Patent
US 8,641,998Method for Obtaining Graphene Oxide Nanoplatelets and Derived Products, and the Graphene Oxide Nanoplatelets Thus Obtained
César Merino Sanchez
US
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Patent
Atlas literature
Patent
US 8,641,998Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows a diagram of the method for manufacturing carbon nanofilaments, obtained as an intermediate product, and the graphene oxide nanoplatelets according to the current invention. 25
Figure 2 shows a TEM image of the carbon nanofilaments before the heat treatment in step d).
Figure 3 shows a TEM image of the carbon nanofilaments after the heat treatment in step d), showing the polygonal geometry of the carbon nanofilaments, and on the other 30 hand, loops bonding the free edges of neighbouring graphene layers of the carbon nanofilaments.
Figure 4 shows a TEM image of the graphene oxide nanoplatelets obtained, showing their polygonal shape, where the outline of one graphene oxide nanoplatelet has 35 been highlighted with dotted lines.
Figure 5 shows an SAED image of graphene oxide 11 nanoplatelets obtained according to the method of the invention, showing an electron diffraction diagram for a sample of highly crystalline graphene oxide nanoplatelets.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Ce sar MER IN O SANCHEZ et al. Atty. Dkt. 007643.00006 Serial No. 13/150,928 (P 461 US A 01) This Listing of Claims will replace all prior versions, and listings, of claims in the application: LISTI NG OF CLAIMS 1.: A method for obtaining graphene oxide nanoplatelets -and-dei-ved pfreducs, said method comprising the following steps: a) dosing of at least the following compounds: i. a hydrocarbon or mixture of hydrocarbons, ii. a compound of nickel and a compound of sulphur to generate catalytic particles, iii. a car ri er gas, b) placing the dosed compounds listed in step a) inside a furnace with a working temperature of between 900 ° C and 1500 ° C, where a chemical vapour deposition method occurs by a floating catalyst method, c) obtaining an intermediate material comprising carbon nanofilaments, the structure of which comprises a continuous graphitic ribbon where said ribbon comprises a stacking of less than eleven graphene layers spirally rolled around and along a nanofilament main axis, d) heat treatment of the carbon nanofilaments obtained in step c) by exposing them to a temperature comprised between 1500 ° C and 3000 ° C in an inert atmosphere in order to purify, dehydrogenate, defunctionalise and crystallise said nanofilaments to a modified structure in which loops are formed between gr a phene la yers b y carbon-carbon bonds 4he SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.1.svg 0.44 6 Black and white e) chemical etching comprising a phase of liquid phase oxidation of the treated carbon nanofilaments from step d), causing their fragmentation, so that starting the cleaving of said graphene layers, wherein at least part of the carbon-carbon bonds, created in step d) in the form of loops between adjacent graphene spirally rolled layers, are maintained, f) completing the carbon nanofilament cleaving method by a physical method in order to obtain graphene oxide nanoplatelets with the following features: polygonal geometry, Page 2 of 8 Ce sar MER IN O SANCHEZ et al. Atty. Dkt. 007643.00006 Serial No. 13/150,928 (P 461 US A 01) less than six stacked graphene layers, a maximum length comprised between 0.1 g m and 50 gm.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived pfreducs according to claim 1, characterised in that the hydrocarbon used in step a) of the method is methane or a mixture consisting mainly of methane in a percentage of more than 50%.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived pfr-edc according to claim 1, characterised in that the carrier gas used in step a) of the method is hydrogen.
: A method for obtaining graphene oxide nanoplatelets -and-deriv'ed pfreducs according to claim 1, characterised in that once the mixture of the nickel compound and the sulphur compound is in the furnace of step b) they form catalytic particles having a molar ratio of sulphur-nickel within the interval between 1.2 and 3.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived predctt according to claim 1, characterised in that the furnace used in step b) of the method is a vertical furnace.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived predctt according to claim 1, characterised in that the treatment carried out in step d) of the method lasts longer than 15 minutes.
: A method for obtaining graphene oxide nanoplatelets -and-derived pfeduces according to claim 1, characterised in that the liquid phase oxidation carried out in step e) of the method is performed in a dehydrated medium.
: A method for obtaining graphene oxide nanoplatelets -and-der-ved pfreducs according to claim 1, characterised in that the liquid phase oxidation of step e) is preceded by an intercalation step into the graphene layers where said intercalation is performed in an acid medium.
: A method for obtaining graphene oxide nanoplatelets-and -derived preducts according to claim 1, characterised in that the physical method used in step f) for completing the graphene oxide cleaving consists in the application of ultrasound. SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.2.svg 0.16 6.48 Black and white
: A method for obtaining graphene oxide nanoplatelets according to claim 1 or graphene nanoplatelets according to claim and derivative products according to c 10, characterised in that a functionalisation step is performed by bonding a functional group to either the graphene oxide nanoplatelets or to the graphene nanoplatelets.
: A method for obtaining a la y ered substrate, the method comprising performing a deposition, onto the substrate, of the graphene oxide nanoplatelets of claim 1 or the graphene nanoplatelets of claim 10 and derivative roducts accorg to clai 1 r SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.4.svg 0.16 4.38 Black and white
: A method for obtaining graphene -e-d e nanoplatelets and deri-vative preod4s according to claim 10, characterised in that the reduction step consists of a chemical reduction in either a liquid phase or in a vapour phase.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive preod4s according to claim 11, characterised in that the chemical reduction is performed with the addition of ammonia.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive predtts according to claim 11, characterised in that the chemical reduction is performed with the addition of a surfactant.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive predtts according to claim 10, characterised in that the reduction step consists of a thermal reduction by either a high-temperature thermal flash or by progressive heating.
: A method for obtaining graphene -e-x ide nanoplatelets and derivative preduces- according to claim 14, characterised in that the thermal reduction is performed in either a reducing atmosphere or in an inert atmosphere.
: A method for obtaining graphene -e-id e nanoplatelets and derivat-ive preod4s according to claim 10, characterised in that a doping step is performed on the graphene nanoplatelets.
: A method for obtaining a la y ered substrate -gr aphe ne-exide SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.5.svg 0.16 6.25 Black and white deposition is performed by the methods chosen from electrophoresis, immersion, spin coating, doctor blading or inkjet printing.
canceled
Materials described outside the worked examples.
graphene oxide nanoplatelets
carbon nanofilaments
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 shows a TEM image of the carbon nanofilaments before the heat treatment in step d).
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
number of stacked graphene layers in intermediate carbon nanofilaments | — | carbon nanofilaments |
number of stacked graphene layers in graphene oxide nanoplatelets | — |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,641,998Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows a diagram of the method for manufacturing carbon nanofilaments, obtained as an intermediate product, and the graphene oxide nanoplatelets according to the current invention. 25
Figure 2 shows a TEM image of the carbon nanofilaments before the heat treatment in step d).
Figure 3 shows a TEM image of the carbon nanofilaments after the heat treatment in step d), showing the polygonal geometry of the carbon nanofilaments, and on the other 30 hand, loops bonding the free edges of neighbouring graphene layers of the carbon nanofilaments.
Figure 4 shows a TEM image of the graphene oxide nanoplatelets obtained, showing their polygonal shape, where the outline of one graphene oxide nanoplatelet has 35 been highlighted with dotted lines.
Figure 5 shows an SAED image of graphene oxide 11 nanoplatelets obtained according to the method of the invention, showing an electron diffraction diagram for a sample of highly crystalline graphene oxide nanoplatelets.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Ce sar MER IN O SANCHEZ et al. Atty. Dkt. 007643.00006 Serial No. 13/150,928 (P 461 US A 01) This Listing of Claims will replace all prior versions, and listings, of claims in the application: LISTI NG OF CLAIMS 1.: A method for obtaining graphene oxide nanoplatelets -and-dei-ved pfreducs, said method comprising the following steps: a) dosing of at least the following compounds: i. a hydrocarbon or mixture of hydrocarbons, ii. a compound of nickel and a compound of sulphur to generate catalytic particles, iii. a car ri er gas, b) placing the dosed compounds listed in step a) inside a furnace with a working temperature of between 900 ° C and 1500 ° C, where a chemical vapour deposition method occurs by a floating catalyst method, c) obtaining an intermediate material comprising carbon nanofilaments, the structure of which comprises a continuous graphitic ribbon where said ribbon comprises a stacking of less than eleven graphene layers spirally rolled around and along a nanofilament main axis, d) heat treatment of the carbon nanofilaments obtained in step c) by exposing them to a temperature comprised between 1500 ° C and 3000 ° C in an inert atmosphere in order to purify, dehydrogenate, defunctionalise and crystallise said nanofilaments to a modified structure in which loops are formed between gr a phene la yers b y carbon-carbon bonds 4he SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.1.svg 0.44 6 Black and white e) chemical etching comprising a phase of liquid phase oxidation of the treated carbon nanofilaments from step d), causing their fragmentation, so that starting the cleaving of said graphene layers, wherein at least part of the carbon-carbon bonds, created in step d) in the form of loops between adjacent graphene spirally rolled layers, are maintained, f) completing the carbon nanofilament cleaving method by a physical method in order to obtain graphene oxide nanoplatelets with the following features: polygonal geometry, Page 2 of 8 Ce sar MER IN O SANCHEZ et al. Atty. Dkt. 007643.00006 Serial No. 13/150,928 (P 461 US A 01) less than six stacked graphene layers, a maximum length comprised between 0.1 g m and 50 gm.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived pfreducs according to claim 1, characterised in that the hydrocarbon used in step a) of the method is methane or a mixture consisting mainly of methane in a percentage of more than 50%.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived pfr-edc according to claim 1, characterised in that the carrier gas used in step a) of the method is hydrogen.
: A method for obtaining graphene oxide nanoplatelets -and-deriv'ed pfreducs according to claim 1, characterised in that once the mixture of the nickel compound and the sulphur compound is in the furnace of step b) they form catalytic particles having a molar ratio of sulphur-nickel within the interval between 1.2 and 3.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived predctt according to claim 1, characterised in that the furnace used in step b) of the method is a vertical furnace.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived predctt according to claim 1, characterised in that the treatment carried out in step d) of the method lasts longer than 15 minutes.
: A method for obtaining graphene oxide nanoplatelets -and-derived pfeduces according to claim 1, characterised in that the liquid phase oxidation carried out in step e) of the method is performed in a dehydrated medium.
: A method for obtaining graphene oxide nanoplatelets -and-der-ved pfreducs according to claim 1, characterised in that the liquid phase oxidation of step e) is preceded by an intercalation step into the graphene layers where said intercalation is performed in an acid medium.
: A method for obtaining graphene oxide nanoplatelets-and -derived preducts according to claim 1, characterised in that the physical method used in step f) for completing the graphene oxide cleaving consists in the application of ultrasound. SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.2.svg 0.16 6.48 Black and white
: A method for obtaining graphene oxide nanoplatelets according to claim 1 or graphene nanoplatelets according to claim and derivative products according to c 10, characterised in that a functionalisation step is performed by bonding a functional group to either the graphene oxide nanoplatelets or to the graphene nanoplatelets.
: A method for obtaining a la y ered substrate, the method comprising performing a deposition, onto the substrate, of the graphene oxide nanoplatelets of claim 1 or the graphene nanoplatelets of claim 10 and derivative roducts accorg to clai 1 r SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.4.svg 0.16 4.38 Black and white
: A method for obtaining graphene -e-d e nanoplatelets and deri-vative preod4s according to claim 10, characterised in that the reduction step consists of a chemical reduction in either a liquid phase or in a vapour phase.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive preod4s according to claim 11, characterised in that the chemical reduction is performed with the addition of ammonia.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive predtts according to claim 11, characterised in that the chemical reduction is performed with the addition of a surfactant.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive predtts according to claim 10, characterised in that the reduction step consists of a thermal reduction by either a high-temperature thermal flash or by progressive heating.
: A method for obtaining graphene -e-x ide nanoplatelets and derivative preduces- according to claim 14, characterised in that the thermal reduction is performed in either a reducing atmosphere or in an inert atmosphere.
: A method for obtaining graphene -e-id e nanoplatelets and derivat-ive preod4s according to claim 10, characterised in that a doping step is performed on the graphene nanoplatelets.
: A method for obtaining a la y ered substrate -gr aphe ne-exide SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.5.svg 0.16 6.25 Black and white deposition is performed by the methods chosen from electrophoresis, immersion, spin coating, doctor blading or inkjet printing.
canceled
Materials described outside the worked examples.
graphene oxide nanoplatelets
carbon nanofilaments
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 shows a TEM image of the carbon nanofilaments before the heat treatment in step d).
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
number of stacked graphene layers in intermediate carbon nanofilaments | — | carbon nanofilaments |
number of stacked graphene layers in graphene oxide nanoplatelets | — |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,641,998Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows a diagram of the method for manufacturing carbon nanofilaments, obtained as an intermediate product, and the graphene oxide nanoplatelets according to the current invention. 25
Figure 2 shows a TEM image of the carbon nanofilaments before the heat treatment in step d).
Figure 3 shows a TEM image of the carbon nanofilaments after the heat treatment in step d), showing the polygonal geometry of the carbon nanofilaments, and on the other 30 hand, loops bonding the free edges of neighbouring graphene layers of the carbon nanofilaments.
Figure 4 shows a TEM image of the graphene oxide nanoplatelets obtained, showing their polygonal shape, where the outline of one graphene oxide nanoplatelet has 35 been highlighted with dotted lines.
Figure 5 shows an SAED image of graphene oxide 11 nanoplatelets obtained according to the method of the invention, showing an electron diffraction diagram for a sample of highly crystalline graphene oxide nanoplatelets.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Ce sar MER IN O SANCHEZ et al. Atty. Dkt. 007643.00006 Serial No. 13/150,928 (P 461 US A 01) This Listing of Claims will replace all prior versions, and listings, of claims in the application: LISTI NG OF CLAIMS 1.: A method for obtaining graphene oxide nanoplatelets -and-dei-ved pfreducs, said method comprising the following steps: a) dosing of at least the following compounds: i. a hydrocarbon or mixture of hydrocarbons, ii. a compound of nickel and a compound of sulphur to generate catalytic particles, iii. a car ri er gas, b) placing the dosed compounds listed in step a) inside a furnace with a working temperature of between 900 ° C and 1500 ° C, where a chemical vapour deposition method occurs by a floating catalyst method, c) obtaining an intermediate material comprising carbon nanofilaments, the structure of which comprises a continuous graphitic ribbon where said ribbon comprises a stacking of less than eleven graphene layers spirally rolled around and along a nanofilament main axis, d) heat treatment of the carbon nanofilaments obtained in step c) by exposing them to a temperature comprised between 1500 ° C and 3000 ° C in an inert atmosphere in order to purify, dehydrogenate, defunctionalise and crystallise said nanofilaments to a modified structure in which loops are formed between gr a phene la yers b y carbon-carbon bonds 4he SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.1.svg 0.44 6 Black and white e) chemical etching comprising a phase of liquid phase oxidation of the treated carbon nanofilaments from step d), causing their fragmentation, so that starting the cleaving of said graphene layers, wherein at least part of the carbon-carbon bonds, created in step d) in the form of loops between adjacent graphene spirally rolled layers, are maintained, f) completing the carbon nanofilament cleaving method by a physical method in order to obtain graphene oxide nanoplatelets with the following features: polygonal geometry, Page 2 of 8 Ce sar MER IN O SANCHEZ et al. Atty. Dkt. 007643.00006 Serial No. 13/150,928 (P 461 US A 01) less than six stacked graphene layers, a maximum length comprised between 0.1 g m and 50 gm.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived pfreducs according to claim 1, characterised in that the hydrocarbon used in step a) of the method is methane or a mixture consisting mainly of methane in a percentage of more than 50%.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived pfr-edc according to claim 1, characterised in that the carrier gas used in step a) of the method is hydrogen.
: A method for obtaining graphene oxide nanoplatelets -and-deriv'ed pfreducs according to claim 1, characterised in that once the mixture of the nickel compound and the sulphur compound is in the furnace of step b) they form catalytic particles having a molar ratio of sulphur-nickel within the interval between 1.2 and 3.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived predctt according to claim 1, characterised in that the furnace used in step b) of the method is a vertical furnace.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived predctt according to claim 1, characterised in that the treatment carried out in step d) of the method lasts longer than 15 minutes.
: A method for obtaining graphene oxide nanoplatelets -and-derived pfeduces according to claim 1, characterised in that the liquid phase oxidation carried out in step e) of the method is performed in a dehydrated medium.
: A method for obtaining graphene oxide nanoplatelets -and-der-ved pfreducs according to claim 1, characterised in that the liquid phase oxidation of step e) is preceded by an intercalation step into the graphene layers where said intercalation is performed in an acid medium.
: A method for obtaining graphene oxide nanoplatelets-and -derived preducts according to claim 1, characterised in that the physical method used in step f) for completing the graphene oxide cleaving consists in the application of ultrasound. SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.2.svg 0.16 6.48 Black and white
: A method for obtaining graphene oxide nanoplatelets according to claim 1 or graphene nanoplatelets according to claim and derivative products according to c 10, characterised in that a functionalisation step is performed by bonding a functional group to either the graphene oxide nanoplatelets or to the graphene nanoplatelets.
: A method for obtaining a la y ered substrate, the method comprising performing a deposition, onto the substrate, of the graphene oxide nanoplatelets of claim 1 or the graphene nanoplatelets of claim 10 and derivative roducts accorg to clai 1 r SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.4.svg 0.16 4.38 Black and white
: A method for obtaining graphene -e-d e nanoplatelets and deri-vative preod4s according to claim 10, characterised in that the reduction step consists of a chemical reduction in either a liquid phase or in a vapour phase.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive preod4s according to claim 11, characterised in that the chemical reduction is performed with the addition of ammonia.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive predtts according to claim 11, characterised in that the chemical reduction is performed with the addition of a surfactant.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive predtts according to claim 10, characterised in that the reduction step consists of a thermal reduction by either a high-temperature thermal flash or by progressive heating.
: A method for obtaining graphene -e-x ide nanoplatelets and derivative preduces- according to claim 14, characterised in that the thermal reduction is performed in either a reducing atmosphere or in an inert atmosphere.
: A method for obtaining graphene -e-id e nanoplatelets and derivat-ive preod4s according to claim 10, characterised in that a doping step is performed on the graphene nanoplatelets.
: A method for obtaining a la y ered substrate -gr aphe ne-exide SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.5.svg 0.16 6.25 Black and white deposition is performed by the methods chosen from electrophoresis, immersion, spin coating, doctor blading or inkjet printing.
canceled
Materials described outside the worked examples.
graphene oxide nanoplatelets
carbon nanofilaments
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 shows a TEM image of the carbon nanofilaments before the heat treatment in step d).
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
number of stacked graphene layers in intermediate carbon nanofilaments | — | carbon nanofilaments |
number of stacked graphene layers in graphene oxide nanoplatelets | — |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 8,641,998Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows a diagram of the method for manufacturing carbon nanofilaments, obtained as an intermediate product, and the graphene oxide nanoplatelets according to the current invention. 25
Figure 2 shows a TEM image of the carbon nanofilaments before the heat treatment in step d).
Figure 3 shows a TEM image of the carbon nanofilaments after the heat treatment in step d), showing the polygonal geometry of the carbon nanofilaments, and on the other 30 hand, loops bonding the free edges of neighbouring graphene layers of the carbon nanofilaments.
Figure 4 shows a TEM image of the graphene oxide nanoplatelets obtained, showing their polygonal shape, where the outline of one graphene oxide nanoplatelet has 35 been highlighted with dotted lines.
Figure 5 shows an SAED image of graphene oxide 11 nanoplatelets obtained according to the method of the invention, showing an electron diffraction diagram for a sample of highly crystalline graphene oxide nanoplatelets.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Ce sar MER IN O SANCHEZ et al. Atty. Dkt. 007643.00006 Serial No. 13/150,928 (P 461 US A 01) This Listing of Claims will replace all prior versions, and listings, of claims in the application: LISTI NG OF CLAIMS 1.: A method for obtaining graphene oxide nanoplatelets -and-dei-ved pfreducs, said method comprising the following steps: a) dosing of at least the following compounds: i. a hydrocarbon or mixture of hydrocarbons, ii. a compound of nickel and a compound of sulphur to generate catalytic particles, iii. a car ri er gas, b) placing the dosed compounds listed in step a) inside a furnace with a working temperature of between 900 ° C and 1500 ° C, where a chemical vapour deposition method occurs by a floating catalyst method, c) obtaining an intermediate material comprising carbon nanofilaments, the structure of which comprises a continuous graphitic ribbon where said ribbon comprises a stacking of less than eleven graphene layers spirally rolled around and along a nanofilament main axis, d) heat treatment of the carbon nanofilaments obtained in step c) by exposing them to a temperature comprised between 1500 ° C and 3000 ° C in an inert atmosphere in order to purify, dehydrogenate, defunctionalise and crystallise said nanofilaments to a modified structure in which loops are formed between gr a phene la yers b y carbon-carbon bonds 4he SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.1.svg 0.44 6 Black and white e) chemical etching comprising a phase of liquid phase oxidation of the treated carbon nanofilaments from step d), causing their fragmentation, so that starting the cleaving of said graphene layers, wherein at least part of the carbon-carbon bonds, created in step d) in the form of loops between adjacent graphene spirally rolled layers, are maintained, f) completing the carbon nanofilament cleaving method by a physical method in order to obtain graphene oxide nanoplatelets with the following features: polygonal geometry, Page 2 of 8 Ce sar MER IN O SANCHEZ et al. Atty. Dkt. 007643.00006 Serial No. 13/150,928 (P 461 US A 01) less than six stacked graphene layers, a maximum length comprised between 0.1 g m and 50 gm.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived pfreducs according to claim 1, characterised in that the hydrocarbon used in step a) of the method is methane or a mixture consisting mainly of methane in a percentage of more than 50%.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived pfr-edc according to claim 1, characterised in that the carrier gas used in step a) of the method is hydrogen.
: A method for obtaining graphene oxide nanoplatelets -and-deriv'ed pfreducs according to claim 1, characterised in that once the mixture of the nickel compound and the sulphur compound is in the furnace of step b) they form catalytic particles having a molar ratio of sulphur-nickel within the interval between 1.2 and 3.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived predctt according to claim 1, characterised in that the furnace used in step b) of the method is a vertical furnace.
: A method for obtaining graphene oxide nanoplatelets -and-de-ived predctt according to claim 1, characterised in that the treatment carried out in step d) of the method lasts longer than 15 minutes.
: A method for obtaining graphene oxide nanoplatelets -and-derived pfeduces according to claim 1, characterised in that the liquid phase oxidation carried out in step e) of the method is performed in a dehydrated medium.
: A method for obtaining graphene oxide nanoplatelets -and-der-ved pfreducs according to claim 1, characterised in that the liquid phase oxidation of step e) is preceded by an intercalation step into the graphene layers where said intercalation is performed in an acid medium.
: A method for obtaining graphene oxide nanoplatelets-and -derived preducts according to claim 1, characterised in that the physical method used in step f) for completing the graphene oxide cleaving consists in the application of ultrasound. SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.2.svg 0.16 6.48 Black and white
: A method for obtaining graphene oxide nanoplatelets according to claim 1 or graphene nanoplatelets according to claim and derivative products according to c 10, characterised in that a functionalisation step is performed by bonding a functional group to either the graphene oxide nanoplatelets or to the graphene nanoplatelets.
: A method for obtaining a la y ered substrate, the method comprising performing a deposition, onto the substrate, of the graphene oxide nanoplatelets of claim 1 or the graphene nanoplatelets of claim 10 and derivative roducts accorg to clai 1 r SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.4.svg 0.16 4.38 Black and white
: A method for obtaining graphene -e-d e nanoplatelets and deri-vative preod4s according to claim 10, characterised in that the reduction step consists of a chemical reduction in either a liquid phase or in a vapour phase.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive preod4s according to claim 11, characterised in that the chemical reduction is performed with the addition of ammonia.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive predtts according to claim 11, characterised in that the chemical reduction is performed with the addition of a surfactant.
: A method for obtaining graphene -exid e nanoplatelets and derivat-ive predtts according to claim 10, characterised in that the reduction step consists of a thermal reduction by either a high-temperature thermal flash or by progressive heating.
: A method for obtaining graphene -e-x ide nanoplatelets and derivative preduces- according to claim 14, characterised in that the thermal reduction is performed in either a reducing atmosphere or in an inert atmosphere.
: A method for obtaining graphene -e-id e nanoplatelets and derivat-ive preod4s according to claim 10, characterised in that a doping step is performed on the graphene nanoplatelets.
: A method for obtaining a la y ered substrate -gr aphe ne-exide SVG 13150928.08-29-2013.HL₅₄₀₂IAPXXIFW1.CLM.5.svg 0.16 6.25 Black and white deposition is performed by the methods chosen from electrophoresis, immersion, spin coating, doctor blading or inkjet printing.
canceled
Materials described outside the worked examples.
graphene oxide nanoplatelets
carbon nanofilaments
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 2 shows a TEM image of the carbon nanofilaments before the heat treatment in step d).
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
number of stacked graphene layers in intermediate carbon nanofilaments | — | carbon nanofilaments |
number of stacked graphene layers in graphene oxide nanoplatelets | — |
Related documents with shared materials, methods, properties, or citations.
nickel compound and sulphur compound catalytic particles
methane
CH₄
hydrogen
H₂
nickel-sulphur catalytic particles
graphene nanoplatelets
ammonia
NH₃
Figure 3 shows a TEM image of the carbon nanofilaments after the heat treatment in step d), showing the polygonal geometry of the carbon nanofilaments, and on the other 30 hand, loops bonding the free edges of neighbouring graphene layers of the carbon nanofilaments.
Figure 4 shows a TEM image of the graphene oxide nanoplatelets obtained, showing their polygonal shape, where the outline of one graphene oxide nanoplatelet has 35 been highlighted with dotted lines.
Figure 5 shows an SAED image of graphene oxide 11 nanoplatelets obtained according to the method of the invention, showing an electron diffraction diagram for a sample of highly crystalline graphene oxide nanoplatelets.
maximum length of graphene oxide nanoplatelets | — | graphene oxide nanoplatelets |
molar ratio sulphur:nickel in catalytic particles | — | nickel-sulphur catalytic particles |
Temperature | 1500–3000 °C | — |
Temperature | 900–1500 °C | — |
Duration | ≥ 15 minutes | — |
nickel compound and sulphur compound catalytic particles
methane
CH₄
hydrogen
H₂
nickel-sulphur catalytic particles
graphene nanoplatelets
ammonia
NH₃
Figure 3 shows a TEM image of the carbon nanofilaments after the heat treatment in step d), showing the polygonal geometry of the carbon nanofilaments, and on the other 30 hand, loops bonding the free edges of neighbouring graphene layers of the carbon nanofilaments.
Figure 4 shows a TEM image of the graphene oxide nanoplatelets obtained, showing their polygonal shape, where the outline of one graphene oxide nanoplatelet has 35 been highlighted with dotted lines.
Figure 5 shows an SAED image of graphene oxide 11 nanoplatelets obtained according to the method of the invention, showing an electron diffraction diagram for a sample of highly crystalline graphene oxide nanoplatelets.
maximum length of graphene oxide nanoplatelets | — | graphene oxide nanoplatelets |
molar ratio sulphur:nickel in catalytic particles | — | nickel-sulphur catalytic particles |
Temperature | 1500–3000 °C | — |
Temperature | 900–1500 °C | — |
Duration | ≥ 15 minutes | — |
nickel compound and sulphur compound catalytic particles
methane
CH₄
hydrogen
H₂
nickel-sulphur catalytic particles
graphene nanoplatelets
ammonia
NH₃
Figure 3 shows a TEM image of the carbon nanofilaments after the heat treatment in step d), showing the polygonal geometry of the carbon nanofilaments, and on the other 30 hand, loops bonding the free edges of neighbouring graphene layers of the carbon nanofilaments.
Figure 4 shows a TEM image of the graphene oxide nanoplatelets obtained, showing their polygonal shape, where the outline of one graphene oxide nanoplatelet has 35 been highlighted with dotted lines.
Figure 5 shows an SAED image of graphene oxide 11 nanoplatelets obtained according to the method of the invention, showing an electron diffraction diagram for a sample of highly crystalline graphene oxide nanoplatelets.
maximum length of graphene oxide nanoplatelets | — | graphene oxide nanoplatelets |
molar ratio sulphur:nickel in catalytic particles | — | nickel-sulphur catalytic particles |
Temperature | 1500–3000 °C | — |
Temperature | 900–1500 °C | — |
Duration | ≥ 15 minutes | — |
nickel compound and sulphur compound catalytic particles
methane
CH₄
hydrogen
H₂
nickel-sulphur catalytic particles
graphene nanoplatelets
ammonia
NH₃
Figure 3 shows a TEM image of the carbon nanofilaments after the heat treatment in step d), showing the polygonal geometry of the carbon nanofilaments, and on the other 30 hand, loops bonding the free edges of neighbouring graphene layers of the carbon nanofilaments.
Figure 4 shows a TEM image of the graphene oxide nanoplatelets obtained, showing their polygonal shape, where the outline of one graphene oxide nanoplatelet has 35 been highlighted with dotted lines.
Figure 5 shows an SAED image of graphene oxide 11 nanoplatelets obtained according to the method of the invention, showing an electron diffraction diagram for a sample of highly crystalline graphene oxide nanoplatelets.
maximum length of graphene oxide nanoplatelets | — | graphene oxide nanoplatelets |
molar ratio sulphur:nickel in catalytic particles | — | nickel-sulphur catalytic particles |
Temperature | 1500–3000 °C | — |
Temperature | 900–1500 °C | — |
Duration | ≥ 15 minutes | — |