Specific Process Knowledge/Characterization/XRD/XRD Powder

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The XRD Powder setup

The XRD Powder located in the basement of building 346 at Nanolab, Room 904.

The "XRD powder" is an Aeris Research edition benchtop X-ray diffractometer from Malvern Panalytical. It is meant for phase analysis of powders, is easy to use, and offers the option of making measurements while heating the sample in a N₂ atmosphere. The setup allows X-ray diffraction measurements in Bragg-Brentano mode (i.e., Theta-2Theta measurements where the incident and diffraction arms of the goniometer are coupled). We have a very limited selection of optics for this instrument, so there is little that the user can adjust.

Please contact the equipment responsible if you would like to mount the special sample holder for heating during the measurement.

The user manual(s), user APV(s), technical information, and contact information can be found in LabManager:

XRD Powder in LabManager

Process information

• A detailed manual on the Aeris XRD is found on the of the International Ocean Discovery Project.

Malvern Panalytical has a large collection of webinars on XRD. You have to register to view them but the amount of email you receive afterwards is modest, so it's worth it in my opinion (Rebecca, July 2022).

• A nice webinar about sample preparation: XRD data quality with good sample preparation

• A tutorial which also mentions sample preparation about half-way through and explains very briefly some of the issues that can arise from displaced samples, not having a thick enough sample layer, odd sized sample particles, etc.

Software

After making a measurement, you will need dedicated software for the data export and analysis.

For data export

On the Cleanroom drive you can find the DataViewer software, which is a very basic program that allows you to view your measurement results and export to other formats, e.g., csv or txt. To install DataViewer, go to the folder O:\CleanroomDrive\_Equipment\XRD Powder\XRD Aeris\XRDMP and click "setup" (XRDMP stands for XRD Measurement Program). This will open a menu that allows you to install both DataViewer and XRDMP Creator. Just choose to install DataViewer. XRDMP Creater is only needed if you have made an agreement with the equipment responsible that you are allowed to create your own measurement routines.

For data analysis

We have a license for the software "HighScore" for Rietveld refinement, allowing quantification of the phase composition. This is so far only available on the support computer by the instrument, but will become available on a remote computer.

Additional software for measurements in a heated atmosphere

If you are going to make measurements in a heated N₂ atmosphere, you will need the Nambicon software to control the heater. It is found in the folder O:\CleanroomDrive\_Equipment\XRD Powder\XRD Aeris\Anton Paar Nambicon.

Equipment performance and process related parameters

Equipment		XRD Powder
Purpose	Crystal structure analysis and thin film thickness measurement	Phase ID Crystal Size Crystallinity
X-ray generator	Maximum rated output	600 W
	Rated tube voltage	40 kV
	Rated tube current	15 mA
	Type	Sealed tube
	Target	Cu
	Focus size	0.4 mm x 12 mm (Line)
Goniometer	Scanning mode	incident / receiver coupled
	Goniomenter radius	145 mm
	Minimum step size	0.001° (3.6")
	Sample stage	Fixed with rotation
	Sample size	Powders
Optics	Incident side	0.04° soller slit Ni and Cu filter Divergence slits Beam mask
	Receiver side	0.04° soller slit Ni filter
Substrates	Measurement temperature	May be heated in N2 up to 500 °C
	Substrate size	Only for powders
	Allowed materials	All materials have to be approved