(I) End Stations for Condensed Matter/Surface Science ...portal.nsrrc.org.tw/uao/Nano/End Stations...

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1 (I) End Stations for Condensed Matter/Surface Science (Soft X-ray) 1. Photoabsorption and Photodesorption End Station Beamline: BL20A1 (HSGM) Contact spokesperson: 陳錦明 (Jin-Ming Chen), ext. 7115, e-mail: [email protected] BL manager: 馬建毅 (Chien-I Ma), ext. 7227, e-mail: [email protected] Areas of research: The end station is intended for studying condensed phase photochemistry and electronic structures of new materials. The research areas include state-selective desorption dynamics of Cl-containing molecular adsorbates on surfaces and gaseous analogues following core-level excitation, electronic relaxation dynamics of core-excited molecules, synchrotron radiation induced surface photochemistry, and electronic structure of high-T c superconductors and magnetic materials. The vapor of liquid or gas phase sample is condensed through a leak valve onto the Si(100) surface at ~ 90 K. The measuring techniques in this end-station include XANES in total electron yield and total X-ray fluorescence yield mode, PSD, XPS, and AES. Experimental techniques: X-ray absorption (including total electron yield and total fluorescence yield), Photon- stimulated desorption (positive and negative ions), Resonant photoemission spectroscopy, Ion kinetic energy distribution Description of end station: Energy range of the BL 20 A1 beamline: 100–1300 eV Detectors: An ultrahigh-vacuum (UHV) chamber with a base pressure of ~ 1 × 10 -10 Torr. The instruments housed in the chamber include a Balzer QMA 410 mass spectrometer, a microchannel plate detector, and a Perkin-Elmer 15-255G double-pass CMA. The gas or liquid sample can be dosed onto the sample cooled down to ~90 K or heated to higher temperatures. The data acquisition software is based on LabView.

Transcript of (I) End Stations for Condensed Matter/Surface Science ...portal.nsrrc.org.tw/uao/Nano/End Stations...

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    (I) End Stations for Condensed Matter/Surface Science (Soft X-ray) 1. Photoabsorption and Photodesorption End Station Beamline: BL20A1 (HSGM) Contact spokesperson: (Jin-Ming Chen), ext. 7115, e-mail: [email protected] BL manager: (Chien-I Ma), ext. 7227, e-mail: [email protected] Areas of research: The end station is intended for studying condensed phase photochemistry and electronic structures of new materials. The research areas include state-selective desorption dynamics of Cl-containing molecular adsorbates on surfaces and gaseous analogues following core-level excitation, electronic relaxation dynamics of core-excited molecules, synchrotron radiation induced surface photochemistry, and electronic structure of high-Tc superconductors and magnetic materials. The vapor of liquid or gas phase sample is condensed through a leak valve onto the Si(100) surface at ~ 90 K. The measuring techniques in this end-station include XANES in total electron yield and total X-ray fluorescence yield mode, PSD, XPS, and AES. Experimental techniques: X-ray absorption (including total electron yield and total fluorescence yield), Photon-stimulated desorption (positive and negative ions), Resonant photoemission spectroscopy, Ion kinetic energy distribution Description of end station: Energy range of the BL 20 A1 beamline: 1001300 eV Detectors: An ultrahigh-vacuum (UHV) chamber with a base pressure of ~ 1 10-10 Torr. The instruments housed in the chamber include a Balzer QMA 410 mass spectrometer, a microchannel plate detector, and a Perkin-Elmer 15-255G double-pass CMA. The gas or liquid sample can be dosed onto the sample cooled down to ~90 K or heated to higher temperatures. The data acquisition software is based on LabView.

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    2. Surface Science StationInterface Structure Beamline: Wide-Range (BL24A) Contact spokesperson: (Yaw-wen Yang), ext: 7314, e-mail: [email protected] BL Manager: (Liang-Jen Fan), ext. 7316, e-mail: [email protected] Experimental Techniques: X-ray Photoemission Spectroscopy (XPS), Ultraviolet Photoemission Spectroscopy (UPS), Near-Edge X-ray Absorption Fine Structure Spectroscopy (NEXAFS). Description of Endstation: The surface/ interface endstation is constructed from a 14 mu-metal spherical chamber pumped by a 400 l/s turbo pump and a 320 l/s ion pump, as shown in the Picture. The base pressure of the endstation is typically around the 210-10 Torr. The major instruments include a PHOBIOS 150 electron energy analyzer from SPEC for high-resolution synchrotron-based photoelectron spectroscopy, two soft x-ray absorption spectrometers constructed from 40-mm micro-channel plates in conjunction with a set of retarding plates, a sputter-ion gun for sample cleaning, a differentially-pumped mass spectrometer (UTI-100C) for temperature programmed desorption (TPD), a low-energy electron diffraction (LEED) apparatus for surface structure determination. Gas adsorption can be done through several leak valves hooked up to a gas manifold.

    The sample mounting can be implemented in several ways. For conventional surface science work where one single crystal is used throughout the experimental period, the sample can be directly fastened to liquid-nitrogen dewar, thereby providing a working temperature range from 100 K to 1500 K. For wafer-type samples, a more elaborate sample mounting scheme is required to achieve a uniform heating and reduced outgassing. To mount multiple samples, two methods can be adopted, but each has its own

    limitation. The first method is to attach up to 30 samples to a stainless steel plate all at once before proceeding with the chamber bakeout. The samples need to be able to endure up to ~120 C in temperature during a typical 24-hour bakeout. Moreover, as-mounted samples cannot be treated with heating or cooling afterwards, and the measurements such as x-ray adsorption are typically carried out in ambient condition. The second method relies on a sample transfer mechanism that allows samples to be transported between UHV and air. Several smaller samples can be simultaneously attached to a molybdenum plate via UHV-compatible carbon tape, but the total area of the samples should be less than that of the molybdenum plate, i.e. 30 mm 30 mm. It is not unusual to load up to six small samples, each with a dimension of 5 mm 5 mm, into the UHV chamber. The samples mounted this way can be heated to 900 K or cooled down to 150 K. However, the required time for pump down during one sample transfer operation can be up to 2 hours in waiting.

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    (II) End stations for Synchrotron-Based Imaging Science 1. Nano-Transmission X-Ray Microscopy (nano-TXM)

    Beamline: BL01B1 (Superconducting Wave-Length Shifter, SWSL) Contact spokesperson: (Yen-Fang Song), ext. 7224, e-mail: [email protected] BL manager: (Gung-Chian Yin), ext. 7229, e-mail: [email protected]

    (Mau-Tsu Tang), ext. 7107, e-mail: [email protected] Scientific application Successful commissioning of Nano-TXM was completed recently and the TXM will be open to general users beginning from the February of 2006. There are many research areas waiting to be explored and conceivable applications include, but not limited to, the following areas: 2D and/ or 3D imaging of nano-scale materials for nanotechnology application; imaging of semiconductor to investigate electromigration, failure mechanism at small dimension, etc.; imaging of cracks and grain boundaries in the materials; imaging of soils and stones in aqueous conditions in geology and agriculture application; cell/ tissue imaging in their natural state for biology application; and the imaging of bones, implants, dental filling, etc. for biomedical applications. Optical Layout

    NSRRC nano-TXM

    Condenser tube

    Monochromatic X-rays

    10 cm

    Ion chamber

    Specimen mount

    Zone plate Phase ring

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    Setup photo

    Experimental Technique 1. Energy range of the SWLS beamline: 8~11 keV 2. Full field observation with field of view: 15 m 15 m for the first order diffraction of zone plate; 5 m 5 m for the third order diffraction of zone plate 3. Usable image contrast mechanism: absorption contrast, phase contrast, 3D tomography 4. Spatial resolution performance(2D): 60 nm with the first order diffraction of zone plate (Fig. a), and 25 nm with the third order diffraction of zone plate (Fig. b). (3D) 60 nm 60 nm 80 nm with tomography (Fig. c)

    Figure a Figure b Figure c

    5. Performance of phase contrast: 12% phase contrast of a plastic zone plate

    (a) without phase ring (b) with phase ring (12% phase contrast)

    Condenser tube

    Specimen Zone plate

    Monochromatic X-rays

    Phase ring

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    2. Photoemission Electron Microscopy Station Beamline: BL05B2 (EPU) Contact spokesperson: (Der-Hsin Wei), ext. 7208, e-mail: [email protected]

    (Yao-Jane Hsu), ext. 7220, e-mail: [email protected] Photoemission Electron Microscopy is an extremely powerful technique of imaging surface features with the contrast mechanism derived from versatile sources including topographical, chemical, and magnetic effects. PEEM directly images, without scanning, surface areas that emit secondary electrons due to the irradiation of X-ray from undulator by means of an electrostatic electron column. The sample transfer mechanism, performed under UHV condition, is specially designed such that multiple samples can be placed in the detection chamber through a fast entry door. If the proposed experiments require in-situ sample cleaning/ preparation, users are advised to contact the spokespersons. Major instrumentation Omicron FOCUS-IS PEEM Experimental technique Microscopy, -XAS Capabilities Energy range of EPU 5.0 beamline: 60 ~ 1400eV Polarization: linear, left/right circular, and elliptical Spatial resolution (UV/SR source): better than 0.15/0.2m Sample requirement: UHV compatible, reasonably flat solid surface, 5~10 mm in diameter (in-situ sample preparation is possible but not necessarily available.) Useful Information Principle of PEEM Sample holder used for PEEM station

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    3. Scanning Photoelectron Microscopy (SPEM) End Station Beamline; BL09A1 (U5) Contact spokesperson: (Chia-Hao Chen), ext. 7238, e-mail: [email protected] The SPEM end station is equipped with Fresnel zone plate optics to focus the monochromatized radiation produced from U5 undulator into an intense, fine X-ray beam, enabling the performance of photoelectron spectroscopy on a sub-micron-sized area of solid-state sample. The spot size at the focal point is about 100 nm. The sample is raster-scanned relative to the focused beam, and the photoelectrons excited from core-levels by the soft X-ray are collected by a 16-channel hemispherical electron energy analyzer to form 2D-elemental mapping of the surface. In this sense, SPEM is not much different from a spatially-resolved XPS but of much improved energy and spatial resolution made possible by intense x-ray beam from an undulator. Major instrumentation Low-energy electron diffraction (LEED) apparatus, PHI hemispherical electron energy analyzer, several ante-chambers housing various setups to perform sample treatments like sputtering, cleavage, sample exchanges, etc. Experimental technique Microscopy, -XPS Capabilities Energy range of the U5 beamline: 60 ~ 1400eV Spatial resolution: ~ 100 nm Sample requirement: UHV-compatible conducting or semiconducting solid surfaces.

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    4. Infrared Microspectroscopy (IMS) Station Beamline: BL14A Contact spokesperson: (Yao-Chang Lee), ext. 7333, e-mail: [email protected]

    BL manager: (Ching-Iue Chen), ext. 7212, e-mail: [email protected] Infrared microspectroscopy (IMS) is a refined technology for the identification and quantification of materials on a microscopic scale. IMS combines confocal microscope and infrared spectroscopy for microanalysis, as shown in Fig 1. Microscopy is the science of creating, recording, and interpreting magnified images, while analytical infrared spectroscopy is the science of emission, reflection, and absorption of radiant energy to determine the structure and composition of matter. The technology is rooted in optics and in the interaction of radiant energy with matter. Because of their common base, microscopy and spectroscopy are inseparable in IMS. Fig. 1 BL14A optical layout

    Major instrumentation FTIR: Thermo Nicolet Magna-860 Confocal Microscope: continuum Experimental technique Confocal Microscopy, FT-IR Capabilities Energy Range of the beamline: 4000650 cm-1 Spectral resolution: 160.125 cm-1 Spatial resolution: better than 10 m Sample requirement: solid or biological samples Reflection mode: 510 m in thickness Transmission mode: 1015 m in thickness Powder sample: no specific requirement Solution sample: no specific requirement

    Source input

    Specimen

    Detector output

    Reflextmaperture

    Dichroic Mirror

    Dichroic Mirror

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    Source input

    Specimen

    Detector output

    Reflextmaperture

    Dichroic Mirror

    Dichroic Mirror

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    Plane mirrorM1

    High order polynamialbendable mirror, M2

    HFM

    High order polynamialbendable mirror, M3

    VFM

    KBr windowFTIR

    F. M.

    BS

    M.M.

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    (III) End Stations for Material Science (Hard X-ray) 1. High Energy Powder X-ray Diffraction Beamline: BL01C2 Contact spokesperson: (Hwo-Shuenn Sheu), ext. 7122 [email protected] BL manager: (Wei-Tsung Chuang), ext. 7121 [email protected] The powder X-ray diffraction end station at BL01C2 is equipped with a Debye-Scherrer type camera for transmission type powder diffraction. The on-line flat imaging plate detecting system (Mar 345) is used to collect two dimensional diffraction pattern. Another translating imaging plate camera coupled with an off-line scanner (Fuji BAS 2500) is also available for in-situ real time and non-ambient crystallographic studies. Major Instrumentation: Mar345 (100mm pixel size, f= 345mm)

    Fuji BAS 2500 (50-100mm pixel size, 200 400 mm)

    Experimental technique: Transmission type with Dybe-Scherrer camera

    Capabilities: Energy range of the beamline: 1235 keV (10.35 ) Working temperature range of samples: 5 K800 K Working pressure of sample achieved with diamond anvil: 50 GBar Beam size: 0.151 mm Translating imaging plate camera. On-line flat imaging plate detection system

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    2. X-ray Absorption Spectroscopy Station (I) Beamline: BL01C (SWLS) Contact spokesperson: (Jyh-Fu Lee), ext. 7117, e-mail: [email protected] BL manager: (Tai, Yu-Li, Tai), ext. 7121, e-mail: [email protected] The end station has setups for performing X-ray absorption experiments on various types of samples including liquids and solids. Of particular research interest is the in-situ study of catalytic and electrochemical systems. The end station consists of gas-ionization chambers with associated electronics for transmission mode, a Lytle detector coupled with various filters for fluorescence mode, and a total electron yield detector (operated with helium flushing). Samples can be cooled down to 15 K with an APD closed-cycle cryostat or thermally treated up to 500

    oC in various gaseous environment followed by measurements at

    liquid N2 temperature. The basic setups are quite similar to those of BL17C and the equipment will be shared by these two stations. Because the photon energy at BL01C can go up to 33 keV, there is a Rh-coated mirror inside the experimental hutch for rejecting the high harmonics.

    X-ray absorption spectroscopy station located inside the BL01C hutch

    Schematic layout of the X-ray absorption station.

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    3. X-ray Absorption Spectroscopy Station (II) Beamline: BL17C (Wiggler-C) Contact spokesperson: (Jyh-Fu Lee), ext. 7117, e-mail:[email protected] BL manager: (Liu, Din-Goa, Liu), ext. 7237, e-mail: [email protected] The end station has setups for performing X-ray absorption experiments on various types of samples including liquids and solids. Of particular research interest is the in-situ study of catalytic and electrochemical systems. The end station consists of gas-ionization chambers with associated electronics for transmission mode, a Lytle detector coupled with various filters for fluorescence mode, and a total electron yield detector (operated with helium flushing). Samples can be cooled down to 15 K with an APD closed-cycle cryostat or thermally treated up to 500

    oC in various gaseous environment followed by measurements at

    liquid N2 temperature. Starting from 2006, the end station will be equipped with one 13-element x-ray array detector to be used in the fluorescence mode with an energy resolution of ~200 eV at 5.9 keV.

    X-ray absorption spectroscopy station located inside the BL17C hutch.

    In-situ catalyst cell with associated control and detection units.

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    4. Small-Angle X-ray Scattering (SAXS) end station Beamline: BL17B3 (Wiggler-B) Contact spokesperson: (U-Ser Jeng), ext: 7108, e-mail: [email protected],

    BL manager (Ying-Huang Lai), ext: 7306, e-mail: [email protected]

    The BL17B3 SAXS endstation was constructed for the purpose of studying the static and dynamic structures of matter including polymers, liquid crystals, macromolecular solutions, nanocomposite, alloy, and nanoparticles. The SAXS endstation is featured in simultaneously time-resolved SAXS/WAXS/DSC measurements, with a time resolution of ~10 sec. for a semi-crystalline system of poly(hexamethylene terephthalate) (PHT). Anomalous scattering is also available for nanoparticles and their composites, containing Pt, Au, and other elements which have characteristics of X-ray absorption in the energy region between 7-14 keV. Grazing incidence SAXS for thin films of polymer or lipid on solid substrates can be conducted.

    Interested users are directed to our web site http://web11.nsrrc.org.tw/endstation/saxs/ for further information.

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    (IV) Micro/Nano Fabrication Station 1. LIGA endstation Beamline: BL 18B1 Contact spokesperson: (Bryan B. Y. Shew), ext.7316, e-mail: [email protected] LIGA is a micromachining technique that includes lithography, electroforming, and micro molding. The use of high intensity and highly collimated SR X-ray in LIGA provides high resolution and high aspect ratio for enhanced lithographic capability. The LIGA technique has been widely used in micro optic, micro mechanic, and microwave applications. At NSRRC, all the LIGA processes, including x-ray mask fabrication, can be done in the micromachining station.

    Facility and equipment (1) BL18B Micromachining Beamline 16 m long, bending magnet SR beamline High vacuum environment (~10-10 torr) 125 m thick Be window No x-ray mirror in the beamline One filter chamber (with 3 filter set)

    (2) Micromachining FAB Area : about 100 m2 Next to micromachining beamline Including lithography (class 1K), chemical, and mechanical (class 10K) blocks

    (3) Main Equipment in the FAB UV mask aligner

    Laser writer

    RIE

    Hot embossing

    Sputter

    Ni plating bath

    Micromachining Beamline

    FAB