nanomaterials Article Ultrasound-Assisted Synthesis of Luminescent Micro- and Nanocrystalline Eu-Based MOFs as Luminescent Probes for Heavy Metal Ions Stefaniia S. Kolesnik 1 , Viktor G. Nosov 1 , Ilya E. Kolesnikov 1 , Evgenia M. Khairullina 1 , Ilya I. Tumkin 1 , Aleksandra A. Vidyakina 1 , Alevtina A. Sysoeva 2 , Mikhail N. Ryazantsev 1,3 , Maxim S. Panov 1 , Vasiliy D. Khripun 1 , Nikita A. Bogachev 1 , Mikhail Yu. Skripkin 1 and Andrey S. Mereshchenko 1,2, *   Citation: Kolesnik, S.S.; Nosov,V.G.; Kolesnikov, I.E.; Khairullina, E.M.; Tumkin, I.I.; Vidyakina, A.A.; Sysoeva, A.A.; Ryazantsev, M.N.; Panov, M.S.; Khripun, V.D.; et al. Ultrasound-Assisted Synthesis of Luminescent Micro- and Nanocrystalline Eu-Based MOFs as Luminescent Probes for Heavy Metal Ions. Nanomaterials 2021, 11, 2448. https://doi.org/10.3390/nano11092448 Academic Editors: Marcin Runowski and Guoping Dong Received: 26 July 2021 Accepted: 16 September 2021 Published: 20 September 2021 Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affil- iations. Copyright: © 2020 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). 1 Saint-Petersburg State University, 7/9 Universitetskaya emb., 199034 St. Petersburg, Russia; staphylinuscaesareus@gmail.com (S.S.K.); nosoff.vitia2018@yandex.ru (V.G.N.); ilya.kolesnikov@spbu.ru (I.E.K.); iskint@mail.ru (E.M.K.); i.i.tumkin@spbu.ru (I.I.T.); vidyakina.aleksandra@mail.ru (A.A.V.); mikhail.n.ryazantsev@gmail.com (M.N.R.); m.s.panov@spbu.ru (M.S.P.); v.khripun@spbu.ru (V.D.K.); allanfrack@yandex.ru (N.A.B.); skripkin1965@yandex.ru (M.Y.S.) 2 Sirius University of Science and Technology, 1 Olympic Ave, 354340 Sochi, Russia; sysoevaaa_04@mail.ru 3 Laboratory of Nanobiotechnology, Saint Petersburg Academic University, ul. Khlopina 8/3, 194021 St. Petersburg, Russia * Correspondence: a.mereshchenko@spbu.ru; Tel.: +7-951-677-5465 Abstract: The luminescent coarse-, micro- and nanocrystalline europium(III) terephthalate tetrahy- drate (Eu 2 bdc 3 ·4H 2 O) metal-organic frameworks were synthesized by the ultrasound-assisted wet- chemical method. Electron micrographs show that the europium(III) terephthalate microparticles are 7 μm long leaf-like plates. According to the dynamic light scattering technique, the average size of the Eu 2 bdc 3 ·4H 2 O nanoparticles is equal to about 8 ± 2 nm. Thereby, the reported Eu 2 bdc 3 ·4H 2 O nanoparticles are the smallest nanosized rare-earth-based MOF crystals, to the best of our knowl- edge. The synthesized materials demonstrate red emission due to the 5 D 0 7 F J transitions of Eu 3+ upon 250 nm excitation into 1 ππ* state of the terephthalate ion. Size reduction results in broadened emission bands, an increase in the non-radiative rate constants and a decrease in both the quantum efficiency of the 5 D 0 level and Eu 3+ and the luminescence quantum yields. Cu 2+ , Cr 3+ , and Fe 3+ ions efficiently and selectively quench the luminescence of nanocrystalline europium(III) terephthalate, which makes it a prospective material for luminescent probes to monitor these ions in waste and drinking water. Keywords: metal-organic framework; luminescence; rare earth; europium; nanoparticle; luminescent probe 1. Introduction Rare-earth-based metal-organic frameworks (MOFs) are actively used in various fields of science and technology as luminescent sensors [111], LED components [12], luminescent probes for bioimaging [13,14], and luminescent thermometers [15,16]. Small-sized crystals of the rare-earth-based MOFs are especially interesting due to their unique properties. Such materials have a large specific surface area, and as a result, they can effectively adsorb other ions and molecules, which is necessary for the development of sensitive luminescent sensors [1719]. The presence of heavy metals in drinking water can cause numerous disorders and diseases of humans and animals [20,21]. Therefore, one must develop new sensors for such pollutants. MOFs are actively used as luminescent and electrochemical sensors for heavy metal ion detection in drinking and wastewater [13,6,7,10]. Nanosized luminescent MOFs are able to penetrate the cell membrane and are therefore used in bioimaging as luminescent probes [13,14]. The nano-sized rare-earth-based MOFs can be synthesized by several synthetic routes [13,14,2225] such as solvothermal, reverse Nanomaterials 2021, 11, 2448. https://doi.org/10.3390/nano11092448 https://www.mdpi.com/journal/nanomaterials