High-heat-energy-efficiency electric heating element and preparation method thereof
Technical Field
The invention relates to an electric heating element, in particular to an electric heating element with high heat efficiency and a preparation method thereof.
Background
The electrothermal film is divided into high-temperature and low-temperature electrothermal films. The high-temperature electrothermal film is generally used for electronic appliances, military affairs and the like, and is produced by the present science and technology. The low-temperature electrothermal film is a semi-transparent polyester film which can generate heat after being electrified and is made by processing and hot-pressing conductive special printing ink and metal current-carrying strips between insulating polyester films. When the electric heating film is used as a heating body, heat is sent into a space in a radiation mode, so that a human body and an object are firstly warmed, and the comprehensive effect of the electric heating film is superior to that of a traditional convection heating mode. The low-temperature radiation electrothermal film system consists of a power supply, a temperature controller, a connecting piece, an insulating layer, an electrothermal film and a decorative surface layer. The power supply is communicated with the electrothermal film through a lead to convert electric energy into heat energy. Because the electric heating film is a pure resistance circuit, the conversion efficiency is high, and except a small loss (2%), most (98%) of the electric heating film is converted into heat energy.
The preparation of the film is a rapidly developed material technology, and the preparation method of the film comprehensively utilizes the basic principles of physics, chemistry, material science and other subjects and adopts various high-technology means. Various types of thin films, such as metal thin films, compound thin films, organic thin films, etc., have been produced by various methods, of which a transparent conductive oxide semiconductor thin film is an important thin film. The transparent conductive oxide semiconductor film has the transparency of visible light, better conductivity, high ultraviolet cut-off and infrared reflection and strong attenuation to microwaves. The special physical properties of the material can be used for manufacturing display devices, transparent electrodes for photoelectric conversion, solar cells, electromagnetic protection, surface heating elements, infrared reflection films and the like.
The preparation technology of thin film materials has been developed so far, and there are many methods for obtaining thin films, but regarding the environment where the film forming reaction occurs and the film forming principle, the following four types are roughly classified into physical vapor deposition technologies including sputtering, thermal evaporation, and ion plating, chemical vapor deposition technologies in which solid substances are generated by chemical reaction and deposited on a substrate, sol-gel technologies, and solution film forming technologies represented by electrochemical reaction deposition.
Disclosure of Invention
A preparation method of an electric heating element with high heat energy efficiency comprises the following steps:
(1) uniformly stirring and mixing tin tetrachloride, boric acid, hydrofluoric acid, titanium tetrachloride, sodium chloride, a coupling agent, a resistance stabilizer and absolute ethyl alcohol to obtain an electrothermal film solution;
(2) cleaning and drying the surface of the base material;
(3) heating the electrothermal film solution into steam, spraying the steam on the surface of a base material by means of carrier gas, and depositing the steam (the deposition is a general term in the industry) on the surface of the base material to form a film;
(4) sintering the film, and naturally cooling the sintered film in the air to obtain an electrothermal film;
(5) and placing an electrode material on the surface of the electrothermal film, and then carrying out heating treatment to obtain the electrothermal element with high heat efficiency.
A preparation method of an electric heating element with high heat energy efficiency comprises the following steps:
(1) uniformly stirring and mixing 45-55 parts by weight of tin tetrachloride, 0.1-1 part by weight of boric acid, 1-10 parts by weight of hydrofluoric acid, 0.3-3 parts by weight of titanium tetrachloride, 1-5 parts by weight of sodium chloride, 1-3 parts by weight of nickel dichloride, 1-5 parts by weight of coupling agent, 1-3 parts by weight of resistance stabilizer and 10-30 parts by weight of absolute ethyl alcohol to obtain an electrothermal film solution;
(2) cleaning the surface of the base material with absolute ethyl alcohol, and then drying the base material in a forced air drying oven at 75-85 ℃ for 1-5 hours;
(3) heating the electrothermal film solution into steam, wherein the steam temperature is 200-300 ℃, the steam is sprayed on the surface of the base material by means of carrier gas, the base material temperature is 550-650 ℃, the spraying distance is 20-30cm, the carrier gas flow is 45-55L/min, and the steam is deposited on the surface of the base material to form a film with the thickness of 1-10 mu m;
(4) sintering the film at the sintering temperature of 700-800 ℃ for 10-30 minutes, and naturally cooling the sintered film in the air to obtain the electrothermal film;
(5) and placing an electrode material on the surface of the electrothermal film, and then carrying out heating treatment to obtain the electrothermal element with high heat efficiency.
Preferably, the substrate may be selected from the group consisting of microcrystalline glass, mica, ceramic, quartz glass, high borosilicate glass.
Preferably, the electrodes may be selected from a conductive paste, a wire or a foil.
Preferably, the carrier gas may be selected from one or more of neon, helium or nitrogen.
Preferably, the coupling agent is used in an amount of 2.5 to 3.5 parts by weight.
Preferably, the coupling agent is at least one of silane coupling agent, titanate coupling agent and aluminate coupling agent, the silane coupling agent can be selected from 3-chloropropylmethyldimethoxysilane and diethylenetriaminopropyltrimethoxysilane, the titanate coupling agent can be selected from isopropyl tri (dioctyl pyrophosphato acyloxy) titanate and isopropyl dioleato acyloxy (dioctyl phosphato acyloxy) titanate, and the aluminate coupling agent can be selected from aluminate coupling agent 821 and aluminate coupling agent DL-411.
Further preferably, the coupling agent is a titanate coupling agent.
Further preferably, the coupling agent is isopropyl dioleayloxy (dioctylphosphonoyl) titanate.
Preferably, the resistance stabilizer is one of bismuth trichloride and strontium chloride or a mixture thereof.
An electric heating element with high heat energy efficiency is prepared by adopting the method.
The performance and the use of the electrothermal film solution are determined by the components and the proportion, different components in the electrothermal film solution can influence each other, the components and the proportion can determine the final performance of the electrothermal film solution, if the components and the proportion are not coordinated with each other, the beneficial effect brought by the single component can be reduced or even eliminated by other components, and in severe cases, the different components are mutually contradicted, so that the overall comprehensive effect cannot be achieved, and negative effects and defective products are generated.
According to the electric heating element with high heat energy efficiency and the preparation method thereof, the optimal components and the proportion of the electric heating film solution are obtained through a large amount of creative labor and repeated verification, so that a plurality of components are integrated and coordinated with each other, and a forward comprehensive effect is generated; the electric heating element made by the method has the advantages of low cost, stable performance, high heat energy conversion efficiency, no open fire, small attenuation, long service life and suitability for various power supply forms.
Detailed Description
The method for testing the adhesion performance of the high-heat-efficiency electric heating element comprises the following steps: the method is carried out according to the national mechanical industry standard JB/T8554-1997 scratch test method for the adhesion of the vapor deposition film and the matrix. The WS-2005 type coating adhesive force automatic scratching instrument is adopted for testing, the testing method is a sound emission measurement mode, the loading rate is 5N/min, and the scratching rate is 2 mm/min.
The resistance change rate test method of the high-heat-energy-efficiency electric heating element comprises the following steps: the loading voltage of 190V is adopted, a VC 9801A type universal meter is used for measuring the effective value of the line current, the heating rate of the electric heating element is 2 ℃/min, the value is read once every ten minutes, the resistance value is calculated according to the measured data, and then the average resistance value is obtained, and the resistance change rate of the electric heating element with high heat efficiency at 1000 ℃ relative to the room temperature is obtained.
Examples 1 to 3
The preparation method of the electric heating element with high heat energy efficiency comprises the following steps:
(1) stirring and uniformly mixing 50 parts by weight of tin tetrachloride, 0.3 part by weight of boric acid, 6 parts by weight of hydrofluoric acid, 1 part by weight of titanium tetrachloride, 2 parts by weight of sodium chloride, 2 parts by weight of nickel dichloride, 2 parts by weight of coupling agent (the kind of the coupling agent is shown in table 1), 2 parts by weight of bismuth trichloride and 20 parts by weight of absolute ethyl alcohol at the rotating speed of 500 revolutions per minute for 8 hours to obtain an electrothermal film solution;
(2) cleaning the surface of quartz glass with absolute ethyl alcohol, and then drying the quartz glass in a forced air drying oven for 2 hours at the temperature of 80 ℃;
(3) heating the electrothermal film solution into steam, wherein the steam temperature is 250 ℃, the steam is sprayed on the surface of the quartz glass by means of carrier gas, the temperature of the quartz glass is 600 ℃, the spraying distance is 25cm, the carrier gas flow is 50L/min, and the steam is deposited on the surface of the quartz glass to form a film with the thickness of 5 mu m, wherein the carrier gas is nitrogen;
(4) sintering the film at 750 deg.c for 20 min, and naturally cooling in air to obtain electrothermal film;
(5) silver paste is smeared on the surface of the electric heating film, and then heating treatment is carried out for 10 minutes at the temperature of 800 ℃, so as to obtain the electric heating element with high heat efficiency.
Table 1: coupling agent type and high heat energy efficiency electric heating element performance test result table
Wherein, isopropyl dioleate acyloxy (dioctyl phosphate acyloxy) titanate is provided by Nanjing Aureox chemical Co., Ltd, CAS number: 61417-49-0.
As shown in Table 1, the rate of change in resistance and the adhesion property were satisfactory when the coupling agent was a titanate-based coupling agent.
Examples 4 to 12
The preparation method of the electric heating element with high heat energy efficiency comprises the following steps:
(1) stirring and uniformly mixing 50 parts by weight of tin tetrachloride, 0.3 part by weight of boric acid, 6 parts by weight of hydrofluoric acid, 1 part by weight of titanium tetrachloride, 2 parts by weight of sodium chloride, 2 parts by weight of nickel dichloride, isopropyl dioleate acyloxy (dioctylphosphate acyloxy) titanate (the dosage of a coupling agent is shown in a table 2), 2 parts by weight of bismuth trichloride and 20 parts by weight of absolute ethyl alcohol at the rotating speed of 500 revolutions per minute for 8 hours to obtain an electrothermal film solution;
(2) cleaning the surface of quartz glass with absolute ethyl alcohol, and then drying the quartz glass in a forced air drying oven for 2 hours at the temperature of 80 ℃;
(3) heating the electrothermal film solution into steam, wherein the steam temperature is 250 ℃, the steam is sprayed on the surface of the quartz glass by means of carrier gas, the temperature of the quartz glass is 600 ℃, the spraying distance is 25cm, the carrier gas flow is 50L/min, and the steam is deposited on the surface of the quartz glass to form a film with the thickness of 5 mu m, wherein the carrier gas is nitrogen;
(4) sintering the film at 750 deg.c for 20 min, and naturally cooling in air to obtain electrothermal film;
(5) silver paste is smeared on the surface of the electric heating film, and then heating treatment is carried out for 10 minutes at the temperature of 800 ℃, so as to obtain the electric heating element with high heat efficiency.
Table 2: coupling agent dosage and high heat energy efficiency electric heating element performance test result table
Wherein, isopropyl dioleate acyloxy (dioctyl phosphate acyloxy) titanate is provided by Nanjing Aureox chemical Co., Ltd, CAS number: 61417-49-0.
As shown in Table 2, the isopropyl dioleate acyloxy (dioctylphosphate acyloxy) titanate coupling agent used in an amount of 3 parts by weight had an ideal resistance change rate and an ideal adhesion property, and the amount used was the most reasonable.
Example 13
The preparation method of the electric heating element with high heat energy efficiency comprises the following steps:
(1) stirring and uniformly mixing 50 parts by weight of tin tetrachloride, 0.3 part by weight of boric acid, 6 parts by weight of hydrofluoric acid, 1 part by weight of titanium tetrachloride, 2 parts by weight of sodium chloride, 2 parts by weight of nickel dichloride, 3 parts by weight of isopropyl dioleate acyloxy (dioctylphosphonoxy) titanate, 2 parts by weight of strontium chloride and 20 parts by weight of absolute ethyl alcohol at the rotating speed of 500 revolutions per minute for 8 hours to obtain an electrothermal film solution;
(2) cleaning the surface of quartz glass with absolute ethyl alcohol, and then drying the quartz glass in a forced air drying oven for 2 hours at the temperature of 80 ℃;
(3) heating the electrothermal film solution into steam, wherein the steam temperature is 250 ℃, the steam is sprayed on the surface of the quartz glass by means of carrier gas, the temperature of the quartz glass is 600 ℃, the spraying distance is 25cm, the carrier gas flow is 50L/min, and the steam is deposited on the surface of the quartz glass to form a film with the thickness of 5 mu m, wherein the carrier gas is nitrogen;
(4) sintering the film at 750 deg.c for 20 min, and naturally cooling in air to obtain electrothermal film;
(5) silver paste is smeared on the surface of the electric heating film, and then heating treatment is carried out for 10 minutes at the temperature of 800 ℃, so as to obtain the electric heating element with high heat efficiency. And (3) performance test results: the adhesion was 157N, and the rate of change in resistance was 1.42%.
Example 14
The preparation method of the electric heating element with high heat energy efficiency comprises the following steps:
(1) stirring and uniformly mixing 50 parts by weight of tin tetrachloride, 0.3 part by weight of boric acid, 6 parts by weight of hydrofluoric acid, 1 part by weight of titanium tetrachloride, 2 parts by weight of sodium chloride, 2 parts by weight of nickel dichloride, 3 parts by weight of isopropyl dioleate acyloxy (dioctyl phosphate acyloxy) titanate, 1 part by weight of bismuth trichloride, 1 part by weight of strontium chloride and 20 parts by weight of absolute ethyl alcohol at the rotating speed of 500 revolutions per minute for 8 hours to obtain an electrothermal film solution;
(2) cleaning the surface of quartz glass with absolute ethyl alcohol, and then drying the quartz glass in a forced air drying oven for 2 hours at the temperature of 80 ℃;
(3) heating the electrothermal film solution into steam, wherein the steam temperature is 250 ℃, the steam is sprayed on the surface of the quartz glass by means of carrier gas, the temperature of the quartz glass is 600 ℃, the spraying distance is 25cm, the carrier gas flow is 50L/min, and the steam is deposited on the surface of the quartz glass to form a film with the thickness of 5 mu m, wherein the carrier gas is nitrogen;
(4) sintering the film at 750 deg.c for 20 min, and naturally cooling in air to obtain electrothermal film;
(5) silver paste is smeared on the surface of the electric heating film, and then heating treatment is carried out for 10 minutes at the temperature of 800 ℃, so as to obtain the electric heating element with high heat efficiency. And (3) performance test results: the adhesion was 194N and the rate of change in resistance was 0.82%.