X-ray Diffraction (XRD) and Reflectivity (XRR)

Instrumentation for X-ray Diffraction:

  • Siemens/Bruker D-5000 system
  • PANalytical / Philips X’pert MRD system # 1
  • PANalytical / Philips X’pert MRD system # 2
  • Small Angle X-ray Scattering system with Pilatus 300 detector
  • Laue system with Multiwire 2D areal detector (Dexco)
  • Shimadzu EDX-7000 Engergy-Dispersive X-ray Fluorescence system
  • Data analysis software packages


Staff Contacts

Mauro Sardela
(217) 244-0547

Natialie Becerra+Stasiewicz
(217) 265-8419

Instrumentation

The following instruments for data acquisition and software packages for data analysis are available in the X-ray analysis lab. Please contact lab staff for further details, for training, lab tour or a demo.

Location

148 Materials Research Laboratory
(217) 265-6799

Siemens/Bruker D-5000 XRD system

Radiation /wavelength: Cu K-alpha, 0.15418 nm

Features: theta/theta vertical goniometer system with optional spinner (phi) rotation (Bragg Brentano configuration).

Main optics: soller slits, divergence slit, scatter slit, receiving slit, detector slit, curved graphite monochromator, scintillation detector

Applications

  • Powder and polycrystalline bulk materials; limited applicability to soft samples.
  • Phase identification, composition quantification, crystallographic structure determination.
  • Crystallite / grain size and strain analysis.
  • Limited texture (preferred orientation) analysis.

PANalytical / Philips X’pert MRD system # 1

Radiation / wavelength: Cu K-alpha 1, 0.154056 nm (high-resolution) or Cu K-alpha, 0.15418 nm (Bragg-Brentano)

Features: theta/2theta vertical four-circle system with phi, psi rotations and x,y,z sample translation, high-speed PIXcel line detector (pixel size 55 microns).

Main Optics

  • Option 1: Line focus beam, high-resolution parallel beam configuration with hybrid mirror with x-ray mirror and 2-bounce monochromator (beam divergence = 30 arc-sec), high-speed line detector PIXcel© with scatter slit.
  • Option 2: Line focus beam high-speed Bragg-Brentano configuration with programmable divergence slit and high-speed line detector PIXcel© with scatter slit and Ni filter.
  • Other options: high-resolution configurations with x-ray mirror and 4-bounce Ge monochromator (beam divergence = 12 arc-sec) and/or open detector and/or triple-axis analyzer crystal (12 arc-sec acceptance).
  • Optional attachment: dome-shaped Anton Paar DHS900 hot stage for in-situ high temperature (up to 900°C) analysis under air or vacuum

Applications

  • High resolution rocking curve analysis.
  • High resolution analysis of lattice constant, strain, residual stress, crystallographic orientation, diffuse scattering, dislocation density, reciprocal lattice mapping. Typical materials: epitaxial thin films and single crystal materials.
  • X-ray reflectivity (thin film thickness, density, porosity, interface and surface roughness and correlation).
  • Ultra-fast Bragg-Brentano applications for samples with vertical mount: phase determination, crystallographic structure determination, etc.
  • In-situ high-temperature (up to 900oC) XRD and XRF analysis including temperature-dependent reciprocal space mapping, pole figures, etc.

PANalytical / Philips X’pert MRD system #2

Radiation / wavelength: Cu K-alpha, 0.15418 nm

Features: theta/2theta vertical four-circle system with phi, psi rotations and x,y,z sample translation, proportional detector and high-speed PIXcel line detector (pixel size 55 microns).

Main Optics

  • Option 1: General thin film and bulk phase, stress and texture analysis. Point focus beam, crossed-slit collimator or x-ray lens, parallel plates collimator, flat graphite monochromator and proportional detector.
  • Option 2: Fast texture and stress configuration using 1D detector. Point focus beam, x-ray lens, PIXcel line detector in high-speed mode
  • Option 3: Micro XRD setup for surface spatial resolution between 100 and 400 microns. Point focus beam, 100-microns monocapillary primary optics, PIXcel line detector in high-speed mode
  • Optional attachment: dome-shaped Anton Paar DHS900 hot stage for in-situ high temperature (up to 900°C) analysis under air or vacuum

Applications

  • General thin film or coatings analysis
  • Medium resolution / high-intensity analysis of lattice constant, strain, crystallographic orientation, diffuse scattering, dislocation density, reciprocal lattice mapping.
  • Glancing incidence x-ray diffraction for analysis of ultra-thin films or analysis of depth-dependent phase, crystallinity and texture variations in materials.
  • Texture / preferred orientation and stress analysis.
  • Micro XRD for applications requiring spatial resolution between 100 and 400 microns.
  • In-situ high-temperature (up to 900oC) XRD analysis for phase transition, thermal expansion coefficient determination, stress and texture variations in materials.
  • Typical materials: textured thin films and bulk materials.

Small Angle X-ray Scattering System with Pilatus 300 detector

Radiation / wavelength: Cu K-alpha, 0.15418 nm

Features: High-speed SAXS, WAXS, GI-SAXS, GI-WAXS data collection using a three-module Pilatus 300 detector with optional environmental controls.

Main optics: Genix3D ULD microfocus source including focusing mirror (beam size at sample: 0.8 x 0.8 mm2), evacuated primary and secondary beam paths, sample stage with theta (angle of incidence) rotation and horizontal/vertical sample translation; high-speed Pilatus 300 detector (172 microns pixel size, 500 eV resolution) for 2D areal data acquisition.

Applications

  • Small-angle x-ray scattering (SAXS), wide-angle x-ray scattering (WAXS), grazing-incidence small-angle x-ray scattering (GI-SAXS) and grazing-incidence wide-angle x-ray scattering (GI-WAXS) applications.
  • SAXS range: q~ 0.1 – 2.8 nm-1 (feature sizes ~ 70 – 2 nm)
  • WAXS measurement range: q~ 2 – 24 nm-1 (feature sizes ~ 3 – 0.25 nm)
  • Samples can be in liquid, powder, membranes or thin film/substrate form.
  • Optional environmental controls for humidity and temperature from -20 to 120 oC.
  • Characteristic distances of ordered materials: shape, average size and distribution of particles and macromolecules, surface-to-volume ratio, pore sizes, etc.

Laue system with Multiwire 2D detector

Radiation: non-monochromatic W source.

Features: Back-scattering Laue with data acquisition using a fast 2D detector; sample stage with multi-axis rotations and full translation capabilities controlled by multi-function joystick allowing for real time sample movement/rotation with simultaneous data visualization. Laue pattern processing and indexing using NorthStar Real-Time Orientation software.

Main optics: Four choices of primary collimators for x-ray beam diameters 0.5, 1, 2 and 3 mm; three-axis rotation goniometer with X,Y,Z translation orientation base; Multiwire MWL120 2D detector with CO2+Ar gas consisting of arrays of 20-microns W wires coated with Au.

Applications

  • Crystallographic orientation of single crystals within 0.25 degree and determination of domains in bulk materials.
  • Sample alignment prior to cleaving/cutting is specific crystallographic direction.
  • Automated indexing of Laue patterns in single crystal materials.

Shimadzu EDX-7000 Energy-dispersive X-ray Fluorescence Spectrometer

Radiation: non-monochromatic or filtered Rh x-ray source

Features: Fast measurements in a small, table-top foot print, automated analysis of up to 12 samples in a single run.

Main optics: x-ray source using Rh target up to 50 kV; four choices of collimator sizes for irradiation areas of diameter 1, 3, 5 and 10 mm; five options of primary filters; 12-sample turret for multiple sample analysis; CMOS camera for sample visualization and alignment; solid state detector with energy resolution < 140 eV Mn K-alpha; fast evacuation and purge time (~ 2 min) for optional use under He environment. PCEDX-Navi and PCEDX-Pro for data processing and analysis, including calibration curve method and matrix correction.

Applications

  • Elemental quantification analysis for elements from Na to U.
  • Samples can be in powder, thin film, bulk or liquid form.
  • Measurements can be done in air or under He environment.
  • Thin film thickness determination (limited cases).
  • Detection limits: ppm (heavy elements) to 0.1 at% (light elements).

Data analysis software

  • PDF+4 powder diffraction files database from the International Center for Diffraction Data (fully updated every year)
  • ICSD (Inorganic Chemistry Structure Database) from FIZ/NIST (fully updated every year)
  • MDI Jade + with pattern analysis, profile fitting, search/match, crystallite / grain size and strain analysis, RIR analysis, whole pattern fitting and Rietveld refinement
  • PANalytical X’pert Reflectivity, Epitaxy, Stress, Texture and High Score Plus
  • Bruker EVA