Nanoparticle syntheses are designed to produce the desired product in high yield but traditionally neglect atom-economy. Here we report that the simple, but significant, change of the solvent from 1-octadecene (1-ODE) to the operationally inert octadecane (ODA) permits an atom-economical synthesis of copper selenophosphate (CuPSe) nanoparticles. This change eliminates the competing selenium (Se) delivery pathways from our first report that required an excess of Se. Instead Se is dispersed in ODA, which promotes a formal eight-electron transfer between CuP and Se. Powder X-ray diffraction and transmission electron microscopy confirm the purity of the CuPSe, while H and C NMR indicate the absence of oxidized ODA or Se species. We utilize the direct pathway to gain insights into stoichiometry and ligand identity using thermogravimetric analysis and X-ray photoelectron spectroscopy. Given the prevalence of 1-ODE in nanoparticle synthesis, this approach could be applied to other chalcogenide reaction pathways to improve stoichiometry and atom-economy.
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