High entropy oxides and methods of synthesis and use thereof

Patent metadata

Field	Value
Publication number	US-2025289727-A1
Application number	US-202318861410-A
Country	US
Kind code	A1
Filing date	May 5, 2023
Priority date	May 6, 2022
Publication date	Sep 18, 2025
Grant date	—

Abstract

The present invention provides compositions and nanomaterials comprising a metal based high entropy oxide comprising at least five metals and their oxides distributed in a crystal structure, with high configurational entropy, a high number of oxygen vacancies and active catalytic sites. The present invention also relates to methods of synthesis of said compositions and nanomaterials using microwave irradiation and methods of use of said compositions and nanomaterials in analyte sensing as nanozymes, electrochemical sensors, and colorimetric sensors.

First claim

1 . A composition prepared by a process comprising the steps of:
combining in a reaction medium at least five metal salts; adding at least one surfactant to the reaction medium; adding at least one compound which contains at least one carbonyl to the reaction medium; and exposing the reaction medium to microwave irradiation.

2 . The composition of claim 1 , wherein the metal salts are each independently selected from the group consisting of titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, niobium, molybdenum, technetium, ruthenium, rhodium, palladium, silver, cadmium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, combinations thereof, oxides thereof, and any oxidation state thereof.

3 . The composition of claim 1 , wherein the metal salts are iron, nickel, copper, cobalt, and manganese.

4 . The composition of claim 1 , wherein the composition comprises five metal salts wherein the ratio of the metal salts is 1:1:1:1:1.

5 . The composition of claim 1 , wherein the metal salts further comprise a bidentate ligand, wherein the bidentate ligand is selected from the group consisting of a diketone, an anhydride, an oxalate, a diamine, a diphosphine, a bipyridine, a phenanthroline, a catecholate, combinations thereof, derivatives thereof, and ions thereof.

6 . The composition of claim 5 , wherein the bidentate ligand is acetylacetonate.

7 . The composition of claim 1 , wherein the at least one surfactant is a quaternary ammonium salt.

8 . The composition of claim 1 , wherein the at least one surfactant is cetyltrimethylammonium chloride (CTAC).

9 . The composition of claim 1 , wherein the at least one compound which contains at least one carbonyl is urea.

10 . The composition of claim 1 , wherein the step of exposing the reaction medium to microwave irradiation is performed at about 250 W to 350 W.

11 . The composition of claim 1 , wherein the step of exposing the reaction medium to microwave irradiation is performed at about 100° C. to about 200° C.

12 . The composition of claim 1 , wherein the step of exposing the reaction medium to microwave irradiation is performed for about 10 to 30 minutes.

13 . A nanomaterial comprising the composition of claim 1 .

14 . A method of sensing analytes comprising the steps of:
providing a nanomaterial comprising at least five metal oxides; and exposing the nanomaterial to at least one analyte in a solution.

15 . The method of claim 14 , further comprising the step of dispersing the nanomaterial on graphene oxide.

16 . The method of claim 14 , wherein the at least one analyte is selected from the group consisting of a steroid, a hormone, an antioxidant, an oxidant, a thiol, combinations thereof, and derivatives thereof.

17 . The method of claim 14 , wherein the at least one analyte is selected from the group consisting of cortisol, hydrogen peroxide, glutathione, and derivatives thereof.

18 . The method of claim 14 , wherein the concentration of the at least one analyte in the solution is lower than 0.50 μM.

19 . The method of claim 14 , wherein the nanomaterial is a nanozyme.

20 . The method of claim 14 , wherein the nanomaterial is an electrochemical sensor or a colorimetric sensor.

21 . (canceled)

Assignees

• Univ Hawaii

Inventors

• Ray Tyler
• Yin Ziyu

Classifications

• C01G53/04

  Oxides · CPC title

• C01G51/04

  Oxides · CPC title

• C01G49/02

  Oxides; Hydroxides {(C01G49/0018 takes precedence)} · CPC title

• C01G45/02

  Oxides · CPC title

• B82Y15/00

  Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors · CPC title