IP Library Granted Patent US 9,567,359
Granted Patent B2
US 9,567,359 · App. 15/189,427 · Granted Feb 14, 2017

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

Inventors: Albert Epshteyn (College Park, MD); Brian L. Chaloux (Alexandria, VA)
Assignee: The United States of America, as represented by the Secretary of the Navy
C07F9/659C01B21/082C01B21/097C01B25/08C07D251/26C07F9/5036C07F9/65216C08G79/06
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Quick Facts
Patent No.
US 9,567,359
App. No.
15/189,427
Granted
Feb 14, 2017
Kind
B2
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.

Claims (25)

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.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2016
From: CHALOUX, BRIAN L.
To: THE GOVERNMENT OF THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY OF THE NAVY
Reel/Frame 038985/0492 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2016
From: EPSHTEYN, ALBERT
To: THE GOVERNMENT OF THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY OF THE NAVY
Reel/Frame 038985/0699 →
Continuity (3)
Continuation In Part 14819563 · Aug 6, 2015
Provisional Application 62035061 · Aug 8, 2014
Related Publication 20160297841A1 · Oct 13, 2016