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BL10XU OUTLINE

Inquiry number

INS-0000000352

ABSTRACT

  Beamline BL10XU is dedicated to high-pressure research in a high-pressure apparatus of diamond anvil cells. We can perform high-pressure powder x-ray diffraction analysis under the conditions of high-pressure and a wide range of temperature from cryogenic region to thousands of kelvin. A major feature of this beamline is high-brilliance and high-energy X-rays produced from synchrotron radiation source of the short-period hybrid in-vacuum type undulator. The monochromatic and focused X-ray beam (14 ∼ 61 keV) irradiates a sample enclosed in a diamond anvil cell (DAC) which enable to generate high-pressures over 300 GPa. The diffracted X-ray image from the sample is collected on imaging plate (IP) area detector or X-ray flat panel detector. In experimental stations, the extreme conditions of cryogenic or high temperature are realized by using a cryostat (10 ∼ 300 K) or a double-sided laser heating system (1500 ∼ 6000 K), respectively. This beamline covers a wide range of scientific research fields such as high-pressure condensed matter physics, material 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.

AREA OF RESEARCH

  • Structure analysis and phase transitions under ultra high pressure (DAC experiment)
  • Earth and planetary science

KEYWORDS

  • Scientific field
    High pressure, Pressure induced structural phase transition, Phase diagram, Equation of state, X-ray diffraction, Earth and planetary science
  • Equipment
    Diamond anvil cell, Imaging plate, X-ray CCD, Cryostat, Laser heating, Ruby fluorescence method, X-ray refractive lens

X-RAY SOURCE AND OPTICS

  In beamline BL10XU, a high-intensity, high-energy, and quasi-monochromatic SR beam is based on a short-period hybrid in-vacuum type undulator. The undulator beam is monochromatized by a liquid-nitrogen-cooled SPring-8 standard double crystal monochromator (DCM), 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. As x-ray focusing device, a stacked compound x-ray refractive lens (CRL) is installed at downstream position of 4.5 m from the DCM. The advantages of CRL are easy alignment and operation, effective use for collimating or focusing in wide range of high-energy x-ray beam, high X-ray transmission, and in-line optics. The CRL device provides successful angular collimation of the X-ray beam from the undulator, resulting in high spatial and angular resolutions suitable for x-ray diffraction experiments and enhancement at the sample position. The x-ray spot size is 0.05 mm (V) × 0.15 mm (H) at sample position (FWHM). About 5 times intensity gain is obtained by CRL when x-rays energy is tuned at 30 keV. The divergence of focused beam is very small, about 10 arc seconds, giving high resolution for X-ray powder diffraction measurements using DACs. Since the initial installation of the CRL in the optics hutch at BL10XU, the CRL has been upgraded to effect significant improvements and optimization of high-pressure X-ray diffraction experiments: first, plastic (poly-methyl methacrylate, PMMA: (C5H8O2)n) CRLs were installed in 1999, next, beryllium CRLs were used in 2002, and now, glassy carbon (GC) CRLs have been in use since 2007.

Fig. 1.  Schematic view of BL10XU optics hutch

Fig. 1. Schematic view of BL10XU optics hutch

Fig. 2 Schematic layout of high pressure research beamline BL10XU

Fig. 2 Schematic layout of high pressure research beamline BL10XU

  • MAJOR FEATURE OF BL10XU

    Available x-ray energy 14 ~ 61 keV
    Energy resolution ΔE/E ∼ 10-4
    X-ray beam size φ 0.002 ∼ 1.0 mm
    Flux density ∼ 1.0 × 1013 photons/sec/mm2

EXPERIMENTAL STATIONS

  The equipment for high-pressure x-ray diffraction experiments, such as X-ray optics and diffractometers, are installed in a tandem-type experimental hutch in BL10XU (Fig.2). High-pressure study with DACs is conducted utilizing x-ray energies from 14 to 61 keV.

Fig. 3. Integration system of X-ray diffraction diffractometer and Raman scattering for high pressure and low temperature experiments in experimental hutch 1

Fig. 3. Integration system of X-ray diffractometer and Raman
scattering for high pressure and low temperature experiments in experimental hutch 1

  In upstream experimental hutch 1, a low vibration closes cycle cryostat and the high load capacity one-circle diffractometer designed for the cryostat have been installed to perform high pressure and low temperature experiments. A helium gas driven membrane system for a DAC mounted in the cryostat can be used to remotely applying pressure on a sample in the DAC. On-line Raman spectroscopy system as optics 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. 3). 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 imaging plate area detector (IP, Rigaku. Co., R-AXIS IV++; 300 × 300 mm2; pixel size 0.1mm) 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 600 mm, depending on a measuring range of diffraction angle and an angular resolution. The Brillouin scattering measurement system can be also installed by switching the diffractometer for the cryostat in the experimental hutch 1.

In upstream experimental hutch 2, high-pressure x-ray diffraction study can be carried out using laser-heating system for high temperature generation 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 equipped, which are mounted on independent optical tables (Fig. 4). The optical tables on which the incident x-ray optics and laser heating optics are mounted have Y-Z translation stages, allowing to precisely aligning these optics to x-ray beam. The DAC diffractometer, which consists of high-precision and high-load X-Y-Z translation stages and one-circle goniometer, is designed for mounting mainly cube type DAC for ultra-high pressure experiments and symmetric piston-cylinder type DAC for high pressure and high temperature experiments using laser heating.

Fig. 4. High-precision diffractometer system for high-pressure x-ray diffraction experiments equipped in the experimental hutch 2.

Fig. 4. High-precision diffractometer system for high-pressure x-ray
diffraction experiments equipped in the experimental hutch 2.

  The diffracted x-rays are collected on the Rigaku imaging plate area detector (IP, R-AXIS IV++; 300×300 mm2; pixel size 0.1mm) or a 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 150 and 450 mm and at 200, 250, 300 mm, respectively, depending on a measuring range of diffraction angle and an angular resolution. On the detector stage, the microscope unit is equipped to visually observe the sample in DACs and to align the sample to x-ray beam. The microscope unit can also used as Raman probe head for on-line pressure measurements and Raman scattering measurements, and Raman signal can be collected by the objective lens and in the return path. Double-sided laser heating system with near-infrared fiber laser 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.5 shows the laser heating system for DACs installed in the BL10XU. The glassy carbon mirror with Ag-coated is employed to deriver 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 of 300 GPa, 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 40 µm.

Fig. 5. The optics of double-sided laser heating and temperature measurements in the experimental hutch 2

Fig. 5. The optics of double-sided laser heating and temperature
measurements in the experimental hutch 2

On the downstream side of experimental hutch 2, an energy domain 57Fe Mössbauer absorption spectroscopy system is equipped, and Mössbauer experiments can be performed under the exactly same extreme conditions as multiple in-situ probes with X-ray diffraction.
As other optical components in the experimental hutch 1 and 2, a slit with four blades for high energy x-rays, ion chamber for intensity monitor of incident x-ray beam, x-ray shutter, attenuator unit for IP, compound refractive lens for x-ray focusing, and direct beam stopper are equipped.

  • DATA EVALUATION SOFTWARE
    The IP detector, R-AXIS IV++, is controlled using x-ray diffraction data acquisition software designed by Rigaku Co., and the software runs on Windows 7.
    Control of the DAC stage, goniometer and stages for optical elements is based on stepping motor controller designed by Tsuji Electronics Co., Ltd. Control program has been developed by users.
    For Raman data acquisition and processing, Andor Solis software is used.
    As an analysis software of X-ray diffraction data, "IPAnalyzer" and "PDindexer" are used, which have been programed by Dr. Y. Seto, Kobe University.
  • EQUIPMENT HIGHLIGHTS
    • Slit optics with four blades
    • Goniometer
    • Imaging plate area detector (IP)
    • Digital X-ray flat panel detector
    • Micro Raman spectroscopy system for pressure measurements (on-line): 532 nm diode laser
    • Electrical resistance measurement system
    • Brillouin scattering measurements system
    • 57Fe Mössbauer spectroscopy system
    • Cryostat and thermostat (10 K ∼)
    • Double-sided laser heating system (1500 ∼ 6000 K)
    • Diamond anvil cell (Bring your own)
    • Sample preparation rooms for high-pressure experiment
    • Microscopes with Raman scattering probe
    • Electric discharge-drilling machine (EDM)
    • Ruby fluorescence system for pressure measurement (off-line)
    • Micro Raman spectroscopy system for pressure measurements (off-line): 785 nm diode laser

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CONTACT INFORMATION

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

Naohisa HIRAO
SPring-8 / JASRI
1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198
Phone : +81-(0)791-58-2750
Fax : +81-(0)791-58-0830
e-mail : hirao

Saori IMADA
SPring-8 / JASRI
1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198
Phone : +81-(0)791-58-2750
Fax : +81-(0)791-58-0830
e-mail : sao.kawaguchi

Yasuo OHISHI
SPring-8 / JASRI
1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198
Phone : +81-(0)791-58-2750
Fax : +81-(0)791-58-0830
e-mail : ohishi

Last modified 2016-09-02 13:59
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