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.
| Original language | English (US) |
|---|---|
| Pages (from-to) | 1681-1691 |
| Number of pages | 11 |
| Journal | Zeitschrift fur Anorganische und Allgemeine Chemie |
| Volume | 643 |
| Issue number | 21 |
| DOIs | |
| State | Published - Nov 17 2017 |
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All Science Journal Classification (ASJC) codes
- Inorganic Chemistry
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Synthesis of Nanocrystalline Gd2O2NCN from a Versatile Single-source Precursor. / Ionescu, Emanuel; Li, Wenjie; Wiehl, Leonore; Mera, Gabriela; Riedel, Ralf.
In: Zeitschrift fur Anorganische und Allgemeine Chemie, Vol. 643, No. 21, 17.11.2017, p. 1681-1691.Research output: Contribution to journal › Article
TY - JOUR
T1 - Synthesis of Nanocrystalline Gd2O2NCN from a Versatile Single-source Precursor
AU - Ionescu, Emanuel
AU - Li, Wenjie
AU - Wiehl, Leonore
AU - Mera, Gabriela
AU - Riedel, Ralf
PY - 2017/11/17
Y1 - 2017/11/17
N2 - 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.
AB - 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.
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U2 - 10.1002/zaac.201700266
DO - 10.1002/zaac.201700266
M3 - Article
AN - SCOPUS:85034968987
VL - 643
SP - 1681
EP - 1691
JO - Zeitschrift fur Anorganische und Allgemeine Chemie
JF - Zeitschrift fur Anorganische und Allgemeine Chemie
SN - 0044-2313
IS - 21
ER -