Patent
US 9,011,986HYDROGEN PASSIVATION INDUCED DISPERSION OF CARBON NANOTUBES AND GRAPHENE
Xiaodong Li
US
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Patent
Atlas literature
Patent
US 9,011,986Patent 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.
A method of dispersing carbon nanoparticles in a media, each carbon nanoparticle defining a surface having a dangling bond, the method comprising: immersing the carbon nanoparticles into the media, wherein the carbon nanoparticles comprise dangling bonds on the surface of the carbon nanoparticles, and wherein the dangling bonds on the surface of adjacent carbon nanoparticles are covalently bonded to each other within the media; and ultrasonicating the media containing the carbon nanoparticles in the presence of hydrogen gas courco to replace the dangling bonds on the surface of the carbon nanoparticles with carbon-hydrogen bonds, wherein ultrasonicatin g the media co ntainin g the carbon nano partic les co mris6 es irradiating the media !,containing te carbon na nop art i cles with sound waves having a fre q uency and apower sufficient to break hyd rogen-hyd rog en bonds in th e hydrpen gas.
2. The method as in claim 1, wherein ultrasonicating the media containing the carbon nanoparticles comprises irradiating the media containing the carbon nanoparticles with sound waves ha v ing a frequency and a power sufficient to break v an der Waals force interaction between adjacent carbon nanoparticles.
The method as in claim 1, wherein ultrasonicating the media containing the carbon nanoparticles comprises irradiating the media containing the carbon nanoparticles with sound wa v es having a frequency of about 20 kHz to about 350 kHz.
The method as in claim 1, wherein the media containing the carbon nanoparticles is ultrasonicated in the presence of t he hydrogen ga s for a period of about 30 minutes to about 5 hours.
The method as in claim 1, wherein the media containing the carbon nanoparticles is ultrasonicated in the presence of t he hydrogen gas for a period of about 1 hour to about 3. 5 hours. 8- 9.
The method as in claim 1, wherein the media comprises ethanol.
T he method as in claim 1, wherein the media comprises a resin.
The method as in claim 1, wherein the carbon nanoparticles comprises carbon nano-tubes. Page 3 of 8 SVG 13771518.10-15-2014.I₁ASAEMWPXXIFW3.CLM32454577.1.307.132.2245.267.svg 0.45 6.46 Graph Black and white
The method as in claim 1, further comprising: after ultr aso nicatin g, applying the media containing the carbon nanoparticles to a surface.
canceled
canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Multi-walled carbon nanotubes (MWCNTs) were dispersed in ethanol by coupled hydrogen passivation (HP) and ultrasonication. MWCNTs were immersed in ethanol and ultrasonicated in the presence of hydrogen gas for varying time periods (0 h, 0.5 h, 1 h, 2 h). Optical images, SEM images, TEM images, and C1s XPS spectra were collected to characterize the dispersion state and surface chemistry of the MWCNTs. Results compared ultrasonication only versus coupled HP and ultrasonication.
2 materials1 process step
MWCNTs well-dispersed by coupled HP and ultrasonication were incorporated into epoxy resin to form MWCNT/epoxy composites. SEM images showed individual MWCNTs well-dispersed in epoxy resin. Elastic modulus was measured as a function of MWCNT percentage.
1 material
Aligned MWCNT sheets were prepared and examined by SEM. Individual MWCNTs were tested for mechanical properties using AFM-based bending over a trench on a Si wafer.
Materials described outside the worked examples.
carbon nanoparticles
hydrogen gas
H₂
Measurements and analyses referenced in the patent, with their drawing references.
Optical images of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for different dispersion time periods: 0 h (I), 0.5 h (II), 1 h (III), and 2 h (IV). Figure 1.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Elastic Modulus Vs Composition | — | multi-walled carbon nano-tubesepoxy |
Thickness |
Patent
Atlas literature
Patent
US 9,011,986Patent 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.
A method of dispersing carbon nanoparticles in a media, each carbon nanoparticle defining a surface having a dangling bond, the method comprising: immersing the carbon nanoparticles into the media, wherein the carbon nanoparticles comprise dangling bonds on the surface of the carbon nanoparticles, and wherein the dangling bonds on the surface of adjacent carbon nanoparticles are covalently bonded to each other within the media; and ultrasonicating the media containing the carbon nanoparticles in the presence of hydrogen gas courco to replace the dangling bonds on the surface of the carbon nanoparticles with carbon-hydrogen bonds, wherein ultrasonicatin g the media co ntainin g the carbon nano partic les co mris6 es irradiating the media !,containing te carbon na nop art i cles with sound waves having a fre q uency and apower sufficient to break hyd rogen-hyd rog en bonds in th e hydrpen gas.
2. The method as in claim 1, wherein ultrasonicating the media containing the carbon nanoparticles comprises irradiating the media containing the carbon nanoparticles with sound waves ha v ing a frequency and a power sufficient to break v an der Waals force interaction between adjacent carbon nanoparticles.
The method as in claim 1, wherein ultrasonicating the media containing the carbon nanoparticles comprises irradiating the media containing the carbon nanoparticles with sound wa v es having a frequency of about 20 kHz to about 350 kHz.
The method as in claim 1, wherein the media containing the carbon nanoparticles is ultrasonicated in the presence of t he hydrogen ga s for a period of about 30 minutes to about 5 hours.
The method as in claim 1, wherein the media containing the carbon nanoparticles is ultrasonicated in the presence of t he hydrogen gas for a period of about 1 hour to about 3. 5 hours. 8- 9.
The method as in claim 1, wherein the media comprises ethanol.
T he method as in claim 1, wherein the media comprises a resin.
The method as in claim 1, wherein the carbon nanoparticles comprises carbon nano-tubes. Page 3 of 8 SVG 13771518.10-15-2014.I₁ASAEMWPXXIFW3.CLM32454577.1.307.132.2245.267.svg 0.45 6.46 Graph Black and white
The method as in claim 1, further comprising: after ultr aso nicatin g, applying the media containing the carbon nanoparticles to a surface.
canceled
canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Multi-walled carbon nanotubes (MWCNTs) were dispersed in ethanol by coupled hydrogen passivation (HP) and ultrasonication. MWCNTs were immersed in ethanol and ultrasonicated in the presence of hydrogen gas for varying time periods (0 h, 0.5 h, 1 h, 2 h). Optical images, SEM images, TEM images, and C1s XPS spectra were collected to characterize the dispersion state and surface chemistry of the MWCNTs. Results compared ultrasonication only versus coupled HP and ultrasonication.
2 materials1 process step
MWCNTs well-dispersed by coupled HP and ultrasonication were incorporated into epoxy resin to form MWCNT/epoxy composites. SEM images showed individual MWCNTs well-dispersed in epoxy resin. Elastic modulus was measured as a function of MWCNT percentage.
1 material
Aligned MWCNT sheets were prepared and examined by SEM. Individual MWCNTs were tested for mechanical properties using AFM-based bending over a trench on a Si wafer.
Materials described outside the worked examples.
carbon nanoparticles
hydrogen gas
H₂
Measurements and analyses referenced in the patent, with their drawing references.
Optical images of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for different dispersion time periods: 0 h (I), 0.5 h (II), 1 h (III), and 2 h (IV). Figure 1.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Elastic Modulus Vs Composition | — | multi-walled carbon nano-tubesepoxy |
Thickness |
Patent
Atlas literature
Patent
US 9,011,986Patent 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.
A method of dispersing carbon nanoparticles in a media, each carbon nanoparticle defining a surface having a dangling bond, the method comprising: immersing the carbon nanoparticles into the media, wherein the carbon nanoparticles comprise dangling bonds on the surface of the carbon nanoparticles, and wherein the dangling bonds on the surface of adjacent carbon nanoparticles are covalently bonded to each other within the media; and ultrasonicating the media containing the carbon nanoparticles in the presence of hydrogen gas courco to replace the dangling bonds on the surface of the carbon nanoparticles with carbon-hydrogen bonds, wherein ultrasonicatin g the media co ntainin g the carbon nano partic les co mris6 es irradiating the media !,containing te carbon na nop art i cles with sound waves having a fre q uency and apower sufficient to break hyd rogen-hyd rog en bonds in th e hydrpen gas.
2. The method as in claim 1, wherein ultrasonicating the media containing the carbon nanoparticles comprises irradiating the media containing the carbon nanoparticles with sound waves ha v ing a frequency and a power sufficient to break v an der Waals force interaction between adjacent carbon nanoparticles.
The method as in claim 1, wherein ultrasonicating the media containing the carbon nanoparticles comprises irradiating the media containing the carbon nanoparticles with sound wa v es having a frequency of about 20 kHz to about 350 kHz.
The method as in claim 1, wherein the media containing the carbon nanoparticles is ultrasonicated in the presence of t he hydrogen ga s for a period of about 30 minutes to about 5 hours.
The method as in claim 1, wherein the media containing the carbon nanoparticles is ultrasonicated in the presence of t he hydrogen gas for a period of about 1 hour to about 3. 5 hours. 8- 9.
The method as in claim 1, wherein the media comprises ethanol.
T he method as in claim 1, wherein the media comprises a resin.
The method as in claim 1, wherein the carbon nanoparticles comprises carbon nano-tubes. Page 3 of 8 SVG 13771518.10-15-2014.I₁ASAEMWPXXIFW3.CLM32454577.1.307.132.2245.267.svg 0.45 6.46 Graph Black and white
The method as in claim 1, further comprising: after ultr aso nicatin g, applying the media containing the carbon nanoparticles to a surface.
canceled
canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Multi-walled carbon nanotubes (MWCNTs) were dispersed in ethanol by coupled hydrogen passivation (HP) and ultrasonication. MWCNTs were immersed in ethanol and ultrasonicated in the presence of hydrogen gas for varying time periods (0 h, 0.5 h, 1 h, 2 h). Optical images, SEM images, TEM images, and C1s XPS spectra were collected to characterize the dispersion state and surface chemistry of the MWCNTs. Results compared ultrasonication only versus coupled HP and ultrasonication.
2 materials1 process step
MWCNTs well-dispersed by coupled HP and ultrasonication were incorporated into epoxy resin to form MWCNT/epoxy composites. SEM images showed individual MWCNTs well-dispersed in epoxy resin. Elastic modulus was measured as a function of MWCNT percentage.
1 material
Aligned MWCNT sheets were prepared and examined by SEM. Individual MWCNTs were tested for mechanical properties using AFM-based bending over a trench on a Si wafer.
Materials described outside the worked examples.
carbon nanoparticles
hydrogen gas
H₂
Measurements and analyses referenced in the patent, with their drawing references.
Optical images of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for different dispersion time periods: 0 h (I), 0.5 h (II), 1 h (III), and 2 h (IV). Figure 1.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Elastic Modulus Vs Composition | — | multi-walled carbon nano-tubesepoxy |
Thickness |
Patent
Atlas literature
Patent
US 9,011,986Patent 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.
A method of dispersing carbon nanoparticles in a media, each carbon nanoparticle defining a surface having a dangling bond, the method comprising: immersing the carbon nanoparticles into the media, wherein the carbon nanoparticles comprise dangling bonds on the surface of the carbon nanoparticles, and wherein the dangling bonds on the surface of adjacent carbon nanoparticles are covalently bonded to each other within the media; and ultrasonicating the media containing the carbon nanoparticles in the presence of hydrogen gas courco to replace the dangling bonds on the surface of the carbon nanoparticles with carbon-hydrogen bonds, wherein ultrasonicatin g the media co ntainin g the carbon nano partic les co mris6 es irradiating the media !,containing te carbon na nop art i cles with sound waves having a fre q uency and apower sufficient to break hyd rogen-hyd rog en bonds in th e hydrpen gas.
2. The method as in claim 1, wherein ultrasonicating the media containing the carbon nanoparticles comprises irradiating the media containing the carbon nanoparticles with sound waves ha v ing a frequency and a power sufficient to break v an der Waals force interaction between adjacent carbon nanoparticles.
The method as in claim 1, wherein ultrasonicating the media containing the carbon nanoparticles comprises irradiating the media containing the carbon nanoparticles with sound wa v es having a frequency of about 20 kHz to about 350 kHz.
The method as in claim 1, wherein the media containing the carbon nanoparticles is ultrasonicated in the presence of t he hydrogen ga s for a period of about 30 minutes to about 5 hours.
The method as in claim 1, wherein the media containing the carbon nanoparticles is ultrasonicated in the presence of t he hydrogen gas for a period of about 1 hour to about 3. 5 hours. 8- 9.
The method as in claim 1, wherein the media comprises ethanol.
T he method as in claim 1, wherein the media comprises a resin.
The method as in claim 1, wherein the carbon nanoparticles comprises carbon nano-tubes. Page 3 of 8 SVG 13771518.10-15-2014.I₁ASAEMWPXXIFW3.CLM32454577.1.307.132.2245.267.svg 0.45 6.46 Graph Black and white
The method as in claim 1, further comprising: after ultr aso nicatin g, applying the media containing the carbon nanoparticles to a surface.
canceled
canceled
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Multi-walled carbon nanotubes (MWCNTs) were dispersed in ethanol by coupled hydrogen passivation (HP) and ultrasonication. MWCNTs were immersed in ethanol and ultrasonicated in the presence of hydrogen gas for varying time periods (0 h, 0.5 h, 1 h, 2 h). Optical images, SEM images, TEM images, and C1s XPS spectra were collected to characterize the dispersion state and surface chemistry of the MWCNTs. Results compared ultrasonication only versus coupled HP and ultrasonication.
2 materials1 process step
MWCNTs well-dispersed by coupled HP and ultrasonication were incorporated into epoxy resin to form MWCNT/epoxy composites. SEM images showed individual MWCNTs well-dispersed in epoxy resin. Elastic modulus was measured as a function of MWCNT percentage.
1 material
Aligned MWCNT sheets were prepared and examined by SEM. Individual MWCNTs were tested for mechanical properties using AFM-based bending over a trench on a Si wafer.
Materials described outside the worked examples.
carbon nanoparticles
hydrogen gas
H₂
Measurements and analyses referenced in the patent, with their drawing references.
Optical images of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for different dispersion time periods: 0 h (I), 0.5 h (II), 1 h (III), and 2 h (IV). Figure 1.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Elastic Modulus Vs Composition | — | multi-walled carbon nano-tubesepoxy |
Thickness |
media (generic)
resin
carbon nano-tubes
single-walled carbon nano-tubes
double-walled carbon nano-tubes
graphene
carbon nanofibers
SEM images of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for different dispersion time periods: 0.5 h (I), 1 h (II), and 2 h (III). Inset: TEM image of dispersed MWCNTs with coupled HP and 2 h ultrasonication. Figure 2.
C1s XPS spectra of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for 1 h dispersion. Figure 3.
TEM image of dispersed MWCNTs with coupled HP and 2 h ultrasonication (inset in Figure 2(b)(III)).
SEM images of pure epoxy resin (Figure 5a), low magnification SEM of MWCNTs well-dispersed in epoxy resin (Figure 5b), and high magnification SEM images of individual MWCNTs well-dispersed in epoxy resin (Figures 5c–e).
Low and high magnification SEM images of an aligned MWCNT sheet. Figure 7.
3D AFM image showing a MWCNT over a trench on a Si wafer; applied bending force as a function of net MWCNT deflection. Figure 8.
| 1–999 nm |
| — |
Duration | 1800–18000 s | — |
Duration | 1–3.5 hours | — |
Duration | 1.5–3 hours | — |
Thickness | ≥ 1 nm | — |
media (generic)
resin
carbon nano-tubes
single-walled carbon nano-tubes
double-walled carbon nano-tubes
graphene
carbon nanofibers
SEM images of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for different dispersion time periods: 0.5 h (I), 1 h (II), and 2 h (III). Inset: TEM image of dispersed MWCNTs with coupled HP and 2 h ultrasonication. Figure 2.
C1s XPS spectra of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for 1 h dispersion. Figure 3.
TEM image of dispersed MWCNTs with coupled HP and 2 h ultrasonication (inset in Figure 2(b)(III)).
SEM images of pure epoxy resin (Figure 5a), low magnification SEM of MWCNTs well-dispersed in epoxy resin (Figure 5b), and high magnification SEM images of individual MWCNTs well-dispersed in epoxy resin (Figures 5c–e).
Low and high magnification SEM images of an aligned MWCNT sheet. Figure 7.
3D AFM image showing a MWCNT over a trench on a Si wafer; applied bending force as a function of net MWCNT deflection. Figure 8.
| 1–999 nm |
| — |
Duration | 1800–18000 s | — |
Duration | 1–3.5 hours | — |
Duration | 1.5–3 hours | — |
Thickness | ≥ 1 nm | — |
media (generic)
resin
carbon nano-tubes
single-walled carbon nano-tubes
double-walled carbon nano-tubes
graphene
carbon nanofibers
SEM images of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for different dispersion time periods: 0.5 h (I), 1 h (II), and 2 h (III). Inset: TEM image of dispersed MWCNTs with coupled HP and 2 h ultrasonication. Figure 2.
C1s XPS spectra of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for 1 h dispersion. Figure 3.
TEM image of dispersed MWCNTs with coupled HP and 2 h ultrasonication (inset in Figure 2(b)(III)).
SEM images of pure epoxy resin (Figure 5a), low magnification SEM of MWCNTs well-dispersed in epoxy resin (Figure 5b), and high magnification SEM images of individual MWCNTs well-dispersed in epoxy resin (Figures 5c–e).
Low and high magnification SEM images of an aligned MWCNT sheet. Figure 7.
3D AFM image showing a MWCNT over a trench on a Si wafer; applied bending force as a function of net MWCNT deflection. Figure 8.
| 1–999 nm |
| — |
Duration | 1800–18000 s | — |
Duration | 1–3.5 hours | — |
Duration | 1.5–3 hours | — |
Thickness | ≥ 1 nm | — |
media (generic)
resin
carbon nano-tubes
single-walled carbon nano-tubes
double-walled carbon nano-tubes
graphene
carbon nanofibers
SEM images of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for different dispersion time periods: 0.5 h (I), 1 h (II), and 2 h (III). Inset: TEM image of dispersed MWCNTs with coupled HP and 2 h ultrasonication. Figure 2.
C1s XPS spectra of dispersed MWCNTs with (a) ultrasonication only and (b) coupled HP and ultrasonication for 1 h dispersion. Figure 3.
TEM image of dispersed MWCNTs with coupled HP and 2 h ultrasonication (inset in Figure 2(b)(III)).
SEM images of pure epoxy resin (Figure 5a), low magnification SEM of MWCNTs well-dispersed in epoxy resin (Figure 5b), and high magnification SEM images of individual MWCNTs well-dispersed in epoxy resin (Figures 5c–e).
Low and high magnification SEM images of an aligned MWCNT sheet. Figure 7.
3D AFM image showing a MWCNT over a trench on a Si wafer; applied bending force as a function of net MWCNT deflection. Figure 8.
| 1–999 nm |
| — |
Duration | 1800–18000 s | — |
Duration | 1–3.5 hours | — |
Duration | 1.5–3 hours | — |
Thickness | ≥ 1 nm | — |