Method of preparing a mesoporous carbon composite material

Patent metadata

Field	Value
Publication number	US-11607670-B2
Application number	US-201816487356-A
Country	US
Kind code	B2
Filing date	Feb 20, 2018
Priority date	Feb 20, 2017
Publication date	Mar 21, 2023
Grant date	Mar 21, 2023

Abstract

A method of preparing a mesoporous carbon composite material having a mesoporous carbon phase and preformed metal nanoparticles located within the mesoporous carbon phase. The present invention also relates to a mesoporous carbon composite material and to a substrate having a film of such mesoporous carbon composite material.

First claim

The invention claimed is:

1. A method of preparing a mesoporous carbon composite material comprising a mesoporous carbon phase and preformed metal nanoparticles located within the mesoporous carbon phase, the method comprising the steps:
a) providing a solution of carbon composite precursors, the solution of carbon composite precursors comprising a structure directing agent capable of forming micelles or lamellar structures, one or several poylmerizable carbon precursor components and a first solvent;
b) inducing the solution of carbon composite precursors to polymerize to form a dispersion of polymer in the first solvent, and separating the polymer from the first solvent;
c) providing preformed stabilized metal nanoparticles;
d) mixing the polymer and the preformed stabilized metal nanoparticles, wherein during the mixing, either the polymer or the preformed stabilized metal nanoparticles or both are dispersed in a second solvent;
e) stabilizing the mixture of step d) by subjecting it to a stabilization heat treatment in the range of from 80° C. to 120° C.; and
f) subjecting the product of step e) to a carbonization heat treatment in the range of from 500° C. to 1000° C.

2. The method according to claim 1 , wherein the method additionally comprises a step:
drying the mixture resulting from step d) to yield a solid, which step is performed between steps d) and e).

3. The method according to claim 1 , wherein the structure directing agent capable of forming micelles or lamellar structures is a surfactant selected from the group consisting of nonionic surfactants, cationic surfactants, anionic surfactants or zwitterionic surfactants ore mixtures thereof.

4. The method according to claim 3 , wherein the surfactant, is a nonionic surfactant, which is a block copolymer.

5. The method according to claim 4 wherein the block copolymer is a poloxamer.

6. The method according to claim 1 , wherein the polymerizable carbon precursor components comprise at least one phenolic compound and, optionally, at least one crosslinkable aldehyde compound, wherein the at least one crosslinkable aldehyde compound is added to the solution during step a) or at the beginning of step b).

7. The method according to claim 6 , wherein the at least one phenolic compound is selected from the group consisting of phenol, catechol, resorcinol, dihydroquinone, phloroglucinol, cresol, halophenol, aminophenol, hydroxybenzoic acid, and dihydroxybiphenyl.

8. The method according to claim 6 , wherein the at least one crosslinkable aldehyde compound is selected from the group consisting of formaldehyde, organoaldehydes, and organodialdehydes, represented by formulae HCHO, R—CHO and OHC—R—CHO, respectively, wherein R is a bond, a straight-chained, branched or cyclic hydrocarbonyl group, which can be either saturated or unsaturated, typically containing at least 1, 2, or 3 carbon atoms and up to 4, 5, 6, 7, 8, 9, or 10 carbon atoms.

9. The method according to claim 6 , wherein the at least one crosslinkable aldehyde compound is formaldehyde.

10. The method according to claim 1 , wherein the preformed metal nanoparticles are nanoparticles of one or more metals selected from the group consisting of Sn, Cu, Ag, Au, Zn, Cd, Hg, Cr, Mn, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt.

11. The method according to claim 10 , wherein the preformed metal nanoparticles are nanoparticles of one or more metals selected from the group consisting of Pt, Pd, Ru, Rh, Ir, Os and Ru.

12. The method according to claim 10 , wherein the preformed metal nanoparticles are nanoparticles of one or more metals selected from the group consisting of Pd, Ru, Rh and Ir.

13. The method according to claim 1 , wherein the preformed stabilized metal nanoparticles do not include carbon nanoparticles, wherein said carbon nanoparticles are carbon blacks, carbon onions, fullerenes, carbon nanodiamonds and carbon nanobuds.

14. The method according to claim 1 , wherein the preformed stabilized metal nanoparticles have a metallic core of one or several metals selected from the group consisting of Sn, Cu, Ag, Au, Zn, Cd, Hg, Cr, Mn, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt stabilized by a quaternary ammonium cation or another ionic stabilizing agent.

15. A method of preparing a mesoporous carbon composite material comprising a mesoporous carbon phase and preformed metal nanoparticles located within the mesoporous carbon phase, the method comprising the steps:
a) providing a solution of carbon composite precursors, the solution of carbon composite precursors comprising a structure directing agent capable of forming micelles or lamellar structures, one or several poylmerizable carbon precursor components and a first solvent;
b) inducing the solution of carbon composite precursors to polymerize to form a dispersion of polymer in the first solvent, and separating the polymer from the first solvent;
c) providing preformed stabilized metal nanoparticles;
d) mixing the polymer and the preformed stabilized metal nanoparticles, wherein during the mixing, either the polymer or the preformed stabilized metal nanoparticles or both are dispersed in a second solvent;
e) stabilizing the mixture of step d) by subjecting it to a stabilization heat treatment in the range of from 80° C. to 120° C.;
f) subjecting the product of step e) to a carbonization heat treatment in the range of from 500° C. to 1000° C.; and
g) applying the mixture resulting from step d) to a substrate to form a polymer film having micelles or lamellar structures and metal nanoparticles within, which step is performed between steps d) and e).

Assignees

• Univ Berlin Tech

Inventors

• Bernsmeier Denis
• Krähnert Ralph
• Sachse René

Classifications

• B01J35/45

  Nanoparticles · CPC title

• B01J37/04

  Mixing {(B01J37/0009, B01J37/0018 take precedence)} · CPC title

• B01J23/44

  Palladium · CPC title

• B01J37/0018

  Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat) · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title