Instrumentation

 

Group's Instrumentation

  1. Bruker Avance NMR (400 MHz for 1H).
  2. Bruker Kappa Apex II diffractometer.
  3. Laser transient absorption facility. Laser excitation in UV and visible: Continuum Leopard SS-10-SV Nd/YAG, 60 ps pulse; Continuum Powerlite 7010 Nd/YAG, 6 ns pulse (266 nm, 355 nm, 532nm), Opotek Vibrant LD 355 II OPO, 6 ns pulse (410 – 2650 nm continuously). Detection in Uv-Vis-NIR at single wavelength with Xe lamp probe (260 – 800 nm, time resolution ca. 100 ps with biplanar tube; 400 – 1600 nm, time resolution 2-3 ns with diode detectors; 260 – 800 nm, time resolution 2-3 ns with PMT). Detection in MIR, spectral region with step-scan FTIR FT-IRS-66/V (4500 – 400 cm-1), time resolution ca. 35 ns, single wavelength with Quantum cascade lasers (2317-2197, 2235-2105, 2230-2020, 2072-1977, 1981-1873, 1903-1774, 1813-1692, 1670-1536, 1395-1306, 1258-1181 and 1135-1051 cm-1), time resolution ca. 5ns. Transient digitizers available: LeCroy HDO4034 350 MHz 12-bit; LeCroy 8620A 6 GHz; Tek DPO 4032 350 MHz; Tek DPO 4054B 500 MHz.
  4. Optical spectroscopy instruments. Resonance Raman spectrometer with Ar-Kr ion laser source (457.9 nm, 476.5 nm, 488.0 nm, 514.5 nm, 530.9 nm, 568.2 nm, 647.1 nm, 752.5 nm). Diode array spectrophotometers (3 HP 8452, 2 Agilent 8453). One spectrometer is equipped with RX-2000 rapid mixing system for stopped flow measurements on millisecond time scale. Cary 5 UV-Vis-NIR spectrophotometers. Thermo Scientific Nexus 670 FTIR spectrometer. High-pressure spectroscopic cells for UV-VIS-NIR-IR spectroscopy up to 5000 psi (34.5 MPa), together with associated gas filling station equipped with Teledyne ISCO high-pressure syringe pumps. Precision Detectors dynamic light scattering system. Specac variable temperature IR cell for IR spectroscopy in the range –190 to 250 °C. Specac infrared spectro-electrochemical cell for FTIR spectro-electrochemical measurements. Oxford Instruments OptistatDN-V cryostat for optical spectroscopy down to –196 °C.
  5. Chromatography and mass-spectrometry instruments. Hewlett-Packard 5890 GC with flame ionization and thermal conductivity detectors; Agilent 6890N GC with flame ionization and thermal conductivity detectors; Agilent 6890N GC-MS; Thermo-Finnegan LCQ Advantage LC-MS; Ion Chromatograph Dionex ICS-1600; Stanford Research System QMS 300 mass-spectrometric gas analyzer equipped with a custom batch gas sampling vacuum system.
  6. Four inert atmosphere dryboxes (one is equipped for electrochemical and UV-vis measurements) and one “wet-box” (air-free but equipped for aqueous chemistry).
  7. MARS 6 Microwave Accelerated Reaction System (CEM Corporation). Beckman Coulter Allegra 64R centrifuge. High pressure autoclaves (three Parr and one Autoclave Engineers, for pressures up to 5000 psi). Glass Contour solvent purification system.
  8. Continuous photolysis systems with various light sources (Xe Arc lamps 75 and 150W, laser diodes, Ar-Kr ion laser).
  9. Electrochemical instrumentation. CHI bipotentiostat; 2 BASi bipotentiostats; 2 BASi potentiostats; PAR VERSASTAT3-200 potentiostat; 2 Pine Research MSR rotators for RDE and RRDE measurements.
  10. Optical probe-based (Ocean Optics) and Clark electrode (YSI 5300A) dissolved/gaseous oxygen measurement systems.
  11. Applied Photophysics DX-18MV sequential stopped-flow system with a diode array option.
  12. Computing Instrumentation: Six quad-core AMD Opteron workstations with 64 cores and 256 GB of memory (ford), One quad-core AMD Opteron workstations with 48 cores and 128 GB of memory (marvin), One quad-core AMD Opteron workstations with 32 cores and 128 GB of memory (arthur), Eight quad-processor quad-core AMD Opteron clustered workstations with 64 GB of memory (trillian/fenchurch), Sixteen dual-processor dual-core AMD Opteron clustered workstations with 16 GB of memory (earth/krikkit). In addition, J. T. Muckerman and his collaborators have access to the Computational Cluster at the BNL CFN through user proposals. Ample personal computers are available for word processing, graphics and laboratory instrument control.

 

BNL Chemistry Department Facilities and Instrumentation

Brookhaven’s Center for Radiation Chemistry Research (ACER) is located in BNL's Chemistry Department. It includes a 60Co gamma-source (0.5 MRad / hr.), a 2 MeV Electron Van de Graaff accelerator with transient absorption detection on the full UV-Vis spectral range (200-800 nm, time resolution ~40 ns), and the Laser-Electron Accelerator Facility (LEAF) based upon a 9 MeV RF photocathode electron gun accelerator. A regeneratively-amplified femtosecond laser system provides 266 nm illumination of the photocathode and other wavelengths (800 nm fundamental, 400 nm second harmonic, and 240-2600 nm by optical parametric amplification) for probe beams. Transient absorption detection systems at LEAF include a pulse-probe apparatus (resolution ~7 ps, 240-1600 nm), an ultrafast-single-shot apparatus (resolution ~10 ps, 400-950 nm) and a digitizer-based apparatus (detector dependant resolution from 150 ps to 5 ns, from 250-2500 nm). A spectrally resolved pulse-probe experiment is planned (resolution ~7 ps, 450-1600 nm).

Other Equipment Available at the Chemistry Department. RXM-100 unit for the characterization of high-surface area catalysts and powders (including instrumentation for the determination of surface areas, temperature programmed reduction or oxidation, a couple of flow reactors for catalytic tests, and reaction products analysis by a mass spectrometer or gas chromatograph); Molecular Beam apparatus with triply-differentially pumped beam source, UHV scattering chamber with integral mass spectrometer and sample preparation and characterization tools (LEED, AES, TPD, PVD); Surface photochemistry apparatus with surface science characterization and sample preparation tools (TPD, AES, LEED), VUV laser source, and time-of-flight mass spectrometer with ion imaging for spatial distributions; Nanoparticle deposition apparatus with gas-phase nanocluster ion source, ion transport and mass selector, UHV sample chamber with surface characterization (UPS/XPS, AES, TPD, 2PPE);.Four UHV chambers with diverse instrumentation for surface characterization (LEED, UPS, XPS, AES, TPD, ISS. They allow detailed studies of chemical reactions on solid surfaces); Variable temperature scanning tunneling microscope that allows cooling of the surface to 30 K and heating to 800 K; Varian AA240FS atomic absorption spectrometer; Ocean Optics Fiber Optic Oxygen Sensor System with computer-controlled Hamilton Microlab 500 Series flow-mixing sample delivery system; and a whole range of electrochemical instrumentation, including one PARC 270, four Voltalab 10-40 potentiostats, BAS 100 and CHI 604 electrochemical analyzers four sets for rotating disk-ring measurements with two Pine bipotentiostats, two Molecular Imaging STMs for in situ surface structural studies, a fast-scan NEXUS 670 Nicolet and Mattson Research Series FTIR spectroscopes for in situ infrared studies, UHV chamber for crystal preparation, RF induction heater adapted for annealing reactive metals, standard equipment for wet-chemistry and high-temperature synthetic work.

 

Instrumentation at the Center for Functional Nanomaterials (CFN)

Existing equipment includes (but not exhaustively):  Elmitec LEEM III, VT UHV STM (Custom Built), Omicron VT UHV STM, Molecular Imaging Fluid and Environmentally Controlled STM, AFM, Electrochemistry, JEOL JEM 3000F and JEM 4000Ex TEM, JEOL JEM 2200FS and JEM 2010FEF TEM, JEOL JSM6400 SEM, PHI 699 Scanning Auger, SILAR robot (Gilson), PLD (Neocera), E-beam evaporator, Lab X-ray diffraction (Rigaku Miniflex), UV spectrometer (Flororat-02-Panorama, Spectrodyn Technologies), Differential Scanning Calorimetry/Thermogravimetric Analysis (DTA/TGA, Netsch), Optical microscopes (Nikon), ICP/AES (Hewlett Packard), AFM (Nanoscope II) Major equipment has been ordered for: Facility for Surfaces, Interfaces, Catalysis—Proximal Probes; Transmission Electron Microscopy Facility; Nanopatterning Facility; Facility for Electronic Materials and Inorganic Nanomaterials; and Facility for Soft and Bio-nanomaterials.

 

Experiments at National Synchrotron Light Source (NSLS)

The following beamlines are currently used by the group PIs and collaborators.

Beamline U7A: Capabilities for doing photoemission and near-edge X-ray absorption spectroscopy. Can be used with single-crystal or powder surfaces. The ultra-high vacuum chamber attached to the beamline is equipped with typical instrumentation (AES, XPS, LEED, TPD) for doing surface science studies.

Beamline U4IR: Newly purchased vacuum FTIR is being interfaced with the existing UHV chamber for grazing incidence single reflection absorption IR spectroscopy on well-defined surfaces.

Beamline U2B: In situ far infrared experiments for electrode materials.

Beam line X7A: The high-resolution mode where a water-cooled Si(111) monochromator and a Ge(220) analyzer or multi-analyser setup provide a resolution of Dd/d = 2 x 10-4. This configuration is used for ab initio solution of complex structures, investigations of phase transitions (subtle lattice distortions, weak superlattice reflections) and studies involving diffraction in the vicinity of absorption edges. The high-throughput mode using a linear position-sensitive detector gating on the Kr-escape peak built by Graham Smith (Instrumentation, BNL) without an analyzer crystal. This lower resolution mode (Dd/d~10-3) allows for much higher counting rates from smaller samples and much faster data collection as a function of temperature. Typically temperature ranges fall between 20 and 700K. With a 40 degree PSD this machine could set new standards in how fast and how many datasets can be measured as a function of temperature or charge state (electrochemistry). Instrument could also have image plate/CCD capability for single crystal work. The PDF mode, where a semiconductor detector is employed. Compromising resolution even further but providing good counting statistics combined with reasonable energy discrimination provides data for pair-distribution function (PDF) studies.

Beamline X7B: Capabilities to acquire fast X-ray diffraction spectra using an image plate or CCD detector. Time-resolved XRD experiments can be carried out in a remarkably wide variety of temperature and pressure conditions (-190 C < T < 900 C, P < 45 atm). Equipment to perform in situ kinetic studies is attached to the X-ray diffraction cell that contains the catalytic material and the products of reaction can be detected with a mass spectrometer. In situ synthesis can be performed and monitored using special capillary cells.

Beamlines X18/X19A: Capabilities for recording XANES and EXAFS spectra of catalytic materials. A set of reactors is available that can be combined with instrumentation to make EXAFS measurements in transmission or fluorescence yield mode.

Beamlines X18/X19A: The electrochemistry-oriented X22A beam line for SXS in situ studies.

Beamlines X11A, X8A and X23: For in situ XANES and EXAFS measurements for electrode materials.

 

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Last Modified: November 4, 2013