SPECIAL EDITION: CELEBRATING THE 60TH ANNIVERSARY OF PROFESSOR DAVID AVNIR Hydrogen peroxide induced formation of peroxystannate nanoparticles Sergey Sladkevich Æ Vitaly Gutkin Æ Ovadia Lev Æ Elena A. Legurova Æ Dzhalil F. Khabibulin Æ Martin A. Fedotov Æ Vladimir Uvarov Æ Tatiana A. Tripol’skaya Æ Petr V. Prikhodchenko Received: 18 March 2008 / Accepted: 10 June 2008 / Published online: 30 July 2008 Ó Springer Science+Business Media, LLC 2008 Abstract Stable, amorphous potassium peroxystannate nanoparticles of controlled average size—in the range 10– 100 nm—and of controlled hydrogen peroxide content—in the range of 19–30 wt%—were synthesized by hydrogen peroxide induced polymerization in water–potassium hexa- hydroxostannate solutions. The sol phase and the precipitate were characterized by vibrational spectroscopies, 119 Sn NMR, XPS and XRD using crystalline K 2 Sn(OH) 6 and K 2 Sn(OOH) 6 reference materials. This is the first study to show that per- oxocoordination induces polymerization of a main group element. 119 Sn NMR studies show that peroxotin coordination and polymerization took place already in the hydrogen per- oxide–water phase. The high abundance of peroxotin bonds revealed by 119 Sn MAS NMR, vibrational spectroscopy, and XPS suggests that the particles are predominantly made of peroxo bridged tin networks. Although the particles are highly stable in the dry phase as well as in alcohol solutions and do not lose hydrogen peroxide upon storage, they release their stored hydrogen peroxide content by exposure to water. Keywords Tin Á Hydrogen peroxide Á Peroxytin Á Peroxostannate Á Peroxocoordination Á Solid phase active oxygen Á Nanoparticles 1 Introduction Transition-element peroxoacids are frequently used as pre- cursors for metal oxide film and particle formation [1]. However, when it comes to the long term storage of hydrogen peroxide in solid state materials, the transition metals are much inferior compared to the more inert main group element matrices [2]. Surprisingly, to date, there is no reported effort to produce main group metal peroxyparticles whose amorphous skeleton comprises of peroxobridges or with hydrogen per- oxide coordinated directly to the backbone. Until now all the published reports on peroxide loaded non transition metal oxide gels pertain to imbibed, hydrogen bonded or unex- plained attachment of the hydrogen peroxide to the oxide. In this article we describe the formation of peroxystannate nanoparticles of ca. 10–100 nm by mixing hydrogen peroxide with aqueous potassium hexahydroxostannate solutions. In addition to the importance of doped tin oxides [3] and crys- talline stannates [4] in contemporary science and technology, the hydroperoxostannates are appealing case study materials due to the availability of crystalline K 2 Sn(OH) 6 and K 2 Sn(OOH) 6 reference materials which allowed us to deci- pher the FTIR, XPS, and 119 Sn MAS NMR spectra of the peroxystannate nanoparticles. Potassium hydroperoxostan- nates were only recently synthesized [5]. Three properties of hydrogen peroxide are responsible for much of its contemporary popularity. Hydrogen peroxide is S. Sladkevich Á V. Gutkin Á O. Lev (&) Á P. V. Prikhodchenko (&) The Casali Institute and The Chemistry Institute, The Hebrew University of Jerusalem, Jerusalem 91904, Israel e-mail: ovadia@vms.huji.ac.il P. V. Prikhodchenko e-mail: prikhman@gmail.com V. Gutkin Á V. Uvarov The Harwey Kreuger Family Center for Nanoscience and Nanotechnology, The Hebrew University of Jerusalem, Jerusalem 91904, Israel E. A. Legurova Á T. A. Tripol’skaya Á P. V. Prikhodchenko Institute of General and Inorganic Chemistry RAS, Leninskii Prosp. 31, Moscow 119991, Russia D. F. Khabibulin Á M. A. Fedotov Boreskov Institute of Catalysis, SB RAS, Prosp. Lavrentieva 5, Novosibirsk 630090, Russia 123 J Sol-Gel Sci Technol (2009) 50:229–240 DOI 10.1007/s10971-008-1800-6