Indium


Zero-Valent Reaction:

In

Synthesis Setup:

Schlenck

Chemicals:

Iron pentacarbonyl, acetone


Procedure:

Indium chloride disproportionates very well in both dimethyl sulfoxide and tetrahdyrofuran. These solvents can be used for intercalation. We have also found that InCl slowly disproportionates in acetone. Indium chloride is air sensitive; intercalation reactions are performed under inert N2 atmosphere using standard Schlenck techniques. Follow the procedure for Cr or setup on a Schlenk line as above.


Place the substrate or 2D materials in the round-bottom flask, evacuate and flush with N2. In a glovebox, prepare two stock solutions. The first (solution 1) should be 3mL of acetone in an air-free septa vial. The second (solution 2) should be 0.015 g InCl dissolved in 3mL of air free acetone. Inject solution 1 of just acetone into the round bottom flask and heat to just below reflux (50°C). Dropwise, inject solution 2 over the course of an hour. Let the solution heat for an additional 20-30 mins. Remove the substrate from solution and rinse with hot ethanol and hot acetone (∼45°C).


Notes: This one you can actually be lazy on because InCl disproportionates so slowly in acetone. You can actually inject the entire solution in and reflux for an hour. I advise the slower route for better results.


How much can be intercalated into Bi2Se3 nanoribbons:

Fe(CO)5 acetone time ~ intercalated in Bi2Se3
0.015 g Total = 6 mLs 1.5 hours 7-17 atm % ± 10%


Relevant Publications:

K.J. Koski, C.D. Wessells, B.W. Reed, J.J. Cha, D. Kong, and Y.Cui, Chemical intercalation of zero-valent metals into 2D layered Bi2Se3 Nanoribbons. J. Am. Chem. Soc. 134, 13773 (2012).

M. Wang, D. Williams, G. Lahti, S. Teshima, D. Dominguez-Aguilar, K. J. Koski, Chemical intercalation of heavy metal, semimetal, and semiconductor atoms into 2D layered chalcogenides. 2D Materials, 5, 045005 (2018)


Supported by NSF DMR-1658019