Breakerspace XRD Tutorial

Overview:

Use our Panalytical Aeris Research XRD (X-ray diffractometer) to analyze properties such as phase composition, crystal structure, and orientation of solid samples, with precise results in less than five minutes.

Index:

Standard operating protocol - (startup, operation, shutdown)
Materials and sample prep
Detailed operating instructions
Data processing and analysis
Common failure modes
Manufacturer manuals
Links
Exercises

Standard operating protocol:

Instrument startup:

Make sure at least one position in the sample changer is free (no sample holder in place)
Turn the mains power switch at the rear of the instrument
Make sure that the cover is closed
Press the power button to switch on the instrument
Turn the HT keyswitch to switch on the HT generator

Operation:

Prepare your sample externally at the sample prep table
Put the sample holder in a loading position on the sample changer
Select a measurement program from the drop-down list
Put in a descriptive sample name
Start the measurement
Export results to networked workstation or USB drive
Fill out your information in the X-ray safety log book
Repeat as needed - additional samples can be loaded and added to the queue while current sample is being measured

Instrument shut down:

Press the Power button to switch off the instrument
Turn the HT Keyswitch counter-clockwise to switch off the HT generator
If the instrument will be switched off for a long period of time, you can also switch off the mains power supply

Compatible materials and sample prep:

The Aeris has a Cu Kα x-ray generator with penetration on the order of 100 µm. For powder samples, grain size should be on the order of 5-10 µm to ensure sufficient grains of various compounds contribute to the reflection of the beam. This source will cause fluorescence in samples with iron and manganese, and may not provide suitable results for samples with those elements.

Panalytical provides an excellent sample preparation guide, available in paper form in the lab and here in pdf form, please refer to it for instructions on use of the different types of sample holders and associated sample prep techniques.

Page 1.4 lists all the various types of sample holders that can be obtained. Of those, we have:

PW1811/00 and PW1811/27 for back or front loading of powders
PW1812/00 for odd shapes (fixed with plasticine or wax)
PW1813/26 for metal plates, membrane filters, pressed pellets, etc.

XRD sample holders are stored in a drawer at the sample prep table. The adjacent cabinet has small supplies you may need, such as spatulas. Perform all sample loading steps at the table and transfer sample holders to the instrument on the tray once complete.

Detailed operating instructions:

Sample Loading:

Remove plastic sample changer cover
Place a prepared sample in any of the six positions on the sample changer
Replace plastic sample changer cover

GIF of sample loading

Running a measurement program:

GIF of selecting and running a program

Exporting data:

GIF of data export

Data can be saved on a USB drive, or exported to a shared network drive on the XRD workstation to the right of the instrument. The workstation can be accessed using a common login. The user name is XRD double check! and the password is xrd-password. Data can be found in the folder C:\ fill in folder path

Screenshot of folder showing path

New measurement programs:

New measurement programs can be created using the software XRDMP Creator on the workstation that supports the XRD, though programs stored on the instrument should cover most basic analysis needs. Documentation on the use of XRDMP Creator is available in the XRDMP Creator Help menu. If you need to create new programs and need assistance, please contact Breakerspace staff.

Advanced mode:

Advanced mode is used to change optical components, manage data (including importing programs, and deleting programs and results), and other advanced configuration tools. Lab users typically will not need to access advanced mode, and instruction of its use is beyond the scope of this tutorial.

Hardware configuration:

The incident beam path includes a fixed divergence slit, beta-filter, soller slits, and a beam mask. The diffracted beam path includes large soller slits and a large beta-filter. The typical configuration is:

Divergence slit -
Beta-filter -
Soller slits -
Beam Mask -
Large soller slits -
Large beta-filter -

Our instrument has a PIXcel^3D, which can provide scanning or static area detection in 2D mode, and scannning or static line detection in 1D mode.

Data processing and analysis:

Data from the Aeris can be processed using HighScore Plus 5.0 or newer
To get started, please see the HighScore Plus Quickstart Guide

Common failure modes:

Booting the instrument with all sample changer positions occupied will result in a somewhat opaquely worded error

Manufacturer’s manuals:

Exercises:

coming soon