Method for preparing rare-earth doped fluoride nanoparticles
View Patent ↗The invention is directed to a process of combining an aqueous solution of a fluoride with an aqueous solution of a host multi-valent metal salt and an aqueous solution of a salt forming a reactant mixture resulting in a precipitate of aqueously insoluble rare-earth doped multi-valent metal fluoride nanoparticles.
1. A process comprising reacting aqueous solutions consisting essentially of an aqueous solution of one or more fluorides with an aqueous solution of a host multi-valent metal salt and one or more rare-earth salts to form aqueously insoluble rare-earth doped multi-valent metal fluoride nanoparticles characterized by d50<100 nanometers, the rare-earth doped multi-valent metal fluoride being characterized by an aqueous solubility of less than 0.1 g/100 g of water; wherein the concentrations of the solution of the one or more fluorides and the solution of the host multi-valent metal salt and the one or more rare earth salts are in stoichiometric amounts forming a rare-earth doped multi-valent metal fluoride, and the aqueous solution of one or more fluorides and the aqueous solution of a host multi-valent metal salt and the one or more rare-earth salts are independently at least 0.1 normal; wherein the relative concentration of the rare earth cation with respect to that of the multi-valent metal cation is in the range of 2 to 20% on a molar basis; and, wherein the fluoride is selected from alkali metal fluorides, ammonium fluoride, hydrogen fluoride, or mixtures thereof.
2. The process of claim 1 wherein the multi-valent cation is selected from the group consisting of Ca +2 , Mg +2 , Sr +2 , Y +3 , La +3 , Ac +3 , Cr +3 , Mo +3 , Ir +3 , Cu +2 , Ga +3 , Pb +2 , Ce +3 , Nd +3 , Eu +3 , Er +3 , Yb +3 , and Lu +3 .
3. The process of claim 2 wherein the host multi-valent metal cation is Ca +2 or La +3 .
4. The process of claim 1 wherein the aqueous solution of a fluoride is an aqueous ammonium fluoride solution.
5. The process of claim 1 wherein the concentration of the host multi-valent metal cation salt is about 0.8 normal.
6. The process of claim 1 further comprising a batch process wherein the reaction mixture is formed in a vessel.
7. The process of claim 1 further comprising a continuous process wherein the reaction mixture is formed in a mixing chamber fed by continuous feed streams of reactants.