CN105916220A - Composite electric heating film preparation method - Google Patents

Composite electric heating film preparation method Download PDF

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Publication number
CN105916220A
CN105916220A CN201610304033.4A CN201610304033A CN105916220A CN 105916220 A CN105916220 A CN 105916220A CN 201610304033 A CN201610304033 A CN 201610304033A CN 105916220 A CN105916220 A CN 105916220A
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China
Prior art keywords
heating film
electric heating
solution
mixed
electric
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Pending
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CN201610304033.4A
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Chinese (zh)
Inventor
刘娜
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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Priority to CN201610304033.4A priority Critical patent/CN105916220A/en
Publication of CN105916220A publication Critical patent/CN105916220A/en
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/10Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12Heating 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
    • H05B3/14Heating 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
    • H05B3/145Carbon only, e.g. carbon black, graphite
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/84Heating arrangements specially adapted for transparent or reflecting areas, e.g. for demisting or de-icing windows, mirrors or vehicle windshields
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/013Heaters using resistive films or coatings
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/031Heaters specially adapted for heating the windscreen wiper area

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  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a composite electric heating film preparation method, comprising a substrate, a first electric heating film and a second electric heating film. The composite electric heating film combines the advantages of a graphene electric heating film and a semiconductor electric heating film, and a grapheme far infrared electric heating portion can be activated by tiny current, thereby saving energy by 60% compared with a traditional electric heating mode, and improving an electric energy utilization rate; the semiconductor electric heating film employing the materials and compounding ratio has the characteristics of small heat transfer resistance, chemical stability, heat stability and electro-thermal conversion efficiency, wherein the electric heating film resistance possesses positive temperature characteristics, and can automatically adjust current size and self current-limitation characteristics according to film thickness nonuniformity, thereby guaranteeing electric heating film heating uniformity.

Description

A kind of preparation method of composite electric heating film
Technical field
The present invention relates to household electrical appliances and manufacture field, be specifically related to the preparation method of a kind of composite electric heating film.
Background technology
It is little that traditional method using resistance wire to carry out heating service also exists electrical heating area, and electrical heating efficiency is low, and resistance wire uses easily oxidation, the shortcoming that the life-span is short for a long time.Therefore, increasing electric heating film initially enters the visual field of people.
Semiconductor conducting film has been widely used in the glass defrosting of the equipment such as automobile, aircraft, refrigerator.But mainly use the mode of magnetron sputtering and spray pyrolysis to prepare.But the equipment used in this preparation process is much more expensive, additionally, due to the shape of household electrical appliance is the most extremely complex, the mode of magnetron sputtering and spray pyrolysis is used to be difficult to be compound on electrical heating utensil semiconductor conducting film
Inorganic SnO2The hardness of electric heating film own is high, is combined jail with carrier, has stable high-temperature performance, can work under the higher temperature of 500 DEG C, there are good non-oxidizability, a chemical attack ability, and a preferably resistance stability, and there is the key properties such as energy-conservation, light and handy, long-lived, the flames of anger, starting current are little.Its very thin thickness, typically in terms of micron (one thousandth of a millimeter), unique distinction is the transparency, it is seen that light transmission rate is up to more than 90%.
Graphene (Graphene) was caused the extensive concern of scientist by the report such as the professor Geim of Univ Manchester UK with its peculiar performance from 2004 and great interest is predicted probably causes revolutionary variation in a lot of fields.Single-layer graphene with two dimensional crystal structure exist thickness 0.1334nm it be construct other dimension carbonaceous material elementary cell it can wrap up and form the fullerene of zero dimension and roll and form one-dimensional carbon nanotube layer layer stack and amass and form three-dimensional graphite.Graphene is that a kind of semiconductor not having energy gap has the carrier mobility (2 × 10cm/v) of high 100 times than silicon and at room temperature has a micron order free path and big coherence length therefore Graphene is the ideal material of nanometric circuit.Graphene has good thermal conductivity [3000W/ (m K)], high intensity (110GPa) and the specific surface area (2630m/g) of super large.The performance of these excellences makes Graphene have the application prospect of light in fields such as nano electron device, gas sensor, energy storage and composites.
Summary of the invention
The present invention provides the preparation method of a kind of composite electric heating film, composite electric heating film prepared by the method, has the electrical heating conversion performance of excellence and longer service life.
To achieve these goals, it is achieved above-mentioned purpose, the invention provides the preparation method of a kind of composite electric heating film, this composite electric heating film includes substrate, the first electric heating film and the second electric heating film;
The method comprises the steps:
(1) the first electric heating film layer slurry is prepared
Weigh the graphene powder of 6-7 weight portion, the far infrared transmission agent of 0.5-2 weight portion, the bonding diluent of 3-5 weight portion, stir after first graphene powder being mixed with far infrared transmission agent, after being subsequently adding bonding diluent mixing, form slurry;Described bonding diluent is resistant to elevated temperatures phenolic resin, and the particle diameter of graphene powder is: 30-60nm;
(2) the first electric heating film is formed
Slurry being coated uniformly on substrate surface and forms film, form the first electric heating film after drying or drying, wherein the THICKNESS CONTROL of the first electric heating film is in 5-15 μm;
(3) the second electric heating film powder is prepared
Stannous chloride solution is mixed in alcohol solvent, to obtain the first organic solution;Trichloride antimony solution and manganese dioxide solution are mixed in alcohol solvent, to obtain the second organic solution;Described second organic solution is slowly mixed together in described first organic solution, to obtain described Electric radiant Heating Film solution;
Wherein, stannous chloride solution is mixed in alcohol solvent, trichloride antimony solution and manganese dioxide solution are mixed in alcohol solvent, when second organic solution is mixed in the first organic solution, it is respectively necessary in constant temperature blender with magnetic force stirring 2-4 hour, so that stannous chloride solution, trichloride antimony solution and manganese dioxide solution can be sufficiently mixed in alcohol solvent, the temperature of constant temperature blender with magnetic force is 80 degrees Celsius;
The concentration range of described stannous chloride solution is 0.3-0.8 mol/L, and the concentration range of described trichloride antimony solution is 0.05-0.2 mol/L, and the concentration range of described manganese dioxide solution is 0.01-0.03 mol/L.
Calcining described Electric radiant Heating Film solution, use Muffle furnace equipment to calcine described Electric radiant Heating Film solution, wherein, the temperature range of calcination process is 600-800 degree Celsius, and calcination time is 40-60 minute, obtains the second electric heating film powder;
(4) the second electric heating film is formed
Using described Electric radiant Heating Film powder to be deposited with on described first electric heating film, the vacuum of evaporation is 1.0 × 10-3Handkerchief, vaporization voltage is 5 volts, and evaporation time is 60 seconds, and wherein the THICKNESS CONTROL of the second electric heating film is in 5-10 μm.
Composite electric heating film prepared by the present invention combines Graphene electric heating film and the advantage of semi-conductor electricity heating film, small electric current just can activate Graphene infrared ray heating part, than traditional Electric heating saving energy 60%, improve the utilization rate of electric energy, the semi-conductor electricity heating film heat transfer resistance using above-mentioned material and proportioning is little, chemical stability and heat endurance, electric-thermal conversion efficiency is high, wherein, the resistance of this electric heating film has positive temperature characterisitic, can be according to the uneven size being automatically adjusted electric current of thickness and the characteristic of self-limiting, thus ensure that the uniformity that electric heating film heats.
Detailed description of the invention
Embodiment one
Weigh the graphene powder of 6 weight portions, the far infrared transmission agent of 0.5 weight portion, the bonding diluent of 3 weight portions, stir after first graphene powder being mixed with far infrared transmission agent, after being subsequently adding bonding diluent mixing, form slurry;Described bonding diluent is resistant to elevated temperatures phenolic resin, and the particle diameter of graphene powder is: 30-60nm.
Slurry being coated uniformly on substrate surface and forms film, form the first electric heating film after drying or drying, wherein the THICKNESS CONTROL of the first electric heating film is in 5 μm.
Described stannous chloride solution is mixed in alcohol solvent, to obtain the first organic solution;Described trichloride antimony solution and described manganese dioxide solution are mixed in alcohol solvent, to obtain the second organic solution;Described second organic solution is slowly mixed together in described first organic solution, to obtain described Electric radiant Heating Film solution;
Wherein, stannous chloride solution is mixed in alcohol solvent, trichloride antimony solution and manganese dioxide solution are mixed in alcohol solvent, when second organic solution is mixed in the first organic solution, it is respectively necessary in constant temperature blender with magnetic force stirring 2 hours, so that stannous chloride solution, trichloride antimony solution and manganese dioxide solution can be sufficiently mixed in alcohol solvent, the temperature of constant temperature blender with magnetic force is 80 degrees Celsius.
The concentration range of described stannous chloride solution is 0.3 mol/L, and the concentration range of described trichloride antimony solution is 0.05 mol/L, and the concentration range of described manganese dioxide solution is 0.01 mol/L.
Calcining described Electric radiant Heating Film solution, use Muffle furnace equipment to calcine described Electric radiant Heating Film solution, wherein, the temperature range of calcination process is 600 degrees Celsius, and calcination time is 40 minutes, obtains the second electric heating film powder.
Using described Electric radiant Heating Film powder to be deposited with on described first electric heating film, the vacuum of evaporation is 1.0 × 10-3Handkerchief, vaporization voltage is 5 volts, and evaporation time is 60 seconds, and wherein the THICKNESS CONTROL of the second electric heating film is in 5 μm.
Embodiment two
Weigh the graphene powder of 7 weight portions, the far infrared transmission agent of 2 weight portions, the bonding diluent of 5 weight portions, stir after first graphene powder being mixed with far infrared transmission agent, after being subsequently adding bonding diluent mixing, form slurry;Described bonding diluent is resistant to elevated temperatures phenolic resin, and the particle diameter of graphene powder is: 30-60nm.
Slurry being coated uniformly on substrate surface and forms film, form the first electric heating film after drying or drying, wherein the THICKNESS CONTROL of the first electric heating film is in 15 μm.
Described stannous chloride solution is mixed in alcohol solvent, to obtain the first organic solution;Described trichloride antimony solution and described manganese dioxide solution are mixed in alcohol solvent, to obtain the second organic solution;Described second organic solution is slowly mixed together in described first organic solution, to obtain described Electric radiant Heating Film solution;
Wherein, stannous chloride solution is mixed in alcohol solvent, trichloride antimony solution and manganese dioxide solution are mixed in alcohol solvent, when second organic solution is mixed in the first organic solution, it is respectively necessary in constant temperature blender with magnetic force stirring 4 hours, so that stannous chloride solution, trichloride antimony solution and manganese dioxide solution can be sufficiently mixed in alcohol solvent, the temperature of constant temperature blender with magnetic force is 80 degrees Celsius.
The concentration range of described stannous chloride solution is 0.8 mol/L, and the concentration range of described trichloride antimony solution is 0.2 mol/L, and the concentration range of described manganese dioxide solution is 0.03 mol/L.
Calcining described Electric radiant Heating Film solution, use Muffle furnace equipment to calcine described Electric radiant Heating Film solution, wherein, the temperature range of calcination process is 800 degrees Celsius, and calcination time is 60 minutes, obtains the second electric heating film powder.
Using described Electric radiant Heating Film powder to be deposited with on described first electric heating film, the vacuum of evaporation is 1.0 × 10-3Handkerchief, vaporization voltage is 5 volts, and evaporation time is 60 seconds, and wherein the THICKNESS CONTROL of the second electric heating film is in 10 μm.
Testing embodiment 1-2, test result shows: the electrical heating conversion efficiency of embodiment 1-2 is up to more than 90%.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.

Claims (1)

1. a preparation method for composite electric heating film, this composite electric heating film includes substrate, the first electric heating film and the second electric heating film;
The method comprises the steps:
(1) the first electric heating film layer slurry is prepared
Weigh the graphene powder of 6-7 weight portion, the far infrared transmission agent of 0.5-2 weight portion, the bonding diluent of 3-5 weight portion, stir after first graphene powder being mixed with far infrared transmission agent, after being subsequently adding bonding diluent mixing, form slurry;Described bonding diluent is resistant to elevated temperatures phenolic resin, and the particle diameter of graphene powder is: 30-60nm;
(2) the first electric heating film is formed
Slurry being coated uniformly on substrate surface and forms film, form the first electric heating film after drying or drying, wherein the THICKNESS CONTROL of the first electric heating film is in 5-15 μm;
(3) the second electric heating film powder is prepared
Stannous chloride solution is mixed in alcohol solvent, to obtain the first organic solution;Trichloride antimony solution and manganese dioxide solution are mixed in alcohol solvent, to obtain the second organic solution;Described second organic solution is slowly mixed together in described first organic solution, to obtain described Electric radiant Heating Film solution;
Wherein, stannous chloride solution is mixed in alcohol solvent, trichloride antimony solution and manganese dioxide solution are mixed in alcohol solvent, when second organic solution is mixed in the first organic solution, it is respectively necessary in constant temperature blender with magnetic force stirring 2-4 hour, so that stannous chloride solution, trichloride antimony solution and manganese dioxide solution can be sufficiently mixed in alcohol solvent, the temperature of constant temperature blender with magnetic force is 80 degrees Celsius;
The concentration range of described stannous chloride solution is 0.3-0.8 mol/L, and the concentration range of described trichloride antimony solution is 0.05-0.2 mol/L, and the concentration range of described manganese dioxide solution is 0.01-0.03 mol/L;
Calcining described Electric radiant Heating Film solution, use Muffle furnace equipment to calcine described Electric radiant Heating Film solution, wherein, the temperature range of calcination process is 600-800 degree Celsius, and calcination time is 40-60 minute, obtains the second electric heating film powder;
(4) the second electric heating film is formed
Using described Electric radiant Heating Film powder to be deposited with on described first electric heating film, the vacuum of evaporation is 1.0 × 10-3Handkerchief, vaporization voltage is 5 volts, and evaporation time is 60 seconds, and wherein the THICKNESS CONTROL of the second electric heating film is in 5-10 μm.
CN201610304033.4A 2016-05-09 2016-05-09 Composite electric heating film preparation method Pending CN105916220A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107682944A (en) * 2017-10-24 2018-02-09 张东升 A kind of semiconductor thermoelectric film and preparation method thereof
CN108615585A (en) * 2018-05-15 2018-10-02 盐城工学院 A kind of preparation method of doped stannum oxide composite conductive thin film
CN111556598A (en) * 2020-05-27 2020-08-18 佛山(华南)新材料研究院 Flexible low-voltage infrared electrothermal film and preparation method thereof
CN111996499A (en) * 2020-08-31 2020-11-27 中能华邦环保科技有限公司 Evaporation plating equipment for inner and outer membranes of nano tube meteorological furnace

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1082803A (en) * 1992-07-09 1994-02-23 连铁军 A kind of thermostable transparent electric heating film and production method thereof
CN102036433A (en) * 2010-12-21 2011-04-27 吕一诺 Infrared electric heating film heating tube with double-film layer structure as well as preparation method and application thereof
CN103338538A (en) * 2013-07-19 2013-10-02 南京中脉科技控股有限公司 Graphene radiation heating film and preparation method and application thereof
CN104080208A (en) * 2013-03-26 2014-10-01 颜彬 Manufacturing method of electrothermal film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1082803A (en) * 1992-07-09 1994-02-23 连铁军 A kind of thermostable transparent electric heating film and production method thereof
CN102036433A (en) * 2010-12-21 2011-04-27 吕一诺 Infrared electric heating film heating tube with double-film layer structure as well as preparation method and application thereof
CN104080208A (en) * 2013-03-26 2014-10-01 颜彬 Manufacturing method of electrothermal film
CN103338538A (en) * 2013-07-19 2013-10-02 南京中脉科技控股有限公司 Graphene radiation heating film and preparation method and application thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107682944A (en) * 2017-10-24 2018-02-09 张东升 A kind of semiconductor thermoelectric film and preparation method thereof
CN108615585A (en) * 2018-05-15 2018-10-02 盐城工学院 A kind of preparation method of doped stannum oxide composite conductive thin film
CN111556598A (en) * 2020-05-27 2020-08-18 佛山(华南)新材料研究院 Flexible low-voltage infrared electrothermal film and preparation method thereof
CN111556598B (en) * 2020-05-27 2022-05-27 佛山(华南)新材料研究院 Flexible low-voltage infrared electrothermal film and preparation method thereof
CN111996499A (en) * 2020-08-31 2020-11-27 中能华邦环保科技有限公司 Evaporation plating equipment for inner and outer membranes of nano tube meteorological furnace

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Application publication date: 20160831