CN114258166A - Preparation method of graphene integrated heating decorative plate - Google Patents
Preparation method of graphene integrated heating decorative plate Download PDFInfo
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- CN114258166A CN114258166A CN202111674944.3A CN202111674944A CN114258166A CN 114258166 A CN114258166 A CN 114258166A CN 202111674944 A CN202111674944 A CN 202111674944A CN 114258166 A CN114258166 A CN 114258166A
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Images
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method of a graphene integrated heating decorative plate, which relates to the technical field of graphene and comprises the following steps: material processing, solution preparation, gas processing, tablet pressing, film packaging and auxiliary material addition; according to the invention, the graphene nanometer solution is treated by the reactive gas and the carbon precursor, vapor deposition can increase domain size of graphene, reduce domain boundary of graphene, and improve space saturation between graphene domains, so that the graphene is filled with carbon atoms to form a granulation layer with higher density, physical and chemical properties of the graphene layer are improved, and the addition of the carbon nanotube and the carbon nanofiber is matched to enhance conductivity, stability and far infrared conversion efficiency, and the thermal conversion efficiency of the graphene can be effectively improved through verification; in addition, the waste asphalt is used for preparing the graphene, so that the waste asphalt is convenient to circulate, the waste asphalt is low in price and easy to obtain, the preparation cost of the graphene is reduced, and the economic benefit is improved.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a preparation method of a graphene integrated heating decorative plate.
Background
Graphene (Graphene) is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The graphene has excellent optical, electrical and mechanical propertiesThe material has the characteristics of having important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. In the electric heating products in the existing market, different electric heating products have different technical contents and different characteristics and application fields, and a plurality of electric heating products are roughly divided into a plurality of types, namely metal resistance hot wires, printing ink types, ultra-thin metal sheet types, carbon fiber types and functional polymer electric heating types;
in recent years, due to the application of a graphene technology, a graphene electrothermal film has entered into life, the graphene electrothermal film is under the action of an electric field, carbon molecular groups in a heating body generate Brownian motion, violent friction and impact are generated among carbon molecules, generated heat energy is transmitted outwards in the form of far infrared radiation and convection, the surface of a system is rapidly heated under the action of the carbon molecules, and the heat conversion efficiency of the existing graphene electrothermal film is low due to the saturation degree of internal carbon atoms, so that the invention provides a preparation method of the graphene integrated heating decorative plate to solve the problems in the prior art.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a graphene integrated heating decorative plate, which can effectively improve the heat conversion efficiency of graphene.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme: the preparation method of the graphene integrated heating decorative plate comprises the following steps:
material treatment, namely screening and centrifuging waste asphalt, adding an auxiliary agent, mixing, and carbonizing at high temperature to obtain a graphene raw material;
preparing a solution, namely mixing and stirring a graphene raw material, carbon nanofibers, carbon nanotubes, nano polyethylene and a resin solution to prepare a graphene nano solution;
gas treatment, namely introducing reactive gas and a carbon precursor, carrying out vapor deposition treatment on the graphene nano solution, and cooling the graphene nano solution to room temperature after treatment;
pressing into tablets, freezing the graphene nano solution in vacuum, drying and solidifying into gel, then pressing the graphene nano gel into the gel sheets by using a tablet press, and drying to form a film;
film packaging, namely taking a PI film as a packaging film, forming a PTC thermosensitive film monitoring circuit on the surface of the packaging film by adopting a vacuum coating process, pressing and attaching the packaging film and a graphene film, and spraying a polymer on the surface for protection;
adding auxiliary materials, sprinkling film ball beads in the polymer, filling negative ion powder in the film balls to obtain a finished film, and laminating the finished film, a capacitance current absorption layer and a PVC protective layer to prepare the plate.
The further improvement lies in that: in the material treatment, waste asphalt is subjected to crushing treatment and screening treatment, then is mixed and stirred with a solvent to obtain a mixture, the mixture is subjected to centrifugal filtration to remove particles to obtain a supernatant slurry, then is subjected to separation treatment to obtain asphalt, a bottom material is obtained by stirring and reacting the asphalt and an auxiliary agent, the bottom material is subjected to high-temperature carbonization treatment and is ground to obtain carbon powder, the carbon powder is roasted at high temperature and is mixed and stirred with an acetone solution to obtain a carbon powder mixed solution, the carbon powder mixed solution is introduced into an ultrasonic oscillator to be subjected to oscillation dispersion treatment, and then is atomized and dried to obtain graphene.
The further improvement lies in that: in the material treatment, the solvent is one or more of dichlorohydrocarbon of C2-C5, alkane of C6-C9 or monocyclic aromatic hydrocarbon of C9-C10, and the auxiliary agent is the mixture of polyethylene glycol dimethyl ether, calcium carbonate and molybdenum sulfide.
The further improvement lies in that: in the preparation of the solution, the graphene raw material, the carbon nanofiber, the nano polyethylene and the resin solution are mixed and stirred at normal temperature, the stirring reaction speed is controlled to be 300-500 revolutions per minute, and the stirring is carried out for 1-3 hours.
The further improvement lies in that: in the gas treatment, the graphene nanometer solution is put into a reaction furnace, then the mixed gas containing the reactive gas and the carbon precursor is introduced into the graphene nanometer solution at the speed of 80-120 ml/min in the standard state, the temperature in the reaction furnace is raised to 100-15 ℃, the graphene nanometer solution is subjected to heat treatment for 10-30 seconds in the pressure environment of 100-.
The further improvement lies in that: in the gas treatment, the carbon precursor is any one of carbon monoxide, carbon dioxide, methane, ethane, ethyl, butylene, pentane, pentene, cyclopentadiene, hexane, cyclohexane or toluene, and the reaction gas is one or more of argon, nitrogen, hydrogen, ammonia or helium.
The further improvement lies in that: when the graphene nano-solution is pressed into a tablet, a vacuum refrigerator is opened, the graphene nano-solution is pre-frozen, the pre-freezing is maintained for 1 to 1.5 hours, and the pre-freezing is finished; transferring the pre-frozen graphene nano solution onto a dryer, and performing vacuum pumping operation by using a vacuum pump to ensure that the internal vacuum degree is less than 20 Pa, and drying for 2-5 hours to obtain fluffy graphene oxide solid; and then dropwise adding an ethanol solution and water into the graphene oxide solid, moving the graphene oxide solid into an ultrasonic instrument for ultrasonic operation for 1 hour, concentrating, solidifying to form gel, finally pressing the gel into a gel sheet by using a tablet press, and drying to form a film.
The further improvement lies in that: in the thin film packaging process, photoresist is coated on the surface of a PI film, then patterned photoresist is obtained through exposure and development processes, a PTC thermosensitive thin film layer is obtained on the surface of a PI substrate with the patterned photoresist on the surface by a sputtering method or a vacuum evaporation method, and then the photoresist is removed to obtain the PTC thermosensitive thin film patterned circuit.
The further improvement lies in that: in the thin film packaging, at least one coating method of spin coating, spray coating, drop coating and bar coating is adopted to coat the polymer material for 40-60 seconds at the rotating speed of 2000-2500 rpm to form a polymer protective layer, wherein the polymer material is one of polymethyl methacrylate and polydimethylsiloxane.
The further improvement lies in that: the film ball is broken by heating.
The invention has the beneficial effects that:
1. according to the invention, the graphene nanometer solution is treated by the reactive gas and the carbon precursor, vapor deposition can increase the domain size of graphene, reduce the domain boundary of graphene, and improve the space saturation between graphene domains, so that the graphene is filled with carbon atoms to form a granulation layer with higher density, the physical and chemical properties of the graphene layer are improved, and the addition of the carbon nanotube and the carbon nanofiber is matched to enhance the conductivity, the stability and the far infrared conversion efficiency, and the thermal conversion efficiency of the graphene can be effectively improved through verification.
2. According to the method, the waste asphalt is used for preparing the graphene, so that the waste asphalt is convenient to circulate, the waste asphalt is low in price and easy to obtain, the preparation cost of the graphene is reduced, and the economic benefit is improved.
3. The invention is added with the film ball, the film ball is filled with the anion powder, and the film ball is broken by heating, so that the anion powder can be released, and the health care function is provided.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a schematic view of a pressed board according to the present invention.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
Example one
According to fig. 1 and 2, the embodiment provides a preparation method of a graphene integrated heating decoration plate, which includes the following steps:
material treatment, namely screening and centrifuging waste asphalt, adding an auxiliary agent, mixing, and carbonizing at high temperature to obtain a graphene raw material;
preparing a solution, namely mixing and stirring the graphene raw material, the nano carbon fiber, the nano polyethylene and the resin solution at normal temperature, controlling the stirring reaction speed to be 300-;
gas treatment, namely introducing reactive gas and a carbon precursor, carrying out vapor deposition treatment on the graphene nano solution, and cooling the graphene nano solution to room temperature after treatment;
pressing into tablets, opening a vacuum refrigerator, pre-freezing the graphene nano solution, maintaining for 1-1.5 hours, and finishing pre-freezing; transferring the pre-frozen graphene nano solution onto a dryer, and performing vacuum pumping operation by using a vacuum pump to ensure that the internal vacuum degree is less than 20 Pa, and drying for 2-5 hours to obtain fluffy graphene oxide solid; then, dropwise adding an ethanol solution and water into the graphene oxide solid, moving the graphene oxide solid into an ultrasonic instrument for ultrasonic operation for 1 hour, concentrating, solidifying to form gel, finally pressing the gel into a gel sheet by using a tablet press and drying to form a film;
film packaging, namely taking a PI film as a packaging film, forming a PTC thermosensitive film monitoring circuit on the surface of the packaging film by adopting a vacuum coating process, pressing and attaching the packaging film and a graphene film, and spraying a polymer on the surface for protection;
adding auxiliary materials, sprinkling film ball beads in the polymer, filling negative ion powder in the film balls to obtain a finished film, and laminating the finished film, a capacitance current absorption layer and a PVC protective layer to prepare the plate.
According to the invention, the graphene nanometer solution is treated by the reactive gas and the carbon precursor, vapor deposition can increase the domain size of graphene, reduce the domain boundary of graphene, and improve the space saturation between graphene domains, so that the graphene is filled with carbon atoms to form a granulation layer with higher density, the physical and chemical properties of the graphene layer are improved, and the addition of the carbon nanotube and the carbon nanofiber is matched to enhance the conductivity, the stability and the far infrared conversion efficiency, and the thermal conversion efficiency of the graphene can be effectively improved through verification. In addition, the waste asphalt is used for preparing the graphene, so that the waste asphalt is convenient to circulate, the waste asphalt is low in price and easy to obtain, the preparation cost of the graphene is reduced, and the economic benefit is improved. Meanwhile, the film ball is added, the negative ion powder is filled in the film ball, and the film ball is broken by heating, so that the negative ion powder can be released, and a health-care effect is provided.
Example two
The embodiment provides a preparation method of a graphene integrated heating decorative plate, which comprises the following steps:
in the material treatment, waste asphalt is subjected to crushing treatment and screening treatment, then is mixed and stirred with a solvent to obtain a mixture, the mixture is subjected to centrifugal filtration to remove particles to obtain a supernatant slurry, then is subjected to separation treatment to obtain asphalt, a bottom material is obtained by stirring and reacting the asphalt and an auxiliary agent, the bottom material is subjected to high-temperature carbonization treatment and is ground to obtain carbon powder, the carbon powder is roasted at high temperature and is mixed and stirred with an acetone solution to obtain a carbon powder mixed solution, the carbon powder mixed solution is introduced into an ultrasonic oscillator to be subjected to oscillation dispersion treatment, and then is atomized and dried to obtain graphene. The solvent is one or more of dichlorohydrocarbon of C2-C5, alkane of C6-C9 or monocyclic aromatic hydrocarbon of C9-C10, and the auxiliary agent is a mixture of polyethylene glycol dimethyl ether, calcium carbonate and molybdenum sulfide.
The method specifically comprises the following steps: firstly adding waste asphalt into a crusher to perform crushing treatment to obtain waste asphalt blocks, then adding the waste asphalt blocks into a vibration screening machine to perform screening treatment to remove impurities, mixing and stirring the screened waste asphalt blocks and a solvent for 20-30 minutes, performing solvent extraction treatment to dissolve the asphalt in the waste asphalt blocks into the solvent to obtain a mixture, controlling the mixing and stirring speed to be 150-200 r/min, then controlling the rotating speed of an ultrahigh-speed centrifuge to be 2000-3000 r/min, then pouring supernatant slurry into a reaction vessel to perform sedimentation treatment for 5-7 hours, then heating the supernatant slurry in the reaction vessel to 150-200 ℃ to perform distillation separation to obtain the asphalt and recovering the solvent. Adding the obtained asphalt and the auxiliary agent into a mixing and stirring container according to the mass ratio of 100:1-100:5, stirring and reacting for 40-50 minutes to obtain a base material, wherein in the high-temperature carbonization treatment, the pressure in a vacuum drier is 26-32Mpa, the temperature of the high-temperature carbonization treatment is 300-450 ℃, and the powder grade of the grinding treatment is 600-800-mesh sieving. Then baking for 20-25 minutes at a high temperature of 500-600 ℃. And during the final atomization drying, controlling the temperature in the centrifugal spray dryer to be 55-75 ℃ to obtain the graphene.
According to the method, the waste asphalt is used for preparing the graphene, so that the waste asphalt is convenient to circulate, the waste asphalt is low in price and easy to obtain, the preparation cost of the graphene is reduced, and the economic benefit is improved.
EXAMPLE III
The embodiment provides a preparation method of a graphene integrated heating decorative plate, which comprises the following steps:
in the gas treatment, the graphene nanometer solution is put into a reaction furnace, then the mixed gas containing the reactive gas and the carbon precursor is introduced into the graphene nanometer solution at the speed of 80-120 ml/min in the standard state, the temperature in the reaction furnace is raised to 100-15 ℃, the graphene nanometer solution is subjected to heat treatment for 10-30 seconds in the pressure environment of 100-. In the gas treatment, the carbon precursor is any one of carbon monoxide, carbon dioxide, methane, ethane, ethyl, butylene, pentane, pentene, cyclopentadiene, hexane, cyclohexane or toluene, and the reaction gas is one or more of argon, nitrogen, hydrogen, ammonia or helium.
According to the invention, the graphene nanometer solution is treated by the reactive gas and the carbon precursor, vapor deposition can increase the domain size of graphene, reduce the domain boundary of graphene, and improve the space saturation between graphene domains, so that the graphene is filled with carbon atoms to form a granulation layer with higher density, the physicochemical property of the graphene layer is improved, and the thermal conversion efficiency of the graphene can be effectively improved through verification.
Example four
The embodiment provides a preparation method of a graphene integrated heating decorative plate, which comprises the following steps:
in the thin film packaging process, photoresist is coated on the surface of a PI film, then patterned photoresist is obtained through exposure and development processes, a PTC thermosensitive thin film layer is obtained on the surface of a PI substrate with the patterned photoresist on the surface by a sputtering method or a vacuum evaporation method, and then the photoresist is removed to obtain the PTC thermosensitive thin film patterned circuit. In the thin film packaging, at least one coating method of spin coating, spray coating, drop coating and bar coating is adopted to coat the polymer material for 40-60 seconds at the rotating speed of 2000-2500 rpm to form a polymer protective layer, wherein the polymer material is one of polymethyl methacrylate and polydimethylsiloxane.
Arranging a layer of epoxy glue on one side of the PTC circuit of the PI packaging substrate, and pre-curing for 30 minutes at the temperature of 60-140 ℃, wherein the thickness of the pre-cured epoxy glue is 10-30 microns.
The PTC electric heating film surface temperature monitoring device adopts the PTC circuit to monitor the electric heating film surface temperature in a large range, can effectively prevent the electric heating film temperature from being out of control, and improves the use safety of the electric heating film; in addition, PTC circuit patterns are prepared on the surface of the packaging material, the adhesive force is good, PTC and graphene heating layer materials can be isolated, and the defects that the PTC is easy to fall off and poor in bending resistance and the like when being directly arranged on the surface of the graphene heating layer are avoided.
EXAMPLE five
The embodiment provides a preparation method of a graphene integrated heating decorative plate, which comprises the following steps:
adding auxiliary materials, sprinkling film ball beads in the polymer, filling negative ion powder in the film balls, and heating the film balls to crack.
The invention is added with the film ball, the film ball is filled with the anion powder, and the film ball is broken by heating, so that the anion powder can be released, and the health care function is provided.
Verification example: calculating to obtain theoretical sheet resistance R through a formula R ═ rho/d, wherein rho is the resistivity of the graphene film, and d is the thickness of the graphite film; measuring a plurality of square resistance values of the graphene film by a voltammetry method, and calculating the average square resistance; and comparing the average sheet resistance with the theoretical sheet resistance, and judging whether the graphene film is qualified.
After verification: the electrothermal conversion efficiency of the graphene electrothermal film produced by the invention is as high as 99.8%.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The preparation method of the graphene integrated heating decorative plate is characterized by comprising the following steps:
material treatment, namely screening and centrifuging waste asphalt, adding an auxiliary agent, mixing, and carbonizing at high temperature to obtain a graphene raw material;
preparing a solution, namely mixing and stirring a graphene raw material, carbon nanofibers, carbon nanotubes, nano polyethylene and a resin solution to prepare a graphene nano solution;
gas treatment, namely introducing reactive gas and a carbon precursor, carrying out vapor deposition treatment on the graphene nano solution, and cooling the graphene nano solution to room temperature after treatment;
pressing into tablets, freezing the graphene nano solution in vacuum, drying and solidifying into gel, then pressing the graphene nano gel into the gel sheets by using a tablet press, and drying to form a film;
film packaging, namely taking a PI film as a packaging film, forming a PTC thermosensitive film monitoring circuit on the surface of the packaging film by adopting a vacuum coating process, pressing and attaching the packaging film and a graphene film, and spraying a polymer on the surface for protection;
adding auxiliary materials, sprinkling film ball beads in the polymer, filling negative ion powder in the film balls to obtain a finished film, and laminating the finished film, a capacitance current absorption layer and a PVC protective layer to prepare the plate.
2. The preparation method of the graphene integrated heating decoration plate according to claim 1, wherein: in the material treatment, waste asphalt is subjected to crushing treatment and screening treatment, then is mixed and stirred with a solvent to obtain a mixture, the mixture is subjected to centrifugal filtration to remove particles to obtain a supernatant slurry, then is subjected to separation treatment to obtain asphalt, a bottom material is obtained by stirring and reacting the asphalt and an auxiliary agent, the bottom material is subjected to high-temperature carbonization treatment and is ground to obtain carbon powder, the carbon powder is roasted at high temperature and is mixed and stirred with an acetone solution to obtain a carbon powder mixed solution, the carbon powder mixed solution is introduced into an ultrasonic oscillator to be subjected to oscillation dispersion treatment, and then is atomized and dried to obtain graphene.
3. The preparation method of the graphene integrated heating decoration plate according to claim 2, wherein: in the material treatment, the solvent is one or more of dichlorohydrocarbon of C2-C5, alkane of C6-C9 or monocyclic aromatic hydrocarbon of C9-C10, and the auxiliary agent is the mixture of polyethylene glycol dimethyl ether, calcium carbonate and molybdenum sulfide.
4. The preparation method of the graphene integrated heating decoration plate according to claim 1, wherein: in the preparation of the solution, the graphene raw material, the carbon nanofiber, the nano polyethylene and the resin solution are mixed and stirred at normal temperature, the stirring reaction speed is controlled to be 300-500 revolutions per minute, and the stirring is carried out for 1-3 hours.
5. The preparation method of the graphene integrated heating decoration plate according to claim 1, wherein: in the gas treatment, the graphene nanometer solution is put into a reaction furnace, then the mixed gas containing the reactive gas and the carbon precursor is introduced into the graphene nanometer solution at the speed of 80-120 ml/min in the standard state, the temperature in the reaction furnace is raised to 100-15 ℃, the graphene nanometer solution is subjected to heat treatment for 10-30 seconds in the pressure environment of 100-.
6. The preparation method of the graphene integrated heating decoration plate according to claim 5, wherein: in the gas treatment, the carbon precursor is any one of carbon monoxide, carbon dioxide, methane, ethane, ethyl, butylene, pentane, pentene, cyclopentadiene, hexane, cyclohexane or toluene, and the reaction gas is one or more of argon, nitrogen, hydrogen, ammonia or helium.
7. The preparation method of the graphene integrated heating decoration plate according to claim 1, wherein: when the graphene nano-solution is pressed into a tablet, a vacuum refrigerator is opened, the graphene nano-solution is pre-frozen, the pre-freezing is maintained for 1 to 1.5 hours, and the pre-freezing is finished; transferring the pre-frozen graphene nano solution onto a dryer, and performing vacuum pumping operation by using a vacuum pump to ensure that the internal vacuum degree is less than 20 Pa, and drying for 2-5 hours to obtain fluffy graphene oxide solid; and then dropwise adding an ethanol solution and water into the graphene oxide solid, moving the graphene oxide solid into an ultrasonic instrument for ultrasonic operation for 1 hour, concentrating, solidifying to form gel, finally pressing the gel into a gel sheet by using a tablet press, and drying to form a film.
8. The preparation method of the graphene integrated heating decoration plate according to claim 1, wherein: in the thin film packaging process, photoresist is coated on the surface of a PI film, then patterned photoresist is obtained through exposure and development processes, a PTC thermosensitive thin film layer is obtained on the surface of a PI substrate with the patterned photoresist on the surface by a sputtering method or a vacuum evaporation method, and then the photoresist is removed to obtain the PTC thermosensitive thin film patterned circuit.
9. The preparation method of the graphene integrated heating decoration plate according to claim 8, wherein: in the thin film packaging, at least one coating method of spin coating, spray coating, drop coating and bar coating is adopted to coat the polymer material for 40-60 seconds at the rotating speed of 2000-2500 rpm to form a polymer protective layer, wherein the polymer material is one of polymethyl methacrylate and polydimethylsiloxane.
10. The preparation method of the graphene integrated heating decoration plate according to claim 1, wherein: the film ball is broken by heating.
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Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107182140A (en) * | 2016-03-11 | 2017-09-19 | 江苏同创节能科技有限公司 | A kind of graphene is modified the preparation method of far-infrared electrothermal film |
CN109423130A (en) * | 2017-06-26 | 2019-03-05 | 北京绿能嘉业新能源有限公司 | The manufacturing process of graphene nano far-infrared negative-ion electric heating film |
CN109449308A (en) * | 2018-10-30 | 2019-03-08 | 厦门信果石墨烯科技有限公司 | A kind of graphene isolation gear film and preparation method |
CN109618433A (en) * | 2018-12-20 | 2019-04-12 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene safe voltage heating film |
CN111825086A (en) * | 2020-08-07 | 2020-10-27 | 河南墨特石墨烯科技有限公司 | Graphene preparation method |
CN112351523A (en) * | 2020-11-17 | 2021-02-09 | 黄华 | Preparation method of graphene carbon nanotube flexible conductive film |
CN112911741A (en) * | 2021-01-18 | 2021-06-04 | 安徽宇航派蒙健康科技股份有限公司 | Preparation method of flexible graphene electrothermal film |
CN112920569A (en) * | 2021-04-07 | 2021-06-08 | 深圳市骏鼎达新材料股份有限公司 | Carbon fiber composite material and preparation method thereof |
-
2021
- 2021-12-31 CN CN202111674944.3A patent/CN114258166A/en active Pending
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107182140A (en) * | 2016-03-11 | 2017-09-19 | 江苏同创节能科技有限公司 | A kind of graphene is modified the preparation method of far-infrared electrothermal film |
CN109423130A (en) * | 2017-06-26 | 2019-03-05 | 北京绿能嘉业新能源有限公司 | The manufacturing process of graphene nano far-infrared negative-ion electric heating film |
CN109449308A (en) * | 2018-10-30 | 2019-03-08 | 厦门信果石墨烯科技有限公司 | A kind of graphene isolation gear film and preparation method |
CN109618433A (en) * | 2018-12-20 | 2019-04-12 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene safe voltage heating film |
CN111825086A (en) * | 2020-08-07 | 2020-10-27 | 河南墨特石墨烯科技有限公司 | Graphene preparation method |
CN112351523A (en) * | 2020-11-17 | 2021-02-09 | 黄华 | Preparation method of graphene carbon nanotube flexible conductive film |
CN112911741A (en) * | 2021-01-18 | 2021-06-04 | 安徽宇航派蒙健康科技股份有限公司 | Preparation method of flexible graphene electrothermal film |
CN112920569A (en) * | 2021-04-07 | 2021-06-08 | 深圳市骏鼎达新材料股份有限公司 | Carbon fiber composite material and preparation method thereof |
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