McMaster Analytical X-ray Diffraction Facility (MAX)

McMaster University, Hamilton, Ontario
What the facility does

X-ray diffraction characterization of materials and chemicals (structures, phase ID, texture, residual stress, reflectometry, reciprocal space mapping, training).

Areas of expertise

The McMaster Analytical X-ray Diffraction Facility (MAX) is a service, research, and teaching facility. It is a one-stop solution to materials characterization problems. Experienced and dedicated staff help determine structural and compositional information of material through their advanced knowledge in X-ray diffraction. Not only does MAX offer a suite of diffractometers and sample preparation space that can be used for characterization needs, but staff members are fully equipped and available to train users, acquire various data, prepare characterization reports, and consult on user’s specific questions.

As a user’s facility we offer training services on our instruments, or if preferred, we can perform full sample characterization starting from sample preparation to final results. To facilitate our user’s learning experience and networking, we also organize various tutorials and workshops throughout the year. Our vision is to be one of the leading X-ray diffraction facilities in the world for the quality of the scientific research and for promoting interactions amongst researchers in various fields nationally and internationally.

Research services

Single Crystal Diffraction (SCD): The MAX Diffraction Facility has a dual microsource (Mo/Cu – molybdenum/copper) for single crystal structure determination. We can determine solid state structures, and molecular structures (inorganic, metal organic, organic, polymeric). A Mo image plate single crystal diffractometer is also in regular use, in particular for solid state samples. We have also developed a software package (MAX3D) which allows us to study diffraction data in detail in three dimensions. We can rapidly and readily identify regions of diffuse scattering, incommensurate scattering, twinning, or Bragg spot distortions.

Texture and Residual Stress Analyses (XRD3): We use area detectors for efficient scanning of reciprocal space for diffraction from polycrystalline solids. We have developed unique techniques for quality and orientation analyses of electronic thin films and nanowire surfaces, including visualization of the full diffraction pattern, and real-time scanning of raw pole figures (MAX3D). Quantitative component orientation distribution analyses are performed using Bruker’s Texture software or the MTex module in MATLab. Leptos (Bruker) is used for residual stress analysis with area detector data. Co radiation is used to eliminate fluorescence from ferrous materials. The Eiger2-500 detector is a zero background, real-time area detector, which allows for high-speed, high-resolution powder diffraction. We also have low and high temperature accessories – sample temperature range: 90K to 850K, and x-y microbeam mapping capabilities.

Rapid Phase Analyses (XRD2): A single 2D frame of diffraction data from a rotating polycrystalline solid or powder gives very high S/N in a very short time, making it a cost-effective analysis. It has the advantage of minimizing preferred orientation effects (after integrating 2D to 1D) as well as giving visual evidence of the granularity of the (various) phase(s). The Eiger detector on our Co (cobalt) instrument also allows data collection using 1D or 2D continuous scans, which result in sharper diffraction features.

High Resolution Powder Diffraction (XRD): High spatial resolution in a powder diffraction pattern allows for quantitative phase analyses, Rietveld structure refinement, and ab initio crystal structure solutions. We use focusing optics on a Rigaku SmartLab diffractometer to obtain a sharp diffraction pattern with a linear detector. Bruker’s DIFFRAC.EVA software is used for phase analysis and TOPAS is used for phase refinement, structure refinement, or ab initio structure solution. The SmartLab can also be configured with a 4-bounce Ge mirror and a 2-bounce analyzer for HRXRD on thin films.

X-ray Reflectometry (XRR): Reflectometry measurements of nano-layered (crystalline or non-crystalline) materials can be done with our Rigaku SmartLab thin film instrument. The variation in layer density will give an interference pattern which will Fourier transform to a sequence of thicknesses, given a suitable starting model.

Sectors of application
  • Automotive
  • Chemical industries
  • Education
  • Life sciences, pharmaceuticals and medical equipment
  • Manufacturing and processing
  • Mining, minerals and metals
Bruker VENTURE Dual Source (Cu Iµs/Mo IµS) single crystal diffractometerSingle crystal and microcrystal structure solution, absolute configuration, reciprocal space mapping, microdiffraction of powders or polycrystalline solids or films.
Rigaku High Resolution X-ray Diffraction SmartLabWith thin film or Bragg Brentano configurations. Linear detector. High resolution thin film diffraction using 4-bounce Ge (germanium) monochromator and 2-bounce analyzer. Also suitable for X-ray Reflectometry on thin films. Also can do phase ID, phase quantification, and ab initio structure solution from powders.
Bruker D8 DAVINCI Diffractometer with Co parallel-beam source and Eiger2 R 500K area detectorPhase ID, weight percentage estimations, texture, residual stress, reciprocal space mapping, microdiffraction; suitable for ferrous materials, powders, alloys, additive manufacturing products, polymers, thin films, etc.
Bruker D8 DISCOVER Diffractometer, Cu source, Bruker Vantec-500 area detectorPhase ID, weight percentage estimations, texture, residual stress, reciprocal space mapping, microdiffraction; powders, alloys, additive manufacturing products, polymers, thin films, etc.
STOE single crystal diffractometer, Mo source, Imaging Plate detectorStructure determination from single crystal; ambient temperature to 85K; solid state, inorganic, organic, organometallic crystals; twinning; reciprocal space mapping.
PANanalytical X’Pert Pro x-ray diffractometer (XRPD), Cu Kα1 source, X’Celerator linear detectorPhaseID, weight percentage estimations, Rietveld refinements; powders.