We recently started working on an air-sensitive material which we usually keep in a nitrogen glovebox. We need a sturdy and reliable way to transfer the material to a UHV-system for characterization without any exposure to air. What would be the best way to do this?
There are a multitude of devices described on the internet: https://www.youtube.com/watch?v=7I_dAIzx0AY https://www.researchgate.net/publication/221729191_Airtight_container_for_the_transfer_of_atmosphere-sensitive_materials_into_vacuum-operated_characterization_instruments http://orbit.dtu.dk/files/55725523/Low_cost_transportable_device.pdf
What is the dimensions and nature of the sample? What is the UHV system?
How about using an Aldrich AtmostBag:
https://www.sigmaaldrich.com/labware/products/aldrich-atmosbag.html
Otherwise can you use a piece of glassware fitted with valves so that you can fill with an inert gas, seal, and then transport.
At my previous institute we built our own adapter system by which we also could transform our UHV-air-lock into a minor glovebox. You can find some descriptions in my PhD Thesis (DOI: 10.5445/IR/1000076200 , document page 43=content page 37). The descriptions are only in German, but if you're interested in details, feel free to ask. At the Elettra synchrotron to which we transferred those samples they put a vacuum tent similar to the Bag Jules Lloyd Hammond suggested in front of their vacuum setup in order to be able to use screwdrivers under clean conditions. We didn't observe oxygen contamination of our samples, so both sides seemed to work.
Hallo Derek,
you need a container consisting of UHV-standard parts. You fill this container within the glovebox. After this you connect the container in a suitable manner with the transfer unit of the UHV-chamber. Then you pump down and transfer into UHV main chamber. It is principially easy but you need at least one valve and this could be expensive.
Yours
R. Mitdank
Hello Derek,
in the context of our work we had a direct connection between the two, that is, we could reach from (a kind of load lock chamber of) the UHV system into the glove box with a magnetic transfer rod. (The glove box was ordered to have an extra port with a 4.5" CF flange for that purpose).
- sufficiently slowly vent the load lock with the glove box atmosphere, do the transfer, and get back to pumping. Typically, within 10 min we were below 10-8 mbar.
In working like this (and adhering to a strict protocol concerning venting & pumping) we managed to get data from very air-sensive colloidal magnetic nanopartices. Since we had to go through solution phase, working with well distilled solvents in the glove box was also a must.
Cheers
Kai
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