Molybdenum

Zero-Valent Reaction:

Synthesis Setup:

Chemicals:

Molybdenum hexacarbonyl, acetone

Procedure:

Much like Co, Mn, and Fe, molybdenum is intercalated by the decomposition of molybdenum carbonyl in a solution under inert atmosphere. Again, either use a Schlenk line or use the procedure and setup explained for Cr. Moly carbonyl has a bad reputation in materials science departments. It is used in organic chemistry classes without concern; beware of this strange safety dichotomy and handle the reaction material by reading the MSDS before proceeding.

Setup the reaction according to Fig 3. Place the 2D material in the round-bottom flask, evacuate and flushed with N2 gas. In a glovebox, create two stock solutions. Stock solution 1 should be 5 mL of anhydrous acetone. Stock solution 2 should be created from 0.01-0.03 g of moly carbonyl dissolved in 5mL of air free acetone. Inject stock solution 1 of anhydrous acetone into the round-bottom flask and heat to just below reflux (~45-48°C). Dropwise, inject in the molybdenum (solution 2) over the course of 2-3 hours (note, go slow). After all solution has been injected, allow the mixture to sit just below reflux for 1 more hour. Remove substrates or material from the solution and rinsed with hot acetone and hot ethanol, exposing to air at this point is okay. Remove the substrate and rinse with acetone (25°C).

How much can be intercalated into Bi₂Se₃ nanoribbons:

Mo(CO)₆	acetone	time	~ intercalated in Bi₂Se₃
0.01-0.03 g	Total = 10 mLs	3 hours	2 atm % ± 1%

Relevant Publications:

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