# US 10,501,659 B2 · Method of making a fuser member > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,501,659 B2 - Document ID: US10501659B2 - Status: Granted - Kind: B2 - Application number: 14/693,625 - Filed: 2015-04-22 - Published: 2016-10-27 - Granted: 2019-12-10 - Earliest claimed: 2015-04-22 - Assignees: Xerox Corporation - Applicants: Xerox Corporation - Inventors: Matthew M. Kelly; Yu Qi; Timothy L. Harper - Web page: https://patentgrep.com/patent/US10501659B2 ## CPC - C09D 7/61: inorganic - C08J 3/203: {Solid polymers with solid and/or liquid additives} - C08J 3/22: using masterbatch techniques - C08J 3/226: {using a polymer as a carrier} - C09D 7/70: {characterised by shape, e.g. fibres, flakes or microspheres} - C09D 127/12: containing fluorine atoms - C09D 201/04: containing halogen atoms - G03G 15/2057: {relating to the chemical composition of the heat element and layers thereof} - G03G 15/206: {Structural details or chemical composition of the pressure elements and layers thereof} - C08J 2327/12: containing fluorine atoms - C08J 2427/12: containing fluorine atoms - C08K 3/041: {Carbon nanotubes} - C08K 2201/016: Additives defined by their aspect ratio - C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D) - C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29) - G03G: ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY - C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09) ## Abstract Described herein is a method of manufacturing a fuser member. The method includes mixing a high load fluoropolymer/carbon nanotube composition in a high shear mixer. The method includes mixing the high load fluoropolymer/carbon nanotube composition in the high shear mixer for 3 or more times. A fluoropolymer is added to the high load fluoropolymer/carbon nanotube composition to form a low load fluoropolymer/carbon nanotube composition. The low load fluoropolymer/carbon nanotube composition is mixed in a rubber compounding mixer for 3 or more times. The low load fluoropolymer/carbon nanotube composition is coated on a fuser substrate, cured and polished. ## Claims ### Claim 1 A method of making a fuser member suitable for use with an image forming system, comprising: mixing a high load fluoropolymer/carbon nanotube composition wherein the carbon nanotubes comprise from about 8 weight percent to about 30 weight percent of the high load composition in a mixer; mixing the high load fluoropolymer/carbon nanotube composition in a high shear mixer and mixing the high load fluoropolymer/carbon nanotube composition for 3 or more times; adding more of the fluoropolymer to the high load fluoropolymer/carbon nanotube composition to form a low load fluoropolymer/carbon nanotube composition wherein the carbon nanotubes comprise from about 0.1 weight percent to about 7 weight percent of the low load composition; mixing the low load fluoropolymer/carbon nanotube composition in a rubber compounding mixer for 3 or more times; coating the low load fluoropolymer/carbon nanotube composition on an intermediate layer disposed on a fuser substrate; curing the coated low load fluoropolymer/carbon nanotube composition to form a fuser release layer on the fuser substrate; and polishing the fuser release layer to a surface roughness of from about 0.6 microns to about 1.2 microns, wherein the fuser release layer comprises the fluoropolymer, a plurality of the carbon nanotubes, each carbon nanotube having an aspect ratio ranging from about 10 to about 1,000,000, each carbon nanotube having a diameter of from 1 nanometer to about 20 nanometers; and carbon nanotube fluoropolymer clusters having a size ranges from about 5 micron to about 250 micron; and wherein the carbon nanotube fluoropolymer clusters are from about 0.01 volume percent to about 15 volume percent of the surface layer. ### Claim 2 (depends on 1) The method of claim 1, wherein the fluoropolymer comprises a fluoroelastomer selected from the group consisting of copolymers of: vinylidenefluoride, hexafluoropropylene and tetrafluoropropylene and tetrafluoroethylene, terpolymers of vinylidenefluoride, hexafluoropropylene and tetrafluoroethylene, and tetrapolymers of vinylidenefluoride, hexafluoropropylene, tetrafluoroethylene, and a cure site monomer. ### Claim 3 (depends on 1) The method of claim 1, wherein the fluoropolymer comprises a fluoroplastic selected from the group consisting of: polytetrafluoroethylene (PTFE); perfluoroalkoxy polymer resin (PFA); copolymers of tetrafluoroethylene (TFE) and hexafluoropropylene (HFP); copolymers of hexafluoropropylene (HFP) and vinylidene fluoride (VDF or VF2); terpolymers of tetrafluoroethylene (TFE), vinylidene fluoride (VDF), and hexafluoropropylene (HFP); tetrapolymers of tetrafluoroethylene (TFE), vinylidene fluoride (VF2), and hexafluoropropylene (HFP) and a cure site monomer; and mixtures thereof. ### Claim 4 (depends on 1) The method of claim 1, wherein the fluoropolymer comprises a perfluoropolyether. ### Claim 5 (depends on 1) The method of claim 1, wherein the fuser substrate comprises a material selected from the group consisting of: polyimide, polyaramide, polyether ether ketone, polyetherimide, polyphthalamide, polyamide-imide, polyketone, polyphenylene sulfide, fluoropolyimides, fluoropolyurethanes, aluminum, nickel and stainless steel. ### Claim 6 (depends on 1) The method of claim 1, wherein the curing is at a temperature of from about 150° C. to about 360° C. ### Claim 7 (depends on 1) The method of claim 1, wherein the carbon nanotubes are selected from the group consisting of single wall carbon nanotubes or multi-wall carbon nanotubes. ### Claim 8 (depends on 1) The method of claim 1, wherein an organic solvent is added to the low load fluoropolymer/carbon nanotube composition prior to coating. ### Claim 9 (depends on 8) The method of claim 8, wherein the organic solvent is selected from the group consisting of: methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK), methyl-tertbutyl ether (MTBB), methyl n-amyl ketone (MAK), tetrahydrofuran (THF), methyl alcohol, ethyl alcohol, acetone, ethyl acetate, butyl acetate, low molecular weight carbonyls, dimethyl formamide (DMF), dimethyl sulfoxide (DMSO) and N-methyl 2 pyrrolidone (NMP). ### Claim 10 (depends on 1) The method of claim 1, wherein a fluoro-surfactant is added to the low load fluoropolymer/carbon nanotube composition prior to coating. ### Claim 11 A surface layer comprising: a fluoropolymer, a plurality of carbon nanotubes, each carbon nanotube having an aspect ratio ranging from about 10 to about 1,000,000, each carbon nanotube having a diameter of from 1 nanometer to about 20 nanometers; and carbon nanotube fluoropolymer clusters having a size ranges from about 5 micron to about 250 micron; and wherein the carbon nanotube fluoropolymer clusters are from about 0.01 volume percent to about 15 volume percent of the surface layer, wherein the surface layer is formed by mixing a high load fluoropolymer/carbon nanotube composition in a high shear mixer and mixing the high load fluoropolymer/carbon nanotube composition for 3 or more times wherein the high load fluoropolymer/carbon nanotube composition comprises from about 8 weight percent to about 30 weight percent of the high load composition; adding more of the fluoropolymer to the high load fluoropolymer/carbon nanotube composition to form a low load fluoropolymer/carbon nanotube composition wherein the carbon nanotubes comprise from about 0.1 weight percent to about 7 weight percent of the low load composition; mixing the low load fluoropolymer/carbon nanotube composition in a rubber compounding mixer for 3 or more times; and coating the low load composition and curing to form the surface layer, wherein the surface layer has a surface roughness of from about 0.6 microns to about 1.2 microns. ### Claim 12 (depends on 11) The surface layer of claim 11, wherein each of the plurality of carbon nanotubes is selected from the group consisting of: a single wall carbon nanotube (SWCNT), and a multi-wall carbon nanotube (MWCNT). ### Claim 13 (depends on 11) The surface layer of claim 11, wherein an organic solvent is added to the low load composition prior to coating. ### Claim 14 A fuser member comprising: a substrate layer; an intermediate layer disposed on the substrate layer; and a release layer disposed on the intermediate layer, the release layer comprising; a fluoropolymer, a plurality of carbon nanotubes, each carbon nanotube having an aspect ratio ranging from about 10 to about 1,000,000, each carbon nanotube having a diameter of from 1 nanometer to about 20 nanometers; and carbon nanotube fluoropolymer clusters having a size ranges from about 5 micron to about 250 micron; and wherein the carbon nanotube fluoropolymer clusters are from about 0.01 volume percent to about 15 volume percent of the release layer, wherein the release layer is formed by mixing a high load fluoropolymer/carbon nanotube composition in a high shear mixer and mixing the high load fluoropolymer/carbon nanotube composition for 3 or more times wherein the high load fluoropolymer/carbon nanotube composition comprises from about 8 weight percent to about 30 weight percent of the high load composition; adding more of the fluoropolymer to the high load fluoropolymer/carbon nanotube composition to form a low load fluoropolymer/carbon nanotube composition wherein the carbon nanotubes comprise from about 0.1 weight percent to about 7 weight percent of the low load composition; mixing the low load fluoropolymer/carbon nanotube composition in a rubber compounding mixer for 3 or more times; and coating the low load composition and curing to form the release layer, wherein the release layer has a surface roughness of from about 0.6 microns to about 1.2 micron. ### Claim 15 (depends on 14) The fuser member of claim 14 wherein each of the plurality of carbon nanotubes is selected from the group consisting of: a single wall carbon nanotube (SWCNT), and a multi-wall carbon nanotube (MWCNT). ### Claim 16 (depends on 14) The fuser member of claim 14 wherein the release layer has a thermal diffusivity from about 0.01 (mm2/s) to about 0.5 (mm2/s), and a thermal conductivity from about 0.2 W/(m*K) to about 1.0 W/(m*K). ### Claim 17 (depends on 14) The fuser member of claim 14 wherein the release layer has a composite modulus from about 2,000 psi to about 10,000 psi. ### Claim 18 (depends on 14) The fuser member of claim 14 wherein the release layer has a composite toughness from about 2,500 (in.-lbs/in.3) to about 5,000 (in.-lbs/in.3). ### Claim 19 (depends on 14) The fuser member of claim 14 wherein the release layer has a composite tear strength from about 200 (lbs./in.) to about 400 (lbs./in.). ### Claim 20 (depends on 14) The fuser member of claim 14, wherein an organic solvent is added to the low load composition prior to coating.