NDLI: $Ga[OSi(O^{t}Bu)_{3}]_{3}·THF,$ a thermolytic molecular precursor for high surface area gallium-containing silica materials of controlled dispersion and stoichiometry

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Johnson, Gregory R. Dombrowski, James P. Bell, Alexis T. Tilley, T. Don
Description	Author Affiliation: Dombrowski JP ( Department of Chemistry, University of California, Berkeley, Berkeley, California 94720-1460, USA. tdtilley@berkeley.edu and Chemical Sciences Division, Lawrence Berkeley Laboratory, 1 Cyclotron Road, Berkeley, California 94720, USA.); Johnson GR ( Department of Chemical and Biomolecular Engineering, University of California, Berkeley, Berkeley, California 94720-1460, USA.); Bell AT ( Department of Chemical and Biomolecular Engineering, University of California, Berkeley, Berkeley, California 94720-1460, USA and Chemical Sciences Division, Lawrence Berkeley Laboratory, 1 Cyclotron Road, Berkeley, California 94720, USA.); Tilley TD ( Department of Chemistry, University of California, Berkeley, Berkeley, California 94720-1460, USA. tdtilley@berkeley.edu and Chemical Sciences Division, Lawrence Berkeley Laboratory, 1 Cyclotron Road, Berkeley, California 94720, USA.)
Abstract	The molecular precursor tris[(tri-tert-butoxy)siloxy]gallium, as the tetrahydrofuran adduct $Ga[OSi(O^{t}Bu)_{3}]_{3}·THF$ (1), was synthesized via the salt metathesis reaction of gallium trichloride with $NaOSi(O^{t}Bu)_{3}.$ This complex serves as a model for isolated gallium in a silica framework. Complex 1 decomposes thermally in hydrocarbon solvent, eliminating isobutylene, water, and tert-butanol to generate high surface area gallium-containing silica at low temperatures. When thermal decomposition was performed in the presence of P-123 Pluronic as a templating agent the generated material displayed uniform vermicular pores. Textural mesoporosity was evident in untemplated material. Co-thermolysis of 1 with $HOSi(O^{t}Bu)_{3}$ in the presence of P-123 Pluronic led to materials with Ga:Si ratios ranging from 1:3 to 1:50, denoted $UCB1-GaSi_{3},$ $UCB1-GaSi_{10},$ $UCB1-GaSi_{20}$ and $UCB1-GaSi_{50}.$ After calcination at 500 °C these materials exhibited decreasing surface areas and broadening pore distributions with increasing silicon content, indicating a loss of template effects. The position and dispersion of the gallium in UCB1-GaSi materials was investigated using $^{71}Ga$ MAS-NMR, powder XRD, and STEM/EDS elemental mapping. The results indicate a high degree of gallium dispersion in all samples, with gallium oxide clusters or oligomers present at higher gallium content.
ISSN	14779226
Issue Number	27
Journal	Dalton Trans.
Volume Number	45
e-ISSN	13645447
Language	English
Publisher	Royal Society of Chemistry
Publisher Date	2016-07-05
Publisher Place	Great Britain (UK)
Access Restriction	Subscribed
Subject Keyword	Chemistry
Content Type	Text
Resource Type	Article
Subject	Inorganic Chemistry

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