Methods

Methods

Rigaku: Reflectometry, Diffraction and Reciprocal Space Mapping

 

 

 

 

 

 

 

 

  • Powder diffractometry with Q-Q-geometry (2Θ ca. -3° – 160°), gracing-incidence diffraction (GID), reflectometry
  • X-ray source: rotating anode Cu (Kα), line or point focus system
  • Running parameter 45kV, 160mA
  • Filtering of Kβ, soller collimation, flexible absorber
  • Primary optics: Goebel mirror, automated slit system, Johannsson monochromator and microfocus optics
  • Sample environment: several different stages, Eulerian cradle
  • Secondary optics: monochromator, automated slit system
  • Detection system: Hypix 3000 solid state 2D-detector
  • optional: capillary attachment, 0D- and 1D-detection system, heating equipment from Anton Paar
  • Software: SmartLab Guidance, PDXL-Basic, PDXL-Qualitative, Global Fit XRR&RC

Bruker D8 Discover for Reflectometry:

 

 

  • Reflectometer with Q-Q-Geometry (2Θ ca. -10° – 140°) or Gracing-Incidence Diffraction (GID)
  • X-ray source: Anode Cu (Kα) or Mo (Kα)
  • Running Parameter 45kV, 45mA
  • Filtering of Kβ, soller collimation, flexible absorber
  • Primary optics: goebel mirror, slit system or asymetric channel cut monochromator (for both energies)
  • Sample environment: several different stages, eulerian cradle
  • Secondary optics: same as primary optics
  • Detection system: 1-D semiconducting stripe detector (Lynxeye) or scintillation counter
  • Optional: shear cell and heating equipment

 VAXSTER (Versatile Advanced X-ray Scattering Instrument Erlangen) for Small and Wide Angle Scattering

 

 

 

 

 

  • Small- (SAX) and wide angle scattering (WAX), gracing incidence small angle scattering (GISAX)
  • X-ray source: Excillum MetalJet, 10-70kV, focal spot size 5 – 20 mm^2@max. 250W, Ga (Kα, 1.34 A)
  • Collimation: source multilayer optics, collimation through 3 sets of 4-bladed slits
  • Sample stage: mounting of various large space sample stages inside detector tube possible (under vacuum ~10-5 bar), as well as externally (measurement in air/controlled vapor environment), yz-theta goniometer for transmission as well as grazing incidence applications
  • Sample holders: Many different sample holders for mounting on yz-sample stage including: GISAXS sample holder, temperature-controlled Cu-holder with 5 sample-positions, Stopped-flow cell, capillary holder …
  • Detection system: Pilatus 300K detector (500 Hz): three modules à 83.8×33.5 mm², 487×619 pixel à 172×172 µm², readout time of 3 ms, energy range of 4.5-36 keV at a resolution of 500 eV
  • Q-range: Total Q-range: Q = 0.003-4Å-1
    low count rates for small Q-limit, only achievable under ambient conditions;
    high Q-limit only achievable in vacuum
    individual configurations in between; e.g.: WAXS (0.05-2.5 Å-1), MAXS (0.012-0.67 Å-1), SAXS (0.006-0.26 Å-1), Extreme-SAXS (0.003-0.21 Å-1)
  • Software: SPEC

SAXSpace (Anton Paar) for Small and Wide Angle Scattering

 

 

 

 

 

 

 

  • Small angle (SAXS -> approx. 0.04° to 10°) and wide angle (WAXS, up to 74°) X-Ray scattering
  • X-Ray source: 50 W Cu Kα microfocus tube
  • Scatterless Kratky-base collimation system for line and point collimation
  • Primary optics: focusing multilayer mirror to monochromatize and enhance X-Ray intensity
  • Sample holders for liquids, pastes and solids
  • Detection system: 2-D diode-array (CMOS) detector (Pilatus 100k)
  • Temperature range of -30°C to +150°C (peltier heating/cooling)
  • Software: SAXSdrive, SAXStreat and SAXSquant

High Energy X-Ray Laboratory HEXBay

 

 

 

 

 

 

 

  • Focussing Laue method (reflection topography, focussing distance up to 8m, resolution 0.005°), powder diffraction, real structure analysis
  • Motorized collimation system with tungsten blades
  • Sources: 2 tungsten tubes with
    • up to 450 KV, 2.5 mm (0.9 kW) / 5.5 mm (4.5 kW) focal spot (EN 12543)
    • up to 225 KV, 0.4 mm (0.8 kW) / 1 mm (1.8 kW) focal spot (EN 12543)
  • Sample stage: heavy load sample stage (up to 150 kg), Eulerian cradle, omega stage with resolution of 0.2“
  • Sample environment: several furnaces (T up to 1800°C, vacuum, oxygen or inert gas environment), pressure system
  • Detection systems:
    • Imageplate MAR 345, 345 cm diameter, max. resolution 100µm, readout time at max. resolution ~2 min
    • 2 D scintillation system, active area 30 cm x 20 cm, 2 x 14 Bit peltier cooled CCD with 1280 x 1024 pixel, resolution ~ 150 µm, readout time 125 ms
  • Software: SPEC

 Philips/PANalytical X’Pert Pro-MPD Powder Diffractometer

 

 

 

 

 

 

 

 

  • Powder diffraction with Q-Q-Bragg-Brentano geometry (2Θ ca. 5° – 100°), gracing-incidence powder diffraction (GID, incidence angle>≈0.2°), reflectometry
  • X-ray source: Anode Cu (Kα)
  • Running Parameter 40kV, 35mA
  • Filtering of Kβ, soller collimation
  • Primary optics: Goebel mirror, slit system
  • Sample environment: various sample holder systems as reflectometry stage, Eulerian Cradle …
  • Detection system: semiconducting stripe detector (X’Celerator) or Gas ionisation counter (Miniprop)
  • Variable step size
  • optional: capillary optics

Huber Guinier Diffractometer

 

 

 

 

 

 

 

 

 

 

 

  • Powder diffraction in transmission-geometry (2Θ fixed 10° – 100°)
  • X-ray source: Anode Cu (Kα)
  • Running Parameter 40kV, 35mA Primary optics: monochromator: Kα1, high angular resolution
  • Detection system: Image plate online read-out, illumination time: ca. 10min – several hours
  • Software: Huber guinier software

Rotating Anode Setup for Powder Diffraction:

 

 

  • Powder measurement in transmission Debye-Scherrer geometry, texture analysis
  • X-ray source: rotating anode Cu (Kα)
  • Voltage and current up to 44 kV and 75 mA, respectively
  • Primary optics: crossed Goebel mirror setup
  • Sample environment: 6 axis goniometer for adjustment of sample position, In-Situ chamber for variation of temperature ramps up to 550° C, possibility for different atmospheres (vaccum, inert gases)
  • Detection system: 2D ccd detector allows measurement of full diffraction rings (2-Q range from 0 -50°)
  • Software: SPEC

Huber Laue System

 

 

 

 

 

  • Laue Camera for transmission- and backscattering diffraction
  • Anode Molybdenum
  • Image plate detection
  • Primary optics: different collimation systems

BI-200SM Goniometer (Brookhaven Instruments Corporation)

 

 

 

 

 

 

 

 

  • motor driven angle selection (0.01° steps)
  • narrow-band optical filters for laser wavelegths of 633, 514.5, 488 nm
  • 100, 200, 400 μ pinholes for selecting coherence areas (QELS measurements)
  • 1, 2, 3mm apertures for adjusting intensity (classical measurements)
  • Selected photomultiplier tube (PMT) as Detector
  • circulating index matching liquid with dust filter
  • Temperature control approximately+5°C to 80°C
  • needed sample Volume: 1.5mL (strongly diluted)
  • Diode Laser 637 nm (BIC), 30mW
  • Lexel95-2 (Lexel), Argon Laser, 476.5 nm – 514.5 nm, 4 W, 1.33 mm beam diameter, 0.6 mrad beam divergence

UV-Vis Spectrometer TIDAS S 500K

(TIDAS S 500K UV/NIR 1910 DH, J&M Analytik AG)

 

 

 

 

 

 

 

 

 

 

 

  • wavelength range 187.79 – 1016.53 nm
  • spectral resolution < 2.5 nm
  • wavelength accuracy < 1.0 nm
  • wavelength reproducibility 0.1 nm
  • baseline drift at 250 nm: 5 μAU/h
  • signal-to-noise ratio < 20 μAU
  • integration-time range 0.7 – 10 000.0 ms
  • integrated D2- & halogen light source
  • detector MCS – Aspen 780 kHz
  • photodiode array: 1024 pixels
  • Bio-Kine 32 V4.66 for data acquisition and analysis

 Micro DSC III Analyzer (Setaram)

 

 

 

 

 

 

 

 

  • High sensitivity DSC and calorimetry
  • Temperature range: -20 to 120 °C
  • Scanning rate: 0.001 to 1.2 °C/min
  • Vessel volume: 850 µl
  • Resolution: 0.3 µW
  • Cooling rate from 120°C to room
  • temperature: 1.5 h
  • Scanning or isothermal mode
  • Thermal Analysis Software: Calisto

Perkin Elmer DSC 8500 (Perkin Elmer)

 

 

 

 

 

 

 

 

  • Hyper-enabled Double-Furnace Differential Scanning Calorimeter
  • Cooling system: Intracooler 3 (Perkin Elmer), three stage, closed-loop circulationg heat exchanger
  • Temperature range: -100 to 750 °C (by nitrogen usage)
  • In-situ ballistic cooling to 2100 °C/min
  • Scanning rate: 0.1 to 750 °C/min
  • Sample pans: aluminium (50 µl)
  • Analysis Software: Pyris

Stopped-Flow SFM-2000

(SFM-2000, Bio-Logic)

 

 

 

 

 

 

 

 

 

 

 

  • two 10 ml syringes
  • minimal injection volume per syringe: 28 μl
  • flow rate from 0.062 – 10 ml/s per syringe
  • minimum total flow rate for efficient mixing: 1 ml/s
  • ratio range from 1:1 to 1:40
  • duration of flow: 1 ms to 60 000 ms per phase
  • minimal dead time 0.7 ms
  • Berger ball mixer
  • Bio-Kine 32 V4.66 for syringe control

Booking System