Patent
US 10,773,954CONTINUOUS PROCESS FOR PREPARING PRISTINE GRAPHENE NANOPLATELETS
Giulio Cesareo, Maria Riccardo Parrini, Laura Giorgia Rizzi
DIRECTA PLUS S.P.A.·23 December 2015·US
Copyright © 2026 Matter42. All rights reserved.
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Atlas literature
Patent
US 10,773,954Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1-11. Canceled
Canceled
A process for producing pristine graphene nanoplatelets having a C/O ratio > 100: 1, comprising: a) expanding flakes of intercalated graphite having a C/O ratio > 100: 1 and a lateral size of < 500 p m by exposing the flakes to a temperature from 1300 to 12000 ° C for a time of less than 2 seconds, and obtaining an expanded graphite having a C/O ratio > 100: 1; aa) dispersing the obtained expanded graphite having a C/O ratio > 100: 1 in water in the absence of organic solvent and in the absence of a surfactant or in the presence of a surfactant in an amount of less than 1 % by weight of the weight of the graphite; and b) subjecting said aqueous dispersion obtained in procedure (aa) to an exfoliation and a size reduction treatment carried out according to at least one of the following procedures: b1) treatment with ultrasound at an energy level of from 10 to 200Wh per gram of the graphite, or b2) treatment with high pressure homogenization carried out in a homogenizer in which the dispersion of graphite is pumped at a pressure above 35 MPa through one or more micro-channels or necks having a section not greater than 500 p m, in which the particles of the expanded graphite are caused to collide at an energy level from 5 to 200 Wh/g; wherein the exfoliation and the size reduction treatment produces pristine graphene having a C/O ratio > 100: 1 in the form of nanoplatelets, at least 90% of which have a lateral size (x, y) from 50 to 50,000 nm and a thickness (z) from 0.34 to 50 nm, the lateral size being greater than the thickness (x, y> z), and wherein the dispersing of the expanded graphite in water of in procedure (aa) is carried out immediately after the procedure of the expansion of the flakes at the temperature from 1300 to 12000 0 C by collecting the expanded graphite in water just after a formation of the expanded graphite. Currently amended
The process of claim 12, wherein the dispersion of the expanded graphite in water of procedure (aa) is carried out in a continuous way by continuously feeding the flakes of intercalated graphite to the expansion step at the temperature from 1300 to 12000 0 C, continuously discharging the so-obtained expanded graphite in said aqueous medium, and continuously subjecting the expanded graphite dispersed in the aqueous medium to an exfoliation and a size reduction treatment carried out according to at least one of procedure (b i) or procedure (b2). Previously presented
The process of claim 12, wherein the procedure of expansion at [[a]] the temperature from 1300 to 12000 0 C for a time of less than 2 seconds is carried out using an electric arch, a microwave or high frequency induction oven, or by forming plasma. Previously presented
The process of claim 12, wherein (b2) is carried out in a homogenizer in which the dispersion of the expanded graphite is pumped at a pressure above 100 MPa through one or more necks having a section not greater than 500 pm. Withdrawn
The process of claim 12, further comprising concentrating or drying of the aqueous dispersion obtained after the treatment of exfoliation or size reduction according to at least one of procedure (b i) or procedure (b2). Previously presented
Canceled
Canceled
Pristine graphene nanoplatelets, at least 90% of which have a lateral size (x, y) of from 100 to less than 10,000 nm, and a thickness (z) from 0.34 to 50 nm, the lateral size being greater than the thickness (x, y > z), having a C/O ratio > 100: 1. Withdrawn
The pristine graphene nanoplatelets of claim 21, wherein the nanoplatelets are free of surfactant, or comprise an amount of surfactant of less than 1 % by weight of the nanoplatelets. Withdrawn
Materials described outside the worked examples.
intercalated graphite flakes
expanded graphite
pristine graphene nanoplatelets
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
C/O ratio of pristine graphene nanoplatelets | ≥ 100 | pristine graphene nanoplatelets |
lateral size (x,y) of pristine graphene nanoplatelets (claim 12, ≥90%) | 50–50000 |
Patent
Atlas literature
Patent
US 10,773,954Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1-11. Canceled
Canceled
A process for producing pristine graphene nanoplatelets having a C/O ratio > 100: 1, comprising: a) expanding flakes of intercalated graphite having a C/O ratio > 100: 1 and a lateral size of < 500 p m by exposing the flakes to a temperature from 1300 to 12000 ° C for a time of less than 2 seconds, and obtaining an expanded graphite having a C/O ratio > 100: 1; aa) dispersing the obtained expanded graphite having a C/O ratio > 100: 1 in water in the absence of organic solvent and in the absence of a surfactant or in the presence of a surfactant in an amount of less than 1 % by weight of the weight of the graphite; and b) subjecting said aqueous dispersion obtained in procedure (aa) to an exfoliation and a size reduction treatment carried out according to at least one of the following procedures: b1) treatment with ultrasound at an energy level of from 10 to 200Wh per gram of the graphite, or b2) treatment with high pressure homogenization carried out in a homogenizer in which the dispersion of graphite is pumped at a pressure above 35 MPa through one or more micro-channels or necks having a section not greater than 500 p m, in which the particles of the expanded graphite are caused to collide at an energy level from 5 to 200 Wh/g; wherein the exfoliation and the size reduction treatment produces pristine graphene having a C/O ratio > 100: 1 in the form of nanoplatelets, at least 90% of which have a lateral size (x, y) from 50 to 50,000 nm and a thickness (z) from 0.34 to 50 nm, the lateral size being greater than the thickness (x, y> z), and wherein the dispersing of the expanded graphite in water of in procedure (aa) is carried out immediately after the procedure of the expansion of the flakes at the temperature from 1300 to 12000 0 C by collecting the expanded graphite in water just after a formation of the expanded graphite. Currently amended
The process of claim 12, wherein the dispersion of the expanded graphite in water of procedure (aa) is carried out in a continuous way by continuously feeding the flakes of intercalated graphite to the expansion step at the temperature from 1300 to 12000 0 C, continuously discharging the so-obtained expanded graphite in said aqueous medium, and continuously subjecting the expanded graphite dispersed in the aqueous medium to an exfoliation and a size reduction treatment carried out according to at least one of procedure (b i) or procedure (b2). Previously presented
The process of claim 12, wherein the procedure of expansion at [[a]] the temperature from 1300 to 12000 0 C for a time of less than 2 seconds is carried out using an electric arch, a microwave or high frequency induction oven, or by forming plasma. Previously presented
The process of claim 12, wherein (b2) is carried out in a homogenizer in which the dispersion of the expanded graphite is pumped at a pressure above 100 MPa through one or more necks having a section not greater than 500 pm. Withdrawn
The process of claim 12, further comprising concentrating or drying of the aqueous dispersion obtained after the treatment of exfoliation or size reduction according to at least one of procedure (b i) or procedure (b2). Previously presented
Canceled
Canceled
Pristine graphene nanoplatelets, at least 90% of which have a lateral size (x, y) of from 100 to less than 10,000 nm, and a thickness (z) from 0.34 to 50 nm, the lateral size being greater than the thickness (x, y > z), having a C/O ratio > 100: 1. Withdrawn
The pristine graphene nanoplatelets of claim 21, wherein the nanoplatelets are free of surfactant, or comprise an amount of surfactant of less than 1 % by weight of the nanoplatelets. Withdrawn
Materials described outside the worked examples.
intercalated graphite flakes
expanded graphite
pristine graphene nanoplatelets
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
C/O ratio of pristine graphene nanoplatelets | ≥ 100 | pristine graphene nanoplatelets |
lateral size (x,y) of pristine graphene nanoplatelets (claim 12, ≥90%) | 50–50000 |
Patent
Atlas literature
Patent
US 10,773,954Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1-11. Canceled
Canceled
A process for producing pristine graphene nanoplatelets having a C/O ratio > 100: 1, comprising: a) expanding flakes of intercalated graphite having a C/O ratio > 100: 1 and a lateral size of < 500 p m by exposing the flakes to a temperature from 1300 to 12000 ° C for a time of less than 2 seconds, and obtaining an expanded graphite having a C/O ratio > 100: 1; aa) dispersing the obtained expanded graphite having a C/O ratio > 100: 1 in water in the absence of organic solvent and in the absence of a surfactant or in the presence of a surfactant in an amount of less than 1 % by weight of the weight of the graphite; and b) subjecting said aqueous dispersion obtained in procedure (aa) to an exfoliation and a size reduction treatment carried out according to at least one of the following procedures: b1) treatment with ultrasound at an energy level of from 10 to 200Wh per gram of the graphite, or b2) treatment with high pressure homogenization carried out in a homogenizer in which the dispersion of graphite is pumped at a pressure above 35 MPa through one or more micro-channels or necks having a section not greater than 500 p m, in which the particles of the expanded graphite are caused to collide at an energy level from 5 to 200 Wh/g; wherein the exfoliation and the size reduction treatment produces pristine graphene having a C/O ratio > 100: 1 in the form of nanoplatelets, at least 90% of which have a lateral size (x, y) from 50 to 50,000 nm and a thickness (z) from 0.34 to 50 nm, the lateral size being greater than the thickness (x, y> z), and wherein the dispersing of the expanded graphite in water of in procedure (aa) is carried out immediately after the procedure of the expansion of the flakes at the temperature from 1300 to 12000 0 C by collecting the expanded graphite in water just after a formation of the expanded graphite. Currently amended
The process of claim 12, wherein the dispersion of the expanded graphite in water of procedure (aa) is carried out in a continuous way by continuously feeding the flakes of intercalated graphite to the expansion step at the temperature from 1300 to 12000 0 C, continuously discharging the so-obtained expanded graphite in said aqueous medium, and continuously subjecting the expanded graphite dispersed in the aqueous medium to an exfoliation and a size reduction treatment carried out according to at least one of procedure (b i) or procedure (b2). Previously presented
The process of claim 12, wherein the procedure of expansion at [[a]] the temperature from 1300 to 12000 0 C for a time of less than 2 seconds is carried out using an electric arch, a microwave or high frequency induction oven, or by forming plasma. Previously presented
The process of claim 12, wherein (b2) is carried out in a homogenizer in which the dispersion of the expanded graphite is pumped at a pressure above 100 MPa through one or more necks having a section not greater than 500 pm. Withdrawn
The process of claim 12, further comprising concentrating or drying of the aqueous dispersion obtained after the treatment of exfoliation or size reduction according to at least one of procedure (b i) or procedure (b2). Previously presented
Canceled
Canceled
Pristine graphene nanoplatelets, at least 90% of which have a lateral size (x, y) of from 100 to less than 10,000 nm, and a thickness (z) from 0.34 to 50 nm, the lateral size being greater than the thickness (x, y > z), having a C/O ratio > 100: 1. Withdrawn
The pristine graphene nanoplatelets of claim 21, wherein the nanoplatelets are free of surfactant, or comprise an amount of surfactant of less than 1 % by weight of the nanoplatelets. Withdrawn
Materials described outside the worked examples.
intercalated graphite flakes
expanded graphite
pristine graphene nanoplatelets
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
C/O ratio of pristine graphene nanoplatelets | ≥ 100 | pristine graphene nanoplatelets |
lateral size (x,y) of pristine graphene nanoplatelets (claim 12, ≥90%) | 50–50000 |
Patent
Atlas literature
Patent
US 10,773,954Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1-11. Canceled
Canceled
A process for producing pristine graphene nanoplatelets having a C/O ratio > 100: 1, comprising: a) expanding flakes of intercalated graphite having a C/O ratio > 100: 1 and a lateral size of < 500 p m by exposing the flakes to a temperature from 1300 to 12000 ° C for a time of less than 2 seconds, and obtaining an expanded graphite having a C/O ratio > 100: 1; aa) dispersing the obtained expanded graphite having a C/O ratio > 100: 1 in water in the absence of organic solvent and in the absence of a surfactant or in the presence of a surfactant in an amount of less than 1 % by weight of the weight of the graphite; and b) subjecting said aqueous dispersion obtained in procedure (aa) to an exfoliation and a size reduction treatment carried out according to at least one of the following procedures: b1) treatment with ultrasound at an energy level of from 10 to 200Wh per gram of the graphite, or b2) treatment with high pressure homogenization carried out in a homogenizer in which the dispersion of graphite is pumped at a pressure above 35 MPa through one or more micro-channels or necks having a section not greater than 500 p m, in which the particles of the expanded graphite are caused to collide at an energy level from 5 to 200 Wh/g; wherein the exfoliation and the size reduction treatment produces pristine graphene having a C/O ratio > 100: 1 in the form of nanoplatelets, at least 90% of which have a lateral size (x, y) from 50 to 50,000 nm and a thickness (z) from 0.34 to 50 nm, the lateral size being greater than the thickness (x, y> z), and wherein the dispersing of the expanded graphite in water of in procedure (aa) is carried out immediately after the procedure of the expansion of the flakes at the temperature from 1300 to 12000 0 C by collecting the expanded graphite in water just after a formation of the expanded graphite. Currently amended
The process of claim 12, wherein the dispersion of the expanded graphite in water of procedure (aa) is carried out in a continuous way by continuously feeding the flakes of intercalated graphite to the expansion step at the temperature from 1300 to 12000 0 C, continuously discharging the so-obtained expanded graphite in said aqueous medium, and continuously subjecting the expanded graphite dispersed in the aqueous medium to an exfoliation and a size reduction treatment carried out according to at least one of procedure (b i) or procedure (b2). Previously presented
The process of claim 12, wherein the procedure of expansion at [[a]] the temperature from 1300 to 12000 0 C for a time of less than 2 seconds is carried out using an electric arch, a microwave or high frequency induction oven, or by forming plasma. Previously presented
The process of claim 12, wherein (b2) is carried out in a homogenizer in which the dispersion of the expanded graphite is pumped at a pressure above 100 MPa through one or more necks having a section not greater than 500 pm. Withdrawn
The process of claim 12, further comprising concentrating or drying of the aqueous dispersion obtained after the treatment of exfoliation or size reduction according to at least one of procedure (b i) or procedure (b2). Previously presented
Canceled
Canceled
Pristine graphene nanoplatelets, at least 90% of which have a lateral size (x, y) of from 100 to less than 10,000 nm, and a thickness (z) from 0.34 to 50 nm, the lateral size being greater than the thickness (x, y > z), having a C/O ratio > 100: 1. Withdrawn
The pristine graphene nanoplatelets of claim 21, wherein the nanoplatelets are free of surfactant, or comprise an amount of surfactant of less than 1 % by weight of the nanoplatelets. Withdrawn
Materials described outside the worked examples.
intercalated graphite flakes
expanded graphite
pristine graphene nanoplatelets
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
C/O ratio of pristine graphene nanoplatelets | ≥ 100 | pristine graphene nanoplatelets |
lateral size (x,y) of pristine graphene nanoplatelets (claim 12, ≥90%) | 50–50000 |
pristine graphene nanoplatelets |
thickness (z) of pristine graphene nanoplatelets (claim 12, ≥90%) | 0.34–50 | pristine graphene nanoplatelets |
lateral size (x,y) of pristine graphene nanoplatelets (claim 21, ≥90%) | 100–9999 | pristine graphene nanoplatelets |
final dispersion concentration after concentration step (claim 19) | 6–30 | pristine graphene nanoplatelets |
Thickness | ≤ 10 nm | — |
Duration | 15–120 s | — |
Thickness | 50–50000 nm | — |
Thickness | 30–34 nm | — |
Thickness | 0.34–50 nm | — |
Thickness | ≤ 1 nm | — |
Duration | ≤ 2 seconds | — |
Thickness | ≤ 10000 nm | — |
pristine graphene nanoplatelets |
thickness (z) of pristine graphene nanoplatelets (claim 12, ≥90%) | 0.34–50 | pristine graphene nanoplatelets |
lateral size (x,y) of pristine graphene nanoplatelets (claim 21, ≥90%) | 100–9999 | pristine graphene nanoplatelets |
final dispersion concentration after concentration step (claim 19) | 6–30 | pristine graphene nanoplatelets |
Thickness | ≤ 10 nm | — |
Duration | 15–120 s | — |
Thickness | 50–50000 nm | — |
Thickness | 30–34 nm | — |
Thickness | 0.34–50 nm | — |
Thickness | ≤ 1 nm | — |
Duration | ≤ 2 seconds | — |
Thickness | ≤ 10000 nm | — |
pristine graphene nanoplatelets |
thickness (z) of pristine graphene nanoplatelets (claim 12, ≥90%) | 0.34–50 | pristine graphene nanoplatelets |
lateral size (x,y) of pristine graphene nanoplatelets (claim 21, ≥90%) | 100–9999 | pristine graphene nanoplatelets |
final dispersion concentration after concentration step (claim 19) | 6–30 | pristine graphene nanoplatelets |
Thickness | ≤ 10 nm | — |
Duration | 15–120 s | — |
Thickness | 50–50000 nm | — |
Thickness | 30–34 nm | — |
Thickness | 0.34–50 nm | — |
Thickness | ≤ 1 nm | — |
Duration | ≤ 2 seconds | — |
Thickness | ≤ 10000 nm | — |
pristine graphene nanoplatelets |
thickness (z) of pristine graphene nanoplatelets (claim 12, ≥90%) | 0.34–50 | pristine graphene nanoplatelets |
lateral size (x,y) of pristine graphene nanoplatelets (claim 21, ≥90%) | 100–9999 | pristine graphene nanoplatelets |
final dispersion concentration after concentration step (claim 19) | 6–30 | pristine graphene nanoplatelets |
Thickness | ≤ 10 nm | — |
Duration | 15–120 s | — |
Thickness | 50–50000 nm | — |
Thickness | 30–34 nm | — |
Thickness | 0.34–50 nm | — |
Thickness | ≤ 1 nm | — |
Duration | ≤ 2 seconds | — |
Thickness | ≤ 10000 nm | — |