TUPA03
AS - ANSTO, Clayton, Australia
WEIO02
SLAC, Menlo Park, California, USA
In the past decade, LCLS has been using in-vacuum liquid jet to deliver nanocrystals, microcrystals or other samples to the experimental station. Recently, LCLS has developed a new type of liquid jet, known as "sheet"-jet, with tunable thickness from little over than 1µm to 20nm. This new type jet greatly reduces the x-ray absorbed by the liquid solutions, especially for soft x-ray and tender x-ray applications. In the first part of presentation, the author will describe the optimization processes of such jets using computational fluid dynamics (CFD) tool. The second part will describe the development of the liquid jet sample delivery system for chemRIXS in LCLS. The chemRIXS endstation has been designed in a way it can take both solid and liquid samples. Because solid sample experiments require a UHV environment, to be able to deliver the liquid sample jets to the same vacuum chamber, a special loadlock chamber and sample transport system have been developed to isolate the liquid system from the main vacuum chamber. When solid sample system is extracted, a fully automated system can then drive the liquid jet to the sample/beam interaction point. A recirculation catcher will collect the liquid waste, so the chamber can remain at high vacuum.
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AS - ANSTO, Clayton, Australia
ANSTO, Menai, New South Wales, Australia
WEOB02
DESY, Hamburg, Germany
*Buffet et al., J. Synchr. Rad. 19 647, 2012
**Krywka et al., J. Appl. Cryst. 45 85,2012
***Santoro et al., Rev. Sci. Instr. 85 043901, 2014
****Schwartzkopf and Roth, Nanomaterials 6 239, 2016
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ESRF, Grenoble, France
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WEPB10
CEA, DES-ISAS-DM2S, Université Paris-Saclay, Gif-sur-Yvette, France
CEA, DES-ISAS-DMN, Paris-Saclay University, Gif-sur-Yvette, France
SOLEIL, Gif-sur-Yvette, France
CEA, DES-IRESNE-DEC, Université Paris-Saclay, Saint-Paul-Lez-Durance, France
Since the mid-2000s, the engineers and researchers of CEA and SOLEIL synchrotron facility have worked together to design a world unique beamline for the study of radioactive matter: MARS (Multi Analyses on Radioactive Samples Beamline)*. The facility works in the hard X-ray domain (between 3.0 and 35 keV) combining both X-ray spectroscopy and X-ray diffraction/scattering techniques on two end-stations: CX2 and CX3. MARS beamline is authorized by the ASN (French Nuclear Safety Authority) to analyze samples with radioactivities up to 18.5 GBq per sample for alpha and beta emitters and up to 2 GBq for gamma and neutron emitters. One of its main objectives is to be able to analyze these highly irradiating samples, such as spent nuclear reactor fuel or irradiated nuclear material (solid, liquid), to study their structural and chemical evolutions after irradiation. This article describes the components designed and realized with the major contribution of CEA to analyze such kind of samples: #1 air-tight sample holders; #2 positioning mechanical systems on the X-ray beam; #3 local analyzer devices; #4 two shieldings to safeguard users; #5 a mobile-shielded cask to transport samples.
*Sitaud, B. et al., H. Characterization of radioactive materials using the MARS beamline at the synchrotron SOLEIL. Journal of Nuclear Materials 425, 238-243 (2012).
WEPB11
SOLEIL, Gif-sur-Yvette, France
*Sitaud, B., Solari, P. L., Schlutig, S., Llorens, I. & Hermange, H. Characterization of radioactive materials using the MARS beamline at the synchrotron SOLEIL. J. Nucl. Mater. 425, 238-243 (2012).
MAX IV Laboratory, Lund University, Lund, Sweden
ForMAX is a new beamline at the MAX IV Laboratory for multi-scale structural characterization of hierarchical materials from nm to mm length scales with high temporal resolution. This is achieved by combining full-field microtomography with small- and wide-angle X-ray scattering (SWAXS) in a novel manner. The principal components of the endstation consist of two units of beam conditioning elements, a sample table, an evacuated flight tube and a detector gantry. The beam conditioning units include a diamond vacuum window, an attenuator system, a fast shutter, a slit collimation system, two sets of compound refractive lenses, three X-ray beam intensity monitors, a beam viewer and a telescopic vacuum tube. The sample table has been optimized with respect to flexibility and load capacity, while retaining sub-micron resolution of motion and high stability performance. The nine metre long and one metre diameter evacuated flight tube contains a motorised detector trolley, enabling the sample-detector position for small-angle X-ray scattering (SAXS) to be easily adjusted under vacuum conditions. Finally, a two metre high and two metre wide granite gantry permits independent and easy movement of the tomography microscope and wide-angle X-ray (WAXS) detector in and out of the X-ray beam. To facilitate propagation-based phase-contrast imaging and mounting of bulky sample environments, the gantry is mounted on motorized floor rails. All these characteristics will allow to combine multiple complementary techniques sequentially in the same experiment with fast efficient switching between setups. The ForMAX endstation is presently in the design and construction phase, with commissioning expected to commence early 2022.
LNLS, Campinas, Brazil
TARUMÃ is the sub-microprobe station of the CARNAÚBA (Coherent X-Ray Nanoprobe Beamline) beamline at Sirius Light Source at the Brazilian Synchrotron Light Laboratory (LNLS). It has been designed to allow for simultaneous multi-analytical X-ray techniques, including diffraction, spectroscopy, fluorescence and luminescence and imaging, both in 2D and 3D. Covering the energy range from 2.05 to 15 keV, the fully-coherent monochromatic beam size varies from 550 to 120 nm after the achromatic KB (Kirkpatrick-Baez) focusing optics, granting a flux of up to 1e11ph/s/100mA at the probe for high-throughput experiments with flyscans. In addition to the multiple techniques available at TARUMÃ, the large working distance of 440 mm after the ultra-high vacuum (UHV) KB system allows for another key aspect of this station, namely, a broad range of decoupled and independent sample environments. Indeed, exchangeable modular setups outside vacuum allow for in situ, in operando, cryogenic and/or in vivo experiments, covering research areas in biology, chemistry, physics, geophysics, agriculture, environment and energy, to name a few. An extensive systemic approach, heavily based on precision engineering concepts and predictive design, has been adopted for first-time-right development, effectively achieving altogether: the alignment and stability requirements of the large KB mirrors with respect to the beam and to the sample*; and the nanometer-level positioning, flyscan, tomographic and setup modularity requirements of the samples. This work presents the overall station architecture, the key aspects of its main components, and the first commissioning results.
* G.B.Z.L. Moreno et al. "Exactly constrained KB Mirrors for Sirius/LNLS Beamlines: Design and Commissioning of the TARUMÃ Station Nanofocusing Optics at the CARNAÚBA Beamline", presented at MEDSI’20, paper TUOB01, this conference.
ANL, Lemont, Illinois, USA
An enhancement design of an existing 26-ID nanoprobe [1] instrument (NPI) at APS is being completed as part of work for the APS-Upgrade (APS-U) project. As part of this enhancement design, a new vacuum chamber geometry configuration has been implemented that balances the desired simultaneous x-ray measurement methods with accessibility and serviceability of the nanoprobe. The main enabling feature on the vacuum chamber is a slanted mid-level vacuum sealing plane. The new chamber design geometrically optimizes the ability to perform simultaneous diffraction, fluorescence and optical or laser pump probe measurements on the sample. A large diffraction door geometry is strategically placed near the sample for ease of access. The newly designed chamber can be readily serviced by removal of the upper chamber section, on which most larger instrument assemblies or beamline attachments are not interfaced. The mechanical design intent and geometry of this chamber concept is described in this paper.
WEPC01
ANL, Lemont, Illinois, USA
The COVID-19 pandemic has resulted in a highly increased need for remote beamline operations. Usually, in situ X-ray scattering experiments require significant onsite user and beamline staff presence, making them difficult and often impractical during limited operations. One of the major problems was the switching of capillary samples for in situ heating/cooling experiments. Therefore, we developed a specialized robotic system for changing samples utilizing easily accessible standardized parts and 3-D printing. The first version of this design is fully operational and has been installed at the 17-BM beamline. This system allows for changing between 14 capillary based samples by using three stepper motor based translational stages and pneumatic gripper. The destination can be intercrossed with hot or cold air blower stream, allowing users to remotely collect X-ray powder diffraction data from multiple samples at various temperatures. Currently, we are working on the development of a second robotic system, which will fit entirely onto one breadboard. This will allow us to move the system from one beamline to another if needed. The second piece of instrumentation we have developed is a remotely operated beam attenuation system with adjustable attenuation level. The system uses electric solenoids that push tantalum foils in and out of the beam. Five solenoids each hold different numbers of foils, and can be controlled independently, allowing for a total of 32 unique attenuation levels. A 6th solenoid holds a beamstop which can be used as a fast shutter. The control and communication is performed by an Arduino Yun microcontroller. All structural parts were 3-D printed, making for a cost-effective alternative to systems currently on the market.
LNLS, Campinas, Brazil
TARUMÃ is the sub-microprobe station of CAR-NAÚBA (Coherent X-Ray Nanoprobe Beamline) at Sirius at the Brazilian Synchrotron Light Laboratory (LNLS). Covering the tender-to-hard energy range from 2.05 to 15 keV with achromatic fixed-shape optics, the fully coherent submicron focused beam can be used for multiple simultaneous advancedμand nanoscale X-ray techniques that include ptychography coherent diffraction imaging (ptycho-CDI), absorption spectroscopy (XAS), diffraction (XRD), fluorescence (XRF) and luminescence (XEOL). Among the broad range of materials of interest, studies of light elements present in soft tissues and other biological systems put TARUMÃ in a unique position in the Life and Environmental Sciences program at LNLS. Yet, to mitigate the detrimental effect of the high photon flux of the focused beam due to radiation damage, cryocooling may be required. Here we present the design and first results of a novel open-atmosphere cryogenic system for online sample conditioning down to 110 K. The high-stiffness and thermally-stable sample holder follows the predictive design approach based on precision engineering principles to preserve the nanometer-level positioning requirements, whereas a commercial nitrogen blower is used with a cold gas flow exhaustion system that has been developed in order to avoid unwanted cooling of surrounding parts and water condensation or icing.
LNLS, Campinas, Brazil
UNICAMP, Campinas, São Paulo, Brazil
CARNAÚBA (Coherent X-Ray Nanoprobe Beamline) is a state-of-the-art multi-technique beamline at the 4th-generation Sirius Light Source at the Brazilian Synchrotron Light Laboratory (LNLS), with achromatic optics and fully-coherent X-ray beam in the energy range between 2.05 and 15 keV. At the TARUMÃ station, the in-vacuum KB focusing system has been designed with a large working distance of 440 mm, allowing for a broad range of independent sample environments to be developed in open atmosphere to benefit from the spot size between 550 to 120 nm with a flux in the order of 1e11 ph/s/100mA. Hence, together with a number of different detectors that can be simultaneously used, a wide variety of studies of organic and inorganic materials and systems are possible using cutting-edge X-ray-based techniques in theμand nanoscale, including coherent diffractive imaging (CDI), fluorescence (XRF), optical luminescence (XEOL), absorption spectroscopy (XAS), and diffraction (XRD). Even though samples over the centimeter range can be taken at Tarumã, the small beam and relatively low energies point towards optimized and reduced-size sample holders for in situ experiments. This work describes two related setups that have been developed in-house: a small-volume electrochemical cell with static fluid*; and another multifunctional environment that can be used both as a microfluidic device and as an electrochemistry cell that allows for fluid control over samples deposited on a working electrode. The mechanical design of the devices, as well as the architecture for the fluid and electrical supply systems, according to the precision engineering concepts required for nanopositioning performance, are described in details.
*Vicente, Rafael A., et al., "Bragg Coherent Diffraction Imaging for In Situ Studies in Electrocatalysis," ACS nano (2021).
CLS, Saskatoon, Saskatchewan, Canada
A compact X-ray emission spectrometer (mini-XES) has been designed and fabricated for use at the Brockhouse undulator beamline*. The mini-XES uses cylindrical von Hamos geometry tuned for Fe K-edge and uses a Pilatus 100 K area detector from Dectris**. It is based on a general design implemented at the APS***. The mini-XES design was developed to be as simple to fabricate and as easy to operate as possible. We tried to minimize the number of components, so there are only two main parts that create a chamber. Those two components are joined and aligned by a NW-80 flange. From the beginning, the design was trying to achieve no tools assembly, alignment, and operation. For lower precision alignment we decided to use the centering ring of the NW-80 flange which, together with two posts integrated with the chamber, provides an adequate method for joining the two parts of the enclosure. We use level vials for horizontal adjustment of the holder for the 10 crystals. For high precision alignment of the holder of the crystal, we used the Thorlab KC1/M kinematic mount, which had the adjustment screws accessible from outside of the chamber. The fabrication was done in-house using uPrint SE Plus 3D Printer****. The first tests of the spectrometer were completed in the Brockhouse wiggler beamline and were successful. Future improvements will aim to reduce the background scatter and better position the detector, to improve the fill. Now that the relatively inexpensive design was tested and tried, there is an option to upgrade it to 3D printed tungsten or steel version that would intrinsically provide the required shielding.
* B. Diaz et al., Rev. Sci. Instrum 85, 085104 (2014)
** https://www.dectris.com
*** B. A. Mattern et al., Rev. Sci. Instrum 83, 023901 (2012)
**** https://support.stratasys.com
BNL, Upton, New York, USA
NYIT, Old Westbury, New York, USA
SBU, Stony Brook, New York, USA
BNL, Upton, New York, USA
Open Platform and Liquids Scattering (OPLS) is a new experimental station recently built and currently being commissioned at the Soft Matter Interfaces (SMI) beamline 12-ID at NSLS-II. The new instrument expands SMI’s beamline scientific capabilities via the addition of X-ray scattering techniques from liquid surfaces and interfaces. The design of this new instrument, located inside the 12-ID beamline shielding enclosure (hutch B), is based on a single Ge (111) crystal deflector, which bounces the incident x-ray beam downward towards a liquid sample which must be maintained in a horizontal orientation (gravity-driven consideration). The OPLS instrument has a variable deflector-to-sample distance ranging from 0.6 m to 1.5 m. X-ray detectors are mounted on a 2-theta scattering arm located downstream of the sample location. The 2-theta arm is designed to hold up to three X-ray detectors, with fixed 2-theta angular offsets, each dedicated to a different X-ray technique such as X-ray reflectivity, grazing-incidence X-ray scattering, and small- and wide-angle X-ray scattering. Currently, the OPLS experimental station intercepts the SMI beam that otherwise propagates to the experimental endstation located in hutch C and can be retracted to a ’parking’ position laterally out of this beam to allow installation of a removable beam pipe that is needed to support operations in hutch C. The design of OPLS is flexible enough to quickly adapt to a planned future configuration of the SMI beamline in which a OPLS is illuminated separately from the main SMI branch via a second, canted undulator source and a separate photon delivery system. In this future configuration, both branches will be able to operate independently and simultaneously.
ANL, Lemont, Illinois, USA
The X-ray Photon Correlation Spectroscopy (XPCS) beamline at the Advanced Photon Source (APS) has been selected as one of the nine feature beamlines being de-signed to take advantage of the increase in coherent flux provided by the APS Upgrade. The 8-ID-E enclosure at the beamline will have a dedicated instrument for per-forming Wide Angle XPCS (WA-XPCS) measurements across a range of length and time scales. The instrument will feature a high-stability 6-circle diffractometer, a moveable Long Distance Detector Positioner (LDDP) for positioning a large pixel array detector, and a removable flight path assembly. For intermediate sample to detector distances of 1.5 to 2 meters, a large pixel array detector will be positioned on the diffractometer detector arm. For longer sample to detector distances up to 4 meters, an horizontal scattering geometry will be utilized based on the LDDP to position a second large pixel array detector. The LDDP will consist of a large granite base on which sits a combination of motorized stages. The base will sit on air casters that allow the LDDP to be coarsely posi-tioned manually within the enclosure. Final positioning of the detector will be achieved with the mounted stages. The spatial relationship between the sample and the free moving LDDP will be monitored using a laser tracking system. A moveable flight path will be supported by the diffractometer arm and a mobile floor support to mini-mize air scattering while using the LDDP. The WA-XPCS instrument has been designed with users and beamline staff in mind and will allow them to efficiently utilize the highly enhanced coherent beam provided by the APS Upgrade.
WEPC15
ANL, Lemont, Illinois, USA
Over the last two years, we have developed a 3D printed nylon mesh holder for serial synchrotron crystallography (SSX) experiments. We are moving away from the complications in some devices to a cheap, easy, and user-friendly format. The device uses a new, patented*, two-layer (one rigid and one flexible) substrate technique developed at Argonne. The SSX device and method, which incorporates a modular high-performance computing data analysis backend, was used to demonstrate never-before-seen molecular dynamics** and discovered the methylated form of the SARS-CoV-2 Nsp10/16 protein*** complex. Named ALEX (Advanced Lightweight Encapsulation for Crystallography) for short, we are actively using, upgrading, and reaching out to collaborators. We are using ALEX for serial experiments at APS but feel the design might be useful for other applications.
* Patent #16/903, 601
** Currently in writing stage
*** Accepted for publication