Facilities

University of Illinois Chicago

CDAC Laboratories

Renovated laboratory and office space has been committed to the program (4500 ft2 space in total). All laboratories meet requirements for climate control, power and cooling water needs for specific instruments. The dedicated laboratory spaces used for each of two Raman spectroscopy setups, one Brillouin spectroscopy setup, and a laser heating apparatus. In addition, sample preparation facilities are located in a wet chemical laboratory that is equipped with fume hoods. The sample preparation laboratory includes microscopes, gasket drills (mechanical, laser, and spark erosion), pressure calibration systems, and gas and cryogenic loading devices. The space we occupy started as a functioning optical laboratory with eight research-grade optical tables. This laboratory facility was reconfigured and repurposed for our specific needs, is managed by CDAC research faculty and is available for research and training purposes for personnel throughout the Center.

Research Resources Center and Chicago Biomedical Consortium

The main UIC campus and the medical campus combine to house the Research Resources Center, which includes an extensive collection of state-of-the-art imaging, characterization and nanotechnology facilities that are available on a user fee basis. These laboratories are fully staffed with skilled professional instrument scientists that are available for consultation as well as comprehensive training. For instrumentation that is not available at the UIC location, the Chicago Biomedical Consortium provides additional capabilities at Northwestern University and The University of Chicago at internal user rates.

Brookhaven National Laboratory

National Synchrotron Light Source II

Synchrotron IR is an important tool in CDAC. In the early 1990’s, the CDAC Director developed the field of high-pressure synchrotron IR microspectroscopy, which takes advantage of the high flux of synchrotron radiation at long wavelengths.  This program was begun at NSLS U2A and has transitioned to the Frontier Synchrotron Infrared Spectroscopy (FIS) beamline facility at the NSLS-II, and is managed by UIC Research Professor Zhenxian Liu and funded by NSF and DOE-NNSA through CDAC. The FIS facility has custom-built, long-working distance IR microscopes for diffraction-limited high P-T IR spectroscopy, as well as Raman spectroscopy and laser heating. With new developments/upgrades implemented, the facility allows a wide range of micro-spectroscopic studies at broad range of pressures (to over 300 GPa) and temperatures (from 5 K to several thousand K). Coupled with the synchrotron IR radiation, this facility provides diffraction-limited observation of DAC samples in cryostats or under laser heated hot spots from the far to mid-IR spectral range. We have guaranteed beam time at the FIS facility for the proposed research as a result of our management and funding of operations of the beamline.  FIS also serves as a focal point for expanding extreme conditions science to other NSLS-II beamlines, including x-ray beamlines that will be used during the downtime at the APS for its upgrade.

  • End Station A is a dedicated facility for experiments at simultaneous high P-T experiments utilizing the DAC and external and laser heating techniques. Major equipment at this laser-interlocked end station includes a new Vertex-80 FTIR spectrometer, a custom IR microscope with long working distance objective, a 100W CO2 laser, an integrated optical system for temperature calibration, and a portable ruby system for pressure calibration.

  • End Station B is a dedicated facility for experiments at high pressure and low temperature using DACs and cryogenic techniques. The core equipment consists of a Bruker Vertex 80v FTIR spectrometer equipped with a Bruker Hyperion IR microscope, a new custom IR microscope with long working distance (40 mm) and large numerical aperture (0.5), a custom micro-Raman system, and a full range of optics and accessories capable of complete IR/visible characterization. The diamond window and vacuum optics have extended the accessible spectral range to the far IR (to 10 cm-1).

Argonne National Laboratory

HPCAT, Advanced Photon Source

The Advanced Photon Source (APS) is a third-generation high-energy synchrotron x-ray facility at Argonne National Laboratory and is a critical resource for the proposed research program. Experiments relevant to the proposed work may be performed at several different sectors within the APS. Most of the proposed experiments will take place at the dedicated high-pressure sector, HPCAT (Sector 16), which is a principal component of our high pressure program. HPCAT is dedicated to providing state-of-the-art x-ray capabilities in extreme conditions science. The full spectrum of high-pressure x-ray experiments can be performed at this facility, including high P-T powder diffraction with laser and resistive heating, single-crystal x-ray diffraction to megabar pressures, and a variety of inelastic scattering experiments. With accurate control of the electron bunch length and spacing between bunches, the APS offers many possible operational modes ideally suited for probing dynamical processes under extreme conditions. These studies complement shock-wave studies with fourth-generation hard x-ray free-electron lasers (e.g., LCLS-II) which offer a short, brilliant pulse. APS has beamlines optimized for time-resolved, x-ray diffraction, EXAFS, along with ultrafast, high-intensity diagnostic lasers. In addition, new x-ray spectroscopy methods include nuclear resonant x-ray spectroscopy of different Mössbauer elements and resonant or non-resonant x-ray emission spectroscopy, including capabilities for studying the dramatic effects of pressure on strongly correlated d- and f- electron systems.

The APS upgrade (APS-U) combined with that of HPCAT will add to the capabilities of future research on the proposed topics. On the other hand, the upgrade will require shut down of the storage ring and termination of the synchrotron x-ray experiments for a year starting in July 2022, according to current plans. Although this will preclude access to the x-ray beamline facilities that we have helped create and use during this time, we will be able to use the supporting laboratories for many experiments. During this time we will use other synchrotron x-ray sources, including the NSLS-II and PETRA III for x-ray diffraction and spectroscopy experiments.

Once the upgrade is complete, APS-U will allow experiments with improved temporal resolution by 2-3 orders of magnitude, and will enable and optimize time-resolved techniques to study kinetics and mechanisms of physical and chemical processes with a resolution ranging from sub-micro-seconds to hours. The improvement will enable further studies of the dynamics of fundamental transformations (e.g., melting, phase transitions, metastability) and transport properties (e.g., diffusivity, conductivity) under extreme conditions. HPCAT-U will also improve spatial resolution by an order of magnitude. Development of sub-µm to nm x-ray high pressure probes at HPCAT will expand the characterization of materials in an expanded P-T range, and in so doing, advance our understanding the origin of pressure-induced superconductivity, ferroelectricity, colossal magnetoresistivity, phonon softening, Fermi-surface nesting, d-electron spin pairing, f-electron delocalization, and insulator-metal and metal-insulator transitions. The development of the x-ray microscopy technique at HPCAT also creates a new tool with important implications for the proposed project.

  • An extensive array of instrumentation has been developed, implemented, and commissioned at HPCAT allowing a full spectrum of measurements on high-pressure samples. X-ray emission spectroscopy provides information on the filled electronic states of molecules and solids. X-ray Raman spectroscopy probes pressure-induced chemical bonding changes in light elements. Medium-resolution (0.1-1 eV) inelastic x-ray scattering spectroscopy accesses high-energy electronic phenomena, including the electronic band structure, Fermi surface, excitons, plasmons, and their dispersions. Element-specific x-ray absorption near-edge spectroscopy reveals information on oxidation state, magnetic spin, crystal-field energy, and chemical bonding changes, while extended-edge x-ray absorption fine structure reveals atomic coordination at high pressure. Resonant inelastic x-ray scattering spectroscopy probes shallow core excitations, multiplet structures, and spin-resolved electronic structure. Nuclear resonant inelastic x-ray spectroscopy provides the phonon density of states and thermodynamic information on Mössbauer elements, and nuclear resonant x-ray forward scattering is a Mössbauer absorption measurement in the time domain. These tools, coupled with x-ray diffraction, optical spectroscopy, and electromagnetic probes, hydrostatic or uniaxial pressure media, laser and resistive heating and cryogenic cooling capabilities have enabled integrated investigations of structural, vibrational, electronic, and magnetic properties at a full range of extreme conditions. A detailed description of the equipment available in each of the four stations is given below.

    16-ID-D: Spectroscopy Station. The ID-D station is dedicated to x-ray spectroscopy of materials under high pressure, with a typical beam size at the sample position of 20 (v) x 50 (h) μm2. The sample stack can accommodate heavy devices such as cryostats and external heaters. An on-line spectrometer system is available for Raman and pressure measurements. The station employs a Bruker liquid nitrogen-cooled Si (111) double crystal monochromator with 2 meV energy resolution, and energy from 4.5 – 35 keV. Focusing to 4 mm (v) x 6 mm (h) μm2 is achieved with 320 mm x 400 mm IDT KB mirrors. Established techniques include:

    • Nuclear Resonant Inelastic and Nuclear Forward Scattering

    • Inelastic and X-Ray Raman Scattering

    • Resonant and Non–Resonant X-Ray Emission Spectroscopy

    • Partial Fluorescence Yield X-Ray Absorption Spectroscopy

    With NRIXS at HPCAT, one can study sound velocities, magnetism and phonon density of states of materials under high pressure and at high to cryogenic temperatures. XES yields information about inner-shell and valance band electronic structure, bonding delocalization of electrons and magnetic properties in materials at high pressure. The emission spectrometer employs a spherically bent, 17-element, silicon analyzer of 1-meter radius, in near-backscattering geometry. HPCAT also has the capability for resonant emission as well as resonant inelastic x-ray scattering. X-ray Raman spectroscopy probes the nature of bonding in compounds; elements such as oxygen, nitrogen, carbon and boron have been studied at high pressures. Also, electronic excitations such as the collective plasmon excitations as well as single-particle excitations can be studied at HPCAT. This sort of inelastic x-ray scattering reveals information on the dielectric response function of materials under high pressure. At present 16-ID-D has a dedicated backscattering spectrometer with about 1 eV energy resolution. Capabilities for higher resolution spectroscopy are continuously being developed.

16-ID-B: Micro-Diffraction Station

The ID-B station has been configured into two major setups, one for general purpose micro-diffraction, and the other dedicated for laser heating experiments. Although the station is optimized for powder diffraction measurements in the diamond anvil cell, high pressure single crystal diffraction may also be carried out conveniently. This two-table configuration in ID-B provides the necessary space and stability for a wide variety of different micro-diffraction applications (Fig. I-3). On the laser heating table, the laser-heated DAC is combined with micro-focused synchrotron x-ray diffraction and allows the opportunity for structure-related studies of materials in-situ under ultrahigh P-T conditions. The integrated system at HPCAT combines YLF laser heating, resistive heating and micro-focused x-ray diffraction with either an imaging plate or CCD detector. The laser heating unit employs a double-sided arrangement with two identical Nd:YLF lasers (Photonics GS40, TEM01 mode, wavelength = 1053 nm), providing a total maximum output of 170 W with a power stability > 99%. For most applications, the laser is focused to a spot of ~ 30 μm; temperatures are measured on a sample area of 4×4 μm2 using an Inspectrum 300 imaging spectrograph equipped with a thermoelectric-cooled back-illuminated Hamamatsu CCD (1024 x 250 pixels), from both sides of the sample. By aligning an x-ray beam coinciding with the laser heating spot, x-ray diffraction can be carried out at simultaneous high pressures and temperatures. The typical x-ray beam size at the sample is 5×5 µm2. In addition to these state-of-the-art techniques, control systems have been developed for easy, efficient and safe operations. This system has been used for x-ray diffraction studies of a wide range of materials to over 200 GPa and above 3000 K.

The general purpose table is designed for angle dispersive diffraction measurements with a monochromatic beam, and is capable of holding bulky and heavy equipment (e.g. cryostat, graphite resistive heating assembly, large high-pressure cells) and with minimum space restrictions. The open structure and flexibility of the general purpose table allows easy modifications for performing especially demanding experiments (e.g. single crystal measurements) and the development of new techniques (e.g. high-resolution diffraction with point detectors). Double-diaphragm and piezoelectric pressure control is available for time-resolved diffraction experiments. The standard equipment on the general purpose table includes:

  • A pair of 200 mm KB mirrors with a cleanup pinhole, providing a clean pseudo-Gaussian beam of 6×6 μm2 at FWHM. On demand the beam can be focused past the sample position or on the detector plane to minimize divergence or increase resolution, or just defocused for uniform sample illumination. For experiments requiring a large, low-divergence, unfocused beam the KB mirrors can be moved away.

  • A heavy-duty sample stack with ample traveling range and high load capacity of 100+ kg. The sample stack has four linear and two rotational degrees of freedom. The sample stack normally is equipped with a kinematic heavy-duty cryostat or standard DAC mounting assembly, which can easily be replaced with additional stages for specific experiments (e.g. four-circle diffractometer for single crystal measurements, or combined x-y-w stage for side diffraction experiments).

  • Two area detectors: MAR345 IP and MAR CCD. The standard sample-to-detector distance varies from 250 to 1100 mm, but can be changed beyond that. The horizontal tilt and position of the MAR345 IP can be easily changed to maximize the range of collected diffraction angles and optimize the quality of the spectra by minimizing the point spread function (by adjusting the horizontal tilt of the IP). The Pilatus detector is also available on request.

  • The BM-D station is fully operational for micro x-ray diffraction and x-ray absorption spectroscopy (Fig. I-4). The station features a Si (111) double crystal monochromator in pseudo-channel cut mode and normally operates at 6-45 keV but can be configured to operate up to 60-70 keV on request. Focusing to 5 µm x 5 µm FWHM is achieved with 320 mm Pt-coated Si KB mirrors. Techniques commissioned on the beamline include:

    • ADXD at simultaneous high P and high T or high P and low T

    • Single crystal diffraction with the multigrain method

    • Radial ADXD for stress-corrected cell parameters, texture and strength of materials at high pressure in the DAC that has been adapted with a membrane drive.

    • X-ray absorption spectroscopy with ion chamber capability

    Both external resistive heating and cryostat operations have been commissioned on the beamline.

  • The BM-B station is dedicated for the use of a white beam with third generation characteristics. A channel-cut Si (111) monochomator delivers a focused beam at 5-70 keV with a focus of 5 µm x 5 µm FWHM using a 200 mm Rh-coated Si KB mirror. Both white-beam Laue diffraction with the DAC and studies with the Paris-Edinburgh press have been commissioned. Liquid viscosity measurements with white-beam radiography and ultrasonic elastic wave velocity measurements can also be performed. The instrument allows changing the distance between the focusing optics and sample, with flexible focused beam sizes from 5 μm to 15 μm or larger depending on experimental requirements. Special features of the beamline include:

    • Five-dimensional remote control for pinhole and tip (x, y, z, pitch and yaw)

    • Gas driven membrane control of pressure for diamond anvil cells

    • Low temperature experiments to liquid He temperature

    • Point-detector (Ge detector) and area-detector (MarCCD) operation

    • Automatic liquid nitrogen refill system for Ge detector

    • Paris-Edinburgh type large volume press with resistive heating capacity (PE anvils, boron-epoxy gaskets, cylindrical graphite heater, 8V-220A power supply; temperature and pressure range up to 1300 K under 10 GPa or 2200 K under 7 GPa)

Two auxillary laboratories at HPCAT house a fully-equipped high-pressure facility that includes sample loading and characterization, complementing the main HPCAT laboratories at Sector 16. Apart from microscopes for aligning diamond cells, diamond polishing and shaping facilities, fume hood, gas loading system capable of loading H2 (in addition to a number of other inert gases), specialized coil winding for magnetic measurements, DC and AC conductivity measurement systems, multi-wavelength Raman spectroscopy system (660 nm, 488 nm and 532 nm) equipped with ultra narrow-band notch filters make these laboratories a self-contained facility for training and ex-situ measurements. These facilities complement those available at UIC and are available for use through the UIC-HPCAT MOU referred to above.

Academic Partner Laboratories

Each of the six Academic Partners in CDAC operates laboratories that support their individual scientific programs, and each has access to university-wide facilities and resources at the respective home institutions. The CDAC Academic Partners make their laboratories available for Center personnel to engage in collaborative research efforts and promote cross-disciplinary research and training. Specialized facilities at each partner institution are unique and provide exceptional training opportunities for graduate students and postdoctoral researchers.

Dorfman Laboratory / Michigan State University

In addition to the specialized facilities in the Dorfman Laboratory, the Department of Earth and Environmental Sciences at MSU complete sample preparation equipment including fume hood access. Additional capabilities are available in MSU’s Composite Materials and Structures Center. The MSU Center for Advanced Microscopy provides polishing and ion milling systems capable of machining samples to nm tolerances for microscopy and elemental analysis. The MSU Fraunhofer Center for Coatings and Diamond Technologies commissioned a split-sphere multianvil press for high-pressure synthesis in summer 2016, and provides facilities for diamond growth and machining including carbon-vapor deposition and laser polishing systems. Starting materials may also be synthesized in controlled atmosphere furnaces in the MSU Solid State Ionics Laboratory. Compositions of samples can be determined by wavelength-dependent X-ray fluorescence using the Bruker S4 PIONEER instrument in the laboratory of Dr. Tyrone Rooney. An additional, energy-dispersive XRF system is available in the Department of Chemistry. Trace elements may also be analyzed in the Rooney laboratory by laser inductively-coupled plasma mass spectroscopy for microprobe composition analysis, two Cameca electron microprobes (SX-100, MBX) are available at the R.B. Mitchell Electron Microbeam Analysis Laboratory, a user facility at the University of Michigan. X-ray diffractometers are available at MSU on a fee basis from the MSU Chemical Engineering and Materials Science Teaching Laboratory and the MSU Chemistry Department Center for Crystallographic Research; powder, thin film and single-crystal capabilities are available. Phases may also be identified by Raman spectroscopy using the Horiba Aramis Raman confocal microscope/spectrometer at the CMSC, equipped with visible, near-IR and UV lasers and both Peltier-cooled and liquid-N2-cooled CCD detectors.

Ertekin Laboratory / University of Illinois at Urbana-Champaign

UIUC has extensive computational facilities available to the Ertekin group, including the University of Illinois Shared Computing Cluster, which includes 52 compute nodes and 624 compute cores. Nodes are connected by a high-bandwidth, low-latency Voltaire QDR Infiniband network for high-performance scalability. The Blue Waters Petascale Computing Project at the National Center for Supercomputing Applications at UIUC, for which 7% of the computing time is allocated to faculty access. Other computational resources are available through other supercomputing user centers such as the NERSC and XSEDE.

Jacobsen Laboratory / Northwestern University

The Mineral Physics Laboratory at Northwestern University houses an extensive array of sample preparation and characterization capabilities housed in over 1000 ft2 of newly-renovated laboratory space adjacent to the Technological Institute. Also available are the Northwestern University Atomic and Nanoscale Characterization Experimental Center and the Northwestern University Materials Research and Engineering Center. The Electron Probe Instrumentation Center houses both SEM and TEM capabilities along with a FIB instrument. The Keck Interdisciplinary Surface Science Facility and the Nanoscale Integrated Fabrication, Testing and Instrumentation Facility and Optical Microscopy and Metallography Facility also house additional specialized facilities for materials characterization. Many of the facilities at Northwestern are accessible through the Chicago Biomedical Consortium.

Lang Laboratory / University of Tennessee-Knoxville

UTK benefits from a very close relationship with Oak Ridge National Laboratory (ORNL). The ORNL Spallation Neutron Source (SNS) and 85 MW High Flux Isotope Reactor (HFIR) provides unique capabilities for neutron scattering experiments. Several other user facilities are available, such as the ShaRE Shared Research Equipment User Facility (TEM characterization) and the CNMS Center for Nanophase Materials Sciences (thin-film synthesis). In addition, the state-of-the-art microscopy capabilities at the ORNL, Advanced Microscopy Laboratory, are available through existing collaborations, as well as the computational resources of the UTK-ORNL Joint Institute for Computational Sciences. Access to these facilities will be available through user proposals and collaborations with the Joint Institutes for Computational Science (JICS), Advanced Materials (JIAM) and Neutron Sciences (JINS). On the UTK campus, the Lang group operates a general sample preparation laboratory, a high pressure-temperature laboratory and an analysist laboratory. At ORNL, the Lang group has access to the Nanoscale-Ordered Materials Diffractometer at the SNS. In addition, the Lang group has an ongoing collaboration with the Helmholz Center for Heavy Ion Research in Darmstadt, Germany, which includes all of the necessary instrumentation for irradiation of samples.

Miyagi Laboratory / University of Utah

The Miyagi laboratory contains complete facilities for the preparation of samples high pressure experiments using diamond anvil cells. In addition, the group has access to the Utah Nanofab Facility, which houses FIB/SEM and TEM instruments for sample characterization. Radial diffraction experiments are carried out at Beamline 12.2.2 at the Advanced Light Source, Lawrence Berkeley National Laboratory. Shock compression experiments are performed at the Matter in Extreme Conditions End Station of the Linear Coherent Light Source’s free electron laser. Each of these off-site laboratories has extensive sample preparation laboratories that are available for use by the group.

Zurek Laboratory / University at Buffalo

Facilities available for use by the Zurek group include a dedicated cluster, which is maintained by the university’s Center for Computational Research (CCR), which also maintains a Linux Cluster with 8000 processors, which is also available for more demanding computational work. The Zurek group has fully equipped office space that allows for 12 full time coworkers. The group has sufficient space to host visitors from across the Center for joint theory-experimental research collaborations, which have become an increasingly important part of the CDAC program since Professor Zurek joined the group of Academic Partners in 2013.