Patent
US 9,556,354A method for fabricating a semicrystalline polymer/graphene oxide composite film
Jung-Tsai Chen
US
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US 9,556,354Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for fabricating a semicrystalline polymer/graphene oxide composite film, comprising: providing a polymer/graphene oxide casting solution by dissolving a polymer in a first solvent to obtain a mixture solution, adding a graphene oxide solution into the mixture solution, and stirring until uniform wherein the graphene oxide solution comprises a second solvent and graphene oxide dispersed in the second solvent, wherein the polymer is polyvinyl alcohol; performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate to form a first film on the substrate wherein the graphene oxide in the first film has a layered structure and distributed in the polymer; performing a crystallization procedure by drying the first film with heat to form the first film having a first semicrystalline -typed polymer wherein the first semicrystalline -typed polymer has a porous structure and the first semicrystalline -typed polymer and graphene oxide are distributed uniformly in the first film with respect to each other so as to have the first semicrystalline- typed polymer exist between graphene oxide and graphene oxide also exist between the first semicrystalline- typed polymers; and performing a recrystallization procedure by having the composite film having the first semicrystalline -typed polymer undergo heat treatment to induce the first semicrystalline -typed polymer comprising 2 polyvinyl alcohol between adjacent layers of graphene oxide to form a second semicrystalline -typed polymer so as to obtain a composite film having the first semicrystalline -typed polymer and the second semicrystalline -typed polymer, wherein the second semicrystalline -typed polymer fills and seals the porous structure of the first semicrystalline-typed polymer to block gas from flowing through and to increase a length that gas passes from one side of the composite film to the other side of the composite film, and said composite film has a weight ratio of the semicrystalline polyvinyl alcohol to graphene oxide of the composite film being 1000:1~50:1, and is characterized by an X-ray powder diffraction pattern comprising peaks at 20.1±0.2, 22.5±0.2 and 29.5±0.2 2-theta degree.
The method according to claim 1, wherein the graphene oxide solution is prepared by dissolving sodium nitrate in concentrated sulfuric acid by heating and stirring to obtain a sodium nitrate/sulfuric acid solution; adding graphene oxide into the sodium nitrate/sulfuric acid solution and stirring until uniform to obtain a first mixture; lowering the temperature of the first mixture by placing in an ice bath; slowly adding potassium permanganate (KMnO 4) after the first mixture is stabilized; slowly adding deionized water; setting the solution to obtain graphene oxide precipitation; performing vacuum drying to obtain graphene oxide flakes; and dispersing graphene oxide in deionized water by supersonic 3 oscillation to ensure graphene oxide completely being dispersed in deionized water and being exfoliated with a single layered structure so as to obtain the graphene oxide solution.
(Original)The method according to claim 1, wherein the first solvent is deionized water.
(Original)The method according to claim 1, wherein the mixture solution is a polyvinyl alcohol solution and comprises polyvinyl alcohol and deionized water with a weight ratio (polyvinyl alcohol/deionized water) of 1:100 ~ 20:100.
(Original)The method according to claim 1, wherein the second solvent is deionized water.
(Original)The method according to claim 1, wherein the graphene oxide solution comprises graphene oxide and deionized water with a weight ratio (graphene oxide/deionized water) of 1:50000 ~ 1:1000.
(Original) The method according to claim 1, wherein the polymer is polyvinyl alcohol and the step of performing a crystallization procedure by drying the first film with heat comprises: drying the first film at 80 ~ 100 ° C for 1~ 3 hr; and processing the first film by vacuum drying for 18 ~ 24 hr at room temperature to have polyvinyl alcohol form into a first semicrystalline-typed polyvinyl alcohol.
(Original)The method according to claim 1, wherein the heat treatment in the recrystallization procedure is controlled within a temperature range of 80 ~ 140 °C.
(Original)The method according to claim 1, after the recrystallization procedure, further comprising: performing a quenching procedure by placing the composite film in a temperature range of 3 ~15°C.
(Original)The method according to claim 1, wherein the polymer is polyvinyl alcohol and the semicrystalline polymer/graphene oxide composite film is semicrystalline polyvinyl alcohol/graphene oxide composite film having a film thickness of 5 ~ 100 pm.
The method according to claim 1, wherein the step of performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate is performed by using a doctor blade to form a wet film with a thickness of 100 ~ 1000 pm.
The method according to claim 1, wherein the step of performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate is performed by using a doctor blade to form a wet first film with a thickness of 300 pm.
The method according to claim 1 7 1, wherein the weight ratio of the semicrystalline polyvinyl alcohol to graphene oxide of the composite film is 1000:1. 6
canceled
Layer stacks claimed or described, ordered top of device to substrate.
semicrystalline polyvinyl alcohol/graphene oxide composite film (gas barrier film)
Materials described outside the worked examples.
polyvinyl alcohol
graphene oxide
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
XRD peaks of semicrystalline PVA/GO composite film at 20.1±0.2, 22.5±0.2, 29.5±0.2 2-theta degrees | — | semicrystalline polyvinyl alcohol/graphene oxide composite film |
Temperature |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,556,354Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for fabricating a semicrystalline polymer/graphene oxide composite film, comprising: providing a polymer/graphene oxide casting solution by dissolving a polymer in a first solvent to obtain a mixture solution, adding a graphene oxide solution into the mixture solution, and stirring until uniform wherein the graphene oxide solution comprises a second solvent and graphene oxide dispersed in the second solvent, wherein the polymer is polyvinyl alcohol; performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate to form a first film on the substrate wherein the graphene oxide in the first film has a layered structure and distributed in the polymer; performing a crystallization procedure by drying the first film with heat to form the first film having a first semicrystalline -typed polymer wherein the first semicrystalline -typed polymer has a porous structure and the first semicrystalline -typed polymer and graphene oxide are distributed uniformly in the first film with respect to each other so as to have the first semicrystalline- typed polymer exist between graphene oxide and graphene oxide also exist between the first semicrystalline- typed polymers; and performing a recrystallization procedure by having the composite film having the first semicrystalline -typed polymer undergo heat treatment to induce the first semicrystalline -typed polymer comprising 2 polyvinyl alcohol between adjacent layers of graphene oxide to form a second semicrystalline -typed polymer so as to obtain a composite film having the first semicrystalline -typed polymer and the second semicrystalline -typed polymer, wherein the second semicrystalline -typed polymer fills and seals the porous structure of the first semicrystalline-typed polymer to block gas from flowing through and to increase a length that gas passes from one side of the composite film to the other side of the composite film, and said composite film has a weight ratio of the semicrystalline polyvinyl alcohol to graphene oxide of the composite film being 1000:1~50:1, and is characterized by an X-ray powder diffraction pattern comprising peaks at 20.1±0.2, 22.5±0.2 and 29.5±0.2 2-theta degree.
The method according to claim 1, wherein the graphene oxide solution is prepared by dissolving sodium nitrate in concentrated sulfuric acid by heating and stirring to obtain a sodium nitrate/sulfuric acid solution; adding graphene oxide into the sodium nitrate/sulfuric acid solution and stirring until uniform to obtain a first mixture; lowering the temperature of the first mixture by placing in an ice bath; slowly adding potassium permanganate (KMnO 4) after the first mixture is stabilized; slowly adding deionized water; setting the solution to obtain graphene oxide precipitation; performing vacuum drying to obtain graphene oxide flakes; and dispersing graphene oxide in deionized water by supersonic 3 oscillation to ensure graphene oxide completely being dispersed in deionized water and being exfoliated with a single layered structure so as to obtain the graphene oxide solution.
(Original)The method according to claim 1, wherein the first solvent is deionized water.
(Original)The method according to claim 1, wherein the mixture solution is a polyvinyl alcohol solution and comprises polyvinyl alcohol and deionized water with a weight ratio (polyvinyl alcohol/deionized water) of 1:100 ~ 20:100.
(Original)The method according to claim 1, wherein the second solvent is deionized water.
(Original)The method according to claim 1, wherein the graphene oxide solution comprises graphene oxide and deionized water with a weight ratio (graphene oxide/deionized water) of 1:50000 ~ 1:1000.
(Original) The method according to claim 1, wherein the polymer is polyvinyl alcohol and the step of performing a crystallization procedure by drying the first film with heat comprises: drying the first film at 80 ~ 100 ° C for 1~ 3 hr; and processing the first film by vacuum drying for 18 ~ 24 hr at room temperature to have polyvinyl alcohol form into a first semicrystalline-typed polyvinyl alcohol.
(Original)The method according to claim 1, wherein the heat treatment in the recrystallization procedure is controlled within a temperature range of 80 ~ 140 °C.
(Original)The method according to claim 1, after the recrystallization procedure, further comprising: performing a quenching procedure by placing the composite film in a temperature range of 3 ~15°C.
(Original)The method according to claim 1, wherein the polymer is polyvinyl alcohol and the semicrystalline polymer/graphene oxide composite film is semicrystalline polyvinyl alcohol/graphene oxide composite film having a film thickness of 5 ~ 100 pm.
The method according to claim 1, wherein the step of performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate is performed by using a doctor blade to form a wet film with a thickness of 100 ~ 1000 pm.
The method according to claim 1, wherein the step of performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate is performed by using a doctor blade to form a wet first film with a thickness of 300 pm.
The method according to claim 1 7 1, wherein the weight ratio of the semicrystalline polyvinyl alcohol to graphene oxide of the composite film is 1000:1. 6
canceled
Layer stacks claimed or described, ordered top of device to substrate.
semicrystalline polyvinyl alcohol/graphene oxide composite film (gas barrier film)
Materials described outside the worked examples.
polyvinyl alcohol
graphene oxide
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
XRD peaks of semicrystalline PVA/GO composite film at 20.1±0.2, 22.5±0.2, 29.5±0.2 2-theta degrees | — | semicrystalline polyvinyl alcohol/graphene oxide composite film |
Temperature |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,556,354Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for fabricating a semicrystalline polymer/graphene oxide composite film, comprising: providing a polymer/graphene oxide casting solution by dissolving a polymer in a first solvent to obtain a mixture solution, adding a graphene oxide solution into the mixture solution, and stirring until uniform wherein the graphene oxide solution comprises a second solvent and graphene oxide dispersed in the second solvent, wherein the polymer is polyvinyl alcohol; performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate to form a first film on the substrate wherein the graphene oxide in the first film has a layered structure and distributed in the polymer; performing a crystallization procedure by drying the first film with heat to form the first film having a first semicrystalline -typed polymer wherein the first semicrystalline -typed polymer has a porous structure and the first semicrystalline -typed polymer and graphene oxide are distributed uniformly in the first film with respect to each other so as to have the first semicrystalline- typed polymer exist between graphene oxide and graphene oxide also exist between the first semicrystalline- typed polymers; and performing a recrystallization procedure by having the composite film having the first semicrystalline -typed polymer undergo heat treatment to induce the first semicrystalline -typed polymer comprising 2 polyvinyl alcohol between adjacent layers of graphene oxide to form a second semicrystalline -typed polymer so as to obtain a composite film having the first semicrystalline -typed polymer and the second semicrystalline -typed polymer, wherein the second semicrystalline -typed polymer fills and seals the porous structure of the first semicrystalline-typed polymer to block gas from flowing through and to increase a length that gas passes from one side of the composite film to the other side of the composite film, and said composite film has a weight ratio of the semicrystalline polyvinyl alcohol to graphene oxide of the composite film being 1000:1~50:1, and is characterized by an X-ray powder diffraction pattern comprising peaks at 20.1±0.2, 22.5±0.2 and 29.5±0.2 2-theta degree.
The method according to claim 1, wherein the graphene oxide solution is prepared by dissolving sodium nitrate in concentrated sulfuric acid by heating and stirring to obtain a sodium nitrate/sulfuric acid solution; adding graphene oxide into the sodium nitrate/sulfuric acid solution and stirring until uniform to obtain a first mixture; lowering the temperature of the first mixture by placing in an ice bath; slowly adding potassium permanganate (KMnO 4) after the first mixture is stabilized; slowly adding deionized water; setting the solution to obtain graphene oxide precipitation; performing vacuum drying to obtain graphene oxide flakes; and dispersing graphene oxide in deionized water by supersonic 3 oscillation to ensure graphene oxide completely being dispersed in deionized water and being exfoliated with a single layered structure so as to obtain the graphene oxide solution.
(Original)The method according to claim 1, wherein the first solvent is deionized water.
(Original)The method according to claim 1, wherein the mixture solution is a polyvinyl alcohol solution and comprises polyvinyl alcohol and deionized water with a weight ratio (polyvinyl alcohol/deionized water) of 1:100 ~ 20:100.
(Original)The method according to claim 1, wherein the second solvent is deionized water.
(Original)The method according to claim 1, wherein the graphene oxide solution comprises graphene oxide and deionized water with a weight ratio (graphene oxide/deionized water) of 1:50000 ~ 1:1000.
(Original) The method according to claim 1, wherein the polymer is polyvinyl alcohol and the step of performing a crystallization procedure by drying the first film with heat comprises: drying the first film at 80 ~ 100 ° C for 1~ 3 hr; and processing the first film by vacuum drying for 18 ~ 24 hr at room temperature to have polyvinyl alcohol form into a first semicrystalline-typed polyvinyl alcohol.
(Original)The method according to claim 1, wherein the heat treatment in the recrystallization procedure is controlled within a temperature range of 80 ~ 140 °C.
(Original)The method according to claim 1, after the recrystallization procedure, further comprising: performing a quenching procedure by placing the composite film in a temperature range of 3 ~15°C.
(Original)The method according to claim 1, wherein the polymer is polyvinyl alcohol and the semicrystalline polymer/graphene oxide composite film is semicrystalline polyvinyl alcohol/graphene oxide composite film having a film thickness of 5 ~ 100 pm.
The method according to claim 1, wherein the step of performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate is performed by using a doctor blade to form a wet film with a thickness of 100 ~ 1000 pm.
The method according to claim 1, wherein the step of performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate is performed by using a doctor blade to form a wet first film with a thickness of 300 pm.
The method according to claim 1 7 1, wherein the weight ratio of the semicrystalline polyvinyl alcohol to graphene oxide of the composite film is 1000:1. 6
canceled
Layer stacks claimed or described, ordered top of device to substrate.
semicrystalline polyvinyl alcohol/graphene oxide composite film (gas barrier film)
Materials described outside the worked examples.
polyvinyl alcohol
graphene oxide
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
XRD peaks of semicrystalline PVA/GO composite film at 20.1±0.2, 22.5±0.2, 29.5±0.2 2-theta degrees | — | semicrystalline polyvinyl alcohol/graphene oxide composite film |
Temperature |
Related documents with shared materials, methods, properties, or citations.
Patent
Atlas literature
Patent
US 9,556,354Patent drawings and their descriptions. Click a drawing to enlarge it.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A method for fabricating a semicrystalline polymer/graphene oxide composite film, comprising: providing a polymer/graphene oxide casting solution by dissolving a polymer in a first solvent to obtain a mixture solution, adding a graphene oxide solution into the mixture solution, and stirring until uniform wherein the graphene oxide solution comprises a second solvent and graphene oxide dispersed in the second solvent, wherein the polymer is polyvinyl alcohol; performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate to form a first film on the substrate wherein the graphene oxide in the first film has a layered structure and distributed in the polymer; performing a crystallization procedure by drying the first film with heat to form the first film having a first semicrystalline -typed polymer wherein the first semicrystalline -typed polymer has a porous structure and the first semicrystalline -typed polymer and graphene oxide are distributed uniformly in the first film with respect to each other so as to have the first semicrystalline- typed polymer exist between graphene oxide and graphene oxide also exist between the first semicrystalline- typed polymers; and performing a recrystallization procedure by having the composite film having the first semicrystalline -typed polymer undergo heat treatment to induce the first semicrystalline -typed polymer comprising 2 polyvinyl alcohol between adjacent layers of graphene oxide to form a second semicrystalline -typed polymer so as to obtain a composite film having the first semicrystalline -typed polymer and the second semicrystalline -typed polymer, wherein the second semicrystalline -typed polymer fills and seals the porous structure of the first semicrystalline-typed polymer to block gas from flowing through and to increase a length that gas passes from one side of the composite film to the other side of the composite film, and said composite film has a weight ratio of the semicrystalline polyvinyl alcohol to graphene oxide of the composite film being 1000:1~50:1, and is characterized by an X-ray powder diffraction pattern comprising peaks at 20.1±0.2, 22.5±0.2 and 29.5±0.2 2-theta degree.
The method according to claim 1, wherein the graphene oxide solution is prepared by dissolving sodium nitrate in concentrated sulfuric acid by heating and stirring to obtain a sodium nitrate/sulfuric acid solution; adding graphene oxide into the sodium nitrate/sulfuric acid solution and stirring until uniform to obtain a first mixture; lowering the temperature of the first mixture by placing in an ice bath; slowly adding potassium permanganate (KMnO 4) after the first mixture is stabilized; slowly adding deionized water; setting the solution to obtain graphene oxide precipitation; performing vacuum drying to obtain graphene oxide flakes; and dispersing graphene oxide in deionized water by supersonic 3 oscillation to ensure graphene oxide completely being dispersed in deionized water and being exfoliated with a single layered structure so as to obtain the graphene oxide solution.
(Original)The method according to claim 1, wherein the first solvent is deionized water.
(Original)The method according to claim 1, wherein the mixture solution is a polyvinyl alcohol solution and comprises polyvinyl alcohol and deionized water with a weight ratio (polyvinyl alcohol/deionized water) of 1:100 ~ 20:100.
(Original)The method according to claim 1, wherein the second solvent is deionized water.
(Original)The method according to claim 1, wherein the graphene oxide solution comprises graphene oxide and deionized water with a weight ratio (graphene oxide/deionized water) of 1:50000 ~ 1:1000.
(Original) The method according to claim 1, wherein the polymer is polyvinyl alcohol and the step of performing a crystallization procedure by drying the first film with heat comprises: drying the first film at 80 ~ 100 ° C for 1~ 3 hr; and processing the first film by vacuum drying for 18 ~ 24 hr at room temperature to have polyvinyl alcohol form into a first semicrystalline-typed polyvinyl alcohol.
(Original)The method according to claim 1, wherein the heat treatment in the recrystallization procedure is controlled within a temperature range of 80 ~ 140 °C.
(Original)The method according to claim 1, after the recrystallization procedure, further comprising: performing a quenching procedure by placing the composite film in a temperature range of 3 ~15°C.
(Original)The method according to claim 1, wherein the polymer is polyvinyl alcohol and the semicrystalline polymer/graphene oxide composite film is semicrystalline polyvinyl alcohol/graphene oxide composite film having a film thickness of 5 ~ 100 pm.
The method according to claim 1, wherein the step of performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate is performed by using a doctor blade to form a wet film with a thickness of 100 ~ 1000 pm.
The method according to claim 1, wherein the step of performing a film forming procedure by coating the polymer/graphene oxide casting solution on a substrate is performed by using a doctor blade to form a wet first film with a thickness of 300 pm.
The method according to claim 1 7 1, wherein the weight ratio of the semicrystalline polyvinyl alcohol to graphene oxide of the composite film is 1000:1. 6
canceled
Layer stacks claimed or described, ordered top of device to substrate.
semicrystalline polyvinyl alcohol/graphene oxide composite film (gas barrier film)
Materials described outside the worked examples.
polyvinyl alcohol
graphene oxide
Additional fabrication and treatment steps described in the patent.
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
XRD peaks of semicrystalline PVA/GO composite film at 20.1±0.2, 22.5±0.2, 29.5±0.2 2-theta degrees | — | semicrystalline polyvinyl alcohol/graphene oxide composite film |
Temperature |
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Temperature | 80–100 °C | — |
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