US 12,077,440 B1
Method of making graphitic carbon-carbon composite
Richard D. Hreha, Centerville, OH (US); and Jeffrey R. Josken, West Carrollton, OH (US)
Assigned to Systima Technologies, Inc., Mukilteo, WA (US)
Filed by Systima Technologies, Inc., Mukilteo, WA (US)
Filed on Apr. 5, 2022, as Appl. No. 17/713,381.
Claims priority of provisional application 63/225,645, filed on Jul. 26, 2021.
Claims priority of provisional application 63/170,755, filed on Apr. 5, 2021.
Int. Cl. C01B 32/205 (2017.01); C08J 5/24 (2006.01)
CPC C01B 32/205 (2017.08) [C08J 5/243 (2021.05); C01P 2006/10 (2013.01); C08J 2387/00 (2013.01)] 17 Claims
 
1. A method of making a graphitic carbon-carbon composite from thermosetting polymer resin comprising the steps of:
a) infusing bis-Schiff base resin into a carbon fiber reinforcement to form an uncured resin embedded composite, the bis-Schiff base resin comprising the structure of Formula (I):

OG Complex Work Unit Chemistry
wherein:
R comprises at least one aromatic moiety,
X comprises an aromatic moiety, an aliphatic moiety, or a hydrogen and
X′ comprises an aromatic moiety, an aliphatic moiety, or a hydrogen;
b) positioning the uncured resin embedded composite on a substrate under a vacuum enclosure;
c) curing the carbon fiber reinforcement embedded with bis-Schiff base resin at a first elevated temperature under vacuum to form a polymer matrix composite;
d) heating the polymer matrix composite at a second elevated temperature under inert atmosphere to form a porous carbon-carbon composite;
e) re-infusing bis-Schiff base resin into the porous carbon-carbon composite resulting from step (d) and curing the newly infused bis-Schiff base resin under vacuum at a third elevated temperature to generate a reinfused porous carbon-carbon composite;
f) heating the reinfused porous carbon-carbon composite resulting from step (e) at a fourth elevated temperature under inert gas to densify the resulting reinfused porous carbon-carbon composite from step (e) and form the graphitic carbon-carbon composite;
wherein the second elevated temperature and/or at least one instance of the fourth elevated temperature is greater than 1800° C.