Patent
Atlas literature
Patent
US 11,912,840 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1-9 illustrate both of the modes as preferred embodiments of the present invention.
FIGS. 2 and 3 describe the process according to the 25 present invention carried out in a continuous flow mode. The initial composition is loaded into the …
FIG. 3), a check valve can be applied downstream of the latter, or a pressure relief valve, to ensure that the starting composition remains at a predetermined …
FIG. 4. 2 parts of commercial synthetic graphite SFG₆ produced by Timcal are dispersed in 98 parts of styrene (Sigma Aldrich) by means of a magnetic anchor …
FIG. 5. This mode envisages the presence of a storage tank (7) containing an emergency fluid, charged through stream f8, which is preferably the main solvent. …
FIG. 6. For this purpose, the pressurization tank (8) is filled with styrene (the surge fluid used) through stream (f10 bis). During the charging of the …
FIG. 7 envisages the presence of a second device (10) situated downstream of the main circuit (sonication loop) which comprises the device in which the …
FIG. 8 provides for 25 the presence of a storage tank (11) having a much greater volume than that of the main circuit (sonication loop), for example, two times …
FIG. 9. The pressurization is effected by means of expansion fluid con- tained in the pressurization tank (8). The pressure used in the 30 sonication loop was …
FIG. 10. The same product was also subjected to atomic force microscopy (AFM) thus verifying that the GRS obtained has a thickness not exceeding 10 nm. The …
FIG. 11), a good exfoliation degree can be observed. It was also estimated, through AFM, that the GRS has a thickness not greater than 10 nm. The concentration …
FIG. 12. Also in this case, an AFM analysis was carried out, estimating a thickness of the GRS not greater than 10 nm. The concentration of GRS 5 on “Product …
FIG. 13 is a photograph of the Product 1A (see Example 1) compared with the same composition of Example 1 not treated with ultrasounds.
FIG. 14 is a photograph of the Product 1A (see example 1) compared with the same composition of Example 1 treated with ultrasounds at atmospheric pressure. …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A composition, comprising: a solvent having an interfacial tension different from that of graphite material and comprising 10 to 70% by weight of a polystyrene and 20 to 80% by weight of a styrene monomer, and graphene and graphene nanoplatelets (GRS) stably dis-persed without any evident formations of deposits or separated phases for at least 30 days in the solvent in a mass concentration of 0.05 to 5% by weight, wherein the composition is produced by a process compris-ing combining a graphite and a styrene monomer to form a mixture; subjecting the mixture to ultrasound treatment to exfoliate the graphite to graphene and to simultaneously polym-erize the styrene monomer to form a polystyrene, and decanting or separating by centrifugation the produced mixture comprising the polystyrene, the exfoliated gra-43 44 phene, unpolymerized styrene and non-exfoliated graphite to remove the graphite not completely exfoli-ated, wherein the ultrasound treatment is conducted at a frequency spectrum ranging from 18 kHz to 20 kHz and an ultrasound power of 60 to 110 W/cm3 in a degassed environment at a pressure of from 12 to 25 bar absolute and at a temperature ranging from 20° C. to 200° C. for 0.5 seconds to 5 minutes; and wherein the graphene and the graphene nanoplatelets have an average thickness higher than or equal to the thick-ness of a single graphene layer up to 50 nm, the thickness being measured on samples of graphene and graphene nanoplatelets deposited on a silicon wafer coated with silicon oxide, with intermittent contact atomic force microscopy, called AFM tapping mode.
The composition according to claim 1, wherein the graphene and the graphene nanoplatelets have a carbon/oxygen molar ratio of higher or equal to 10.
A polymer composite or a polymer nano-composite, comprising: the composition according to claim 1.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Graphite exfoliated in styrene monomer under high-pressure ultrasound conditions to produce product 1A (stable dispersion of graphene/GNP in styrene/polystyrene solvent) and product 1B (after removal of non-exfoliated graphite by decantation/centrifugation). TEM photograph of product 1B provided in FIG. 10.
4 materials1 process step
Graphite exfoliated in styrene monomer under high-pressure ultrasound conditions; TEM photograph of product 2B provided in FIG. 11.
4 materials1 process step
Graphite exfoliated under ultrasound conditions; TEM photograph of product 4B provided in FIG. 12.
3 materials1 process step
Same composition as Example 1 treated with ultrasounds at atmospheric pressure; compared with Product 1A in FIG. 14 to demonstrate the importance of elevated pressure.
Materials described outside the worked examples.
expanding agent
graphite
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Dispersion Stability | stable without evident formations of deposits or separated phases | graphenegraphene nanoplatelets (GRS) |
Carbon Oxygen Molar Ratio |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 8
Patent
Atlas literature
Patent
US 11,912,840 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1-9 illustrate both of the modes as preferred embodiments of the present invention.
FIGS. 2 and 3 describe the process according to the 25 present invention carried out in a continuous flow mode. The initial composition is loaded into the …
FIG. 3), a check valve can be applied downstream of the latter, or a pressure relief valve, to ensure that the starting composition remains at a predetermined …
FIG. 4. 2 parts of commercial synthetic graphite SFG₆ produced by Timcal are dispersed in 98 parts of styrene (Sigma Aldrich) by means of a magnetic anchor …
FIG. 5. This mode envisages the presence of a storage tank (7) containing an emergency fluid, charged through stream f8, which is preferably the main solvent. …
FIG. 6. For this purpose, the pressurization tank (8) is filled with styrene (the surge fluid used) through stream (f10 bis). During the charging of the …
FIG. 7 envisages the presence of a second device (10) situated downstream of the main circuit (sonication loop) which comprises the device in which the …
FIG. 8 provides for 25 the presence of a storage tank (11) having a much greater volume than that of the main circuit (sonication loop), for example, two times …
FIG. 9. The pressurization is effected by means of expansion fluid con- tained in the pressurization tank (8). The pressure used in the 30 sonication loop was …
FIG. 10. The same product was also subjected to atomic force microscopy (AFM) thus verifying that the GRS obtained has a thickness not exceeding 10 nm. The …
FIG. 11), a good exfoliation degree can be observed. It was also estimated, through AFM, that the GRS has a thickness not greater than 10 nm. The concentration …
FIG. 12. Also in this case, an AFM analysis was carried out, estimating a thickness of the GRS not greater than 10 nm. The concentration of GRS 5 on “Product …
FIG. 13 is a photograph of the Product 1A (see Example 1) compared with the same composition of Example 1 not treated with ultrasounds.
FIG. 14 is a photograph of the Product 1A (see example 1) compared with the same composition of Example 1 treated with ultrasounds at atmospheric pressure. …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A composition, comprising: a solvent having an interfacial tension different from that of graphite material and comprising 10 to 70% by weight of a polystyrene and 20 to 80% by weight of a styrene monomer, and graphene and graphene nanoplatelets (GRS) stably dis-persed without any evident formations of deposits or separated phases for at least 30 days in the solvent in a mass concentration of 0.05 to 5% by weight, wherein the composition is produced by a process compris-ing combining a graphite and a styrene monomer to form a mixture; subjecting the mixture to ultrasound treatment to exfoliate the graphite to graphene and to simultaneously polym-erize the styrene monomer to form a polystyrene, and decanting or separating by centrifugation the produced mixture comprising the polystyrene, the exfoliated gra-43 44 phene, unpolymerized styrene and non-exfoliated graphite to remove the graphite not completely exfoli-ated, wherein the ultrasound treatment is conducted at a frequency spectrum ranging from 18 kHz to 20 kHz and an ultrasound power of 60 to 110 W/cm3 in a degassed environment at a pressure of from 12 to 25 bar absolute and at a temperature ranging from 20° C. to 200° C. for 0.5 seconds to 5 minutes; and wherein the graphene and the graphene nanoplatelets have an average thickness higher than or equal to the thick-ness of a single graphene layer up to 50 nm, the thickness being measured on samples of graphene and graphene nanoplatelets deposited on a silicon wafer coated with silicon oxide, with intermittent contact atomic force microscopy, called AFM tapping mode.
The composition according to claim 1, wherein the graphene and the graphene nanoplatelets have a carbon/oxygen molar ratio of higher or equal to 10.
A polymer composite or a polymer nano-composite, comprising: the composition according to claim 1.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Graphite exfoliated in styrene monomer under high-pressure ultrasound conditions to produce product 1A (stable dispersion of graphene/GNP in styrene/polystyrene solvent) and product 1B (after removal of non-exfoliated graphite by decantation/centrifugation). TEM photograph of product 1B provided in FIG. 10.
4 materials1 process step
Graphite exfoliated in styrene monomer under high-pressure ultrasound conditions; TEM photograph of product 2B provided in FIG. 11.
4 materials1 process step
Graphite exfoliated under ultrasound conditions; TEM photograph of product 4B provided in FIG. 12.
3 materials1 process step
Same composition as Example 1 treated with ultrasounds at atmospheric pressure; compared with Product 1A in FIG. 14 to demonstrate the importance of elevated pressure.
Materials described outside the worked examples.
expanding agent
graphite
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Dispersion Stability | stable without evident formations of deposits or separated phases | graphenegraphene nanoplatelets (GRS) |
Carbon Oxygen Molar Ratio |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 8
Patent
Atlas literature
Patent
US 11,912,840 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1-9 illustrate both of the modes as preferred embodiments of the present invention.
FIGS. 2 and 3 describe the process according to the 25 present invention carried out in a continuous flow mode. The initial composition is loaded into the …
FIG. 3), a check valve can be applied downstream of the latter, or a pressure relief valve, to ensure that the starting composition remains at a predetermined …
FIG. 4. 2 parts of commercial synthetic graphite SFG₆ produced by Timcal are dispersed in 98 parts of styrene (Sigma Aldrich) by means of a magnetic anchor …
FIG. 5. This mode envisages the presence of a storage tank (7) containing an emergency fluid, charged through stream f8, which is preferably the main solvent. …
FIG. 6. For this purpose, the pressurization tank (8) is filled with styrene (the surge fluid used) through stream (f10 bis). During the charging of the …
FIG. 7 envisages the presence of a second device (10) situated downstream of the main circuit (sonication loop) which comprises the device in which the …
FIG. 8 provides for 25 the presence of a storage tank (11) having a much greater volume than that of the main circuit (sonication loop), for example, two times …
FIG. 9. The pressurization is effected by means of expansion fluid con- tained in the pressurization tank (8). The pressure used in the 30 sonication loop was …
FIG. 10. The same product was also subjected to atomic force microscopy (AFM) thus verifying that the GRS obtained has a thickness not exceeding 10 nm. The …
FIG. 11), a good exfoliation degree can be observed. It was also estimated, through AFM, that the GRS has a thickness not greater than 10 nm. The concentration …
FIG. 12. Also in this case, an AFM analysis was carried out, estimating a thickness of the GRS not greater than 10 nm. The concentration of GRS 5 on “Product …
FIG. 13 is a photograph of the Product 1A (see Example 1) compared with the same composition of Example 1 not treated with ultrasounds.
FIG. 14 is a photograph of the Product 1A (see example 1) compared with the same composition of Example 1 treated with ultrasounds at atmospheric pressure. …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A composition, comprising: a solvent having an interfacial tension different from that of graphite material and comprising 10 to 70% by weight of a polystyrene and 20 to 80% by weight of a styrene monomer, and graphene and graphene nanoplatelets (GRS) stably dis-persed without any evident formations of deposits or separated phases for at least 30 days in the solvent in a mass concentration of 0.05 to 5% by weight, wherein the composition is produced by a process compris-ing combining a graphite and a styrene monomer to form a mixture; subjecting the mixture to ultrasound treatment to exfoliate the graphite to graphene and to simultaneously polym-erize the styrene monomer to form a polystyrene, and decanting or separating by centrifugation the produced mixture comprising the polystyrene, the exfoliated gra-43 44 phene, unpolymerized styrene and non-exfoliated graphite to remove the graphite not completely exfoli-ated, wherein the ultrasound treatment is conducted at a frequency spectrum ranging from 18 kHz to 20 kHz and an ultrasound power of 60 to 110 W/cm3 in a degassed environment at a pressure of from 12 to 25 bar absolute and at a temperature ranging from 20° C. to 200° C. for 0.5 seconds to 5 minutes; and wherein the graphene and the graphene nanoplatelets have an average thickness higher than or equal to the thick-ness of a single graphene layer up to 50 nm, the thickness being measured on samples of graphene and graphene nanoplatelets deposited on a silicon wafer coated with silicon oxide, with intermittent contact atomic force microscopy, called AFM tapping mode.
The composition according to claim 1, wherein the graphene and the graphene nanoplatelets have a carbon/oxygen molar ratio of higher or equal to 10.
A polymer composite or a polymer nano-composite, comprising: the composition according to claim 1.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Graphite exfoliated in styrene monomer under high-pressure ultrasound conditions to produce product 1A (stable dispersion of graphene/GNP in styrene/polystyrene solvent) and product 1B (after removal of non-exfoliated graphite by decantation/centrifugation). TEM photograph of product 1B provided in FIG. 10.
4 materials1 process step
Graphite exfoliated in styrene monomer under high-pressure ultrasound conditions; TEM photograph of product 2B provided in FIG. 11.
4 materials1 process step
Graphite exfoliated under ultrasound conditions; TEM photograph of product 4B provided in FIG. 12.
3 materials1 process step
Same composition as Example 1 treated with ultrasounds at atmospheric pressure; compared with Product 1A in FIG. 14 to demonstrate the importance of elevated pressure.
Materials described outside the worked examples.
expanding agent
graphite
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Dispersion Stability | stable without evident formations of deposits or separated phases | graphenegraphene nanoplatelets (GRS) |
Carbon Oxygen Molar Ratio |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 8
Patent
Atlas literature
Patent
US 11,912,840 B2Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1-9 illustrate both of the modes as preferred embodiments of the present invention.
FIGS. 2 and 3 describe the process according to the 25 present invention carried out in a continuous flow mode. The initial composition is loaded into the …
FIG. 3), a check valve can be applied downstream of the latter, or a pressure relief valve, to ensure that the starting composition remains at a predetermined …
FIG. 4. 2 parts of commercial synthetic graphite SFG₆ produced by Timcal are dispersed in 98 parts of styrene (Sigma Aldrich) by means of a magnetic anchor …
FIG. 5. This mode envisages the presence of a storage tank (7) containing an emergency fluid, charged through stream f8, which is preferably the main solvent. …
FIG. 6. For this purpose, the pressurization tank (8) is filled with styrene (the surge fluid used) through stream (f10 bis). During the charging of the …
FIG. 7 envisages the presence of a second device (10) situated downstream of the main circuit (sonication loop) which comprises the device in which the …
FIG. 8 provides for 25 the presence of a storage tank (11) having a much greater volume than that of the main circuit (sonication loop), for example, two times …
FIG. 9. The pressurization is effected by means of expansion fluid con- tained in the pressurization tank (8). The pressure used in the 30 sonication loop was …
FIG. 10. The same product was also subjected to atomic force microscopy (AFM) thus verifying that the GRS obtained has a thickness not exceeding 10 nm. The …
FIG. 11), a good exfoliation degree can be observed. It was also estimated, through AFM, that the GRS has a thickness not greater than 10 nm. The concentration …
FIG. 12. Also in this case, an AFM analysis was carried out, estimating a thickness of the GRS not greater than 10 nm. The concentration of GRS 5 on “Product …
FIG. 13 is a photograph of the Product 1A (see Example 1) compared with the same composition of Example 1 not treated with ultrasounds.
FIG. 14 is a photograph of the Product 1A (see example 1) compared with the same composition of Example 1 treated with ultrasounds at atmospheric pressure. …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A composition, comprising: a solvent having an interfacial tension different from that of graphite material and comprising 10 to 70% by weight of a polystyrene and 20 to 80% by weight of a styrene monomer, and graphene and graphene nanoplatelets (GRS) stably dis-persed without any evident formations of deposits or separated phases for at least 30 days in the solvent in a mass concentration of 0.05 to 5% by weight, wherein the composition is produced by a process compris-ing combining a graphite and a styrene monomer to form a mixture; subjecting the mixture to ultrasound treatment to exfoliate the graphite to graphene and to simultaneously polym-erize the styrene monomer to form a polystyrene, and decanting or separating by centrifugation the produced mixture comprising the polystyrene, the exfoliated gra-43 44 phene, unpolymerized styrene and non-exfoliated graphite to remove the graphite not completely exfoli-ated, wherein the ultrasound treatment is conducted at a frequency spectrum ranging from 18 kHz to 20 kHz and an ultrasound power of 60 to 110 W/cm3 in a degassed environment at a pressure of from 12 to 25 bar absolute and at a temperature ranging from 20° C. to 200° C. for 0.5 seconds to 5 minutes; and wherein the graphene and the graphene nanoplatelets have an average thickness higher than or equal to the thick-ness of a single graphene layer up to 50 nm, the thickness being measured on samples of graphene and graphene nanoplatelets deposited on a silicon wafer coated with silicon oxide, with intermittent contact atomic force microscopy, called AFM tapping mode.
The composition according to claim 1, wherein the graphene and the graphene nanoplatelets have a carbon/oxygen molar ratio of higher or equal to 10.
A polymer composite or a polymer nano-composite, comprising: the composition according to claim 1.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Graphite exfoliated in styrene monomer under high-pressure ultrasound conditions to produce product 1A (stable dispersion of graphene/GNP in styrene/polystyrene solvent) and product 1B (after removal of non-exfoliated graphite by decantation/centrifugation). TEM photograph of product 1B provided in FIG. 10.
4 materials1 process step
Graphite exfoliated in styrene monomer under high-pressure ultrasound conditions; TEM photograph of product 2B provided in FIG. 11.
4 materials1 process step
Graphite exfoliated under ultrasound conditions; TEM photograph of product 4B provided in FIG. 12.
3 materials1 process step
Same composition as Example 1 treated with ultrasounds at atmospheric pressure; compared with Product 1A in FIG. 14 to demonstrate the importance of elevated pressure.
Materials described outside the worked examples.
expanding agent
graphite
Measurements and analyses referenced in the patent, with their drawing references.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Dispersion Stability | stable without evident formations of deposits or separated phases | graphenegraphene nanoplatelets (GRS) |
Carbon Oxygen Molar Ratio |
Patents and literature cited by this patent (applicant and examiner references).
Cited patents · 8
| ≥10 mol/mol |
graphenegraphene nanoplatelets (GRS) |
Average Thickness | single graphene layer to 50 nm nm | graphenegraphene nanoplatelets (GRS) |
Temperature | 600–850 °C | — |
Thickness | ≥ 10 nm | — |
Duration | 0.5–300 s | — |
Duration | 1–60 s | — |
Duration | 2–30 seconds | — |
Thickness | 3–15 mm | — |
Temperature | 20–200 °C | — |
Temperature | 40–200 °C | — |
Temperature | 40–170 °C | — |
Temperature | 60–130 °C | — |
Duration | 2–60 minutes | — |
Pressure | 8–50 bar | — |
Pressure | 12–25 bar | — |
Pressure | ≥ 0.1 Pa | — |
— | ≥ 60 W | — |
— | ≥ 110 W | — |
Duration | ≥ 2 minutes | — |
— | 60–110 W | — |
Cited non-patent literature · 1
| ≥10 mol/mol |
graphenegraphene nanoplatelets (GRS) |
Average Thickness | single graphene layer to 50 nm nm | graphenegraphene nanoplatelets (GRS) |
Temperature | 600–850 °C | — |
Thickness | ≥ 10 nm | — |
Duration | 0.5–300 s | — |
Duration | 1–60 s | — |
Duration | 2–30 seconds | — |
Thickness | 3–15 mm | — |
Temperature | 20–200 °C | — |
Temperature | 40–200 °C | — |
Temperature | 40–170 °C | — |
Temperature | 60–130 °C | — |
Duration | 2–60 minutes | — |
Pressure | 8–50 bar | — |
Pressure | 12–25 bar | — |
Pressure | ≥ 0.1 Pa | — |
— | ≥ 60 W | — |
— | ≥ 110 W | — |
Duration | ≥ 2 minutes | — |
— | 60–110 W | — |
Cited non-patent literature · 1
| ≥10 mol/mol |
graphenegraphene nanoplatelets (GRS) |
Average Thickness | single graphene layer to 50 nm nm | graphenegraphene nanoplatelets (GRS) |
Temperature | 600–850 °C | — |
Thickness | ≥ 10 nm | — |
Duration | 0.5–300 s | — |
Duration | 1–60 s | — |
Duration | 2–30 seconds | — |
Thickness | 3–15 mm | — |
Temperature | 20–200 °C | — |
Temperature | 40–200 °C | — |
Temperature | 40–170 °C | — |
Temperature | 60–130 °C | — |
Duration | 2–60 minutes | — |
Pressure | 8–50 bar | — |
Pressure | 12–25 bar | — |
Pressure | ≥ 0.1 Pa | — |
— | ≥ 60 W | — |
— | ≥ 110 W | — |
Duration | ≥ 2 minutes | — |
— | 60–110 W | — |
Cited non-patent literature · 1
| ≥10 mol/mol |
graphenegraphene nanoplatelets (GRS) |
Average Thickness | single graphene layer to 50 nm nm | graphenegraphene nanoplatelets (GRS) |
Temperature | 600–850 °C | — |
Thickness | ≥ 10 nm | — |
Duration | 0.5–300 s | — |
Duration | 1–60 s | — |
Duration | 2–30 seconds | — |
Thickness | 3–15 mm | — |
Temperature | 20–200 °C | — |
Temperature | 40–200 °C | — |
Temperature | 40–170 °C | — |
Temperature | 60–130 °C | — |
Duration | 2–60 minutes | — |
Pressure | 8–50 bar | — |
Pressure | 12–25 bar | — |
Pressure | ≥ 0.1 Pa | — |
— | ≥ 60 W | — |
— | ≥ 110 W | — |
Duration | ≥ 2 minutes | — |
— | 60–110 W | — |
Cited non-patent literature · 1
