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Issue 83, 2017, Issue in Progress
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Monitoring the mechanism of formation of [Ce(1,10-phenanthroline)2(NO3)3] by in situ luminescence analysis of 5d–4f electronic transitions

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Abstract

This work introduces the application of the in situ luminescence analysis of coordination sensors (ILACS) technique for monitoring the emission of Ce3+ 5d–4f electronic transitions under real reaction conditions during the formation of [Ce(phen)2(NO3)3] (phen = 1,10-phenanthroline). The mechanism of formation indicated by the ILACS data was confirmed by several additional methods, including ex situ and synchrotron-based in situ X-ray diffraction (XRD) analysis, in situ light transmission, and in situ infrared (IR) spectroscopy, among others. Initially, the in situ luminescence measurements presented a broad emission band at 415–700 nm, which was assigned to the Ce3+ ions in ethanolic solution. Upon the addition of the phen solution to the reactor, a gradual shift of the emission band to lower energies (500–900 nm) was observed. This occurs due to the changes in the Ce3+ coordination environment during its incorporation into the solid [Ce(phen)2(NO3)3] complex. In situ IR measurements during the crystallization of [Ce(phen)2(NO3)3] confirmed the kinetics of the crystallization process by detecting changes in the phen and nitrate vibrations at e.g. 842 and 1301 cm−1, respectively. Simultaneous in situ XRD measurements confirmed the induction time of approximately 3 minutes after the addition of the phen solution, previously detected by the in situ luminescence measurements, coinciding with the onset of the [Ce(phen)2(NO3)3] Bragg reflections. In situ monitoring of events occurring during the formation of solid materials is a crucially important step for developing rational synthesis approaches and for tailoring structure-related properties, such as luminescence.

Graphical abstract: Monitoring the mechanism of formation of [Ce(1,10-phenanthroline)2(NO3)3] by in situ luminescence analysis of 5d–4f electronic transitions

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Supplementary files

Article information


Submitted
07 Jul 2017
Accepted
07 Nov 2017
First published
15 Nov 2017

This article is Open Access

RSC Adv., 2017,7, 52794-52800
Article type
Paper

Monitoring the mechanism of formation of [Ce(1,10-phenanthroline)2(NO3)3] by in situ luminescence analysis of 5d–4f electronic transitions

L. R. Arana, P. Lindenberg, H. Said, M. Radke, N. Heidenreich, C. S. Cunha, S. Leubner and H. Terraschke, RSC Adv., 2017, 7, 52794
DOI: 10.1039/C7RA07488C

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