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Beamlines and New End Stations

AuthorM.-T. TangNational Synchrotron Radiation Research Center, Hsinchu, Taiwan

It was a very busy year in 2009 at NSRRC. By the end of 2009, the total number of constructed beamlines has reached a historical high of 29 (see the floor map), includ-ing 3 Taiwanese beamlines at SPring-8. In May, the newly constructed beamline BL23A was opened to her strongly demanding small angle scattering users. Also in May, the drug design beamline BL15A consuming X-rays gener-ated from the last in-achromatic superconducting wig-gler (IASW) started her construction phase. Several major beamline maintenance and upgrades covering over nine X-ray beamlines and four VUV/soft X-ray beamlines were conducted during the summer ring shutdown. In August, the pass of BL07A beamline radiation survey started the

SP12U Inelastic X-ray Scattering

SP12B X-ray Absorption, Diffraction

12NSRRC Beamlines

hard X-ray : 3

at SPring-8, JapanProtein Crystallography,

: Participating Research Group ( )

SWLS: Superconducting Wavelength Shifter

EPU5.6: Elliptically Polarized UndulatorIASW: In-Archomatic Superconducting Wiggler

U5: Undulator (5 cm, 76 Periods)

W20: Wiggler (1.8 T, 27 Poles)U9: Undulator (9 cm, 48 Periods)

SW: Superconducting Wiggler (3.2 T, 32 Poles)

Insertion Devices

SP12D HE Photoemission

soft X-ray hard X-ray

20

19

1817

1615 1413

12

11

1009

08

07

0605

04030201

2122

23

24

SW

U5

EPU5.6

W20

U9

SWLS

01A 01B X-Ray Microscopy - SWLS01C

White X-ray - SWLS

EXAFS, Powder Diffraction - SWLS

03A Gas Phase (HF-CGM) - BM

04A 04B

Beam Diagnosis - BM

05A Spin-Polarized PES, PEEM - EPU 05B

Soft X-ray Scattering - EPU

07AX-ray Scattering - IASW

XPS, UPS (L-SGM) - BM 08A

09ASPEM, XPS - U5

11AMCD, XAS (Dragon) - BM11B

13B13C

13A SW6 - X-ray Membrane ScatteringSW6 - Protein CrystallographySW6 - Protein Crystallography

14A BM - IR Microscopy

15A

16A

IASW - Drug Design

17B W20 - X-ray Scattering

17C W20 - EXAFS

18A BM - Beam Diagnosis18B BM - LIGA

19A BM - X-ray Lithography19B BM - Photo-Stimulated Desorption

20A20B

BM - (H-SGM) XASBM - X-ray Instrumentation

21A

21BU9 - (White Light) Chemical Dynamics

23A IASW - SAXS

24A BM - (WR-SGM) XPS, UPS

Gas Phase (Seya) - BM

Beam Diagnosis - BM

U9 - (CGM) Angle-Resolved UPS, Spectroscopy

under construction

: 11: 12

NSRRC Beamlines

IR, VUV : 5

IASW

IAS

W

IASW

( )

( )

BM - Tender X-ray Absorption, Diffraction

( )

at Hsinchu, Taiwan

17A W20 - X-ray Diffraction

beam diagnosis : 6

10A Beam Diagnosis - BM

XAS, XPS ( M-AGM) - BM 08B

21C BM - Beam Diagnosis

( )

: 2

SRCD - BM 04C

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commissioning phase of the beamline. Most of the beam-lines except BL17A benefited proportionally in terms of photon flux after the ring current was raised from 300 mA to 360 mA in December. A major modification of the SEYA beamline will be undertaken in 2010. The two orders of magnitude increase in photon flux will put synchrotron radiation circular dichroism (SRCD) at NSRRC into a world competing business.

To highlight the advancement in instrumentation, the dedicated small/wide angle X-ray scattering (SWAXS) instrument located at the BL23A beamline for structural characterization with soft matter and nanoparticles has been opened to all NSRRC users in May. The new BL23A SWAXS endstation features simultaneous, time-resolved SAXS/WAXS with DSC, shear, stretching device, and stopped-flow device for polymers and liquid crystals. So-lution SAXS for colloidal particles, proteins, and biomacro-molecules can be conducted here. With the double multi-layer monochromator (DMM) mode for a high flux beam of ~1011 photons/s, scattering time resolution can be within 100 ms for structural dynamics studies with polymer crystallization; with the double crystal monochromator (DCM) mode for a beam of an energy resolution of a few eV, anomalous scattering is also available for multiphase nanoparticles, polymer-nanoparticle composites, alloys, and lipid vesicle/metal ion complex, containing elements of characteristic X-ray absorptions in the energy region

between 5-23 keV. Grazing incidence SAXS/WAXS for poly-mer, lipid or nanoparticle thin films/monolayers on solid substrates can be performed (Fig. 1). A deflecting mirror for a precise bending of the X-ray beam downwards grants GISAXS for nanostructures formed at the air-liquid/liquid-liquid interfaces.

The BL07A is the first contract beamline constructed under the collaborative task of the Associated Universi-ties Team (AUT ) and NSRRC. The X-ray absorption spectrosco py (XAS) station at BL07A was constructed in August 2009, and commissioned together with the beam-line in succession. The generic XAS station design similar to BL01C1 and BL17C aims to allow a user-friendly environ-ment. The beamline provides X-ray photons of 5-23 keV, covering the K-edge energy of the elements from Ti to Ru in the periodic table. Total photon flux was estimated to be one and two orders of magnitude higher than those of BL01C1 and BL17C, respectively. Even for the samples of small size (such as in diamond anvil cell), the number of photons impinging the sample is still high enough to produce data of good quality. High photon flux also offers other advantages in terms of faster data collection and lower detection limit (in concentration). The 8-circle dif-fractometer on the beamline was stationed for X-ray scat-tering. A high quality single crystal Cr known for having a modulated structure caused by charge density wave (CDW) at room temperature was aligned at the diffractometer and

Fig. 1: Grazing incidence small angle X-ray scattering with in situ surface pressure-area isotherm measurement for the mono-layer of ligand-capped silver nanoparticles compressed at the air-water interface. The GISAXS pattern (shown at right) indicates an in–plane correlation peak of the nanoparticles.

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two satellite reflec-tions at (2-q 0 0) and (2+q 0 0), q~0.032 were measured. The results are compared with the identical measurement done at SP12B1 where ten times intensity in-crease is visibly clear (Fig. 2).

The construc-t i o n o f t h e d r u g design BL15A wil l conclude the con-s t r u c t i o n o f h a rd X-ray beamline at TLS. The beamline is de-signed mainly for macromolecule crystallography (5.6 -15.5 keV), with a minor application for small molecule crystallography (6.7 -19 keV). As for the construction time-line, the double crystal monochromator (DCM) and the mirrors will be installed and tested in April and October 2010, respectively. The beamline construction excluding the experimental station will be completed in Dec. 2010 and ready for radiation survey in early 2011.

The side line of BL12XU at SPring-8 has completed the construction stage in 2008 and now is in the commission-ing stage. This beamline is characterized by a combination of diamond monochromator (DM) and a downstream high resolution monochromator, followed by a micro-focusing system of the Kirkpatrick-Baez design that reduces the beam size to 40 μm × 40 μm at the sample position. To facilitate rapid energy tuning, both the endstation and the beamline section downstream of the DM are supported by a precision platform that rotates with the outgoing beam of DM. This beamline will deliver X-ray photons from 6 keV to 12 keV and is dedicated to hard X-ray photoemis-sion spectroscopy (HAXPES) research. The purpose of us-ing hard X-rays is to have a much larger electron inelastic mean free path than that of the conventional photoemis-sion using VUV and soft X-rays to probe the electronic structure deep under the surface. This property can be ap-plied to many strongly correlated system having different electronic structure on surface, and buried interface.

The design goal is to have the electron energy analyzer detecting photoelectrons emitted along the polarization vector or the horizontal geometry and along the direction normal to the polarization vector or the vertical geom-

etry. The s-orbitals contribute most to the bonding and is favored to be detected in the horizontal geometry. The d-orbitals of transition metals are most concerned in strongly correlated systems. The s-orbitals become rela-tively insensitive in the vertical geometry. Figure 3 shows a comparison of photoemission spectra of a less strongly correlated system ZnO as a test system. The top panel shows a normal XPS (hν= 1486.6 eV) spectrum; the strong peak at about 11 eV is due to Zn 3d; the spectral weight between 4 and 9 eV comes primarily from O 2p mixed with

Fig. 2: Comparison of satellite reflection measured at 07A and 12B2 beamlines. The data taken at 12B2 was in the reciprocal space, and in real space for 07A.

Fig. 3: Comparison of photoemission spectra of a less strong correlated system ZnO as a test system.(see text for details)

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a small component of Zn 4s, consistent with calculated photoionization cross sections. In the middle panel a HAXPES spectrum is measured using 7.7 keV photons in the horizontal geometry; the Zn 4s signal is much enhanced compared to XPS. By using the vertical geometry shown in the bottom panel the Zn 4s becomes much suppressed

showing a spectra similar to normal XPS. These results dem-onstrate the usefulness of these two geometries to distin-guish bonding (s) and correlation related oribitals (d).

As for the task of experimental stations, the detec-tor upgrade plan for protein crystallography beamlines, including BL13B1 (Q315 upgraded to Q315r) and BL13C1

Fig. 5: The 2009 IFCB International Training Program in Cell and Molecular Biology was held in June 15~26, 2009. 41 trainees were taking PX training at NSRRC.

Fig. 4: S c h e m a t i c s s h o w i n g the application of the quasi-2D detector in both the non-resonant and resonant IXS setup of the spectrometer at SPring-8.

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(Q210 upgraded to Q315r) in Taiwan and SP12B2 (Q4r upgraded to Q210r) in SPring-8, was accomplished by the end of 2009. Based on the collaborative task among NSRRC, Academia Sinica and Osaka University, a new and high performance protein crystallography CCD detector MX225HE was installed in SP44XU beamline at SPring-8, and as a consequence, 25% of the beamtime is dedicated to Taiwanese utilization. A three-year contract signed with RIKEN has agreed upon the access of Taiwanese research-ers and utilization of the Protein Tectonics Platform (PTP) at SPring-8 to produce proteins and grow crystals since April 2009.

A detector development project was launched in 2009 under a MOU signed with NSLS, with the first detec-tor from the project to be delivered to SPring-8 SP12XU. The quasi-2D strips detector is designed and fabricated for non-resonant and resonant inelastic X-ray scattering ex-periments shown in Fig. 4. The detector is equipped with 15 individual sensors for each analyzer to collect scattered X-rays of energies from 6 to 30 keV. Based on the hybrid cMOS technology, the leakage current of the selected sen-sors is less than 1 nA. Benefiting from extremely low noise of the sensors, the detector is potentially applicable for many hard X-ray experiments. All the circuit and mecha-nism tests have been done. The radiation exposure test is scheduled in April 2010.

User training and promotion has been two of the ma-jor missions of NSRRC, and extensive efforts were made on planning and organization of versatile activities. In 2009, there were two training courses organized for X-ray ab-sorption spectroscopy (February and June), one course for X-ray powder diffraction (July), and nine training courses, mini-schools and workshops for protein crystallography (spreading over the year), among which three courses were mainly organized for international users (SLRI, IFCB, A-IMBN/AMBO Fig. 5).

ContributorsM.-T. Tang, U-S. Jeng, J.-F. Lee, C.-H. Du, D.-G. Liu, K.-D. Tsuei, K.-L. Yu, S. H. Chang, and Y.-C. Jean.

Contacted E-mailmautsu@nsrrc.org.tw

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