CN113086977B - Preparation method of double-layer graphene oxide film - Google Patents
Preparation method of double-layer graphene oxide film Download PDFInfo
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- CN113086977B CN113086977B CN202010016491.4A CN202010016491A CN113086977B CN 113086977 B CN113086977 B CN 113086977B CN 202010016491 A CN202010016491 A CN 202010016491A CN 113086977 B CN113086977 B CN 113086977B
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
Abstract
The invention relates to the technical field of graphene manufacturing, and discloses a preparation method of a double-layer graphene oxide film, which comprises the following steps: preparing graphene oxide slurry with solid content of 5% by using a hummers method; b, coating the graphene oxide slurry on a PET (polyethylene terephthalate) film serving as a substrate to prepare two wet films with the sizes of 300mm multiplied by 150mm multiplied by 3 mm; c, adopting a formula of 1: 8, diluting the epoxy resin by using ethanol; d, respectively spraying the diluted epoxy resin obtained in the step c on the surface of the wet film by using a spraying pot; e, sending the two wet films into a blast drying oven for baking to obtain a dry film; f, coating a curing agent on the dry film and then pasting the dry film and the curing agent together; g, placing the double-layer dry film into a blast drying oven to be baked so as to cure the epoxy resin; h, taking down the glass plate and the PET substrate to prepare a double-layer smooth graphene oxide dry film; the method solves the problem of unevenness such as volume shrinkage, bulging and the like caused by excessive water due to excessive thickness in the film coating process of the graphene oxide film, and has the advantages of safe operation, low cost and less impurities.
Description
Technical Field
The invention relates to the technical field of graphene manufacturing, in particular to a preparation method of a double-layer graphene oxide film.
Background
The graphene oxide film is a film prepared by taking graphene oxide slurry as a raw material, is reduced and applied to the field of heat conduction and heat dissipation, and is a novel heat conduction material; this patent is mainly to the graphene oxide film forming process in, can't obtain the problem of thicker and keep smooth film through stoving moisture, provides a solution, can reach under the condition of anticipated thickness at the film, keeps the planarization of film.
Disclosure of Invention
A preparation method of a double-layer graphene oxide film comprises the following steps:
selecting a 300-mesh 500-mesh crystalline flake graphite raw material, preparing graphene oxide by a hummers method (oxidation-reduction method), adding water and the graphene oxide into a stirring tank, and uniformly stirring to prepare graphene oxide slurry with the solid content of 5%;
b, coating the graphene oxide slurry prepared in the step a on a PET (polyethylene terephthalate) film serving as a substrate by adopting a coating machine, and repeating the operation twice to prepare two wet films with the sizes of 300mm multiplied by 150mm multiplied by 3 mm;
c, adopting a formula of 1: 8, diluting the epoxy resin by using ethanol;
d, respectively spraying the epoxy resin diluted in the step c on the surfaces of the graphene oxide slurry of the two wet films prepared in the step b by using a spraying pot;
e, feeding the two wet films into a forced air drying oven, and baking for 3-4 hours at the temperature of 70-80 ℃ to obtain two graphene oxide dry films;
f, taking out the two dry films, airing, coating a polyamide resin curing agent on one surface of the dry film with the epoxy resin, and pasting the surfaces of the two dry films coated with the polyamide resin curing agent together to obtain a double-layer dry film;
g, respectively pressing the upper surface and the lower surface of the double-layer dry film by using glass plates, and placing the double-layer dry film into a blast drying oven to be baked for 3-4 hours at the high temperature of 110-120 ℃ so as to cure the epoxy resin;
and h, taking out the double-layer dry film, cooling to normal temperature, and respectively taking down the upper glass plate, the lower glass plate and the PET substrate to obtain the double-layer flat graphene oxide dry film.
Preferably, the preparation method of the double-layer graphene oxide film comprises the following steps:
selecting a 300-mesh 500-mesh crystalline flake graphite raw material, preparing graphene oxide by a hummers method (oxidation-reduction method), adding water and the graphene oxide into a stirring tank, and uniformly stirring to prepare graphene oxide slurry with the solid content of 5%;
b, coating the graphene oxide slurry prepared in the step a on a PET (polyethylene terephthalate) film serving as a substrate by adopting a coating machine, and repeating the operation twice to prepare two wet films with the sizes of 300mm multiplied by 150mm multiplied by 3 mm;
c, adopting a formula of 1: 8, diluting the epoxy resin by using ethanol;
d, respectively spraying the epoxy resin diluted in the step c on the surfaces of the graphene oxide slurry of the two wet films prepared in the step b by using a spraying pot;
e, feeding the two wet films into a blast drying oven, and baking for 4 hours at 70 ℃ to obtain two graphene oxide dry films;
f, taking out the two dry films, airing, coating a polyamide resin curing agent on one surface of the dry film with the epoxy resin, and pasting the surfaces of the two dry films coated with the polyamide resin curing agent together to obtain a double-layer dry film;
g, respectively pressing the upper surface and the lower surface of the double-layer dry film by using glass plates, and baking the double-layer dry film in a blast drying oven at a high temperature of 110 ℃ for 4 hours to cure the epoxy resin;
and h, taking out the double-layer dry film, cooling to normal temperature, and respectively taking down the upper glass plate, the lower glass plate and the PET substrate to obtain the double-layer flat graphene oxide dry film.
Preferably, the preparation method of the double-layer graphene oxide film comprises the following steps:
selecting a 300-mesh 500-mesh crystalline flake graphite raw material, preparing graphene oxide by a hummers method (oxidation-reduction method), adding water and the graphene oxide into a stirring tank, and uniformly stirring to prepare graphene oxide slurry with the solid content of 5%;
b, coating the graphene oxide slurry prepared in the step a on a PET (polyethylene terephthalate) film serving as a substrate by adopting a coating machine, and repeating the operation twice to prepare two wet films with the sizes of 300mm multiplied by 150mm multiplied by 3 mm;
c, adopting a formula of 1: 8, diluting the epoxy resin by using ethanol;
d, respectively spraying the epoxy resin diluted in the step c on the surfaces of the graphene oxide slurry of the two wet films prepared in the step b by using a spraying pot;
e, feeding the two wet films into a blast drying oven, and baking for 3 hours at the temperature of 80 ℃ to obtain two graphene oxide dry films;
f, taking out the two dry films, airing, coating a polyamide resin curing agent on one surface of the dry film with the epoxy resin, and pasting the surfaces of the two dry films coated with the polyamide resin curing agent together to obtain a double-layer dry film;
pressing the upper surface and the lower surface of the double-layer dry film by using a glass plate, and baking the double-layer dry film in a blast drying oven at a high temperature of 120 ℃ for 3 hours to cure the epoxy resin;
and h, taking out the double-layer dry film, cooling to normal temperature, and respectively taking down the upper glass plate, the lower glass plate and the PET substrate to obtain the double-layer flat graphene oxide dry film.
The invention has the beneficial effects that:
the problems of unsmooth volume shrinkage, bulging and the like caused by excessive water due to excessive thickness in the film coating process of the graphene oxide film are solved;
secondly, the operation is safe, and flammable and explosive volatile matters containing toxicity are not involved;
thirdly, the adopted epoxy resin is low in price, and the production cost is effectively controlled;
and fourthly, the epoxy resin is a carbon skeleton high molecular organic matter, and impurities are not generated in processing environments such as high-temperature reduction of the graphene oxide film and the like.
Detailed Description
The first embodiment is as follows:
a preparation method of a double-layer graphene oxide film comprises the following steps:
selecting a 300-mesh 500-mesh crystalline flake graphite raw material, preparing graphene oxide by a hummers method (oxidation-reduction method), adding water and the graphene oxide into a stirring tank, and uniformly stirring to prepare graphene oxide slurry with the solid content of 5%.
And b, coating the graphene oxide slurry prepared in the step a on a PET (polyethylene terephthalate) film serving as a substrate by adopting a coating machine, and repeating the operation twice to prepare two wet films with the sizes of 300mm multiplied by 150mm multiplied by 3 mm.
c, adopting a formula of 1: 8, diluting the epoxy resin with ethanol.
d, respectively spraying the epoxy resin diluted in the step c on the surfaces of the graphene oxide slurry of the two wet films prepared in the step b by using a spraying pot.
And e, feeding the two wet films into an air-blast drying oven, and baking for 4 hours at 70 ℃ to obtain two graphene oxide dry films.
And f, taking out the two dry films, airing, coating a polyamide resin curing agent on one surface of each dry film with the epoxy resin, and adhering the surfaces of the two dry films coated with the polyamide resin curing agent together to obtain the double-layer dry film.
And g, respectively pressing the upper surface and the lower surface of the double-layer dry film by using glass plates, and baking the double-layer dry film in a blast drying oven at a high temperature of 110 ℃ for 4 hours to cure the epoxy resin.
And h, taking out the double-layer dry film, cooling to normal temperature, and respectively taking down the upper glass plate, the lower glass plate and the PET substrate to obtain the double-layer flat graphene oxide dry film.
Example two:
a preparation method of a double-layer graphene oxide film comprises the following steps:
selecting a 300-mesh 500-mesh crystalline flake graphite raw material, preparing graphene oxide by a hummers method (oxidation-reduction method), adding water and the graphene oxide into a stirring tank, and uniformly stirring to prepare graphene oxide slurry with the solid content of 5%.
And b, coating the graphene oxide slurry prepared in the step a on a PET (polyethylene terephthalate) film serving as a substrate by adopting a coating machine, and repeating the operation twice to prepare two wet films with the sizes of 300mm multiplied by 150mm multiplied by 3 mm.
c, adopting a formula of 1: 8, diluting the epoxy resin with ethanol.
d, respectively spraying the epoxy resin diluted in the step c on the surfaces of the graphene oxide slurry of the two wet films prepared in the step b by using a spraying pot.
And e, feeding the two wet films into a blast drying oven, and baking for 3 hours at the temperature of 80 ℃ to obtain two graphene oxide dry films.
And f, taking out the two dry films, airing, coating a polyamide resin curing agent on one surface of each dry film with the epoxy resin, and adhering the surfaces of the two dry films coated with the polyamide resin curing agent together to obtain the double-layer dry film.
And g, pressing the upper surface and the lower surface of the double-layer dry film by using glass plates, and baking the double-layer dry film in a forced air drying oven at a high temperature of 120 ℃ for 3 hours to cure the epoxy resin.
And h, taking out the double-layer dry film, cooling to normal temperature, and respectively taking down the upper glass plate, the lower glass plate and the PET substrate to obtain the double-layer flat graphene oxide dry film.
The foregoing is merely a preferred embodiment of the invention and all such equivalent alterations and permutations and derivations thereof are intended to be included within the scope of the invention.
Claims (3)
1. The preparation method of the double-layer graphene oxide film is characterized in that
The method comprises the following steps:
a, selecting a 300-mesh and 500-mesh crystalline flake graphite raw material, preparing graphene oxide by a hummers method, adding water and the graphene oxide into a stirring tank, and uniformly stirring to prepare graphene oxide slurry with the solid content of 5%;
b, coating the graphene oxide slurry prepared in the step a on a polyethylene terephthalate film serving as a substrate by adopting a coating machine, and repeating the operation twice to prepare two wet films with the sizes of 300mm multiplied by 150mm multiplied by 3 mm;
c, adopting a formula of 1: 8, diluting the epoxy resin by using ethanol;
d, respectively spraying the epoxy resin diluted in the step c on the surfaces of the graphene oxide slurry of the two wet films prepared in the step b by using a spraying pot;
e, feeding the two wet films into a forced air drying oven, and baking for 3-4 hours at the temperature of 70-80 ℃ to obtain two graphene oxide dry films;
f, taking out the two dry films, airing, coating a polyamide resin curing agent on one surface of the dry film with the epoxy resin, and pasting the surfaces of the two dry films coated with the polyamide resin curing agent together to obtain a double-layer dry film;
g, respectively pressing the upper surface and the lower surface of the double-layer dry film by using glass plates, and placing the double-layer dry film into a blast drying oven to be baked for 3-4 hours at the high temperature of 110-120 ℃ so as to cure the epoxy resin;
and h, taking out the double-layer dry film, cooling to normal temperature, and respectively taking down the upper glass plate, the lower glass plate and the polyethylene terephthalate film substrate to obtain the double-layer flat graphene oxide dry film.
2. The method for preparing a double-layer graphene oxide film according to claim 1, wherein the method is characterized in that
The method comprises the following steps:
a, selecting a 300-mesh and 500-mesh crystalline flake graphite raw material, preparing graphene oxide by a hummers method, adding water and the graphene oxide into a stirring tank, and uniformly stirring to prepare graphene oxide slurry with the solid content of 5%;
b, coating the graphene oxide slurry prepared in the step a on a polyethylene terephthalate film serving as a substrate by adopting a coating machine, and repeating the operation twice to prepare two wet films with the sizes of 300mm multiplied by 150mm multiplied by 3 mm;
c, adopting a formula of 1: 8, diluting the epoxy resin by using ethanol;
d, respectively spraying the epoxy resin diluted in the step c on the surfaces of the graphene oxide slurry of the two wet films prepared in the step b by using a spraying pot;
e, feeding the two wet films into a blast drying oven, and baking for 4 hours at 70 ℃ to obtain two graphene oxide dry films;
f, taking out the two dry films, airing, coating a polyamide resin curing agent on one surface of the dry film with the epoxy resin, and pasting the surfaces of the two dry films coated with the polyamide resin curing agent together to obtain a double-layer dry film;
g, respectively pressing the upper surface and the lower surface of the double-layer dry film by using glass plates, and baking the double-layer dry film in a blast drying oven at a high temperature of 110 ℃ for 4 hours to cure the epoxy resin;
and h, taking out the double-layer dry film, cooling to normal temperature, and respectively taking down the upper glass plate, the lower glass plate and the polyethylene terephthalate film substrate to obtain the double-layer flat graphene oxide dry film.
3. The method for preparing a double-layer graphene oxide film according to claim 1, wherein the method is characterized in that
The method comprises the following steps:
a, selecting a 300-mesh and 500-mesh crystalline flake graphite raw material, preparing graphene oxide by a hummers method, adding water and the graphene oxide into a stirring tank, and uniformly stirring to prepare graphene oxide slurry with the solid content of 5%;
b, coating the graphene oxide slurry prepared in the step a on a polyethylene terephthalate film serving as a substrate by adopting a coating machine, and repeating the operation twice to prepare two wet films with the sizes of 300mm multiplied by 150mm multiplied by 3 mm;
c, adopting a formula of 1: 8, diluting the epoxy resin by using ethanol;
d, respectively spraying the epoxy resin diluted in the step c on the surfaces of the graphene oxide slurry of the two wet films prepared in the step b by using a spraying pot;
e, feeding the two wet films into a blast drying oven, and baking for 3 hours at the temperature of 80 ℃ to obtain two graphene oxide dry films;
f, taking out the two dry films, airing, coating a polyamide resin curing agent on one surface of the dry film with the epoxy resin, and pasting the surfaces of the two dry films coated with the polyamide resin curing agent together to obtain a double-layer dry film;
pressing the upper surface and the lower surface of the double-layer dry film by using a glass plate, and baking the double-layer dry film in a blast drying oven at a high temperature of 120 ℃ for 3 hours to cure the epoxy resin;
and h, taking out the double-layer dry film, cooling to normal temperature, and respectively taking down the upper glass plate, the lower glass plate and the polyethylene terephthalate film substrate to obtain the double-layer flat graphene oxide dry film.
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