Solvent self-reactions with P(CN)3 to produce films and particles of C3N3P

Patent metadata

Field	Value
Publication number	US-9567359-B2
Application number	US-201615189427-A
Country	US
Kind code	B2
Filing date	Jun 22, 2016
Priority date	Aug 8, 2014
Publication date	Feb 14, 2017
Grant date	Feb 14, 2017

Abstract

A material with the empirical formula C 3 N 3 P is made by polymerizing P(CN) 3 in a polar aprotic solvent such as acetonitrile, by heating, irradiation with ultraviolet light, and/or using a polymerization initiator and/or a catalyst.

First claim

What is claimed is:

1. A method of making C 3 N 3 P, the method comprising:
providing, in a sealable vessel, a solution of P(CN) 3 in a polar aprotic solvent, and then
heating the solution to at least 185° C. while the vessel is sealed, thereby obtain a polymer having the empirical formula C 3 N 3 P.

2. The method of claim 1 , wherein said polar aprotic solvent is acetonitrile.

3. The method of claim 1 , wherein a polymerization initiator and/or a catalyst is included in said polar aprotic solvent.

4. The method of claim 3 , wherein said polymerization initiator and/or catalyst is azobisisobutyronitrile.

5. The method of claim 1 , wherein said polymer is entirely amorphous.

6. The method of claim 1 , wherein a substrate is included in said sealable vessel prior to said heating, and wherein said polymer is a film on the substrate, the film having a thickness of between about 100 microns and about 1 nanometer.

7. The method of claim 1 , wherein said polymer is in the form of particles 10 nm to 10 μm in size.

8. A method of making C 3 N 3 P, the method comprising:
providing a starting solution of P(CN) 3 in a polar aprotic solvent,
irradiating the starting solution with ultraviolet light, thereby obtaining a dendrimeric prepolymer comprising C 3 N 3 P, and
separating the prepolymer from the P(CN) 3 and solvent.

9. The method of claim 8 , wherein said polar aprotic solvent is acetonitrile.

10. The method of claim 8 , wherein a polymerization initiator and/or a catalyst is included in said polar aprotic solvent.

11. The method of claim 8 , further comprising thermally treating the prepolymer to obtain a cross-linked C 3 N 3 P polymer.

12. The method of claim 11 , wherein said cross-linked C 3 N 3 P polymer is entirely amorphous.

13. A method of making C 3 N 3 P, the method comprising:
providing a starting solution of P(CN) 3 and a polymerization initiator and/or a catalyst in a polar aprotic solvent;
heating the solution, thereby obtaining a dendrimeric prepolymer comprising C 3 N 3 P; and
separating the prepolymer from the P(CN) 3 and solvent.

14. The method of claim 13 , wherein said polar aprotic solvent is acetonitrile.

15. The method of claim 13 , wherein said polymerization initiator and/or catalyst is azobisisobutyronitrile.

16. The method of claim 13 , further comprising thermally treating the prepolymer to obtain a cross-linked C 3 N 3 P polymer.

17. The method of claim 16 , wherein said cross-linked C 3 N 3 P polymer is entirely amorphous.

Assignees

• Us Navy

Inventors

• Epshteyn Albert
• Chaloux Brian L

Classifications

• C07F9/6521

  Six-membered rings · CPC title

• C01B25/08

  Other phosphides · CPC title

• C07F9/659 Primary

  having three phosphorus atoms as ring hetero atoms in the same ring {(C07F9/65812 takes precedence)} · CPC title

• C01B21/082

  Compounds containing nitrogen and non-metals {and optionally metals}(C01B21/06, C01B21/08 take precedence) · CPC title

• C01B21/097

  containing phosphorus atoms · CPC title