Single-source synthesis of ceramic oxide nanoparticles

Patent Number: 10,407,347
Issued: 9/10/2019
Official Filing: View the Complete Patent
Abstract: The tris(trimethylsilyl)silanol (H-SST) ligand can be reacted with a Group 4 or 5 metal alkoxides in a solvent to form an SST-modified metal alkoxide precursor. Exemplary Group 4 precursors include [Ti(SST).sub.2(OR).sub.2] (OR=OPr.sup.i, OBu.sup.t, ONep); [Ti(SST).sub.3(OBu.sup.n)]; [Zr(SST).sub.2(OBu.sup.t).sub.2(py)]; [Zr(SST).sub.3(OR)] (OR=OBu.sup.t, ONep); [Hf(SST).sub.2(OBu.sup.t).sub.2]; and [Hf(SST).sub.2(ONep).sub.2(py).sub.n] (n=1, 2), where OPr.sup.i=OCH(CH.sub.3).sub.2, OBu.sup.t=OC(CH.sub.3).sub.3, OBu.sup.n=O(CH.sub.2).sub.3CH.sub.3, ONep=OCH.sub.2C(CH.sub.3).sub.3, and py=pyridine. Exemplary Group 5 precursors include [V(SST).sub.3(py).sub.2]; [Nb(SST).sub.3(OEt).sub.2]; [Nb(O)(SST).sub.3(py)]; 2[H][(Nb(.mu.-O).sub.2(SST)).sub.6(.mu..sub.6-O)]; [Nb.sub.8O.sub.10(OEt).sub.18(SST).sub.2.1/5Na.sub.2O]; [Ta(SST)(.mu.-OEt)(OEt).sub.3].sub.2; and [Ta(SST).sub.3(OEt).sub.2]; where OEt=OCH.sub.2CH.sub.3. When thermally processed, the precursors can form unusual core-shell nanoparticles. For example, HfO.sub.2/SiO.sub.2 core/shell nanoparticles have demonstrated resistance to damage in extreme irradiation and thermal environments.
Filed: 2/21/2018
Application Number: 15/901,776
Government Interests: STATEMENT OF GOVERNMENT INTEREST This invention was made with Government support under Contract No. DE-NA0003525 awarded by the United States Department of Energy/National Nuclear Security Administration. The Government has certain rights in the invention.