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Synthesis of Nanocrystalline Gd2O2NCN from a Versatile Single-source Precursor

Ionescu, Emanuel and Li, Wenjie and Wiehl, Leonore and Mera, Gabriela and Riedel, Ralf (2017):
Synthesis of Nanocrystalline Gd2O2NCN from a Versatile Single-source Precursor.
In: Zeitschrift für anorganische und allgemeine Chemie, WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim, pp. 1681-1691, 643, (21), ISSN 00442313,
DOI: 10.1002/zaac.201700266,
[Online-Edition: https://doi.org/10.1002/zaac.201700266],
[Article]

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.

Item Type: Article
Erschienen: 2017
Creators: Ionescu, Emanuel and Li, Wenjie and Wiehl, Leonore and Mera, Gabriela and Riedel, Ralf
Title: Synthesis of Nanocrystalline Gd2O2NCN from a Versatile Single-source Precursor
Language: English
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.

Journal or Publication Title: Zeitschrift für anorganische und allgemeine Chemie
Volume: 643
Number: 21
Publisher: WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Divisions: 11 Department of Materials and Earth Sciences
11 Department of Materials and Earth Sciences > Material Science
11 Department of Materials and Earth Sciences > Material Science > Dispersive Solids
Date Deposited: 11 Dec 2017 12:26
DOI: 10.1002/zaac.201700266
Official URL: https://doi.org/10.1002/zaac.201700266
Additional Information:

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

Funders: 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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