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Layered α-TiCl₃: Microsheets on YSZ Substrates for Ethylene Polymerization with Enhanced Activity

  • The transition metal halide α-titanium(III) chloride (α-TiCl₃) is a layered two-dimensional compound and a well-established Ziegler–Natta catalyst for the polymerization of ethylene. A new synthesis technique is used to obtain thin sheets of α-TiCl₃ that show exceptional physical properties in contrast to their bulk counterparts, due to an enlarged surface-to-volume ratio. Chemical vapor transport (CVT) of α-titanium(III) chloride directly on substrates results in microsheets that exhibit an improved catalytic effect. For rational planning of synthesis conditions, thermodynamic simulations of occurring gas-phase equilibria were performed. Based on these calculation results, crystal growth was achieved by adding GaCl₃via pure short term CVT in a temperature gradient of 700–600 K on yttrium-stabilized zirconia (YSZ) substrates. Phase pure, as-grown, single crystal sheets with high crystallinity and a thickness of around 4 μm were obtained. These thin sheets of α-TiCl₃ on YSZ substrates were implemented as catalysts for the ethyleneThe transition metal halide α-titanium(III) chloride (α-TiCl₃) is a layered two-dimensional compound and a well-established Ziegler–Natta catalyst for the polymerization of ethylene. A new synthesis technique is used to obtain thin sheets of α-TiCl₃ that show exceptional physical properties in contrast to their bulk counterparts, due to an enlarged surface-to-volume ratio. Chemical vapor transport (CVT) of α-titanium(III) chloride directly on substrates results in microsheets that exhibit an improved catalytic effect. For rational planning of synthesis conditions, thermodynamic simulations of occurring gas-phase equilibria were performed. Based on these calculation results, crystal growth was achieved by adding GaCl₃via pure short term CVT in a temperature gradient of 700–600 K on yttrium-stabilized zirconia (YSZ) substrates. Phase pure, as-grown, single crystal sheets with high crystallinity and a thickness of around 4 μm were obtained. These thin sheets of α-TiCl₃ on YSZ substrates were implemented as catalysts for the ethylene polymerization reaction. A significant improvement of catalytic activity of 16% was achieved, probably due to an increased surface-to-volume ratio. As a highlight, the as-grown microsheets were exfoliated subsequently to a thickness lower than 200 nm and an even higher catalytic activity of up to 24% was confirmed experimentally due to delamination effects. This is the first time that an improved catalytic effect of α-TiCl₃ is observed as a result of downscaling from bulk to microsheets by CVT.show moreshow less

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Metadaten
Author: Martin GrönkeORCiD, Ubed S. F. Arrozi, Nadine Bronkalla, Peer SchmidtORCiD, Martin ValldorORCiD, Steffen Oswald, Thomas G. Woodcock, Victoria Eckert, Qi HaoORCiD, Laura Plüschke, Albena LedererORCiD, Kornelius Nielsch, Bernd BüchnerORCiD, Stefan KaskelORCiD, Silke HampelORCiD
URL:https://pubs.acs.org/doi/10.1021/acs.chemmater.9b01818
DOI:https://doi.org/10.1021/acs.chemmater.9b01818
Title of the source (English):Chemistry of Materials
Document Type:Scientific journal article peer-reviewed
Language:English
Year of publication:2019
Tag:2D layered compounds; Chemical vapor transport; Crystal growth; Halides; Nanocrystals (1); Thermodynamic modeling
Volume/Year:31
Issue number:14
First Page:5305
Last Page:5313
Faculty/Chair:Fakultät 2 Umwelt und Naturwissenschaften / FG Anorganische Chemie
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