CN109600869B - Electrothermal film with PTC effect and preparation method thereof - Google Patents
Electrothermal film with PTC effect and preparation method thereof Download PDFInfo
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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
- H05B3/00—Ohmic-resistance heating
- H05B3/02—Details
- H05B3/06—Heater elements structurally combined with coupling elements or holders
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
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Abstract
The invention provides an electrothermal film with PTC effect and a preparation method thereof, wherein the electrothermal film comprises conductive filler, supporting material and third component, the conductive filler is filled in the third component, and the thermal expansion coefficient of the third component is larger than that of the supporting material. According to the invention, through adjusting and combining the third component, the electrothermal films with PTC effects at different temperatures are designed in the electrothermal films of the same supporting material, so that the problem of thermal expansion of a body provided by a high polymer supporting material in the prior art can be effectively solved, the product development flow is shortened, and the development cost is reduced.
Description
Technical Field
The invention relates to the technical field of electric heating materials, in particular to an electric heating film with a PTC effect and a preparation method thereof.
Background
The PTC effect refers to a positive temperature coefficient effect, which means that when the temperature of a material increases to a certain temperature, the resistivity of the material increases rapidly, and the material changes from a conductor to a poor conductor or even an insulator. Because of this feature, materials with PTC effect are often used to design and prepare electric heating materials that require self-limiting temperature under the condition of electrical heating, and the electric heating materials can achieve the effect of self-limiting temperature due to the decrease in heating power caused by the increase in resistance after heating to a certain temperature.
The polymer-based electrothermal film is generally prepared by adding conductive particles such as carbon black, carbon fiber, graphene or metal into a polymer supporting material as conductive filler. The electrothermal film heats up after being electrified, and if a covering is locally arranged, the local heat is easily accumulated, so that the local temperature is overhigh. Since the heat resistance of the polymer material is generally poor, the heat accumulation can burn and damage the electrothermal film, and more serious phenomenon is that the fire accident occurs due to the combustion of the covering. Therefore, it is necessary to achieve temperature limitation of the polymer electrothermal film. In this regard, the method adopted at present mainly uses a temperature sensor to measure the temperature, and when a certain temperature is reached, the relay is powered off. The disadvantage of this method is that if the local position of the excessive temperature is just not the place where the temperature sensor is placed, or the temperature controller itself fails by accident, both of these conditions can lead to failure of the temperature monitoring and temperature runaway. Another type of method is to use an electrothermal film with PTC effect. If the temperature of a certain part of the electrothermal film is too high, the heating power of the part can be automatically reduced due to the PTC effect, so that the purpose of automatic adjustment is achieved.
In the technology, the PTC effect of the electrothermal film is realized by the dilution effect generated by the thermal expansion of the polymer matrix. The principle is as follows: in the conductive heating process, the volume expansion of the polymer support body of the electrothermal film is caused by the temperature rise, so that the conductive fillers which are originally contacted with each other are separated due to the expansion of the support body, thereby changing a conductive path into a non-conductive path, causing the heating power and the temperature of the electrothermal film to be reduced, and realizing the purpose of self temperature limitation.
The disadvantage of this type of technology is that the PTC effect is mainly dependent on the volumetric expansion of the support after heating, and the need for a polymeric support provides both the thermal expansion capability and the mechanical and dimensional stability capabilities of the system, which is difficult to achieve in practical use. The temperature of the electric heating material which shows the PTC effect depends on the thermal expansion degree of the supporting body, so that the temperature of the same supporting material with the PTC effect of the electric heating material is the same, and the requirements of the electric heating material on the lower limit temperature of different occasions cannot be met. If the temperature of the electrothermal film is required to be 50 ℃, the temperature of the electrothermal film is required to be 80 ℃ in some cases. In addition, when the temperature of the PTC effect is different, the PTC effect can be realized only by replacing the supporting material of the heating element, and the replacement of the supporting material can lead to the change of processing parameters and even processing equipment, so that the product has long development period and high development cost.
Disclosure of Invention
The invention aims to provide a high polymer electrothermal film with PTC effect based on conductive filler and a third component and a preparation method thereof. In the invention, carbon black can be used as conductive filler, and the thermal expansion coefficient of the third component is higher than that of the heating element supporting material, so that the volume expansion and the PTC effect realization capability of the electrothermal film are provided; and the heating element supporting material provides mechanical property and dimensional stability. According to the invention, through adjusting and combining the third component, the electrothermal films with PTC effects at different temperatures can be designed in the electrothermal films of the same supporting material, so that the problem of thermal expansion of a body provided by a polymer supporting material in the prior art can be effectively solved, the product development flow is shortened, and the development cost is reduced.
The technical problems to be solved by the invention are realized by adopting the following technical scheme:
an electrothermal film with PTC effect comprises conductive filler, supporting material and third component, wherein the conductive filler is filled in the third component, and the thermal expansion coefficient of the third component is larger than that of the supporting material.
Optionally, the conductive filler is carbon black, and the supporting material is polyurethane.
Optionally, the third component is a water-insoluble organic molecule, a high molecular polymer, or a combination thereof, and the third component has a melting point higher than the self-limiting temperature that the electrothermal film needs to achieve.
Optionally, the melting point of the third component is 10-25 ℃ higher than the self-limiting temperature to be achieved by the electrothermal film.
Optionally, the third component is microcrystalline wax, EVA resin or PMMA.
Optionally, the weight ratio of the carbon black to the third component is 50-80:20-50.
Optionally, the weight ratio of the carbon black to the third component is 60-70:30-40.
The invention also provides application of the novel electrothermal film with the PTC effect in occasions needing self-temperature limitation, such as electrothermal floor heating.
The invention also provides a preparation method of the electrothermal film with the PTC effect, which comprises the following steps:
preparing third component particles containing conductive filler: mixing the conductive filler and the third component in a weight ratio of 40-90:30-60, adding into a screw extruder for melt extrusion, cooling, granulating and crushing to obtain third component particles containing the conductive filler;
preparing conductive carbon paste: adding 30-60% of third component particles containing conductive filler into a supporting material emulsion with solid content of 50-70% by weight, and stirring at room temperature to be uniform, thus obtaining conductive carbon slurry;
preparing an electrothermal film: and coating the conductive carbon paste on a substrate to obtain the electrothermal film with the PTC effect.
Optionally, the mesh number of the third component particles is 100-400 mesh.
The beneficial effects of the invention are as follows: compared with the prior art, the invention has the remarkable improvement that:
1. in the prior art, the realization of the PTC effect of the electrothermal film completely depends on the thermal expansion effect of the polymer support, and once the temperature of the PTC effect required by the product changes, the support material has to be replaced, so that the development period is prolonged and the development cost is increased. According to the technical scheme, the PTC effect temperature required by the product depends on the third component, and the support body can be made of polyurethane polymer materials with good mechanical properties and good heat resistance. Because the temperature of the electrothermal film is not higher than the melting point of the third component all the time, even though the electrothermal film is heated for many times, the third component still exists in the supporting material in the form of particles or flattened particles, and the polyurethane supporting material and the third component do not form homogeneous materials in the electrothermal film. The electrothermal film prepared by the technology is a heterogeneous electrothermal film (shown in the attached figure 1), wherein one phase is a third component with large thermal expansion coefficient, the third component generates large volume expansion when heated, carbon black is mainly distributed in the third component, and the PTC effect is realized by the dilution effect generated by the volume expansion of the third component; the other phase is polyurethane, which only plays a supporting role. Thus, the support component and the component providing the PTC effect can be separated, and when the temperature of the PTC effect required by the product changes, the support material of the heating element is not required to be replaced, and only the third component is required to be replaced.
2. The temperature for realizing the PTC effect cannot be controlled in the prior art, and the PTC effect with different temperatures can be realized by the invention. Since the volume of the organic material expands sharply around the melting point, the third component with a different melting point can be selected according to the temperature required by the PTC effect, and organic molecules or polymers with a melting point 10-25 ℃ above the temperature of the PTC effect are generally selected. If PMMA with a melting point of 92 ℃ is selected as the third component, the prepared electrothermal film can show obvious PTC effect at the temperature of about 70-80 ℃.
Drawings
FIG. 1 is a schematic view of the structure of the PTC electrothermal film of the present invention, wherein 1-supporting material, 2-third component, 3-conductive filler;
FIG. 2 is a graph showing the results of testing the finished product obtained in example 1 of the present invention;
FIG. 3 is a graph showing the test results of example 2 of the present invention;
FIG. 4 is a graph showing the test results of example 3 of the present invention;
FIG. 5 is a graph showing the results of testing the finished product obtained in example 4 of the present invention.
Detailed Description
In the following, an electrothermal film having PTC effect and a method for manufacturing the same will be described in more detail with reference to the accompanying drawings, in which preferred embodiments of the present invention are shown, it being understood that the present invention described herein can be modified by those skilled in the art, while still achieving the advantageous effects of the present invention. Accordingly, the following description is to be construed as broadly known to those skilled in the art and not as limiting the invention.
The invention is more particularly described by way of example in the following paragraphs with reference to the drawings. Advantages and features of the invention will become more apparent from the following description and from the claims. It should be noted that the drawings are in a very simplified form and are all to a non-precise scale, merely for convenience and clarity in aiding in the description of embodiments of the invention.
Referring to fig. 1, the electrothermal film provided by the invention comprises a conductive filler 3, a supporting material 1 and a third component 2, wherein the conductive filler 3 is filled in the third component 2, and the thermal expansion coefficient of the third component 2 is larger than that of the supporting material 1.
In this embodiment, the conductive filler 3 is carbon black, and in other embodiments, the conductive filler 3 may be one of conductive materials such as graphite, conductive fiber, copper powder, silver powder, or a mixture thereof.
In this embodiment, the supporting material 1 is polyurethane, and in other embodiments, the supporting material 1 may be other polymer materials, such as Polyethylene (PE), polypropylene (PP), polyvinylidene fluoride (PVDF), and the like.
The thermal expansion coefficient of the third component is higher than that of the heating element supporting material, and the capacity of volume expansion and PTC effect realization of the electrothermal film is provided; and as a supporting material for the heating element, mechanical properties and dimensional stability are provided. According to the invention, through adjusting and combining the third component, the electrothermal films with PTC effects at different temperatures can be designed in the electrothermal films of the same supporting material, so that the problem of thermal expansion of a body provided by a polymer supporting material in the prior art can be effectively solved, the product development flow is shortened, and the development cost is reduced.
The invention provides a preparation method of the electrothermal film, which comprises the following steps:
preparing third component particles containing conductive filler: mixing the conductive filler and the third component in a weight ratio of 40-90:30-60, adding into a screw extruder for melt extrusion, cooling, granulating and crushing to obtain third component particles containing the conductive filler;
specifically, the carbon black and the third component are mixed according to the weight ratio of 40-90:30-60, and are added into a screw extruder, and the temperature of each zone of the screw extruder is set to be 0-30 ℃ higher than the melting point of the third component. Then carrying out melt extrusion, cooling and granulating to obtain slices containing carbon black, crushing the slices by a crusher, and sieving by using a plurality of layers of sieves with different meshes to obtain third component particles containing carbon black and having meshes of 100-400 meshes;
preparing conductive carbon paste: adding 30-60% of third component particles containing conductive filler into a supporting material emulsion with solid content of 50-70% by weight, and stirring at room temperature to be uniform, thus obtaining conductive carbon slurry;
preparing an electrothermal film: and coating the conductive carbon paste on a substrate to obtain the electrothermal film with the PTC effect.
According to the preparation method of the novel electrothermal film with the PTC effect, the weight ratio of carbon black to the third component in the third component particles containing the conductive filler is 50-80:20-50, and the preferable weight ratio is 60-70:30-40.
According to the preparation method of the novel electrothermal film with the PTC effect, the third component refers to a water-insoluble organic small molecule or high molecular polymer or a combination thereof, and the selection is based on that the melting point of the third component is higher than the self-limiting temperature which needs to be realized by the electrothermal film, preferably 10-25 ℃. If the self-limiting temperature of the electrothermal film is about 60 ℃, microcrystalline wax with the melting point of 77 ℃ or EVA resin with the melting point of 75 ℃ can be selected.
Further, in the case of preparing an electrothermal film, the coating can be performed on a substrate by using a coater, and the thickness of the coating film is preferably 50 to 150. Mu.m.
According to the preparation method of the novel electrothermal film with the PTC effect, polyurethane emulsion is used as a supporting material in the preparation of the conductive carbon paste, and the chemical structure of polyurethane is not limited.
The invention also provides application of the novel electrothermal film with the PTC effect in occasions needing self-temperature limitation, such as electrothermal floor heating.
In the present invention, the carbon black is first blended with the third component and melt extruded for pelletization to allow the carbon black to be stably and uniformly present in the third component so that the carbon black is not directly distributed in the support polyurethane. Because the self-temperature limiting effect of the electrothermal film, the temperature of the electrothermal film is not higher than the melting point of the third component all the time, even if the electrothermal film is heated for many times, carbon black can not be separated from the constraint of the third component and can be diffused into other parts of the electrothermal film, so that the aim of the invention is conveniently realized, and the repeatability of the PTC effect of the electrothermal film after many times of heating is very good.
The following examples of the electrothermal film preparation method are given to clearly illustrate the present invention, and it should be understood that the present invention is not limited to the following examples, and other modifications by conventional means by those skilled in the art are within the scope of the present invention.
Example 1
Preparation of carbon black-containing third component particles
The carbon black used had a diameter average of 15 nm. 600 g of carbon black was mixed with 400 g of microcrystalline wax powder and fed into a 6 temperature zone twin screw extruder, the temperature of each zone of the screw extruder being set to: 80 ℃, 85 ℃, 82 ℃. The rotation speed of the screw is regulated according to the outlet pressure of the screw, and the outlet pressure is kept to be 5-10Mpa. The screw extruder is directly connected with a cooling granulator, and the slice containing carbon black is obtained after granulation. Crushing the slices by an electric crusher, sieving by a sieving machine with 3 layers of sieves, wherein the sieves are respectively 50 meshes, 200 meshes and 300 meshes, and collecting third component particles with the mesh number of 200-300 meshes.
Preparation of conductive carbon paste
200 g of the third component particles containing carbon black and having a size of 200-300 meshes prepared in the first step and 800 g of polyurethane emulsion with a solid content of 60% are added into a reaction kettle provided with a stirring device, and stirring is carried out at room temperature until the third component particles can be uniformly dispersed in the mixed system without sedimentation, thus obtaining the conductive carbon paste.
Preparation of electrothermal film
Coating the aqueous conductive carbon paste on a substrate, wherein the thickness of the coating is 100 mu m, and drying the coated substrate at 80 ℃ for half an hour to obtain the electrothermal film with the PTC effect.
The finished product in this embodiment is subjected to performance test, and the result of the power-on test is shown in fig. 2.
Example 2
Unlike example 1, in preparing the carbon black-containing third component fine particles, the third component used was PMMA; the temperature of each zone of the screw extruder was set as follows: 95 ℃, 100 ℃, 97 ℃.
The rest of the procedure is the same as in example 1.
The finished product in this embodiment is subjected to performance test, and the result of the power-on test is shown in fig. 3.
Example 3
Unlike example 1, in the preparation of the carbon black-containing third component particles, 700 g of carbon black was mixed with 300 g of microcrystalline wax and melt extruded into a twin screw extruder.
The rest of the procedure is the same as in example 1.
The finished product in this embodiment is subjected to performance test, and the result of the power-on test is shown in fig. 4.
Example 4
Unlike example 2, in the preparation of the conductive carbon paste, 250 g of mixed particles of PMMA and carbon black were added to 750 g of polyurethane emulsion having a solid content of 60%, and stirring was performed to prepare the conductive carbon paste.
The rest of the procedure is the same as in example 2.
The finished product in this embodiment is subjected to performance test, and the result of the power-on test is shown in fig. 5.
In summary, the third component of the invention has a higher thermal expansion coefficient than the thermal expansion coefficient of the heating element supporting material, and provides the volume expansion and the PTC effect realization capability of the electrothermal film; and as a supporting material for the heating element, mechanical properties and dimensional stability are provided. According to the invention, through adjusting and combining the third component, the electrothermal films with PTC effects at different temperatures can be designed in the electrothermal films of the same supporting material, so that the problem of thermal expansion of a body provided by a polymer supporting material in the prior art can be effectively solved, the product development flow is shortened, and the development cost is reduced. In the present invention, the carbon black is first blended with the third component and melt extruded for pelletization to allow the carbon black to be stably and uniformly present in the third component so that the carbon black is not directly distributed in the support polyurethane. Therefore, even if the electrothermal film is heated for a plurality of times, carbon black can not be separated from the constraint of the third component and can not be diffused into other parts of the electrothermal film, so that the purpose of the invention is conveniently realized, and the repeatability of the PTC effect of the electrothermal film after the electrothermal film is heated for a plurality of times is very good.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (8)
1. The preparation method of the electrothermal film with the PTC effect is characterized by comprising conductive filler, supporting materials and a third component, wherein the conductive filler is filled in the third component, and the thermal expansion coefficient of the third component is larger than that of the supporting materials, and the preparation method comprises the following steps:
preparing third component particles containing conductive filler: mixing the conductive filler and the third component in a weight ratio of 40-90:30-60, adding into a screw extruder for melt extrusion, cooling, granulating and crushing to obtain third component particles containing the conductive filler;
preparing conductive carbon paste: adding 30-60% of third component particles containing conductive filler into a supporting material emulsion with solid content of 50-70% by weight, and stirring at room temperature to be uniform, thus obtaining conductive carbon slurry;
preparing an electrothermal film: and coating the conductive carbon paste on a substrate to obtain the electrothermal film with the PTC effect.
2. A method of preparing an electrothermal film having PTC effect according to claim 1, wherein the conductive filler is carbon black and the supporting material is polyurethane.
3. A method of preparing an electrothermal film having PTC effect according to claim 2, wherein the third component is a water-insoluble organic molecule, and the third component has a melting point higher than a self-limiting temperature to be achieved by the electrothermal film.
4. A method of preparing an electrothermal film having PTC effect according to claim 3, wherein the melting point of the third component is 10-25 ℃ higher than the self-limiting temperature to be achieved by the electrothermal film.
5. A method of preparing an electrothermal film having PTC effect according to claim 1, wherein the third component is microcrystalline wax, EVA resin or PMMA.
6. A method of preparing an electrically heated film having a PTC effect according to claim 3 wherein the weight ratio of carbon black to the third component is 50-80:20-50.
7. A method for preparing an electrically heated film having a PTC effect according to claim 6, wherein the weight ratio of carbon black to the third component is 60-70:30-40.
8. A method of preparing an electrothermal film having PTC effect according to claim 1, wherein the mesh number of the third component particles is 100 to 400 mesh.
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| CN111031614B (en) * | 2019-12-18 | 2022-02-11 | 华东理工大学 | Carbon material-based efficient PTC (positive temperature coefficient) effect electrothermal film and preparation method thereof |
| CN111363342A (en) * | 2020-04-29 | 2020-07-03 | 合肥微晶材料科技有限公司 | Water-based graphene slurry with PTC (positive temperature coefficient) characteristic |
| CN111925686A (en) * | 2020-07-31 | 2020-11-13 | 深圳石墨烯创新中心有限公司 | Graphene heating ink with PTC self-temperature-limiting function and preparation method thereof |
| CN113174097B (en) * | 2021-02-25 | 2024-01-30 | 嘉兴市振明包装材料有限公司 | Self-temperature-limiting heating element, manufacturing method thereof and self-temperature-limiting heating sheet |
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| JPS566309A (en) * | 1979-06-28 | 1981-01-22 | Yokohama Rubber Co Ltd | Temperature sensor |
| JP3911345B2 (en) * | 1998-06-18 | 2007-05-09 | Ｔｄｋ株式会社 | Organic positive temperature coefficient thermistor |
| JP3506628B2 (en) * | 1998-06-24 | 2004-03-15 | Ｔｄｋ株式会社 | Manufacturing method of organic positive temperature coefficient thermistor |
| CN1172323C (en) * | 1999-06-04 | 2004-10-20 | Tdk株式会社 | Organic positive temp. coefficient thermistor |
| JP3896232B2 (en) * | 1999-10-01 | 2007-03-22 | Ｔｄｋ株式会社 | Organic positive temperature coefficient thermistor and manufacturing method thereof |
| US6607679B2 (en) * | 2001-01-12 | 2003-08-19 | Tdk Corporation | Organic PTC thermistor |
| TWI267530B (en) * | 2001-11-15 | 2006-12-01 | Tdk Corp | Organic PTC thermistor and making method |
| JP3914899B2 (en) * | 2002-06-24 | 2007-05-16 | Ｔｄｋ株式会社 | PTC thermistor body, PTC thermistor, method for manufacturing PTC thermistor body, and method for manufacturing PTC thermistor |
| JP3831363B2 (en) * | 2003-06-24 | 2006-10-11 | Ｔｄｋ株式会社 | Organic positive temperature coefficient thermistor, manufacturing method thereof, and measuring method of oxygen content thereof |
| CN102427617B (en) * | 2011-09-02 | 2013-07-10 | 西安盖沃热能科技有限公司 | Unidirectional heat transfer flame retardation PTC macromolecule self-limiting temperature electrothermal film and preparation method thereof |
| TW201604901A (en) * | 2014-07-30 | 2016-02-01 | 聚鼎科技股份有限公司 | Positive temperature coefficient device |
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