CN109673068B - Production method for manufacturing electrothermal film by using graphene composite nano material - Google Patents
Production method for manufacturing electrothermal film by using graphene composite nano material Download PDFInfo
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- CN109673068B CN109673068B CN201811589173.6A CN201811589173A CN109673068B CN 109673068 B CN109673068 B CN 109673068B CN 201811589173 A CN201811589173 A CN 201811589173A CN 109673068 B CN109673068 B CN 109673068B
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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
- H05B3/12—Heater 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—Heater 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
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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
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
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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
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
Abstract
The invention discloses a production method for manufacturing an electrothermal film by using a graphene composite nano material, which comprises the following steps: adding zinc acetate dihydrate into diethylene glycol for refluxing, centrifugally cleaning and collecting a product after the reaction is finished, and drying to obtain ZnO nano powder; adding ZnO nano powder into a graphene oxide ethanol solution to obtain a mixed solution, performing ultrasonic dispersion on the mixed solution, uniformly mixing, performing freeze drying to obtain powder, and performing thermal reduction to obtain a ZnO-Go nano composite material; the ZnO-Go nano composite material and aluminum chloride are used as reactants, copper acetate monohydrate and manganese acetate tetrahydrate are used as doping agents, ethylene glycol monomethyl ether is used as a cosolvent, ethanol is used as a solvent, a coating liquid is obtained by dissolution and aging, a substrate to be coated is heated, and the coating liquid is hydrolyzed on the surface of the substrate to form the AZO electrothermal film. The formula of the electrothermal film liquid makes full use of the excellent physical and chemical properties of graphene, and the produced electrothermal film has the advantages of excellent performance, stable power and lower power attenuation.
Description
Technical Field
The invention relates to a production method for manufacturing an electrothermal film by using a graphene composite nano material, in particular to the technical field of electric heating.
Background
Graphene is a new material with a single-layer sheet structure formed by carbon atoms, and has excellent characteristics of high charge carrying capacity, low resistivity, high electrical conductivity, high thermal conductivity and the like. The graphene has extremely high conductivity, and the concentration of hole and electron carriers can reach 1013cm-2Electrons directly migrate in the graphene layer without scattering, and the carrier mobility can reach 15000cm2V. s. The graphene structure is also very stable, and the flexible outer surface can be subjected to bending deformation to adapt to external force, so that the lattice structure is kept stable, the thermal conductivity of the graphene structure is more excellent than that of any known material, and the thermal conductivity of the graphene structure is as high as 5300W/m.K. The graphene has light weight, extremely large specific surface area, remarkable electrochemical performance and excellent heat conduction performance, is very suitable to be used as a nano-scale substrate for synthesizing a new composite material, is used for improving the electrochemical performance and stability of the nano-material, and has wide application prospect.
Based on the characteristics, the graphene is used for compounding related compounds to obtain a new modified material, and the new material is used for participating in the preparation of the electrothermal membrane liquid, so that the prepared electrothermal membrane has excellent performance, and the stability of the conductivity and the thermal stability of the work are greatly improved.
At present, the electrothermal film produced by the prior art is frequently used under the high-temperature condition to cause two phenomena, namely poor thermal stability and easy damage. Secondly, under the condition of high temperature for a long time (generally more than 100 hours), the conductivity is sharply reduced, and the power attenuation of the electrothermal film is serious, so that the use value is lost. The invention aims to overcome the defects of the prior art and provides a high-temperature-resistant electrothermal film which keeps stable conductivity and good thermal stability under the working condition of high temperature (300-750 ℃) and a production method thereof.
Disclosure of Invention
The invention aims to provide a production method for manufacturing an electrothermal film by using a graphene composite nano material.
A production method for manufacturing an electrothermal film by using a graphene composite nano material comprises the following steps:
step one, adding 40-60g of zinc acetate dihydrate into 700-900 ml of diethylene glycol, uniformly mixing, refluxing the solution at 150-160 ℃ for 1-1.5 hours, centrifugally cleaning and collecting the product after the reaction is finished, and drying at 78-80 ℃ for 10-12 hours to obtain ZnO nano powder;
step two, adding 40-60g of ZnO nano powder into 800-850ml of graphene oxide ethanol solution to obtain a mixed solution, carrying out ultrasonic dispersion on the mixed solution for 1-1.5 hours to obtain a gray ZnO-GO suspension, uniformly mixing, carrying out freeze drying to obtain powder, and carrying out thermal reduction at 550-650 ℃ to obtain the ZnO-Go nano composite material;
step three, taking ZnO-Go nano composite material and aluminum chloride as reactants, taking copper acetate monohydrate and manganese acetate tetrahydrate as doping agents, taking ethylene glycol monomethyl ether as a cosolvent and ethanol as a solvent, and dissolving and aging to obtain the coating liquid, wherein the specific method comprises the following steps: weighing 10-20g of ZnO-Go nanocomposite, adding the ZnO-Go nanocomposite into 100-200ml of ethylene glycol monomethyl ether, uniformly stirring, weighing 0.5-1.2g of aluminum trichloride hexahydrate, weighing 0.2-0.5g of copper acetate monohydrate, and adding 0.15-0.4g of manganese acetate tetrahydrate into the solution for continuous stirring; measuring 350ml of ethanol, slowly adding the solution into the solution, stirring the solution for 2 hours by using a magnetic stirring instrument to obtain a transparent and stable solution, and aging the solution for 24 hours to obtain a coating solution;
and step four, heating the substrate to be coated to 300-400 ℃, and thermally decomposing the coating liquid prepared in the step three on the surface of the substrate by spraying to form the AZO electrothermal film.
Compared with the prior art, the invention has the following beneficial effects: the formula of the electrothermal film liquid fully utilizes the excellent physical and chemical characteristics of graphene, the proportioning is scientific and reasonable, the produced electrothermal film appliance has excellent performance and rapid temperature rise, and only 3 minutes and 15 seconds are needed when the temperature is raised from 20 ℃ to 750 ℃ (while 4 minutes and 23 seconds are needed when the graphene nano material is not compounded); and the power is extremely stable, the test shows that the power attenuation is only 3.71 percent when the electric heating film continuously works for 720 hours (30 days) under the rated voltage AC 220V, and the power attenuation is 15.13 percent when the electric heating film is not compounded with the graphene nano material. Compared with the actual measurement of the electrothermal film quartz glass heating tube manufactured by other manufacturers purchased from the market and the electrothermal film quartz glass heating tube manufactured by the other manufacturers without compounding the graphene nano material, the electrothermal film quartz glass heating tube has the unusual effect no matter the heating rate or the power attenuation resistance.
Drawings
FIG. 1 is a graph showing a temperature increase rate comparison between example 1 of the present invention and a comparative example;
fig. 2 is a graph comparing the power attenuation change of the inventive example 2 and the comparative example.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The production method of the electrothermal film by taking the quartz glass tube as the film applying substrate comprises the following steps: step one, adding 40g of zinc acetate dihydrate into 700ml of diethylene glycol, uniformly mixing, refluxing the solution at the temperature of 150 ℃ and 160 ℃ for 1-1.5 hours, centrifugally cleaning and collecting the product after the reaction is finished, and drying at the temperature of 78-80 ℃ for 10-12 hours to obtain ZnO nano powder;
step two, adding 40g of ZnO nano powder into 800ml of graphene oxide ethanol solution to obtain a mixed solution, carrying out ultrasonic dispersion on the mixed solution for 1-1.5 hours to obtain a gray ZnO-GO suspension, uniformly mixing, carrying out freeze drying to obtain powder, and carrying out thermal reduction at 550-650 ℃ to obtain a ZnO-Go nanocomposite;
weighing 15g of ZnO-Go nanocomposite, adding the ZnO-Go nanocomposite into 100ml of ethylene glycol monomethyl ether, uniformly stirring, weighing 0.65g of aluminum trichloride hexahydrate, weighing 0.2g of copper acetate monohydrate, and adding 0.15g of manganese acetate tetrahydrate into the solution, and continuously stirring; measuring 350ml of ethanol, slowly adding the solution into the solution, stirring the solution for 2 hours by using a magnetic stirring instrument to obtain a transparent and stable solution, and aging the solution for 24 hours to obtain a coating solution;
step four, taking a quartz glass tube as a film applying substrate, cleaning and drying the quartz glass tube by ethanol, putting the cleaned and dried quartz glass tube into a muffle furnace, heating the cleaned and dried quartz glass tube to 350 ℃, and adding N into the muffle furnace2The gas and the coating liquid are sprayed out from the gas nozzle and the liquid nozzle through the delivery pipe by utilizing the air pressure, the gas nozzle and the liquid nozzle mutually form an angle of 90 degrees, the liquid sprayed out from the liquid nozzle is atomized, the atomized liquid is pushed to enter the spraying electric furnace, the atomized liquid is combined with the surface of the quartz glass tube at high temperature, and an AZO electric heating film is formed on the surface of the tube; silver paste is coated at appropriate positions of two ends of the quartz tube electrothermal film according to requirements, the quartz tube electrothermal film is dried in an electric furnace at 150 ℃, and then the quartz tube electrothermal film is conveyed into a reducing furnace at 500 ℃ for reduction for 20 minutes, so that the electrode is qualified in a uniform and compact silvery white state.
Example 2
The production method of the electrothermal film by taking the quartz glass tube as the film applying substrate comprises the following steps: step one, adding 100g of zinc acetate dihydrate into 900ml of diglycol, uniformly mixing, refluxing the solution at 160 ℃ for 1.5 hours, centrifugally cleaning and collecting the product after the reaction is finished, and drying at 80 ℃ for 12 hours to obtain ZnO nano powder;
and step two, adding 100g of ZnO nano powder into 1000ml of graphene oxide ethanol solution, and ultrasonically dispersing the solution for 1 hour to obtain a gray ZnO-GO suspension. After being uniformly mixed, the mixture is frozen and dried to obtain powder, and then the powder is thermally reduced at 600 ℃ to obtain the ZnO-Go nano composite material.
Step three, weighing 50g of ZnO-Go nano composite material, adding the ZnO-Go nano composite material into 300ml of ethylene glycol monomethyl ether, uniformly stirring, weighing 2.15g of aluminum trichloride hexahydrate, weighing 0.65g of copper acetate monohydrate, and adding 0.45g of manganese acetate tetrahydrate into the solution, and continuously stirring; measuring 700ml of ethanol, slowly adding the solution into the solution, stirring the solution for 2 hours by using a magnetic stirring instrument to obtain a transparent and stable solution, and aging the solution for 24 hours to obtain a coating solution;
step four, taking a quartz glass tube as a film applying substrate, cleaning and drying the quartz glass tube by ethanol, putting the cleaned and dried quartz glass tube into a muffle furnace, heating the cleaned and dried quartz glass tube to 400 ℃, and adding N into the muffle furnace2Gas and coating liquid are sprayed out from an air nozzle and a liquid nozzle through a conveying pipe by utilizing air pressure, the air nozzle and the liquid nozzle form 90 degrees with each other, the liquid sprayed out from the liquid nozzle is atomized, the atomized liquid is pushed to enter a spraying electric furnace, the atomized liquid is combined with the surface of a quartz glass tube at high temperature, an AZO electric heating film is formed on the surface of the tube, silver paste is coated at proper positions at two ends of the quartz electric heating film according to needs, the electric furnace is dried at 200 ℃, and then the electric furnace is sent into a reducing furnace at 600 ℃ for reduction for 20 minutes, so that the electrode is qualified in a uniform and compact silvery white.
The heating rate of the electric heating film quartz glass heating tube made of the composite graphene nano material prepared in the embodiment 1 is compared with that of the electric heating film quartz glass heating tube made of the non-composite graphene nano material, and specific comparison data are shown in fig. 1. Fig. 1 shows that the temperature rise speed of the electric heating film quartz glass heating tube made of the composite graphene nano material prepared in embodiment 1 is high.
Actual measurement and comparison are carried out on the electric heating film quartz glass heating tube made of the composite graphene nano material prepared in the embodiment 2, the electric heating film quartz glass heating tube made of the composite graphene nano material which is not compounded with the electric heating film quartz glass heating tube made of other manufacturers purchased from the market, specific comparison data are shown in the figure 2 in detail, and the fact that the electric heating film quartz glass heating tube made of the composite graphene nano material prepared in the embodiment 2 is rapidly heated and the power is stable can be known from the figure 2.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. A production method for manufacturing an electrothermal film by using a graphene composite nano material is characterized by comprising the following steps: the specific method comprises the following steps:
step one, adding 40-60g of zinc acetate dihydrate into 700-900 ml of diethylene glycol, uniformly mixing, refluxing the solution at 150-160 ℃ for 1-1.5 hours, centrifugally cleaning and collecting the product after the reaction is finished, and drying at 78-80 ℃ for 10-12 hours to obtain ZnO nano powder;
step two, adding 40-60g of ZnO nano powder into 800-850ml of graphene oxide ethanol solution to obtain a mixed solution, carrying out ultrasonic dispersion on the mixed solution for 1-1.5 hours to obtain a gray ZnO-GO suspension, uniformly mixing, carrying out freeze drying to obtain powder, and carrying out thermal reduction at 550-650 ℃ to obtain the ZnO-Go nano composite material;
step three, taking ZnO-Go nano composite material and aluminum chloride as reactants, taking copper acetate monohydrate and manganese acetate tetrahydrate as doping agents, taking ethylene glycol monomethyl ether as a cosolvent and ethanol as a solvent, and dissolving and aging to obtain the coating liquid, wherein the specific method comprises the following steps: weighing 10-20g of ZnO-Go nanocomposite, adding the ZnO-Go nanocomposite into 100-200ml of ethylene glycol monomethyl ether, uniformly stirring, weighing 0.5-1.2g of aluminum trichloride hexahydrate, weighing 0.2-0.5g of copper acetate monohydrate, and adding 0.15-0.4g of manganese acetate tetrahydrate into the solution for continuous stirring; measuring 350ml of ethanol, slowly adding the solution into the solution, stirring the solution for 2 hours by using a magnetic stirring instrument to obtain a transparent and stable solution, and aging the solution for 24 hours to obtain a coating solution;
and step four, heating the substrate to be coated to 300-400 ℃, and thermally decomposing the coating liquid prepared in the step three on the surface of the substrate by spraying to form the AZO electrothermal film.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103816885A (en) * | 2014-02-20 | 2014-05-28 | 阜阳师范学院 | Preparation and application of nano zinc oxide photocatalyst |
| CN104219797A (en) * | 2014-09-10 | 2014-12-17 | 浙江碳谷上希材料科技有限公司 | Graphene electrothermal film |
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| CN108165956A (en) * | 2017-12-29 | 2018-06-15 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method for the AZO laminated films for adding graphene |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI10797U1 (en) * | 2014-12-04 | 2015-03-10 | Wicetec Oy | A conductor joint for connecting a copper conductor |
| KR20180106625A (en) * | 2017-03-21 | 2018-10-01 | 에스케이씨 주식회사 | Sheet type heating element and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103816885A (en) * | 2014-02-20 | 2014-05-28 | 阜阳师范学院 | Preparation and application of nano zinc oxide photocatalyst |
| CN104219797A (en) * | 2014-09-10 | 2014-12-17 | 浙江碳谷上希材料科技有限公司 | Graphene electrothermal film |
| CN104232108A (en) * | 2014-09-10 | 2014-12-24 | 浙江碳谷上希材料科技有限公司 | Preparation method of pure inorganic composite membrane based on graphene |
| CN105813241A (en) * | 2016-05-09 | 2016-07-27 | 苏州思创源博电子科技有限公司 | Preparation method of infrared electrothermal film |
| CN108165956A (en) * | 2017-12-29 | 2018-06-15 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method for the AZO laminated films for adding graphene |
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