Scalable and high yield synthesis of transition metal bis-diazabutadienes

摘要

The present disclosure is directed at the synthesis of transition metal bis-diazabutadienes as precursors to enable atomic layer deposition (ALD) or chemical vapor deposition (CVD) of transition metals on metallic surfaces. The transition metal bis-diazabutadienes may be prepared in a two-step synthetic procedure at relatively high yields and are particularly suitable for industrial scale-up.

主权项

1. A method for forming a transition metal bis-diazabutadiene comprising:
reacting in a first step, in the absence of a reducing agent, a diazabutadiene (DABD) with a transition metal halide and forming a DABD-metal halide complex, wherein said DABD has the following structure: wherein R1 is a C1-C12 alkyl group, amine or a C6-C18 aryl group and R2 is hydrogen, a C1-C10 alkyl, a C6-C18 aryl group, amino, C1-C12 alkylamino or a C2-C24 dialkylamino group; said formed DABD-metal halide complex has the following structure: wherein R1 is a C1-C12 alkyl group, amine or a C6-C18 aryl group and R2 is hydrogen, a C1-C10 alkyl, a C6-C18 aryl group, amino, C1-C12 alkylamino or a C2-C24 dialkylamino group, X is Cl or Br and M is a transition metal; reacting in a second step said DABD-metal halide complex with additional DABD in the presence of a reducing agent and forming a transition metal bis-diazabutadiene of the following structure: wherein R1 is a C1-C12 alkyl group, amine or a C6-C18 aryl group and R2 is hydrogen, a C1-C10 alkyl, a C6-C18 aryl group, amino, C1-C12 alkylamino or a C2-C24 dialkylamino group and M is a transition metal; wherein said yield of the transition metal bis-diazabutadiene is at or greater than 85%.