Patent
US 9,309,122Patent
Atlas literature
Patent
US 9,309,122Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Method for producing a dispersion of graphene particles or sheets in a liquid mediu m L, including the following steps: (a) a bar or block (5) of graphite- b ased massive material M is provided; (b) said material M is rubbed on the surface S (2) of a substrate so as to create a trace of friction of said material M on said surface S (2) of said substrate; (c) said substrate is soaked in a liquid medium L (6) and said liquid medium L (6) is subjected to ultrasound in order to obtain a dispersion of graphene particles or sheets in said liquid medium L (6), in which method steps (b) and (c) can be performed at least partially in sequence, or simultaneously.
Method according to claim 1, characterized in that the graphite-based material is chosen from pencil leads, natural graphite a nd synthetic graphite.
Method according to cla i ms 1 to 3, characterized in that it also comprises a step (d) in which any organic or inorganic materials present in said dispersion are separated, preferably by sedimentation or centrifugation, or by chemical dissolution..3 5- 5. Method according to any one of claims 1 to 4, characterized in that it also comprises a step (e) in which said dispersion is red u ced of excessively thick graphite particles and/or graphene sheets that may be present in said dispersion, preferably by sedimentation or by centrifugation.
Method according to any one of claims 1 to 7, characterized in that the thickness of said graphene particles or sheets is between 1 and 50n m and/or the number of parallel graphene sheets is between I and 5 0, preferably between 1 and 30 and even more preferably between 1 and 15. 9, Method according to any one o f claims I to 8, characterized in that the speed o f friction between said material M (5) and said surface S (2) is between 0. 001m.s' and 0.im.s'.
Method according to any one of cla i ms 1 to 9, characterized in that said substrate is selected from the polymers, preferably flexible and/or transparent polymers, glasses, ceramics a n d silicon, 11. Method according to one of claims 1 to 10, in which said surface S (2) of said substrate and said massive material M (5) are in relative movement according to at least two axes, so as to cause a lateral offset between two adjacent segments of traces of said material M (5) on said surface S (2).
Method according to claim 11, in which said substrate is a disk capable of rotating about its axis, and in which the trace of friction of said massive material M (5) on said surface (2) is continuously or periodically offset by lateral displacement means (9) so as to obtain a continuous trace, preferably in the form of a spiral, 13. M ethod according to one of claims 1 to 12, in which steps (b) and (c) are performed simultaneously, and in which at least some of said dispersion is collected periodically or continuously, 14. Method according to one of claims 1 to 13, characterized in that said dispersion is subjected to a s e cond ultrasound tr e atm e nt, preferably with an ultrasound power and/or a duration greater than those in step (c).
Method according to one of claims 1 to 13, characterized in that said dispersion is then subjected to a microwave heating treatment.
Method for preparing graphene particles or sheets, in which a dispersion of graphen e particles or sheets is prepared according to any one of claims 1 to 15, followed by one or more 3i steps in which the graphene particles or sheets are collected from said suspension.
D evice for imple m enting the method according to one of claims 1 to 13, including:-means (3) capable of holding said bar or bloc k (5) of massive material M.-a substrate equipped with a surface S (2) capable of being in contact with said bar or block (5) of massive material M,-means (1) for displacement enabling a relative displacement between said massive material M and said substrate to be generated,-means for regulation and/or control of the pressure force (4) enabling the pressure force between said m assive m aterial M and said surface S of said substrate to be kept constant and/or measured d u ring said relative displacement,-a liquid container (19) enabling the surface S to be at least partially immersed in a liquid phase (6),-a n ultrasound generator (7) enabling said liquid (6) to be subjected to ultrasound,-optionally, drainage means (22) f o r the continuous or periodic drainage of said liquid container (19), in order to collect said liquid phase (6). Claims What is claimed is:
Method according to claim I, characterized in that the liquid phase L (6) is a reducing medium, and advantageously comprises a reducing agent selected from the group consisting of: NaBII14, hydrazine a nd ammoniac.
Method according to any one of claims I to 5, characterized in that it also comprises a step in w hich the graphene sheets are collected from said suspension, and a step of re-dispersing said graphene sheets in a liquid phase.
Method according to any one of claims I to 6, characterized in that said surface S (2) has a roughness of between 0.0 1 p m and I Opm.
, and 34-35 and ADD claims 38-39 as follows.
(Previously Amended) The method of claim 18, wherein at least some of said dispersion is collected one of periodically and continuously.
(Previously Amended) The method of claim 18, further comprising subjecting said dispersion to a second ultrasound treatment for a duration of time which is greater than that of the first ultrasound treatment.
(Previously Added) The method of claim 31, further comprising subjecting said dispersion to a microwave heating treatment after the second ultrasound treatment. unknown
(Previously Amended) The method of claim 18, further comprising collecting the one of said graphene particles and said graphene sheets from said suspension.
A device for producing a dispersion of one of graphene particles and graphene sheets in a liquid medium, the device comprising: means for holding a graphite-based ma ssiv e material includin g at least 10% b y mass of g ra p hite; a substrate equipped with a surface configured for contact with said graphite- based ma ssi ve material; means for enabling a relative displacement between said graphite-based massive material and said substrate; -5- means for one of regulating, controlling and measuring a pressure force between said graphite-based massive material and said surface of said substrate; a liquid container for receiving a liquid and configured to permit at least a partial immersion of said surface of said substrate in said liquid; and an ultrasound generator configured to subject said liquid to ultrasound waves.
The device of claim 34, further comprising[[:]] means for one of a continuous and a periodic drainage of liquid from said liquid.
36-37.. canceled
canceled
(Currently Added) The method of claim 18, wherein the graphite-based material includes at least 50% by mass of graphite. unknown
(Currently Added) The method of claim 18, wherein the graphite-based material includes a geometric shape of a block or a rod. unknown
Layer stacks claimed or described, ordered top of device to substrate.
graphene dispersion production device
No layer stack recorded.
Materials described outside the worked examples.
graphite-based massive material
graphene particles or sheets
Patent
Atlas literature
Patent
US 9,309,122Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Method for producing a dispersion of graphene particles or sheets in a liquid mediu m L, including the following steps: (a) a bar or block (5) of graphite- b ased massive material M is provided; (b) said material M is rubbed on the surface S (2) of a substrate so as to create a trace of friction of said material M on said surface S (2) of said substrate; (c) said substrate is soaked in a liquid medium L (6) and said liquid medium L (6) is subjected to ultrasound in order to obtain a dispersion of graphene particles or sheets in said liquid medium L (6), in which method steps (b) and (c) can be performed at least partially in sequence, or simultaneously.
Method according to claim 1, characterized in that the graphite-based material is chosen from pencil leads, natural graphite a nd synthetic graphite.
Method according to cla i ms 1 to 3, characterized in that it also comprises a step (d) in which any organic or inorganic materials present in said dispersion are separated, preferably by sedimentation or centrifugation, or by chemical dissolution..3 5- 5. Method according to any one of claims 1 to 4, characterized in that it also comprises a step (e) in which said dispersion is red u ced of excessively thick graphite particles and/or graphene sheets that may be present in said dispersion, preferably by sedimentation or by centrifugation.
Method according to any one of claims 1 to 7, characterized in that the thickness of said graphene particles or sheets is between 1 and 50n m and/or the number of parallel graphene sheets is between I and 5 0, preferably between 1 and 30 and even more preferably between 1 and 15. 9, Method according to any one o f claims I to 8, characterized in that the speed o f friction between said material M (5) and said surface S (2) is between 0. 001m.s' and 0.im.s'.
Method according to any one of cla i ms 1 to 9, characterized in that said substrate is selected from the polymers, preferably flexible and/or transparent polymers, glasses, ceramics a n d silicon, 11. Method according to one of claims 1 to 10, in which said surface S (2) of said substrate and said massive material M (5) are in relative movement according to at least two axes, so as to cause a lateral offset between two adjacent segments of traces of said material M (5) on said surface S (2).
Method according to claim 11, in which said substrate is a disk capable of rotating about its axis, and in which the trace of friction of said massive material M (5) on said surface (2) is continuously or periodically offset by lateral displacement means (9) so as to obtain a continuous trace, preferably in the form of a spiral, 13. M ethod according to one of claims 1 to 12, in which steps (b) and (c) are performed simultaneously, and in which at least some of said dispersion is collected periodically or continuously, 14. Method according to one of claims 1 to 13, characterized in that said dispersion is subjected to a s e cond ultrasound tr e atm e nt, preferably with an ultrasound power and/or a duration greater than those in step (c).
Method according to one of claims 1 to 13, characterized in that said dispersion is then subjected to a microwave heating treatment.
Method for preparing graphene particles or sheets, in which a dispersion of graphen e particles or sheets is prepared according to any one of claims 1 to 15, followed by one or more 3i steps in which the graphene particles or sheets are collected from said suspension.
D evice for imple m enting the method according to one of claims 1 to 13, including:-means (3) capable of holding said bar or bloc k (5) of massive material M.-a substrate equipped with a surface S (2) capable of being in contact with said bar or block (5) of massive material M,-means (1) for displacement enabling a relative displacement between said massive material M and said substrate to be generated,-means for regulation and/or control of the pressure force (4) enabling the pressure force between said m assive m aterial M and said surface S of said substrate to be kept constant and/or measured d u ring said relative displacement,-a liquid container (19) enabling the surface S to be at least partially immersed in a liquid phase (6),-a n ultrasound generator (7) enabling said liquid (6) to be subjected to ultrasound,-optionally, drainage means (22) f o r the continuous or periodic drainage of said liquid container (19), in order to collect said liquid phase (6). Claims What is claimed is:
Method according to claim I, characterized in that the liquid phase L (6) is a reducing medium, and advantageously comprises a reducing agent selected from the group consisting of: NaBII14, hydrazine a nd ammoniac.
Method according to any one of claims I to 5, characterized in that it also comprises a step in w hich the graphene sheets are collected from said suspension, and a step of re-dispersing said graphene sheets in a liquid phase.
Method according to any one of claims I to 6, characterized in that said surface S (2) has a roughness of between 0.0 1 p m and I Opm.
, and 34-35 and ADD claims 38-39 as follows.
(Previously Amended) The method of claim 18, wherein at least some of said dispersion is collected one of periodically and continuously.
(Previously Amended) The method of claim 18, further comprising subjecting said dispersion to a second ultrasound treatment for a duration of time which is greater than that of the first ultrasound treatment.
(Previously Added) The method of claim 31, further comprising subjecting said dispersion to a microwave heating treatment after the second ultrasound treatment. unknown
(Previously Amended) The method of claim 18, further comprising collecting the one of said graphene particles and said graphene sheets from said suspension.
A device for producing a dispersion of one of graphene particles and graphene sheets in a liquid medium, the device comprising: means for holding a graphite-based ma ssiv e material includin g at least 10% b y mass of g ra p hite; a substrate equipped with a surface configured for contact with said graphite- based ma ssi ve material; means for enabling a relative displacement between said graphite-based massive material and said substrate; -5- means for one of regulating, controlling and measuring a pressure force between said graphite-based massive material and said surface of said substrate; a liquid container for receiving a liquid and configured to permit at least a partial immersion of said surface of said substrate in said liquid; and an ultrasound generator configured to subject said liquid to ultrasound waves.
The device of claim 34, further comprising[[:]] means for one of a continuous and a periodic drainage of liquid from said liquid.
36-37.. canceled
canceled
(Currently Added) The method of claim 18, wherein the graphite-based material includes at least 50% by mass of graphite. unknown
(Currently Added) The method of claim 18, wherein the graphite-based material includes a geometric shape of a block or a rod. unknown
Layer stacks claimed or described, ordered top of device to substrate.
graphene dispersion production device
No layer stack recorded.
Materials described outside the worked examples.
graphite-based massive material
graphene particles or sheets
Patent
Atlas literature
Patent
US 9,309,122Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Method for producing a dispersion of graphene particles or sheets in a liquid mediu m L, including the following steps: (a) a bar or block (5) of graphite- b ased massive material M is provided; (b) said material M is rubbed on the surface S (2) of a substrate so as to create a trace of friction of said material M on said surface S (2) of said substrate; (c) said substrate is soaked in a liquid medium L (6) and said liquid medium L (6) is subjected to ultrasound in order to obtain a dispersion of graphene particles or sheets in said liquid medium L (6), in which method steps (b) and (c) can be performed at least partially in sequence, or simultaneously.
Method according to claim 1, characterized in that the graphite-based material is chosen from pencil leads, natural graphite a nd synthetic graphite.
Method according to cla i ms 1 to 3, characterized in that it also comprises a step (d) in which any organic or inorganic materials present in said dispersion are separated, preferably by sedimentation or centrifugation, or by chemical dissolution..3 5- 5. Method according to any one of claims 1 to 4, characterized in that it also comprises a step (e) in which said dispersion is red u ced of excessively thick graphite particles and/or graphene sheets that may be present in said dispersion, preferably by sedimentation or by centrifugation.
Method according to any one of claims 1 to 7, characterized in that the thickness of said graphene particles or sheets is between 1 and 50n m and/or the number of parallel graphene sheets is between I and 5 0, preferably between 1 and 30 and even more preferably between 1 and 15. 9, Method according to any one o f claims I to 8, characterized in that the speed o f friction between said material M (5) and said surface S (2) is between 0. 001m.s' and 0.im.s'.
Method according to any one of cla i ms 1 to 9, characterized in that said substrate is selected from the polymers, preferably flexible and/or transparent polymers, glasses, ceramics a n d silicon, 11. Method according to one of claims 1 to 10, in which said surface S (2) of said substrate and said massive material M (5) are in relative movement according to at least two axes, so as to cause a lateral offset between two adjacent segments of traces of said material M (5) on said surface S (2).
Method according to claim 11, in which said substrate is a disk capable of rotating about its axis, and in which the trace of friction of said massive material M (5) on said surface (2) is continuously or periodically offset by lateral displacement means (9) so as to obtain a continuous trace, preferably in the form of a spiral, 13. M ethod according to one of claims 1 to 12, in which steps (b) and (c) are performed simultaneously, and in which at least some of said dispersion is collected periodically or continuously, 14. Method according to one of claims 1 to 13, characterized in that said dispersion is subjected to a s e cond ultrasound tr e atm e nt, preferably with an ultrasound power and/or a duration greater than those in step (c).
Method according to one of claims 1 to 13, characterized in that said dispersion is then subjected to a microwave heating treatment.
Method for preparing graphene particles or sheets, in which a dispersion of graphen e particles or sheets is prepared according to any one of claims 1 to 15, followed by one or more 3i steps in which the graphene particles or sheets are collected from said suspension.
D evice for imple m enting the method according to one of claims 1 to 13, including:-means (3) capable of holding said bar or bloc k (5) of massive material M.-a substrate equipped with a surface S (2) capable of being in contact with said bar or block (5) of massive material M,-means (1) for displacement enabling a relative displacement between said massive material M and said substrate to be generated,-means for regulation and/or control of the pressure force (4) enabling the pressure force between said m assive m aterial M and said surface S of said substrate to be kept constant and/or measured d u ring said relative displacement,-a liquid container (19) enabling the surface S to be at least partially immersed in a liquid phase (6),-a n ultrasound generator (7) enabling said liquid (6) to be subjected to ultrasound,-optionally, drainage means (22) f o r the continuous or periodic drainage of said liquid container (19), in order to collect said liquid phase (6). Claims What is claimed is:
Method according to claim I, characterized in that the liquid phase L (6) is a reducing medium, and advantageously comprises a reducing agent selected from the group consisting of: NaBII14, hydrazine a nd ammoniac.
Method according to any one of claims I to 5, characterized in that it also comprises a step in w hich the graphene sheets are collected from said suspension, and a step of re-dispersing said graphene sheets in a liquid phase.
Method according to any one of claims I to 6, characterized in that said surface S (2) has a roughness of between 0.0 1 p m and I Opm.
, and 34-35 and ADD claims 38-39 as follows.
(Previously Amended) The method of claim 18, wherein at least some of said dispersion is collected one of periodically and continuously.
(Previously Amended) The method of claim 18, further comprising subjecting said dispersion to a second ultrasound treatment for a duration of time which is greater than that of the first ultrasound treatment.
(Previously Added) The method of claim 31, further comprising subjecting said dispersion to a microwave heating treatment after the second ultrasound treatment. unknown
(Previously Amended) The method of claim 18, further comprising collecting the one of said graphene particles and said graphene sheets from said suspension.
A device for producing a dispersion of one of graphene particles and graphene sheets in a liquid medium, the device comprising: means for holding a graphite-based ma ssiv e material includin g at least 10% b y mass of g ra p hite; a substrate equipped with a surface configured for contact with said graphite- based ma ssi ve material; means for enabling a relative displacement between said graphite-based massive material and said substrate; -5- means for one of regulating, controlling and measuring a pressure force between said graphite-based massive material and said surface of said substrate; a liquid container for receiving a liquid and configured to permit at least a partial immersion of said surface of said substrate in said liquid; and an ultrasound generator configured to subject said liquid to ultrasound waves.
The device of claim 34, further comprising[[:]] means for one of a continuous and a periodic drainage of liquid from said liquid.
36-37.. canceled
canceled
(Currently Added) The method of claim 18, wherein the graphite-based material includes at least 50% by mass of graphite. unknown
(Currently Added) The method of claim 18, wherein the graphite-based material includes a geometric shape of a block or a rod. unknown
Layer stacks claimed or described, ordered top of device to substrate.
graphene dispersion production device
No layer stack recorded.
Materials described outside the worked examples.
graphite-based massive material
graphene particles or sheets
Patent
Atlas literature
Patent
US 9,309,122Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
Method for producing a dispersion of graphene particles or sheets in a liquid mediu m L, including the following steps: (a) a bar or block (5) of graphite- b ased massive material M is provided; (b) said material M is rubbed on the surface S (2) of a substrate so as to create a trace of friction of said material M on said surface S (2) of said substrate; (c) said substrate is soaked in a liquid medium L (6) and said liquid medium L (6) is subjected to ultrasound in order to obtain a dispersion of graphene particles or sheets in said liquid medium L (6), in which method steps (b) and (c) can be performed at least partially in sequence, or simultaneously.
Method according to claim 1, characterized in that the graphite-based material is chosen from pencil leads, natural graphite a nd synthetic graphite.
Method according to cla i ms 1 to 3, characterized in that it also comprises a step (d) in which any organic or inorganic materials present in said dispersion are separated, preferably by sedimentation or centrifugation, or by chemical dissolution..3 5- 5. Method according to any one of claims 1 to 4, characterized in that it also comprises a step (e) in which said dispersion is red u ced of excessively thick graphite particles and/or graphene sheets that may be present in said dispersion, preferably by sedimentation or by centrifugation.
Method according to any one of claims 1 to 7, characterized in that the thickness of said graphene particles or sheets is between 1 and 50n m and/or the number of parallel graphene sheets is between I and 5 0, preferably between 1 and 30 and even more preferably between 1 and 15. 9, Method according to any one o f claims I to 8, characterized in that the speed o f friction between said material M (5) and said surface S (2) is between 0. 001m.s' and 0.im.s'.
Method according to any one of cla i ms 1 to 9, characterized in that said substrate is selected from the polymers, preferably flexible and/or transparent polymers, glasses, ceramics a n d silicon, 11. Method according to one of claims 1 to 10, in which said surface S (2) of said substrate and said massive material M (5) are in relative movement according to at least two axes, so as to cause a lateral offset between two adjacent segments of traces of said material M (5) on said surface S (2).
Method according to claim 11, in which said substrate is a disk capable of rotating about its axis, and in which the trace of friction of said massive material M (5) on said surface (2) is continuously or periodically offset by lateral displacement means (9) so as to obtain a continuous trace, preferably in the form of a spiral, 13. M ethod according to one of claims 1 to 12, in which steps (b) and (c) are performed simultaneously, and in which at least some of said dispersion is collected periodically or continuously, 14. Method according to one of claims 1 to 13, characterized in that said dispersion is subjected to a s e cond ultrasound tr e atm e nt, preferably with an ultrasound power and/or a duration greater than those in step (c).
Method according to one of claims 1 to 13, characterized in that said dispersion is then subjected to a microwave heating treatment.
Method for preparing graphene particles or sheets, in which a dispersion of graphen e particles or sheets is prepared according to any one of claims 1 to 15, followed by one or more 3i steps in which the graphene particles or sheets are collected from said suspension.
D evice for imple m enting the method according to one of claims 1 to 13, including:-means (3) capable of holding said bar or bloc k (5) of massive material M.-a substrate equipped with a surface S (2) capable of being in contact with said bar or block (5) of massive material M,-means (1) for displacement enabling a relative displacement between said massive material M and said substrate to be generated,-means for regulation and/or control of the pressure force (4) enabling the pressure force between said m assive m aterial M and said surface S of said substrate to be kept constant and/or measured d u ring said relative displacement,-a liquid container (19) enabling the surface S to be at least partially immersed in a liquid phase (6),-a n ultrasound generator (7) enabling said liquid (6) to be subjected to ultrasound,-optionally, drainage means (22) f o r the continuous or periodic drainage of said liquid container (19), in order to collect said liquid phase (6). Claims What is claimed is:
Method according to claim I, characterized in that the liquid phase L (6) is a reducing medium, and advantageously comprises a reducing agent selected from the group consisting of: NaBII14, hydrazine a nd ammoniac.
Method according to any one of claims I to 5, characterized in that it also comprises a step in w hich the graphene sheets are collected from said suspension, and a step of re-dispersing said graphene sheets in a liquid phase.
Method according to any one of claims I to 6, characterized in that said surface S (2) has a roughness of between 0.0 1 p m and I Opm.
, and 34-35 and ADD claims 38-39 as follows.
(Previously Amended) The method of claim 18, wherein at least some of said dispersion is collected one of periodically and continuously.
(Previously Amended) The method of claim 18, further comprising subjecting said dispersion to a second ultrasound treatment for a duration of time which is greater than that of the first ultrasound treatment.
(Previously Added) The method of claim 31, further comprising subjecting said dispersion to a microwave heating treatment after the second ultrasound treatment. unknown
(Previously Amended) The method of claim 18, further comprising collecting the one of said graphene particles and said graphene sheets from said suspension.
A device for producing a dispersion of one of graphene particles and graphene sheets in a liquid medium, the device comprising: means for holding a graphite-based ma ssiv e material includin g at least 10% b y mass of g ra p hite; a substrate equipped with a surface configured for contact with said graphite- based ma ssi ve material; means for enabling a relative displacement between said graphite-based massive material and said substrate; -5- means for one of regulating, controlling and measuring a pressure force between said graphite-based massive material and said surface of said substrate; a liquid container for receiving a liquid and configured to permit at least a partial immersion of said surface of said substrate in said liquid; and an ultrasound generator configured to subject said liquid to ultrasound waves.
The device of claim 34, further comprising[[:]] means for one of a continuous and a periodic drainage of liquid from said liquid.
36-37.. canceled
canceled
(Currently Added) The method of claim 18, wherein the graphite-based material includes at least 50% by mass of graphite. unknown
(Currently Added) The method of claim 18, wherein the graphite-based material includes a geometric shape of a block or a rod. unknown
Layer stacks claimed or described, ordered top of device to substrate.
graphene dispersion production device
No layer stack recorded.
Materials described outside the worked examples.
graphite-based massive material
graphene particles or sheets
pencil lead
natural graphite
synthetic graphite
NaBH₄
hydrazine
N₂H₄
ammoniac
NH₃
pencil lead
natural graphite
synthetic graphite
NaBH₄
hydrazine
N₂H₄
ammoniac
NH₃
pencil lead
natural graphite
synthetic graphite
NaBH₄
hydrazine
N₂H₄
ammoniac
NH₃
pencil lead
natural graphite
synthetic graphite
NaBH₄
hydrazine
N₂H₄
ammoniac
NH₃
