Alkyl group VA metal compounds

• US 6,956,127 B2
• Filed: 01/17/2003
• Issued: 10/18/2005
• Est. Priority Date: 01/17/2002
• Status: Expired due to Fees

• Current Assignee: Shipley Company, LLC (Dow, Inc.)
• Original Assignee: Shipley Company, LLC (Dow, Inc.)
• Inventors: DiCarlo, Ronald L. Jr., Shenai-Khatkhate, Deodatta Vinayak, Power, Michael Brendan, Amamchyan, Artashes
• Primary Examiner(s): NAZARIO GONZALEZ, PORFIRIO
• Application Number:
  US10/346,275
• Publication Number:
  US 20030181746A1
• Time in Patent Office: 1,005 Days
• Field of Search: 556/70, 568/8, 568/16, 427/587, 427/593, 438/604, 438/606, 438/681
• US Class Current: 556/70
• CPC Class Codes: C07F 9/5068 from starting materials having the structure >P-Hal
• CPC Class Codes: C07F 9/52 Halophosphines
• CPC Class Codes: C07F 9/72 Aliphatic compounds
• CPC Class Codes: C23C 16/301 AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi

Abstract

Disclosed are methods of preparing monoalkyl Group VA metal dihalide compounds in high yield and high purity by the reaction of a Group VA metal trihalide with an organo lithium reagent or a compound of the formula R_nM¹X_3−n, where R is an alkyl, M¹ is a Group IIIA metal, X is a halogen and n is an integer fro 1 to 3. Such monoalkyl Group VA metal dihalide compounds are substantially free of oxygenated impurities, ethereal solvents and metallic impurities. Monoalkyl Group VA metal dihydride compounds can be easily produced in high yield and high purity by reducing such monoalkyl Group VA metal dihalide compounds.

Claims

1. A method of preparing a Group VA metal dihalide compound comprising the step of reacting a Group VA metal trihalide with a reagent selected from the group consisting of an (C₁-C₁₀)alkyl lithium compound and a compound of the formula R_nM¹X₃₋

n wherein each R is (C₁-C₁₀)alkyl, amino-substituted (C₁-C₁₀)alkyl, aryl or substituted aryl, M¹ is a Group IIIA metal, X is a halogen, and n is an integer from 1 to 3, in an organic solvent free of oxygen substitution.

2. A method for preparing a Group VA metal dihalide compound comprising the step of reacting a Group VA metal trihalide with a reagent selected from the group consisting of an organo lithium compound and a compound of the formula R_nM¹X₃₋

n wherein each R is (C₁-C₁₀) alkyl, amino-substituted (C₁-C₁₀)alkyl, aryl or substituted aryl, M¹ is a Group IIIA metal, X is a halogen and n is an integer from 1 to 3, in the presence of a tertiary amine in an organic solvent free of oxygen substitution.

4. The method of claim 2 or 3 wherein the tertiary amine has the formula NR⁴R⁵R⁶, wherein R⁴, R⁵ and R⁶ are independently selected from (C₁-C₆)alkyl, di (C₁-C₆) alkylamino-substituted-(C₁-C₆)alkyl and phenyl, and wherein R⁴ and R⁵ may be taken together along with the nitrogen to which they are attached to form a 5-7 membered heterocyclic ring.

3. A method for preparing Group VA metal dihydride compounds comprising the step of reducing a Group VA metal dihalide in the presence of a tertiary amine in an organic solvent wherein the organic solvent is free of oxygen substitution.

5. The method of claim 3 wherein the Group VA metal dihydride compounds have the formula RMH₂ or H₂MR¹ MH₂, wherein R is (C₁-C₁₀)alkyl, amino-substituted (C₁-C₁₀)alkyl, aryl or substituted aryl;

R¹ is (C₁-C₁₀)alkylene, (C₈-C₂₀)aralkylene or (C₆-C₂₀)arylene; and

M is arsenic or phosphorous.

6. The method of claim 3 wherein the Group VA metal dihydride compounds are substantially free of ethereal solvents.

7. A method for manufacturing an electronic device comprising the step of depositing a film of a Group VA metal on an electronic device substrate comprising the steps of:

a) conveying a Group VA metal dihydride compound or a Group VA metal dihalide compound in the gaseous phase to a deposition chamber containing the substrate;

b) decomposing the Group VA metal dihydride compound or a Group VA metal dihalide compound in the deposition chamber; and

c) depositing a film of Group VA metal on the substrate;

wherein the Group VA metal dihydride compound is prepared by the method of claim 3.

8. A method for depositing a film of a Group VA metal on a substrate comprising the steps of:

a) conveying a Group VA metal dihalide compound or a Group VA dihydride compound in the gaseous phase to a deposition chamber containing the substrate;

b) decomposing the Group VA metal dihalide compound or the Group VA metal dihydride compound in the deposition chamber; and

c) depositing a film of Group VA metal on the substrate;

wherein the monoalkyl Group VA dihydride compound is prepared by the method of claim 3.

9. A method for depositing a film of a Group VA metal on a substrate comprising of the steps of:

a) conveying a Group VA metal dihydride compound of the formula RMH₂ or H₂MR¹ MH₂ in the gaseous phase to a deposition chamber containing the substrate;

b) decomposing the Group VA metal compound in the deposition chamber; and

c) depositing a film of the Group VA metal on the substrate;

wherein the Group VA metal compound is substantially free of ethereal solvents; and

wherein R is (C₁-C₁₀)alkyl, amino-substituted (C₁-C₁₀)alkyl, aryl or substituted aryl;

R¹ is (C₁-C₁₀)alkylene, (C₈-C₂₀)aralkylene or (C₆-C₂₀)arylene; and

M is arsenic or phosphorus.