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Synthesis and Structural Characterization of β‐Ketoiminate‐Stabilized Gallium Hydrides for Chemical Vapor Deposition Applications
Author(s) -
Marchand Peter,
Pugh David,
Parkin Ivan P.,
Carmalt Claire J.
Publication year - 2014
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201402998
Subject(s) - gallium , hydride , chemical vapor deposition , stoichiometry , thermogravimetric analysis , bimetallic strip , chemistry , amorphous solid , thermal stability , crystallography , x ray photoelectron spectroscopy , thin film , analytical chemistry (journal) , inorganic chemistry , materials science , hydrogen , metal , organic chemistry , nanotechnology , chemical engineering , engineering
Bis‐β‐ketoimine ligands of the form [(CH 2 ) n {N(H)C(Me)CHC(Me)O} 2 ] (L n H 2 , n =2, 3 and 4) were employed in the formation of a range of gallium complexes [Ga(L n )X] (X=Cl, Me, H), which were characterised by NMR spectroscopy, mass spectrometry and single‐crystal X‐ray diffraction analysis. The β‐ketoimine ligands have also been used for the stabilisation of rare gallium hydride species [Ga(L n )H] ( n =2 ( 7 ); n =3 ( 8 )), which have been structurally characterised for the first time, confirming the formation of five‐coordinate, monomeric species. The stability of these hydrides has been probed through thermal analysis, revealing stability at temperatures in excess of 200 °C. The efficacy of all the gallium β‐ketoiminate complexes as molecular precursors for the deposition of gallium oxide thin films by chemical vapour deposition (CVD) has been investigated through thermogravimetric analysis and deposition studies, with the best results being found for a bimetallic gallium methyl complex [L 3 {GaMe 2 } 2 ] ( 5 ) and the hydride [Ga(L 3 )H] ( 8 ). The resulting films ( F5 and F8 , respectively) were amorphous as‐deposited and thus were characterised primarily by XPS, EDXA and SEM techniques, which showed the formation of stoichiometric ( F5 ) and oxygen‐deficient ( F8 ) Ga 2 O 3 thin films.