Lithium-niobium hexakis(alkoxides)
LiNb(OR)6 , Li(Ta(OR)6 for Li(Nb,Ta)O3 MOCVD
Lithium-niobium hexakis(ethoxide) LiNb(OEt)6 (M = 370.21) is white crystalline solid, characterized by IR, 1H NMR, MS, DTA, termochemically, by conductivity measurements, single crystal XRD. [[i], [ii]]
[i] N.Y. Turova, E.P. Turevskaya, V.G. Kessler, M.I. Yanovskaya,
[ii] D.J. Eichorst, D.A. Payne, S.R. Wilson, K.E. Howard, Inorg. Chem., 1990, 29, 1458.
Single-Source Precursor Lithium-niobium hexakis(ethoxide) LiNb(OEt)6 was applied for the growth of LiNbO3 films by spray MOCVD process. However, this method was reported to
produce a film which is polycrystaline and black, therefore unsuitable for optical applications [[i] ]
[i] A.A. Wernberg, H.J. Gysling, Chem. Mater., 1993, 5 (8), pp 1056–1058 « MOCVD deposition of epitaxial lithium niobate, LiNbO3, thin films using the single source precursor lithium niobium ethoxide, LiNb(OEt)6 »
New heterometallic alkoxides lithium-niobium hexakis(neopentoxide) [LiNb(OCH2CMe3)6]2 and lithium-niobium hexakis(trimethylsilylmethoxide) [LiNb(OCH2SiMe3)6]2 were prepared from the corresponding homometallic alkoxides. The complexes are moderately soluble in hydrocarbons and sublime in moderate to good recoveries. The structure of [LiNb(OCH2SiMe3)6]2 contains an Nb2Li2(μ-O)4(μ3-O)2 central-core geometry, as determined by single-crystal XRD. Complex [LiNb(OCH2CMe3)6]2 is isostructural to [LiNb(OCH2SiMe3)6]2 , according to 1H NMR data. Bulk pyrolysis of [LiNb(OCH2CMe3)6]2 gives crystalline LiNbO3 under N2 at 600°C.
[LiNb(OCH2CMe3)6]2 was tested as precursor for the growth of lithium niobate thin films by spray MOCVD, however, LiNbO3 films
were not obtained under conditions that give LiNbO3 films from [LiNb(OEt)6]∞.[[i]]
[i] S. C. Goel, J. A. Hollingsworth, A. M. Beatty, K. D. Robinson, William E. Buhro, Polyhedron, 1998, vol.17, Iss.5-6, p.781-790 Preparation of volatile molecular lithium-niobium alkoxides. Crystal structures of [Nb(μ-OCH2SiMe3)(OCH2SiMe3)4]2 and [LiNb(μ3-OCH2SiMe3)-(μ2-OCH2SiMe3)2(OCH2SiMe3]2