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 with a Cu source 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. The instrument has a 1D strip detector, which makes data acquisition very efficient, so you can measure your samples relatively quickly. The detector also has a fluorescence suppression option, so you can measure samples containing for instance iron with the copper radiation.

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 - requires login

Process information

• Tips for choosing among the scan and hardware parameters including fluorescence suppression: XRD Powder measurement tips

• 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). Some useful webinars include:
  • Better XRD data quality with good sample preparation
  • A beginner’s 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

To adjust measurement parameters and analyze the data, you will need dedicated software which is described here: XRD Powder software

Equipment performance and process related parameters

Equipment		XRD Powder
Purpose	Crystal structure analysis	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
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