# US 2014/0154166 A1 · Exfoliation of graphene by multilayer coextrusion > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 2014/0154166 A1 - Document ID: US20140154166A1 - Status: Published application - Kind: A1 - Application number: 14/176,362 - Filed: 2014-02-10 - Published: 2014-06-05 - Earliest claimed: 2010-12-30 - Assignees: Empire Technology Development LLC - Applicants: Empire Technology Development LLC - Inventors: Carlos A. Cruz - Web page: https://patentgrep.com/patent/US20140154166A1 ## CPC - B29C 48/23: with means for avoiding adhesion of the layers, e.g. for forming peelable layers - B29C 48/21: the layers being joined at their surfaces - B29C 48/495: Feedblocks (extrusion moulding of multi-component articles B29C48/16) - B29C 48/71: for layer multiplication (extrusion of multi-component articles B29C48/16) - B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites - B82Y 40/00: Manufacture or treatment of nanostructures - C01B 32/19: by exfoliation - C01B 32/194: After-treatment - B29C 48/08: flexible, e.g. films - B29K 2023/06: {PE, i.e. polyethylene} - B29K 2023/12: {PP, i.e. polypropylene} - B29K 2025/06: {PS, i.e. polystyrene} - B29K 2031/04: {Polymers of vinyl acetate, e.g. PVAc, i.e. polyvinyl acetate} - B29K 2033/12: {Polymers of methacrylic acid esters, e.g. PMMA, i.e. polymethylmethacrylate} - B29K 2995/0093: hydrophobic - B32B 9/007: {comprising carbon, e.g. graphite, composite carbon} - B32B 17/10935: {as a preformed layer, e.g. formed by extrusion} - B32B 37/153: {at least one layer is extruded and immediately laminated while in semi-molten state} - B32B 2264/108: Carbon, e.g. graphite particles - B32B 2313/04: Carbon - Y10T 156/11: Methods of delaminating, per se; i.e. , separating at bonding face - Y10T 156/1116: Using specified organic delamination solvent - Y10T 156/1189: with shearing during delaminating - Y10T 156/1195: Delaminating from release surface - Y10T 156/1972: Shearing delaminating means - B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00) - B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - B29K: INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR {MOULDS, } REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS - B32B: LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract Exfolilation of graphene from graphite using multilayer coextrusion is generally disclosed. In some example embodiments, graphite may be dispersed within a first processing material, and the first processing material and a second processing material may be co-extruded through a plurality of series coupled layer multiplication dies to exfoliate graphene from the graphite. The graphene may be separated from the resulting multi-layered material. In some example embodiments, graphite flake and/or expanded graphite may be dispersed within the first processing material. ## Claims ### Claim 1 An apparatus for producing graphene from graphite, comprising: a multilayer co-extrusion device comprising a plurality of series-coupled layer multiplication dies, the multilayer co-extrusion apparatus being configured to exfoliate graphene by co-extrusion of a first processing material and a second processing material through the plurality of series coupled layer multiplication dies to produce a resulting material including a plurality of alternating layers of the first processing material and the second processing material, the first processing material comprising a first graphite material dispersed in a first substrate, the second processing material comprising a second substrate material. ### Claim 2 (depends on 1) The apparatus of claim 1, wherein the multilayer co-extrusion device is configured for co-extrusion the first processing material and the second processing material, the second processing material comprising a second graphite material dispersed in the second substrate material. ### Claim 3 (depends on 1) The apparatus of claim 1, wherein the multilayer co-extrusion device further comprises: a first extruder configured to supply the first processing material to a feed block, the feed block being fluidicly coupled to the plurality of series coupled layer multiplication dies; and a second extruder configured to supply the second processing material to the feed block. ### Claim 4 (depends on 1) The apparatus of claim 1, wherein the plurality of series coupled layer multiplication dies includes at least 11 series coupled layer multiplication dies. ### Claim 5 (depends on 4) The apparatus of claim 4, wherein the plurality of series coupled layer multiplication dies includes at least 18 series coupled layer multiplication dies. ### Claim 6 A method of producing graphene from graphite, comprising: dispersing a first graphite material in a first substrate material to form a first processing material; and exfoliating graphene from the first graphite material by co-extrusion of the first processing material and a second processing material through one or more layer multiplication dies to yield a resulting material including individual layers of the first processing material interposed between individual layers of the second processing material, the second processing material comprising a second substrate material. ### Claim 7 (depends on 6) The method of claim 6, further comprising: separating the graphene from the first substrate material and the second substrate material. ### Claim 8 (depends on 7) The method of claim 7, separating the graphene comprising dissolving one or more of the first substrate material and/or the second substrate material in a solvent. ### Claim 9 (depends on 8) The method of claim 8, wherein the solvent comprises one or more of water and/or an organic solvent. ### Claim 10 (depends on 6) The method of claim 6, wherein the first substrate material and the second substrate material each comprise one or more of one or more hydrophobic polymers or one or more hydrophilic polymers. ### Claim 11 (depends on 6) The method of claim 6, wherein one of the first substrate material and the second substrate material comprises one or more hydrophobic polymers; and wherein the other of the first substrate material and the second substrate material comprises one or more hydrophilic polymers. ### Claim 12 (depends on 6) The method of claim 6, wherein the one or more layer multiplication dies include at least 11 series coupled dies. ### Claim 13 (depends on 12) The method of claim 12, wherein the resulting material comprises about 4096 of the individual layers of the first processing material and the individual layers of the second processing material. ### Claim 14 (depends on 12) The method of claim 12, wherein the one or more layer multiplication dies include at least 18 series coupled dies. ### Claim 15 (depends on 14) The method of claim 14, wherein the resulting material comprises about 524,288 of the individual layers of the first processing material and the individual layers of the second processing material. ### Claim 16 (depends on 6) The method of claim 6, wherein the first graphite material comprises one or more of graphite flake or expanded graphite. ### Claim 17 (depends on 6) The method of claim 6, further comprising: dispersing a second graphite material in the second substrate material to form the second processing material. ### Claim 18 (depends on 6) The method of claim 6, wherein the co-extrusion comprises one or more of cold extrusion or low temperature extrusion. ### Claim 19 A method of delaminating a multi-sheet substance, comprising: mixing a multi-sheet substance comprising a plurality of stacked sheets with a first substrate material to form a first processing material; delaminating one or more sheets from the multi-sheet substance by application of shear stress to the first processing material; and separating the one or more delaminated sheets from the first substrate material. ### Claim 20 (depends on 19) The method of claim 19, application of shear stress to the first processing material comprising multilayer co-extrusion the first processing material and a second processing material through one or more series coupled layer multiplication dies arranged to produce a resulting material comprising a plurality of alternating layers comprising the first processing material and the second processing material upon co-extrusion of the first processing material and the second processing material therethrough. ### Claim 21 (depends on 19) The method of claim 19, wherein the multi-sheet substance comprises a first graphite material; wherein the one or more delaminated sheets comprise graphene; and wherein the first substrate material comprises one or more of an organic polymer and/or a wax. ### Claim 22 (depends on 21) The method of claim 21, wherein the first graphite material comprises one or more of graphite flake or expanded graphite.