Patent
Atlas literature
Patent
US 9,493,355Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1. For instance, in some embodiments that are illustrated in Panel I of
FIG. 2D illustrates the deintercalation of functionalized GNRs. [0017] FIGURE 3 provides scanning electron microscopy (SEM) images of various solubility tests. …
FIG. 3A shows an SEM image of pristine Mitsui MWNTs, and a 0.1 mg/mL suspension in chlorofo rm.
FIG. 4B). The images show that commercial MWNTs are non-dispersible in organic solvents after short sonication using an ultrasonic cleaner. However, HD-GNRs …
FIG. 5 B provides an optical microscope of NTL- originated functionalized HD-GNRs. [0020] FIGURE 6 shows an HD-GNR fabricated device and related conductivity …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 8B) of a single HD-GNR used in a device for conductivity measurements. AFM images were obtained with a Digital Instruments nanoscope III a, operating in …
FIG. 9B. Current and potential were then measured. [0024] FIGURE 10 provides calculation of the hypothetical degree of edge functionalization with HD groups …
FIG. 10). If all of the edge carbons are functionalized, then the functional groups would contribute 1 wt % of the total weight to the HD-GNRs; 0.5 wt % if …
FIG. 11 C) are shown. [0026] FIGURE 12 shows the EGA for hydrogen terminated GNRs (H-GNRs). The colors represent fragments with m/z 15 (red), 29 (orange), 43 …
FIG. 12). The methyl fragment could be the result of rea rr angements with successive cleavage on defects and edges where carbons are expected to be …
FIG. 13B shows comparison of functionalized HD-GNRs, O- GNRs, B-GNRs, GNRs and MWNTs. Peaks at 21.8 0, 25.3 0, 35.90, 42.4, 44.40, 51.8 0, 56.8 0, and 58.4 0 …
FIG. 14. [00166] The XRD diffractogram for the as-prepared sample contains well-pronounced diffraction lines at 12.0 0 and 24.2 0 20 angle, which co rr espond to …
FIG. 15). Interestingly, no intermediate stage compound was detected in the sample. [00168] Such results are unexpected for graphite intercalation compounds …
FIG. 16A is a GC plot (purple curve) of trapped (at 0 0 C) condensate from HD-GNRs heated at 150 ° C in high vacuum for 1 hour. The concentration of the …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 18). This is an additional argument in support of formation of the intercalation compound. It is known that when several species are intercalated into …
FIG. 19), where the (002) signal was observed at 26.2 0 20 angle, which corresponds to non-intercalated material. The results were also confirmed by TGA (
FIG. 20), where Applicants observed a weight loss of-2% in the region between room temperature and 800 °C. [00183] Summary [00184] In this Example, a high …
FIG. 21D shows the polymerization of the added monomers on the opened MWNTs and the subsequent formation of PF-GNRs upon quenching. For clarity, double bonds …
FIGS. 22-25. [00216] Thermogravimetric mass spectrometry (TG/MS) was used to qualitatively confirm the presence of the polystyrene chains, to estimate the …
FIG. 23B) SEM images are shown. The spherical nanoparticles are amorphous carbon byproducts. Thermal annealing at 2800 ° C under argon atmosphere improved the …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 27. [00218] Raman spectroscopy was also used to characterize the graphitic structure of the GNRs. An increase in the intensity of the D band over the G …
FIG. 28B provides representative SEM images of split MWNTs. The majority of MWNTs were split. Ribbon-like structure could be indentified in the image.
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 30C is an SEM image of NTL MWNTs after liquid-phase intercalation followed by addition of styrene. It is shown that NTL MWNTs are split but not completely …
FIG. 31B is an SEM image of Baytubes after liquid-phase intercalation followed by polymerization. The image shows that the Baytubes are split due to …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 33B is an SEM image of MWNTs treated with lithium naphthalenide followed by styrene. [0048] FIGURE 34 provides SEM images of carboxyl-functionalized GNRs …
FIG. 34B is 2 m. [0049] FIGURE 35 provides TEM images of GNR-(COOH)n. The scale bar in
FIG. 35B is 10 nm. [0050] FIGURE 36 provides the Raman spectrum of GNR-(COOH)n. The excitation laser wavelength is 514 nm.
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1. A method of preparing functionalized graphene nanoribbons, wherein the method comprises: exposing a plurality of carbon nanotubes to an alkali metal source in the presence of an aprotic solvent, wherein the exposing opens the carbon nanotubes; and exposing the opened carbon nanotubes to an electrophile to form functionalized graphene nanoribbons. withdrawn
2. The method of claim 1, further comprising a step of exposing the opened carbon nanotubes to a protic solvent. withdrawn
4. The method of claim 1, wherein the carbon nanotubes are opened parallel to their longitudinal axis. withdrawn
5. The method of claim 1, wherein the method takes place at room temperature. withdrawn
6. The method of claim 1, wherein the carbon nanotubes are selected from the group consisting of single-walled carbon nanotubes, double-walled carbon nanotubes, triple- walled carbon nanotubes, multi-walled carbon nanotubes, ultra-sho rt carbon nanotubes, and combinations thereof. withdrawn
7. The method of claim 1, wherein the carbon nanotubes comprise multi-walled carbon nanotubes. withdrawn
8. The method of claim 1, wherein the alkali metal source is selected from the group consisting of lithium, potassium, sodium, rubidium, caesium, alloys thereof, and combinations thereof. withdrawn
9. The method of claim 1, wherein the alkali metal source comprises potassium. withdrawn
10. The method of claim 1, wherein the aprotic solvent is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,4-dioxane, glyme, 1,2-dimethoxyethane, diglyme, tetraglyme, amines, N,N,N',N'-tetramethylethylenediamine, triethylamine, 1,4- diazabicyclo[2.2.2] octane, trialkylamines, dialkylarylamines, alkyldiarylamines, dimethylformamide, and combinations thereof. withdrawn
11. The method of claim 1, wherein the electrophile is selected from the group consisting of water, alcohols, organic halides, alkenes, alkyl halides, acyl halides, allylic halides, benzyl halides, benzylic halides, alkenyl halides, aryl halides, alkynyl halides, fluoralkly halides, perfluoroalkyl halides, aldehydes, ketones, methyl vinyl ketones, esters, sulfonate esters, acids, acid chlorides, carboxylic acids, carboxylic esters, carboxylic acid chlorides, carboxylic acid 3 Application No. 14/345,016 Docket No.: 11321-P₂₃₁WOUS Amendment dated Reply to Office Action of anhydrides, carbonyl bearing compounds, enones, nitriles, carbon dioxide, halogens, monomers, vinyl monomers, ring-opening monomers, isoprenes, butadienes, styrenes, acrylonitriles, methyl vinyl ketones, methacrylates, 1,4-dimethoxy-2-vinylbenzene, methyl methacrylate, alkyl acrylates, alkyl methacrylates, trimethylsilyl chlorides, tert-butyldimethylsilyl chlorides, triphenylsilyl chlorides, epoxides, carbon dioxide, carbon disulfide, tert-butanol, 2- methylpropene, bromine, chlorine, iodine, fluorine, and combinations thereof. withdrawn
12. The method of claim 1, wherein the electrophile comprises carbon dioxide. withdrawn
13. The method of claim 1, wherein the electrophile is a monomer. withdrawn
16. The method of claim 1, wherein the formed graphene nanoribbons comprise edge-functionalized graphene nanoribbons. withdrawn
17. The method of claim 1, wherein the formed graphene nanoribbons have a conductivity ranging from about 0.1 S/cm to about 9,000 S/cm. withdrawn
18. The method of claim 1, further comprising a step of deintercalating functional groups from one or more layers of graphene nanoribbons. withdrawn
20. The method of claim 1, further comprising a step of exfoliating one or more layers of graphene from the formed graphene nanoribbons. withdrawn
22. A method of preparing graphene nanoribbons, wherein the method comprises: exposing a plurality of carbon nanotubes to an alkali metal source in the presence of an aprotic solvent, wherein the exposing opens the carbon nanotubes parallel to their longitudinal axis; and exposing the opened carbon nanotubes to a protic solvent to form unfunctionalized graphene nanoribbons.
24. The method of claim 22, wherein the method takes place at room temperature.
25. The method of claim 22, wherein the carbon nanotubes are selected from the group consisting of single-walled carbon nanotubes, double-walled carbon nanotubes, triple- walled carbon nanotubes, multi-walled carbon nanotubes, ultra-sho rt carbon nanotubes, and combinations thereof.
26. The method of claim 22, wherein the alkali metal source is selected from the group consisting of lithium, potassium, sodium, rubidium, eaesium cesium, alloys thereof, and combinations thereof.
27. The method of claim 22, wherein the aprotic solvent is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,4-dioxane, glyme, 1,2-dimethoxyethane, diglyme, tetraglyme, amines, N,N,N',N'-tetramethylethylenediamine, triethylamine, 1,4- diazabicyclo [2.2.2] octane, trialkylamines, dialkylarylamines, alkyldiarylamines, dimethylformamide, and combinations thereof.
28. The method of claim 22, wherein the protic solvent is selected from the group consisting of formic acid, n-butanol, isopropanol, n-propanol, ethanol, methanol, acetic acid, water, hydrochloric acid, sulfuric acid, ammonia, diethyl amine, dialkylamines, monoalkylamines, diarylamines, monoarylamines, monoalkymonoarylamines, and combinations thereof.
29. The method of claim 22, further comprising a step of adding an electrophile to the unfunctionalized graphene nanoribbons, wherein the electrophile functionalizes the graphene nanoribbons.
36. The method of claim 22, wherein the formed graphene nanoribbons have a conductivity ranging from about 0.1 S/cm to about 9,000 S/cm.
39. The method of claim 22, further comprising a step of exfoliating one or more layers of graphene from the formed graphene nanoribbons.
23. canceled
41. A composite comprising graphene nanoribbons, wherein the graphene nanoribbons are edge-functionalized. withdrawn
42. The composite of claim 41, wherein the graphene nanorribons contain unfunctionalized basal planes. withdrawn
43. The composite of claim 41, wherein the graphene nanoribbons are edge- functionalized with polymers. withdrawn
45. The composite of claim 41, wherein the graphene nanoribbons are edge- functionalized with functional groups selected from the group consisting of alkyl groups, acyl groups, allylic groups, benzyl groups, benzylic groups, alkenyl groups, aryl groups, alkynyl groups, aldehydes, ketones, esters, carboxyl groups, carbonyl groups, halogens, and combinations thereof. withdrawn
46. The composite of claim 41, wherein the edge-functionalized graphene nanorribons comprise at least one of alkyl-functionalized graphene nanoribbons, hexadecylated graphene nanoribbons, octylated graphene nanoribbons, butylated graphene nanoribbons, and combinations thereof. withdrawn
47. The composite of claim 41, wherein the composites are utilized as components of at least one of transparent conductive displays, de-icing circuits, gas barrier composites, screens, and combinations thereof. withdrawn
48. A fiber comprising graphene nanoribbons, wherein the graphene nanoribbons are edge-functionalized. withdrawn
49. The fiber of claim 48, wherein the graphene nanorribons contain unfunctionalized basal planes. withdrawn
50. The fiber of claim 48, wherein the graphene nanoribbons are edge- functionalized with polymers. withdrawn
51. The fiber of claim 48, wherein the polymers are selected from the group consisting of polystyrenes, polyisoprenes, polybutadienes, polyacrylonitriles, polymethyl vinyl ketones, poly alkyl acrylates, polyalkyl methacrylates, polyols, and combinations thereof. withdrawn
52. The fiber of claim 48, wherein the graphene nanoribbons are edge- functionalized with functional groups selected from the group consisting of alkyl groups, acyl groups, allylic groups, benzyl groups, benzylic groups, alkenyl groups, aryl groups, alkynyl groups, aldehydes, ketones, esters, carboxyl groups, carbonyl groups, halogens, and combinations thereof. withdrawn
53. The fiber of claim 48, wherein the edge-functionalized graphene nanorribons comprise at least one of alkyl-functionalized graphene nanoribbons, hexadecylated graphene nanoribbons, octylated graphene nanoribbons, butylated graphene nanoribbons, and combinations thereof. withdrawn
54. The fiber of claim 48, wherein the fibers are utilized as components of at least one of transparent conductive displays, de-icing circuits, gas barrier fibers, screens, and combinations thereof. withdrawn
Materials described outside the worked examples.
carbon nanotubes
alkali metal source
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2D illustrates the deintercalation of functionalized GNRs. [0017] FIGURE 3 provides scanning electron microscopy (SEM) images of various solubility tests. …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
conductivity of graphene nanoribbons | 0.1–9000 S/cm | graphene nanoribbons |
Temperature | 40–900 °C |
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Patent
Atlas literature
Patent
US 9,493,355Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1. For instance, in some embodiments that are illustrated in Panel I of
FIG. 2D illustrates the deintercalation of functionalized GNRs. [0017] FIGURE 3 provides scanning electron microscopy (SEM) images of various solubility tests. …
FIG. 3A shows an SEM image of pristine Mitsui MWNTs, and a 0.1 mg/mL suspension in chlorofo rm.
FIG. 4B). The images show that commercial MWNTs are non-dispersible in organic solvents after short sonication using an ultrasonic cleaner. However, HD-GNRs …
FIG. 5 B provides an optical microscope of NTL- originated functionalized HD-GNRs. [0020] FIGURE 6 shows an HD-GNR fabricated device and related conductivity …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 8B) of a single HD-GNR used in a device for conductivity measurements. AFM images were obtained with a Digital Instruments nanoscope III a, operating in …
FIG. 9B. Current and potential were then measured. [0024] FIGURE 10 provides calculation of the hypothetical degree of edge functionalization with HD groups …
FIG. 10). If all of the edge carbons are functionalized, then the functional groups would contribute 1 wt % of the total weight to the HD-GNRs; 0.5 wt % if …
FIG. 11 C) are shown. [0026] FIGURE 12 shows the EGA for hydrogen terminated GNRs (H-GNRs). The colors represent fragments with m/z 15 (red), 29 (orange), 43 …
FIG. 12). The methyl fragment could be the result of rea rr angements with successive cleavage on defects and edges where carbons are expected to be …
FIG. 13B shows comparison of functionalized HD-GNRs, O- GNRs, B-GNRs, GNRs and MWNTs. Peaks at 21.8 0, 25.3 0, 35.90, 42.4, 44.40, 51.8 0, 56.8 0, and 58.4 0 …
FIG. 14. [00166] The XRD diffractogram for the as-prepared sample contains well-pronounced diffraction lines at 12.0 0 and 24.2 0 20 angle, which co rr espond to …
FIG. 15). Interestingly, no intermediate stage compound was detected in the sample. [00168] Such results are unexpected for graphite intercalation compounds …
FIG. 16A is a GC plot (purple curve) of trapped (at 0 0 C) condensate from HD-GNRs heated at 150 ° C in high vacuum for 1 hour. The concentration of the …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 18). This is an additional argument in support of formation of the intercalation compound. It is known that when several species are intercalated into …
FIG. 19), where the (002) signal was observed at 26.2 0 20 angle, which corresponds to non-intercalated material. The results were also confirmed by TGA (
FIG. 20), where Applicants observed a weight loss of-2% in the region between room temperature and 800 °C. [00183] Summary [00184] In this Example, a high …
FIG. 21D shows the polymerization of the added monomers on the opened MWNTs and the subsequent formation of PF-GNRs upon quenching. For clarity, double bonds …
FIGS. 22-25. [00216] Thermogravimetric mass spectrometry (TG/MS) was used to qualitatively confirm the presence of the polystyrene chains, to estimate the …
FIG. 23B) SEM images are shown. The spherical nanoparticles are amorphous carbon byproducts. Thermal annealing at 2800 ° C under argon atmosphere improved the …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 27. [00218] Raman spectroscopy was also used to characterize the graphitic structure of the GNRs. An increase in the intensity of the D band over the G …
FIG. 28B provides representative SEM images of split MWNTs. The majority of MWNTs were split. Ribbon-like structure could be indentified in the image.
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 30C is an SEM image of NTL MWNTs after liquid-phase intercalation followed by addition of styrene. It is shown that NTL MWNTs are split but not completely …
FIG. 31B is an SEM image of Baytubes after liquid-phase intercalation followed by polymerization. The image shows that the Baytubes are split due to …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 33B is an SEM image of MWNTs treated with lithium naphthalenide followed by styrene. [0048] FIGURE 34 provides SEM images of carboxyl-functionalized GNRs …
FIG. 34B is 2 m. [0049] FIGURE 35 provides TEM images of GNR-(COOH)n. The scale bar in
FIG. 35B is 10 nm. [0050] FIGURE 36 provides the Raman spectrum of GNR-(COOH)n. The excitation laser wavelength is 514 nm.
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1. A method of preparing functionalized graphene nanoribbons, wherein the method comprises: exposing a plurality of carbon nanotubes to an alkali metal source in the presence of an aprotic solvent, wherein the exposing opens the carbon nanotubes; and exposing the opened carbon nanotubes to an electrophile to form functionalized graphene nanoribbons. withdrawn
2. The method of claim 1, further comprising a step of exposing the opened carbon nanotubes to a protic solvent. withdrawn
4. The method of claim 1, wherein the carbon nanotubes are opened parallel to their longitudinal axis. withdrawn
5. The method of claim 1, wherein the method takes place at room temperature. withdrawn
6. The method of claim 1, wherein the carbon nanotubes are selected from the group consisting of single-walled carbon nanotubes, double-walled carbon nanotubes, triple- walled carbon nanotubes, multi-walled carbon nanotubes, ultra-sho rt carbon nanotubes, and combinations thereof. withdrawn
7. The method of claim 1, wherein the carbon nanotubes comprise multi-walled carbon nanotubes. withdrawn
8. The method of claim 1, wherein the alkali metal source is selected from the group consisting of lithium, potassium, sodium, rubidium, caesium, alloys thereof, and combinations thereof. withdrawn
9. The method of claim 1, wherein the alkali metal source comprises potassium. withdrawn
10. The method of claim 1, wherein the aprotic solvent is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,4-dioxane, glyme, 1,2-dimethoxyethane, diglyme, tetraglyme, amines, N,N,N',N'-tetramethylethylenediamine, triethylamine, 1,4- diazabicyclo[2.2.2] octane, trialkylamines, dialkylarylamines, alkyldiarylamines, dimethylformamide, and combinations thereof. withdrawn
11. The method of claim 1, wherein the electrophile is selected from the group consisting of water, alcohols, organic halides, alkenes, alkyl halides, acyl halides, allylic halides, benzyl halides, benzylic halides, alkenyl halides, aryl halides, alkynyl halides, fluoralkly halides, perfluoroalkyl halides, aldehydes, ketones, methyl vinyl ketones, esters, sulfonate esters, acids, acid chlorides, carboxylic acids, carboxylic esters, carboxylic acid chlorides, carboxylic acid 3 Application No. 14/345,016 Docket No.: 11321-P₂₃₁WOUS Amendment dated Reply to Office Action of anhydrides, carbonyl bearing compounds, enones, nitriles, carbon dioxide, halogens, monomers, vinyl monomers, ring-opening monomers, isoprenes, butadienes, styrenes, acrylonitriles, methyl vinyl ketones, methacrylates, 1,4-dimethoxy-2-vinylbenzene, methyl methacrylate, alkyl acrylates, alkyl methacrylates, trimethylsilyl chlorides, tert-butyldimethylsilyl chlorides, triphenylsilyl chlorides, epoxides, carbon dioxide, carbon disulfide, tert-butanol, 2- methylpropene, bromine, chlorine, iodine, fluorine, and combinations thereof. withdrawn
12. The method of claim 1, wherein the electrophile comprises carbon dioxide. withdrawn
13. The method of claim 1, wherein the electrophile is a monomer. withdrawn
16. The method of claim 1, wherein the formed graphene nanoribbons comprise edge-functionalized graphene nanoribbons. withdrawn
17. The method of claim 1, wherein the formed graphene nanoribbons have a conductivity ranging from about 0.1 S/cm to about 9,000 S/cm. withdrawn
18. The method of claim 1, further comprising a step of deintercalating functional groups from one or more layers of graphene nanoribbons. withdrawn
20. The method of claim 1, further comprising a step of exfoliating one or more layers of graphene from the formed graphene nanoribbons. withdrawn
22. A method of preparing graphene nanoribbons, wherein the method comprises: exposing a plurality of carbon nanotubes to an alkali metal source in the presence of an aprotic solvent, wherein the exposing opens the carbon nanotubes parallel to their longitudinal axis; and exposing the opened carbon nanotubes to a protic solvent to form unfunctionalized graphene nanoribbons.
24. The method of claim 22, wherein the method takes place at room temperature.
25. The method of claim 22, wherein the carbon nanotubes are selected from the group consisting of single-walled carbon nanotubes, double-walled carbon nanotubes, triple- walled carbon nanotubes, multi-walled carbon nanotubes, ultra-sho rt carbon nanotubes, and combinations thereof.
26. The method of claim 22, wherein the alkali metal source is selected from the group consisting of lithium, potassium, sodium, rubidium, eaesium cesium, alloys thereof, and combinations thereof.
27. The method of claim 22, wherein the aprotic solvent is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,4-dioxane, glyme, 1,2-dimethoxyethane, diglyme, tetraglyme, amines, N,N,N',N'-tetramethylethylenediamine, triethylamine, 1,4- diazabicyclo [2.2.2] octane, trialkylamines, dialkylarylamines, alkyldiarylamines, dimethylformamide, and combinations thereof.
28. The method of claim 22, wherein the protic solvent is selected from the group consisting of formic acid, n-butanol, isopropanol, n-propanol, ethanol, methanol, acetic acid, water, hydrochloric acid, sulfuric acid, ammonia, diethyl amine, dialkylamines, monoalkylamines, diarylamines, monoarylamines, monoalkymonoarylamines, and combinations thereof.
29. The method of claim 22, further comprising a step of adding an electrophile to the unfunctionalized graphene nanoribbons, wherein the electrophile functionalizes the graphene nanoribbons.
36. The method of claim 22, wherein the formed graphene nanoribbons have a conductivity ranging from about 0.1 S/cm to about 9,000 S/cm.
39. The method of claim 22, further comprising a step of exfoliating one or more layers of graphene from the formed graphene nanoribbons.
23. canceled
41. A composite comprising graphene nanoribbons, wherein the graphene nanoribbons are edge-functionalized. withdrawn
42. The composite of claim 41, wherein the graphene nanorribons contain unfunctionalized basal planes. withdrawn
43. The composite of claim 41, wherein the graphene nanoribbons are edge- functionalized with polymers. withdrawn
45. The composite of claim 41, wherein the graphene nanoribbons are edge- functionalized with functional groups selected from the group consisting of alkyl groups, acyl groups, allylic groups, benzyl groups, benzylic groups, alkenyl groups, aryl groups, alkynyl groups, aldehydes, ketones, esters, carboxyl groups, carbonyl groups, halogens, and combinations thereof. withdrawn
46. The composite of claim 41, wherein the edge-functionalized graphene nanorribons comprise at least one of alkyl-functionalized graphene nanoribbons, hexadecylated graphene nanoribbons, octylated graphene nanoribbons, butylated graphene nanoribbons, and combinations thereof. withdrawn
47. The composite of claim 41, wherein the composites are utilized as components of at least one of transparent conductive displays, de-icing circuits, gas barrier composites, screens, and combinations thereof. withdrawn
48. A fiber comprising graphene nanoribbons, wherein the graphene nanoribbons are edge-functionalized. withdrawn
49. The fiber of claim 48, wherein the graphene nanorribons contain unfunctionalized basal planes. withdrawn
50. The fiber of claim 48, wherein the graphene nanoribbons are edge- functionalized with polymers. withdrawn
51. The fiber of claim 48, wherein the polymers are selected from the group consisting of polystyrenes, polyisoprenes, polybutadienes, polyacrylonitriles, polymethyl vinyl ketones, poly alkyl acrylates, polyalkyl methacrylates, polyols, and combinations thereof. withdrawn
52. The fiber of claim 48, wherein the graphene nanoribbons are edge- functionalized with functional groups selected from the group consisting of alkyl groups, acyl groups, allylic groups, benzyl groups, benzylic groups, alkenyl groups, aryl groups, alkynyl groups, aldehydes, ketones, esters, carboxyl groups, carbonyl groups, halogens, and combinations thereof. withdrawn
53. The fiber of claim 48, wherein the edge-functionalized graphene nanorribons comprise at least one of alkyl-functionalized graphene nanoribbons, hexadecylated graphene nanoribbons, octylated graphene nanoribbons, butylated graphene nanoribbons, and combinations thereof. withdrawn
54. The fiber of claim 48, wherein the fibers are utilized as components of at least one of transparent conductive displays, de-icing circuits, gas barrier fibers, screens, and combinations thereof. withdrawn
Materials described outside the worked examples.
carbon nanotubes
alkali metal source
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2D illustrates the deintercalation of functionalized GNRs. [0017] FIGURE 3 provides scanning electron microscopy (SEM) images of various solubility tests. …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
conductivity of graphene nanoribbons | 0.1–9000 S/cm | graphene nanoribbons |
Temperature | 40–900 °C |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,493,355Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1. For instance, in some embodiments that are illustrated in Panel I of
FIG. 2D illustrates the deintercalation of functionalized GNRs. [0017] FIGURE 3 provides scanning electron microscopy (SEM) images of various solubility tests. …
FIG. 3A shows an SEM image of pristine Mitsui MWNTs, and a 0.1 mg/mL suspension in chlorofo rm.
FIG. 4B). The images show that commercial MWNTs are non-dispersible in organic solvents after short sonication using an ultrasonic cleaner. However, HD-GNRs …
FIG. 5 B provides an optical microscope of NTL- originated functionalized HD-GNRs. [0020] FIGURE 6 shows an HD-GNR fabricated device and related conductivity …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 8B) of a single HD-GNR used in a device for conductivity measurements. AFM images were obtained with a Digital Instruments nanoscope III a, operating in …
FIG. 9B. Current and potential were then measured. [0024] FIGURE 10 provides calculation of the hypothetical degree of edge functionalization with HD groups …
FIG. 10). If all of the edge carbons are functionalized, then the functional groups would contribute 1 wt % of the total weight to the HD-GNRs; 0.5 wt % if …
FIG. 11 C) are shown. [0026] FIGURE 12 shows the EGA for hydrogen terminated GNRs (H-GNRs). The colors represent fragments with m/z 15 (red), 29 (orange), 43 …
FIG. 12). The methyl fragment could be the result of rea rr angements with successive cleavage on defects and edges where carbons are expected to be …
FIG. 13B shows comparison of functionalized HD-GNRs, O- GNRs, B-GNRs, GNRs and MWNTs. Peaks at 21.8 0, 25.3 0, 35.90, 42.4, 44.40, 51.8 0, 56.8 0, and 58.4 0 …
FIG. 14. [00166] The XRD diffractogram for the as-prepared sample contains well-pronounced diffraction lines at 12.0 0 and 24.2 0 20 angle, which co rr espond to …
FIG. 15). Interestingly, no intermediate stage compound was detected in the sample. [00168] Such results are unexpected for graphite intercalation compounds …
FIG. 16A is a GC plot (purple curve) of trapped (at 0 0 C) condensate from HD-GNRs heated at 150 ° C in high vacuum for 1 hour. The concentration of the …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 18). This is an additional argument in support of formation of the intercalation compound. It is known that when several species are intercalated into …
FIG. 19), where the (002) signal was observed at 26.2 0 20 angle, which corresponds to non-intercalated material. The results were also confirmed by TGA (
FIG. 20), where Applicants observed a weight loss of-2% in the region between room temperature and 800 °C. [00183] Summary [00184] In this Example, a high …
FIG. 21D shows the polymerization of the added monomers on the opened MWNTs and the subsequent formation of PF-GNRs upon quenching. For clarity, double bonds …
FIGS. 22-25. [00216] Thermogravimetric mass spectrometry (TG/MS) was used to qualitatively confirm the presence of the polystyrene chains, to estimate the …
FIG. 23B) SEM images are shown. The spherical nanoparticles are amorphous carbon byproducts. Thermal annealing at 2800 ° C under argon atmosphere improved the …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 27. [00218] Raman spectroscopy was also used to characterize the graphitic structure of the GNRs. An increase in the intensity of the D band over the G …
FIG. 28B provides representative SEM images of split MWNTs. The majority of MWNTs were split. Ribbon-like structure could be indentified in the image.
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 30C is an SEM image of NTL MWNTs after liquid-phase intercalation followed by addition of styrene. It is shown that NTL MWNTs are split but not completely …
FIG. 31B is an SEM image of Baytubes after liquid-phase intercalation followed by polymerization. The image shows that the Baytubes are split due to …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 33B is an SEM image of MWNTs treated with lithium naphthalenide followed by styrene. [0048] FIGURE 34 provides SEM images of carboxyl-functionalized GNRs …
FIG. 34B is 2 m. [0049] FIGURE 35 provides TEM images of GNR-(COOH)n. The scale bar in
FIG. 35B is 10 nm. [0050] FIGURE 36 provides the Raman spectrum of GNR-(COOH)n. The excitation laser wavelength is 514 nm.
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1. A method of preparing functionalized graphene nanoribbons, wherein the method comprises: exposing a plurality of carbon nanotubes to an alkali metal source in the presence of an aprotic solvent, wherein the exposing opens the carbon nanotubes; and exposing the opened carbon nanotubes to an electrophile to form functionalized graphene nanoribbons. withdrawn
2. The method of claim 1, further comprising a step of exposing the opened carbon nanotubes to a protic solvent. withdrawn
4. The method of claim 1, wherein the carbon nanotubes are opened parallel to their longitudinal axis. withdrawn
5. The method of claim 1, wherein the method takes place at room temperature. withdrawn
6. The method of claim 1, wherein the carbon nanotubes are selected from the group consisting of single-walled carbon nanotubes, double-walled carbon nanotubes, triple- walled carbon nanotubes, multi-walled carbon nanotubes, ultra-sho rt carbon nanotubes, and combinations thereof. withdrawn
7. The method of claim 1, wherein the carbon nanotubes comprise multi-walled carbon nanotubes. withdrawn
8. The method of claim 1, wherein the alkali metal source is selected from the group consisting of lithium, potassium, sodium, rubidium, caesium, alloys thereof, and combinations thereof. withdrawn
9. The method of claim 1, wherein the alkali metal source comprises potassium. withdrawn
10. The method of claim 1, wherein the aprotic solvent is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,4-dioxane, glyme, 1,2-dimethoxyethane, diglyme, tetraglyme, amines, N,N,N',N'-tetramethylethylenediamine, triethylamine, 1,4- diazabicyclo[2.2.2] octane, trialkylamines, dialkylarylamines, alkyldiarylamines, dimethylformamide, and combinations thereof. withdrawn
11. The method of claim 1, wherein the electrophile is selected from the group consisting of water, alcohols, organic halides, alkenes, alkyl halides, acyl halides, allylic halides, benzyl halides, benzylic halides, alkenyl halides, aryl halides, alkynyl halides, fluoralkly halides, perfluoroalkyl halides, aldehydes, ketones, methyl vinyl ketones, esters, sulfonate esters, acids, acid chlorides, carboxylic acids, carboxylic esters, carboxylic acid chlorides, carboxylic acid 3 Application No. 14/345,016 Docket No.: 11321-P₂₃₁WOUS Amendment dated Reply to Office Action of anhydrides, carbonyl bearing compounds, enones, nitriles, carbon dioxide, halogens, monomers, vinyl monomers, ring-opening monomers, isoprenes, butadienes, styrenes, acrylonitriles, methyl vinyl ketones, methacrylates, 1,4-dimethoxy-2-vinylbenzene, methyl methacrylate, alkyl acrylates, alkyl methacrylates, trimethylsilyl chlorides, tert-butyldimethylsilyl chlorides, triphenylsilyl chlorides, epoxides, carbon dioxide, carbon disulfide, tert-butanol, 2- methylpropene, bromine, chlorine, iodine, fluorine, and combinations thereof. withdrawn
12. The method of claim 1, wherein the electrophile comprises carbon dioxide. withdrawn
13. The method of claim 1, wherein the electrophile is a monomer. withdrawn
16. The method of claim 1, wherein the formed graphene nanoribbons comprise edge-functionalized graphene nanoribbons. withdrawn
17. The method of claim 1, wherein the formed graphene nanoribbons have a conductivity ranging from about 0.1 S/cm to about 9,000 S/cm. withdrawn
18. The method of claim 1, further comprising a step of deintercalating functional groups from one or more layers of graphene nanoribbons. withdrawn
20. The method of claim 1, further comprising a step of exfoliating one or more layers of graphene from the formed graphene nanoribbons. withdrawn
22. A method of preparing graphene nanoribbons, wherein the method comprises: exposing a plurality of carbon nanotubes to an alkali metal source in the presence of an aprotic solvent, wherein the exposing opens the carbon nanotubes parallel to their longitudinal axis; and exposing the opened carbon nanotubes to a protic solvent to form unfunctionalized graphene nanoribbons.
24. The method of claim 22, wherein the method takes place at room temperature.
25. The method of claim 22, wherein the carbon nanotubes are selected from the group consisting of single-walled carbon nanotubes, double-walled carbon nanotubes, triple- walled carbon nanotubes, multi-walled carbon nanotubes, ultra-sho rt carbon nanotubes, and combinations thereof.
26. The method of claim 22, wherein the alkali metal source is selected from the group consisting of lithium, potassium, sodium, rubidium, eaesium cesium, alloys thereof, and combinations thereof.
27. The method of claim 22, wherein the aprotic solvent is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,4-dioxane, glyme, 1,2-dimethoxyethane, diglyme, tetraglyme, amines, N,N,N',N'-tetramethylethylenediamine, triethylamine, 1,4- diazabicyclo [2.2.2] octane, trialkylamines, dialkylarylamines, alkyldiarylamines, dimethylformamide, and combinations thereof.
28. The method of claim 22, wherein the protic solvent is selected from the group consisting of formic acid, n-butanol, isopropanol, n-propanol, ethanol, methanol, acetic acid, water, hydrochloric acid, sulfuric acid, ammonia, diethyl amine, dialkylamines, monoalkylamines, diarylamines, monoarylamines, monoalkymonoarylamines, and combinations thereof.
29. The method of claim 22, further comprising a step of adding an electrophile to the unfunctionalized graphene nanoribbons, wherein the electrophile functionalizes the graphene nanoribbons.
36. The method of claim 22, wherein the formed graphene nanoribbons have a conductivity ranging from about 0.1 S/cm to about 9,000 S/cm.
39. The method of claim 22, further comprising a step of exfoliating one or more layers of graphene from the formed graphene nanoribbons.
23. canceled
41. A composite comprising graphene nanoribbons, wherein the graphene nanoribbons are edge-functionalized. withdrawn
42. The composite of claim 41, wherein the graphene nanorribons contain unfunctionalized basal planes. withdrawn
43. The composite of claim 41, wherein the graphene nanoribbons are edge- functionalized with polymers. withdrawn
45. The composite of claim 41, wherein the graphene nanoribbons are edge- functionalized with functional groups selected from the group consisting of alkyl groups, acyl groups, allylic groups, benzyl groups, benzylic groups, alkenyl groups, aryl groups, alkynyl groups, aldehydes, ketones, esters, carboxyl groups, carbonyl groups, halogens, and combinations thereof. withdrawn
46. The composite of claim 41, wherein the edge-functionalized graphene nanorribons comprise at least one of alkyl-functionalized graphene nanoribbons, hexadecylated graphene nanoribbons, octylated graphene nanoribbons, butylated graphene nanoribbons, and combinations thereof. withdrawn
47. The composite of claim 41, wherein the composites are utilized as components of at least one of transparent conductive displays, de-icing circuits, gas barrier composites, screens, and combinations thereof. withdrawn
48. A fiber comprising graphene nanoribbons, wherein the graphene nanoribbons are edge-functionalized. withdrawn
49. The fiber of claim 48, wherein the graphene nanorribons contain unfunctionalized basal planes. withdrawn
50. The fiber of claim 48, wherein the graphene nanoribbons are edge- functionalized with polymers. withdrawn
51. The fiber of claim 48, wherein the polymers are selected from the group consisting of polystyrenes, polyisoprenes, polybutadienes, polyacrylonitriles, polymethyl vinyl ketones, poly alkyl acrylates, polyalkyl methacrylates, polyols, and combinations thereof. withdrawn
52. The fiber of claim 48, wherein the graphene nanoribbons are edge- functionalized with functional groups selected from the group consisting of alkyl groups, acyl groups, allylic groups, benzyl groups, benzylic groups, alkenyl groups, aryl groups, alkynyl groups, aldehydes, ketones, esters, carboxyl groups, carbonyl groups, halogens, and combinations thereof. withdrawn
53. The fiber of claim 48, wherein the edge-functionalized graphene nanorribons comprise at least one of alkyl-functionalized graphene nanoribbons, hexadecylated graphene nanoribbons, octylated graphene nanoribbons, butylated graphene nanoribbons, and combinations thereof. withdrawn
54. The fiber of claim 48, wherein the fibers are utilized as components of at least one of transparent conductive displays, de-icing circuits, gas barrier fibers, screens, and combinations thereof. withdrawn
Materials described outside the worked examples.
carbon nanotubes
alkali metal source
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2D illustrates the deintercalation of functionalized GNRs. [0017] FIGURE 3 provides scanning electron microscopy (SEM) images of various solubility tests. …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
conductivity of graphene nanoribbons | 0.1–9000 S/cm | graphene nanoribbons |
Temperature | 40–900 °C |
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US 9,493,355Patent drawings and their descriptions. Click a drawing to enlarge it.
FIG. 1. For instance, in some embodiments that are illustrated in Panel I of
FIG. 2D illustrates the deintercalation of functionalized GNRs. [0017] FIGURE 3 provides scanning electron microscopy (SEM) images of various solubility tests. …
FIG. 3A shows an SEM image of pristine Mitsui MWNTs, and a 0.1 mg/mL suspension in chlorofo rm.
FIG. 4B). The images show that commercial MWNTs are non-dispersible in organic solvents after short sonication using an ultrasonic cleaner. However, HD-GNRs …
FIG. 5 B provides an optical microscope of NTL- originated functionalized HD-GNRs. [0020] FIGURE 6 shows an HD-GNR fabricated device and related conductivity …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 8B) of a single HD-GNR used in a device for conductivity measurements. AFM images were obtained with a Digital Instruments nanoscope III a, operating in …
FIG. 9B. Current and potential were then measured. [0024] FIGURE 10 provides calculation of the hypothetical degree of edge functionalization with HD groups …
FIG. 10). If all of the edge carbons are functionalized, then the functional groups would contribute 1 wt % of the total weight to the HD-GNRs; 0.5 wt % if …
FIG. 11 C) are shown. [0026] FIGURE 12 shows the EGA for hydrogen terminated GNRs (H-GNRs). The colors represent fragments with m/z 15 (red), 29 (orange), 43 …
FIG. 12). The methyl fragment could be the result of rea rr angements with successive cleavage on defects and edges where carbons are expected to be …
FIG. 13B shows comparison of functionalized HD-GNRs, O- GNRs, B-GNRs, GNRs and MWNTs. Peaks at 21.8 0, 25.3 0, 35.90, 42.4, 44.40, 51.8 0, 56.8 0, and 58.4 0 …
FIG. 14. [00166] The XRD diffractogram for the as-prepared sample contains well-pronounced diffraction lines at 12.0 0 and 24.2 0 20 angle, which co rr espond to …
FIG. 15). Interestingly, no intermediate stage compound was detected in the sample. [00168] Such results are unexpected for graphite intercalation compounds …
FIG. 16A is a GC plot (purple curve) of trapped (at 0 0 C) condensate from HD-GNRs heated at 150 ° C in high vacuum for 1 hour. The concentration of the …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 18). This is an additional argument in support of formation of the intercalation compound. It is known that when several species are intercalated into …
FIG. 19), where the (002) signal was observed at 26.2 0 20 angle, which corresponds to non-intercalated material. The results were also confirmed by TGA (
FIG. 20), where Applicants observed a weight loss of-2% in the region between room temperature and 800 °C. [00183] Summary [00184] In this Example, a high …
FIG. 21D shows the polymerization of the added monomers on the opened MWNTs and the subsequent formation of PF-GNRs upon quenching. For clarity, double bonds …
FIGS. 22-25. [00216] Thermogravimetric mass spectrometry (TG/MS) was used to qualitatively confirm the presence of the polystyrene chains, to estimate the …
FIG. 23B) SEM images are shown. The spherical nanoparticles are amorphous carbon byproducts. Thermal annealing at 2800 ° C under argon atmosphere improved the …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 27. [00218] Raman spectroscopy was also used to characterize the graphitic structure of the GNRs. An increase in the intensity of the D band over the G …
FIG. 28B provides representative SEM images of split MWNTs. The majority of MWNTs were split. Ribbon-like structure could be indentified in the image.
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 30C is an SEM image of NTL MWNTs after liquid-phase intercalation followed by addition of styrene. It is shown that NTL MWNTs are split but not completely …
FIG. 31B is an SEM image of Baytubes after liquid-phase intercalation followed by polymerization. The image shows that the Baytubes are split due to …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 33B is an SEM image of MWNTs treated with lithium naphthalenide followed by styrene. [0048] FIGURE 34 provides SEM images of carboxyl-functionalized GNRs …
FIG. 34B is 2 m. [0049] FIGURE 35 provides TEM images of GNR-(COOH)n. The scale bar in
FIG. 35B is 10 nm. [0050] FIGURE 36 provides the Raman spectrum of GNR-(COOH)n. The excitation laser wavelength is 514 nm.
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
1. A method of preparing functionalized graphene nanoribbons, wherein the method comprises: exposing a plurality of carbon nanotubes to an alkali metal source in the presence of an aprotic solvent, wherein the exposing opens the carbon nanotubes; and exposing the opened carbon nanotubes to an electrophile to form functionalized graphene nanoribbons. withdrawn
2. The method of claim 1, further comprising a step of exposing the opened carbon nanotubes to a protic solvent. withdrawn
4. The method of claim 1, wherein the carbon nanotubes are opened parallel to their longitudinal axis. withdrawn
5. The method of claim 1, wherein the method takes place at room temperature. withdrawn
6. The method of claim 1, wherein the carbon nanotubes are selected from the group consisting of single-walled carbon nanotubes, double-walled carbon nanotubes, triple- walled carbon nanotubes, multi-walled carbon nanotubes, ultra-sho rt carbon nanotubes, and combinations thereof. withdrawn
7. The method of claim 1, wherein the carbon nanotubes comprise multi-walled carbon nanotubes. withdrawn
8. The method of claim 1, wherein the alkali metal source is selected from the group consisting of lithium, potassium, sodium, rubidium, caesium, alloys thereof, and combinations thereof. withdrawn
9. The method of claim 1, wherein the alkali metal source comprises potassium. withdrawn
10. The method of claim 1, wherein the aprotic solvent is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,4-dioxane, glyme, 1,2-dimethoxyethane, diglyme, tetraglyme, amines, N,N,N',N'-tetramethylethylenediamine, triethylamine, 1,4- diazabicyclo[2.2.2] octane, trialkylamines, dialkylarylamines, alkyldiarylamines, dimethylformamide, and combinations thereof. withdrawn
11. The method of claim 1, wherein the electrophile is selected from the group consisting of water, alcohols, organic halides, alkenes, alkyl halides, acyl halides, allylic halides, benzyl halides, benzylic halides, alkenyl halides, aryl halides, alkynyl halides, fluoralkly halides, perfluoroalkyl halides, aldehydes, ketones, methyl vinyl ketones, esters, sulfonate esters, acids, acid chlorides, carboxylic acids, carboxylic esters, carboxylic acid chlorides, carboxylic acid 3 Application No. 14/345,016 Docket No.: 11321-P₂₃₁WOUS Amendment dated Reply to Office Action of anhydrides, carbonyl bearing compounds, enones, nitriles, carbon dioxide, halogens, monomers, vinyl monomers, ring-opening monomers, isoprenes, butadienes, styrenes, acrylonitriles, methyl vinyl ketones, methacrylates, 1,4-dimethoxy-2-vinylbenzene, methyl methacrylate, alkyl acrylates, alkyl methacrylates, trimethylsilyl chlorides, tert-butyldimethylsilyl chlorides, triphenylsilyl chlorides, epoxides, carbon dioxide, carbon disulfide, tert-butanol, 2- methylpropene, bromine, chlorine, iodine, fluorine, and combinations thereof. withdrawn
12. The method of claim 1, wherein the electrophile comprises carbon dioxide. withdrawn
13. The method of claim 1, wherein the electrophile is a monomer. withdrawn
16. The method of claim 1, wherein the formed graphene nanoribbons comprise edge-functionalized graphene nanoribbons. withdrawn
17. The method of claim 1, wherein the formed graphene nanoribbons have a conductivity ranging from about 0.1 S/cm to about 9,000 S/cm. withdrawn
18. The method of claim 1, further comprising a step of deintercalating functional groups from one or more layers of graphene nanoribbons. withdrawn
20. The method of claim 1, further comprising a step of exfoliating one or more layers of graphene from the formed graphene nanoribbons. withdrawn
22. A method of preparing graphene nanoribbons, wherein the method comprises: exposing a plurality of carbon nanotubes to an alkali metal source in the presence of an aprotic solvent, wherein the exposing opens the carbon nanotubes parallel to their longitudinal axis; and exposing the opened carbon nanotubes to a protic solvent to form unfunctionalized graphene nanoribbons.
24. The method of claim 22, wherein the method takes place at room temperature.
25. The method of claim 22, wherein the carbon nanotubes are selected from the group consisting of single-walled carbon nanotubes, double-walled carbon nanotubes, triple- walled carbon nanotubes, multi-walled carbon nanotubes, ultra-sho rt carbon nanotubes, and combinations thereof.
26. The method of claim 22, wherein the alkali metal source is selected from the group consisting of lithium, potassium, sodium, rubidium, eaesium cesium, alloys thereof, and combinations thereof.
27. The method of claim 22, wherein the aprotic solvent is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,4-dioxane, glyme, 1,2-dimethoxyethane, diglyme, tetraglyme, amines, N,N,N',N'-tetramethylethylenediamine, triethylamine, 1,4- diazabicyclo [2.2.2] octane, trialkylamines, dialkylarylamines, alkyldiarylamines, dimethylformamide, and combinations thereof.
28. The method of claim 22, wherein the protic solvent is selected from the group consisting of formic acid, n-butanol, isopropanol, n-propanol, ethanol, methanol, acetic acid, water, hydrochloric acid, sulfuric acid, ammonia, diethyl amine, dialkylamines, monoalkylamines, diarylamines, monoarylamines, monoalkymonoarylamines, and combinations thereof.
29. The method of claim 22, further comprising a step of adding an electrophile to the unfunctionalized graphene nanoribbons, wherein the electrophile functionalizes the graphene nanoribbons.
36. The method of claim 22, wherein the formed graphene nanoribbons have a conductivity ranging from about 0.1 S/cm to about 9,000 S/cm.
39. The method of claim 22, further comprising a step of exfoliating one or more layers of graphene from the formed graphene nanoribbons.
23. canceled
41. A composite comprising graphene nanoribbons, wherein the graphene nanoribbons are edge-functionalized. withdrawn
42. The composite of claim 41, wherein the graphene nanorribons contain unfunctionalized basal planes. withdrawn
43. The composite of claim 41, wherein the graphene nanoribbons are edge- functionalized with polymers. withdrawn
45. The composite of claim 41, wherein the graphene nanoribbons are edge- functionalized with functional groups selected from the group consisting of alkyl groups, acyl groups, allylic groups, benzyl groups, benzylic groups, alkenyl groups, aryl groups, alkynyl groups, aldehydes, ketones, esters, carboxyl groups, carbonyl groups, halogens, and combinations thereof. withdrawn
46. The composite of claim 41, wherein the edge-functionalized graphene nanorribons comprise at least one of alkyl-functionalized graphene nanoribbons, hexadecylated graphene nanoribbons, octylated graphene nanoribbons, butylated graphene nanoribbons, and combinations thereof. withdrawn
47. The composite of claim 41, wherein the composites are utilized as components of at least one of transparent conductive displays, de-icing circuits, gas barrier composites, screens, and combinations thereof. withdrawn
48. A fiber comprising graphene nanoribbons, wherein the graphene nanoribbons are edge-functionalized. withdrawn
49. The fiber of claim 48, wherein the graphene nanorribons contain unfunctionalized basal planes. withdrawn
50. The fiber of claim 48, wherein the graphene nanoribbons are edge- functionalized with polymers. withdrawn
51. The fiber of claim 48, wherein the polymers are selected from the group consisting of polystyrenes, polyisoprenes, polybutadienes, polyacrylonitriles, polymethyl vinyl ketones, poly alkyl acrylates, polyalkyl methacrylates, polyols, and combinations thereof. withdrawn
52. The fiber of claim 48, wherein the graphene nanoribbons are edge- functionalized with functional groups selected from the group consisting of alkyl groups, acyl groups, allylic groups, benzyl groups, benzylic groups, alkenyl groups, aryl groups, alkynyl groups, aldehydes, ketones, esters, carboxyl groups, carbonyl groups, halogens, and combinations thereof. withdrawn
53. The fiber of claim 48, wherein the edge-functionalized graphene nanorribons comprise at least one of alkyl-functionalized graphene nanoribbons, hexadecylated graphene nanoribbons, octylated graphene nanoribbons, butylated graphene nanoribbons, and combinations thereof. withdrawn
54. The fiber of claim 48, wherein the fibers are utilized as components of at least one of transparent conductive displays, de-icing circuits, gas barrier fibers, screens, and combinations thereof. withdrawn
Materials described outside the worked examples.
carbon nanotubes
alkali metal source
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
FIG. 2D illustrates the deintercalation of functionalized GNRs. [0017] FIGURE 3 provides scanning electron microscopy (SEM) images of various solubility tests. …
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
conductivity of graphene nanoribbons | 0.1–9000 S/cm | graphene nanoribbons |
Temperature | 40–900 °C |
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aprotic solvent
electrophile
protic solvent
polymer-functionalized graphene nanoribbons
edge-functionalized graphene nanoribbons
graphene nanoribbons
unfunctionalized graphene nanoribbons
FIG. 3A shows an SEM image of pristine Mitsui MWNTs, and a 0.1 mg/mL suspension in chlorofo rm.
FIG. 5 B provides an optical microscope of NTL- originated functionalized HD-GNRs. [0020] FIGURE 6 shows an HD-GNR fabricated device and related conductivity …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 8B) of a single HD-GNR used in a device for conductivity measurements. AFM images were obtained with a Digital Instruments nanoscope III a, operating in …
FIG. 9B. Current and potential were then measured. [0024] FIGURE 10 provides calculation of the hypothetical degree of edge functionalization with HD groups …
FIG. 12). The methyl fragment could be the result of rea rr angements with successive cleavage on defects and edges where carbons are expected to be …
FIG. 14. [00166] The XRD diffractogram for the as-prepared sample contains well-pronounced diffraction lines at 12.0 0 and 24.2 0 20 angle, which co rr espond to …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 18). This is an additional argument in support of formation of the intercalation compound. It is known that when several species are intercalated into …
FIG. 23B) SEM images are shown. The spherical nanoparticles are amorphous carbon byproducts. Thermal annealing at 2800 ° C under argon atmosphere improved the …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 27. [00218] Raman spectroscopy was also used to characterize the graphitic structure of the GNRs. An increase in the intensity of the D band over the G …
FIG. 28B provides representative SEM images of split MWNTs. The majority of MWNTs were split. Ribbon-like structure could be indentified in the image.
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 30C is an SEM image of NTL MWNTs after liquid-phase intercalation followed by addition of styrene. It is shown that NTL MWNTs are split but not completely …
FIG. 31B is an SEM image of Baytubes after liquid-phase intercalation followed by polymerization. The image shows that the Baytubes are split due to …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 33B is an SEM image of MWNTs treated with lithium naphthalenide followed by styrene. [0048] FIGURE 34 provides SEM images of carboxyl-functionalized GNRs …
FIG. 34B is 2 m. [0049] FIGURE 35 provides TEM images of GNR-(COOH)n. The scale bar in
FIG. 35B is 10 nm. [0050] FIGURE 36 provides the Raman spectrum of GNR-(COOH)n. The excitation laser wavelength is 514 nm.
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
| — |
Temperature | 154–374 °C | — |
Temperature | 400–474 °C | — |
Temperature | 480–612 °C | — |
Temperature | 139–293 °C | — |
Temperature | 121–247 °C | — |
Temperature | 448–526 °C | — |
Temperature | 526–628 °C | — |
Temperature | 328–453 °C | — |
Temperature | 453–636 °C | — |
Temperature | 400–600 °C | — |
Temperature | 140–300 °C | — |
Temperature | 100–900 °C | — |
Temperature | 384–474 °C | — |
Temperature | 240–900 °C | — |
Temperature | 530–900 °C | — |
Temperature | 50–500 °C | — |
Temperature | 25–900 °C | — |
Pressure | 0.00001 Torr | — |
Pressure | ≤ 0.00001 Torr | — |
THREE-DIMENSIONAL (3D) PRINTING OF GRAPHENE MATERIALS
aprotic solvent
electrophile
protic solvent
polymer-functionalized graphene nanoribbons
edge-functionalized graphene nanoribbons
graphene nanoribbons
unfunctionalized graphene nanoribbons
FIG. 3A shows an SEM image of pristine Mitsui MWNTs, and a 0.1 mg/mL suspension in chlorofo rm.
FIG. 5 B provides an optical microscope of NTL- originated functionalized HD-GNRs. [0020] FIGURE 6 shows an HD-GNR fabricated device and related conductivity …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 8B) of a single HD-GNR used in a device for conductivity measurements. AFM images were obtained with a Digital Instruments nanoscope III a, operating in …
FIG. 9B. Current and potential were then measured. [0024] FIGURE 10 provides calculation of the hypothetical degree of edge functionalization with HD groups …
FIG. 12). The methyl fragment could be the result of rea rr angements with successive cleavage on defects and edges where carbons are expected to be …
FIG. 14. [00166] The XRD diffractogram for the as-prepared sample contains well-pronounced diffraction lines at 12.0 0 and 24.2 0 20 angle, which co rr espond to …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 18). This is an additional argument in support of formation of the intercalation compound. It is known that when several species are intercalated into …
FIG. 23B) SEM images are shown. The spherical nanoparticles are amorphous carbon byproducts. Thermal annealing at 2800 ° C under argon atmosphere improved the …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 27. [00218] Raman spectroscopy was also used to characterize the graphitic structure of the GNRs. An increase in the intensity of the D band over the G …
FIG. 28B provides representative SEM images of split MWNTs. The majority of MWNTs were split. Ribbon-like structure could be indentified in the image.
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 30C is an SEM image of NTL MWNTs after liquid-phase intercalation followed by addition of styrene. It is shown that NTL MWNTs are split but not completely …
FIG. 31B is an SEM image of Baytubes after liquid-phase intercalation followed by polymerization. The image shows that the Baytubes are split due to …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 33B is an SEM image of MWNTs treated with lithium naphthalenide followed by styrene. [0048] FIGURE 34 provides SEM images of carboxyl-functionalized GNRs …
FIG. 34B is 2 m. [0049] FIGURE 35 provides TEM images of GNR-(COOH)n. The scale bar in
FIG. 35B is 10 nm. [0050] FIGURE 36 provides the Raman spectrum of GNR-(COOH)n. The excitation laser wavelength is 514 nm.
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
| — |
Temperature | 154–374 °C | — |
Temperature | 400–474 °C | — |
Temperature | 480–612 °C | — |
Temperature | 139–293 °C | — |
Temperature | 121–247 °C | — |
Temperature | 448–526 °C | — |
Temperature | 526–628 °C | — |
Temperature | 328–453 °C | — |
Temperature | 453–636 °C | — |
Temperature | 400–600 °C | — |
Temperature | 140–300 °C | — |
Temperature | 100–900 °C | — |
Temperature | 384–474 °C | — |
Temperature | 240–900 °C | — |
Temperature | 530–900 °C | — |
Temperature | 50–500 °C | — |
Temperature | 25–900 °C | — |
Pressure | 0.00001 Torr | — |
Pressure | ≤ 0.00001 Torr | — |
THREE-DIMENSIONAL (3D) PRINTING OF GRAPHENE MATERIALS
aprotic solvent
electrophile
protic solvent
polymer-functionalized graphene nanoribbons
edge-functionalized graphene nanoribbons
graphene nanoribbons
unfunctionalized graphene nanoribbons
FIG. 3A shows an SEM image of pristine Mitsui MWNTs, and a 0.1 mg/mL suspension in chlorofo rm.
FIG. 5 B provides an optical microscope of NTL- originated functionalized HD-GNRs. [0020] FIGURE 6 shows an HD-GNR fabricated device and related conductivity …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 8B) of a single HD-GNR used in a device for conductivity measurements. AFM images were obtained with a Digital Instruments nanoscope III a, operating in …
FIG. 9B. Current and potential were then measured. [0024] FIGURE 10 provides calculation of the hypothetical degree of edge functionalization with HD groups …
FIG. 12). The methyl fragment could be the result of rea rr angements with successive cleavage on defects and edges where carbons are expected to be …
FIG. 14. [00166] The XRD diffractogram for the as-prepared sample contains well-pronounced diffraction lines at 12.0 0 and 24.2 0 20 angle, which co rr espond to …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 18). This is an additional argument in support of formation of the intercalation compound. It is known that when several species are intercalated into …
FIG. 23B) SEM images are shown. The spherical nanoparticles are amorphous carbon byproducts. Thermal annealing at 2800 ° C under argon atmosphere improved the …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 27. [00218] Raman spectroscopy was also used to characterize the graphitic structure of the GNRs. An increase in the intensity of the D band over the G …
FIG. 28B provides representative SEM images of split MWNTs. The majority of MWNTs were split. Ribbon-like structure could be indentified in the image.
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 30C is an SEM image of NTL MWNTs after liquid-phase intercalation followed by addition of styrene. It is shown that NTL MWNTs are split but not completely …
FIG. 31B is an SEM image of Baytubes after liquid-phase intercalation followed by polymerization. The image shows that the Baytubes are split due to …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 33B is an SEM image of MWNTs treated with lithium naphthalenide followed by styrene. [0048] FIGURE 34 provides SEM images of carboxyl-functionalized GNRs …
FIG. 34B is 2 m. [0049] FIGURE 35 provides TEM images of GNR-(COOH)n. The scale bar in
FIG. 35B is 10 nm. [0050] FIGURE 36 provides the Raman spectrum of GNR-(COOH)n. The excitation laser wavelength is 514 nm.
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
| — |
Temperature | 154–374 °C | — |
Temperature | 400–474 °C | — |
Temperature | 480–612 °C | — |
Temperature | 139–293 °C | — |
Temperature | 121–247 °C | — |
Temperature | 448–526 °C | — |
Temperature | 526–628 °C | — |
Temperature | 328–453 °C | — |
Temperature | 453–636 °C | — |
Temperature | 400–600 °C | — |
Temperature | 140–300 °C | — |
Temperature | 100–900 °C | — |
Temperature | 384–474 °C | — |
Temperature | 240–900 °C | — |
Temperature | 530–900 °C | — |
Temperature | 50–500 °C | — |
Temperature | 25–900 °C | — |
Pressure | 0.00001 Torr | — |
Pressure | ≤ 0.00001 Torr | — |
THREE-DIMENSIONAL (3D) PRINTING OF GRAPHENE MATERIALS
aprotic solvent
electrophile
protic solvent
polymer-functionalized graphene nanoribbons
edge-functionalized graphene nanoribbons
graphene nanoribbons
unfunctionalized graphene nanoribbons
FIG. 3A shows an SEM image of pristine Mitsui MWNTs, and a 0.1 mg/mL suspension in chlorofo rm.
FIG. 5 B provides an optical microscope of NTL- originated functionalized HD-GNRs. [0020] FIGURE 6 shows an HD-GNR fabricated device and related conductivity …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 6B shows change in electrical properties after different thermal treatment compared to as-prepared HD-GNRs. [0021] FIGURE 7 is an SEM image showing width …
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 7) and -30 nm thick. The thickness was estimated from the atomic force microscopy (AFM) image. See
FIG. 8B) of a single HD-GNR used in a device for conductivity measurements. AFM images were obtained with a Digital Instruments nanoscope III a, operating in …
FIG. 9B. Current and potential were then measured. [0024] FIGURE 10 provides calculation of the hypothetical degree of edge functionalization with HD groups …
FIG. 12). The methyl fragment could be the result of rea rr angements with successive cleavage on defects and edges where carbons are expected to be …
FIG. 14. [00166] The XRD diffractogram for the as-prepared sample contains well-pronounced diffraction lines at 12.0 0 and 24.2 0 20 angle, which co rr espond to …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 17) are the same as for the unheated sample (red curve) except for 85,000 scans. Parameters for the 1H- C CP spectrum of 100% silica (control sample) are …
FIG. 18). This is an additional argument in support of formation of the intercalation compound. It is known that when several species are intercalated into …
FIG. 23B) SEM images are shown. The spherical nanoparticles are amorphous carbon byproducts. Thermal annealing at 2800 ° C under argon atmosphere improved the …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 24B is a transmission electron microscope (TEM) image of the edge structure of multi-layered (5-layered) PF-GNRs. [0039] FIGURE 25 is an SEM image of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 26C provides x-ray photoelectron spectroscopy (XPS) of GNRs. The inset is high-resolution XPS C ls spectrum of GNRs, indicating GNRs are free of …
FIG. 27. [00218] Raman spectroscopy was also used to characterize the graphitic structure of the GNRs. An increase in the intensity of the D band over the G …
FIG. 28B provides representative SEM images of split MWNTs. The majority of MWNTs were split. Ribbon-like structure could be indentified in the image.
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 29A shows an SEM image of Mitsui MWNTs treated with potassium vapor followed by addition of isoprene. Most MWNTs are opened. However, they are not fully …
FIG. 30C is an SEM image of NTL MWNTs after liquid-phase intercalation followed by addition of styrene. It is shown that NTL MWNTs are split but not completely …
FIG. 31B is an SEM image of Baytubes after liquid-phase intercalation followed by polymerization. The image shows that the Baytubes are split due to …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 32B shows Raman spectra of Mitsui MWNTs, NTL MWNTs and Baytubes. Baytubes have the highest WO 2013/040356 PCT/US₂₀₁₂/055414 11 IDA G, indi c ating m os t …
FIG. 33B is an SEM image of MWNTs treated with lithium naphthalenide followed by styrene. [0048] FIGURE 34 provides SEM images of carboxyl-functionalized GNRs …
FIG. 34B is 2 m. [0049] FIGURE 35 provides TEM images of GNR-(COOH)n. The scale bar in
FIG. 35B is 10 nm. [0050] FIGURE 36 provides the Raman spectrum of GNR-(COOH)n. The excitation laser wavelength is 514 nm.
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
FIG. 36. In addition, the Raman spectrum showed that the ratio of D peak to G peak is 1: 3. The Raman spectrum utilized a 514 nm excitation laser. [00245] …
| — |
Temperature | 154–374 °C | — |
Temperature | 400–474 °C | — |
Temperature | 480–612 °C | — |
Temperature | 139–293 °C | — |
Temperature | 121–247 °C | — |
Temperature | 448–526 °C | — |
Temperature | 526–628 °C | — |
Temperature | 328–453 °C | — |
Temperature | 453–636 °C | — |
Temperature | 400–600 °C | — |
Temperature | 140–300 °C | — |
Temperature | 100–900 °C | — |
Temperature | 384–474 °C | — |
Temperature | 240–900 °C | — |
Temperature | 530–900 °C | — |
Temperature | 50–500 °C | — |
Temperature | 25–900 °C | — |
Pressure | 0.00001 Torr | — |
Pressure | ≤ 0.00001 Torr | — |
THREE-DIMENSIONAL (3D) PRINTING OF GRAPHENE MATERIALS
