I need to do a low temperature (200°C) molten salt coactivated magnesiothermic reduction (MgR) of SiO2 but I don't have a proper crucible. In literature SS sealed containers are often used for MgR reactions, but when looking for "sealed SS containers" on Google I can't easily find something that seems fit for the purpose, as I need an airtight system which preserves the internal inert atmosphere (Ar).
Does anyone has a suggestion on where to look?
Thank you in advance for any suggestion.
Dear Eva Gualtieri many thanks for this interesting technical question. Various companies sell stainless steel crucibles which are not "sealed" but have lids, e.g.:
https://www.southernlabware.com/laboratory-supplies/crucibles/crucible-stainless-steel-with-lid.html
Even if those lids / covers are loose-fitting I assume that your could run the reaction under a flow of argon or nitrogen. Stainless steel is recommended in any case as slumina could also be reduced by the magnesium.
It might also be useful to have a look at the answers given to a closely related RG question about magnesiothermic reactions:
How to do the magnesiothermic reduction of silica?
https://www.researchgate.net/post/How-to-do-the-magnesiothermic-reduction-of-silica
(6 answers)
Also please see the following very interesting review article entitled:
A review of magnesiothermic reduction of silica to porous silicon for lithium-ion battery applications and beyond
Article A Review of magnesiothermic reduction of silica to porous si...
This paper has been posted by the authors as public full text on RG, so that it can be freely downloaded as pdf file.
I hope this helps. Good luck with your research and best wishes, Frank Edelmann
I hope the following link for company might help you:
http://www.decentmining.com/product/multi-firing-fire-assay-clay-crucible?gclid=CjwKCAjwos-HBhB3EiwAe4xM96qlTze13rXlQe7xwFj2YMieTnMjyqiLPoNZCDnPjcxLokxPgZ3-3RoC6cwQAvD_BwE
Dear Frank T. Edelmann and Aref Wazwaz
I would like to thank you both for spending your time to answer me, but my search is not finished yet. I want to add some other details,
In my lab I have a quite small tubular furnace (4.5 cm minimum diameter) so it's not easy to find a crucible small enough to fit, but big enough to contain my reaction product. I have boat-shaped quartz crucibles, but I'm not sure if it's suitable for a MgR.
Boat shaped SS crucibles would be the perfect solution for my case, but I can't find them for sale, I'd have to look for some custom made crucible.
Well, good luck to me.
You are most welcome dear
Dr Eva Gualtieri . I hope that I could help you more to solve your issue completely very soon. Wish you the best always.
Dear Eva, I just came across an offer of boat-shaped crucibles made of tungsten instead of stainless steel. The company also sells a variety of other crucibles. It migth be worth having a look at their homepage:
https://www.alibaba.com/product-detail/vacuum-evaporation-coating-tungsten-boat-and_60562147414.html
Does your institution have a repair workshop where they can make custom stainless steel crucibles / boats for you?
Thank you again for the suggestions Frank T. Edelmann !
I should probably ask the mechanical engineering department for custom-made crucibles (I am quite new in my University so don't know if they have such repair workshops, but hopefully they have them).
For the moment I will try to carry on a trial reaction in an old quartz boat to see what happens, if it won't be successful/will give me problems I'll purchase something better by September.
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