Method of producing porous metal-carbon materials
A method for creating a metal-carbon composite. In one embodiment, the method includes the steps of providing a polymer Schiff base transition metal film precursor having a chemical structure of the formula [M(Schiff)] n and a recurring unit and a transition metal selected from the group consisting of nickel, palladium, platinum, cobalt, copper, iron; Schiff is a tetradentate Schiff base ligand selected from the group consisting of Salen (residue of bis(salicylaldehyde)-ethylenediamine), Saltmen (residue of bis(salicylaldehyde)-tetramethylethylenediamine, Salphen (residue of bis-(salicylaldehyde)-o-phenylenediamine), a substituent in a Schiff base is selected from the group consisting of H—, and carbon-containing substituents, preferably CH 3 —, C 2 H 5 —, CH 3 O—, C 2 H 5 O—, and Y is a bridge in a Schiff base depositing the polymer Schiff base transition metal precursor film onto a support substrate; and heating the polymer Schiff base transition metal precursor film and support substrate in a furnace in an inert atmosphere.
1. A method for creating a metal-carbon composite comprising the steps of:
a. providing a polymer Schiff base transition metal film precursor having a chemical structure of the formula [M(Schiff)] n and the recurring unit of the following structure:
wherein n is an integer between 2 and 50,000; M is a transition metal selected from the group consisting of nickel, palladium, platinum, cobalt, copper, and iron; Schiff is a tetradentate Schiff base ligand selected from the group consisting of Salen (residue of bis(salicylaldehyde)-ethylenediamine), Saltmen (residue of bis(salicylaldehyde)-tetramethylethylenediamine, and Salphen (residue of bis-(salicylaldehyde)-o-phenylenediamine); R is a substituent in a Schiff base selected from the group consisting of H—; and carbon-containing substituents, preferably CH 3 —, C 2 H 5 —, CH 3 O—, C 2 H 5 O—; and Y is a bridge in a Schiff base and has the following structure:
—CH 2 —CH 2 —,
or
when the Schiff base is a Salen, a Saltmen and a Salphen, respectively,
b. depositing the polymer Schiff base transition metal precursor film onto a support substrate; and
c. heating the polymer Schiff base transition metal precursor film and support substrate in a furnace in an inert atmosphere.
2. The method of claim 1 wherein the support substrate is a glassy carbon plate.
3. The method of claim 1 wherein the inert atmosphere is selected from one or more of nitrogen, argon, and helium.
4. The method of claim 1 wherein the polymer Schiff base transition metal precursor film and support substrate are heated between 500° C.-750° C. for 1-4 hours.
5. The method of claim 4 wherein the polymer Schiff base transition metal precursor film and support substrate are heated from 550° C. to 650° C.
6. The method of claim 4 wherein the polymer Schiff base transition metal precursor film and support substrate are heated from 580° C. to 620° C.
7. The method of claim 4 wherein the polymer Schiff base transition metal precursor film and support substrate are heated for 2-3 hours.
8. The method of claim 1 wherein the deposition of the polymer Schiff base transition metal precursor film onto a support substrate comprises polymerization by application of a constant potential to the substrate.
9. The method of claim 8 wherein the support substrate is a glassy carbon plate.
10. The method of claim 8 wherein the constant potential of +0.98V, as measured against a standard silver/silver chloride reference electrode, is applied to the substrate.
11. The method of claim 8 wherein the polymerization of a polymer film occurs with the substrate positioned in a solution containing tetraethylammonium tetrafluoroborate and the Schiff base monomer complex.
12. The method of claim 11 where a solvent of the solution is acetonitrile.
13. The method of claim 12 wherein the support with the polymer film on it is rinsed with acetonitrile prior to being placed in the furnace.
14. The method of claim 11 where a solvent of the solution is propylene carbonate.