Synthesis of metal oxynitrides using flame spray pyrolysis

Patent metadata

Field	Value
Publication number	US-10899616-B2
Application number	US-202016851311-A
Country	US
Kind code	B2
Filing date	Apr 17, 2020
Priority date	Jun 20, 2019
Publication date	Jan 26, 2021
Grant date	Jan 26, 2021

Abstract

The present disclosure is directed to methods for producing metal oxynitrides using flame synthesis. Embodiments of the disclosure may provide advantages over prior synthesis techniques by reducing synthesis time. Additionally, methods and systems disclosed herein may achieve better incorporation of nitrogen atoms into the oxide structure due in part to the higher homogeneity of flame made particles and ability to control the reaction environment.

First claim

The invention claimed is:

1. A method for synthesizing a metal oxynitride using flame synthesis, the method comprising:
providing a solution containing at least one precursor and a solvent to a flame spray pyrolysis system,
exposing a portion of the solution to a precursor flame generated by the flame spray pyrolysis system, and
recovering the metal oxynitride without further processing,
wherein each of the at least one precursor comprises a metal, and wherein the flame spray pyrolysis system comprises:
a burner fuel inlet for providing a burner fuel and a burner oxidant to form a burner flame characterized by an equivalence ratio to support the precursor flame.

2. The method as in claim 1 , wherein the burner fuel comprises a hydrocarbon, hydrogen gas, or both with a flowrate of about 0.01 L/min to about 15 L/min.

3. The method as in claim 1 , wherein the burner oxidant is a gaseous mixture comprising 5-100% oxygen.

4. The method as in claim 1 , wherein the solvent comprises at least one flammable liquid.

5. The method of claim 1 , wherein the solution is provided at a flowrate between about 10 μL/min to about 50 mL/min.

6. The method of claim 1 , wherein the flame spray pyrolysis system further comprises a precursor inlet for providing a precursor oxidant to the precursor flame.

7. The method as in claim 6 , further comprising:
providing the precursor oxidant at a pressure drop of 0-5.0 bar across the flame spray pyrolysis system.

8. The method of claim 1 , wherein the metal includes one of the group consisting of: gallium (Ga), zinc (Zn), tantalum (Ta), titanium (Ti), zirconium (Zr), lanthanum (La), magnesium (Mg), calcium (Ca), strontium (Sr), barium (Ba), niobium (Nb), yttrium (Y), cerium (Ce), vanadium (V), molybdenum (Mo), tungsten (W), iron (Fe), praseodymium (Pr), neodymium (Nd), europium (Eu), aluminum (Al), lithium (Li), sodium (Na), manganese (Mn), scandium (Sc), and beryllium (Be).

9. The method of claim 1 , wherein all of the at least one precursor comprises the same metal, and wherein the metal oxynitride comprises one metal.

10. The method of claim 1 , wherein the solution contains at least two precursors: a first precursor and a second precursor, and wherein the first precursor comprises a first metal and the second precursor comprises a second metal, and wherein the first metal is different from the second metal.

11. The method of claim 10 , further comprising a third precursor comprising a third metal, and wherein the third metal is different from both the first metal and the second metal.

12. The method of claim 1 , further comprising:
providing the burner fuel and the burner oxidant at the equivalence ratio between about 0.25 to about 4.0, wherein the equivalence ratio characterizes the burner fuel to the burner oxidant ratio relative to a stoichiometric ratio of the burner fuel to the burner oxidant.

13. The method of claim 1 , wherein providing the solution containing at least one precursor and the solvent into the flame spray pyrolysis system comprises:
flowing a fraction of the burner flame fuel, the burner flame oxidant, or both through the solution to form a precursor saturated vapor, wherein the precursor saturated vapor contains the solution in a gaseous phase or as an aerosol.

14. The method of claim 13 , further comprising heating the solution.

15. The method of claim 1 , wherein each of the precursors independently comprise the metal in a form from one of the group consisting of: nitrates, nitrate hydrates, chlorides, chloride hydrates, acetylacetonates, acetates, iodides, oxides, nitrides, phosphides, sulphates, sulphides, perchlorates, ethylhexanoates, propoxides, butoxides, carbonates, pentanedionates, hexonate and naphthenates.

16. The method of claim 1 , wherein the solution further contains a nitrogen compound.

17. The method of claim 16 , wherein the nitrogen compound comprises urea.

Assignees

• Univ South Carolina

Inventors

• Sasmaz Erdem
• Cordonnier Nicole
• Meekins Benjamin
• Naglic Jennifer

Classifications

• C01P2002/85

  by XPS, EDX or EDAX data · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01B21/0821 Primary

  Oxynitrides of metals, boron or silicon · CPC title