Could anyone suggest an alternative solvent (greener, less odors) for EDT or mercaptoethanol to dissolve metal chalcogenides (e.g. Cu2S) or precursors for metal chalcogenides (such as ZnCl2, Ni(acac)2) in conjunction with an amine?
Dear Thomas, many thanks for sharing this very interesting technical question with the RG community. First of all please note that there is a fundamental difference in solubility between transition metal sulfides (e.g. Cu2S) on the one hand and precursors for metal chalcogenides (such as ZnCl2, Ni(acac)2) on the other hand. Transition metal sulfides are generally more or les insoluble in both water and organic solvents. In contrast, transition metal chlorides are easily soluble in water, while acetylacetonate precursors such as Ni(acac)2 normally dissolve in common organic solvents. The problem here is the choice of sulfur precursors. There are numerous relevant research articles available right here in the "Publications" section of RG. For example, diorganodisulfides have been employed as sulfur-sources in the following study:
Diorganyl Dichalcogenides as Useful Synthons for Colloidal Semiconductor Nanocrystals
Article Diorganyl Dichalcogenides as Useful Synthons for Colloidal S...
Compounds like diphenyldisulfide are practically odorless. The author of this article has an RG account. Thus you can easily contact him and request the full text of the paper.
Good luck with your research and best wishes, Frank Edelmann
Dear Dr Thomas Stergiopoulos . See the following useful RG link: Article Tools and techniques for solvent selection: Green solvent se...
Kindly check also the following good link: https://www.sigmaaldrich.com/deepweb/assets/sigmaaldrich/product/documents/115/677/greener_solvent_alternatives.pdf
Also check please the following very good link: https://www.merckgroup.com/en/research/science-space/envisioning-tomorrow/scarcity-of-resources/cyrene.html
Dear Frank,
thank you very much for your feedback. Actually, I am trying to reproduce Richard Brutchey's recipe with thiol/amine system. It works very well (I tried to dissolve 0.1-1 M Sb2S3 in ethylenediamine/1,2 ethanedithiol 10:1 v/v co-solvent inside the glovebox). My main issue is now the toxicity and the odor of the thiol: I carefully (and quickly) opened the small antichamber of the glovebox to take out the waste (tips, gloves etc.) but the lab was practically full of toxic smells for lots of hours. This is why I am now looking towards a thiol-free recipe :).
Dear Thomas, many thanks for your kind response and explanation. I fully agree with you in that the use of 1,2-ethanedithiol should be avoided if at all possible. To the best of my knowledge, 1,2-ethanedithiol is not really very toxic, but of course the stench of this compound is indeed unbearable. I would also strongly suggest not to take it inside the drybox. Chances are, that you will never get rid of the bad smell in the drybox. Instead, you should search the chemical literature for terms like "thiol-free synthesis of metal sulfide nanoparticles". That way I found the following very useful review article in which various alternative sulfur sources are highlighted:
Synthetic developments on the preparation of sulfides from thiol-free reagents
https://pubs.rsc.org/en/content/articlepdf/2021/qo/d0qo01226b
Article Synthetic developments on the preparation of sulfides from t...
Unfortunately this paper has not yet been posted as public full text on RG. However, three of the authors have RG profiles. Thus it should be very easy to contact one of them directly via RG and request the full text of the article. The review also has 146 references to original research papers, so it should guide you to a number of suitable alternatives such as diphenyl disulfide etc. which do not have such a bad smell.
Good luck with your research and best wishes, Frank Edelmann
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