Patent
US 9,376,537Process for Preparing Completely Delaminated Graphene Oxide/Rubber Nanocomposite
Li LIU
US
Copyright © 2026 Matter42. All rights reserved.
Patent
Atlas literature
Patent
US 9,376,537Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1 A and 1 B show atom force microscope (AFM) images of a graphene oxide in graphene oxide/water sol. The AFM images show that graphene oxide is present …
FIGS. 2A and 2B show transmission electron microscope (TEM) images of graphene oxide in a graphene oxide/water sol. The TEM images show that there are obvious …
FIGS. 3A and 3B show high resolution transmission electron microscope (HRTEM) images of a graphene oxide/styrene butadiene rubber nanocomposite (Example 4). …
FIG. 4. Example 1 8 [0030] Adding 10 g graphite oxide to 10 L water, treating by ultrasonic waves for 2 h at a power of 800 W, at a frequency of 1000 Hz, and …
FIG. 5B shows Akron abrasion Schalla m ach patte rn of a white carbon black/styrene butadiene rubber vulcanizate (Contrast 2). It is shown that the Schalla m …
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 preparing a dela m inated graphene oxide/rubber nanocomposite, the method comprising: (1) preparing a graphene oxide/water sol comprising dispersing graphene oxide in deionized water, and treating by ultrasonic waves at a power of 10-2000 W, and at a frequency of 10-20000 Hz, for 10 min-6 h at a temperature of 0-1000 C, to obtain the graphene oxide/water sol; (2) pretreating the graphene oxide/water sol comprising adding a surfactant to the graphene oxide/water sol, treating by ultrasonic waves for 5 m in-5 h or stirring for 5 m in-5 h at a stirring speed of 50-10000 r/min to obtain a pretreated graphene oxide/water dispersion; (3) preparing a graphene oxide/rubber compounding emulsion comprising treating the graphene oxide/water sol or the graphene oxide/water dispersion in addition to a rubber latex by ultrasonic waves for min-6 h, or stirring the graphene oxide/water sol or the graphene oxide/water dispersion in addition to the rubber latex for 10 min-6 h at a stirring speed of 5 0- 10000 r/min, to obtain a stabilized graphene oxide/rubber compounding emulsion; (4) preparing the graphene oxide/rubber nanocomposite comprising selecting one of the following processes to prepare the graphene oxide/rubber nanocomposite: A) ion flocculation process comprising adding a flocculant which demulsifies the graphene oxide/rubber compounding emulsion to perform flocculation, dehydrating and drying a flocculate of the flocculation to obtain the graphene oxide/rubber nanocomposite; and B) spray drying process comprising passing the graphene 44 oxide/rubber compounding emulsion through a spray drier to produce small composite liquid drops, and dehydrating the composite liquid drops in a drying medium to obtain the graphene oxide/rubber nanocomposite; or adding a gasified flocculant to the drying medium of the spray drier to simultaneously perform flocculation and dehydration to obtain the graphene oxide/rubber nanocomposite.
The method of claim 1, wherein a solid content of graphene oxide in the graphene oxide/water sol is 0.01-20 wt%.
The method of claim 1, wherein the surfactant is selected from the group consisting of carboxylic styrene butadiene latex, butadiene-vinylpyridine copylymer latex, carboxylated styrene-butadiene latex, epoxy latex, carboxylic chloroprene rubber latex, carboxylic acrylonitrile styrene butadien rubber latex, and carboxyl polybutadiene, amino-propyl-tri-ethoxy silane coupling agent KH550, y-(methacryloxypropyl)-tri-methoxy silane coupling agent KH570, and quaternary ammonium salt which have a solid content of 10-80 wt %; the surfactant is 0.01 phr-100 phr by weight, and phr denotes the weight parts of the surfactant per every hundred weight parts of rubbe r.
The method of claim 1, wherein the rubber latex is selected from the group consisting of styrene butadiene latex, natural latex, neoprene latex, butyl latex, NBR latex, butadiene latex, ethylene propylene rubber latex, polyisoprene rubber latex, fluorine rubber latex, silica rubber latex, and polyurethane rubber latex which have a solid content of 10-80 wt %.
The method of claim 1, wherein the flocculant is selected from the group consisting of sulphuric acid, hydrochloric acid, calcium chloride, sodium chloride, potassium chloride, sodium sulphate, aluminium sulphate, ferric trichloride, poly aluminium chloride, and poly ferric chloride which have a weight percentage of 0.1-10 wt %.
The method of claim 1, wherein the flocculate is dried at a temperature of 4 3000C.
The method of claim 1, wherein the drying medium in the spray drier is hot air having a temperature of 60-3000C. 46
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Control sample: calcium chloride solution (1%) added to 500 g styrene butadiene latex (solid content 20 wt%) to perform flocculation. The flocculate is water-washed and dehydrated at 80°C for 24 h to obtain styrene butadiene rubber flocculated gel. The gel is then mixed in a two-roll rubber mixing mill.
3 materials1 process step
Graphene oxide/styrene butadiene rubber nanocomposite prepared by emulsion compounding with flocculation. At 4 phr graphene oxide loading, the vulcanizate exhibited tensile strength of 14.2 MPa (7.1× pure SBR), tensile strength at 100% elongation of 3.7 MPa (3.7× pure SBR), tensile strength at 300% elongation of 11.1 MPa (5.6× pure SBR), and air permeability coefficient of 2.35×10⁻ m² s⁻¹ Pa⁻¹ (3/10 of pure SBR). HRTEM images confirm graphene oxide is evenly dispersed as single sheets in the SBR substrate.
3 materials
Graphene oxide/styrene butadiene rubber nanocomposite. XRD shows no characteristic diffraction peaks of graphene oxide in the vulcanizate, indicating graphene oxide is present as single sheets highly delaminated in the SBR substrate.
3 materials
Graphene oxide/styrene butadiene rubber nanocomposite. XRD shows no characteristic diffraction peaks of graphene oxide in the vulcanizate, confirming highly delaminated single-sheet dispersion.
3 materials
Graphene oxide/styrene butadiene rubber vulcanizate showing clear Schallamach pattern in Akron abrasion test, indicating excellent interfacial bonding between graphene oxide and rubber substrate without massive delamination.
Materials described outside the worked examples.
surfactant
styrene butadiene rubber (SBR)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
AFM images (FIGS. 1A and 1B) of graphene oxide in graphene oxide/water sol show graphene oxide present in single sheet or few sheets; traverse scale is micron-sized and longitudinal scale is nano-sized.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Tensile Strength | 14.2 MPa | graphene oxide/rubber nanocomposite |
Patent
Atlas literature
Patent
US 9,376,537Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1 A and 1 B show atom force microscope (AFM) images of a graphene oxide in graphene oxide/water sol. The AFM images show that graphene oxide is present …
FIGS. 2A and 2B show transmission electron microscope (TEM) images of graphene oxide in a graphene oxide/water sol. The TEM images show that there are obvious …
FIGS. 3A and 3B show high resolution transmission electron microscope (HRTEM) images of a graphene oxide/styrene butadiene rubber nanocomposite (Example 4). …
FIG. 4. Example 1 8 [0030] Adding 10 g graphite oxide to 10 L water, treating by ultrasonic waves for 2 h at a power of 800 W, at a frequency of 1000 Hz, and …
FIG. 5B shows Akron abrasion Schalla m ach patte rn of a white carbon black/styrene butadiene rubber vulcanizate (Contrast 2). It is shown that the Schalla m …
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 preparing a dela m inated graphene oxide/rubber nanocomposite, the method comprising: (1) preparing a graphene oxide/water sol comprising dispersing graphene oxide in deionized water, and treating by ultrasonic waves at a power of 10-2000 W, and at a frequency of 10-20000 Hz, for 10 min-6 h at a temperature of 0-1000 C, to obtain the graphene oxide/water sol; (2) pretreating the graphene oxide/water sol comprising adding a surfactant to the graphene oxide/water sol, treating by ultrasonic waves for 5 m in-5 h or stirring for 5 m in-5 h at a stirring speed of 50-10000 r/min to obtain a pretreated graphene oxide/water dispersion; (3) preparing a graphene oxide/rubber compounding emulsion comprising treating the graphene oxide/water sol or the graphene oxide/water dispersion in addition to a rubber latex by ultrasonic waves for min-6 h, or stirring the graphene oxide/water sol or the graphene oxide/water dispersion in addition to the rubber latex for 10 min-6 h at a stirring speed of 5 0- 10000 r/min, to obtain a stabilized graphene oxide/rubber compounding emulsion; (4) preparing the graphene oxide/rubber nanocomposite comprising selecting one of the following processes to prepare the graphene oxide/rubber nanocomposite: A) ion flocculation process comprising adding a flocculant which demulsifies the graphene oxide/rubber compounding emulsion to perform flocculation, dehydrating and drying a flocculate of the flocculation to obtain the graphene oxide/rubber nanocomposite; and B) spray drying process comprising passing the graphene 44 oxide/rubber compounding emulsion through a spray drier to produce small composite liquid drops, and dehydrating the composite liquid drops in a drying medium to obtain the graphene oxide/rubber nanocomposite; or adding a gasified flocculant to the drying medium of the spray drier to simultaneously perform flocculation and dehydration to obtain the graphene oxide/rubber nanocomposite.
The method of claim 1, wherein a solid content of graphene oxide in the graphene oxide/water sol is 0.01-20 wt%.
The method of claim 1, wherein the surfactant is selected from the group consisting of carboxylic styrene butadiene latex, butadiene-vinylpyridine copylymer latex, carboxylated styrene-butadiene latex, epoxy latex, carboxylic chloroprene rubber latex, carboxylic acrylonitrile styrene butadien rubber latex, and carboxyl polybutadiene, amino-propyl-tri-ethoxy silane coupling agent KH550, y-(methacryloxypropyl)-tri-methoxy silane coupling agent KH570, and quaternary ammonium salt which have a solid content of 10-80 wt %; the surfactant is 0.01 phr-100 phr by weight, and phr denotes the weight parts of the surfactant per every hundred weight parts of rubbe r.
The method of claim 1, wherein the rubber latex is selected from the group consisting of styrene butadiene latex, natural latex, neoprene latex, butyl latex, NBR latex, butadiene latex, ethylene propylene rubber latex, polyisoprene rubber latex, fluorine rubber latex, silica rubber latex, and polyurethane rubber latex which have a solid content of 10-80 wt %.
The method of claim 1, wherein the flocculant is selected from the group consisting of sulphuric acid, hydrochloric acid, calcium chloride, sodium chloride, potassium chloride, sodium sulphate, aluminium sulphate, ferric trichloride, poly aluminium chloride, and poly ferric chloride which have a weight percentage of 0.1-10 wt %.
The method of claim 1, wherein the flocculate is dried at a temperature of 4 3000C.
The method of claim 1, wherein the drying medium in the spray drier is hot air having a temperature of 60-3000C. 46
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Control sample: calcium chloride solution (1%) added to 500 g styrene butadiene latex (solid content 20 wt%) to perform flocculation. The flocculate is water-washed and dehydrated at 80°C for 24 h to obtain styrene butadiene rubber flocculated gel. The gel is then mixed in a two-roll rubber mixing mill.
3 materials1 process step
Graphene oxide/styrene butadiene rubber nanocomposite prepared by emulsion compounding with flocculation. At 4 phr graphene oxide loading, the vulcanizate exhibited tensile strength of 14.2 MPa (7.1× pure SBR), tensile strength at 100% elongation of 3.7 MPa (3.7× pure SBR), tensile strength at 300% elongation of 11.1 MPa (5.6× pure SBR), and air permeability coefficient of 2.35×10⁻ m² s⁻¹ Pa⁻¹ (3/10 of pure SBR). HRTEM images confirm graphene oxide is evenly dispersed as single sheets in the SBR substrate.
3 materials
Graphene oxide/styrene butadiene rubber nanocomposite. XRD shows no characteristic diffraction peaks of graphene oxide in the vulcanizate, indicating graphene oxide is present as single sheets highly delaminated in the SBR substrate.
3 materials
Graphene oxide/styrene butadiene rubber nanocomposite. XRD shows no characteristic diffraction peaks of graphene oxide in the vulcanizate, confirming highly delaminated single-sheet dispersion.
3 materials
Graphene oxide/styrene butadiene rubber vulcanizate showing clear Schallamach pattern in Akron abrasion test, indicating excellent interfacial bonding between graphene oxide and rubber substrate without massive delamination.
Materials described outside the worked examples.
surfactant
styrene butadiene rubber (SBR)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
AFM images (FIGS. 1A and 1B) of graphene oxide in graphene oxide/water sol show graphene oxide present in single sheet or few sheets; traverse scale is micron-sized and longitudinal scale is nano-sized.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Tensile Strength | 14.2 MPa | graphene oxide/rubber nanocomposite |
Patent
Atlas literature
Patent
US 9,376,537Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1 A and 1 B show atom force microscope (AFM) images of a graphene oxide in graphene oxide/water sol. The AFM images show that graphene oxide is present …
FIGS. 2A and 2B show transmission electron microscope (TEM) images of graphene oxide in a graphene oxide/water sol. The TEM images show that there are obvious …
FIGS. 3A and 3B show high resolution transmission electron microscope (HRTEM) images of a graphene oxide/styrene butadiene rubber nanocomposite (Example 4). …
FIG. 4. Example 1 8 [0030] Adding 10 g graphite oxide to 10 L water, treating by ultrasonic waves for 2 h at a power of 800 W, at a frequency of 1000 Hz, and …
FIG. 5B shows Akron abrasion Schalla m ach patte rn of a white carbon black/styrene butadiene rubber vulcanizate (Contrast 2). It is shown that the Schalla m …
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 preparing a dela m inated graphene oxide/rubber nanocomposite, the method comprising: (1) preparing a graphene oxide/water sol comprising dispersing graphene oxide in deionized water, and treating by ultrasonic waves at a power of 10-2000 W, and at a frequency of 10-20000 Hz, for 10 min-6 h at a temperature of 0-1000 C, to obtain the graphene oxide/water sol; (2) pretreating the graphene oxide/water sol comprising adding a surfactant to the graphene oxide/water sol, treating by ultrasonic waves for 5 m in-5 h or stirring for 5 m in-5 h at a stirring speed of 50-10000 r/min to obtain a pretreated graphene oxide/water dispersion; (3) preparing a graphene oxide/rubber compounding emulsion comprising treating the graphene oxide/water sol or the graphene oxide/water dispersion in addition to a rubber latex by ultrasonic waves for min-6 h, or stirring the graphene oxide/water sol or the graphene oxide/water dispersion in addition to the rubber latex for 10 min-6 h at a stirring speed of 5 0- 10000 r/min, to obtain a stabilized graphene oxide/rubber compounding emulsion; (4) preparing the graphene oxide/rubber nanocomposite comprising selecting one of the following processes to prepare the graphene oxide/rubber nanocomposite: A) ion flocculation process comprising adding a flocculant which demulsifies the graphene oxide/rubber compounding emulsion to perform flocculation, dehydrating and drying a flocculate of the flocculation to obtain the graphene oxide/rubber nanocomposite; and B) spray drying process comprising passing the graphene 44 oxide/rubber compounding emulsion through a spray drier to produce small composite liquid drops, and dehydrating the composite liquid drops in a drying medium to obtain the graphene oxide/rubber nanocomposite; or adding a gasified flocculant to the drying medium of the spray drier to simultaneously perform flocculation and dehydration to obtain the graphene oxide/rubber nanocomposite.
The method of claim 1, wherein a solid content of graphene oxide in the graphene oxide/water sol is 0.01-20 wt%.
The method of claim 1, wherein the surfactant is selected from the group consisting of carboxylic styrene butadiene latex, butadiene-vinylpyridine copylymer latex, carboxylated styrene-butadiene latex, epoxy latex, carboxylic chloroprene rubber latex, carboxylic acrylonitrile styrene butadien rubber latex, and carboxyl polybutadiene, amino-propyl-tri-ethoxy silane coupling agent KH550, y-(methacryloxypropyl)-tri-methoxy silane coupling agent KH570, and quaternary ammonium salt which have a solid content of 10-80 wt %; the surfactant is 0.01 phr-100 phr by weight, and phr denotes the weight parts of the surfactant per every hundred weight parts of rubbe r.
The method of claim 1, wherein the rubber latex is selected from the group consisting of styrene butadiene latex, natural latex, neoprene latex, butyl latex, NBR latex, butadiene latex, ethylene propylene rubber latex, polyisoprene rubber latex, fluorine rubber latex, silica rubber latex, and polyurethane rubber latex which have a solid content of 10-80 wt %.
The method of claim 1, wherein the flocculant is selected from the group consisting of sulphuric acid, hydrochloric acid, calcium chloride, sodium chloride, potassium chloride, sodium sulphate, aluminium sulphate, ferric trichloride, poly aluminium chloride, and poly ferric chloride which have a weight percentage of 0.1-10 wt %.
The method of claim 1, wherein the flocculate is dried at a temperature of 4 3000C.
The method of claim 1, wherein the drying medium in the spray drier is hot air having a temperature of 60-3000C. 46
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Control sample: calcium chloride solution (1%) added to 500 g styrene butadiene latex (solid content 20 wt%) to perform flocculation. The flocculate is water-washed and dehydrated at 80°C for 24 h to obtain styrene butadiene rubber flocculated gel. The gel is then mixed in a two-roll rubber mixing mill.
3 materials1 process step
Graphene oxide/styrene butadiene rubber nanocomposite prepared by emulsion compounding with flocculation. At 4 phr graphene oxide loading, the vulcanizate exhibited tensile strength of 14.2 MPa (7.1× pure SBR), tensile strength at 100% elongation of 3.7 MPa (3.7× pure SBR), tensile strength at 300% elongation of 11.1 MPa (5.6× pure SBR), and air permeability coefficient of 2.35×10⁻ m² s⁻¹ Pa⁻¹ (3/10 of pure SBR). HRTEM images confirm graphene oxide is evenly dispersed as single sheets in the SBR substrate.
3 materials
Graphene oxide/styrene butadiene rubber nanocomposite. XRD shows no characteristic diffraction peaks of graphene oxide in the vulcanizate, indicating graphene oxide is present as single sheets highly delaminated in the SBR substrate.
3 materials
Graphene oxide/styrene butadiene rubber nanocomposite. XRD shows no characteristic diffraction peaks of graphene oxide in the vulcanizate, confirming highly delaminated single-sheet dispersion.
3 materials
Graphene oxide/styrene butadiene rubber vulcanizate showing clear Schallamach pattern in Akron abrasion test, indicating excellent interfacial bonding between graphene oxide and rubber substrate without massive delamination.
Materials described outside the worked examples.
surfactant
styrene butadiene rubber (SBR)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
AFM images (FIGS. 1A and 1B) of graphene oxide in graphene oxide/water sol show graphene oxide present in single sheet or few sheets; traverse scale is micron-sized and longitudinal scale is nano-sized.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Tensile Strength | 14.2 MPa | graphene oxide/rubber nanocomposite |
Patent
Atlas literature
Patent
US 9,376,537Patent drawings and their descriptions. Click a drawing to enlarge it.
FIGS. 1 A and 1 B show atom force microscope (AFM) images of a graphene oxide in graphene oxide/water sol. The AFM images show that graphene oxide is present …
FIGS. 2A and 2B show transmission electron microscope (TEM) images of graphene oxide in a graphene oxide/water sol. The TEM images show that there are obvious …
FIGS. 3A and 3B show high resolution transmission electron microscope (HRTEM) images of a graphene oxide/styrene butadiene rubber nanocomposite (Example 4). …
FIG. 4. Example 1 8 [0030] Adding 10 g graphite oxide to 10 L water, treating by ultrasonic waves for 2 h at a power of 800 W, at a frequency of 1000 Hz, and …
FIG. 5B shows Akron abrasion Schalla m ach patte rn of a white carbon black/styrene butadiene rubber vulcanizate (Contrast 2). It is shown that the Schalla m …
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 preparing a dela m inated graphene oxide/rubber nanocomposite, the method comprising: (1) preparing a graphene oxide/water sol comprising dispersing graphene oxide in deionized water, and treating by ultrasonic waves at a power of 10-2000 W, and at a frequency of 10-20000 Hz, for 10 min-6 h at a temperature of 0-1000 C, to obtain the graphene oxide/water sol; (2) pretreating the graphene oxide/water sol comprising adding a surfactant to the graphene oxide/water sol, treating by ultrasonic waves for 5 m in-5 h or stirring for 5 m in-5 h at a stirring speed of 50-10000 r/min to obtain a pretreated graphene oxide/water dispersion; (3) preparing a graphene oxide/rubber compounding emulsion comprising treating the graphene oxide/water sol or the graphene oxide/water dispersion in addition to a rubber latex by ultrasonic waves for min-6 h, or stirring the graphene oxide/water sol or the graphene oxide/water dispersion in addition to the rubber latex for 10 min-6 h at a stirring speed of 5 0- 10000 r/min, to obtain a stabilized graphene oxide/rubber compounding emulsion; (4) preparing the graphene oxide/rubber nanocomposite comprising selecting one of the following processes to prepare the graphene oxide/rubber nanocomposite: A) ion flocculation process comprising adding a flocculant which demulsifies the graphene oxide/rubber compounding emulsion to perform flocculation, dehydrating and drying a flocculate of the flocculation to obtain the graphene oxide/rubber nanocomposite; and B) spray drying process comprising passing the graphene 44 oxide/rubber compounding emulsion through a spray drier to produce small composite liquid drops, and dehydrating the composite liquid drops in a drying medium to obtain the graphene oxide/rubber nanocomposite; or adding a gasified flocculant to the drying medium of the spray drier to simultaneously perform flocculation and dehydration to obtain the graphene oxide/rubber nanocomposite.
The method of claim 1, wherein a solid content of graphene oxide in the graphene oxide/water sol is 0.01-20 wt%.
The method of claim 1, wherein the surfactant is selected from the group consisting of carboxylic styrene butadiene latex, butadiene-vinylpyridine copylymer latex, carboxylated styrene-butadiene latex, epoxy latex, carboxylic chloroprene rubber latex, carboxylic acrylonitrile styrene butadien rubber latex, and carboxyl polybutadiene, amino-propyl-tri-ethoxy silane coupling agent KH550, y-(methacryloxypropyl)-tri-methoxy silane coupling agent KH570, and quaternary ammonium salt which have a solid content of 10-80 wt %; the surfactant is 0.01 phr-100 phr by weight, and phr denotes the weight parts of the surfactant per every hundred weight parts of rubbe r.
The method of claim 1, wherein the rubber latex is selected from the group consisting of styrene butadiene latex, natural latex, neoprene latex, butyl latex, NBR latex, butadiene latex, ethylene propylene rubber latex, polyisoprene rubber latex, fluorine rubber latex, silica rubber latex, and polyurethane rubber latex which have a solid content of 10-80 wt %.
The method of claim 1, wherein the flocculant is selected from the group consisting of sulphuric acid, hydrochloric acid, calcium chloride, sodium chloride, potassium chloride, sodium sulphate, aluminium sulphate, ferric trichloride, poly aluminium chloride, and poly ferric chloride which have a weight percentage of 0.1-10 wt %.
The method of claim 1, wherein the flocculate is dried at a temperature of 4 3000C.
The method of claim 1, wherein the drying medium in the spray drier is hot air having a temperature of 60-3000C. 46
Embodiments described in the patent, grouped by the materials and process steps they use.
2 materials1 process step
Control sample: calcium chloride solution (1%) added to 500 g styrene butadiene latex (solid content 20 wt%) to perform flocculation. The flocculate is water-washed and dehydrated at 80°C for 24 h to obtain styrene butadiene rubber flocculated gel. The gel is then mixed in a two-roll rubber mixing mill.
3 materials1 process step
Graphene oxide/styrene butadiene rubber nanocomposite prepared by emulsion compounding with flocculation. At 4 phr graphene oxide loading, the vulcanizate exhibited tensile strength of 14.2 MPa (7.1× pure SBR), tensile strength at 100% elongation of 3.7 MPa (3.7× pure SBR), tensile strength at 300% elongation of 11.1 MPa (5.6× pure SBR), and air permeability coefficient of 2.35×10⁻ m² s⁻¹ Pa⁻¹ (3/10 of pure SBR). HRTEM images confirm graphene oxide is evenly dispersed as single sheets in the SBR substrate.
3 materials
Graphene oxide/styrene butadiene rubber nanocomposite. XRD shows no characteristic diffraction peaks of graphene oxide in the vulcanizate, indicating graphene oxide is present as single sheets highly delaminated in the SBR substrate.
3 materials
Graphene oxide/styrene butadiene rubber nanocomposite. XRD shows no characteristic diffraction peaks of graphene oxide in the vulcanizate, confirming highly delaminated single-sheet dispersion.
3 materials
Graphene oxide/styrene butadiene rubber vulcanizate showing clear Schallamach pattern in Akron abrasion test, indicating excellent interfacial bonding between graphene oxide and rubber substrate without massive delamination.
Materials described outside the worked examples.
surfactant
styrene butadiene rubber (SBR)
Additional fabrication and treatment steps described in the patent.
Measurements and analyses referenced in the patent, with their drawing references.
AFM images (FIGS. 1A and 1B) of graphene oxide in graphene oxide/water sol show graphene oxide present in single sheet or few sheets; traverse scale is micron-sized and longitudinal scale is nano-sized.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Tensile Strength | 14.2 MPa | graphene oxide/rubber nanocomposite |
calcium chloride solution
CaCl₂
TEM images (FIGS. 2A and 2B) of graphene oxide in graphene oxide/water sol show obvious folding structures at the edge of graphene oxide.
HRTEM images (FIGS. 3A and 3B) of graphene oxide/styrene butadiene rubber nanocomposite (Example 4) show graphene oxide is evenly dispersed in the SBR substrate in a form of single sheet.
XRD profiles (FIG. 4) of graphite oxide, SBR vulcanizate (Contrast 1), and graphene oxide/SBR vulcanizates (Examples 1 and 9). Characteristic diffraction peaks of graphene oxide do not occur in the nanocomposite, indicating highly delaminated single-sheet dispersion.
FIG. 5A shows clear Schallamach pattern for graphene oxide/SBR vulcanizate (Example 10), indicating rubber substrate and graphene oxide are not massively delaminated and interfacial bonding is excellent. FIG. 5B shows white carbon black/SBR vulcanizate (Contrast 2) for comparison.
Tensile Strength At 100 Percent Elongation |
| 3.7 MPa |
graphene oxide/rubber nanocomposite |
Tensile Strength At 300 Percent Elongation | 11.1 MPa | graphene oxide/rubber nanocomposite |
Air Permeability Coefficient | 2.35e-? m² s⁻¹ Pa⁻¹ | graphene oxide/rubber nanocomposite |
— | 10–2000 W | — |
— | 10–1000 W | — |
calcium chloride solution
CaCl₂
TEM images (FIGS. 2A and 2B) of graphene oxide in graphene oxide/water sol show obvious folding structures at the edge of graphene oxide.
HRTEM images (FIGS. 3A and 3B) of graphene oxide/styrene butadiene rubber nanocomposite (Example 4) show graphene oxide is evenly dispersed in the SBR substrate in a form of single sheet.
XRD profiles (FIG. 4) of graphite oxide, SBR vulcanizate (Contrast 1), and graphene oxide/SBR vulcanizates (Examples 1 and 9). Characteristic diffraction peaks of graphene oxide do not occur in the nanocomposite, indicating highly delaminated single-sheet dispersion.
FIG. 5A shows clear Schallamach pattern for graphene oxide/SBR vulcanizate (Example 10), indicating rubber substrate and graphene oxide are not massively delaminated and interfacial bonding is excellent. FIG. 5B shows white carbon black/SBR vulcanizate (Contrast 2) for comparison.
Tensile Strength At 100 Percent Elongation |
| 3.7 MPa |
graphene oxide/rubber nanocomposite |
Tensile Strength At 300 Percent Elongation | 11.1 MPa | graphene oxide/rubber nanocomposite |
Air Permeability Coefficient | 2.35e-? m² s⁻¹ Pa⁻¹ | graphene oxide/rubber nanocomposite |
— | 10–2000 W | — |
— | 10–1000 W | — |
calcium chloride solution
CaCl₂
TEM images (FIGS. 2A and 2B) of graphene oxide in graphene oxide/water sol show obvious folding structures at the edge of graphene oxide.
HRTEM images (FIGS. 3A and 3B) of graphene oxide/styrene butadiene rubber nanocomposite (Example 4) show graphene oxide is evenly dispersed in the SBR substrate in a form of single sheet.
XRD profiles (FIG. 4) of graphite oxide, SBR vulcanizate (Contrast 1), and graphene oxide/SBR vulcanizates (Examples 1 and 9). Characteristic diffraction peaks of graphene oxide do not occur in the nanocomposite, indicating highly delaminated single-sheet dispersion.
FIG. 5A shows clear Schallamach pattern for graphene oxide/SBR vulcanizate (Example 10), indicating rubber substrate and graphene oxide are not massively delaminated and interfacial bonding is excellent. FIG. 5B shows white carbon black/SBR vulcanizate (Contrast 2) for comparison.
Tensile Strength At 100 Percent Elongation |
| 3.7 MPa |
graphene oxide/rubber nanocomposite |
Tensile Strength At 300 Percent Elongation | 11.1 MPa | graphene oxide/rubber nanocomposite |
Air Permeability Coefficient | 2.35e-? m² s⁻¹ Pa⁻¹ | graphene oxide/rubber nanocomposite |
— | 10–2000 W | — |
— | 10–1000 W | — |
calcium chloride solution
CaCl₂
TEM images (FIGS. 2A and 2B) of graphene oxide in graphene oxide/water sol show obvious folding structures at the edge of graphene oxide.
HRTEM images (FIGS. 3A and 3B) of graphene oxide/styrene butadiene rubber nanocomposite (Example 4) show graphene oxide is evenly dispersed in the SBR substrate in a form of single sheet.
XRD profiles (FIG. 4) of graphite oxide, SBR vulcanizate (Contrast 1), and graphene oxide/SBR vulcanizates (Examples 1 and 9). Characteristic diffraction peaks of graphene oxide do not occur in the nanocomposite, indicating highly delaminated single-sheet dispersion.
FIG. 5A shows clear Schallamach pattern for graphene oxide/SBR vulcanizate (Example 10), indicating rubber substrate and graphene oxide are not massively delaminated and interfacial bonding is excellent. FIG. 5B shows white carbon black/SBR vulcanizate (Contrast 2) for comparison.
Tensile Strength At 100 Percent Elongation |
| 3.7 MPa |
graphene oxide/rubber nanocomposite |
Tensile Strength At 300 Percent Elongation | 11.1 MPa | graphene oxide/rubber nanocomposite |
Air Permeability Coefficient | 2.35e-? m² s⁻¹ Pa⁻¹ | graphene oxide/rubber nanocomposite |
— | 10–2000 W | — |
— | 10–1000 W | — |