X-ray diffraction facility

This facility provides mineral identification and quantification, structure refinements, and mineral analytical advice to RSES, the wider ANU community and external customers.

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Dr Michael Förster
michael.forster@anu.edu.au
61251049

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About

Empyrean S3 XRD at RSES
Empyrean S3 XRD, Bragg-Brentano mode, programmable xy+z stage
Empyrean S3 Micro-XRD
Tranmission geometry
XRD analysis of stone axe with Empyrean S3

The XRD facility provides mineral and phase identification and quantification services, crystal structure refinements, and mineral analytical advice to RSES, the wider ANU community and external customers. The Empyrean Series 3 multipurpose XRD accommodates various diffraction geometries, such as micro-XRD and Bragg-Brentano, and a range of sample formats (powders, solids, slurries). 

  • Contact lab manager for quote. Choice between DIY and service.
  • Prerequisites for DIY users: Basic knowledge in Mineralogy (eg. course EMSC 2023).

Instrumentation

Malvern Panalytical Empyrean Series 3 multipurpose X-ray diffractometer with PIXcel3D detector (0D, 1D, 2D modes), CoKalpha radiation (point or line focus)

  • Powder XRD
    • Bragg-Brentano geometry  (incoming optic: BBHD)
    • Transmission geometry
    • Capillary spinner
    • Spinning stage
    • Automatic sample changer (45 samples)
  • Micro-XRD and solid samples
    • Footprint: 50-100 µm  (incoming optic: focussing lens)
    • Programmable xy+z stage
    • Alignment camera
  • Slurry-cell
    • In situ monitoring of crystal growth in liquid medium in transmission mode
  • Irradiated area (beam footprint)
    • Spot analyses:                     50-100 µm
    • Powders and large solids:  2-20 mm length, 8-20 mm width

Sample formats

  • Powders
  • Mineral separates
  • Solids    (hand specimen, thin sections, samples in polished resin-stubs, archaeological artefacts, pottery shards, stone tools, paper, etc. ..)
  • Liquid slurries (for in situ observation of crystal growth)
  • Pastes   (e.g., cement)
  • Sample weight:   1 mg - 10 kg
  • Sample size:        50 µm – 10x10x10 cm
  • Sample holders
    • Low-background (Si or quartz single-crystals)
    • End-loaded
    • Front-loaded
    • Capillary
    • Transmission foils (Kapton, Mylar)

Services

  • Qualitative analysis
  • Quantitative analysis  (determination of phase abundances and amorphous content)
  • Clay identification  (treatments: Mg-saturation, glycolation, 350°C, 550°C)
  • Clay separation  (settling method)
  • Sample preparation  (crushing, milling, micronizing)
  • Illite crystallinity determination  (based on FWHM of 001-reflection, 10 Å)
  • Crystal structure refinement  (Rietveld method)
  • Calcite/Aragonite quantification  (e.g., corals, shells)
  • Training in usage of instruments and software

Sample Preparation Facilities

  • McCrone Micronizing Mill
  • Rocklabs Benchtop Mill
  • Spintron Centrifuge
  • Branson Ultrasonic Probe
  • Millipore Filter Method set-up for preparation of oriented clay samples
  • Drying oven (40°C) and furnace (<1200°C)
  • Fume-hood
  • Capillary alignment microscope
  • Tumbler
  • Accessories: Agate mortars, sieves, balances, desiccators

Data Analysis Software

  • ICDD PDF-2 Database
  • HighScore Plus, DiffracPlusEva 10.0
    • Search/Match
    • Quantitative analysis
    • Rietveld refinement
  • Siroquant V4 and SiPhase
    • Quantitative analysis
  • Topas (academic version)
    • Quantitative analysis
    • Rietveld refinement
  • Newmod
    • Modelling of interlayered clay minerals

Location

ANU