Microwave assisted synthesis of metal oxyhydroxides

Patent metadata

Field	Value
Publication number	US-10961631-B2
Application number	US-201816224972-A
Country	US
Kind code	B2
Filing date	Dec 19, 2018
Priority date	Apr 29, 2016
Publication date	Mar 30, 2021
Grant date	Mar 30, 2021

Abstract

A method for making a metal oxyhydroxide electrocatalytic material comprises titrating a precursor solution with a (bi)carbonate salt, the precursor solution comprising a first metal salt and a solvent, wherein the titration induces reactions between the (bi)carbonate salt and the first metal salt to provide first metal carbonate species in the titrated precursor solution; and exposing the titrated precursor solution to microwave radiation to decompose the first metal carbonate species to form the metal oxyhydroxide electrocatalytic material and carbon dioxide. Mixed metal oxyhydroxide electrocatalytic materials such as nickel-iron oxyhydroxide may be formed. Also provided are the materials themselves, electrocatalytic systems comprising the materials, and methods of using the materials and systems.

First claim

What is claimed is:

1. A metal oxyhydroxide electrocatalytic material,
wherein the metal oxyhydroxide electrocatalytic material is an oxyhydroxide (OOH) of one, two, or three metals selected from the group consisting of Fe, Ni, and Co;
wherein the metal oxyhydroxide electrocatalytic material is porous having a morphology which is a continuous matrix having irregularly shaped pores distributed throughout the matrix as determined by scanning electron microscopy;
wherein the metal oxyhydroxide electrocatalytic material is nanoamorphous as determined by high resolution transmission electron microscopy electron diffraction patterns exhibiting a lack of selected area electron diffraction spots at about a 5 nm spatial resolution;
and further wherein the metal oxyhydroxide electrocatalytic material has a homogeneous distribution of metal atoms throughout the material as exhibited by oxygen (O) 1s X-ray photoelectron spectroscopy spectra having no more than a single peak.

2. The material of claim 1 , wherein the metal oxyhydroxide electrocatalytic material is a nickel-iron oxyhydroxide electrocatalytic material.

3. The material of claim 2 , wherein the nickel-iron oxyhydroxide electrocatalytic material is Ni 0.8 :Fe 0.2 OOH.

4. The material of claim 2 , wherein the metal oxyhydroxide electrocatalytic material is Ni 0.5 Fe 0.5 OOH.

5. The material of claim 1 , wherein the metal oxyhydroxide electrocatalytic material is a nickel-cobalt oxyhydroxide electrocatalytic material.

6. The material of claim 1 , wherein the metal oxyhydroxide electrocatalytic material is a nickel-iron-cobalt oxyhydroxide electrocatalytic material.

7. The material of claim 1 , wherein the oxygen (O) 1s X-ray photoelectron spectroscopy spectra have no more than a single peak within a range of binding energies of 531.2 eV or lower.

8. An electrocatalytic system comprising an electrochemical cell configured to contain a fluid, an electrode comprising the material of claim 1 , and a counter electrode in electrical communication with the electrode.

9. The system of claim 8 , wherein the electrode further comprises a substrate and the material is in the form of a film thereon.

10. A method of using the electrocatalytic system of claim 8 , the method comprising applying an electric potential between the electrode and the counter electrode to catalyze an electrochemical reaction at an interface of the fluid and the material.

11. The method of claim 10 , wherein the fluid is an aqueous electrolyte solution and the electrochemical reaction is the hydrogen evolution reaction or the oxygen evolution reaction.

12. A metal oxyhydroxide electrocatalytic material,
wherein the metal oxyhydroxide electrocatalytic material is an oxyhydroxide (OOH) of one or more metals;
wherein the metal oxyhydroxide electrocatalytic material is porous having a morphology which is a continuous matrix having irregularly shaped pores distributed throughout the matrix as determined by scanning electron microscopy;
wherein the metal oxyhydroxide electrocatalytic material is nanoamorphous as determined by high resolution transmission electron microscopy electron diffraction patterns exhibiting a lack of selected area electron diffraction spots at about a 5 nm spatial resolution;
wherein the metal oxyhydroxide electrocatalytic material has a homogeneous distribution of metal atoms throughout the material as exhibited by oxygen (O) 1s X-ray photoelectron spectroscopy spectra having no more than a single peak;
and further wherein the metal oxyhydroxide electrocatalytic material is a tungsten-iron-cobalt oxyhydroxide electrocatalytic material.

13. A metal oxyhydroxide electrocatalytic material,
wherein the metal oxyhydroxide electrocatalytic material is an oxyhydroxide (OOH) of one or more metals;
wherein the metal oxyhydroxide electrocatalytic material is porous having a morphology which is a continuous matrix having irregularly shaped pores distributed throughout the matrix as determined by scanning electron microscopy;
wherein the metal oxyhydroxide electrocatalytic material is nanoamorphous as determined by high resolution transmission electron microscopy electron diffraction patterns exhibiting a lack of selected area electron diffraction spots at about a 5 nm spatial resolution;
wherein the metal oxyhydroxide electrocatalytic material has a homogeneous distribution of metal atoms throughout the material as exhibited by oxygen (O) 1s X-ray photoelectron spectroscopy spectra having no more than a single peak;
and further wherein the metal oxyhydroxide electrocatalytic material is an oxyhydroxide of a single metal.

Assignees

• Univ Kansas

Inventors

• Leonard Kevin C
• Barforoush Joseph M
• Seuferling Tess E
• Song Kelly R

Classifications

• C25B11/04 Primary

  characterised by the material · CPC title

• C25B1/55 Primary

  Photoelectrolysis · CPC title

• C25B11/075

  consisting of a single catalytic element or catalytic compound · CPC title

• C25B11/077

  the compound being a non-noble metal oxide · CPC title

• C25B11/055

  characterised by the substrate or carrier material · CPC title