in LabVIEW, respectively.
Sample and detector stages and optics for Raman spectroscopy system and laser heating system can be controlled from LabVIEW software.
For Raman data acquisition and processing, Teledyne Princeton Instruments LightField software is installed.

EQUIPMENT HIGHLIGHTS

• Image plate area detector
• X-ray flat panel detector
• CdTe hybrid pixel array detector
• Micro Raman spectroscopy system for pressure measurements (on-line): 532 nm (hutch 1, 2) and 633 nm (hutch 2) diode lasers
• Electrical resistance measurement system
• Energy-domain ⁵⁷Fe-Mössbauer spectroscopy system
• Cryostat and thermostat (7 K ∼)
• Double-sided laser heating system (1500 ∼ 6000 K)
• Multi-channel collimator system for XRD
• Diamond anvil cell (Bring your own)
• Sample preparation room in experimental hall
• Microscopes with Raman scattering probe
• Electric discharge-drilling machine (EDM)
• Ruby fluorescence system for pressure measurement (off-line): 488 mm diode laser
• Micro Raman spectroscopy system for pressure measurements (off-line): 785 nm diode laser
• Micro Raman spectroscopy system (off-line): 532 nm diode laser

PUBLICATION SEARCH

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BL10XU PUBLICATION SEARCH

CONTACT INFORMATION

Please note that each e-mail address is followed by "@spring8.or.jp."

Hirokazu KADOBAYASHI
Japan Synchrotron Radiation Research Institute (JASRI)
1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198
Phone : +81-(0)791-58-0833
Fax : +81-(0)791-58-0830
e-mail : kadobayashi

Sho KAKIZAWA
Japan Synchrotron Radiation Research Institute (JASRI)
1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198
Phone : +81-(0)791-58-0833
Fax : +81-(0)791-58-0830
e-mail : kakizawa

Saori KAWAGUCHI
Japan Synchrotron Radiation Research Institute (JASRI)
1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198
Phone : +81-(0)791-58-0833
Fax : +81-(0)791-58-0830
e-mail : sao.kawaguchi