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Preparation of highly reactive metal powders: preparation, characterization, and chemistry of iron, cobalt, nickel, palladium, and platinum microparticles

Journal Article · · Organometallics; (United States)
DOI:https://doi.org/10.1021/om00075a004· OSTI ID:5949907

Anhydrous metal halides of iron cobalt, nickel, palladium, and platinum are readily reduced in glyme or tetra-hydro-furan (THF) with lithium in the presence of a small amount of naphthalene and yield finely divided, black metal powders of exceptional reactivity. Metal powders of Fe and Co react with C/sub 6/F/sub 5/X (X = Br, I) to yield solvated M(C/sub 6/F/sub 5/)/sub 2/ and MX/sub 2/. Powders of palladium and platinum react with C/sub 6/F/sub 5/I to yield solvated M(C/sub 6/F/sub 5/)I (M = Pd, Pt). Nickel powder reacts with C/sub 6/F/sub 5/I to yield the solvated species Ni(C/sub 6/F/sub 5/)/sub 2/ and NiI/sub 2/, however, with C/sub 6/F/sub 5/Br the product is solvated Ni(C/sub 6/F/sub 5/)Br. In most cases the metal powders are sufficiently reactive that a stoichiometric amount of C/sub 6/F/sub 5/X to the metal powder is used. The coordinated ether of all of these organometallic compounds is exceptionally labile and is displaced with a variety of ligands: phosphines, amines, sulfides, isocyanides, diolefins, and carbon monoxide. Many of the resultant compounds are novel and most are obtained in high yields. Palladium metal powder to which has been added 2,2'-bipyridine (bpy) reacts with iodobenzene to yield Pd(C/sub 6/H/sub 5/)I(bpy). Surface analyses including ESCA (electron spectroscopy) and BET were performed on the highly reactive Ni, Pt, and Pd metal powders. 32 references, 4 tables.

Research Organization:
Univ. of Nebraska, Lincoln
DOE Contract Number:
AC02-80ER10603
OSTI ID:
5949907
Journal Information:
Organometallics; (United States), Journal Name: Organometallics; (United States) Vol. 2:3; ISSN ORGND
Country of Publication:
United States
Language:
English