IP Library Granted Patent US 11,718,536
Granted Patent B2
US 11,718,536 · App. 17/387,417 · Granted Aug 8, 2023

Solvent-free synthesis of lanthanide oxide and mixed lanthanide oxide nanoparticles

Inventors: LaRico Juan Treadwell (Albuquerque, NM); Avi Gabriel Bregman (Albuquerque, NM); Marissa Ringgold (Albuquerque, NM)
Assignee: National Technology & Engineering Solutions of Sandia, LLC
C01F17/241C01F17/235C01P2002/72C01P2002/82C01P2002/88C01P2004/03C01P2004/32C01P2004/62C01P2004/64
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Quick Facts
Patent No.
US 11,718,536
App. No.
17/387,417
Granted
Aug 8, 2023
Kind
B2
Abstract

Lanthanide oxides and mixed lanthanide oxides can be produced using furnace or microwave assisted solid-state synthesis. The use of Ln-tri(methylsilyl)amide-based precursors yields spherical nanoparticles. The formation of spherical shaped nanoparticles is likely due to the preferential single-step decomposition of the Ln-TMS as well as the low activation energy to overcome decomposition. Reaction temperature, initial metal ion ratio, and reaction dwell time can be used to control the final nanoparticle size. The method enables solvent-free, high-yield synthesis of morphology-controlled lanthanide oxides.

Claims (11)

1. A method to synthesize lanthanide (Ln) oxide nanoparticles, comprising heating of at least one Ln-tri(methylsilyl)amide precursor at a reaction temperature for a dwell time to produce Ln-oxide nanoparticles.

2. The method of claim 1 , wherein more than one Ln-tri(methylsilyl)amide precursor are combined to produce mixed Ln-oxide nanoparticles.

3. The method of claim 2 , wherein the mixed Ln-oxide nanoparticles comprise binary, ternary, quaternary mixed Ln-oxides.

4. The method of claim 1 , wherein the at least one Ln-tri(methylsilyl)amide precursor comprises cerium (III) tri(methylsilyl)amide or samarium (III) tri(methylsilyl)amide.

5. The method of claim 1 , wherein the reaction temperature is greater than 500° C.

6. The method of claim 1 , wherein the reaction temperature is less than about 1000° C.

7. The method of claim 1 , wherein the dwell time is greater than 5 minutes.

8. The method of claim 2 , wherein the Ln-oxide or mixed Ln-oxide nanoparticles are spherical.

9. The method of claim 8 , wherein the spherical Ln-oxide or mixed Ln-oxide nanoparticles have a diameter of less than 500 nm.

10. The method of claim 1 , wherein the heating is performed in a microwave oven.

11. The method of claim 1 , wherein the heating is performed in a thermal furnace.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 8, 2021
From: TREADWELL, LARICO JUAN; BREGMAN, AVI GABRIEL; RINGGOLD, MARISSA
To: NATIONAL TECHNOLOGY & ENGINEERING SOLUTIONS OF SANDIA, LLC
Reel/Frame 057741/0610 →
CONFIRMATORY LICENSE Recorded Aug 13, 2021
From: NATIONAL TECHNOLOGY & ENGINEERING SOLUTIONS OF SANDIA, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 057168/0871 →
Continuity (2)
Provisional Application 63058189 · Jul 29, 2020
Related Publication 20220033272A1 · Feb 3, 2022