CN108966376B - Collapsible electric heat membrane device based on graphite alkene - Google Patents
Collapsible electric heat membrane device based on graphite alkene Download PDFInfo
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- CN108966376B CN108966376B CN201810753780.5A CN201810753780A CN108966376B CN 108966376 B CN108966376 B CN 108966376B CN 201810753780 A CN201810753780 A CN 201810753780A CN 108966376 B CN108966376 B CN 108966376B
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- 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
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- 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
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- H05B3/03—Electrodes
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- 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—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
Abstract
The invention discloses a foldable electrothermal film device based on graphene, which comprises a heating element, a protective film and a cut-off body; the heating element is a graphene film, the thickness of the heating element is not more than 200 layers, so that the resistance of the heating element in unit area is greatly improved, in addition, the defect density ID/IG is not more than 0.05, and the electric conductivity reaches 1.2-1.5 MS/m. After being folded for 5000 times, the original electrical performance is kept.
Description
Technical Field
The invention relates to a novel heat conducting device, in particular to a foldable electric heating film device based on graphene.
Background
In 2010, Andre GeiM and Konstantin Novoselov, two professors of Manchester university in England, raised the worldwide hot trend of graphene research because of the first successful separation of stable graphene to obtain the Nobel prize of physics. The graphene has excellent electrical properties (the electron mobility can reach 2 multiplied by 105cM2/Vs at room temperature), outstanding heat conduction properties (5000W/(MK)), extraordinary specific surface area (2630M2/g), Young modulus (1100GPa) and breaking strength (125GPa), excellent electric conduction and heat conduction properties of the graphene completely exceed those of metal, meanwhile, the graphene has the advantages of high temperature resistance and corrosion resistance, and the good mechanical properties and the low density of the graphene enable the graphene to have the potential of replacing metal in the field of electric heating materials.
The graphene film of macroscopically assembled graphene oxide or graphene nanosheets is the main application form of nanoscale graphene, and common preparation methods are a suction filtration method, a scraping method, a spin-coating method, a spraying method, a dip-coating method and the like. Through further chemical or high-temperature treatment, the defects of the graphene can be repaired, the conductivity and the thermal conductivity of the graphene film can be effectively improved, and the graphene film can be widely applied to electric heating materials.
However, currently, the graphene oxide itself is not enough in size and contains a lot of fragments, so that the graphene oxide cannot be developed sufficiently in the aspect of electric heating, the electric conductivity is limited to 1MS/m, and the demand of rapid development of science and technology cannot be met. Moreover, the resistance of the micron-thick graphene film is too small, so that the film is easy to overheat; the resistance of the nano-scale chemical reduction graphene film is too large, and both of the nano-scale chemical reduction graphene film and the nano-scale chemical reduction graphene film cannot be well applied to an electric heating material. Therefore, a graphene film with the thickness of tens of nanometers is designed, a damaged structure of the graphene film is repaired at high temperature, a path is provided for high heat conduction of the graphene film, and the graphene film have good synergistic effect to control the resistivity of the film. Meanwhile, due to the existence of interlayer crosslinking of the graphene film, the film has excellent strength and thermal conductivity, is tear-resistant and is easy to radiate. In addition, the thickness of the graphene film gives it excellent flexibility, resistance to bending deformation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a foldable electric heating film device based on graphene.
The purpose of the invention is realized by the following technical scheme: a foldable electric heating film device based on graphene comprises a heating element, a protective film and two intercepting bodies, wherein the protective film is positioned on the upper side and the lower side of the heating element, and the two intercepting bodies are respectively connected with two ends of the heating element; the fluid intercepting body is a metal electrode; the heating element is a graphene film and is prepared by the following method:
(1) preparing the graphene oxide into a graphene oxide aqueous solution with the concentration of 0.5-10ug/mL, and performing suction filtration to form a film, wherein the number of layers in the thickness direction is not more than 200.
(2) And (3) putting the graphene oxide film attached to the suction filtration substrate into a closed container, and fumigating at the high temperature of 80-100 ℃ from the bottom to the top for 0.1-1 h.
(3) And uniformly coating the melted solid transfer agent on the surface of the reduced graphene oxide film, and cooling at room temperature until the film is separated from the substrate.
(4) Heating the reduced graphene oxide film treated in the step 3 to sublimate or volatilize the solid transfer agent;
(5) heating the reduced graphene oxide film at 1 ℃/min to 300 ℃ (slowly heating to increase the area of the graphene film in the unit space of the surface fold expansion of the graphene film); and then heating at the temperature of 10 ℃/min, placing at the temperature of 2000 ℃, and preserving heat for 6-12 hours to remove most of atomic defects in the graphene without recovering the stacking structure in the graphene.
(6) And (5) spraying a layer of metal nanoparticles on the surface of the graphene film treated in the step (5) in a magnetron sputtering mode. The metal nanoparticles are selected from titanium, tungsten, iron, magnesium and molybdenum. The molar amount of sputtered metal nanoparticles is no greater than 30% of the molar amount of carbon atoms in the graphene film. The graphene film sputtered with the metal nanoparticles is chloridized at 800-1200 ℃, and the metal nanoparticles are dissipated in the form of chloride.
(7) And (3) processing the chlorinated graphene film at the high temperature of 2000 ℃ to obtain the interlayer crosslinked graphene film.
Further, the solid transfer agent is selected from materials such as paraffin, naphthalene, arsenic trioxide, camphor, sulfur, norbornene, rosin and other small molecule solid materials which can be sublimated or volatilized under certain conditions and are insoluble in water.
Further, the sublimation temperature of the solid transfer agent is controlled below 320 ℃.
Further, the chlorination treatment refers to: and (3) placing the graphene film sputtered with the metal nano particles in an environment with the chlorine content of 0.5-10% for heating treatment for 0.1-4 h.
Further, in step 7, the 2000 ℃ high temperature process temperature rise process is as follows: below 1500 ℃, 5-20 ℃ per minute; above 1500 ℃ and 2-5 ℃ per minute.
Further, the protective film is a transparent polymer such as PDMS or PET.
According to the invention, firstly, an ultrathin graphene film is obtained in a solid transfer mode, so that a foundation is laid for the high resistance of a device; further, the surface wrinkles of the graphene film are increased through slow heating (1 ℃/min), and the area of the graphene film in a unit space is expanded; and then heating at a speed of 10 ℃/min and placing at 2000 ℃ to remove most of atomic defects in the graphene, but not recovering the stacking structure in the graphene. Further sputtering metal particles on the surface of the ultrathin graphene film, and reacting the metal particles with the graphene at high temperature to form metal carbide; then, under the action of chlorine, metal carbide forms metal chloride and escapes, meanwhile, the carbon structure is converted to a diamond structure, the strength (reaching 7-20GPa) and the thermal stability of the film are greatly improved, the graphene film structure is recovered to a great extent by high-temperature treatment at 2000 ℃, but an interlayer cross-linking structure is not influenced, an AB accumulation structure is not formed, and a foundation is provided for high-band-gap high conductivity of graphene.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Detailed Description
Example 1
As shown in fig. 1, a foldable electrothermal film device based on graphene comprises a heating element, a protective film and two cut-off bodies, wherein the protective film is positioned at the upper side and the lower side of the heating element, and the two cut-off bodies are respectively connected with two ends of the heating element; the protective film is a PET film, and the fluid stopping body is a metal electrode; the heating element is a graphene film and is prepared by the following method:
(1) preparing graphene oxide into a graphene oxide aqueous solution with the concentration of 0.5ug/mL, and performing suction filtration to form a film by taking the AAO film as a substrate.
(2) And (3) putting the graphene oxide membrane attached to the AAO membrane into a closed container, and fumigating the graphene oxide membrane at the high temperature of 80 ℃ from the bottom to the top for 1 h.
(3) And uniformly coating the melted solid transfer agent paraffin on the surface of the reduced graphene oxide film, and cooling at room temperature until the film is separated from the AAO film substrate.
(4) Heating the reduced graphene oxide film treated in the step 3 at 200 ℃ to volatilize the solid transfer agent;
(5) heating the reduced graphene oxide film at 1 ℃/min to 300 ℃ (slowly heating to increase the area of the graphene film in the unit space of the surface fold expansion of the graphene film); and then heating at the temperature of 10 ℃/min, placing at the temperature of 2000 ℃, and preserving heat for 6 hours to remove most of atomic defects in the graphene without recovering the stacking structure in the graphene.
(6) And (3) spraying a layer of titanium nano particles on the surface of the graphene film treated in the step (5) in a magnetron sputtering mode, and controlling sputtering parameters to finally obtain the mol weight of the sputtered metal nano particles, which is 29.4% of the mol weight of carbon atoms in the graphene film. The graphene film sputtered with the metal nanoparticles is then chlorinated at 800 ℃ and the titanium nanoparticles escape as chlorides. The method specifically comprises the following steps: and (3) placing the graphene film sputtered with the metal nanoparticles in an environment with the chlorine content of 0.5% for heating treatment for 0.1 h.
(7) Placing the chlorinated graphene film in a high-temperature furnace, and heating to 1500 ℃ at 5 ℃ per minute; and raising the temperature to 2000 ℃ per minute at the temperature of 2 ℃ to obtain the interlayer crosslinked graphene film.
The thickness of the graphene film obtained by the embodiment is 11nm (about 35 layers), so that the relatively large resistivity of the graphene film can be ensured; through Raman test, the graphene film with the graphene mold having a plurality of cross-linked structures has stronger sp3Carbon bonding Peak (1360 cm)-1) The degree of crosslinking (the degree of crosslinking is sp3 carbon content-percent by mass) was 1.2%, as measured by the ID/IG area ratio; the interlayer spacing of the electron diffraction fringes of the graphene film with the cross-linked structure is smaller than that of the normal graphene film, the defect density ID/IG of the graphene film is less than or equal to 0.05, and the electric conductivity is 1.2MS/m, so that the graphene film has beneficial electric heating performance. The graphene film has a strength of 20 GPa; after folding 5000 times, the conductivity decreased by 0.2%.
Example 2
A foldable electric heating film device based on graphene comprises a heating element, a protective film and two intercepting bodies, wherein the protective film is positioned on the upper side and the lower side of the heating element, and the two intercepting bodies are respectively connected with two ends of the heating element; the protective film is a PDMS film, and the fluid stopping body is a metal electrode; the heating element is a graphene film and is prepared by the following method:
(1) preparing the graphene oxide into a graphene oxide aqueous solution with the concentration of 10ug/mL, and performing suction filtration to form a film by taking the AAO film as a substrate.
(2) And (3) putting the graphene oxide membrane attached to the AAO membrane into a closed container, and fumigating the graphene oxide membrane at the high temperature of 100 ℃ from the bottom to the top for 0.1 h.
(3) And uniformly coating the melted solid transfer agent camphor on the surface of the reduced graphene oxide film, and cooling at room temperature until the film is separated from the AAO film substrate.
(4) Heating the reduced graphene oxide film treated in the step (3) at 80 ℃ to sublimate or volatilize the solid transfer agent;
(5) heating the reduced graphene oxide film at 1 ℃/min to 300 ℃ (slowly heating to increase the area of the graphene film in the unit space of the surface fold expansion of the graphene film); and then heating at the temperature of 10 ℃/min, placing at the temperature of 2000 ℃, and preserving heat for 8 hours to remove most of atomic defects in the graphene without recovering the stacking structure in the graphene.
(6) And (3) spraying a layer of iron nanoparticles on the surface of the graphene film treated in the step (5) in a magnetron sputtering mode, and controlling sputtering parameters to finally obtain the sputtered metal nanoparticles with the molar weight of 8.6% of the molar weight of carbon atoms in the graphene film. The graphene film sputtered with the metal nanoparticles is then chlorinated at 1200 c, and the iron nanoparticles escape as chlorides. The method specifically comprises the following steps: and (3) placing the graphene film sputtered with the metal nanoparticles in an environment with the chlorine content of 10% for heating treatment for 4 h.
(7) Placing the chlorinated graphene film in a high-temperature furnace, and heating to 1500 ℃ at 20 ℃ per minute; raising the temperature to 2000 ℃ per minute at 5 ℃, and preserving the heat for 1h to obtain the interlayer crosslinked graphene film.
The thickness of the graphene film obtained by the embodiment is 68nm (about 200 layers), so that the relatively large resistivity of the graphene film can be ensured; through Raman test, the graphene film with the graphene mold having a plurality of cross-linked structures has stronger sp3Carbon bonding Peak (1360 cm)-1) The degree of crosslinking (the degree of crosslinking is sp3 carbon content-percent by mass) was 2.5%, as measured by the ID/IG area ratio; the interlayer spacing of the electron diffraction fringes of the graphene film with the cross-linked structure is smaller than that of the normal graphene film, the defect ID/IG of the graphene film is less than or equal to 0.05, and the electric conductivity is 1.3MS/m, so that the graphene film has beneficial electric heating performance. The graphene film has a strength of 18 GPa; after folding 5000 times, the conductivity decreased by 0.5%.
Example 3
A foldable electric heating film device based on graphene comprises a heating element, a protective film and two intercepting bodies, wherein the protective film is positioned on the upper side and the lower side of the heating element, and the two intercepting bodies are respectively connected with two ends of the heating element; the protective film is a PDMS film, and the fluid stopping body is a metal electrode; the heating element is a graphene film and is prepared by the following method:
(1) preparing the graphene oxide into a graphene oxide aqueous solution with the concentration of 5ug/mL, and performing suction filtration to form a film by taking the AAO film as a substrate.
(2) And (3) putting the graphene oxide membrane attached to the AAO membrane into a closed container, and fumigating the graphene oxide membrane at the high temperature of 100 ℃ from the bottom to the top for 1 h.
(3) And uniformly coating the melted solid transfer agent paraffin on the surface of the reduced graphene oxide film, and cooling at room temperature until the film is separated from the AAO film substrate.
(4) Heating the reduced graphene oxide film treated in the step 3 at 200 ℃ to volatilize the solid transfer agent;
(5) heating the reduced graphene oxide film at 1 ℃/min to 300 ℃ (slowly heating to increase the area of the graphene film in the unit space of the surface fold expansion of the graphene film); and then heating at the temperature of 10 ℃/min, placing at the temperature of 2000 ℃, and preserving heat for 12 hours to remove most of atomic defects in the graphene without recovering the stacking structure in the graphene.
(6) And (3) spraying a layer of molybdenum nanoparticles on the surface of the graphene film treated in the step (5) in a magnetron sputtering mode, and controlling sputtering parameters to finally obtain the final sputtered metal nanoparticles with the molar weight of 15.8% of the molar weight of carbon atoms in the graphene film. The graphene film sputtered with the metal nanoparticles was then chlorinated at 1000 ℃ and the molybdenum nanoparticles escaped as chlorides. The method specifically comprises the following steps: and (3) placing the graphene film sputtered with the metal nanoparticles in an environment with the chlorine content of 5% for heating treatment for 1 h.
(7) Placing the chlorinated graphene film in a high-temperature furnace, and heating to 1500 ℃ at 10 ℃ per minute; and raising the temperature to 2000 ℃ per minute at the temperature of 2 ℃ to obtain the interlayer crosslinked graphene film.
The thickness of the graphene film obtained by the embodiment is 29nm (about 90 layers), so that the relatively large resistivity of the graphene film can be ensured; through Raman test, the graphene film with the graphene mold having a plurality of cross-linked structures has stronger sp3Carbon bonding Peak (1360 cm)-1) The degree of crosslinking (the degree of crosslinking is sp3 carbon content-percent by mass) was 4.4% as measured by the ID/IG area ratio; the interlayer spacing of the electron diffraction fringes of the graphene film with the cross-linked structure is smaller than that of the normal graphene film, the defect density ID/IG of the graphene film is less than or equal to 0.05, and the electric conductivity is 1.5MS/m, so that the graphene film has beneficial electric heating performance. The graphene film has a strength of 15 GPa; the conductivity decreased by 0.4% after folding 5000 times.
Claims (6)
1. The foldable electric heating film device based on graphene is characterized by comprising a heating element, a protective film and two intercepting bodies, wherein the protective film is positioned on the upper side and the lower side of the heating element, and the two intercepting bodies are respectively connected with two ends of the heating element; the fluid intercepting body is a metal electrode; the heating element is a graphene film and is prepared by the following method:
(1) preparing graphene oxide into a graphene oxide aqueous solution with the concentration of 0.5-10ug/mL, and performing suction filtration to form a film, wherein the number of layers in the thickness direction is not more than 200;
(2) putting the graphene oxide film attached to the suction filtration substrate into a closed container, and fumigating at the high temperature of 80-100 ℃ from the bottom to the top for 0.1-1 h;
(3) uniformly coating the melted solid transfer agent on the surface of the reduced graphene oxide film, and cooling at room temperature until the film is separated from the substrate;
(4) heating the reduced graphene oxide film treated in the step (3) to sublimate or volatilize the solid transfer agent;
(5) heating the reduced graphene oxide film at 1 ℃/min to 300 ℃; then heating at the temperature of 10 ℃/min, placing at 2000 ℃, and preserving heat for 6-12 hours to remove most of atomic defects in the graphene without recovering the stacking structure in the graphene;
(6) spraying a layer of metal nanoparticles on the surface of the graphene film treated in the step (5) in a magnetron sputtering mode; the metal nanoparticles are selected from titanium, tungsten, iron, magnesium and molybdenum, the molar weight of the sputtered metal nanoparticles is not more than 30% of the molar weight of carbon atoms in the graphene film, the graphene film sputtered with the metal nanoparticles is subjected to chlorination treatment at 800-1200 ℃, and the metal nanoparticles escape in the form of chloride;
(7) and (3) processing the chlorinated graphene film at the high temperature of 2000 ℃ to obtain the interlayer crosslinked graphene film.
2. The electrothermal film device of claim 1, wherein the solid transfer agent is selected from the group consisting of paraffin, camphor, and rosin.
3. The electrothermal film device of claim 1, wherein the sublimation temperature of the solid transfer agent is controlled to be less than 320 degrees.
4. The electrothermal film device of claim 1, wherein the chlorination treatment is: and (3) placing the graphene film sputtered with the metal nano particles in an environment with the chlorine content of 0.5-10% for heating treatment for 0.1-4 h.
5. The electrothermal film device according to claim 1, wherein in step (7), the 2000 ℃ high temperature process heating process is as follows: below 1500 ℃, 5-20 ℃ per minute; above 1500 ℃ and 2-5 ℃ per minute.
6. The electrothermal film device of claim 1, wherein the protective film is PDMS or PET.
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