Synthesis of Silyl Aluminum Reagents: Relevance Toward Atomic Layer Deposition of Metal Silicides and the Serendipitous Synthesis of a Novel Al-Hydride Cluster.

Autor: Bashkurov R; Schulich Faculty of Chemistry, Technion-Israel Institute of Technology, Haifa 32000, Israel., Kratish Y; Schulich Faculty of Chemistry, Technion-Israel Institute of Technology, Haifa 32000, Israel., Mokhtarzadeh CC; Intel Corporation, 2501 NE Century Boulevard, Hillsboro, Oregon 97124, United States., Fridman N; Schulich Faculty of Chemistry, Technion-Israel Institute of Technology, Haifa 32000, Israel., Bravo-Zhivotovskii D; Schulich Faculty of Chemistry, Technion-Israel Institute of Technology, Haifa 32000, Israel., Romero PE; Intel Corporation, 2501 NE Century Boulevard, Hillsboro, Oregon 97124, United States.; Pontificia Universidad Católica de Chile, Escula de Ingenieria, Vicuna Mackenna 4860, Macul, Santiago, Chile., Clendenning SB; Intel Corporation, 2501 NE Century Boulevard, Hillsboro, Oregon 97124, United States., Apeloig Y; Schulich Faculty of Chemistry, Technion-Israel Institute of Technology, Haifa 32000, Israel.
Jazyk: angličtina
Zdroj: Inorganic chemistry [Inorg Chem] 2020 Dec 07; Vol. 59 (23), pp. 17488-17496. Date of Electronic Publication: 2020 Nov 24.
DOI: 10.1021/acs.inorgchem.0c02730
Abstrakt: The novel mono-silyl [(R 3 Si)AlX 2 ] 2 , di-silyl [(R 3 Si) 2 AlX] 2 , tri-silyl (R 3 Si) 3 Al·Et 2 O, and -ate-complex [(R 3 Si) 4 Al] - ·Li + (Et 2 O) 2 have been synthesized by reaction of AlX 3 (X = Cl, Br) with silyl lithium reagents ( t BuMe 2 SiLi, Et 3 SiLi) in Et 2 O. Treatment of these compounds with Me 3 N yields the corresponding amine-coordinated silyl aluminum complexes (R 3 Si)AlX 2 ·NMe 3 , (R 3 Si) 2 AlX·NMe 3 , and (R 3 Si) 3 Al·NMe 3 . An intramolecular amine-coordinated mono-silyl aluminum complex Me 2 N(CH 2 ) 3 ( t BuMe 2 Si) 2 SiAlCl 2 was prepared by the reaction of Me 2 N(CH 2 ) 3 ( t BuMe 2 Si) 2 SiLi with AlCl 3 in Et 2 O. In addition, reaction of [( t BuMe 2 Si) 2 AlBr] 2 with LiAlH 4 yields the novel aluminum hydride cluster [( t BuMe 2 Si) 2 Al(μ-H)AlH 3 ] 6 which upon addition of TMEDA yields the ion pair [(( t BuMe 2 Si) 2 AlH) 2 (μ-H)] - [AlH 2 (TMEDA) 2 ] + . The amine-coordinated di- and tri-silyl aluminum complexes possess higher thermal stability than the analogous etherate complexes and are reasonably volatile (100-140 °C, 0.2 Torr). The materials presented herein were analyzed via thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC) to assess their viability as potential ALD precursors.
Databáze: MEDLINE