Procedures
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.
Sample Form:
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. Contact XRD Facility Manager Dr. Stacey Smith for more information, trainings, assistance in running an experiment, or help submitting a sample for analysis.
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.
Trainings
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 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.
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 | |||||
| Type of Holder | 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 |
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.
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.
Miscellaneous Topics
- Other, specialized topics and questions can be addressed via one-on-one training.