Synthesis and thermal behavior of [Li（thf）3（μ-Cl）La{N（SiMe3）2}3] and its investigation as spin-coating precursor for lanthanum-based layer formation
来源期刊：Journal of Rare Earths2018年第5期
论文作者：Andrea Preuβ Elaheh Pousaneh Julian Noll Tobias Rüffer Alexaner Jakob Lutz Mertens Michael Mehring Heinrich Lang
文章页码：537 - 543
摘 要：The lanthanum（Ⅲ） complex [Li（thf）3（μ-CI）La{N（SiMe3）2}3]（3） was obtained by the reaction of LaCl3 with three equiv of Li[N（SiMe3）2]3 in a tetrahydrofuran solution. The molecular structure of 3 in the solid state was characterized by a tetracoordinated anionic lanthanide（Ⅲ） amide in form of an adduct with LiCl（thf）3 as evidenced by single crystal X-ray structure analysis. In order to study the suitability of 3 as a precursor for the deposition of La2O3/LiLaSiO4 by thin layer deposition techniques,its thermal behavior was investigated by thermogravimetry（TG） and TG-MS-coupled studies. TG studies show a two-step decomposition process, whereby volatile decomposition products can be detected during the second decomposition step. TG measurements under an atmosphere of oxygen produced La2O3, Calcination processes of 3 under ambient atmosphere for 10 h at 1000 ℃ gave La2O3 and LiLaSiO4,which was confirmed by PXRD studies. Metal-organic 3 was applied as spin-coating precursor for La2O3 thin film formation giving the as-deposited layers nearly crack-free.
Andrea Preuβ1，Elaheh Pousaneh1，Julian Noll1，Tobias Rüffer1，Alexaner Jakob1，Lutz Mertens2，Michael Mehring2，Heinrich Lang1
1. Technische Universitt Chemnitz, Faculty of Natural Sciences, Institute of Chemistry,Inorganic Chemistry2. Technische Universitt Chemnitz, Faculty of Natural Sciences, Institute of Chemistry,Coordination Chemistry
摘 要：The lanthanum（Ⅲ） complex [Li（thf）3（μ-CI）La{N（SiMe3）2}3]（3） was obtained by the reaction of LaCl3 with three equiv of Li[N（SiMe3）2]3 in a tetrahydrofuran solution. The molecular structure of 3 in the solid state was characterized by a tetracoordinated anionic lanthanide（Ⅲ） amide in form of an adduct with LiCl（thf）3 as evidenced by single crystal X-ray structure analysis. In order to study the suitability of 3 as a precursor for the deposition of La2O3/LiLaSiO4 by thin layer deposition techniques,its thermal behavior was investigated by thermogravimetry（TG） and TG-MS-coupled studies. TG studies show a two-step decomposition process, whereby volatile decomposition products can be detected during the second decomposition step. TG measurements under an atmosphere of oxygen produced La2O3, Calcination processes of 3 under ambient atmosphere for 10 h at 1000 ℃ gave La2O3 and LiLaSiO4,which was confirmed by PXRD studies. Metal-organic 3 was applied as spin-coating precursor for La2O3 thin film formation giving the as-deposited layers nearly crack-free.
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