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.

Amorphous nanoscopic iron(III) oxide with interesting magnetic properties was prepared by sonolysis of Fe(acac)(3) under Ar in tetraglyme with a small amount of added water. The organics content and the surface area of the Fe(2)O(3) nanoparticles can be controlled with an amount of water in the reaction mixture and it increases from 48 m(2)g(-1) for dry solvent up to 260 m(2)g(-1) when wet Ar is employed. For further monitoring of the particle size and morphology and for the study of the surface, magnetic and thermal properties, the sample with 2 vol.% of H(2)O was chosen. SEM showed nanoscopic composite particles of a uniform size distribution and nearly spherical shapes with an estimated diameter of 20 nm. Such composites are built from amorphous iron(III) oxide nanoparticles (3 nm) embedded in an acetate matrix as proved by TEM and IR spectroscopy. Temperature-dependent Mössbauer spectra demonstrate a very narrow magnetic transition with an unusually low transition temperature around 25K reflecting the system of magnetically non-interacting ultrasmall particles with a narrow size distribution. The in-field (5T) Mössbauer spectrum recorded at 5K shows a minimum change compared to the zero-field spectrum indicating an absence of the long-range magnetic ordering. The composite particles are thermally stable up to 150 degrees C, which is confirmed by DSC, TG, and by the constant surface area. At higher temperatures, acetate groups are removed from the particle surface, which is documented by the increased surface area and disappearance of their IR bands.

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.