Silicon Crystal Monochromator Research Articles

Crystallographic Data Collection Using a Multilayer Monochromator on an Undulator Beamline at the Shanghai Synchrotron Radiation Facility

To resolve photons hungry for weak diffraction samples by the crystallographic method, a double-multilayer monochromator (DMM) was employed on an undulator beamline (BL17UM) at the Shanghai Synchrotron Radiation Facility (SSRF) to provide a focused sub-micron beam with high brightness for macromolecular crystallography experiments. High-quality crystallographic datasets from model protein crystal samples were collected and processed by an existing crystallographic program for structure solution and refinement. The data quality was compared with datasets from a normal silicon crystal monochromator to evaluate the bandwidth of the DMM effect on these crystallographic data. This experiment demonstrates that multilayer optics on an undulator beamline may play a valuable role in satisfying the demands of structure-related research, which requires novel methods.

A thermal deformation optimization method forcryogenically cooled silicon crystal monochromators under high heat load.

A method to optimize the thermal deformation of an indirectly cryo-cooled silicon crystal monochromator exposed to intense X-rays at a low-emittance diffraction-limited synchrotron radiation source is presented. The thermal-induced slope error of the monochromator crystal has been studied as a function of heat transfer efficiency, crystal temperature distribution and beam footprint size. A partial cooling method is proposed, which flattens the crystal surface profile within the beam footprint by modifying the cooling contact area to optimize the crystal peak temperature. The optimal temperature varies with different photon energies, which is investigated, and a proper cooling strategy is obtained to fulfil the thermal distortion requirements over the entire photon energy range. At an absorbed power up to 300 W with a maximum power density of 44.8 W mm-2 normal incidence beam from an in-vacuum undulator, the crystal thermal distortion does not exceed 0.3 µrad at 8.33 keV. This method will provide references for the monochromator design on diffraction-limited synchrotron radiation or free-electron laser light sources.

Pink-Beam Serial Synchrotron Crystallography at Pohang Light Source II

Serial crystallography (SX) enables the determination of room-temperature structures with minimal radiation damage. The photon flux of the pink beam of 1.2% bandwidth (BW) is one order higher than that of the monochromatic beam from a silicon crystal monochromator, and the energy resolution of 1.2% BW is enough to solve the structure; therefore, it is useful to use the pink beam for time-resolved serial synchrotron crystallography (SSX). Here, we demonstrate a pink-beam serial synchrotron crystallographic study at the 1C beamline at the Pohang Light Source II. Lysozyme crystals embedded in a beef tallow injection matrix were delivered through a syringe into the X-ray interaction point. Pink-beam SSX was performed with different X-ray exposure positions to the injection stream (center and edge) and X-ray exposure times (50 and 100 ms). All lysozyme crystal structures were successfully determined at a high resolution of 1.7 Å. Background analysis showed that X-ray diffraction data exposed to the edge of the injection stream could improve the signal-to-noise ratio. All the diffraction data and room-temperature lysozyme structures were comprehensively compared. The data collection strategy and analysis will be helpful in further pink-beam SSX experiments and their applications.

Cryo-cooled silicon crystal monochromators: a study of power load, temperature and deformation.

Crystal monochromators are often the primary optics in hard X-ray synchrotron beamlines. Management of power load is central to their design. Strict requirements on stability and deformation are to be met, as new-generation synchrotron sources deliver brighter beams of X-rays. This article sets out to illustrate an overall picture of the deformation caused by heat load in a cryo-cooled Si crystal monochromator using first principles. A theoretical model has been developed to predict the temperature distribution and surface deformation by applying intrinsic properties of Si material and the cooling system parameters. The model explains the universal behaviour of crystal slope error versus absorbed power; it has been benchmarked against experimental data and used to interpret finite-element analysis of cryogenically cooled crystals.

Performance of a cryo-cooled crystal monochromator illuminated by hard X-rays with MHz repetition rate at the European X-ray Free-Electron Laser.

Due to the high intensity and MHz repetition rate of photon pulses generated by the European X-ray Free-Electron Laser, the heat load on silicon crystal monochromators can become large and prevent ideal transmission in Bragg diffraction geometry due to crystal deformation. Here, we present experimental data illustrating how heat load affects the performance of a cryogenically cooled monochromator under such conditions. The measurements are in good agreement with a depth-uniform model of X-ray dynamical diffraction taking beam absorption and heat deformation of the crystals into account.

Multiple energy synchrotron biomedical imaging system

A multiple energy imaging system that can extract multiple endogenous or induced contrast materials as well as water and bone images would be ideal for imaging of biological subjects. The continuous spectrum available from synchrotron light facilities provides a nearly perfect source for multiple energy x-ray imaging. A novel multiple energy x-ray imaging system, which prepares a horizontally focused polychromatic x-ray beam, has been developed at the BioMedical Imaging and Therapy bend magnet beamline at the Canadian Light Source. The imaging system is made up of a cylindrically bent Laue single silicon (5,1,1) crystal monochromator, scanning and positioning stages for the subjects, flat panel (area) detector, and a data acquisition and control system. Depending on the crystal’s bent radius, reflection type, and the horizontal beam width of the filtered synchrotron radiation (20–50 keV) used, the size and spectral energy range of the focused beam prepared varied. For example, with a bent radius of 95 cm, a (1,1,1) type reflection and a 50 mm wide beam, a 0.5 mm wide focused beam of spectral energy range 27 keV–43 keV was obtained. This spectral energy range covers the K-edges of iodine (33.17 keV), xenon (34.56 keV), cesium (35.99 keV), and barium (37.44 keV); some of these elements are used as biomedical and clinical contrast agents. Using the developed imaging system, a test subject composed of iodine, xenon, cesium, and barium along with water and bone were imaged and their projected concentrations successfully extracted. The estimated dose rate to test subjects imaged at a ring current of 200 mA is 8.7 mGy s−1, corresponding to a cumulative dose of 1.3 Gy and a dose of 26.1 mGy per image. Potential biomedical applications of the imaging system will include projection imaging that requires any of the extracted elements as a contrast agent and multi-contrast K-edge imaging.

Development of the neutron diffraction method for stress measurements in thick steel samples.

The results of development of neutron method for stress measurements in bulk steel components are considered. Enhancement of the maximum available path length (∼⃒85mm) was achieved by using optimized bent perfect silicon crystal monochromators, position sensitive detectors and neutron wavelengths, corresponding to the minimums of neutron total cross section near Bragg edges.

The new NCPSS BL19U2 beamline at the SSRF for small-angle X-ray scattering from biological macromolecules in solution.

The beamline BL19U2 is located in the Shanghai Synchrotron Radiation Facility (SSRF) and is its first beamline dedicated to biological material small-angle X-ray scattering (BioSAXS). The electrons come from an undulator which can provide high brilliance for the BL19U2 end stations. A double flat silicon crystal (111) monochromator is used in BL19U2, with a tunable monochromatic photon energy ranging from 7 to 15 keV. To meet the rapidly growing demands of crystallographers, biochemists and structural biologists, the BioSAXS beamline allows manual and automatic sample loading/unloading. A Pilatus 1M detector (Dectris) is employed for data collection, characterized by a high dynamic range and a short readout time. The highly automated data processing pipeline SASFLOW was integrated into BL19U2, with help from the BioSAXS group of the European Molecular Biology Laboratory (EMBL, Hamburg), which provides a user-friendly interface for data processing. The BL19U2 beamline was officially opened to users in March 2015. To date, feedback from users has been positive and the number of experimental proposals at BL19U2 is increasing. A description of the new BioSAXS beamline and the setup characteristics is given, together with examples of data obtained.

Rotation of X-ray polarization in the glitches of a silicon crystal monochromator.

EXAFS studies on dilute samples are usually carried out by collecting the fluorescence yield using a large-area multi-element detector. This method is susceptible to the 'glitches' produced by all single-crystal monochromators. Glitches are sharp dips or spikes in the diffracted intensity at specific crystal orientations. If incorrectly compensated, they degrade the spectroscopic data. Normalization of the fluorescence signal by the incident flux alone is sometimes insufficient to compensate for the glitches. Measurements performed at the state-of-the-art wiggler beamline I20-scanning at Diamond Light Source have shown that the glitches alter the spatial distribution of the sample's quasi-elastic X-ray scattering. Because glitches result from additional Bragg reflections, multiple-beam dynamical diffraction theory is necessary to understand their effects. Here, the glitches of the Si(111) four-bounce monochromator of I20-scanning just above the Ni K edge are associated with their Bragg reflections. A fitting procedure that treats coherent and Compton scattering is developed and applied to a sample of an extremely dilute (100 micromolal) aqueous solution of Ni(NO3)2. The depolarization of the wiggler X-ray beam out of the electron orbit is modeled. The fits achieve good agreement with the sample's quasi-elastic scattering with just a few parameters. The X-ray polarization is rotated up to ±4.3° within the glitches, as predicted by dynamical diffraction. These results will help users normalize EXAFS data at glitches.

Diffraction-Enhanced Imaging of Musculoskeletal Tissues Using a Conventional X-Ray Tube

In conventional projection radiography, cartilage and other soft tissues do not produce enough radiographic contrast to be distinguishable from each other. Diffraction-enhanced imaging (DEI) uses a monochromatic x-ray beam and a silicon crystal analyzer to produce images in which attenuation contrast is greatly enhanced and x-ray refraction at tissue boundaries can be detected. The aim of this study was to test the efficacy of conventional x-ray tube-based DEI for the detection of soft tissues in experimental samples. Cadaveric human tali (normal and degenerated) and a knee and thumb were imaged with DEI using a conventional x-ray tube and DEI setup that included a double-silicon crystal monochromator and a silicon crystal analyzer positioned between the imaged object and the detector. Diffraction-enhanced images of the cadaveric tali allowed the visualization of cartilage and its specific level of degeneration for each specimen. There was a significant correlation between the grade of cartilage integrity as assessed on the tube diffraction-enhanced images and on their respective histologic sections (r = 0.97, P = .01). Images of the intact knee showed the articular cartilage edge of the femoral condyle, even when superimposed by the tibia. In the thumb image, it was possible to visualize articular cartilage, tendons, and other soft tissues. DEI based on a conventional x-ray tube allows the visualization of skeletal and soft tissues simultaneously. Although more in-depth testing and optimization of the DEI setup must be carried out, these data demonstrate a proof of principle for further development of the technology for future clinical imaging.

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 Mössbauer 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.

A cryogenically cooled channel-cut crystal monochromator using a helium refrigerator and heat exchanger

Silicon crystals at room temperature employed as x-ray monochromators on synchrotron radiation beamlines, when subjected to high-power-density loading, suffer thermal distortions which compromise their x-ray diffraction efficiency and result in a reduction of the inherent brilliance of the synchrotron beam. At cryogenic temperatures however (below 150 K), silicon crystals suffer little or no thermal distortions under high-power-density loading. The design and implementation of a channel-cut silicon crystal monochromator which is cooled to as low as 50 K, using a commercial helium refrigerator and circulation system and a custom-designed heat exchanger for the monochromator crystal, are described. Test results have been obtained on the National Synchrotron Light Source X13B in-vacuum undulator beamline as well as the higher power X25 wiggler beamline.

Nonlinear thermal-distortion predictions of a silicon monochromator using the finite element method

Silicon crystal monochromators at cryogenic temperatures have been used with great success at third-generation synchrotron radiation sources. At the Advanced Photon Source the unique characteristics of silicon at liquid nitrogen temperatures (80 K) have been leveraged to significantly reduce the thermally induced distortions on beamline monochromators. Finite element simulations of the nonlinear (temperature-dependent material properties) thermal stress problem were performed and compared with the experimental measurements. Several critical finite element modeling considerations are discussed for their role in accurately predicting the highly coupled thermal and structural response of the optical component's surface distortion to the high thermal heat flux. Once an understanding of the effects of (i) local element mesh size, (ii) area/surface heat flux versus volumetric heat generation, and (iii) uniform volumetric absorbed power versus a depth-dependent absorbed power, a final series of simulations was performed. Depending on the estimated convection heat-transfer coefficient, the final refined finite element model's predictions correlated well with the experimental measurements. In general, the use of the finite element method in predicting the overall thermal and structural behavior of the surface of the optical components with a high heat flux was shown to be quite effective.

Spectral dependence of point defect production by x rays in RbBr

F-center formation by monochromatic x rays has been studied above and below the bromine and rubidium K-absorption edges in crystals of RbBr. The x-ray beam from a double silicon crystal monochromator on an undulator at the Advanced Photon Source was used to produce these point defects, which were detected by a sensitive laser-induced luminescence method. Experiments were carried out over a wide range of monochromatic x-ray intensity, with emphasis on the nearly linear initial slope of defect formation with exposure. No significant increase in F-center formation efficiency was found upon crossing the bromine K edge, which indicates that additional Auger-cascade mechanisms do not appreciably add to the usual multiple ionization electron-hole recombination processes known to generate point defects.

A high-resolution monochromator for inelastic nuclear resonant scattering experiments using [formula omitted

We report a silicon crystal monochromator with an angular acceptance of 14.1 μrad and an energy bandwidth of 3.6 meV at 23.880 keV X-ray energy – an energy resolution δE/ E of 1.5×10 −7. In combination with an undulator source, the monochromator is used to measure the partial phonon density of states of Sn in 119 SnO 2 by the method of inelastic nuclear resonant scattering using the 23.880 keV nuclear transition of 119 Sn .

Performance of cryogenically cooled, high-heat-load silicon crystal monochromators with porous media augmentation

The performance of two Si crystal x-ray monochromators internally cooled with liquid nitrogen was tested on the F2-wiggler beamline at the Cornell High Energy Synchrotron Source (CHESS). Both crystals were (111)-oriented blocks of rectangular cross section having identical dimensions. Seven 6.4-mm-diameter coolant channels were drilled through the crystals along the beam direction. In one of the crystals, porous Cu mesh inserts were bonded into the channels to enhance the heat transfer. The channels of the second crystal were left as drilled. Symmetric, double-crystal rocking curves were recorded simultaneously for both the first and third order reflections at 8 and 24 keV. The power load on the cooled crystal was adjusted by varying the horizontal beam size using slits. The measured Si(333) rocking curve of the unenhanced crystal at 24 keV at low power was 1.9 arcsec FWHM. The theoretical width is 0.63 arcsec. The difference is due to residual fabrication and mounting strain. For a maximum incident power of 601 W and an average power density of about 10 W/mm2, the rocking curve was 2.7 arcsec. The rocking curve width for the enhanced crystal at low power was 2.4 arcsec. At a maximum incident power of 1803 W and an average power density of about 19 W/mm2, the rocking curve width was 2.2 arcsec FWHM. The use of porous mesh augmentation is a simple, but very effective, means to improve the performance of cryogenically cooled Si monochromators exposed to high power x-ray beams.

Performance of a liquid-nitrogen-cooled, thin silicon crystal monochromator on a high-power, focused wiggler synchrotron beam

An experiment was performed on beamline BL 3 at the European Synchrotron Radiation Facility to test the diffraction performance of a novel internally liquid-nitrogen-cooled, thin silicon crystal monochromator exposed to high heat loads. The beam parameters were chosen to closely match the conditions expected, in terms of absorbed power and beam profile, at the Advanced Photon Source (APS) for the closed gap undulator at 7 GeV and 100 mA. The cooled crystal was oriented at 11.4° in the symmetric Bragg geometry to diffract 30 keV x-rays from the Si(333) planes. The source was a 44-pole wiggler with the insertion device gap set at 25.0 mm corresponding to a deflection parameter, K, of 4.2. A tunable toroidal mirror was used to focus the wiggler beam onto the crystal. Double-crystal rocking curves were measured at several power values using different attenuators. The maximum total power absorbed by the 0.6-mm-thick crystal was 154 W at a storage ring current of 136 mA. The peak power density at normal incidence was about 420 W/mm2 corresponding to an absorbed peak power density on the crystal face of 83 W/mm2. No thermal-induced broadening of the rocking curve was observed above the average measured mounting/fabrication strain of 2 arcsec. Rocking curves were also measured as a function of coolant flow rate and pressure. No systematic broadening occurred due to flow-induced vibrations up to 6 ℓ/min. It has been demonstrated that thin silicon crystals directly cooled with liquid nitrogen can handle high power density synchrotron beams comparable to what is expected for the APS undulators with no appreciable thermal deformation.

Cooling of silicon crystal monochromator for the undulator x rays at the beamline NE3

A double crystal monochromator accommodating water or liquid nitrogen cooling device for a first monochromator crystal was designed and installed in the x-ray undulator beamline NE3 of the 6.5 GeV TRISTAN accumulation ring. In a series of cooling experiments at the BL-NE3 the silicon crystals were set at an incident angle of 7.9° to reflect 14.4 keV photons and its higher harmonics, and its maximum power density on the crystal surface was 4.3 W/mm2 (815 W total power). The water cooled crystal behaved properly only when the peak power density was below 1.0 W/mm2 (185 W total power), while the LN2 cooled one showed no apparent changes in width of rocking curve and its reflectivity against the maximum power and the maximum peak power density 815 W and 4.3 W/mm2, respectively, and no deformation in the pattern of a diffraction spot.

X-ray diffraction tomography at the Australian National Beamline Facility

Preliminary x-ray diffraction tomographic experiments utilizing synchrotron radiation have been performed at the Australian National Beamline Facility (BL20B) of the Photon Factory, National Laboratory for High Energy Physics in Japan. The tomographic instrument arrangement consisted of a double silicon crystal monochromator, motor-driven beam-defining collimation slits, and microcomputer-controlled specimen movement stages and was designed to simultaneously record tomographic data from multiple transmission and scatter radiation detectors. Image plates were used to record the scattering properties of specimen constituents, which facilitated registration of the scatter detectors. The design of the instrument is described and some preliminary results are presented.

Iron(II) sulphate (Fricke solution) oxidation yields for 8.9 and 13.6 keV X-rays from synchrotron radiation.

The oxidation yields (G) for 8.86 and 13.55 keV X-rays produced by synchrotron radiation were measured using an iron(II) sulphate (Fricke) solution. Monoenergetic X-rays were produced using a silicon crystal monochromator. The X-rays were absorbed in 0.4 M sulphuric acid-iron(II) sulphate solution and FeIII ion yields were measured and corrected for escape fractions resulting from scattering using Monte Carlo calculations. Doses in the solution were determined using a thin window, parallel plate chamber calibrated against a primary standard free-air chamber at the Electrotechnical Laboratory (Osaka, Japan). Yields (G) of 1.50 +/- 0.06 and 1.43 +/- 0.06 mumol J-1 were obtained for 8.86 and 13.55 keV X-rays respectively.