X-ray Instrumentation for Materials Characterization

XCT-Wadley Group Image.JPG

(M.R. O'Masta et al 2015)

NMCF maintains several types of X-ray characterization for bulk and surface characterization of materials. X-ray diffraction (XRD) provides information on bulk composition and phase for any  polycrystalline material including geologic, metal alloy, inorganic, organometallic and organic substances. Quantitative elemental and oxide composition of bulk materials - solids, powders, and liquids - can be measured with high sensitivity using X-ray fluorescence (XRF). X-ray photoelectron spectroscopy (XPS) provides quantitative chemical and elemental composition of material surfaces (~ 5 nm) with depth as a function of position. 3-D images of internal structures can be acquired with micro X-ray computed tomography (XCT).

 

  • Versaprobe X-ray Photoelectron Spectrometer (XPS)

    PHI Versaprobe III Scanning XPS with adjacent Processing / Reaction Chambers

    CALENDAR | XPS Rates

     

    Location: MSB 148

    The PHI Versaprobe III XPS instrument provides quantitative elemental and chemical analysis of material surfaces for elements with Z ≥ 3. Small-spot (9-200 micron) and large-area analyses (mm-scale) available, as well as elemental and chemical mapping. Angle-resolved XPS. In situ sample heating and cooling (150 - 850 K). Argon sputtering for removal of surface contamination or depth profiling. Adjacent UHV processing chamber and high-pressure reaction cell available for in situ deposition or processing. Samples up to 60 mm-dia. x 14 mm height.

     

    XPS Technique Summary:

     

    • XPS for Quantitative Elemental Composition of Surfaces (outermost <10 nm)
    • XPS for Quantitative Chemical Analysis of Surfaces (outermost <10 nm)
    • Elemental / Chemical Composition across interfaces with Line Scans
    • Elemental / Chemical Composition across heterogenious regions with Area Maps
    • Surface Specific Chemistry/Composition by Angle-Resolved XPS (~ 1nm)
    • Compositional Profiles with Depth by Ion Sputtering or AR-XPS up to ~ 10µm
    • Surface Kinetics from Compositional Change as a function of temperature (to 600 C)
    • Technique Sensitivity:< 0.1% (atomic percentage)
    • Spatial Resolution:< 10 microns
    • Standard Compositional Error: ~15%
    • Detection of all Elements with Z ≥ 3

     

    Versaprobe III Features:

     

    • Energy resolution: < 0.60 eV @ > 14kcps (10 um); < 0.90 eV @ 2.0 Mcps (100um)
    • Monochromatic Al k-alpha X-rays (1486.6 eV)
    • In situ Hot/Cold stage ( -140 - 600 C)
    • SXI imaging for precise analysis location
    • Floating Column Ar+ Ion gun (0.005 - 5.00 keV) for depth profiling and charge neutralization
    • Narrow aperture for angle-resolved XPS (AR-XPS)
    • Auto dual-charge neutralization
    • Geometry: 45° between X-rays and spectrometer; 0-90° Sample Tilt toward/away spectrometer; Zalar rotation
      • Spot sizes: 9 um – 200 um plus HP/LA (high power-large area - 100 microns x 1400 microns)
      • Line scans: 9 um - 200 um  x 1400 um (max)
      • Compositional/Chemical Maps: typically 9 um beam scanned over 1400 um x 1400um or interpolated StageMaps over ~ 5 mm x 5mm

     

    High-Pressure Reaction Cell for reaction studies of oxides, hydrocarbons or catalytic materials requiring a reducing environment:

     

    • Reaction cell transfer (in situ) to XPS analysis chamber through Prep Chamber; not directly coupled to XPS analysis chamber to minimize cross-contamination
    • Sample heating at high pressures, temperatures to 500 ºC (dynamic mode, 2 bar max.) and 800 ºC (static mode, 1 bar max.)
    • MKS Digital Mass Flow Control (100 sccm) for Oxygen or Hydrogen or other gasses
    • Sample size < 10 mm x <10 mm; thickness < 3mm
    • Complete vacuum pumping and gauging
    • Molybdenum Mount with thermocouple
    • Chamber schematics are available

     

  • Panalytical X-ray Fluorescence Spectrometer (XRF)

    Benchtop Panalytical Epsilon 3x Energy-Dispersive XRF spectrometer

    CALENDAR | XRF Rates

    Location: MSB 108

    XRF spectrometer with a silver (Ag) anode x‐ray tube and 50 micron Be window performs non‐destructive identification and quantification (< 1 ppm) of elements from sodium (Na) to americium (Am) in solids, liquids, loose‐ and pressed‐powders. Silicon drift detector for secondary X-ray detection. Omnian standardless analysis software for peak ID and quantification.

     

    XRF Technique Summary:

     
    • Non-destructive Analysis of Metals, Glasses, Ceramics, Plastics, Geologic Materials, Organics, Art, Ground Water, Catalysts, Pharmacuticals, etc.
    • Elemental Composition of Solids, Liquids, and Loose or Pressed Powders for 11 ≤ Z ≤ 95
    • Identification of Elemental Impurities with Sensitivity < 1 ppm
    • Quantitative Elemental Analysis of Materials using Material Standards or Omnian Standardless Analysis Software Package
    • Spectral Energy Resolution ≤ 145 eV
    • Elemental Sensitivity:< 1 ppm (by weight)
    • Batch analysis with ten-position sample tray
    • Sample size from ~ 5 mg to ~ 1000 g up to 18 ml or 10 x 20 x 10 cm3 ( H x W x D)
     

    XRF Features:

     
    • Source: X‐ray tube with Ag anode and 50 micrometer Be window
    • Software selectable beam filters (Cu 500 μm, Al 50 μm, Al 200 μm, Ti 7 μm, Ag 100 μm, Cu 300 μm)
    • Silicon drift detector (SDD) for X-ray detection with a resolution ≤ 145 eV
    • 50 keV X-ray detection max; 9 W max.
    • 10‐position sample tray with 10 standard sample holders and a set of inserts
    • Sample spinner
    • Helium (He) purge system
    • 2-D Optical Geometry with fixed angles
    • Sample cup: 18 ml (OD: 35 mm; ID: 28 mm; H: 30 mm)
    • High lid for analysis of large samples with maximum dimensions of 10 x 20 x 10 cm3 (H x W x D)
    • Omnian Analysis Software for Element or Oxide Quantification without Calibration Standards
    • Fluorescent Volume Geometry (FVG) and unmeasured 'Dark Matrix' compound corrections with Omnian
  • Empyrean Multipurpose X-ray Diffractometer (XRD)

    Panalytical Empyrean XRD for Bragg-Bretano, GIXRD, & XRR; environmental cell with hot stage

    CALENDAR | Empyrean XRD Rates

    Empyrean.jpg

    Location: MSB 108

    The Empyrean diffractometer from Malvern-Panalytical performs a variety of X-ray diffraction measurements on any type of polycrystalline material including inorganic, organometallic and organic substances. It can be easily configured by each user with the optimal combination of optics, detector and sample stage for their experiment with reproducible alignment every time.

     

    XRD Technique Summary:

     
    • Non-destructive analysis of any polycrystalline material including powders, pressed pellets, fibers, thin films and bulk materials
    • Determine the 3-D structure of any crystal phase at the atomic or molecular level
    • Determine texture, stress and other properties that influence the crystal structure
    • Compare your material to hundreds of thousands of known materials in published databases
    • Easily switch configurations between Bragg-Bretano divergent beam, pseudo-parallel beam, transmission, and triple-axis techniques
    • Run scans in manual mode or create programs for your measurements

     

    XRD Applications:

     
    • X-ray Powder Diffractometry (XPRD)
    • Transmission Geometry XPRD
    • Grazing Incidence X-ray Diffractometry (GIXRD)
    • X-ray Reflectometry (XRR)
    • Texture (Pole Figure)
    • Residual Stress (side inclination or iso-inclination)
    • Rocking Curves
    • Reciprocal Space Mapping
    • 2-D XRPD
    • Microdiffraction
    • In-plane GIXRD

     

    XRD Features:

     
    • Source: X‐ray tube with line-focus Cu anode (1.54 Å wavelength) with customizable beam size from less than 0.5 mm to several cm in length and width
    • Detectors: Prop detector for point (0-D) data collection and GaliPIX3D detector for line (1-D) and area (2-D) data collections
    • Multiple modes for GaliPIX3D detector
      • Scanning line mode (1-D) - maximum active length 7.1763° 2-theta (501 pixels)
      • Static line mode (1-D) - maximum active length 7.1669° 2-theta (501 pixels)
      • Frame-based mode (1-D) - maximum active length 6.8898° 2-theta (481 pixels) equatorial by 5.7632° 2-theta (465 pixels) axial
      • Scanning area mode (2-D) - maxiumum active length  7.1763° 2-theta (501 pixels) by 5.5158° 2-theta (445 pixels)
      • Static area mode (2-D) - maximum active length 7.1669° 2-theta (501 pixels) by 5.5158° 2-theta (445 pixels)
      • Flat field mode (2-D) - maximum active length 7.1763° 2-theta (501 pixels) by 5.7632° 2-theta (465 pixels)
    • Four sample stages available
      • Reflection-Transmission Spinner
      • 3-Axes cradle with auto chi, phi and Z, three interchangeable platforms (static, leveling, and manual XY translation) and five different leg lengths
      • Flat sample bracket
      • Anton Paar HTK1200N oven
    • Incident beam PreFIX modules: Bragg-Bretano HD (BBHD), 2xGe(220) Hybrid Monochromator, and Fixed Divergence Slit (FDS)
    • Diffracted beam PreFIX modules: Fixed Anti-Scatter Slit (FASS), 0.18° Parallel Plate Collimator (PPC), and 2xGe(220) Triple-Axis Analyzer
    • Incident beam accessories: Programmable Attenuator, Soller slits (0.02 and 0.04 rad), set of divergence and incident beam anti-scatter (IBASS) slits, set of masks, and set of microbeam masks and collimators
    • Diffracted beam accessories: Monochromator, beta filter (Ni), and Soller slits (0.02 and 0.04 rad)
    • Other accessories: Beam knife, and fluorescent screens for visualizing X-ray beam
    • Oven stage allows in-situ measurements from room temperature up to 1200 C, under ambient atmosphere, vacuum or inert/reactive gases with or without sample oscillation
    • Steel sample holders for R/T spinner are available in a variety of sizes
      • For powder: 27 mm diameter x 2.4 mm deep, and 16 mm diameter x 2.4 mm deep for front- and/or back-loading
      • For materials of non-standard size and shape: maximum 45 mm diameter x maximum 6.5 mm deep
      • For circular solid samples: 30-32.3 mm diameter x maximum 6 mm deep
      • For transmission mode measurements: Holder ring (40 mm diameter x 6 mm deep) with disposable Kapton foil and polyoxymethylene inserts
    • Alumina sample holders for HTK1200 N oven are 16 mm in diameter and have depths of either 0.8 mm, 0.4 mm or flat
    • Zero-background sample holders for small amounts of material
    • Manual powder press for back-loading samples
    • Software includes Data Collector, Data Viewer, HighScore Plus, Epitaxy, Stress, and an Excel-based "beam size guidance calculator" for determining X-ray beam size
    • Access to PDF4+ database and CSD database on separate data processing computer
    • Various user manuals in hard-copy and electronic formats
  • X'Pert X-ray Diffractometer (XRD)

    Panalytical X'Pert XRD for Bragg-Bretano, GIXRD, XRR, etc.

    CALENDAR | Empyrean XRD Rates

    Empyrean.jpg

    Location: MSB 108

    The Empyrean diffractometer from Malvern-Panalytical performs a variety of X-ray diffraction measurements on any type of polycrystalline material including inorganic, organometallic and organic substances. It can be easily configured by each user with the optimal combination of optics, detector and sample stage for their experiment with reproducible alignment every time.

     

    XRD Technique Summary:

     
    • Non-destructive analysis of any polycrystalline material including powders, pressed pellets, fibers, thin films and bulk materials
    • Determine the 3-D structure of any crystal phase at the atomic or molecular level
    • Determine texture, stress and other properties that influence the crystal structure
    • Compare your material to hundreds of thousands of known materials in published databases
    • Easily switch configurations between Bragg-Bretano divergent beam, pseudo-parallel beam, transmission, and triple-axis techniques
    • Run scans in manual mode or create programs for your measurements

     

    XRD Applications:

     
    • X-ray Powder Diffractometry (XPRD)
    • Transmission Geometry XPRD
    • Grazing Incidence X-ray Diffractometry (GIXRD)
    • X-ray Reflectometry (XRR)
    • Texture (Pole Figure)
    • Residual Stress (side inclination or iso-inclination)
    • Rocking Curves
    • Reciprocal Space Mapping
    • 2-D XRPD
    • Microdiffraction
    • In-plane GIXRD

     

    XRD Features:

     
    • Source: X‐ray tube with line-focus Cu anode (1.54 Å wavelength) with customizable beam size from less than 0.5 mm to several cm in length and width
    • Detectors: Prop detector for point (0-D) data collection and GaliPIX3D detector for line (1-D) and area (2-D) data collections
    • Multiple modes for GaliPIX3D detector
      • Scanning line mode (1-D) - maximum active length 7.1763° 2-theta (501 pixels)
      • Static line mode (1-D) - maximum active length 7.1669° 2-theta (501 pixels)
      • Frame-based mode (1-D) - maximum active length 6.8898° 2-theta (481 pixels) equatorial by 5.7632° 2-theta (465 pixels) axial
      • Scanning area mode (2-D) - maxiumum active length  7.1763° 2-theta (501 pixels) by 5.5158° 2-theta (445 pixels)
      • Static area mode (2-D) - maximum active length 7.1669° 2-theta (501 pixels) by 5.5158° 2-theta (445 pixels)
      • Flat field mode (2-D) - maximum active length 7.1763° 2-theta (501 pixels) by 5.7632° 2-theta (465 pixels)
    • Four sample stages available
      • Reflection-Transmission Spinner
      • 3-Axes cradle with auto chi, phi and Z, three interchangeable platforms (static, leveling, and manual XY translation) and five different leg lengths
      • Flat sample bracket
      • Anton Paar HTK1200N oven
    • Incident beam PreFIX modules: Bragg-Bretano HD (BBHD), 2xGe(220) Hybrid Monochromator, and Fixed Divergence Slit (FDS)
    • Diffracted beam PreFIX modules: Fixed Anti-Scatter Slit (FASS), 0.18° Parallel Plate Collimator (PPC), and 2xGe(220) Triple-Axis Analyzer
    • Incident beam accessories: Programmable Attenuator, Soller slits (0.02 and 0.04 rad), set of divergence and incident beam anti-scatter (IBASS) slits, set of masks, and set of microbeam masks and collimators
    • Diffracted beam accessories: Monochromator, beta filter (Ni), and Soller slits (0.02 and 0.04 rad)
    • Other accessories: Beam knife, and fluorescent screens for visualizing X-ray beam
    • Oven stage allows in-situ measurements from room temperature up to 1200 C, under ambient atmosphere, vacuum or inert/reactive gases with or without sample oscillation
    • Steel sample holders for R/T spinner are available in a variety of sizes
      • For powder: 27 mm diameter x 2.4 mm deep, and 16 mm diameter x 2.4 mm deep for front- and/or back-loading
      • For materials of non-standard size and shape: maximum 45 mm diameter x maximum 6.5 mm deep
      • For circular solid samples: 30-32.3 mm diameter x maximum 6 mm deep
      • For transmission mode measurements: Holder ring (40 mm diameter x 6 mm deep) with disposable Kapton foil and polyoxymethylene inserts
    • Alumina sample holders for HTK1200 N oven are 16 mm in diameter and have depths of either 0.8 mm, 0.4 mm or flat
    • Zero-background sample holders for small amounts of material
    • Manual powder press for back-loading samples
    • Software includes Data Collector, Data Viewer, HighScore Plus, Epitaxy, Stress, and an Excel-based "beam size guidance calculator" for determining X-ray beam size
    • Access to PDF4+ database and CSD database on separate data processing computer
    • Various user manuals in hard-copy and electronic formats
  • Rigaku X-Ray Diffractometer (XRD)

    Rigaku SmartLab XRD for Bragg-Bretano, GIXRD, XRR, etc.

    Calendar | Rigaku XRD Rates

    SmartLab.jpg

    Location: MSB 108

    The SmartLab X-ray diffractometer from Rigaku is configured for the analysis of thin films by X-ray diffraction

     

    XRD Technique Summary:

     
    • Non-destructive analysis of any polycrystalline material, particularly thin films
    • Determine the 3-D structure of any crystal phase at the atomic or molecular level
    • Determine texture, stress, epitaxy relationships and other properties that influence the crystal structure
    • Compare your material to hundreds of thousands of known materials in published databases

     

    XRD Applications:

     
    • X-ray Powder Diffractometry (XPRD)
    • Grazing Incidence X-ray Diffractometry (GIXRD)
    • X-ray Reflectometry (XRR)
    • Texture (Pole Figure)
    • Residual Stress
    • Rocking Curves
    • Reciprocal Space Mapping

     

    XRD Features:

     
    • Source: Water-cooled sealed X‐ray tube with Cu anode (1.54 Å wavelength)
    • Highly sensitive detector with in-plane arm
    • Multiple sample stages, including a non-ambient chamber for high-temperature in situ measurements
    • Customizable optics for the incident and diffracted beam
    • Auto-alignment of samples
    • Access to PDF4+ database and CSD database on separate data processing computer
    • Various user manuals in hard-copy and electronic formats
  • Xradia X-Ray Computed Tomography (XCT)

    Xradia MicroXCT-200 X-Ray Computed Tomography for 3-D Visualization

    CALENDAR | XCT Rates

    XCT.jpg

    Location: MSB 108

    The Xradia MicroXCT-200 reconstructs a sample’s 3D internal structure by measuring the X-ray transmission from multiple perspectives. 2D projections of the sample are acquired at discrete angles as the specimen is rotated 180°. These 2D radiographs are reconstructed into a 3D volume using a Filtered Back Projection (FBP) algorithm. The 3D volumes can be quantitatively analyzed using available Avizo software or other programs to provide detailed microstructural measurements and 3D renderings.

     

    XCT Technique Summary:

     
    • Non-destructive measurement of the internal 3-D microstructure of solids
    • 3-D spatial resolution from 0.7-1.0 µm
    • Typical acquisition times of 1-10 hours
    • Works best for samples that are cylindrical in shape
    • Compatible with biological, polymer, ceramic, metal and composite samples
    • Contrast in proportional to material density
    • Compatible with in situ mechanical testing, electrochemical and heating/cooling stages
     

    XCT Features:

     
    • Air-cooled X-ray source with a range of 20-90 kV voltage and 1-8 W power
    • Detector has a 2048 x 2048 pixel array
    • Maximum sample size 100 mm wide by 150 mm tall
    • Maximum sample weight 1 kg
    • Resolution of up to 0.7 microns, depending on sample size, composition and imaging parameters
    • Sample stage travels 90 mm along X-axis, 50 mm along Y-axis, and 10 mm along Z-axis (parallel to X-ray beam), with 360° rotation
    • X-ray detector travels 120 mm
    • X-ray source travels 85 mm
    • Easily interchangeable filters to optimize contrast
    • Two different magnification settings
    • Clamp-, clip- and vise-style sample holders to accomodate a variety of sample sizes and shapes
    • Ergonomic station for comfort during experimental set-up
    • Access to Avizio software for image reconstruction on a separate data-processing computer
    • Various user manuals in hard-copy and electronic formats