This review is devoted to non-hydrolytic sol-gel chemistry. During the last 25 years, non-hydrolytic sol-gel (NHSG) techniques were found to be attractive and versatile methods for the preparation of oxide materials. Compared to conventional hydrolytic approaches, the NHSG route allows reaction control at the atomic scale resulting in homogeneous and well defined products. Due to these features and the ability to design specific materials, the products of NHSG reactions have been used in many fields of application. The aim of this review is to present an overview of NHSG research in recent years with an emphasis on the syntheses of mixed oxides, silicates and phosphates. The first part of the review highlights well known condensation reactions with some deeper insights into their mechanism and also presents novel condensation reactions established in NHSG chemistry in recent years. In the second section we discuss porosity control and novel compositions of selected materials. In the last part, the applications of NHSG derived materials as heterogeneous catalysts and supports, luminescent materials and electrode materials in Li-ion batteries are described.

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Non-hydrolytic sol–gel reactions of acetoxysilanes with trimethylsilyl esters of phosphoric and phosphonic acids provide hybrid xerogels with large surface areas (up to 700 m2 g−1). The presence of SiO6 structural units in bridged-phosphoryl xerogels is related to their microporosity while the absence of such moieties in bridged-acetoxysilane networks is congruent with significant mesoporosity.

A novel non-hydrolytic sol–gel (NHSG) synthesis of mesoporous aluminosilicate xerogels is presented.

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The Ag-Cu bimetallic colloidal nanoparticles (NPs) were prepared by solvothermal synthesis from metalloorganic precursors in a mixture of organic solvents. The nanoparticles were characterized by dynamic light scattering (DLS) and small angle X-ray scattering (SAXS). The properties of metallic core and organic shell of the nanoparticles were studied by direct inlet probe mass spectrometry (DIP/MS), Knudsen effusion mass spectrometry (KEMS), double-pulse laser-induced breakdown spectroscopy (DPLIBS), and differential scanning calorimetry (DSC). The transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were used for particle characterization before and after thermal analysis. The experiment yielded results that were for AgCu nanoparticles for the first time. The detected liquidus temperature has been compared with the prediction obtained from calculation of the phase diagram of Ag-Cu nanoalloy. The experimental results show that of near-eutectic composition AgCu nanoparticles possess the fcc crystal lattice. Surprisingly, spinodal decomposition was not observed inside the AgCu nanoparticles at temperatures up to 230°C. The depression of the eutectic AgCu melting point was calculated but not observed. The eutectic AgCu microparticles are formed before melting.