# US 4,080,413 A · Porous carbon fuel cell substrates and method of manufacture

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- Number: US 4,080,413 A
- Document ID: US4080413A
- Status: Granted
- Kind: A
- Application number: 05/640,467
- Filed: 1975-12-15
- Granted: 1978-03-21
- Earliest claimed: 1975-12-15
- Assignees: United Technologies Corporation
- Inventors: George K. Layden; Roscoe A. Pike; Michael A. DeCrescente
- Web page: https://patentgrep.com/patent/US4080413A

## CPC

- D01F 9/22: from polyacrylonitriles
- D21H 5/205: {acrylic fibres}
- D21H 13/18: Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylonitriles
- H01M 4/96: Carbon-based electrodes
- Y02E 60/50: Fuel cells
- Y10T 442/56: From synthetic organic fiber
- D01F: CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D21H: PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

Porous carbon sheets suitable for use as fuel cell electrode support plates are produced by stabilizing acrylic filament precursors through the controlled addition of oxygen thereto. The stabilized filaments are thereafter chopped into short lengths, felted and pressed into sheets with the pressing step being performed at a temperature determined by the oxygen content of the stabilized filaments. The sheets are thereafter pyrolyzed to produce the desired porous substrate material.

## Claims

### Claim 1

A process for the manufacture of substrate material having a porosity in the range of 50% to 70% comprising the steps of:
stabilizing a plurality of acrylic polymer filaments, said filaments containing at least 50% acrylonitrile, by heating in an oxidizing atmosphere until 3 to 10% by weight oxygen is introduced into the polymer;
reducing the length of the stabilized filaments to form fibers having an average length commensurate with the desired substrate porosity;
felting the fibers of reduced length to provide a layer of uniform thickness with random fiber orientation;
subjecting the layer of fibers to heat and pressure in the range of 50-1000 psi to cause self-bonding of contiguous fibers whereby a sheet is formed without the aid of a binder for the felted fibers; and
carbonizing the sheet by heating in a non-oxidizing atmosphere to produce a porous substrate material.

### Claim 2 (depends on 1)

The method of claim 1 wherein the step of reducing the length of the stabilized filaments comprises:
mechanically chopping the filaments into lengths commensurate with the desired substrate porosity.

### Claim 3 (depends on 1)

The method of claim 1 wherein the substrate material has a thickness in the range of 15-20 mils and a lateral resistivity in the range of 0.01 to 0.05 ohm-cm. and wherein the step of felting comprises:
distributing the fibers in a water slurry;
collecting the distributed fibers from the slurry on a surface; and
drying the collected fibers.

### Claim 4 (depends on 1)

The method of claim 1 wherein the step of subjecting the layer of fibers to heat and pressure to form a sheet comprises:
placing the layer of fibers in a mold;
heating the mold to a temperature commensurate with the oxygen content of the stabilized filaments; and
applying a pressure in the range of 50 to 1000 psi.

### Claim 5 (depends on 4)

The method of claim 4 wherein the applied temperature is in the range of 160.degree. to 350.degree. C.

### Claim 6 (depends on 5)

The method of claim 5 wherein the step of reducing the length of the stabilized filaments comprises:
mechanically chopping the filaments into lengths commensurate with the desired substrate porosity.

### Claim 7 (depends on 6)

The method of claim 6 wherein the substrate material has a thickness in the range of 15-20 mils and a lateral resistivity in the range of 0.01 to 0.05 ohm-cm. and wherein the step of felting comprises:
distributing the fibers in a water slurry;
collecting the distributed fibers from the slurry on a surface; and
drying the collected fibers.

### Claim 8 (depends on 4)

The method of claim 4 wherein the substrate has a porosity of 55 to 65%, a thickness in the range of 15-20 mils and a lateral resistivity in the range of 0.01 to 0.05 ohm-cm. and wherein the step of stabilizing comprises:
heating the filaments in an oxidizing atmosphere until 4 to 8% by weight of oxygen is introduced into the polymer.

### Claim 9 (depends on 8)

The method of claim 8 wherein the temperature applied during the formation of the sheet is in the range of 180.degree. to 270.degree. C.

### Claim 10 (depends on 4)

The method of claim 4 wherein the step of carbonizing the sheet comprises:
heating in an argon atmosphere to a temperature in the range of 1000.degree. to 1260.degree. C at a rate of 100.degree. C per hour.

### Claim 11 (depends on 9)

The method of claim 9 wherein the step of carbonizing the sheet comprises:
heating in an argon atmosphere to a temperature in the range of 1000.degree. to 1260.degree. C at a rate of 100.degree. C per hour.

### Claim 12 (depends on 11)

The method of claim 11 wherein the step of reducing the length of the stabilized filaments comprises:
mechanically chopping the filaments into lengths commensurate with the desired substrate porosity.

### Claim 13 (depends on 12)

The method of claim 12 wherein the step of felting comprises:
distributing the fibers in a water slurry;
collecting the distributed fibers from the slurry on a surface; and
drying the collected fibers.