# US 11,299,824 B2 · Selective control of oxidation atmospheres in carbon fiber production > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,299,824 B2 - Document ID: US11299824B2 - Status: Granted - Kind: B2 - Application number: 16/546,990 - Filed: 2019-08-21 - Published: 2021-02-25 - Granted: 2022-04-12 - Earliest claimed: 2019-08-21 - Assignees: Hexcel Corporation - Applicants: Hexcel Corporation - Inventors: Peter Andrew Ferrin; Devon Cadwaladar Todd Thomas - Web page: https://patentgrep.com/patent/US11299824B2 ## CPC - D01F 9/22: from polyacrylonitriles - D01F 9/225: {from stabilised polyacrylonitriles} - C01B 32/05: Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30 - D01D 10/02: Heat treatment (heating for finishing D02J13/00) - D01F 6/18: from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide - D01F 9/328: {for manufacturing filaments from polyaddition, polycondensation, or polymerisation products} - D01F: CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - D01D: MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS ## Abstract A method for making carbon fiber in which the tensile strength of carbon fiber is increased without dehumidifying the ambient air that enters every oxidation oven in a multiple oxidation oven system. A positive effect on tensile strength is provided when ambient air entering only the first oven in a series of oxidation ovens is dehumidified. In addition, the ambient air entering the last oven is not dehumidified when one or more of the preceding oxidation ovens is operated with dehumidified air. ## Claims ### Claim 1 A method for making carbon fiber from a precursor fiber wherein the precursor fiber is subjected to an oxidation treatment in a plurality of oxidation ovens to form an oxidized fiber, said oxidized fiber then being subjected to a carbonization treatment to form said carbon fiber, said plurality of oxidation ovens being surrounded by ambient air which has an ambient air humidity of from 2 to 10 grams of water per kilogram of air and wherein said oxidation treatment comprises the steps of: providing at least a first oxidation oven that defines a first oxidation zone having a first oxidation zone atmosphere comprising first oxidation air which enters said first oxidation zone via one or more first oxidation air entrances, said first oxidation zone atmosphere having a first oxidation atmosphere, humidity wherein said first oxidation air comprises dehumidified ambient air such that said first oxidation atmosphere humidity is from 1 to 3 grams of water per kilogram of air and wherein said first oxidation atmosphere humidity is at least 1 gram of water per kilogram of air less than said ambient air humidity and wherein the temperature or temperatures within said first oxidation zone fall within a first oxidation zone temperature range; passing said precursor fiber through said first oxidation zone to form a partially oxidized fiber; providing a final oxidation oven that defines a final oxidation zone having a final oxidation zone atmosphere comprising said ambient air which enters said final oxidation zone via one or more ambient air entrances wherein the temperature or temperatures within said final oxidation zone fall within a final oxidation zone temperature range which is higher than said first oxidation zone temperature range; passing said partially oxidized fiber through said final oxidation zone to form said oxidized fiber. ### Claim 2 (depends on 1) The method for making a carbon fiber according to claim 1 wherein said precursor fiber is a polyacrylonitrile fiber. ### Claim 3 (depends on 1) The method for making a carbon fiber according to claim 1 wherein said first oxidation zone temperature or temperatures are in the range of from 200° C. to 300° C. and wherein said final oxidation zone temperature or temperatures are in the range of from 200° C. to 300° C. ### Claim 4 (depends on 1) The method for making a carbon fiber according to claim 1 wherein the speed at which said precursor fiber is passed through said first oxidation zone is such that the residence time of said precursor fiber within said first oxidation zone is from 10 minutes to 40 minutes and wherein the speed at which said partially oxidized fiber is passed through said final oxidation zone is such that the residence time of said partially oxidized fiber within said final oxidation zone is from 10 minutes to 40 minutes. ### Claim 5 (depends on 1) The method for making a carbon fiber according to claim 1 wherein said ambient air has an ambient air humidity of from 2 to 4 grams of water per kilogram of air. ### Claim 6 (depends on 1) The method for making a carbon fiber according to claim 1 wherein said final oxidation zone comprises a first temperature sub-zone and a second temperature sub-zone wherein said precursor fiber is passed through said first temperature sub-zone of the final oxidation zone before being passed through said second temperature sub-zone of the final oxidation zone and wherein the temperature in said second temperature sub-zone is higher than the temperature in said first temperature subzone. ### Claim 7 (depends on 1) The method for making a carbon fiber according to claim 1 wherein said first oxidation zone comprises a first temperature sub-zone and a second temperature sub-zone wherein said precursor fiber is passed through said first temperature sub-zone of the first oxidation zone before being passed through said second temperature sub-zone of the first oxidation zone and wherein the temperature in said second temperature sub-zone is higher than the temperature in said first temperature subzone. ### Claim 8 (depends on 7) The method for making a carbon fiber according to claim 7 wherein said final oxidation zone comprises a first temperature sub-zone and a second temperature sub-zone wherein said precursor fiber is passed through said first temperature sub-zone of the final oxidation zone before being passed through said second temperature sub-zone of the final oxidation zone and wherein the temperature in said second temperature sub-zone of the final oxidation zone is higher than the temperature in said first temperature subzone of the final oxidation zone. ### Claim 9 (depends on 7) The method for making a carbon fiber according to claim 7 wherein the temperature in said second temperature sub-zone is from 1° C. to 10° C. higher than the temperature in said first temperature sub-zone. ### Claim 10 (depends on 1) The method for making a carbon fiber according to claim 1 wherein at least a second oxidation oven is provided that defines a second oxidation zone wherein the temperature or temperatures in said second oxidation zone fall within a second oxidation zone temperature range which is higher than said first oxidation zone temperature range and lower than said final oxidation zone temperature range, said second oxidation zone having a second oxidation zone atmosphere comprising second oxidation air wherein said second oxidation air enters said second oxidation zone via one or more second oxidation air entrances, said second oxidation zone atmosphere having a second oxidation atmosphere humidity wherein said second oxidation air comprises dehumidified ambient air such that said second oxidation atmosphere humidity is from 1 to 3 grams of water per kilogram of air and wherein said second oxidation atmosphere humidity is at least 1 gram of water per kilogram of air less than said ambient air humidity and wherein said partially oxidized fiber is passed through said second oxidation zone to form a first further oxidized fiber, said first further oxidized fiber being passed through said final oxidation zone to form said oxidized fiber. ### Claim 11 (depends on 10) The method for making a carbon fiber according to claim 10 wherein said first oxidation zone temperature or temperatures, said second oxidation zone temperature or temperatures and said final oxidation zone temperature or temperatures are all in the range of from 200° C. to 300° C. ### Claim 12 (depends on 10) The method for making a carbon fiber according to claim 10 wherein the speed at which said precursor fiber is passed through said first oxidation zone is such that the residence time of said precursor fiber within said first oxidation zone is from 10 minutes to 40 minutes, wherein the speed at which said partially oxidized fiber is passed through said second oxidation zone is such that the residence time of said partially oxidized fiber within said second oxidation zone is from 10 minutes to 40 minutes and wherein the speed at which said first further oxidized fiber is passed through said final oxidation zone is such that the residence time of said first further oxidized fiber within said final oxidation zone is from 10 minutes to 40 minutes. ### Claim 13 (depends on 10) The method for making a carbon fiber according to claim 10 wherein said ambient air has an ambient air humidity of from 2 to 4 grams of water per kilogram of air. ### Claim 14 (depends on 10) The method for making a carbon fiber according to claim 10 wherein at least a third oxidation oven is provided that defines a third oxidation zone wherein the temperature or temperatures in said third oxidation zone fall within a third oxidation zone temperature range which is higher than said second oxidation zone temperature range and lower than said final oxidation zone temperature range, said third oxidation zone having a third oxidation zone atmosphere comprising third oxidation air wherein said third oxidation air enters said third oxidation zone via one or more third oxidation air entrances, said third oxidation zone atmosphere having a third oxidation atmosphere humidity wherein said third oxidation air comprises dehumidified ambient air such that said third oxidation atmosphere humidity is from 1 to 3 grams of water per kilogram of air and wherein said third oxidation atmosphere humidity is at least 1 gram of water per kilogram of air less than said ambient air humidity and wherein said first further oxidized fiber is passed through said third oxidation zone to form a second further oxidized fiber, said second further oxidized fiber being passed through said final oxidation zone to form said oxidized fiber. ### Claim 15 (depends on 14) The method for making a carbon fiber according to claim 14 wherein said first oxidation zone temperature or temperatures, said second oxidation zone temperature or temperatures, said third oxidation zone temperature or temperatures and said final oxidation zone temperature or temperatures are all in the range of from 200° C. to 300° C. ### Claim 16 (depends on 14) The method for making a carbon fiber according to claim 14 wherein the speed at which said precursor fiber is passed through said first oxidation zone is such that the residence time of said precursor fiber within said first oxidation zone is from 10 minutes to 40 minutes, wherein the speed at which said partially oxidized fiber is passed through said second oxidation zone is such that the residence time of said partially oxidized fiber within said second oxidation zone is from 10 minutes to 40 minutes, wherein the speed at which said first further oxidized fiber is passed through said third oxidation zone is such that the residence time of said first further oxidized fiber within said third oxidation zone is from 10 minutes to 40 minutes and wherein the speed at which said second further oxidized fiber is passed through said final oxidation zone is such that the residence time of said second further oxidized fiber within said final oxidation zone is from 10 minutes to 40 minutes. ### Claim 17 (depends on 14) The method for making a carbon fiber according to claim 14 wherein said ambient air has an ambient air humidity of from 2 to 4 grams of water per kilogram of air.