IP Library Granted Patent US 8,598,245
Granted Patent B2
US 8,598,245 · App. 13/087,224 · Granted Dec 3, 2013

Insulating materials comprising polysilazane, methods of forming such insulating materials, and precursor formulations comprising polysilazane

Inventors: Robert S. Larson (North Ogden, UT); Michael E. Fuller (Ogden, UT)
Assignee: Alliant Techsystems Inc.
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Quick Facts
Patent No.
US 8,598,245
App. No.
13/087,224
Granted
Dec 3, 2013
Kind
B2
Abstract

Methods of forming an insulating material comprising combining a polysilazane, a cross-linking compound, and a gas-generating compound to form a reaction mixture, and curing the reaction mixture to form a modified polysilazane. The gas-generating compound may be water, an alcohol, an amine, or combinations thereof. The cross-linking compound may be an isocyanate, an epoxy resin, or combinations thereof. The insulating material may include a matrix comprising one of a reaction product of a polysilazane and an isocyanate and a reaction product of a polysilazane and an epoxy resin. The matrix also comprises a plurality of interconnected pores produced from one of reaction of the polysilazane and the isocyanate and from reaction of the polysilazane and the epoxy resin. A precursor formulation that comprises a polysilazane, a cross-linking compound, and a gas-generating compound is also disclosed.

Claims (28)

1. A method of forming an insulating material, comprising:

combining a polysilazane, a filler, a cross-linking compound, and a gas-generating compound to form a reaction mixture, the gas-generating compound selected from the group consisting of water, an alcohol, an amine, and combinations thereof; the cross-linking compound selected from the group consisting of an isocyanate, an epoxy resin, and combinations thereof; and the filler selected from the group consisting of fumed silica, glass microspheres, boron carbide, zinc borate, and expanding graphite;

reacting the polysilazane with at least one of the gas-generating compounds and an epoxy resin cross-linking compound to form a gaseous product in the reaction mixture; and

curing the reaction mixture to form a modified polysilazane comprising a plurality of pores.

2. The method of claim 1 , wherein curing the reaction mixture comprises exposing the reaction mixture to a temperature between about 20° C. and about 25° C.

3. The method of claim 1 , wherein combining a polysilazane, a cross-linking compound, and a gas-generating compound to form a reaction mixture comprises combining a polysilazane, an aromatic isocyanate, and water.

4. The method of claim 1 , wherein combining a polysilazane, a cross-linking compound, and a gas-generating compound to form a reaction mixture comprises combining a polysilazane, methylene diphenyl diisocyanate, dipropylene glycol, and water.

5. The method of claim 1 , further comprising coating the modified polysilazane with a filler and a polysilazane matrix, the filler comprising at least one of fumed silica, glass microspheres, boron carbide, zinc borate, and expanding graphite.

6. The method of claim 1 , further comprising forming a coating over the modified polysilazane, the coating comprising graphite and glass microspheres.

7. The method of claim 1 , wherein combining a polysilazane, a cross-linking compound, and a gas-generating compound to form a reaction mixture comprises combining a polysilazane, a blocked isocyanate, an unblocked isocyanate, water, an alcohol, and a surfactant.

8. An insulating material, comprising:

a matrix comprising one of a reaction product of a polysilazane and an isocyanate or a reaction product of a polysilazane and an epoxy resin, and further comprising a filler selected from the group consisting of fumed silica, glass microspheres, boron carbide, zinc borate, and expanding graphite;

wherein the matrix comprises a plurality of pores formed by a gaseous product of one of a reaction of the polysilazane and a gas-generating compound selected from the group consisting of water, an alcohol, an amine, and combinations thereof, or by reaction of the polysilazane and the epoxy resin.

9. The insulating material of claim 8 , wherein the insulating material has a density of less than about 0.16 g/cm 3 .

10. A precursor formulation, comprising:

a polysilazane;

a cross-linking compound selected from the group consisting of an isocyanate, an epoxy resin, and combinations thereof;

a gas-generating compound selected from the group consisting of water, an alcohol, an amine, and combinations thereof; and

a filler selected from the group consisting of fumed silica, glass microspheres, boron carbide, zinc borate, and expanding graphite.

11. The precursor formulation of claim 10 , further comprising a catalyst, wherein the catalyst comprises a metal salt complex, a quaternary ammonium salt, an alkali metal carboxylate, a tertiary amine, or a quaternary amine.

12. The precursor formulation of claim 10 , further comprising a surfactant.

13. A precursor formulation, comprising:

a polysilazane;

a cross-linking compound comprising a blocked isocyanate; and

a gas-generating compound selected from the group consisting of water, an alcohol, an amine, and combinations thereof.

14. The precursor formulation of claim 13 , wherein the cross-linking compound further comprises an unblocked isocyanate, and wherein the gas-generating compound comprises water and an alcohol.

15. The precursor formulation of claim 13 , wherein the precursor formulation comprises a polysilazane, dimethyl pyrazole, methylene diphenyl diisocyanate, water, and polybutadiene with terminal isocyanate groups.

16. The precursor formulation of claim 13 , wherein the precursor formulation comprises a polysilazane, methylene diphenyl diisocyanate, water, α-hydro-Ω-hydroxy poly(oxy(methyl-1,2-ethanediyl)) ether, and 2,2-bis(hydroxymethyl)-1,3-propanediol.

Assignments (10)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 8, 2021
From: NORTHROP GRUMMAN INNOVATION SYSTEMS LLC
To: NORTHROP GRUMMAN SYSTEMS CORPORATION
Reel/Frame 055256/0892 →
CHANGE OF NAME Recorded Feb 4, 2021
From: NORTHROP GRUMMAN INNOVATION SYSTEMS, INC.
To: NORTHROP GRUMMAN INNOVATION SYSTEMS LLC
Reel/Frame 055223/0425 →
CHANGE OF NAME Recorded Nov 1, 2018
From: ORBITAL ATK, INC.
To: NORTHROP GRUMMAN INNOVATION SYSTEMS, INC.
Reel/Frame 047400/0381 →
TERMINATION AND RELEASE OF SECURITY INTEREST IN PATENTS Recorded Jun 6, 2018
From: WELLS FARGO BANK, NATIONAL ASSOCIATION, AS ADMINISTRATIVE AGENT
To: ORBITAL ATK, INC.
Reel/Frame 046477/0874 →
RELEASE OF SECURITY INTEREST Recorded Oct 8, 2015
From: BANK OF AMERICA, N.A.
To: ALLIANT TECHSYSTEMS INC.; FEDERAL CARTRIDGE CO.; EAGLE INDUSTRIES UNLIMITED, INC.; AMMUNITION ACCESSORIES, INC.; ORBITAL ATK, INC. (F/K/A ALLIANT TECHSYSTEMS INC.)
Reel/Frame 036816/0624 →
SECURITY AGREEMENT Recorded Sep 30, 2015
From: ORBITAL ATK, INC.; ORBITAL SCIENCES CORPORATION
To: WELLS FARGO BANK, NATIONAL ASSOCIATION, AS ADMINISTRATIVE AGENT
Reel/Frame 036732/0170 →
CHANGE OF NAME Recorded May 22, 2015
From: ALLIANT TECHSYSTEMS INC.
To: ORBITAL ATK, INC.
Reel/Frame 035753/0373 →
SECURITY AGREEMENT Recorded Nov 26, 2013
From: ALLIANT TECHSYSTEMS INC.; CALIBER COMPANY; EAGLE INDUSTRIES UNLIMITED, INC.; FEDERAL CARTRIDGE COMPANY; SAVAGE ARMS, INC.; SAVAGE RANGE SYSTEMS, INC.; SAVAGE SPORTS CORPORATION
To: BANK OF AMERICA, N.A.
Reel/Frame 031731/0281 →
INTELLECTUAL PROPERTY SECURITY AGREEMENT SUPPLEMENT Recorded Oct 19, 2011
From: ALLIANT TECHSYSTEMS INC.
To: BANK OF AMERICA, N.A.
Reel/Frame 027087/0823 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 14, 2011
From: LARSON, ROBERT S.; FULLER, MICHAEL E.
To: ALLIANT TECHSYSTEMS INC.
Reel/Frame 026130/0479 →
Continuity (1)
Related Publication 20120264838A1 · Oct 18, 2012