Group VI precursor compounds
The invention provides a facile process for preparing various Group VI precursor compounds useful in the vapor deposition of such Group VI metals onto solid substrates, especially microelectronic semiconductor device substrates. The process provides an effective means to obtain such volatile materials, which can then be sources of molybdenum, chromium, or tungsten-containing materials to be deposited on such substrates. Additionally, the invention provides a method for vapor deposition of such compounds onto microelectronic device substrates.
1. A process for preparing compounds of the Formula (I)
wherein M is chosen from tungsten and chromium, X is chosen from fluoro, chloro, bromo, and iodo, and each L 1 and L 2 are the same or different and constitute:
(i) a monodentate hydrocarbyl ligand coordinated with M, or
(ii) are taken together to form a bidentate hydrocarbyl ligand coordinated with M;
which comprises:
(A) contacting a compound of the formula
with (a) water containing about 0.1% (w/w) to about 48% (w/w) of a compound of the formula HX, and (b) a compound of the formula L 1 and/or L 2 ; followed by
(B) extraction of the compound of Formula(I) with a non-coordinating, water immiscible solvent, and isolation of the compound of Formula (I) as a solid or liquid.
2. The process of claim 1 , wherein X is fluoro.
3. The process of claim 1 , wherein X is chloro.
4. The process of claim 1 , wherein X is bromo.
5. The process of claim 1 , wherein X is iodo.
6. The process of claim 1 , wherein L 1 and L 2 are dimethoxyethane.
7. The process of claim 1 , wherein the non-coordinating, water-immiscible solvent is dichloromethane, ethyl acetate, diethyl ether, toluene, benzene, or pentane.
8. The process of claim 6 , wherein the non-coordinating, water-immiscible solvent is dichloromethane.
9. The process of claim 1 , wherein M is tungsten.
10. The process of claim 1 , wherein M is chromium.