Sulfur-carbon tubes and/or spheres, and methods of making same

Patent metadata

Field	Value
Publication number	US-10790500-B2
Application number	US-201615753106-A
Country	US
Kind code	B2
Filing date	Aug 16, 2016
Priority date	Aug 17, 2015
Publication date	Sep 29, 2020
Grant date	Sep 29, 2020

Abstract

The invention provides methods of preparing carbon/sulfur composites. In certain embodiments, the composites comprise multidimensional carbon tubular and/or spherical networks loaded with elemental sulfur, as well as compositions comprising such composites.

First claim

What is claimed is:

1. A method of preparing a carbon/sulfur composite, wherein the composite comprises multidimensional carbon tubular or spherical networks associated with elemental sulfur, the method comprising:
contacting (i) a first layer comprising at least one soluble organic compound and a salt solution and (ii) a second layer comprising a gel, a salt solution, and at least one sulfide source, wherein the second layer is substantially free of oxygen gas at the time of contacting; and
directly exposing the first layer to an atmosphere comprising oxygen gas;

whereby the composite is formed once the first layer and the second layer at least partially mix and react.

2. The method of claim 1 , wherein the at least one soluble organic compound is at least one selected from the group consisting of peptone, yeast extract, casamino acids, glucose, cellobiose, glycine, and humic acids.

3. The method of claim 2 , wherein the concentration of the at least one soluble organic compound in the first layer independently varies from about 0.1 g/L to about 25 g/L.

4. The method of claim 1 , wherein the at least one sulfide source is at least one selected from the group consisting of Na 2 S, K 2 S, and FeS.

5. The method of claim 1 , wherein the concentration of the at least one sulfide source in the second layer independently varies from about 100 nM to about 100 mM.

6. The method of claim 1 , wherein, after contacting the first and second layers, an oxygen gas concentration gradient is formed within the first and second layers, wherein the oxygen gas concentration is higher in the first layer as compared to the second layer.

7. The method of claim 1 , wherein, after contacting the first and second layers, a sulfide ion concentration gradient is formed within the first and second layers, wherein the sulfide ion concentration is higher in the second layer as compared to the first layer.

8. The method of claim 1 , which does not comprise at least one step selected from the group consisting of sulfur melt incorporation and impregnation.

9. The method of claim 1 , wherein at least one property selected from the group consisting of composite rigidity, extent of carbon/sulfur network formation in the composite and sulfur loading in the composite is controlled by independently varying the concentration or identity of the at least one soluble organic compound and at least one sulfide source in the layers.

10. The method of claim 1 , wherein the composite comprises at least one structure selected from the group consisting of tubes, filaments, spheres, and platelets.

11. The method of claim 10 , wherein at least one filament has a thickness ranging from about 10 nm to about 100 μm.

12. The method of claim 10 , wherein at least one filament has a length ranging from about 1 μm to about 1,000 μm.

13. The method of claim 10 , wherein at least one filament is rectilinear or twisted.

14. The method of claim 10 , wherein at least one filament is branched.

15. The method of claim 14 , wherein the at least one filament branches at an about 45° to about 90° angle.

16. The method of claim 1 , wherein the composite comprises a tube in at least one form selected from the group consisting of helical, isolated, bundled, and arranged in perpendicular lattices.

17. The method of claim 1 , wherein the composite comprises a sulfur-carbon sphere (SCS).

18. The method of claim 1 , wherein the composite comprises elemental sulfur) (S 0 ).

19. The method of claim 18 , wherein the elemental sulfur in the composite is in at least one form selected from the group consisting of amorphous sulfur, alpha-cyclooctasulfur (α-S 8 ), and beta-cyclooctasulfur (β-S 8 ).

20. The method of claim 1 , wherein the first layer is substantially free of oxygen gas at the time of contacting.

Assignees

• Univ Colorado Regents

Inventors

• Templeton Alexis
• Cosmidis Julie

Classifications

• C01B17/00 Primary

  Sulfur; Compounds thereof · CPC title

• C01P2004/32

  Spheres · CPC title

• C01B17/40 Primary

  Making shaped products, e.g. granules · CPC title

• H01M4/364

  as mixtures · CPC title

• H01M4/362

  Composites · CPC title