Equipment and Trainings
PANalytical X'Pert Pro MPD Diffractometer
The PANalytical X'Pert Pro MPD diffractometer (P-XRD) analyzes polycrystalline samples with a sealed tube Cu X-Ray source and an X'Celerator detector. A Ge monochromator also routinely provides a monochromatic source of the Cu Kα1 wavelength (1.5406 Å). Programmable divergence and anti-scatter slits enable the use of both fixed slit (for amply thick sample volumes) and automated slit (for very thin sample volumes) configurations.
The standard configuration of the instrument includes a 15-position automatic sample changer coupled to a reflection/ transmission sample stage with sample spinning capabilities. A bracket sample stage is available for mounting wafers, films, and other flat solid samples (< 3.0 mm thick).
For in-situ high temperature experiments with powder samples, the instrument is equipped with an Anton Paar HTK 1200 high temperature stage (300-1200°C). For air-sensitive samples, the instrument is equipped with a capillary sample mount and a focusing mirror.
The PANalytical software programs X’Pert Data Collector (v ), X’Pert Data Viewer, and X’Pert HighScore Plus (v. 3.0) are employed to collect, view, and analyze P-XRD data. Access to the International Center for Diffraction Data (ICDD) database is also available.
The P-XRD is routinely used to identify crystalline materials, calculate the crystallite size of nanomaterials, quantify mixtures of crystalline solids, refine crystal structures via Rietveld refinement, perform in-situ high temperature experiments, and perform capillary experiments for air-sensitive samples.
Policies and Procedures
- Use of the P-XRD is free of charge for individuals and groups affiliated with BYU.
- To run experiments autonomously, users must complete the requisite trainings (see the Training Information tab).
- Once trained, schedule time with the P-XRD here.
- To submit a sample to the XRD facility for employees to analyze:
- Print and fill out this form.
- Place your sample and the printed, completed form in the sample submission box in the center of the south wall of C330 BNSN.
- Be sure your sample fits one of the sample sizes listed below. Sample holders are available at the XRD Facility.
- Write your name and your lab's Principle Investigator's initials on the P-XRD queue board.
Contact XRD Facility Manager Dr. Stacey Smith for more information, trainings, assistance in running an experiment, or help submitting a sample for analysis.
Sample Specification Sizes
Materials or particles consisting of more than one crystal or distinct crystal lattice are ‘polycrystalline’ materials. Polycrystalline samples can range from powders and nanoparticles to thin films and machined parts. In essence, if it is solid, crystalline, and can be made to have or form a relatively flat surface, the P-XRD can be used to investigate its atomic structure.
A variety of sample holders are available at the facility. The P-XRD accommodates several sample volumes and forms:
P-XRD Sample Holders | |||||
Composition | Holding Area Dimensions | Sample Volume Required | Sample Form | ||
1 | Standard holder | Steel | 2mm depth, 27mm diameter | 1145 mm3 | Powder |
2 | Standard + 1.0mm insert | Steel + Al | 1mm depth, 25mm diameter | 491 mm3 | Powder |
3 | Standard + 0.5mm insert | Steel + Al | 0.5mm depth, 25mm diameter | 245 mm3 | Powder |
4 | Zero Background holder | Si | 0.1mm depth, 15mm diameter | 18 mm3 | Powder, Solids |
5 | Adjustable height holder | Al | 0-4mm height, 41mm diameter | Variable | Solids |
6 | Tension holder | Al | 0-7mm height, 41mm diameter | Variable | Solids |
7 | Flat slide | Glass | 20mm x 20mm x 0.2mm depth | 80 mm3 | Powder |
SC-XRD
To analyze single crystal samples, the BYU XRD lab is equipped with a MACH3 four circle diffractometer coupled to a Bruker-Nonius FR591 Cu rotating anode X-ray source, a Bruker Apex II CCD detector, and a low temperature (100-300 K) Kryoflex device. The high intensity of the X-ray source combined with the sensitivity of the Apex II detector allows high-resolution data to be collected on crystals with dimensions as small as 10µm. The latest versions of the Bruker Apex2 software are employed to collect, solve, and refine the data.
Access to the Cambridge Structural Database (CSD) is also available.
This instrument is routinely used to solve and refine all molecule single crystal structures. The high intensity of the rotating anode Cu X-ray source can be utilized to collect data on macromolecular samples such as proteins as well.
Powder samples can also be investigated at low temperatures via transmission mode capillary experiments.
Other non-traditional samples such as films and machined parts can be investigated using custom-made sample mounts.
Policies and Procedures
- Use of the SC-XRD is free of charge for individuals and groups affiliated with BYU.
- To submit a sample to the XRD facility for employees to analyze:
- Print and fill out this form.
- Place your sample and the printed, completed form in the sample submission box in the southeast corner of C330 BNSN.
- Be sure your sample fits one of the sample sizes listed below. Sample holders are available at the XRD Facility.
- Write your name and your lab's Principle Investigator's initials on the SC-XRD queue board.
Contact XRD Facility Manager Dr. Stacey Smith for more information, trainings, assistance in running an experiment, or help submitting a sample for analysis.
Sample Specifications
A "single" crystal is a solid in which the crystal lattice is continuous and unbroken (containing no grain boundaries) throughout the entire sample. Single crystals for SC-XRD experiments typically have dimensions between 20-500µm, though crystals with dimensions as small as 10µm have been successfully characterized, and crystals larger than a few hundred µm can be cut into more suitably sized pieces.
Good single crystals typically have well-defined faces and are transparent (not cloudy, cracked, or otherwise opaque). They also often rotate plane polarized light. If the plane of polarization is changed continuously as shown in the video, the crystals grow bright then dark or even change colors. To evaluate crystal quality, a microscope with a polarizing lense is available in C330A BNSN.
The following links are useful resources for growing single crystals.
NCSU: Growing X-Ray Quality Crystals
NCSU: Growing Crystals That Will Make Your Crystallographer Happy
Peter G. Jones: Crystal Growing
Rochester: How to Grow X-Ray Quality Crystals
UCLA: Crystal Growing Tutorial
Bruker: Growing and Mounting Single Crystals Your Diffractometer Will Treasure
MSU: Growing and Mounting Crystals Your Instrument Will Treasure
The two computers along the south wall of room C330 in the XRD facility are available for offline processing of XRD data. The software packages for analyzing data from both the P-XRD and SC-XRD are installed on both computers.
The XRD lab is both a user facility and a service facility. The appropriate trainings must be completed by users who wish to use XRD equipment independently.
Please contact XRD Facility Manager Dr. Stacey Smith if you need training. The following training modules are available:
- X-Ray Safety
- This training is required to obtain access to the facility and the instruments. Complete the online training module and answer all questions of the follow-up quiz correctly to gain access.
- Basic P-XRD
- This training is required to obtain access to the XRD facility and the P-XRD instrument. Topics include sample preparation, instrument setup, running the Data Collector software, writing data collection programs for the 15-position sample changer, and performing basic data processing with the HighScore Plus software and ICDD database.
- P-XRD Operations Instructions Handout
- Crystallite Size Analysis
- Topics include a discussion of the theory/equations involved, data collection requirements, basic profile-fitting techniques using Highscore Plus, determining instrumental broadening parameters, making/using a template, and using a Williamson-Hall plot.
- Rietveld Refinement & Quantitative Analysis of Mixtures
- Topics include a discussion of the theory/equations involved, data collection requirements, determining instrumental broadening parameters, using .cif files, crystal structure nomenclature, and basic fitting techniques using HighScore Plus.
- P-XRD Temperature Variable Experiments
- This training is required to independently use the high temperature stage for the P-XRD instrument. Topics covered include mounting the stage, sample preparation/mounting, operating the stage, writing data collection programs, and processing the data using HighScore Plus.
- P-XRD Capillary Experiments
- This training is required to independently use the capillary stage for the P-XRD. Topics covered include mounting the stage, sample preparation/mounting, operating the stage, writing data collection programs, and processing the data using HighScore Plus.
- SC-SXRD Temperature Variable Experiments
- This training is required to independently use the SC-XRD to perform low temperature experiments. Topics covered include sample preparation/mounting, operating the instrument, writing data collection programs, and processing the data using the Bruker Apex II software.
- Miscellaneous Topics
- Other, specialized topics and questions can be addressed via one-on-one training.