Nickel

Zero-Valent Reaction:

Synthesis Setup:

Chemicals:

Tetrakis(triphenylphosphine) nickel(0), bis(1,5-cyclooctadiene) nickel(0), acetone

Procedure:

Nickel is intercalated by decomposition of nickel(0) coordination compounds. Because these compounds are so sensitive to air, it is necessary to use a Schlenk line or alternative air-free setup. Use Fig 3 or follow the procedure for Cr above. Before beginning, place the 2D material in the round-bottom flask, run nitrogen into the column and flask for ~ 30 mins. Alternatively, if on a Schlenk line, place the 2D materials or substrate in the round bottom flask, evacuate, and flush with N₂ or argon gas.

Prepare two stock solutions in a glovebox. Stock solution 1 should have 5 mL of acetone in a septa vial. Stock solution 2 should contain 5~10 mM of tetrakis(triphenylphosphine) nickel(0) or bis(1,5-cyclooctadiene) nickel(0) dissolved in 5 mL of acetone. For this stock solution, add about 0.01 g of the nickel(0) compound to 5mL of anhydrous acetone in a septa capped vial. Inject in 5mL of air-free acetone (kept in a glovebox and completely free from air) to the flask and heat to reflux. The air free acetone can be placed in a septa capped vial and injected with a syringe that has been flushed with nitrogen three times from the primary flask to prevent any air from getting in. Dropwise, inject the second solution to the flask over the course of 2~3 hours. After completion, wait an additional thirty minutes. Finally, remove substrates or 2D materials from the solution and rinse with acetone in air.

How much can be intercalated into Bi₂Se₃ nanoribbons:

Ni(C₈H₁₂)₂	acetone	time	~ intercalated in Bi₂Se₃
0.01 g	Total = 10 mLs	3 hours	20 atm % ± 3%

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