Patent
US 10,329,391GRAPHENE-REINFORCED POLYMER MATRIX COMPOSITES
NOSKER, Thomas, LYNCH, Jennifer, KEAR, Bernard
RUTGERS, THE STATE UNIVERSITY OF NEW JERSEY·4 February 2016·US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 10,329,391Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1. In (a-c), a 20 p m scale and 1,OOO X magnification shows good distribution of multi-layer graphene or graphene within the PSU matrix at each mixing …
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
FIG. 3 illustrates the morphology of SMG-PEEK90 at (a) 10 p m scale and 1,000 X, (b) 10 p m scale and 5,000 X, (c) 1 p m scale and 10,000 X, and (d) 1 p m …
FIG. 4 illustrates the modulus of a graphite PA- 6,6 composite after various extrusion cycles. WO 2016/018995 PCT/US₂₀₁₅/04
FIG. 5 illustrates the peak stress of a graphite PA- 6,6 composite after various extrusion cycles.
FIG. 6 illustrates the impact energy of a graphite PA- 6,6 composite after various extrusion cycles.
FIG. 7 illustrates the impact strength of an injection molded graphite PA- 6,6 composite after various extrusion cycles.
FIG. 8 illustrates the adhesion on the step/edge of a graphite PA- 6,6 composite after cycle 5.
FIG. 9 illustrates the adhesion/bonding of PA- 6,6 to graphene.
FIG. 10 displays the presence of cracks on the graphene surface of a 35% graphite in PA- 6,6, cycle 3, composite, and a possible mode of surface …
FIG. 11 displays transmission imaged at a relatively high accelerating voltage (10 kV at 5KX for (a) and 10 kV at 30KX for (b)) of a 35% graphite in PA- 6,6, …
FIG. 12 displays transmission imaged at 5 kV at 10 KX for a 35% graphite in PA- 6,6, cycle 3, composite.
FIG. 13 displays transmission imaged at 5 kV (a), 4kV (b), 3kV (c) and 2kV (d) at 5 KX for a 35% graphite in PA- 6,6, cycle 1, composite.
FIG. 14 displays SEM micrographs of G-PA₆₆ Type I specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and a transparent …
FIG. 15 displays SEM micrographs of G-PA₆₆ Type V specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and transparent …
FIG. 16 shows graphs of tensile results for Type I PA₆₆ and G-PA₆₆ specimens: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 17 shows graphs of tensile results for Type V PA₆₆ and G-PA₆₆ specimens: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 18 displays notched Izod impact resistance of PA66, and G-PA₆₆ prepared using a continuous process.
FIG. 19 displays SEM micrographs displaying the morphology of G-PEEK at different scales.
FIG. 20 shows graphs of tensile results for Type I specimens of PEEK and G-PEEK: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 21 displays notched Izod impact resistance for PEEK and G-PEEK.
FIG. 22 shows a graph of the flexural modulus for G-PS specimens as compared with polystyrene (PS). DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS This …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
The samples for XRD analysis were prepared by pressing thin films of each sample 3G-PMC, 30G-PMC, and 90G-PMC at 230oC and 5,500 psi over a 2 minute time period. Each sample was positioned between aluminum sheets prior to pressing using a Carver Uniaxial Press with heated platens.
Diffraction patterns of the pressed films were acquired using a Philips XPert WO 2016/018995 PCT/US₂₀₁₅/042623 powder Diffractometer with sample changer (Xpert) at 40kV and 45mA with an incident slit thickness of 0.3 mm from 4 °-70 0 20 and a step size of 0.02 0
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Thin films of 3G-PMC, 30G-PMC, and 90G-PMC were pressed at 230°C and 5,500 psi for 2 minutes using a Carver Uniaxial Press with heated platens between aluminum sheets for XRD analysis. Diffraction patterns acquired with a Philips XPert powder diffractometer at 40 kV and 45 mA, slit 0.3 mm, 4°–70° 2θ, step size 0.02°. Debye-Scherrer equation applied to FWHM and d-spacing to determine crystal thickness.
3 materials1 process step
Mechanical exfoliation of graphite into multi-layer graphene or graphene via repetitive shear strain in polymer processing equipment generates dangling primary and secondary bonds enabling chemical functionalization. 2% graphite melt-blended with PSU converted to G-PMC using a Randcastle Small Scale Extension Mixer. Discusses potential chemical modifications including covalent bonding to polymer matrix, electrical conductivity enhancement, and catalytic applications.
No measurements recorded
Design modifications to the small batch mixer to increase shear rate for superior mechanical exfoliation of graphite within the polymer matrix. The newly designed mixer has a maximum shear rate 22 times that of the current mixer. Table 2 lists machine modifications and maximum achievable shear rates.
2 materials4 process steps
SMG blended with PEEK using a Randcastle micro-batch mixer (10-gram capacity) at 360°C (680°F) and 100 RPM under nitrogen blanket. Control PEEK3, and SMG-PEEK composites at 2-98 wt% SMG-PEEK mixed for 3, 30, and 90 minutes. At 90 minutes the extrudate appeared rubber-like and fibrous. PEEK has specific gravity 1.3, melt flow 3 g/10 min (400°C, 2.16 kg), Tg 150°C, Tm 340°C, tensile modulus 3.5 GPa, tensile strength 95 MPa.
2 materials1 process step
SMG and PEEK processed in a Randcastle micro-batch mixer with 100-gram capacity at 360°C (680°F) and 30 RPM under nitrogen blanket.
Materials described outside the worked examples.
graphene-reinforced polymer matrix composite
single-layer graphene nanoparticles
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
crystal thickness D (Debye-Scherrer) for 3G-PMC | 40 nm | 3G-PMC |
crystal thickness D (Debye-Scherrer) for 30G-PMC |
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US 10,329,391Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1. In (a-c), a 20 p m scale and 1,OOO X magnification shows good distribution of multi-layer graphene or graphene within the PSU matrix at each mixing …
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
FIG. 3 illustrates the morphology of SMG-PEEK90 at (a) 10 p m scale and 1,000 X, (b) 10 p m scale and 5,000 X, (c) 1 p m scale and 10,000 X, and (d) 1 p m …
FIG. 4 illustrates the modulus of a graphite PA- 6,6 composite after various extrusion cycles. WO 2016/018995 PCT/US₂₀₁₅/04
FIG. 5 illustrates the peak stress of a graphite PA- 6,6 composite after various extrusion cycles.
FIG. 6 illustrates the impact energy of a graphite PA- 6,6 composite after various extrusion cycles.
FIG. 7 illustrates the impact strength of an injection molded graphite PA- 6,6 composite after various extrusion cycles.
FIG. 8 illustrates the adhesion on the step/edge of a graphite PA- 6,6 composite after cycle 5.
FIG. 9 illustrates the adhesion/bonding of PA- 6,6 to graphene.
FIG. 10 displays the presence of cracks on the graphene surface of a 35% graphite in PA- 6,6, cycle 3, composite, and a possible mode of surface …
FIG. 11 displays transmission imaged at a relatively high accelerating voltage (10 kV at 5KX for (a) and 10 kV at 30KX for (b)) of a 35% graphite in PA- 6,6, …
FIG. 12 displays transmission imaged at 5 kV at 10 KX for a 35% graphite in PA- 6,6, cycle 3, composite.
FIG. 13 displays transmission imaged at 5 kV (a), 4kV (b), 3kV (c) and 2kV (d) at 5 KX for a 35% graphite in PA- 6,6, cycle 1, composite.
FIG. 14 displays SEM micrographs of G-PA₆₆ Type I specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and a transparent …
FIG. 15 displays SEM micrographs of G-PA₆₆ Type V specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and transparent …
FIG. 16 shows graphs of tensile results for Type I PA₆₆ and G-PA₆₆ specimens: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 17 shows graphs of tensile results for Type V PA₆₆ and G-PA₆₆ specimens: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 18 displays notched Izod impact resistance of PA66, and G-PA₆₆ prepared using a continuous process.
FIG. 19 displays SEM micrographs displaying the morphology of G-PEEK at different scales.
FIG. 20 shows graphs of tensile results for Type I specimens of PEEK and G-PEEK: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 21 displays notched Izod impact resistance for PEEK and G-PEEK.
FIG. 22 shows a graph of the flexural modulus for G-PS specimens as compared with polystyrene (PS). DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS This …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
The samples for XRD analysis were prepared by pressing thin films of each sample 3G-PMC, 30G-PMC, and 90G-PMC at 230oC and 5,500 psi over a 2 minute time period. Each sample was positioned between aluminum sheets prior to pressing using a Carver Uniaxial Press with heated platens.
Diffraction patterns of the pressed films were acquired using a Philips XPert WO 2016/018995 PCT/US₂₀₁₅/042623 powder Diffractometer with sample changer (Xpert) at 40kV and 45mA with an incident slit thickness of 0.3 mm from 4 °-70 0 20 and a step size of 0.02 0
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Thin films of 3G-PMC, 30G-PMC, and 90G-PMC were pressed at 230°C and 5,500 psi for 2 minutes using a Carver Uniaxial Press with heated platens between aluminum sheets for XRD analysis. Diffraction patterns acquired with a Philips XPert powder diffractometer at 40 kV and 45 mA, slit 0.3 mm, 4°–70° 2θ, step size 0.02°. Debye-Scherrer equation applied to FWHM and d-spacing to determine crystal thickness.
3 materials1 process step
Mechanical exfoliation of graphite into multi-layer graphene or graphene via repetitive shear strain in polymer processing equipment generates dangling primary and secondary bonds enabling chemical functionalization. 2% graphite melt-blended with PSU converted to G-PMC using a Randcastle Small Scale Extension Mixer. Discusses potential chemical modifications including covalent bonding to polymer matrix, electrical conductivity enhancement, and catalytic applications.
No measurements recorded
Design modifications to the small batch mixer to increase shear rate for superior mechanical exfoliation of graphite within the polymer matrix. The newly designed mixer has a maximum shear rate 22 times that of the current mixer. Table 2 lists machine modifications and maximum achievable shear rates.
2 materials4 process steps
SMG blended with PEEK using a Randcastle micro-batch mixer (10-gram capacity) at 360°C (680°F) and 100 RPM under nitrogen blanket. Control PEEK3, and SMG-PEEK composites at 2-98 wt% SMG-PEEK mixed for 3, 30, and 90 minutes. At 90 minutes the extrudate appeared rubber-like and fibrous. PEEK has specific gravity 1.3, melt flow 3 g/10 min (400°C, 2.16 kg), Tg 150°C, Tm 340°C, tensile modulus 3.5 GPa, tensile strength 95 MPa.
2 materials1 process step
SMG and PEEK processed in a Randcastle micro-batch mixer with 100-gram capacity at 360°C (680°F) and 30 RPM under nitrogen blanket.
Materials described outside the worked examples.
graphene-reinforced polymer matrix composite
single-layer graphene nanoparticles
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
crystal thickness D (Debye-Scherrer) for 3G-PMC | 40 nm | 3G-PMC |
crystal thickness D (Debye-Scherrer) for 30G-PMC |
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US 10,329,391Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1. In (a-c), a 20 p m scale and 1,OOO X magnification shows good distribution of multi-layer graphene or graphene within the PSU matrix at each mixing …
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
FIG. 3 illustrates the morphology of SMG-PEEK90 at (a) 10 p m scale and 1,000 X, (b) 10 p m scale and 5,000 X, (c) 1 p m scale and 10,000 X, and (d) 1 p m …
FIG. 4 illustrates the modulus of a graphite PA- 6,6 composite after various extrusion cycles. WO 2016/018995 PCT/US₂₀₁₅/04
FIG. 5 illustrates the peak stress of a graphite PA- 6,6 composite after various extrusion cycles.
FIG. 6 illustrates the impact energy of a graphite PA- 6,6 composite after various extrusion cycles.
FIG. 7 illustrates the impact strength of an injection molded graphite PA- 6,6 composite after various extrusion cycles.
FIG. 8 illustrates the adhesion on the step/edge of a graphite PA- 6,6 composite after cycle 5.
FIG. 9 illustrates the adhesion/bonding of PA- 6,6 to graphene.
FIG. 10 displays the presence of cracks on the graphene surface of a 35% graphite in PA- 6,6, cycle 3, composite, and a possible mode of surface …
FIG. 11 displays transmission imaged at a relatively high accelerating voltage (10 kV at 5KX for (a) and 10 kV at 30KX for (b)) of a 35% graphite in PA- 6,6, …
FIG. 12 displays transmission imaged at 5 kV at 10 KX for a 35% graphite in PA- 6,6, cycle 3, composite.
FIG. 13 displays transmission imaged at 5 kV (a), 4kV (b), 3kV (c) and 2kV (d) at 5 KX for a 35% graphite in PA- 6,6, cycle 1, composite.
FIG. 14 displays SEM micrographs of G-PA₆₆ Type I specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and a transparent …
FIG. 15 displays SEM micrographs of G-PA₆₆ Type V specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and transparent …
FIG. 16 shows graphs of tensile results for Type I PA₆₆ and G-PA₆₆ specimens: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 17 shows graphs of tensile results for Type V PA₆₆ and G-PA₆₆ specimens: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 18 displays notched Izod impact resistance of PA66, and G-PA₆₆ prepared using a continuous process.
FIG. 19 displays SEM micrographs displaying the morphology of G-PEEK at different scales.
FIG. 20 shows graphs of tensile results for Type I specimens of PEEK and G-PEEK: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 21 displays notched Izod impact resistance for PEEK and G-PEEK.
FIG. 22 shows a graph of the flexural modulus for G-PS specimens as compared with polystyrene (PS). DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS This …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
The samples for XRD analysis were prepared by pressing thin films of each sample 3G-PMC, 30G-PMC, and 90G-PMC at 230oC and 5,500 psi over a 2 minute time period. Each sample was positioned between aluminum sheets prior to pressing using a Carver Uniaxial Press with heated platens.
Diffraction patterns of the pressed films were acquired using a Philips XPert WO 2016/018995 PCT/US₂₀₁₅/042623 powder Diffractometer with sample changer (Xpert) at 40kV and 45mA with an incident slit thickness of 0.3 mm from 4 °-70 0 20 and a step size of 0.02 0
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Thin films of 3G-PMC, 30G-PMC, and 90G-PMC were pressed at 230°C and 5,500 psi for 2 minutes using a Carver Uniaxial Press with heated platens between aluminum sheets for XRD analysis. Diffraction patterns acquired with a Philips XPert powder diffractometer at 40 kV and 45 mA, slit 0.3 mm, 4°–70° 2θ, step size 0.02°. Debye-Scherrer equation applied to FWHM and d-spacing to determine crystal thickness.
3 materials1 process step
Mechanical exfoliation of graphite into multi-layer graphene or graphene via repetitive shear strain in polymer processing equipment generates dangling primary and secondary bonds enabling chemical functionalization. 2% graphite melt-blended with PSU converted to G-PMC using a Randcastle Small Scale Extension Mixer. Discusses potential chemical modifications including covalent bonding to polymer matrix, electrical conductivity enhancement, and catalytic applications.
No measurements recorded
Design modifications to the small batch mixer to increase shear rate for superior mechanical exfoliation of graphite within the polymer matrix. The newly designed mixer has a maximum shear rate 22 times that of the current mixer. Table 2 lists machine modifications and maximum achievable shear rates.
2 materials4 process steps
SMG blended with PEEK using a Randcastle micro-batch mixer (10-gram capacity) at 360°C (680°F) and 100 RPM under nitrogen blanket. Control PEEK3, and SMG-PEEK composites at 2-98 wt% SMG-PEEK mixed for 3, 30, and 90 minutes. At 90 minutes the extrudate appeared rubber-like and fibrous. PEEK has specific gravity 1.3, melt flow 3 g/10 min (400°C, 2.16 kg), Tg 150°C, Tm 340°C, tensile modulus 3.5 GPa, tensile strength 95 MPa.
2 materials1 process step
SMG and PEEK processed in a Randcastle micro-batch mixer with 100-gram capacity at 360°C (680°F) and 30 RPM under nitrogen blanket.
Materials described outside the worked examples.
graphene-reinforced polymer matrix composite
single-layer graphene nanoparticles
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
crystal thickness D (Debye-Scherrer) for 3G-PMC | 40 nm | 3G-PMC |
crystal thickness D (Debye-Scherrer) for 30G-PMC |
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In Situ Exfoliation Method to Fabricate a Graphene-Reinforced Polymer Matrix Composite
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Patent
Atlas literature
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US 10,329,391Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1. In (a-c), a 20 p m scale and 1,OOO X magnification shows good distribution of multi-layer graphene or graphene within the PSU matrix at each mixing …
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
FIG. 3 illustrates the morphology of SMG-PEEK90 at (a) 10 p m scale and 1,000 X, (b) 10 p m scale and 5,000 X, (c) 1 p m scale and 10,000 X, and (d) 1 p m …
FIG. 4 illustrates the modulus of a graphite PA- 6,6 composite after various extrusion cycles. WO 2016/018995 PCT/US₂₀₁₅/04
FIG. 5 illustrates the peak stress of a graphite PA- 6,6 composite after various extrusion cycles.
FIG. 6 illustrates the impact energy of a graphite PA- 6,6 composite after various extrusion cycles.
FIG. 7 illustrates the impact strength of an injection molded graphite PA- 6,6 composite after various extrusion cycles.
FIG. 8 illustrates the adhesion on the step/edge of a graphite PA- 6,6 composite after cycle 5.
FIG. 9 illustrates the adhesion/bonding of PA- 6,6 to graphene.
FIG. 10 displays the presence of cracks on the graphene surface of a 35% graphite in PA- 6,6, cycle 3, composite, and a possible mode of surface …
FIG. 11 displays transmission imaged at a relatively high accelerating voltage (10 kV at 5KX for (a) and 10 kV at 30KX for (b)) of a 35% graphite in PA- 6,6, …
FIG. 12 displays transmission imaged at 5 kV at 10 KX for a 35% graphite in PA- 6,6, cycle 3, composite.
FIG. 13 displays transmission imaged at 5 kV (a), 4kV (b), 3kV (c) and 2kV (d) at 5 KX for a 35% graphite in PA- 6,6, cycle 1, composite.
FIG. 14 displays SEM micrographs of G-PA₆₆ Type I specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and a transparent …
FIG. 15 displays SEM micrographs of G-PA₆₆ Type V specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and transparent …
FIG. 16 shows graphs of tensile results for Type I PA₆₆ and G-PA₆₆ specimens: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 17 shows graphs of tensile results for Type V PA₆₆ and G-PA₆₆ specimens: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 18 displays notched Izod impact resistance of PA66, and G-PA₆₆ prepared using a continuous process.
FIG. 19 displays SEM micrographs displaying the morphology of G-PEEK at different scales.
FIG. 20 shows graphs of tensile results for Type I specimens of PEEK and G-PEEK: (a) modulus, (b) stress and % strain at yield, and (c) stress and % strain at …
FIG. 21 displays notched Izod impact resistance for PEEK and G-PEEK.
FIG. 22 shows a graph of the flexural modulus for G-PS specimens as compared with polystyrene (PS). DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS This …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
The samples for XRD analysis were prepared by pressing thin films of each sample 3G-PMC, 30G-PMC, and 90G-PMC at 230oC and 5,500 psi over a 2 minute time period. Each sample was positioned between aluminum sheets prior to pressing using a Carver Uniaxial Press with heated platens.
Diffraction patterns of the pressed films were acquired using a Philips XPert WO 2016/018995 PCT/US₂₀₁₅/042623 powder Diffractometer with sample changer (Xpert) at 40kV and 45mA with an incident slit thickness of 0.3 mm from 4 °-70 0 20 and a step size of 0.02 0
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials1 process step
Thin films of 3G-PMC, 30G-PMC, and 90G-PMC were pressed at 230°C and 5,500 psi for 2 minutes using a Carver Uniaxial Press with heated platens between aluminum sheets for XRD analysis. Diffraction patterns acquired with a Philips XPert powder diffractometer at 40 kV and 45 mA, slit 0.3 mm, 4°–70° 2θ, step size 0.02°. Debye-Scherrer equation applied to FWHM and d-spacing to determine crystal thickness.
3 materials1 process step
Mechanical exfoliation of graphite into multi-layer graphene or graphene via repetitive shear strain in polymer processing equipment generates dangling primary and secondary bonds enabling chemical functionalization. 2% graphite melt-blended with PSU converted to G-PMC using a Randcastle Small Scale Extension Mixer. Discusses potential chemical modifications including covalent bonding to polymer matrix, electrical conductivity enhancement, and catalytic applications.
No measurements recorded
Design modifications to the small batch mixer to increase shear rate for superior mechanical exfoliation of graphite within the polymer matrix. The newly designed mixer has a maximum shear rate 22 times that of the current mixer. Table 2 lists machine modifications and maximum achievable shear rates.
2 materials4 process steps
SMG blended with PEEK using a Randcastle micro-batch mixer (10-gram capacity) at 360°C (680°F) and 100 RPM under nitrogen blanket. Control PEEK3, and SMG-PEEK composites at 2-98 wt% SMG-PEEK mixed for 3, 30, and 90 minutes. At 90 minutes the extrudate appeared rubber-like and fibrous. PEEK has specific gravity 1.3, melt flow 3 g/10 min (400°C, 2.16 kg), Tg 150°C, Tm 340°C, tensile modulus 3.5 GPa, tensile strength 95 MPa.
2 materials1 process step
SMG and PEEK processed in a Randcastle micro-batch mixer with 100-gram capacity at 360°C (680°F) and 30 RPM under nitrogen blanket.
Materials described outside the worked examples.
graphene-reinforced polymer matrix composite
single-layer graphene nanoparticles
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
crystal thickness D (Debye-Scherrer) for 3G-PMC | 40 nm | 3G-PMC |
crystal thickness D (Debye-Scherrer) for 30G-PMC |
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In Situ Exfoliation Method to Fabricate a Graphene-Reinforced Polymer Matrix Composite
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graphite microparticles
thermoplastic polymer
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
FIG. 14 displays SEM micrographs of G-PA₆₆ Type I specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and a transparent …
FIG. 15 displays SEM micrographs of G-PA₆₆ Type V specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and transparent …
FIG. 19 displays SEM micrographs displaying the morphology of G-PEEK at different scales.
FIG. 22 shows a graph of the flexural modulus for G-PS specimens as compared with polystyrene (PS). DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS This …
| 31 nm |
30G-PMC |
crystal thickness D (Debye-Scherrer) for 90G-PMC | 23 nm | 90G-PMC |
XRD (002) FWHM for 3G-PMC | 0.202 degrees | 3G-PMC |
XRD (002) FWHM for 30G-PMC | 0.257 degrees | 30G-PMC |
XRD (002) FWHM for 90G-PMC | 0.353 degrees | 90G-PMC |
XRD d-spacing for 3G-PMC | 3.361 Angstrom | 3G-PMC |
XRD d-spacing for 30G-PMC | 3.353 Angstrom | 30G-PMC |
XRD d-spacing for 90G-PMC | 3.387 Angstrom | 90G-PMC |
Tensile modulus of neat PEEK | 3.5 GPa | PEEK (polyether ether ketone) |
Tensile strength of neat PEEK | 95 MPa | PEEK (polyether ether ketone) |
Duration | ≥ 24 hours | — |
Thickness | 1–1000 µm | — |
Thickness | 100–750 µm | — |
Thickness | ≤ 50 nm | — |
Thickness | ≤ 10 nm | — |
multilayer graphene nanoparticles
graphite microparticles
thermoplastic polymer
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
FIG. 14 displays SEM micrographs of G-PA₆₆ Type I specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and a transparent …
FIG. 15 displays SEM micrographs of G-PA₆₆ Type V specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and transparent …
FIG. 19 displays SEM micrographs displaying the morphology of G-PEEK at different scales.
FIG. 22 shows a graph of the flexural modulus for G-PS specimens as compared with polystyrene (PS). DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS This …
| 31 nm |
30G-PMC |
crystal thickness D (Debye-Scherrer) for 90G-PMC | 23 nm | 90G-PMC |
XRD (002) FWHM for 3G-PMC | 0.202 degrees | 3G-PMC |
XRD (002) FWHM for 30G-PMC | 0.257 degrees | 30G-PMC |
XRD (002) FWHM for 90G-PMC | 0.353 degrees | 90G-PMC |
XRD d-spacing for 3G-PMC | 3.361 Angstrom | 3G-PMC |
XRD d-spacing for 30G-PMC | 3.353 Angstrom | 30G-PMC |
XRD d-spacing for 90G-PMC | 3.387 Angstrom | 90G-PMC |
Tensile modulus of neat PEEK | 3.5 GPa | PEEK (polyether ether ketone) |
Tensile strength of neat PEEK | 95 MPa | PEEK (polyether ether ketone) |
Duration | ≥ 24 hours | — |
Thickness | 1–1000 µm | — |
Thickness | 100–750 µm | — |
Thickness | ≤ 50 nm | — |
Thickness | ≤ 10 nm | — |
multilayer graphene nanoparticles
graphite microparticles
thermoplastic polymer
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
FIG. 14 displays SEM micrographs of G-PA₆₆ Type I specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and a transparent …
FIG. 15 displays SEM micrographs of G-PA₆₆ Type V specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and transparent …
FIG. 19 displays SEM micrographs displaying the morphology of G-PEEK at different scales.
FIG. 22 shows a graph of the flexural modulus for G-PS specimens as compared with polystyrene (PS). DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS This …
| 31 nm |
30G-PMC |
crystal thickness D (Debye-Scherrer) for 90G-PMC | 23 nm | 90G-PMC |
XRD (002) FWHM for 3G-PMC | 0.202 degrees | 3G-PMC |
XRD (002) FWHM for 30G-PMC | 0.257 degrees | 30G-PMC |
XRD (002) FWHM for 90G-PMC | 0.353 degrees | 90G-PMC |
XRD d-spacing for 3G-PMC | 3.361 Angstrom | 3G-PMC |
XRD d-spacing for 30G-PMC | 3.353 Angstrom | 30G-PMC |
XRD d-spacing for 90G-PMC | 3.387 Angstrom | 90G-PMC |
Tensile modulus of neat PEEK | 3.5 GPa | PEEK (polyether ether ketone) |
Tensile strength of neat PEEK | 95 MPa | PEEK (polyether ether ketone) |
Duration | ≥ 24 hours | — |
Thickness | 1–1000 µm | — |
Thickness | 100–750 µm | — |
Thickness | ≤ 50 nm | — |
Thickness | ≤ 10 nm | — |
multilayer graphene nanoparticles
graphite microparticles
thermoplastic polymer
FIG. 2, mechanical exfoliation has reduced the graphene nanoparticle thickness in the 90G-PMC sample to 8.29 nm. Example 3. X-ray Diffraction Analysis (XRD) XRD …
FIG. 14 displays SEM micrographs of G-PA₆₆ Type I specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and a transparent …
FIG. 15 displays SEM micrographs of G-PA₆₆ Type V specimens, showing good distribution of graphene flakes in the polymer matrix in (a)-(d), and transparent …
FIG. 19 displays SEM micrographs displaying the morphology of G-PEEK at different scales.
FIG. 22 shows a graph of the flexural modulus for G-PS specimens as compared with polystyrene (PS). DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS This …
| 31 nm |
30G-PMC |
crystal thickness D (Debye-Scherrer) for 90G-PMC | 23 nm | 90G-PMC |
XRD (002) FWHM for 3G-PMC | 0.202 degrees | 3G-PMC |
XRD (002) FWHM for 30G-PMC | 0.257 degrees | 30G-PMC |
XRD (002) FWHM for 90G-PMC | 0.353 degrees | 90G-PMC |
XRD d-spacing for 3G-PMC | 3.361 Angstrom | 3G-PMC |
XRD d-spacing for 30G-PMC | 3.353 Angstrom | 30G-PMC |
XRD d-spacing for 90G-PMC | 3.387 Angstrom | 90G-PMC |
Tensile modulus of neat PEEK | 3.5 GPa | PEEK (polyether ether ketone) |
Tensile strength of neat PEEK | 95 MPa | PEEK (polyether ether ketone) |
Duration | ≥ 24 hours | — |
Thickness | 1–1000 µm | — |
Thickness | 100–750 µm | — |
Thickness | ≤ 50 nm | — |
Thickness | ≤ 10 nm | — |