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Synthesis of Nanocrystalline Gd2O2NCN from a Versatile Single-source Precursor

Ionescu, Emanuel ; Li, Wenjie ; Wiehl, Leonore ; Mera, Gabriela ; Riedel, Ralf (2017)
Synthesis of Nanocrystalline Gd2O2NCN from a Versatile Single-source Precursor.
In: Zeitschrift für anorganische und allgemeine Chemie, 643 (21)
doi: 10.1002/zaac.201700266
Artikel, Bibliographie

Kurzbeschreibung (Abstract)

Nanocrystalline Gd2O2NCN (P3m1, crystallite size 30–40 nm) was synthesized upon ammonolysis of bis[[(N-carboxymethyl,N-carboxy-κO-methyl)amino-κN]-ethyl]-glycinato(3-)-κN,κO]gadolinium(III) (diethylenetriamine pentaacetic acid gadolinium(III) dihydrogen salt or gadopentetic acid, Gd-H2DTPA hereafter) at 900 °C. The conversion of Gd-H2DTPA into Gd2O2NCN takes place in several steps, probably via transient formation of iminodiacetate-, glycinate-, and carbamate-containing complexes of Gd. Thermal treatment in air of Gd-H2DTPA at 750 and 1300 °C delivers nanocrystalline bixbyite-type Gd2O3 (Ia3, crystallite size 30–70 nm); in an argon or nitrogen atmosphere the formation of monoclinic Gd2O3 (C2/m) was observed at 1300 °C. The synthesized Gd2O2NCN converts upon thermal treatment in air, nitrogen, or argon atmosphere into monoclinic Gd2O3 (C2/m). In ammonia atmosphere, Gd2O2NCN seems to be stable against decomposition, even upon prolonged exposure to 1000 °C. This study indicates that Gd-H2DTPA may be a robust, low-cost, and flexible precursor for nanoscaled Gd-based nanopowders. Moreover, precursor approaches based on metal complexes using H5DTPA as a ligand are suggested as promising access pathways towards nanocrystalline materials in the M/O/C/N system.

Typ des Eintrags: Artikel
Erschienen: 2017
Autor(en): Ionescu, Emanuel ; Li, Wenjie ; Wiehl, Leonore ; Mera, Gabriela ; Riedel, Ralf
Art des Eintrags: Bibliographie
Titel: Synthesis of Nanocrystalline Gd2O2NCN from a Versatile Single-source Precursor
Sprache: Englisch
Publikationsjahr: 3 November 2017
Verlag: WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Titel der Zeitschrift, Zeitung oder Schriftenreihe: Zeitschrift für anorganische und allgemeine Chemie
Jahrgang/Volume einer Zeitschrift: 643
(Heft-)Nummer: 21
DOI: 10.1002/zaac.201700266
URL / URN: https://doi.org/10.1002/zaac.201700266
Kurzbeschreibung (Abstract):

Nanocrystalline Gd2O2NCN (P3m1, crystallite size 30–40 nm) was synthesized upon ammonolysis of bis[[(N-carboxymethyl,N-carboxy-κO-methyl)amino-κN]-ethyl]-glycinato(3-)-κN,κO]gadolinium(III) (diethylenetriamine pentaacetic acid gadolinium(III) dihydrogen salt or gadopentetic acid, Gd-H2DTPA hereafter) at 900 °C. The conversion of Gd-H2DTPA into Gd2O2NCN takes place in several steps, probably via transient formation of iminodiacetate-, glycinate-, and carbamate-containing complexes of Gd. Thermal treatment in air of Gd-H2DTPA at 750 and 1300 °C delivers nanocrystalline bixbyite-type Gd2O3 (Ia3, crystallite size 30–70 nm); in an argon or nitrogen atmosphere the formation of monoclinic Gd2O3 (C2/m) was observed at 1300 °C. The synthesized Gd2O2NCN converts upon thermal treatment in air, nitrogen, or argon atmosphere into monoclinic Gd2O3 (C2/m). In ammonia atmosphere, Gd2O2NCN seems to be stable against decomposition, even upon prolonged exposure to 1000 °C. This study indicates that Gd-H2DTPA may be a robust, low-cost, and flexible precursor for nanoscaled Gd-based nanopowders. Moreover, precursor approaches based on metal complexes using H5DTPA as a ligand are suggested as promising access pathways towards nanocrystalline materials in the M/O/C/N system.

Zusätzliche Informationen:

Special Issue: Dedicated to Professor Wolfgang Schnick on the Occasion of his 60th Birthday

Fachbereich(e)/-gebiet(e): 11 Fachbereich Material- und Geowissenschaften
11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft
11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft > Fachgebiet Disperse Feststoffe
Hinterlegungsdatum: 11 Dez 2017 12:26
Letzte Änderung: 30 Jul 2018 05:44
PPN:
Sponsoren: Funded by FP7 People: Marie-Curie Actions. Grant Number: FP7-PITN-GA-2010-264873 (FUNEA), Funded by European Union COST Action. Grant Number: CM 1302 Smart Inorganic Polymers, Funded by Technische Universität Darmstadt. Grant Number: Re-entry Fellowship
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