Polymer Lamellae as Reaction Intermediates in the Formation of Copper Nanospheres as Evidenced by In Situ X‐ray Studies

Abstract

The classical nucleation theory (CNT) is the most common theoretical framework used to explain particle formation. However, nucleation is a complex process with reaction pathways which are often not covered by the CNT. Herein, we study the formation mechanism of copper nanospheres using in situ X‐ray absorption and scattering measurements. We reveal that their nucleation involves coordination polymer lamellae as pre‐nucleation structures occupying a local minimum in the reaction energy landscape. Having learned this, we achieved a superior monodispersity for Cu nanospheres of different sizes. This report exemplifies the importance of developing a more realistic picture of the mechanism involved in the formation of inorganic nanoparticles to develop a rational approach to their synthesis.

Rational Design of Mesoporous CuO–CeO2 Catalysts for NH3-SCR Applications Guided by Multiple In Situ Spectroscopies

“…To this end, the use of optical spectroscopy is of great interest, allowing continuous data collection from outside the furnace (reaction) chamber, not affecting the calcination process. Applying in situ X-ray spectroscopy to nanomaterial synthesis has previously been shown to allow a description of the direct structural phase transformation. , For a detailed understanding of the processes underlying the synthesis, the use of other techniques would be highly desirable, such as Raman spectroscopy, which probes the extended structure via phonons but also the short-range structure of solids, diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy, providing information on surface and adsorbed species, and UV–visible (UV–vis) spectroscopy, which gives details on the metal coordination environment.…”