Patent
US 10,811,736PROCESS FOR RECYCLING GRAPHENE FROM AN ELECTRODE MATERIAL
Nicolas DELAPORTE
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 10,811,736Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a schematic illustration of the method for recycling graphene-based electrodes according to one embodiment of the present technology.
Figure 2 is a photograph showing the separation of graphene from a LTO powder according to one embodiment.
Figure 3 shows thermogravimetric curves of a LiFePO 4/C (LFP) powder and a graphene (EG) powder.
Figure 4 shows thermogravimetric curves of a graphene powder before (EG) and after (recycled EG) applying the recycling method according to one embodiment.
Figure 5 shows X-ray diffraction patterns of a) a self-standing graphene layer, b) a layer of recycled graphene according to one embodiment on a Celgard ® separator, c) an oxide layer on a Celgard ® separator, and d) a Celgard ® separator alone. The peaks assigned to the oxide particles are …
Figure 6 shows Scanning Electron Microscopy (SEM) images of the recycled graphene layer according to one embodiment and obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. The circles indicate possible residual oxide particles.
Figure 7 shows SEM images of the oxide film deposited on a Celgard ® separator, obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. An optical photograph of the oxide film is also provided.
Figure 8 shows the specific charge (squares) and discharge (circles) capacities of a self- standing graphene electrode cycled at rates ranging from 50 to 1000 mA/g.
Figure 9 shows the specific charge (squares) and discharge (circles) capacities of a recycled graphene anode cycled at rates ranging from 50 to 1000 mA/g.
Figure 10 shows SEM images of a self-standing graphene layer obtained at a) 250X, b) 1000X and c) 5000X.
Figure 11 shows charge/discharge profiles at rates ranging from 50 to 1000 mA/g for a self-standing graphene electrode, where the second cycle for each current density is represented.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A process for recycling an electrode material comprising graphene and an electrochemically active material, the process comprising the steps of: adding, in any order, water and a nonmiscible solvent to the electrode material, thereby forming a biphasic system comprising an organic phase and an aqueous phase; and separating the organic layer and the aqueous phase; and filtering the organic phase to recover graphene. Original
The process of claim 1, wherein the non-miscible solvent is a carbonate ester. Original
The process of claim 1, wherein the biphasic system has a water/solvent ratio comprised between about 3:1 and about 1:2. Currently amended
The process of ' claim 1, wherein step (ii) further comprises washing the organic phase with deionized water prior to the filtration step (iii) to remove residual traces of electrochemically active material. Currently amended
The process of claim 1, the process further comprising, before step (i), steps of washing the electrode material using a solvent to obtain a suspension of graphene and electrochemically active material, and of filtering of said suspension. Currently amended
The process of claim 1, further comprising, before step (i), a thermal treatment step performed at a temperature of between about 400 ° C and about 550 ° C for at least 20 minutes. Currently amended
The process of claim 1, wherein the electrochemically active material is selected from TiO 2, Li 2 TiO 3, Li 4 Ti 5 O 12, H 2 Ti 5 O 11 and H 2 Ti 4 O 9, or a combination thereof, LiM'P 0 4 wherein M' is Fe, Ni, Mn, Co, or a combination thereof, LiV 3 0 8, V 2 0 5, LiMn 2 0 4, LiM" 0 2, wherein M" is Mn, C o, Ni, or a combination thereof, Li(NiM"') 0 2, wherein M"' is Mn, C o, A l, Fe, Cr, Ti, or Zr, and combinations thereof. Currently amended
The process of claim 1, wherein the electrochemically active material is a lithium titanate or a lithium metal phosphate. Currently amended
The process of ' claim 1, further comprising steps of separating the aqueous phase and of regenerating the electrochemically active material. Currently amended
The process of claim, further comprising an additional washing step with a solvent after the filtration step. Currently amended
The process of claim, further comprising a pre- drying step before the thermal treatment step. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material
Preparation of graphene-based electrode and electrochemical cell (text truncated in source document).
Materials described outside the worked examples.
electrochemically active material
water
H₂O
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 6 shows Scanning Electron Microscopy (SEM) images of the recycled graphene layer according to one embodiment and obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. The circles indicate possible residual oxide particles.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0.01–1.5 V | — |
Temperature |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,811,736Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a schematic illustration of the method for recycling graphene-based electrodes according to one embodiment of the present technology.
Figure 2 is a photograph showing the separation of graphene from a LTO powder according to one embodiment.
Figure 3 shows thermogravimetric curves of a LiFePO 4/C (LFP) powder and a graphene (EG) powder.
Figure 4 shows thermogravimetric curves of a graphene powder before (EG) and after (recycled EG) applying the recycling method according to one embodiment.
Figure 5 shows X-ray diffraction patterns of a) a self-standing graphene layer, b) a layer of recycled graphene according to one embodiment on a Celgard ® separator, c) an oxide layer on a Celgard ® separator, and d) a Celgard ® separator alone. The peaks assigned to the oxide particles are …
Figure 6 shows Scanning Electron Microscopy (SEM) images of the recycled graphene layer according to one embodiment and obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. The circles indicate possible residual oxide particles.
Figure 7 shows SEM images of the oxide film deposited on a Celgard ® separator, obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. An optical photograph of the oxide film is also provided.
Figure 8 shows the specific charge (squares) and discharge (circles) capacities of a self- standing graphene electrode cycled at rates ranging from 50 to 1000 mA/g.
Figure 9 shows the specific charge (squares) and discharge (circles) capacities of a recycled graphene anode cycled at rates ranging from 50 to 1000 mA/g.
Figure 10 shows SEM images of a self-standing graphene layer obtained at a) 250X, b) 1000X and c) 5000X.
Figure 11 shows charge/discharge profiles at rates ranging from 50 to 1000 mA/g for a self-standing graphene electrode, where the second cycle for each current density is represented.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A process for recycling an electrode material comprising graphene and an electrochemically active material, the process comprising the steps of: adding, in any order, water and a nonmiscible solvent to the electrode material, thereby forming a biphasic system comprising an organic phase and an aqueous phase; and separating the organic layer and the aqueous phase; and filtering the organic phase to recover graphene. Original
The process of claim 1, wherein the non-miscible solvent is a carbonate ester. Original
The process of claim 1, wherein the biphasic system has a water/solvent ratio comprised between about 3:1 and about 1:2. Currently amended
The process of ' claim 1, wherein step (ii) further comprises washing the organic phase with deionized water prior to the filtration step (iii) to remove residual traces of electrochemically active material. Currently amended
The process of claim 1, the process further comprising, before step (i), steps of washing the electrode material using a solvent to obtain a suspension of graphene and electrochemically active material, and of filtering of said suspension. Currently amended
The process of claim 1, further comprising, before step (i), a thermal treatment step performed at a temperature of between about 400 ° C and about 550 ° C for at least 20 minutes. Currently amended
The process of claim 1, wherein the electrochemically active material is selected from TiO 2, Li 2 TiO 3, Li 4 Ti 5 O 12, H 2 Ti 5 O 11 and H 2 Ti 4 O 9, or a combination thereof, LiM'P 0 4 wherein M' is Fe, Ni, Mn, Co, or a combination thereof, LiV 3 0 8, V 2 0 5, LiMn 2 0 4, LiM" 0 2, wherein M" is Mn, C o, Ni, or a combination thereof, Li(NiM"') 0 2, wherein M"' is Mn, C o, A l, Fe, Cr, Ti, or Zr, and combinations thereof. Currently amended
The process of claim 1, wherein the electrochemically active material is a lithium titanate or a lithium metal phosphate. Currently amended
The process of ' claim 1, further comprising steps of separating the aqueous phase and of regenerating the electrochemically active material. Currently amended
The process of claim, further comprising an additional washing step with a solvent after the filtration step. Currently amended
The process of claim, further comprising a pre- drying step before the thermal treatment step. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material
Preparation of graphene-based electrode and electrochemical cell (text truncated in source document).
Materials described outside the worked examples.
electrochemically active material
water
H₂O
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 6 shows Scanning Electron Microscopy (SEM) images of the recycled graphene layer according to one embodiment and obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. The circles indicate possible residual oxide particles.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0.01–1.5 V | — |
Temperature |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,811,736Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a schematic illustration of the method for recycling graphene-based electrodes according to one embodiment of the present technology.
Figure 2 is a photograph showing the separation of graphene from a LTO powder according to one embodiment.
Figure 3 shows thermogravimetric curves of a LiFePO 4/C (LFP) powder and a graphene (EG) powder.
Figure 4 shows thermogravimetric curves of a graphene powder before (EG) and after (recycled EG) applying the recycling method according to one embodiment.
Figure 5 shows X-ray diffraction patterns of a) a self-standing graphene layer, b) a layer of recycled graphene according to one embodiment on a Celgard ® separator, c) an oxide layer on a Celgard ® separator, and d) a Celgard ® separator alone. The peaks assigned to the oxide particles are …
Figure 6 shows Scanning Electron Microscopy (SEM) images of the recycled graphene layer according to one embodiment and obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. The circles indicate possible residual oxide particles.
Figure 7 shows SEM images of the oxide film deposited on a Celgard ® separator, obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. An optical photograph of the oxide film is also provided.
Figure 8 shows the specific charge (squares) and discharge (circles) capacities of a self- standing graphene electrode cycled at rates ranging from 50 to 1000 mA/g.
Figure 9 shows the specific charge (squares) and discharge (circles) capacities of a recycled graphene anode cycled at rates ranging from 50 to 1000 mA/g.
Figure 10 shows SEM images of a self-standing graphene layer obtained at a) 250X, b) 1000X and c) 5000X.
Figure 11 shows charge/discharge profiles at rates ranging from 50 to 1000 mA/g for a self-standing graphene electrode, where the second cycle for each current density is represented.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A process for recycling an electrode material comprising graphene and an electrochemically active material, the process comprising the steps of: adding, in any order, water and a nonmiscible solvent to the electrode material, thereby forming a biphasic system comprising an organic phase and an aqueous phase; and separating the organic layer and the aqueous phase; and filtering the organic phase to recover graphene. Original
The process of claim 1, wherein the non-miscible solvent is a carbonate ester. Original
The process of claim 1, wherein the biphasic system has a water/solvent ratio comprised between about 3:1 and about 1:2. Currently amended
The process of ' claim 1, wherein step (ii) further comprises washing the organic phase with deionized water prior to the filtration step (iii) to remove residual traces of electrochemically active material. Currently amended
The process of claim 1, the process further comprising, before step (i), steps of washing the electrode material using a solvent to obtain a suspension of graphene and electrochemically active material, and of filtering of said suspension. Currently amended
The process of claim 1, further comprising, before step (i), a thermal treatment step performed at a temperature of between about 400 ° C and about 550 ° C for at least 20 minutes. Currently amended
The process of claim 1, wherein the electrochemically active material is selected from TiO 2, Li 2 TiO 3, Li 4 Ti 5 O 12, H 2 Ti 5 O 11 and H 2 Ti 4 O 9, or a combination thereof, LiM'P 0 4 wherein M' is Fe, Ni, Mn, Co, or a combination thereof, LiV 3 0 8, V 2 0 5, LiMn 2 0 4, LiM" 0 2, wherein M" is Mn, C o, Ni, or a combination thereof, Li(NiM"') 0 2, wherein M"' is Mn, C o, A l, Fe, Cr, Ti, or Zr, and combinations thereof. Currently amended
The process of claim 1, wherein the electrochemically active material is a lithium titanate or a lithium metal phosphate. Currently amended
The process of ' claim 1, further comprising steps of separating the aqueous phase and of regenerating the electrochemically active material. Currently amended
The process of claim, further comprising an additional washing step with a solvent after the filtration step. Currently amended
The process of claim, further comprising a pre- drying step before the thermal treatment step. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material
Preparation of graphene-based electrode and electrochemical cell (text truncated in source document).
Materials described outside the worked examples.
electrochemically active material
water
H₂O
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 6 shows Scanning Electron Microscopy (SEM) images of the recycled graphene layer according to one embodiment and obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. The circles indicate possible residual oxide particles.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0.01–1.5 V | — |
Temperature |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 10,811,736Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a schematic illustration of the method for recycling graphene-based electrodes according to one embodiment of the present technology.
Figure 2 is a photograph showing the separation of graphene from a LTO powder according to one embodiment.
Figure 3 shows thermogravimetric curves of a LiFePO 4/C (LFP) powder and a graphene (EG) powder.
Figure 4 shows thermogravimetric curves of a graphene powder before (EG) and after (recycled EG) applying the recycling method according to one embodiment.
Figure 5 shows X-ray diffraction patterns of a) a self-standing graphene layer, b) a layer of recycled graphene according to one embodiment on a Celgard ® separator, c) an oxide layer on a Celgard ® separator, and d) a Celgard ® separator alone. The peaks assigned to the oxide particles are …
Figure 6 shows Scanning Electron Microscopy (SEM) images of the recycled graphene layer according to one embodiment and obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. The circles indicate possible residual oxide particles.
Figure 7 shows SEM images of the oxide film deposited on a Celgard ® separator, obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. An optical photograph of the oxide film is also provided.
Figure 8 shows the specific charge (squares) and discharge (circles) capacities of a self- standing graphene electrode cycled at rates ranging from 50 to 1000 mA/g.
Figure 9 shows the specific charge (squares) and discharge (circles) capacities of a recycled graphene anode cycled at rates ranging from 50 to 1000 mA/g.
Figure 10 shows SEM images of a self-standing graphene layer obtained at a) 250X, b) 1000X and c) 5000X.
Figure 11 shows charge/discharge profiles at rates ranging from 50 to 1000 mA/g for a self-standing graphene electrode, where the second cycle for each current density is represented.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A process for recycling an electrode material comprising graphene and an electrochemically active material, the process comprising the steps of: adding, in any order, water and a nonmiscible solvent to the electrode material, thereby forming a biphasic system comprising an organic phase and an aqueous phase; and separating the organic layer and the aqueous phase; and filtering the organic phase to recover graphene. Original
The process of claim 1, wherein the non-miscible solvent is a carbonate ester. Original
The process of claim 1, wherein the biphasic system has a water/solvent ratio comprised between about 3:1 and about 1:2. Currently amended
The process of ' claim 1, wherein step (ii) further comprises washing the organic phase with deionized water prior to the filtration step (iii) to remove residual traces of electrochemically active material. Currently amended
The process of claim 1, the process further comprising, before step (i), steps of washing the electrode material using a solvent to obtain a suspension of graphene and electrochemically active material, and of filtering of said suspension. Currently amended
The process of claim 1, further comprising, before step (i), a thermal treatment step performed at a temperature of between about 400 ° C and about 550 ° C for at least 20 minutes. Currently amended
The process of claim 1, wherein the electrochemically active material is selected from TiO 2, Li 2 TiO 3, Li 4 Ti 5 O 12, H 2 Ti 5 O 11 and H 2 Ti 4 O 9, or a combination thereof, LiM'P 0 4 wherein M' is Fe, Ni, Mn, Co, or a combination thereof, LiV 3 0 8, V 2 0 5, LiMn 2 0 4, LiM" 0 2, wherein M" is Mn, C o, Ni, or a combination thereof, Li(NiM"') 0 2, wherein M"' is Mn, C o, A l, Fe, Cr, Ti, or Zr, and combinations thereof. Currently amended
The process of claim 1, wherein the electrochemically active material is a lithium titanate or a lithium metal phosphate. Currently amended
The process of ' claim 1, further comprising steps of separating the aqueous phase and of regenerating the electrochemically active material. Currently amended
The process of claim, further comprising an additional washing step with a solvent after the filtration step. Currently amended
The process of claim, further comprising a pre- drying step before the thermal treatment step. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
1 material
Preparation of graphene-based electrode and electrochemical cell (text truncated in source document).
Materials described outside the worked examples.
electrochemically active material
water
H₂O
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
Figure 6 shows Scanning Electron Microscopy (SEM) images of the recycled graphene layer according to one embodiment and obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. The circles indicate possible residual oxide particles.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Voltage | 0.01–1.5 V | — |
Temperature |
Related documents with shared materials, methods, properties, or citations.
carbonate ester
diethyl carbonate
dimethyl carbonate
ethyl methyl carbonate
titanium dioxide
TiO₂
lithium metatitanate
Li₂TiO₃
lithium titanate
Li₄Ti₅O₁₂
hydrogen titanate
H₂Ti₅O₁₁
hydrogen titanate
H₂Ti₄O₉
lithium metal phosphate
LiM'PO₄
lithium vanadium oxide
LiV₃O₈
vanadium pentoxide
V₂O₅
lithium manganese oxide
LiMn₂O₄
lithium metal oxide
LiM''O₂
lithium titanate
lithium metal phosphate
lithium iron phosphate
LiFePO₄
carbon-coated lithium iron phosphate
LiFePO₄/C
Figure 7 shows SEM images of the oxide film deposited on a Celgard ® separator, obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. An optical photograph of the oxide film is also provided.
Figure 10 shows SEM images of a self-standing graphene layer obtained at a) 250X, b) 1000X and c) 5000X.
Figure 11 shows charge/discharge profiles at rates ranging from 50 to 1000 mA/g for a self-standing graphene electrode, where the second cycle for each current density is represented.
| 30–1000 °C |
| — |
Duration | 20–60 minutes | — |
Duration | ≥ 20 minutes | — |
Temperature | 400–550 °C | — |
GRAPHENE OXIDE-BASED POROUS 3D MESH
carbonate ester
diethyl carbonate
dimethyl carbonate
ethyl methyl carbonate
titanium dioxide
TiO₂
lithium metatitanate
Li₂TiO₃
lithium titanate
Li₄Ti₅O₁₂
hydrogen titanate
H₂Ti₅O₁₁
hydrogen titanate
H₂Ti₄O₉
lithium metal phosphate
LiM'PO₄
lithium vanadium oxide
LiV₃O₈
vanadium pentoxide
V₂O₅
lithium manganese oxide
LiMn₂O₄
lithium metal oxide
LiM''O₂
lithium titanate
lithium metal phosphate
lithium iron phosphate
LiFePO₄
carbon-coated lithium iron phosphate
LiFePO₄/C
Figure 7 shows SEM images of the oxide film deposited on a Celgard ® separator, obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. An optical photograph of the oxide film is also provided.
Figure 10 shows SEM images of a self-standing graphene layer obtained at a) 250X, b) 1000X and c) 5000X.
Figure 11 shows charge/discharge profiles at rates ranging from 50 to 1000 mA/g for a self-standing graphene electrode, where the second cycle for each current density is represented.
| 30–1000 °C |
| — |
Duration | 20–60 minutes | — |
Duration | ≥ 20 minutes | — |
Temperature | 400–550 °C | — |
GRAPHENE OXIDE-BASED POROUS 3D MESH
carbonate ester
diethyl carbonate
dimethyl carbonate
ethyl methyl carbonate
titanium dioxide
TiO₂
lithium metatitanate
Li₂TiO₃
lithium titanate
Li₄Ti₅O₁₂
hydrogen titanate
H₂Ti₅O₁₁
hydrogen titanate
H₂Ti₄O₉
lithium metal phosphate
LiM'PO₄
lithium vanadium oxide
LiV₃O₈
vanadium pentoxide
V₂O₅
lithium manganese oxide
LiMn₂O₄
lithium metal oxide
LiM''O₂
lithium titanate
lithium metal phosphate
lithium iron phosphate
LiFePO₄
carbon-coated lithium iron phosphate
LiFePO₄/C
Figure 7 shows SEM images of the oxide film deposited on a Celgard ® separator, obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. An optical photograph of the oxide film is also provided.
Figure 10 shows SEM images of a self-standing graphene layer obtained at a) 250X, b) 1000X and c) 5000X.
Figure 11 shows charge/discharge profiles at rates ranging from 50 to 1000 mA/g for a self-standing graphene electrode, where the second cycle for each current density is represented.
| 30–1000 °C |
| — |
Duration | 20–60 minutes | — |
Duration | ≥ 20 minutes | — |
Temperature | 400–550 °C | — |
GRAPHENE OXIDE-BASED POROUS 3D MESH
carbonate ester
diethyl carbonate
dimethyl carbonate
ethyl methyl carbonate
titanium dioxide
TiO₂
lithium metatitanate
Li₂TiO₃
lithium titanate
Li₄Ti₅O₁₂
hydrogen titanate
H₂Ti₅O₁₁
hydrogen titanate
H₂Ti₄O₉
lithium metal phosphate
LiM'PO₄
lithium vanadium oxide
LiV₃O₈
vanadium pentoxide
V₂O₅
lithium manganese oxide
LiMn₂O₄
lithium metal oxide
LiM''O₂
lithium titanate
lithium metal phosphate
lithium iron phosphate
LiFePO₄
carbon-coated lithium iron phosphate
LiFePO₄/C
Figure 7 shows SEM images of the oxide film deposited on a Celgard ® separator, obtained at: a) 250X, b) 1000X, c) 5000X and d) 10000X. An optical photograph of the oxide film is also provided.
Figure 10 shows SEM images of a self-standing graphene layer obtained at a) 250X, b) 1000X and c) 5000X.
Figure 11 shows charge/discharge profiles at rates ranging from 50 to 1000 mA/g for a self-standing graphene electrode, where the second cycle for each current density is represented.
| 30–1000 °C |
| — |
Duration | 20–60 minutes | — |
Duration | ≥ 20 minutes | — |
Temperature | 400–550 °C | — |