Method for producing copper-selenide nanoparticles, aggregated bodies of copper-selenide nanoparticles, copper-selenide nanoparticles, and film-coated structure
In a method for producing nanoparticles of copper selenide, a flowable copper precursor is formed by combining a copper starting material and a ligand, and a flowable selenium precursor is formed by suspending a selenium starting material in a liquid. Then a flowable copper-selenium mixture including a lower-polarity solvent is formed by combining the flowable copper precursor and the flowable selenium precursor. The flowable copper-selenium mixture is conducted through at least one heating unit, and the nanoparticles of copper selenide are isolated in an oxygen-depleted environment. The isolation includes combining a solution containing the nanoparticles of copper selenide and a deoxygenated, higher-polarity solvent to precipitate the nanoparticles.
1. A method for producing copper-selenide nanoparticles by flow process, the method comprising:
forming a flowable copper precursor by combining a copper starting material and a ligand;
forming a flowable selenium precursor by suspending a selenium starting material in a liquid;
forming a flowable copper-selenium mixture by combining the flowable copper precursor and the flowable selenium precursor, the flowable copper-selenium mixture including a lower-polarity solvent;
forming a segmented flow of the flowable copper-selenium mixture by appending a segment of an immiscible, non-reacting fluid to each of a series of fixed-length segments of the flowable copper-selenium mixture;
forming a solution containing copper-selenide nanoparticles by conducting the segmented flow of the flowable copper-selenium mixture through at least one heating unit; and
isolating the nanoparticles of copper selenide in an oxygen-depleted environment, including combining the solution containing copper-selenide nanoparticles and a deoxygenated, higher-polarity solvent to precipitate the nanoparticles of copper selenide, the higher-polarity solvent being more polar than the lower-polarity solvent.
2. The method of claim 1 wherein combining the copper starting material and the ligand includes combining with the lower-polarity solvent.
3. The method of claim 1 wherein the liquid includes the lower-polarity solvent.
4. The method of claim 1 wherein the at least one heating unit includes a conduit arranged in a controlled-temperature medium.
5. The method of claim 1 wherein the ligand comprises an amine ligand.
6. The method of claim 5 wherein in the flowable copper-selenium mixture, 0.5 mol or more of the amine ligand is contained in 1 mol equivalent of copper.
7. The method of claim 1 wherein the deoxygenated higher-polarity solvent is sparged with a non-reacting gas to remove dissolved oxygen.
8. The method of claim 1 wherein each of the copper precursor and the selenium precursor are sparged with a non-reacting gas to remove dissolved oxygen.