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Single-source synthesis of ceramic oxide nanoparticles

United States Patent

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10,407,347
September 10, 2019
View the Complete Patent at the US Patent & Trademark Office
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.
15/ 901,776
February 21, 2018
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C04B 35/16 (20060101)C08K 3/22 (20060101)C08K 3/36 (20060101)C04B 35/628 (20060101)C01G 27/02 (20060101)B01J 13/02 (20060101)C07F 9/00 (20060101)C07F 7/08 (20060101)C04B 35/64 (20060101)C04B 35/626 (20060101)C07F 7/28 (20060101)C07F 7/02 (20060101)A61K 41/00 (20060101)B01J 13/06 (20060101)
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.