Exploring Volatile Precursors: Synthesis, Characterization and Thermal Properties of Thulium Fluoroacetylacetonate Complexes

Five trifluoroacetylacetonate (<i>tfaa</i><sup>−</sup>) complexes [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)]<sub>2</sub>, [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>...

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Main Authors: Daniel Fuhrmann, Kristin Kaden, Marika Kandler, Maik Icker, Harald Krautscheid
Format: Article
Language:English
Published: MDPI AG 2023-10-01
Series:Crystals
Subjects:
Online Access:https://www.mdpi.com/2073-4352/13/10/1467
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author Daniel Fuhrmann
Kristin Kaden
Marika Kandler
Maik Icker
Harald Krautscheid
author_facet Daniel Fuhrmann
Kristin Kaden
Marika Kandler
Maik Icker
Harald Krautscheid
author_sort Daniel Fuhrmann
collection DOAJ
description Five trifluoroacetylacetonate (<i>tfaa</i><sup>−</sup>) complexes [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)]<sub>2</sub>, [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>], [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>] · <i>diglyme</i>, [Tm(<i>tfaa</i>)<sub>3</sub>(DME)] (DME = 1,2-dimethoxyethane) and [TmCl<sub>2</sub>(<i>tfaa</i>)(<i>diglyme</i>)] (<i>diglyme</i> = bis(2-methoxyethyl) ether) of thulium have been synthesized and characterized by X-ray single-crystal structure analysis and spectroscopic techniques. Thermoanalytical studies at elevated temperatures provide information about their volatility. The results are compared with the hexafluoroacetylacetonate (<i>hfaa</i><sup>−</sup>) complexes of thulium known in the literature, which were reported as volatile precursors for CVD application. The reported high volatility of [Tm(<i>hfaa</i>)<sub>3</sub>(DME)] was confirmed and compared with those of the aqueous complexes which show a lower transport rate. In addition, the new crystal structures of the hexafluoroacetylacetonate complexes [Tm(<i>hfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>], [Tm(<i>hfaa</i>)<sub>2</sub>(<i>tfa</i>)(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub> (<i>tfa</i><sup>−</sup> = trifluoroacetate), [Tm(<i>hfaa</i>)<sub>3</sub>(DME)NaCl]<sub>2</sub> and Na[Tm(<i>hfaa</i>)<sub>4</sub>] are presented.
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spelling doaj.art-1285cfcb0b464394b26dbfd50e7589d62023-11-19T16:09:38ZengMDPI AGCrystals2073-43522023-10-011310146710.3390/cryst13101467Exploring Volatile Precursors: Synthesis, Characterization and Thermal Properties of Thulium Fluoroacetylacetonate ComplexesDaniel Fuhrmann0Kristin Kaden1Marika Kandler2Maik Icker3Harald Krautscheid4Fakultät für Chemie und Mineralogie, Universität Leipzig, Johannisallee 29, D-04103 Leipzig, GermanyFakultät für Chemie und Mineralogie, Universität Leipzig, Johannisallee 29, D-04103 Leipzig, GermanyFakultät für Chemie und Mineralogie, Universität Leipzig, Johannisallee 29, D-04103 Leipzig, GermanyFakultät für Chemie und Mineralogie, Universität Leipzig, Johannisallee 29, D-04103 Leipzig, GermanyFakultät für Chemie und Mineralogie, Universität Leipzig, Johannisallee 29, D-04103 Leipzig, GermanyFive trifluoroacetylacetonate (<i>tfaa</i><sup>−</sup>) complexes [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)]<sub>2</sub>, [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>], [Tm(<i>tfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>] · <i>diglyme</i>, [Tm(<i>tfaa</i>)<sub>3</sub>(DME)] (DME = 1,2-dimethoxyethane) and [TmCl<sub>2</sub>(<i>tfaa</i>)(<i>diglyme</i>)] (<i>diglyme</i> = bis(2-methoxyethyl) ether) of thulium have been synthesized and characterized by X-ray single-crystal structure analysis and spectroscopic techniques. Thermoanalytical studies at elevated temperatures provide information about their volatility. The results are compared with the hexafluoroacetylacetonate (<i>hfaa</i><sup>−</sup>) complexes of thulium known in the literature, which were reported as volatile precursors for CVD application. The reported high volatility of [Tm(<i>hfaa</i>)<sub>3</sub>(DME)] was confirmed and compared with those of the aqueous complexes which show a lower transport rate. In addition, the new crystal structures of the hexafluoroacetylacetonate complexes [Tm(<i>hfaa</i>)<sub>3</sub>(H<sub>2</sub>O)<sub>2</sub>], [Tm(<i>hfaa</i>)<sub>2</sub>(<i>tfa</i>)(H<sub>2</sub>O)<sub>2</sub>]<sub>2</sub> (<i>tfa</i><sup>−</sup> = trifluoroacetate), [Tm(<i>hfaa</i>)<sub>3</sub>(DME)NaCl]<sub>2</sub> and Na[Tm(<i>hfaa</i>)<sub>4</sub>] are presented.https://www.mdpi.com/2073-4352/13/10/1467thuliumβ-diketonatesCVD precursorcrystal structuresthermal behavior
spellingShingle Daniel Fuhrmann
Kristin Kaden
Marika Kandler
Maik Icker
Harald Krautscheid
Exploring Volatile Precursors: Synthesis, Characterization and Thermal Properties of Thulium Fluoroacetylacetonate Complexes
Crystals
thulium
β-diketonates
CVD precursor
crystal structures
thermal behavior
title Exploring Volatile Precursors: Synthesis, Characterization and Thermal Properties of Thulium Fluoroacetylacetonate Complexes
title_full Exploring Volatile Precursors: Synthesis, Characterization and Thermal Properties of Thulium Fluoroacetylacetonate Complexes
title_fullStr Exploring Volatile Precursors: Synthesis, Characterization and Thermal Properties of Thulium Fluoroacetylacetonate Complexes
title_full_unstemmed Exploring Volatile Precursors: Synthesis, Characterization and Thermal Properties of Thulium Fluoroacetylacetonate Complexes
title_short Exploring Volatile Precursors: Synthesis, Characterization and Thermal Properties of Thulium Fluoroacetylacetonate Complexes
title_sort exploring volatile precursors synthesis characterization and thermal properties of thulium fluoroacetylacetonate complexes
topic thulium
β-diketonates
CVD precursor
crystal structures
thermal behavior
url https://www.mdpi.com/2073-4352/13/10/1467
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AT marikakandler exploringvolatileprecursorssynthesischaracterizationandthermalpropertiesofthuliumfluoroacetylacetonatecomplexes
AT maikicker exploringvolatileprecursorssynthesischaracterizationandthermalpropertiesofthuliumfluoroacetylacetonatecomplexes
AT haraldkrautscheid exploringvolatileprecursorssynthesischaracterizationandthermalpropertiesofthuliumfluoroacetylacetonatecomplexes