For air sensitive materials, the handling of samples during storage, shipment, and measurement should be carefully considered depending on the possibility for sample degradation under ambient conditions. e sample holders discussed above as-is are not specifically designed to be sealed against oxygen or moisture from the air. Nevertheless, we have tested some protocols for working with hygroscopic materials that are suitable for minimizing moisture uptake.
Shipping and Storage of Air Sensitive Samples
Example of coffee bag for sealing samples under inert gas.
Seal samples under inert gas for shipping to avoid degradation.
- load samples under inert gas into individual containers
- close container tightly and cover with parafilm
- place sealed containers into coffee bags under inter gas to avoid air leaks during shipment
Note: if samples should be loaded in the glovebox, then they should be placed in a properly sealed container that can withstand medium vacuum conditions during the purging of the antechamber.
Preparation of Samples in the Glovebox
Samples are then unpackaged and loaded under argon in a glovebox, and sealed with an extra layer of polyimide tape.
Glovebox for handling air sensitive samples under inert environment to prevent degradation.Sealing Samples into the Sample Holders
For very sensitive samples, an extra layer of polyimide tape is used to cover the primary windows with a high amount of contact between tape and sample holder around the window edges. Loaded sample holders are kept in sealed containers under argon until just before measurement. If multiple measurements are to be performed during the same beamtime, the sample holders are additionally stored in a desiccator between measurements.
Sample holder with additional layer of polyimide tape added over the primary sample well windows.
Clips added over the additional layer of polyimide tape to clamp down and provide pressure around the sealed layers.Method Success
Although this has been successful for very hygroscopic materials like LiZrCl-type solid state electrolytes, we cannot guarantee that it will work for everything. Note, this is not suitable for materials that react violently or produce harmful products when exposed to air.