Powder X-ray Diffractometer at the Imaging and Chemical Analysis Laboratory (ICAL), MSU-Bozeman

Powder X-ray Diffractometer (XRD)

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Bruker D8 ADVANCE powder diffractometer

Provenance: Dave Mogk, Montana State University-Bozeman
Reuse: Image used by permission from Bruker

This XRD instrument is set up with standard goniometer and Bragg-Brentano X-ray optics for acquisition of XRD spectra for phase identification. It can also be rapidly reconfigured with parallel beam X-ray optics for grazing incident diffraction (GID) thin film analysis and reflectometry (surface roughness, density, thickness of layers) analysis.  Software packages include Rietveld, thin film, residual stress, and nanoparticle analysis. JADE software is also available for data reduction and representation. This instrument is also equipped with an environmental chamber with a HTK 1200 N oven chamber for measurements from room temperature up to 1200°C.

Bruker D8 ADVANCE Powder X-ray powder diffractometer (XRD)

Applications are found in all physical and material sciences to characterize the atomic structure of natural and engineered materials. Applications include:

• Phase identification
• Unit cell refinement (Rietveld method)
• Quantitative XRD
• Grazing Incident Diffraction and Reflectometry
• Residual Stress Analysis
• Phase transitions as a function of Temperature in the attached furnace

X-ray powder diffraction is typically used for a) phase identification based on crystal strucure, b) Rietveld analysis is used for crystal unit cell refinements and for quantitative analysis, c) grazing incident diffraction (parallel beam) is used for thin film analysis and reflectometry is used to determine surface roughness, density and thickness. This instrument is equipped with an environmental chamber to do dynamic experiments under a range of temperatures and ambient atmospheric conditions. XRD is commonly used in engineering, material science, ceramics, metallurgy to verify the presence (or absence) of phases, for QA/QC experiments, and in natural (Earth and environmental systems) to identify minerals, their atomic structure, and to perform quantitative analysis to determine abundances of a phase in a complex matrix (soil, rock). XRD is the most common method to characterize clay minerals.

As a regional user facility, we prefer that researchers take our short course in the use of the instruments so that the users can design and implement their experiments to address their own research objectives. ICAL staff are always available to assist with instrument set up, data acquisition and data interpretation. For users with a limited number of samples, it is often more efficient for ICAL staff to simply run the analyses.  Samples submitted by external users (industrial, academic at other institutions or agencies) can be analyzed on a contract basis (i.e. lab personnel will do the work).

Contact the lab manager for details about user fees. In general, user fees are applied only to actual beam time for instrument use and staff time.

Scheduling is supervised by the lab manager. In general, class demonstrations/projects are scheduled to accommodate academic schedules. External clients (other universities, government agencies, corporate) are scheduled for rapid turn-around of results. All certified users (who take our ~10 hour short courses) are authorized to sign up for instrument use 24/7 at our reservation site: https://www.montana.edu/cpa/apps/ical_tools/index.php . We prefer certified users to design and implement their own experiments, but lab staff are available to assist independent users as needed in experiment design, instrument operation and interpretation of results. ICAL is a node of the National Nanotechnology Coordinated Infrastructure program, and our mission is to extend use of these instruments to support research across the STEM disciplines in academic and corporate research. Some limited funds are available through the NNCI/MONT NSF award to support pilot research projects. Please visit https://nano.montana.edu/ for details.

Remote operation is not directly possible for any of the ICAL instruments. But in response to the COVID lockdowns, we have implemented use of real-time video delivery to allow external users to observe analysis of their samples and to provide for direct interaction and decision-making as the experiments proceed.

Samples are usually prepared as powders that are analyzed as random grain mounts. Clay minerals are analyzed as samples that have been separated by size using centrifuge or gravitational settling methods, and oriented samples are prepared using a vacuum-filter apparatus and analyzed with treatments that include air drying, glycolation, and baking at 400 and 550 degrees C.

Phase identification is done by search/match to databases such as ICDD. The instrument is calibrated with NIST corundum and quartz standards.

In addition to search/match software, the JADE analytical software is used to apply Rietveld analysis for structural refinements and for quantitative analysis.

ICAL routinely offers class demonstrations and supports course projects across the STEM disciplines. We encourage interested users to take our 10 hour short courses in the operation of each instrument to become independent users of this facility as part of our professional training program.

• Class demonstrations are available for undergraduates
• Class demonstrations are available for K-12
• Undergraduate student research projects are invited
• Graduate student research projects are invited
• Tutorials and other educational materials related to the lab are available

The ICAL facility is partly funded by the NSF National Nanotechnology Coordinated Infrastructure Program, award #2025391, Montana Nanotechnology Facility (MONT). This XRD instrument was purchased through a grant facilitated by the Energy Research Institute at Montana State University through the DOD Army Research Lab,  Rob Walker, Nicholas Stadie and Stephen Sofie are the PIs.