Organometallic compound purification
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A method of purifying an organometallic compound by heating the organometallic compound in the presence of a trialkyl aluminum compound and a catalyst.
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1. A method of purifying an organometallic compound comprising i) providing a mixture comprising a) an organometallic compound chosen from unsymmetrical dimethyl hydrazine and a compound of the formula R.sup.1R.sup.2.sub.n-1M.sup.1 wherein R.sup.1 is chosen from (C.sub.1-C.sub.20)alkyl, (C.sub.2-C.sub.12)dialkylamino, (C.sub.1-C.sub.12)alkylamino(C.sub.1-C.sub.12)alkyl, di(C.sub.1-C.sub.20)alkylamino(C.sub.1-C.sub.12)alkyl, (C.sub.2-C.sub.20)alkenyl, (C.sub.2-C.sub.20)alkynyl and aryl; each R.sup.2 is independently chosen from hydrogen, (C.sub.1-C.sub.20)alkyl, (C.sub.2-C.sub.12)dialkylamino, (C.sub.1-C.sub.12)alkylamino(C.sub.1-C.sub.12)alkyl, di(C.sub.1-C.sub.20)alkylamino(C.sub.1-C.sub.12)alkyl, (C.sub.2-C.sub.20)alkenyl, (C.sub.2-C.sub.20)alkynyl, aryl and halogen; M.sup.1 is a Group IIA to Group VIA metal; and n is the valence of M.sup.1; and b) a purifying composition comprising an alkyl-metal compound of the formula R.sup.3.sub.xR.sup.4.sub.3-xM.sup.2 wherein R.sup.3 is a (C.sub.1-C.sub.20)alkyl; each R.sup.4 is independent chosen from hydrogen and halogen; M.sup.2 is a Group IIIA metal; and x is an integer from 1-3; and a catalyst compound; and ii) heating the mixture.
3. The method of claim 2 wherein the catalyst compound further comprises a group chosen from hydrogen, halogen, alkyl, alkenyl, alkynyl, aryl, amino, dialkylamino, aminoalkyl, and dialkylaminoalkyl.
4. The method of claim 1 wherein the catalyst compound is chosen from lithium dimethylamide, tert-butyl lithium, n-butyl lithium, aluminum trichloride, aluminum tribromide, aluminum triiodide, gallium trichloride, indium trichloride, calcium dichloride, barium difluoride, tetramethyl ammonium fluoride, and tris(dimethylamino) aluminum.
5. The method of claim 1 wherein the purifying composition is present in an amount of 0.1 to 10 % wt based on the weight of the organometallic compound.
6. The method of claim 1 wherein the alkyl-metal compound and catalyst compound are present in a weight ratio of 10:1 to 1:10.
8. The method of claim 1 wherein M.sup.1 is chosen from a Group IIIA metal, a Group IVA metal and a Group VA metal.
10. The method of claim 1 further comprising a step of removing the organometallic compound form the purifying composition.
Comments from the community
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#1|IP ENTHUSIAST comments:
Very interesting patent because the high purity of precursors is extremely important for semiconductor performance. This patent provides a novel approach to remove impurities which is very difficult because of highly reactive and pyrophoric nature of precursors. Excellent work by inventors.