CN114258167A - Preparation method of carbon nanotube/glass fiber cloth flexible film heater - Google Patents
Preparation method of carbon nanotube/glass fiber cloth flexible film heater Download PDFInfo
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- CN114258167A CN114258167A CN202011011868.3A CN202011011868A CN114258167A CN 114258167 A CN114258167 A CN 114258167A CN 202011011868 A CN202011011868 A CN 202011011868A CN 114258167 A CN114258167 A CN 114258167A
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- fiber cloth
- carbon nanotube
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- 239000004744 fabric Substances 0.000 title claims abstract description 37
- 239000003365 glass fiber Substances 0.000 title claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 35
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 238000000576 coating method Methods 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002109 single walled nanotube Substances 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000010410 layer Substances 0.000 claims description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 239000011247 coating layer Substances 0.000 claims description 4
- 239000011889 copper foil Substances 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 239000011152 fibreglass Substances 0.000 claims 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 230000002265 prevention Effects 0.000 abstract description 3
- 238000003466 welding Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 42
- 230000001276 controlling effect Effects 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 238000007611 bar coating method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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
- H05B3/20—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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D21/00—Measuring or testing not otherwise provided for
- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
-
- 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
-
- 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 preparation method of a carbon nano tube/glass fiber cloth flexible film heater, which mainly comprises the steps of coating a single-wall carbon nano tube dispersion liquid on a glass fiber cloth substrate layer by adopting a Meyer rod coating method, and welding carbon nano tubes through annealing post-treatment to reduce the surface resistance of a film and increase the electrical stability of the film. The method is characterized in that: (1) the composite film heater with stable structure, high heating rate and super-flexibility is prepared by adopting glass fiber cloth with high flexibility, high heat resistance and high mechanical strength as a substrate and single-walled carbon nanotubes with high electric conductivity and heat conductivity as a raw material; (2) the film heater has simple preparation process and short period, and can heat a film with the surface resistance of 20 omega/sq to 170 ℃ only within 25s under the voltage of 30V; (3) the flexible film heater can be widely applied to various industrial and living fields such as mold heating, wind power blade ice prevention and removal, daily heating pads and the like on a large scale, and has extremely high commercial popularization value.
Description
Technical Field
The invention belongs to the technical field of flexible film heater preparation, and particularly relates to a solution method preparation and coating process of a carbon nanotube material.
Background
The flexible film heater is a film-shaped device which can be bent to a certain degree, can be folded and can generate heat after being electrified. The film heater is a typical planar heater, and has extremely high heat exchange power due to large heat exchange area. The heat dissipation device has the advantages of high heating efficiency, good heat dissipation, high surface power density, difficult ablation and the like. In recent years, flexible film heaters are widely applied to the fields of buildings, industry, agriculture, military, household products and the like to solve the problems of heating, deicing, freezing prevention or heating, and particularly in the field of industrial production, the demand for the flexible film heaters is more prominent. For example, in a workshop or a field construction area, a plurality of valves or molds need to be heated or preheated to meet the requirements of deicing, freezing prevention and the like, but because the valve or the mold is irregular in shape, the heating is very inconvenient by using a resistance wire. Most inorganic thin film heaters are rigid and therefore unsuitable for heating in such applications. For the carbon nanotube/glass fiber cloth composite film heater, the conductive carbon nanotube is coated on the insulating and highly flexible glass fiber substrate by a simple bar coating method, various complex film heating devices can be manufactured, the heater can be bent, folded and wrapped freely according to the shape of a die, the heating speed is high, the power consumption is low, and the heating requirements of parts such as a valve die and the like can be met smoothly. In addition, the carbon nanotube/glass fiber cloth composite film heater belongs to electroheating, and no open fire is generated in heating, so that the carbon nanotube/glass fiber cloth composite film heater is very safe and reliable to use in places needing heating, such as coal mines, chemical plants, oil depots and the like. In the field of daily life, the carbon nanotube/glass fiber cloth composite film heater can be completely suitable for heating equipment with high requirements on flexibility, such as a portable heating mat, a thermal therapy blanket and the like, and has the advantages of small volume, folding and carrying, and low driving voltage, so that the film heater has extremely high application value.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon nanotube/glass fiber cloth flexible film heater, and the prepared composite film heater has a stable structure, a high heating rate and high flexibility, and has great application potential in industrial production, household and daily use and the like.
The technical scheme of the invention is as follows: the main steps are that firstly, the glass fiber cloth substrate is washed clean by water, and the required size is cut. And coating the prepared single-walled carbon nanotube dispersion liquid on a glass fiber cloth substrate layer by adopting a Meyer rod coating method, and coating the next layer after each layer is completely dried. The number of coating layers is controlled according to the sheet resistance of the film. Then, the carbon nano tube/glass fiber cloth film is placed on a heating plate, heated to 200 ℃ for annealing, and repeated twice, so that the carbon nano tube nodes are welded, and the surface resistance of the film is reduced. The annealed film has excellent conductivity and high mechanical strength. And then, sticking a layer of copper foil electrode with the width of about 1cm on any two opposite sides, connecting the two copper electrodes of the film with a voltage-regulating power supply through a lead, and controlling the heating temperature of the surface of the film by controlling the voltage of the voltage-regulating power supply. For the film with the surface resistance of 20 omega/sq, the temperature can be raised to 170 ℃ only within 25s under the voltage of 30V.
The main innovation points of the invention are as follows: the carbon nano tube with high conductivity and high elasticity is compounded with the glass fiber cloth with high flexibility and high mechanical strength by a Meyer rod coating method, so that the novel ultra-flexible film heater is constructed.
The method for preparing the carbon nano tube dispersion liquid in the method of the invention comprises the following steps: the single-walled carbon nanotube with the purity of more than 95 wt%, the outer diameter of 1-2 nm and the length of 5-30 mu m is used as a raw material, sodium dodecyl benzene sulfonate is used as a dispersing agent, and distilled water is used as a solvent. Weighing the single-walled carbon nanotube and sodium dodecyl benzene sulfonate in a ratio of 10: 1, adding distilled water in a corresponding ratio to enable the concentration of the carbon nanotube to be 1-2mg/ml, carrying out ultrasonic treatment for 50min by using an ultrasonic dispersion machine, centrifuging for 20min at a speed of 8000r/min by using a centrifugal machine, and extracting supernatant to obtain carbon nanotube dispersion liquid.
Reagents and materials used in the invention: single-walled carbon nanotubes, glass fiber cloth, sodium dodecyl benzene sulfonate, 3M copper tape, distilled water and the like.
In the invention, a Scanning Electron Microscope (SEM) is adopted to represent the appearance of the prepared carbon nano tube/glass fiber cloth film. And adopting a Gicherie 2700 four-probe resistance measuring instrument to represent the surface resistance of the prepared carbon nano tube/glass fiber cloth film. A T-type thermocouple was used to characterize the temperature at which the film was heated.
Drawings
FIG. 1 is a flow chart of a process for manufacturing a carbon nanotube/glass fiber cloth film heater.
FIG. 2 is a schematic diagram of a carbon nanotube/glass fiber cloth film heater.
FIG. 3 is a SEM low-magnification view of a carbon nanotube/glass fiber cloth film.
FIG. 4 is a high magnification SEM image of a carbon nanotube/glass fiber cloth film.
FIG. 5 is a temperature rise curve of 20 Ω/sq carbon nanotube/glass fiber cloth film under different voltages.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1:
taking 20mg of single-walled carbon nanotube and 200mg of sodium dodecyl benzene sulfonate into a beaker, adding 20mL of distilled water, performing ultrasonic treatment for 50min by using an ultrasonic dispersion machine, centrifuging for 20min at 8000r/min by using a centrifugal machine, and extracting supernatant to obtain the carbon nanotube dispersion liquid with the concentration of 1 mg/mL. A10 cm by 10cm clean glass fiber cloth was then stuck on a hot plate, set at a temperature of 105 ℃. The carbon nanotube dispersion was then layered on a glass fiber cloth substrate using a mayer rod. Before coating each layer, the upper layer is completely dried, and after 5 layers of coating, the surface resistance of the carbon nano tube/glass fiber cloth composite film is about 100 omega/sq. Subsequently, the heating plate on which the composite film was placed was heated to 200 ℃, and after 5 minutes of heat preservation, the plate was annealed to room temperature, and repeated 2 times. The sheet resistance of the film is reduced to 65 omega/sq. A layer of copper foil electrode with the width of about 1cm is pasted on any two opposite sides of the composite film, the two copper electrodes of the film are connected with a voltage-stabilized power supply through a lead, and the heating temperature of the surface of the film is controlled by controlling the voltage of the voltage-regulated power supply. The maximum steady state temperature was 152 ℃ when the voltage was 60V.
Example 2:
taking 40mg of single-walled carbon nanotube and 400mg of sodium dodecyl benzene sulfonate in a beaker, adding 20mL of distilled water, performing ultrasonic treatment for 50min by using an ultrasonic dispersion machine, centrifuging for 20min at 8000r/min by using a centrifugal machine, and extracting supernatant to obtain carbon nanotube suspension with the concentration of 2 mg/mL. A10 cm by 10cm clean glass fiber cloth was then stuck on a hot plate, set at a temperature of 105 ℃. And then, the carbon nanotube suspension is coated on the glass fiber cloth substrate layer by using a Meyer rod. And (3) completely drying the previous layer before coating each layer, and after 7 layers of coating, controlling the surface resistance of the carbon nano tube/glass fiber cloth composite film to be about 20 omega/sq. Subsequently, the heating plate on which the composite film was placed was heated to 200 ℃, and after 5 minutes of heat preservation, the plate was annealed to room temperature, and repeated 2 times. The sheet resistance of the film is reduced to about 8 omega/sq. A layer of copper foil electrode with the width of about 1cm is pasted on any two opposite sides of the composite film, the two copper electrodes of the film are connected with a regulated power supply through a lead, and the heating temperature of the surface of the film is controlled by controlling the voltage of the regulated power supply. The maximum steady state temperature was 214 ℃ when the voltage was 30V.
Claims (10)
1. The invention discloses a preparation method of a carbon nano tube/glass fiber cloth flexible film heater, which mainly comprises the steps of washing a glass fiber cloth substrate with water, and cutting to a required size. And coating the prepared single-walled carbon nanotube dispersion liquid on a glass fiber cloth substrate layer by adopting a Meyer rod coating method, and coating the next layer after each layer is completely dried. The number of coating layers is controlled according to the sheet resistance of the film. Then, the carbon nano tube/glass fiber cloth film is placed on a heating plate, heated to 200 ℃ for annealing, and repeated twice, so that the carbon nano tube nodes are welded, and the surface resistance of the film is reduced. The annealed film has excellent conductivity and high mechanical strength. And then, sticking a layer of copper foil electrode with the width of about 1cm on any two opposite sides, connecting the two copper electrodes of the film with a voltage-regulating power supply through a lead, and controlling the heating temperature of the surface of the film by controlling the voltage of the voltage-regulating power supply.
2. The method according to claim 1, wherein the raw material used is single-walled carbon nanotubes with a purity of > 95 wt%, an outer diameter of 1-2 nm and a length of 5-30 μm.
3. The glass fiber cloth can adopt alkali-free cloth, medium alkali cloth, glass fiber mesh cloth and the like.
4. The method according to claim 1, wherein the conditions for preparing the carbon nanotube dispersion liquid by using the ultrasonic disperser are as follows: the power is 150 and 250W, and the time is 5-80 min. The dispersant can be selected from sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, sodium dodecyl sulfate, and cetyl trimethyl ammonium bromide.
5. The method of claim 1, wherein the carbon nanotube dispersion is prepared at a concentration of 1-2.0 mg/ml.
6. The method of claim 1, wherein the coating is performed by a meyer rod coating method, wherein the meyer rod specification can use RDS 10-24.
7. The method of claim 1, wherein the prepared single-walled carbon nanotube dispersion is coated on the glass fiber cloth substrate layer by using a meyer rod coating method, and after each layer is completely dried, the next layer is coated, wherein the number of the coating layers is 1-10.
8. The method according to claim 1, wherein the number of coating layers is controlled according to the sheet resistance of the film, and the sheet resistance of the film is 1 to 100 Ω/sq.
9. The method according to claim 1, wherein the annealing process comprises heating the glass fiber composite film to 200 ℃ by using a heating plate, preserving the heat for 5min, and naturally cooling to room temperature.
10. The method of claim 1, wherein the fiberglass composite film heater achieves the steady state temperature by controlling internal joule heating. For the same size film, this temperature depends on the sheet resistance of the composite film and the voltage input.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011011868.3A CN114258167A (en) | 2020-09-23 | 2020-09-23 | Preparation method of carbon nanotube/glass fiber cloth flexible film heater |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011011868.3A CN114258167A (en) | 2020-09-23 | 2020-09-23 | Preparation method of carbon nanotube/glass fiber cloth flexible film heater |
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| CN114258167A true CN114258167A (en) | 2022-03-29 |
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| CN202011011868.3A Pending CN114258167A (en) | 2020-09-23 | 2020-09-23 | Preparation method of carbon nanotube/glass fiber cloth flexible film heater |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116497596A (en) * | 2023-03-15 | 2023-07-28 | 大连工业大学 | Single-walled carbon nanotube/flexible fabric composite electrothermal film and preparation method and application thereof |
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-
2020
- 2020-09-23 CN CN202011011868.3A patent/CN114258167A/en active Pending
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