Synthesis of Transition-Metal Nitrides from Nanoscale Metal Particles Prepared by Homogeneous Reduction of Metal Halides with an Alkalide

Abstract

Transition-metal nitrides have been synthesized by heating nanoscale metal particles under flowing N2(g) or NH3(g). In some cases reaction temperatures are significantly lower than those required by conventional heating procedures. Nanoscale metal particles of Mo, Nb, Ta, Fe−Mo, Fe−Nb, and Cu−Nb were prepared by reduction of the respective metal chloride or mixture of chlorides with the sodide, [K+(15-crown-5)2]Na-, in dimethyl ether solution. The previously characterized nitrides that were prepared (with synthesis conditions indicated) include γ-Mo2N (800 °C, N2) and Mo2N (720 °C, N2), Ta3N5 (650 °C, NH3), Fe3Mo3N (>650 °C, N2), and a mixture of niobium nitride phases (800 °C, N2). A previously unreported phase has been found in the Ba−Nb−N system.

Growth Confined by the Nitrogen Source: Synthesis of Pure Metal Nitride Nanoparticles in Mesoporous Graphitic Carbon Nitride

“…Several attempts towards nanostructured metal nitrides are also found in the literature. The conversion of metal [31] and metal oxide nanoparticles [31][32][33][34] or solvothermal synthesis [35][36][37] has been shown to generate various nanometersized structures of metal nitrides with various compositions. The synthesis of metal nitrides in the pores of mpg-C 3 N 4 from the corresponding sol-gel oxide precursors represents an effective combination of the previously described nanoreactor approaches for the generation of nanostructures and the synthesis of nitrides from oxides using nitrogen sources.…”

The study of polymerization kinetics of methacrylamide by oxidation: Reduction system using potassium permanganate/glycine in aqueous medium

“…Conventional synthesis of Ta 3 N 5 is mainly based on the high‐temperature reaction of nitrogen, ammonia, or a hydrogen/nitrogen mixture with metallic Ta, its oxide, or its chloride, usually at temperatures around 1000 °C 2. 15, 16 The most serious disadvantage associated with these preparation methods is the lack of control over crystallinity and particle size, and therefore the thus‐synthesized Ta 3 N 5 generally has a large size and a small specific surface area. To overcome these problems, templates, such as poly(styrene‐ co ‐acrylamide) (PSAM) colloidal spheres,14 C 3 N 4 ,11 SiO 2 ,17 and triblock copolymer P‐123,10 have been introduced to control the porous structure and particle size of the final Ta 3 N 5 product, and in this way high photocatalytic activity has been achieved.…”

Electron-Transfer Processes Mediated by Alkalides: A Critical Approach

“…It was demonstrated for Au-Zn, Au-Cu, Cu-Te and Zn-Te by their XP spectra. Transition metal nitrides like for example Mo 2 N, Ta 3 N 5 , Fe 3 Mo 3 N and a mixture of niobium nitride phases were synthesized by heating nanoscale metal particles under flowing gaseous N 2 or NH 3 [130]. A major advantage of this method is the simple ability to control overall stoichiometry by adjusting initial compositions.…”