PXRD Sample holders
You can refer to the videos on the learning centre page for how to prepare powders as thin surfaces on slides or packed into a recession.
For all sample preparations you must:
-
Ensure no loose powder remains on the holder: your sample forming a secure, flat, even surface.
-
Clean the edges of the sample holder so that they can be handled without contamination.
-
Label the sample with your name, the sample's composition, and the date.
It should look like one of the following:
All sample holders for the Bruker D8 Advanced Eco are a circular design. The plastic sample holders are made from PMMA - it is safe to use ethanol or isopropanol when cleaning them but do not use acetone on them, they will dissolve. The recommended sample preparation is powder on a greased slide atop of a PMMA holder. The slide used in the picture is a 22mm circular cover slip (No1), stocked in the CRL stores. The integrated mirrored surface on some sample holders is a silicon wafer cut along a non-diffracting plane to give close to 0 background. These holders are supplied by Bruker and are expensive; a few are available for specialist measurements but the background from a glass slide is of comparable quality. Air-sensitive sample holders made out of aluminium with a thin Mylar film window are made to order by the Chemistry Design and Fabrications workshop. You can contact the Facility supervisor to enquire about new sample holders.
The Malvern Panalytical X'pert and Empyrean diffractometers both have flat bracket and motorised spinner stages. The most convenient, safe and recommended sample preparation is powder on a greased microscope slide. Microscope slides are stocked in the CRL stores. When using a filled recession holder with the flat bracket stage, a glass slide with an etched recession or a aluminium plate with a drilled recession can be used. Air-sensitive sample holders for the flat bracket stage are made out of aluminium with a thin Mylar film window. These are made to order by the Chemistry Design and Fabrications workshop.
See the following for a template for preparing your powder on a microscope slide:
The spinner stage accepts only steel sample holders. Please note these are different from and not interchangeable with the Bruker air sensitive holders! The silicon insert in the image is a silicon wafer cut along a non-diffracting plane to give close to 0 background, not many of these are available.
You can contact the facility supervisor to enquire about new sample holders.
