Nuclear Resonance Beamline at ESRF

The Nuclear Resonance Beamline at ESRF is dedicated to the excitation of nuclear levels by synchrotron radiation. The sources of radiation and optical elements are optimized to provide an intense, highly monochromatic, collimated and stable X-ray beam of small cross-section at the Mössbauer transition energies between 6 and 30 keV. The set-up of the beamline allows to perform studies in diffraction, small angle scattering, forward scattering and incoherent scattering. Equipment is available to maintain the sample at variable temperature and magnetic field. Fast detectors and timing electronics serve to separate the delayed nuclear scattering from the prompt electronic scattering and to measure the time spectra of nuclear radiation with sub-nanosecond resolution. The general lay-out and the parameters of the beamline are reported. Typical domains of applications are discussed and illustrated by first experimental results.     

XDS: a flexible beamline for X‐ray diffraction and spectroscopy at the Brazilian synchrotron

The majority of the beamlines at the Brazilian Synchrotron Light Source Laboratory (LNLS) use radiation produced in the storage‐ring bending magnets and are therefore currently limited in the flux that can be used in the harder part of the X‐ray spectrum (above ～10 keV). A 4 T superconducting multipolar wiggler (SCW) was recently installed at LNLS in order to improve the photon flux above 10 keV and fulfill the demands set by the materials science community. A new multi‐purpose beamline was then installed at the LNLS using the SCW as a photon source. The XDS is a flexible beamline operating in the energy range between 5 and 30 keV, designed to perform experiments using absorption, diffraction and scattering techniques. Most of the work performed at the XDS beamline concentrates on X‐ray absorption spectroscopy at energies above 18 keV and high‐resolution diffraction experiments. More recently, new setups and photon‐hungry experiments such as total X‐ray scattering, X‐ray diffraction under high pressures, resonant X‐ray emission spectroscopy, among others, have started to become routine at XDS. Here, the XDS beamline characteristics, performance and a few new experimental possibilities are described.     

The sapphire backscattering monochromator at the Dynamics beamline P01 of PETRA III

We report on a high resolution sapphire backscattering monochromator installed at the Dynamics beamline P01 of PETRA III. The device enables nuclear resonance scattering experiments on Mössbauer isotopes with transition energies between 20 and 60 keV with sub-meV to meV resolution. In a first performance test with ¹¹⁹Sn nuclear resonance at a X-ray energy of 23.88 keV an energy resolution of 1.34 meV was achieved. The device extends the field of nuclear resonance scattering at the PETRA III synchrotron light source to many further isotopes like ¹⁵¹Eu, ¹⁴⁹Sm, ¹⁶¹Dy, ¹²⁵Te and ¹²¹Sb.     

Layout and first XRF applications of the BAMline at BESSY II

The first hard x‐ray beamline at BESSY II has been installed by BAM and PTB at a superconducting 7 T wavelength shifter. The main optical elements of the beamline are a double‐multilayer monochromator and a double‐crystal monochromator. Depending on the application, the two devices are used separately or in‐line. The main applications of the monochromatic radiation with photon energies up to 60 keV are x‐ray fluorescence analysis, micro computed tomography, x‐ray topography, detector calibration and reflectometry. Calculable undispersed radiation up to 200 keV is available for radiometric applications. Copyright © 2004 John Wiley & Sons, Ltd.     

Scattering signatures for some human tissues using synchrotron radiation

At photon energies below 100 keV, coherent scatter becomes important and because of its sharply forward peaked nature, it is the dominant interaction at small angles. Further, in the momentum transfer region above 0.5 Å^?1, free atom form factors are sufficient to describe coherent scattering. The angular distribution of the coherent scattering carries detailed information about the object and can be used as a signature of the tissue type of the object. The aim of this work was to analyze the scattering properties of different human tissues according to histological classifications. The coherent scattering signatures of healthy and neoplastic breast, uterus and kidney tissues were measured using x‐ray synchrotron radiation at the XRD2 beamline at the Brazilian Synchrotron Light Laboratory (LNLS). Copyright © 2005 John Wiley & Sons, Ltd.     

Coherent X‐ray scattering beamline at port 9C of Pohang Light Source II

The coherent X‐ray scattering beamline at the 9C port of the upgraded Pohang Light Source (PLS‐II) at Pohang Accelerator Laboratory in Korea is introduced. This beamline provides X‐rays of 5–20 keV, and targets coherent X‐ray experiments such as coherent diffraction imaging and X‐ray photon correlation spectroscopy. The main parameters of the beamline are summarized, and some preliminary experimental results are described.     

Nuclear resonant scattering beamline at the Advanced Photon Source

The principal and engineering aspects of a dedicated synchrotron radiation beamline under construction at the Advanced Photon Source for nuclear resonant scattering purposes are explained. The expected performance in terms of isotopes to be studied, flux, and timing properties is discussed.This work is supported by the US-DOE-BES Materials Sciences, under Contract No. W-31-109-ENG-38.     

The 57Fe Synchrotron Mössbauer Source at the ESRF

The design of a ⁵⁷Fe Synchrotron Mössbauer Source (SMS) for energy‐domain Mössbauer spectroscopy using synchrotron radiation at the Nuclear Resonance beamline (ID18) at the European Synchrotron Radiation Facility is described. The SMS is based on a nuclear resonant monochromator employing pure nuclear reflections of an iron borate (⁵⁷FeBO₃) crystal. The source provides ⁵⁷Fe resonant radiation at 14.4 keV within a bandwidth of 15 neV which is tunable in energy over a range of about ±0.6 µeV. In contrast to radioactive sources, the beam of γ‐radiation emitted by the SMS is almost fully resonant and fully polarized, has high brilliance and can be focused to a 10 µm × 5 µm spot size. Applications include, among others, the study of very small samples under extreme conditions, for example at ultrahigh pressure or combined high pressure and high temperature, and thin films under ultrahigh vacuum. The small cross section of the beam and its high intensity allow for rapid collection of Mössbauer data. For example, the measuring time of a spectrum for a sample in a diamond anvil cell at ～100 GPa is around 10 min, whereas such an experiment with a radioactive point source would take more than one week and the data quality would be considerably less. The SMS is optimized for highest intensity and best energy resolution, which is achieved by collimation of the incident synchrotron radiation beam and thus illumination of the high‐quality iron borate crystal within a narrow angular range around an optimal position of the rocking curve. The SMS is permanently located in an optics hutch and is operational immediately after moving it into the incident beam. The SMS is an in‐line monochromator, i.e. the beam emitted by the SMS is directed almost exactly along the incident synchrotron radiation beam. Thus, the SMS can be easily utilized with all existing sample environments in the experimental hutches of the beamline. Owing to a very strong suppression of electronic scattering for pure nuclear reflections (～10^?9), SMS operation does not required any gating of the prompt electronic scattering. Thus, the SMS can be utilized in any mode of storage ring operation.     

The multi‐purpose hard X‐ray beamline BL10 at the DELTA storage ring

The layout and the characteristics of the hard X‐ray beamline BL10 at the superconducting asymmetric wiggler at the 1.5 GeV Dortmund Electron Accelerator DELTA are described. This beamline is equipped with a Si(111) channel‐cut monochromator and is dedicated to X‐ray studies in the spectral range from ～4 keV to ～16 keV photon energy. There are two different endstations available. While X‐ray absorption studies in different detection modes (transmission, fluorescence, reflectivity) can be performed on a designated table, a six‐axis kappa diffractometer is installed for X‐ray scattering and reflectivity experiments. Different detector set‐ups are integrated into the beamline control software, i.e. gas‐filled ionization chambers, different photodiodes, as well as a Pilatus 2D‐detector are permanently available. The performance of the beamline is illustrated by high‐quality X‐ray absorption spectra from several reference compounds. First applications include temperature‐dependent EXAFS experiments from liquid‐nitrogen temperature in a bath cryostat up to ～660 K by using a dedicated furnace. Besides transmission measurements, fluorescence detection for dilute sample systems as well as surface‐sensitive reflection‐mode experiments are presented.     

Nuclear forward scattering for high energy mössbauer transitions

We have studied nuclear forward scattering of synchrotron radiation for the 67.41 keV resonance of 61Ni using a silicon crystal monochromator with low-index reflections and a multielement detector. This approach can be extended to other high-energy M?ssbauer transitions and does not pose any restrictions on the sample environment. Under conditions of large sample thickness and short nuclear lifetime, typical for work with high-energy nuclear resonances, the nuclear decay follows a universal dependence where both thickness effects and hyperfine interactions are taken into account by time scaling.     

Installation of a combined Raman and AFM microscope as a sample environment for nuclear resonance scattering at P01, PETRA III

A combined Raman and atomic force microscope (AFM) has been installed at beamline P01, PETRA III, DESY in Hamburg and is now available for all users of this beamline. With this unique setup nuclear resonance scattering and simultaneously performed Raman or Atomic Force Microscopy experiments are possible. Here we report on technical details of this new sample environment and on first tests with respect to the study of microstructures of spin crossover materials using ⁵⁷Fe nuclear resonance scattering.     

Quasielastic scattering of synchrotron radiation from non-resonant atoms

The beat pattern produced by nuclear resonant scattering of synchrotron radiation scattered from two stainless steel foils in constant relative motion has been measured at 3-ID beamline at the Advanced Photon Source. Contrary to theoretical prediction and different from the result in glassy material, the scattering in Bragg directions from single crystal of CoGa diffusional smoothening of the quantum beats was absent within the statistical errors. This revised version was published online in August 2006 with corrections to the Cover Date.     

The nuclear-resonance-scattering station at the PETRA II undulator beamline

PETRA II, a 12 GeV accelerator at DESY, Hamburg, is used to produce synchrotron radiation (SR) for experiments in the hard X-ray regime when it is not running as injector for HERA. The beam from an undulator is split by a diamond crystal in Laue geometry to feed two experimental stations, one of which is now dedicated for nuclear resonance experiments. The X-ray energy may be chosen in the range from 5 to 55 keV covering all isotopes already observed with SR and many interesting candidates for new resonances. Tuning may be performed by optimising the magnetic gap and the storage ring energy. In particular, the opportunities for timing experiments are unique due to a very flexible filling mode of the storage ring. The flux at the sample position is comparable to undulator beams at ESRF. The second beamline covers higher energies up to some 300 keV and may also be used for nuclear resonance experiments. This revised version was published online in August 2006 with corrections to the Cover Date.     

Fast scintillation detectors for high-energy X-ray region

We have developed fast scintillation detectors for nuclear resonant scattering experiments using synchrotron radiation and a nuclear excited level existing in >30?keV. A fast x-ray detector using an organic-inorganic perovskite scintillator of phenethylamine lead bromide (PhE-PbBr₄) had a dominant light emission with a fast decay time of 9.9?ns. An x-ray detector equipped with a 0.9-mm-thick PhE-PbBr₄ crystal (size: ～8 × 7?mm²) was used to detect nuclear resonant scattering in ⁶¹Ni (the first excited level: 67.41?keV; half-life: 5.3?ns). We could successfully record the decaying gamma rays emitted from ⁶¹Ni with a relatively high detection efficiency of 24%. A lead-doped plastic scintillator (NE142, Pb ～5?wt% doped) had been known to have a faster decay time of 1.7?ns. Following a test of a single NE142 detector, a four-channel NE142 detector was fabricated and successfully applied to the synchrotron-radiation based M?ssbauer spectroscopy experiment on ⁶¹Ni.     

HAXPES beamline PES‐BL14 at the Indus‐2 synchrotron radiation source

The Hard X‐ray Photo‐Electron Spectroscopy (HAXPES) beamline (PES‐BL14), installed at the 1.5 T bending‐magnet port at the Indian synchrotron (Indus‐2), is now available to users. The beamline can be used for X‐ray photo‐emission electron spectroscopy measurements on solid samples. The PES beamline has an excitation energy range from 3 keV to 15 keV for increased bulk sensitivity. An in‐house‐developed double‐crystal monochromator [Si (111)] and a platinum‐coated X‐ray mirror are used for the beam monochromatization and manipulation, respectively. This beamline is equipped with a high‐energy (up to 15 keV) high‐resolution (meV) hemispherical analyzer with a microchannel plate and CCD detector system with SpecsLab Prodigy and CasaXPS software. Additional user facilities include a thin‐film laboratory for sample preparation and a workstation for on‐site data processing. In this article, the design details of the beamline, other facilities and some recent scientific results are described.     

0.5 mm金刚石X射线相位延迟板及偏振度的标定

在利用步辐射光源的偏振特性进行自旋相关X射线散射及吸收谱实验来研究材料的磁学性质时，需要应用圆偏振光，这就提出了对具有高通量、高偏振度' 长连续可调的圆偏振X射线的需求；另一方面标定实验所用X射线的圆偏振度也成为这一研究领域的关键技术。由于X射线多光束衍射强度与σ场和π场的光程差δ相关，通过测量圆偏振分析晶体的多光束衍射的强度分布，可以获得入射X射线的圆偏振度。实验在美国国家同步辐射光源实验室X25光束线实验站进行，光子能量为7．1keV的圆偏振X射线由线偏振X射线经过一厚度为0．5mm、晶面为[111]的金刚石晶体产生。通过测量多光束衍射强度，确定了斯托克斯参量。实验值与X射线动力学理论计算结果能较好地吻合。     

Characterization of an in‐vacuum PILATUS 1M detector

A dedicated in‐vacuum X‐ray detector based on the hybrid pixel PILATUS 1M detector has been installed at the four‐crystal monochromator beamline of the PTB at the electron storage ring BESSY II in Berlin, Germany. Owing to its windowless operation, the detector can be used in the entire photon energy range of the beamline from 10 keV down to 1.75 keV for small‐angle X‐ray scattering (SAXS) experiments and anomalous SAXS at absorption edges of light elements. The radiometric and geometric properties of the detector such as quantum efficiency, pixel pitch and module alignment have been determined with low uncertainties. The first grazing‐incidence SAXS results demonstrate the superior resolution in momentum transfer achievable at low photon energies.     

Synchrotron radiation refraction topography for characterization of lightweight materials

The employment of synchrotron radiation for refraction topography of materials has considerable advantages over standard x‐ray sources. The much higher beam intensity and the parallel and monochromatic radiation provide faster measurements and better angular and spatial resolution. X‐ray refraction techniques image the inner surface and interface concentration of micro‐structured materials. This effect of x‐ray optics is additional to small‐angle scattering by diffraction, when the scattering objects reach micrometre dimensions. We have developed x‐ray refraction techniques within the last decade in order to meet the growing demands for improved non‐destructive characterization of high‐performance composites, ceramics and other low‐density materials. Sub‐micron particle dimensions, the pore size of ceramics, the crack density distribution and single fibre debonding within damaged composites can be measured and visualized by computer‐generated interface topographs. For this purpose investigations are now being performed at the new hard x‐ray beamline of the Federal Institute for Materials Research and Testing (BAM) at BESSY, Berlin. This BAMline provides monochromatic radiation of photon energies from 5 to 60 keV from a double multilayer and/or a double‐crystal monochromator. A separate instrument is dedicated to the further development and application of synchrotron radiation refraction (SRR) topography. Different from conventional small‐angle scattering cameras with collimating slits and pinholes, scattering angles down to a few seconds of arc are selected by a single‐crystal analyser, similar to a Bonse–Hart diffractometer. A 20 µm spatial resolution of the scattering micro‐structures is achieved by a CCD camera with a fluorescent converter. First SRR topographs of aircraft composites [carbon fibre‐reinforced plastics (CFRP), carbon fibre‐reinforced ceramics (C/C), metal matrix ceramics (MMC)] will be reported. Copyright © 2004 John Wiley & Sons, Ltd.     

New limits on interactions between weakly interacting massive particles and nucleons obtained with CsI(Tl) crystal detectors

New limits are presented on the cross section for weakly interacting massive particle (WIMP) nucleon scattering in the KIMS CsI(T?) detector array at the Yangyang Underground Laboratory. The exposure used for these results is 24?524.3 kg·days. Nuclei recoiling from WIMP interactions are identified by a pulse shape discrimination method. A low energy background due to alpha emitters on the crystal surfaces is identified and taken into account in the analysis. The detected numbers of nuclear recoils are consistent with zero and 90% confidence level upper limits on the WIMP interaction rates are set for electron equivalent energies from 3 to 11 keV. The 90% upper limit of the nuclear recoil event rate for 3.6-5.8 keV corresponding to 2-4 keV in NaI(T?) is 0.0098 counts/kg/keV/day, which is below the annual modulation amplitude reported by DAMA. This is incompatible with interpretations that enhance the modulation amplitude such as inelastic dark matter models. We establish the most stringent cross section limits on spin-dependent WIMP-proton elastic scattering for the WIMP masses greater than 20 GeV/c2.