Scalable and high yield synthesis of transition metal bis-diazabutadienes

• US 9,067,958 B2
• Filed: 10/14/2013
• Issued: 06/30/2015
• Est. Priority Date: 10/14/2013
• Status: Expired due to Fees

• Current Assignee: Intel Corporation
• Original Assignee: Intel Corporation
• Inventors: Romero, Patricio E.
• Primary Examiner(s): NAZARIO GONZALEZ, PORFIRIO
• Application Number:
  US14/053,249
• Publication Number:
  US 20150105573A1
• Time in Patent Office: 624 Days
• Field of Search: 556/35, 427/252
• US Class Current: 1/1
• CPC Class Codes: C07F 15/025 without a metal-carbon linkage
• CPC Class Codes: C07F 15/045 without a metal-carbon linkage
• CPC Class Codes: C07F 15/065 without a metal-carbon linkage
• CPC Class Codes: C23C 16/18 from metallo-organic compounds
• CPC Class Codes: C23C 16/45553 characterized by the use of precursors specially adapted for ALD

Abstract

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.

Claims

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;

2. The method of claim 1 wherein:

R₁ in said diazabutadiene comprises a C₁-C₁₂ alkyl group;

R₂ in said diazabutadiene comprises hydrogen;

R₁ in said DABD-metal halide complex comprises a C₁-C₁₂ alkyl group;

R₂ in said DABD-metal halide complex comprises hydrogen;

R₁ in said transition metal bis-diazabutadiene comprises a C₁-C₁₂ alkyl group; and

R₂ in said transition metal bis-diazabutadiene comprises hydrogen.

3. The method of claim 1 wherein said transition metal halide comprises a transition metal that is selected from Cr, Fe, Co or Ni and said halide is selected from Cl, Br or I.

4. The method of claim 3 wherein said transition metal is Co and said halide is Cl.

5. The method of claim 1 wherein said DABD-metal halide complex comprises:

6. The method of claim 1 wherein said transition metal bis-diazabutadiene comprises the following structure:

7. The method of claim 1 wherein said reducing agent comprises Na, Li, Mg or Al.