NMCF X-ray Instrumentation for Bulk (XRD, XRF, XCT) and Surface (XPS) Characterization

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

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

Location: Jesser 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 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

Location: Jesser 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 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

Location: Jesser 112

Coming soon: 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 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

Location: Jesser Hall room 112

The D2 Phaser bench-top X-ray diffractometer from Bruker was added to the lab in May 2023. It is our best diffractometer for measuring the diffraction of samples that would normally fluoresce under Cu X-rays. It is also great for all techniques in which the omega and 2theta arms move in sync. All samples must fit within our powder samples or our small bulk-sample holders (see below for dimensions).

XRD Applications:

• Bragg-Brentano (para-focusing) geometry in reflection mode
• Phase ID
• Quantification of phases
• Rietveld refinement
• Fluoresence suppression

XRD Features:

• Source: Air-cooled sealed X‐ray tube with Cu anode (1.54 Å wavelength) operating at 300 Watts (30 keV / 10 mA)
• Detector: LYNXEYE XE-T
  • 0-D (point) and 1-D (line) modes available, with pseudo 2-D collection via the BRAGG2D technique
  • up to 192 channels covering up to 5.8° 2theta at once in 1-D mode
  • high resolution and high intensity modes availble
• Sample Stage: Single-sample spinner stage
  • Powder sample holders: 27 mm diameter x 2.4 mm deep; 25 mm diameter x 2 mm deep; 16 mm diameter x 2.4 mm deep; zero-background
  • Bulk sample holder: 44 mm diameter x 6.5 mm deep
• Customizable optics for the incident and diffracted beam
  • Four sizes of fixed divergence slits (0.1, 0.2, 0.6 and 1.0 mm)
  • Three sizes of Soller slits (1.5, 2.5 and 4° )
  • Air scatter screen (1 and 3 mm opening) and air scatter slits (3 and 8 mm opening)
  • Ni filters for K-beta radiation (high intensity mode)
  • Cu attenuator
• Diffractometer radius of 141.5 mm with maximum accessible 2theta of 152°
• Data collection software: Diffrac.Measurement
• Data Analysis software: Diffrac.EVA and TOPAS
  • Nine simultaneous users may run the analysis software on any computer connected to the UVA network. Contact NMCF staff for details.
  • Access to the PDF4+ database for search/match algorithms is available only on one data processing computer in Jesser 118.
  • All other computers have access to the Crystallographic Open Database (COD) and/or Cambridge Structural Database (CSD)
• Various user manuals and tutorials in hard-copy and electronic formats