CN111269463A - Ultrathin low-voltage electric heating film material in low-temperature environment and preparation method thereof - Google Patents
Ultrathin low-voltage electric heating film material in low-temperature environment and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an ultrathin low-voltage electrothermal film material in a low-temperature environment and a preparation method thereof, and the ultrathin low-voltage electrothermal film material is a low-voltage electrothermal film prepared by using macromolecules as a matrix and conductive fillers in different forms as raw materials. The preparation method of the electrothermal film is simple; the electric heating effect is good, the electric heating performance is good at normal temperature and low voltage, and the electric heating performance is good at the environment of 50 ℃ below zero; and the electric heating film has ultra-thin thickness, can be widely applied to the fields such as electronic appliances.
Description
Technical Field
The invention relates to an ultrathin low-voltage electric heating film material in a low-temperature environment and a preparation method thereof, belonging to the field of electric heating.
Background
The internet has promoted the development of various intelligent electronic products, from button cell-phones to smart machines, from heavy desktop computers to thin notebook computers, many electronic products have changed people's life, work and amusement mode, many people can choose to move the official business, go on a business trip, travel and take portable panel computer, can work and entertain everywhere at any time and any place at all. Electronic products bring much convenience to our lives, but it is reported that many electronic products such as tablets, mobile phones and the like are not charged in winter. This occurs because the low temperature has some influence on the inside of the electronic product, so that it cannot be charged under normal conditions. There are many methods for solving the problem, such as charging near a warm source, charging in a quilt, etc., but the complicated methods have less ideal effect, and the electrothermal film is applied to the field of electronic products due to the excellent electrothermal performance of the electrothermal film, thereby providing great possibility for solving the problem.
In recent years, the excellent performances of the flexible electrothermal film in the modern semiconductor industry, physiotherapy and health care, wearable electronic equipment, defogging and defrosting and the like attract more and more attention. In the past, Indium Tin Oxide (ITO) electrothermal films have been widely used as thin film heaters due to their excellent optical transparency and high electrical conductivity. However, the price of ITO has been increasing in recent years. Worse still, the inherent brittleness of indium and tin greatly limits their applications.
In order to overcome these obstacles, researchers have used conductive materials with very high conductivity, such as graphene, to prepare an electrothermal film, and hopefully, the manufacturing cost of the electrothermal film is reduced, and hopefully, the flexibility of the electrothermal film is improved. Graphene is very high in electrical and thermal conductivity (5000W m)-1K-1) But is widely used as a conductive material. The excellent performances endow the electrothermal film prepared by the graphene with extremely low performanceSheet resistance and extremely fast temperature response. However, the reduction degree of graphene directly determines the conductivity of graphene, and graphene with good conductivity has no simple preparation method. The conductivity of the graphene obtained by the Hummers method is greatly influenced by the reduction degree and the reduction method, namely the graphene prepared by thermal reduction has good conductivity, but the graphene prepared by thermal reduction at least at 1500 ℃ or above has excellent conductivity, and the method even consumes energy and time and is not beneficial to secondary dispersion and utilization; the CVD method requires complicated equipment and is not high in safety, and the redispersion, molding and utilization of graphene are not facilitated.
Titanium carbide (Ti)3C2Tx) The graphene is a major hotspot of recent research, is a novel two-dimensional nanomaterial capable of being dispersed in solution and formed by transition metal carbide and nitride, is widely used as an electromagnetic shielding material due to the unique lamellar structure and ultrahigh conductivity, has excellent conductivity, film-forming property and hydrophilicity, has strong interaction force with a polymer, and has a simple production process, easy realization of theoretical conductivity and easier dispersion in a solvent compared with graphene which is a two-dimensional lamellar material, but the research in the field of electric heating is relatively less at present. The use of two-dimensional lamellar conductive fillers alone to make conductive polymers can affect their conductivity due to the voids between lamellar materials. Therefore, the invention combines the two-dimensional titanium conductive component and the one-dimensional conductive component, and fills the gap between the two-dimensional conductive filler by the one-dimensional conductive filler, thereby improving the overall conductivity of the material and preparing the electrothermal film with excellent conductivity, and the prepared electrothermal film not only has good electrothermal performance at minus 50 ℃, but also has ultrathin thickness, and can be widely applied to the field of electronics and electrics.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an ultrathin low-voltage electric heating film material in a low-temperature environment and a preparation method thereof, and an ultrathin electric heating film with excellent electric heating performance at minus 50 ℃ is successfully prepared.
The invention successfully prepares the ultrathin low-pressure low-temperature-resistant electrothermal film with extremely high conductivity by using two conductive fillers with different dimensionalities through a vacuum filtration technology. The electrothermal film prepared by the invention has the thickness of only 30um, and the volume of the electronic product cannot be obviously increased when the electrothermal film is used in the electronic product, and the electrothermal film still has good heating effect in an ultralow temperature environment of 50 ℃ below zero, so that the possibility of application of the electrothermal film in the electronic product is improved.
The method has wider application range, and can improve the electric heating performance of the electric heating film by the synergistic effect between various two-dimensional conductive fillers and linear conductive fillers. The method can obviously improve the service performance of the electrothermal film in extreme environments and improve the application range of the electrothermal film.
The invention relates to an ultrathin low-voltage electric heating film material in a low-temperature environment, which is obtained by processing the following raw materials in parts by mass:
40-60 parts of polymer base material, 30-40 parts of conductive filler A and 10-20 parts of conductive filler B.
The polymer base material is selected from one of cellulose, polyvinyl alcohol, alginic acid, soluble starch, polyethylene glycol, polyoxyethylene, polyacrylic acid, polyvinylpyrrolidone and the like.
The conductive filler A is selected from one of titanium carbide, titanium nitride, titanium carbonitride and the like; the conductive filler B is selected from one of carbon nano tube, carbon fiber, silver nano wire and the like.
The invention relates to a preparation method of an ultrathin low-voltage electrothermal film material in a low-temperature environment, which takes macromolecules as a base material, adds conductive fillers with different forms into the base material, and prepares an ultrathin low-voltage electrothermal film through vacuum filtration. The method specifically comprises the following steps:
step 1: adding 40-60 parts by mass of polymer base material into a three-neck flask provided with a stirrer, a reflux condenser tube and solvent water at 60-80 ℃, and stirring for 4-6h to uniformly disperse the polymer base material to obtain polymer dispersion liquid;
step 2: adding 30-40 parts by mass of conductive filler A and 10-20 parts by mass of conductive filler B into the macromolecular dispersion liquid obtained in the step (1), and ultrasonically stirring for 2-4h to uniformly disperse the conductive filler A and the conductive filler B to obtain electrothermal film slurry;
and step 3: and (3) adding the electrothermal film slurry obtained in the step (2) into a vacuum filtration device, carrying out vacuum filtration for 8-12h under a vacuum condition to obtain an electrothermal film with certain humidity, and then drying the electrothermal film in an oven at the temperature of 80 ℃ to obtain the ultrathin low-voltage electrothermal film.
The thickness of the ultrathin low-voltage electrothermal film prepared by the invention is 30-40 um.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method is simple in preparation process, water is used as a solvent in the preparation process, other toxic and harmful byproducts are not generated, and the requirements of green, environment-friendly and sustainable development are met;
2. the electric heating film prepared by the invention has an ultrathin structure, the thickness range is 30-40um, the electric heating film can have good heating performance under very low voltage, and the electric heating film is suitable for electronic products;
3. the electrothermal film prepared by the invention has good electric heating performance at minus 50 ℃, and the capability of the electrothermal film in resisting extreme environment is obviously improved.
Drawings
Fig. 1 is an optical and SEM picture of an electrothermal film 1 prepared in example 1 (taking titanium carbide and carbon nanotubes as examples).
Fig. 2 is a heating curve (taking titanium carbide and carbon nanotubes as examples) of the electrothermal film 1 prepared in example 1 at normal temperature.
Fig. 3 is a heating curve of 10V at low temperature of the electrothermal film 1 prepared in example 1 (taking titanium carbide and carbon nanotubes as examples).
Detailed Description
The raw materials and tests in examples 1-3 were funded by the national focus development program (2017YFC 0805900).
Example 1:
the novel ultrathin low-temperature-resistant voltage electrothermal film is prepared by taking a polymer base material, solvent water, a titanium compound and a linear conductive filler as raw materials and adopting a vacuum filtration method. Wherein the polymer matrix is cellulose, the titanium compound is titanium carbide, the linear conductive filler is carbon nano-tube, and the preparation method comprises the following steps:
step 1: adding 40 parts by mass of cellulose into a three-neck flask provided with a stirrer, a reflux condenser and solvent water at 60 ℃, and stirring for 4 hours after the addition is finished so as to completely dissolve the cellulose to obtain a cellulose solution;
step 2: taking the cellulose solution obtained in the step 1, adding 40 parts by mass of titanium carbide and 20 parts by mass of carbon nano tubes into the cellulose solution, and then ultrasonically stirring the mixed conductive filler for 2 hours to uniformly mix the mixed conductive filler and the carbon nano tubes to obtain electrothermal film slurry;
and step 3: and (3) adding the electrothermal film slurry obtained in the step (2) into a vacuum filtration device, carrying out vacuum filtration for 8 hours under a vacuum condition to obtain an electrothermal film with certain humidity, and then drying the electrothermal film in an oven at 80 ℃ for 10 minutes to obtain the ultrathin low-voltage electrothermal film. Meanwhile, the electric heating film which independently uses two-dimensional and one-dimensional conductive fillers is prepared for comparing the electric heating performance.
The SEM photo in figure 1 shows that the electrothermal film has an ultrathin structure, figure 2 shows that the electrothermal film has excellent heating performance under low pressure, figure 3 and table 1 show that the electrothermal film 1 can be heated from 50 ℃ below zero to 57 ℃ under 10V voltage, which shows that the electrothermal film has good heating performance under extreme low temperature environment. It can also be seen from table 1 that the electric heating film 1 using the two-dimensional conductive filler and the one-dimensional conductive filler in synergy has better electric heating performance than the electric heating film 2 using the two-dimensional conductive filler and the electric heating film 3 using the one-dimensional conductive filler alone.
TABLE 1 compounding ratio of electrothermal film and corresponding electrothermal performance
Example 2:
the novel ultrathin low-temperature-resistant voltage electrothermal film is prepared by taking a polymer matrix, solvent water, a titanium compound and linear conductive filler as raw materials and adopting a vacuum filtration method. Wherein the polymer matrix is polyvinyl alcohol, the titanium compound is titanium nitride, the linear conductive filler is carbon fiber, and the preparation method comprises the following steps:
step 1: adding 50 parts by mass of polyvinyl alcohol into a three-neck flask provided with a stirrer, a reflux condenser and solvent water at 70 ℃, and stirring for 5 hours after the addition is finished so as to completely dissolve the polyvinyl alcohol to obtain a cellulose solution;
step 2: taking the polyvinyl alcohol solution obtained in the step 1, adding 35 parts by mass of titanium nitride and 15 parts by mass of carbon fiber into the polyvinyl alcohol solution, and then ultrasonically stirring the mixed conductive filler for 2 hours to uniformly mix the mixed conductive filler and the carbon fiber to obtain electrothermal film slurry;
and step 3: and (3) adding the electrothermal film slurry obtained in the step (2) into a vacuum filtration device, carrying out vacuum filtration for 9 hours under a vacuum condition to obtain an electrothermal film with certain humidity, and then drying the electrothermal film in an oven at 80 ℃ for 10 minutes to obtain the ultrathin low-voltage electrothermal film. Meanwhile, the electric heating film which independently uses two-dimensional and one-dimensional conductive fillers is prepared for comparing the electric heating performance.
It can be seen from table 2 that the temperature of the electrothermal film 4 can be raised from-50 ℃ to 53 ℃ under the voltage of 10V, which shows that the electrothermal film has good electrothermal performance under the extreme low temperature environment. It can also be seen from table 2 that the electric heating film 4 using the two-dimensional conductive filler and the one-dimensional conductive filler in synergy has better electric heating performance than the electric heating film 5 using the two-dimensional conductive filler and the electric heating film 6 using the one-dimensional conductive filler alone.
TABLE 2 compounding ratio of electrothermal film and corresponding electrothermal performance
Example 3:
the novel ultrathin low-temperature-resistant voltage electrothermal film is prepared by taking a polymer matrix, solvent water, a titanium compound and linear conductive filler as raw materials and adopting a vacuum filtration method. Wherein the polymer matrix is selected from polyethylene glycol, the titanium compound is selected from titanium carbonitride, the linear conductive filler is selected from silver nanowires, and the preparation method comprises the following steps:
step 1: adding 60 parts by mass of cellulose into a three-neck flask provided with a stirrer, a reflux condenser and solvent water at 80 ℃, and stirring for 6 hours after the addition is finished to completely dissolve the cellulose to obtain a cellulose solution;
step 2: taking the polyethylene glycol solution obtained in the step 1, adding 30 parts by mass of titanium carbonitride and 10 parts by mass of silver nanowires into the polyethylene glycol solution, and then ultrasonically stirring the mixed conductive filler for 4 hours to uniformly mix the mixed conductive filler and the silver nanowires to obtain electrothermal film slurry;
and step 3: and (3) adding the electrothermal film slurry obtained in the step (2) into a vacuum filtration device, carrying out vacuum filtration for 10 hours under a vacuum condition to obtain an electrothermal film with certain humidity, and then drying the electrothermal film in an oven at 80 ℃ for 10 minutes to obtain the ultrathin low-voltage electrothermal film. Meanwhile, the electric heating film which independently uses two-dimensional and one-dimensional conductive fillers is prepared for comparing the electric heating performance.
It can be seen from table 3 that the temperature of the electrothermal film 7 can be raised from-50 ℃ to 63 ℃ under the voltage of 10V, which shows that the electrothermal film has good electrothermal performance under the extreme low temperature environment. It can also be seen from table 3 that the electric heating film 7 using the two-dimensional conductive filler and the one-dimensional conductive filler in synergy has better electric heating performance than the electric heating film 8 using the two-dimensional conductive filler and the electric heating film 9 using the one-dimensional conductive filler alone.
TABLE 3 compounding ratio of electrothermal film and corresponding electrothermal performance
Claims (6)
1. An ultrathin low-voltage electric heating film material in a low-temperature environment is characterized by being prepared from the following raw materials in parts by mass:
40-60 parts of polymer base material, 30-40 parts of conductive filler A and 10-20 parts of conductive filler B.
2. The ultra-thin low voltage electrothermal film material of claim 1, wherein:
the polymer base material is selected from one of cellulose, polyvinyl alcohol, alginic acid, soluble starch, polyethylene glycol, polyoxyethylene, polyacrylic acid, polyvinylpyrrolidone and the like.
3. The ultra-thin low voltage electrothermal film material of claim 1, wherein:
the conductive filler A is selected from one of titanium carbide, titanium nitride, titanium carbonitride and the like; the conductive filler B is selected from one of carbon nano tube, carbon fiber, silver nano wire and the like.
4. A method for preparing an ultrathin low-voltage electrothermal film material under a low-temperature environment according to claim 1, 2 or 3, which is characterized by comprising the following steps: the polymer is used as a base material, conductive fillers in different forms are added into the base material, and the ultrathin low-voltage electrothermal film is prepared by vacuum filtration.
5. The method according to claim 4, characterized by comprising the steps of:
step 1: adding 40-60 parts by mass of polymer base material into a three-neck flask provided with a stirrer, a reflux condenser tube and solvent water at 60-80 ℃, and stirring for 4-6h to uniformly disperse the polymer base material to obtain polymer dispersion liquid;
step 2: adding 30-40 parts by mass of conductive filler A and 10-20 parts by mass of conductive filler B into the macromolecular dispersion liquid obtained in the step (1), and ultrasonically stirring for 2-4h to uniformly disperse the conductive filler A and the conductive filler B to obtain electrothermal film slurry;
and step 3: and (3) adding the electrothermal film slurry obtained in the step (2) into a vacuum filtration device, carrying out vacuum filtration for 8-12h under a vacuum condition to obtain an electrothermal film with certain humidity, and then drying the electrothermal film in an oven at the temperature of 80 ℃ to obtain the ultrathin low-voltage electrothermal film.
6. The method of claim 5, wherein:
the thickness of the ultrathin low-voltage electrothermal film prepared by the invention is 30-40 um.
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Cited By (3)
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| CN112074024A (en) * | 2020-08-27 | 2020-12-11 | 南方科技大学 | Flexible electronic device and 3D printing preparation method |
| CN112210100A (en) * | 2020-10-16 | 2021-01-12 | 东华理工大学 | Preparation method of cellulose-based electrothermal composite film |
| CN113825262A (en) * | 2021-09-22 | 2021-12-21 | 中暖新能源(青岛)有限公司 | Ultrathin low-voltage electric heating film material in low-temperature environment and preparation method thereof |
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| CN112210100A (en) * | 2020-10-16 | 2021-01-12 | 东华理工大学 | Preparation method of cellulose-based electrothermal composite film |
| CN113825262A (en) * | 2021-09-22 | 2021-12-21 | 中暖新能源(青岛)有限公司 | Ultrathin low-voltage electric heating film material in low-temperature environment and preparation method thereof |
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