WO2013177838A1 - Ptc rare-earth thick film circuit intelligent electrical heating element and preparation method therefor - Google Patents

Ptc rare-earth thick film circuit intelligent electrical heating element and preparation method therefor Download PDF

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WO2013177838A1
WO2013177838A1 PCT/CN2012/077518 CN2012077518W WO2013177838A1 WO 2013177838 A1 WO2013177838 A1 WO 2013177838A1 CN 2012077518 W CN2012077518 W CN 2012077518W WO 2013177838 A1 WO2013177838 A1 WO 2013177838A1
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thick film
rare earth
film circuit
ptc
glass
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PCT/CN2012/077518
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French (fr)
Chinese (zh)
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王克政
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佛山市海辰科技有限公司
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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
    • H05B3/10—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
    • 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
    • H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
    • H05B3/26—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base
    • H05B3/262—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base the insulating base being an insulated metal plate
    • 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
    • H05B2203/002—Heaters using a particular layout for the resistive material or resistive elements
    • H05B2203/003—Heaters using a particular layout for the resistive material or resistive elements using serpentine layout
    • 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
    • H05B2203/013—Heaters using resistive films or coatings
    • 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
    • H05B2203/02—Heaters using heating elements having a positive temperature coefficient

Definitions

  • the invention relates to the technical field of thick film circuit electric heating elements, and more particularly to the field of intelligent thick film circuit electric heating elements for automatic control of PTC thick film circuit thermistors.
  • the PTC thick film circuit thermistor is a thick film circuit intelligent electric heating element fabricated by a thick film circuit manufacturing process and a unique control property of the thermistor combined with a thick film resistor circuit.
  • This theoretical concept "PTC thick film circuit controllable electric heating element" has obtained national patents, has been proposed as early as 2004, and has been promoted and applied.
  • the PTC thermistor thick film circuit not only has the general characteristics of the thermistor, but also has the unique and excellent performance that the general thermistor does not have due to its material composition and process uniqueness.
  • controllable electric heating element can be formed in the form of a thick film circuit. Therefore, it has important applications in many fields, especially in the military industry.
  • the object of the present invention is to provide a non-heating temperature field uniform grading and self-control, fast thermal response, high power density, flexible design, compact structure, energy saving, environmental protection, safety and reliability, and high temperature in order to solve the deficiencies of the prior art.
  • Far infrared function PTC rare earth thick film circuit intelligent electric heating element is to provide a non-heating temperature field uniform grading and self-control, fast thermal response, high power density, flexible design, compact structure, energy saving, environmental protection, safety and reliability, and high temperature in order to solve the deficiencies of the prior art.
  • Far infrared function PTC rare earth thick film circuit intelligent electric heating element Far infrared function PTC rare earth thick film circuit intelligent electric heating element.
  • Another object of the present invention is to provide a method for preparing a PTC rare earth thick film circuit intelligent electric heating element.
  • a PTC rare earth thick film circuit intelligent electric heating element which comprises a metal substrate and a PTC thick film circuit thermistor and a rare earth thick film resistor circuit disposed thereon PTC thick film circuit thermistor is superimposed or in the same plane with the rare earth thick film resistor circuit in the form of thick film circuit to control the temperature of the thick film circuit electric heating element, so that the control precision and sensitivity can be greatly improved;
  • the controllable electric heating element is separately formed in the form of a thick film circuit.
  • the metal substrate is a ferrite Cr15 ⁇ 1Cr17 ⁇ 00Cr18Mo2 series stainless steel substrate.
  • the PTC thick film circuit thermistor is made of a PTC thick film circuit thermistor paste
  • the rare earth thick film resistor circuit is made of a rare earth dielectric paste and a rare earth electrode paste.
  • the rare earth medium slurry is composed of a solid phase component and an organic solvent carrier, and the weight ratio thereof is 65: 35 ⁇ 85: 15; solid phase composition: SiO 2 ⁇ Al203 ⁇ CaO ⁇ B2O3 ⁇ La2O3 rare earth oxide glass-ceramic, weight ratio: Si02 30 ⁇ 65 %, Al203 5 ⁇ 26%, CaO 15 ⁇ 38%, B2O3 2 ⁇ 16%, La2O3 0. 3 ⁇ 15%. Co2O3 0 .
  • crystal nucleating agent is TiO2 1 ⁇ 10 %, ZrO: 1 ⁇ 10%; solvent carrier ratio: butyl carbitol 66 ⁇ 89%, citric acid tributyl vinegar 5 ⁇ 15%, ethyl cellulose 0.5 ⁇ 10%, hydrogenated castor oil 0.1 ⁇ 5 %, lecithin 0.1 ⁇ 5 %; rare earth oxides are one or more of lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium and cerium oxide
  • the PTC thick film circuit thermistor slurry is composed of cerium oxide, copper oxide, cerium oxide composite powder, glass ceramic powder and an organic carrier, and the weight ratio of cerium oxide, copper oxide, cerium oxide and organic carrier is 65 ⁇ 85 : 35 ⁇ 15; solid phase composition of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder, the weight of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic in solid phase composition The ratio is 75 ⁇ 55 : 25 ⁇ 45 ; The weight ratio of cerium oxide, copper oxide and cerium oxide powder in cerium oxide, copper oxide and cerium oxide composite powder is: 75 ⁇ 59: 15 ⁇ 40.5 : 10 ⁇ The particle size of 0.5, cerium oxide, copper oxide and cerium oxide composite powder is 0.30--1.0 ⁇ m; the glass-ceramic powder is: CaO ⁇ SiO2 ⁇ A12O3 ⁇ B2O3 ⁇ Bi2O3 ⁇ Rare earth oxide-based glass-ceramics of La2
  • the rare earth electrode slurry is composed of a solid phase component and an organic solvent carrier, and the weight ratio is 70 to 90:30 ⁇ 10.
  • the solid phase composition includes silver-palladium-ruthenium composite powder and glass-ceramic powder, the weight ratio of silver-palladium-iridium composite powder to glass-ceramic powder is 99.4 ⁇ 0.6: 0.6 ⁇ 6; the weight ratio of silver-palladium-ruthenium composite powder is: 0.6 ⁇ 10.
  • the nucleating agent is: Ti021 ⁇ 10%, ZrO21 ⁇ 10 %; rare earth oxides are one or more of cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum and cerium oxide.
  • PTC rare earth thick film circuit intelligent electric heating element characterized in that it is prepared by metal substrate, rare earth medium slurry, PTC thick film circuit thermistor paste, electrode paste and package slurry according to the process flow
  • the process of forming a PTC rare earth thick film circuit electric heating element is as follows:
  • the preparation process of the rare earth medium slurry comprises the following steps:
  • each oxide and crystal nucleating agent are mixed and smelted according to the weight ratio, and the melting temperature is: 1100 ⁇ 1450 °C. After 90-180 minutes of heat preservation, the water is quenched to obtain glass micro-slag; the glass micro-slag is ball-milled to prepare a glass-ceramic powder having a particle diameter of 1 to 3 ⁇ m;
  • 3 medium slurry preparation the weight ratio of the solid phase component to the organic solvent carrier is 65: 85 ⁇ 35 :15; After R-S01 bidirectional rotation + vibration machine, after mixing, stirring and dispersing for one hour, the three sticks are rolled to obtain the finished product, and the viscosity value is 150 ⁇ 200PaS / RPM.
  • the preparation process of the PTC thick film circuit thermistor paste comprises the following steps:
  • cerium oxide, copper oxide and cerium oxide composite powder weight ratio of cerium oxide, copper oxide and cerium oxide: 75 ⁇ 59 : 15 ⁇ 40.5 : 10 ⁇ 0.5, after three-dimensional stirring, mixing and uniform, ball milling to obtain composite powder, the particle size is: 0.30 ⁇ 1.0 ⁇ m;
  • solid phase composition consists of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder, the weight ratio is: 75 ⁇ 55 : 25 ⁇ 45; solid phase composition and organic carrier weight ratio: 65 ⁇ 85: 35 ⁇ 15, the solid phase powder and the organic carrier solvent are subjected to two-way rotation + vibration machine of R-S01 type, stirred and mixed uniformly, and then subjected to three-roll repeated rolling to obtain a finished product, and the viscosity value is 150 ⁇ 200 PaS / RPM. .
  • the preparation process of the rare earth electrode slurry comprises the following steps:
  • glass-ceramic powder The oxides and crystal nucleating agents are uniformly mixed according to the weight ratio of raw materials, and then smelted at a temperature of 1100 ⁇ 1450 °C. , heat preservation for 1-3 hours, water quenching to obtain glass micro slag, ball milling to obtain 3 micron glass micropowder;
  • the invention adopts a metal substrate, a series of rare earth electronic pastes and a series of rare earth electronic pastes prepared on a metal substrate.
  • the above rare earth electronic paste is specially designed for the electric heating field, and also discloses a dielectric slurry and an electrode slurry.
  • the formulation of PTC thick film circuit thermistor slurry is a further upgrade and improvement of the prior art, except that the heating temperature field is uniform and gradable, the thermal response is fast, the power density is large, the design is flexible, the structure is compact, and the energy saving and environmental protection are Safe and reliable, it also has high-temperature far-infrared function.
  • the temperature of the intelligent electric heating element is wide: 25-400 °C.
  • High and low voltage (3-380V), AC and DC: Ac, Dc can be used, widely used in solar energy, wind energy, lithium-ion batteries and other new energy fields.
  • each functional phase formula contains rare earth elements. Due to the addition of rare earth metals, the compatibility, wettability, thermal properties, electrical properties, processability and adaptability of the slurry are significantly improved.
  • the rare earth thick film circuit electric heating element is named after the rare earth thick film based on the metal substrate. The successful development and application of circuit intelligent electric heating elements has pioneering and innovative significance.
  • FIG. 1 is a schematic structural view of a PTC rare earth thick film circuit intelligent electric heating element according to the present invention.
  • the invention discloses a PTC rare earth thick film circuit intelligent electric heating element, which comprises a metal substrate 1 and a PTC thick film circuit thermistor 2 and a rare earth thick film resistor circuit 3 disposed thereon, and a PTC thick film circuit heat.
  • the varistor is in the form of a thick film circuit and the rare earth thick film resistor circuit is superimposed or in the same plane to control the temperature of the thick film circuit electric heating element, so that the control precision and sensitivity can be greatly improved; and the thick film circuit can be separately used.
  • the metal substrate is a ferritic Cr15, 1Cr17 or 00Cr18Mo2 series stainless steel substrate.
  • PTC rare earth thick film circuit intelligent electric heating element is prepared by metal substrate, series rare earth electronic paste, series rare earth electronic paste on metal substrate and sintered process.
  • the series rare earth electronic paste comprises a rare earth medium slurry and a rare earth electrode slurry, and the series of electronic pastes are composed of a functional phase and an organic carrier.
  • the series rare earth electronic paste also includes a PTC thick film circuit thermistor paste, and the above rare earth electronic paste is specialized in the field of electric heating.
  • the series of rare earth electronic pastes refers to a series of dielectric pastes, PTC thick film circuit thermistor pastes, electrode pastes, encapsulating pastes and the like doped rare earth oxides lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, ⁇ , ⁇ and ⁇ And other chemical elements, according to different temperature, different power, different uses of electronic paste resistance, temperature coefficient, electrical properties, thermal properties and far-infrared function requirements, according to the experimental mathematical model to add different types, different proportions of rare earth oxides, To add or replace one or more of the ingredients in the formula.
  • the rare earth medium slurry is composed of a solid phase component and an organic solvent carrier, and the weight ratio thereof is 65:35 ⁇ 85 : 15
  • the solid phase composition is: SiO2 - Al203 ⁇ CaO ⁇ B2O3 ⁇ La2O3 and other rare earth oxide-based glass-ceramics, the weight ratio is: Si02 30 ⁇ 65 %, Al203 5 ⁇ 26%, CaO 15 ⁇ 38%, B2O3 2 ⁇ 16%, La2O3 0. 3 ⁇ 15%. Co2O3 0.05 ⁇ 6 %.
  • the nucleating agent is TiO2 1 ⁇ 10%, ZrO: 1 ⁇ 10%.
  • the solvent carrier ratio is: butyl carbitol 66 ⁇ 89%, citric acid tributyl vinegar 5 ⁇ 15%, ethyl cellulose 0.5 ⁇ 10%, hydrogenated castor oil 0.1 ⁇ 5 %, lecithin 0.1 ⁇ 5 %.
  • the rare earth oxides are: antimony, bismuth, antimony, bismuth, antimony, bismuth, antimony, antimony and antimony oxide. According to the requirements of thermal, chemical, mechanical and far-infrared functions of the dielectric pastes of different temperatures and different uses, the rare earth oxides may be added with different types and different proportions of rare earth oxides according to the experimental mathematical model. To add or replace one or more of the requirements for the composition of the glass-ceramics.
  • 3 medium slurry preparation the weight ratio of the solid phase component to the organic solvent carrier is 65: 85 ⁇ 35 :15; After R-S01 two-way rotation + vibration machine, after mixing, stirring and dispersing for one hour, the three sticks are rolled to obtain the finished product.
  • the viscosity value is 150 ⁇ 200PaS / RPM.
  • PTC thick film circuit thermistor paste consists of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder and organic carrier.
  • the weight ratio of cerium oxide, copper oxide, cerium oxide and organic carrier is 65. ⁇ 85 : 35 ⁇ 15 ;
  • the weight ratio of cerium oxide, copper oxide and cerium oxide powder in cerium oxide, copper oxide and cerium oxide composite powder is: 75 ⁇ 59: 15 ⁇ 40.5 : 10 ⁇
  • the particle size of 0.5, cerium oxide, copper oxide and cerium oxide composite powder is 0.30--1.0 ⁇ m;
  • the glass ceramic powder is: CaO ⁇ SiO2 ⁇ A12O3 ⁇ B2O3 ⁇ Bi2O3 ⁇ Rare earth oxide-based glass-ceramics such as La2 03; weight ratio of each oxide:
  • the nucleating agent is: TiO21 ⁇ 8 %, ZrO21 ⁇ 10%; the weight ratio of each component of the organic carrier: terpineol 68 ⁇ 78 %, 2 ⁇ 18 % citric acid citrate, 0.4 ⁇ 9% ethyl cellulose, 0.4 ⁇ 9% nitrocellulose, hydrogenated castor oil 0.1 to 6%, lecithin 0 .1 ⁇ 6%.
  • rare earth oxides are lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium and cerium oxide.
  • Rare earth oxides can be added according to different power, temperature, and different applications of PTC thick film circuit thermistor paste resistance, temperature coefficient, thermal performance, and far infrared function, according to the experimental mathematical model to add different types, different proportions Rare earth oxides. To add or replace one or more of the ingredient composition requirements.
  • the preparation of the PTC thick film circuit thermistor paste includes the following process steps:
  • glass-ceramic powder According to the above oxide and crystal nucleating agent ratio, the mixture is uniformly mixed in a three-dimensional mixer, and the furnace is smelted at a temperature of 1100 ⁇ After heat preservation at 1450 ° C for 1 ⁇ 3 hours, the glass melt is water quenched to obtain micro slag, which is ball milled for 4-6 hours with steamed water as a medium, and obtained by using ball milling to obtain a glass micropowder having a particle size of 3-5 ⁇ m micron;
  • cerium oxide, copper oxide and cerium oxide composite powder the weight ratio of cerium oxide, copper oxide and cerium oxide is: 75 ⁇ 59 : 15 ⁇ 40.5 : 10 ⁇ 0.5, the composite powder is obtained by three-dimensional stirring and mixing; the composite powder is ball milled for 9 to 18 hours with ethanol as the medium, and the particle size is controlled to be 0.30--1.0 ⁇ m;
  • solid phase composition consists of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder, the weight ratio is: 75 ⁇ 55 : 25 ⁇ 45; solid phase composition and organic carrier weight ratio: 65 ⁇ 85: 35 ⁇ 15.
  • the solid phase powder and the organic carrier solvent are subjected to R-S01 bidirectional rotation + vibration machine, stirred and uniformly mixed, and three-roll repeated rolling is performed to obtain a PTC thick film circuit thermistor slurry. Viscosity value is 150 ⁇ 200PaS / RPM.
  • the rare earth electrode slurry is composed of a solid phase component and an organic solvent carrier, and the weight ratio is 70 to 90:30 ⁇ 10.
  • the solid phase composition includes silver-palladium-ruthenium composite powder and glass-ceramic powder, the weight ratio of silver-palladium-iridium composite powder to glass-ceramic powder is 99.4 ⁇ 0.6: 0.6 ⁇ 6; the weight ratio of silver-palladium-ruthenium composite powder is: 0.6 ⁇ 10:99 ⁇ 82:0.4 ⁇ 8; particle size: 3 ⁇ m.
  • the weight ratio of the organic solvent carrier is: terpineol 60 ⁇ 98%, tributyl citrate 10 ⁇ 30%, ethyl cellulose 2 ⁇ 10 %, nitrocellulose 1 ⁇ 5 %, hydrogenated castor oil 0.1 ⁇ 5 %, lecithin 0.1 ⁇ 5 %.
  • Glass-ceramics are SiO2 ⁇ A12O3 ⁇ CaO ⁇ B203 ⁇ Bi2O3 ⁇ La2O3 rare earth, oxide-based glass-ceramics, the weight ratio of each oxide is: SiO2 20 ⁇ 60%, A12O35 ⁇ 35 %, CaO 10 ⁇ 35 %, B2031 ⁇ 15 %, La2O3 0. 3 ⁇ 15%, Bi2O3 10 ⁇ 30%.
  • the crystal nucleating agent is: Ti021 ⁇ 10%, ZrO21 ⁇ 10%.
  • rare earth oxides are: antimony, bismuth, antimony, bismuth, antimony, bismuth, antimony, antimony and antimony oxide.
  • Rare earth oxides can be added according to the requirements of electrical conductivity, thermal properties and chemical properties of electrode pastes at different temperatures, and different types and different proportions of rare earth oxides are added according to the experimental mathematical model. To add or replace one or more of the ingredient composition requirements.
  • the preparation of the rare earth electrode slurry includes the following process steps:
  • glass-ceramic powder The oxide and crystal nucleating agent are uniformly mixed according to the weight ratio of raw materials, and the temperature is: 1100 ⁇ 1450 °C , heat preservation for 1-3 hours, water quenching to obtain glass micro slag, ball milling to obtain 3 micron glass micropowder;
  • a rare earth thick film electric heating element is prepared according to a process flow by using a spare metal substrate, a rare earth medium slurry, a PTC thick film circuit thermistor paste, an electrode slurry, and a package slurry.
  • the slurry is left for too long and needs to be homogenized before use.
  • the thickness of the dielectric layer is required to be >65 ⁇ m, and the thickness of the thermal thick film circuit is >15 ⁇ m;
  • the PTC thick film circuit thermistor paste and the electrode paste are compatible with a plurality of metal substrate dielectric pastes.
  • a metal substrate dielectric paste for example, an aluminum alloy substrate, a copper alloy substrate, a titanium alloy substrate, or the like.
  • the PTC thick film circuit thermistor paste, electrode paste, and package slurry can be prepared on an alumina substrate (Al2O3), On a substrate such as an aluminum nitride (AIN) substrate, a silicon carbide (SiC) substrate, a glass-ceramic substrate, or a polymer composite ceramic, a strong bond-bonding effect is produced, and a high-efficiency far-infrared function is obtained.
  • AIN aluminum nitride
  • SiC silicon carbide
  • Metal substrate based PTC rare earth thick film circuit intelligent electric heating element is currently high and low voltage, AC and DC can start, small volume, large surface thermal load, high thermal efficiency, fast hot start, uniform temperature field, self-control, excellent thermal conductivity Strong thermal shock capability, with far-infrared function, easy to process, green, low-carbon, environmentally friendly, safe and reliable, widely adapt to new energy requirements such as solar, wind, lithium-ion batteries and other new intelligent electric heating components.
  • This embodiment is a rare earth thick film circuit electric heating element for a two-second heat (up to 98 ° C) non-heating and oxygen-increasing electric kettle, and is selected according to the technical requirements of the product drawings.
  • the metal substrate is as shown in the figure above.
  • the oxalic acid anodizing treatment is carried out, and the prepared series rare earth electronic slurry contains encapsulating slurry, PTC thick film circuit thermistor slurry, rare earth electrode slurry, rare earth medium slurry, according to the following process And drawings require the preparation of rare earth thick film circuit controllable electric heating elements:
  • dielectric layer thickness > 65 ⁇ m
  • thermal thick film circuit square film thickness > 15 ⁇ m
  • the rare earth thick film circuit controllable electric heating element meets the following design requirements.
  • the rare earth thick film circuit controllable electric heating element performance parameter of the embodiment of the invention thermal response rate: 150 ° C / sec
  • the thickness of the rare earth dielectric slurry film layer is: ⁇ 65 ⁇ m
  • thixotropic is suitable for screen printing
  • Electrode layer thickness >12 ⁇ m
  • Unit dosage 88cm2 / gram.
  • circuit trace of the thick film circuit heating element on the substrate may be concentric or
  • the substrate of the Kimede spiral-shaped, thick-film circuit heating element may also be a substrate of different shapes and different materials, and any changes made by those skilled in the art without departing from the essence of the invention belong to the present invention.
  • the scope of protection of the invention is only one of the preferred embodiments of the present invention, and the invention may not be limited thereto.
  • the circuit trace of the thick film circuit heating element on the substrate may be concentric or
  • the substrate of the Kimede spiral-shaped, thick-film circuit heating element may also be a substrate of different shapes and different materials, and any changes made by those skilled in the art without departing from the essence of the invention belong to the present invention. The scope of protection of the invention.

Abstract

A PTC rare-earth thick film circuit intelligent electrical heating element and a preparation method. It is characterized in that the intelligent electrical heating element comprises a metal substrate, and a PTC thick film circuit thermistor and a rare-earth thick film resistance circuit which are arranged thereon. The PTC thick film circuit thermistor is superposed on the rare-earth thick film resistance circuit in the form of a thick film circuit or located in the same plane as that of the rare-earth thick film resistance circuit to control the temperature of the thick film circuit electrical heating element to enable the control accuracy and sensitivity to be substantially increased; and can be individually made into a controllable electrical heating element in the form of a thick film circuit. The requirements of startup with both an alternating current and a direct current, uniform gradable self-control of a temperature field, good heat-conducting performance, strong thermal-shock resistance, having a far infrared function, being easy to process, and being capable of wide adaptation to new energies such as solar energy, wind energy, lithium ion battery, etc. can be achieved.

Description

一种PTC稀土厚膜电路智能电热元件及其制备方法  PTC rare earth thick film circuit intelligent electric heating element and preparation method thereof 技术领域Technical field
本发明涉及厚膜电路电热元件技术领域，更具体的是涉及一种PTC厚膜电路热敏电阻自动控制的智能厚膜电路电热元件领域。The invention relates to the technical field of thick film circuit electric heating elements, and more particularly to the field of intelligent thick film circuit electric heating elements for automatic control of PTC thick film circuit thermistors.
背景技术Background technique
随着电子技术的迅猛发展，热敏电阻的应用领域日益增多。PTC厚膜电路热敏电阻即采用厚膜电路制作工艺融合热敏电阻独特控制性质结合厚膜电阻电路而制作的厚膜电路智能电热元件。这一理论概念《PTC厚膜电路可控电热元件》已获得国家专利，早在2004年以前已经提出，并且得以推广应用。PTC热敏电阻厚膜电路，不但具有热敏电阻一般特性，而且由于其材料的组成及工艺的独特性，又使其具有一般热敏电阻所没有的独特优良性能。它可以厚膜电路的形式和厚膜电阻电路叠加或处于同一平面内，来控制厚膜电路电热元件的温度，使控制精度和灵敏度得以大幅度提高。又可单独以厚膜电路形式做成可控电热元件。因而在很多领域尤其在军工领域有着重要的应用。With the rapid development of electronic technology, the application field of thermistors is increasing. The PTC thick film circuit thermistor is a thick film circuit intelligent electric heating element fabricated by a thick film circuit manufacturing process and a unique control property of the thermistor combined with a thick film resistor circuit. This theoretical concept "PTC thick film circuit controllable electric heating element" has obtained national patents, has been proposed as early as 2004, and has been promoted and applied. The PTC thermistor thick film circuit not only has the general characteristics of the thermistor, but also has the unique and excellent performance that the general thermistor does not have due to its material composition and process uniqueness. It can be used in the form of thick film circuit and thick film resistor circuit superimposed or in the same plane to control the temperature of the thick film circuit electric heating element, so that the control precision and sensitivity can be greatly improved. Alternatively, the controllable electric heating element can be formed in the form of a thick film circuit. Therefore, it has important applications in many fields, especially in the military industry.
迄今为止，国内外绝大部分具有（PTC）效应的热敏电阻仍是BaTiO3 陶瓷掺杂制备而成，由于其室温电阻率高，因而在大电流容量下的应用受到了限制，同时由于其材料本身和工艺缺陷，导致功率衰竭等先天问题，目前应用范围受限。正温系数PTC热敏电阻元件因其制作工艺性差，元件灵敏度低，大多在微电子领域使用，难以在电热领域大面积推广。专利号为ZL200410050830.1，创新性地运用“PTC厚膜电路可控电热元件”，圆满地解决了上述问题，得到推广使用。为落实欧盟双指令（ WEEE/ROHS ），本发明在现有技术的基础上，使PTC厚膜电路热敏电阻控制精度和灵敏度以及稀土厚膜电路智能电热元件的电性能、热性能得以大幅度数量级提高。 So far, most of the thermistors with (PTC) effect at home and abroad are still BaTiO3. Ceramic doping is prepared. Due to its high room temperature resistivity, its application under high current capacity is limited. At the same time, due to its inherent defects in the material itself and process defects, power failure and other congenital problems are limited. The positive temperature coefficient PTC thermistor element is poor in manufacturing process and low in component sensitivity, and is mostly used in the field of microelectronics, and it is difficult to promote it in the field of electric heating. Patent No. ZL200410050830.1, innovative use of "PTC thick film circuit controllable electric heating elements", satisfactorily solved the above problems, and was promoted and used. To implement the EU Dual Directive ( WEEE/ROHS The invention improves the electrical precision and sensitivity of the PTC thick film circuit thermistor and the electrical and thermal properties of the rare earth thick film circuit intelligent electric heating element by a large order on the basis of the prior art.
技术问题technical problem
本发明的目的就是为了解决现有技术之不足而提供的一种不仅加热温度场均匀可分级自控、热响应快、功率密度大、设计灵活、结构紧凑、节能环保、安全可靠外，还具有高温远红外功能的PTC稀土厚膜电路智能电热元件。The object of the present invention is to provide a non-heating temperature field uniform grading and self-control, fast thermal response, high power density, flexible design, compact structure, energy saving, environmental protection, safety and reliability, and high temperature in order to solve the deficiencies of the prior art. Far infrared function PTC rare earth thick film circuit intelligent electric heating element.
本发明的另一目的是提供一种PTC稀土厚膜电路智能电热元件的制备方法。Another object of the present invention is to provide a method for preparing a PTC rare earth thick film circuit intelligent electric heating element.
技术解决方案Technical solution
本发明是采用如下技术解决方案来实现上述目的：一种PTC稀土厚膜电路智能电热元件，其特征在于，它包括金属基板及其上设置的PTC厚膜电路热敏电阻和稀土厚膜电阻电路，PTC厚膜电路热敏电阻是以厚膜电路的形式和稀土厚膜电阻电路叠加或处于同一平面内，来控制厚膜电路电热元件的温度，使控制精度和灵敏度得以大幅度提高；又可单独以厚膜电路形式做成可控电热元件。The present invention achieves the above object by using the following technical solution: a PTC rare earth thick film circuit intelligent electric heating element, which comprises a metal substrate and a PTC thick film circuit thermistor and a rare earth thick film resistor circuit disposed thereon PTC thick film circuit thermistor is superimposed or in the same plane with the rare earth thick film resistor circuit in the form of thick film circuit to control the temperature of the thick film circuit electric heating element, so that the control precision and sensitivity can be greatly improved; The controllable electric heating element is separately formed in the form of a thick film circuit.
作为上述方案的进一步说明：所述金属基板为铁素体Cr15\1Cr17\00Cr18Mo2系列不锈钢基板。Further, the metal substrate is a ferrite Cr15\1Cr17\00Cr18Mo2 series stainless steel substrate.
所述PTC厚膜电路热敏电阻由PTC厚膜电路热敏电阻浆料制成，稀土厚膜电阻电路由稀土介质浆料和稀土电极浆料制成。The PTC thick film circuit thermistor is made of a PTC thick film circuit thermistor paste, and the rare earth thick film resistor circuit is made of a rare earth dielectric paste and a rare earth electrode paste.
所述稀土介质浆料由固相成分与有机溶剂载体组成,其重量比为：65 : 35 ~ 85 : 15;固相成分为：Si02 ~ Al203~CaO~B2O3 ~ La2O3稀土氧化物系微晶玻璃,重量配比为：Si02 30 ~ 65 ％、Al203 5 ~ 26 ％、CaO 15~38 ％、 B2O3 2 ~16 ％、La2O3 0 . 3 ~15 ％。Co2O3 0 . 05~ 6 ％；晶核剂为TiO2 1 ~ 10 ％、ZrO : 1 ~10 ％；溶剂载体配比为：丁基卡必醇 66 ~89 ％、柠檬酸三丁醋 5~ 15% 、乙基纤维素 0.5 ~10 ％、氢化蓖麻油 0.1 ~ 5 ％、卵磷脂 0.1~5 ％；稀土氧化物为镧、铈、钕、钷、钆、铒、钪、钇和氧化铽中的一种或多种The rare earth medium slurry is composed of a solid phase component and an organic solvent carrier, and the weight ratio thereof is 65: 35 ~ 85: 15; solid phase composition: SiO 2 ~ Al203 ~ CaO ~ B2O3 ~ La2O3 rare earth oxide glass-ceramic, weight ratio: Si02 30 ~ 65 %, Al203 5 ~ 26%, CaO 15~38%, B2O3 2~16%, La2O3 0. 3 ~15%. Co2O3 0 . 05~ 6 %; crystal nucleating agent is TiO2 1 ~ 10 %, ZrO: 1 ~ 10%; solvent carrier ratio: butyl carbitol 66 ~ 89%, citric acid tributyl vinegar 5 ~ 15%, ethyl cellulose 0.5 ~ 10%, hydrogenated castor oil 0.1 ~ 5 %, lecithin 0.1~5 %; rare earth oxides are one or more of lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium and cerium oxide
所述PTC厚膜电路热敏电阻浆料，由二氧化钌、氧化铜、氧化钇复合粉和微晶玻璃粉及有机载体组成，二氧化钌、氧化铜、氧化钇与有机载体的重量比为 65 ~85 : 35 ~15；二氧化钌、氧化铜、氧化钇复合粉与微晶玻璃粉组成固相成分，固相成分中二氧化钌、氧化铜、氧化钇复合粉与微晶玻璃的重量比为 75 ~ 55 : 25~ 45 ；二氧化钌、氧化铜、氧化钇复合粉中的二氧化钌、氧化铜、氧化钇粉的重量比为：75 ~59：15~40.5 : 10 ~ 0.5，二氧化钌、氧化铜、氧化钇复合粉的粒径为：0.30--1.0μm；微晶玻璃粉为：CaO~SiO2 ~ A12O3 ~ B2O3 ~ Bi2O3 ~ La2 03 的稀土氧化物系微晶玻璃；各氧化物重量比：SiO2 20 ~ 60 ％、A12O3 5 ~ 35 ％、CaO 10 ~ 350%、Bi2O31O ~ 30 ％、B203 1~ 10 ％、 La2O3 O.3 ~8 ％；晶核剂为：TiO21~8 ％、ZrO21~10 %；有机载体各组分的重量比：松油醇 68 ~ 78 ％、柠檬酸三丁醋 2 ~ 18 ％、乙基纤维素 0 .4 ~ 9％、硝基纤维素 0 .4~ 9％、氢化蓖麻油 0 .1 ~ 6% 、卵磷脂 0 .1 ~ 6％；上述稀土氧化物为；镧、铈、钕、钷、钆、铒、钪、钇和氧化铽中的一种或几种。The PTC thick film circuit thermistor slurry is composed of cerium oxide, copper oxide, cerium oxide composite powder, glass ceramic powder and an organic carrier, and the weight ratio of cerium oxide, copper oxide, cerium oxide and organic carrier is 65 ~ 85 : 35 ~ 15; solid phase composition of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder, the weight of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic in solid phase composition The ratio is 75 ~ 55 : 25~ 45 ; The weight ratio of cerium oxide, copper oxide and cerium oxide powder in cerium oxide, copper oxide and cerium oxide composite powder is: 75 ~ 59: 15 ~ 40.5 : 10 ~ The particle size of 0.5, cerium oxide, copper oxide and cerium oxide composite powder is 0.30--1.0μm; the glass-ceramic powder is: CaO~SiO2 ~ A12O3 ~ B2O3 ~ Bi2O3 ~ Rare earth oxide-based glass-ceramics of La2 03; weight ratio of each oxide: SiO2 20 ~ 60 %, A12O3 5 ~ 35 %, CaO 10 ~ 350%, Bi2O31O ~ 30 %, B203 1~ 10 %, La2O3 O.3 ~ 8%; nucleating agent: TiO21~8 %, ZrO21~10%; weight ratio of each component of organic carrier: terpineol 68 ~ 78 %, 2 ~ 18 % citric acid citrate, 0.4 ~ 9% ethyl cellulose, 0.4 ~ 9% nitrocellulose, hydrogenated castor oil 0.1 to 6%, lecithin 0 .1 ~ 6%; the above rare earth oxides are one or more of cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum and cerium oxide.
所述稀土电极浆料由固相成分与有机溶剂载体组成，重量比为 70 ~ 90：30~10 ；固相成分包括银钯钇复合粉与微晶玻璃粉，银钯钇复合粉与微晶玻璃粉重量比为 99.4 ~0.6：0.6~6；银钯钇复合粉重量比为： 0.6 ~10 ：99~82：0.4 ~ 8；粒径为：3μm；有机溶剂载体重量比为：松油醇 60 ~ 98 ％、柠檬酸三丁醋 10~30 ％、乙基纤维素 2 ~10 ％、硝基纤维素 1~5 ％、氢化蓖麻油 0.1~5 ％、卵磷脂 0.1~5 ％；微晶玻璃为SiO2 ~A12O3~CaO~B203~Bi2O3 ~La2O3 的稀土、氧化物系微晶玻璃，各氧化物的成分重量比为：SiO2 20~60 ％、A12O35~35 ％、CaO 10~35 ％、B2031~15 ％、La2O3 0. 3~15 ％、 Bi2O3 10 ~30 ％。晶核剂为：Ti021~10 ％、ZrO21~10 ％；稀土氧化物为镧、铈、钕、钷、钆、铒、钪、钇和氧化铽中的一种或几种。The rare earth electrode slurry is composed of a solid phase component and an organic solvent carrier, and the weight ratio is 70 to 90:30~10. The solid phase composition includes silver-palladium-ruthenium composite powder and glass-ceramic powder, the weight ratio of silver-palladium-iridium composite powder to glass-ceramic powder is 99.4 ~ 0.6: 0.6~6; the weight ratio of silver-palladium-ruthenium composite powder is: 0.6 ~ 10. : 99~82: 0.4 ~ 8; particle size: 3μm; organic solvent carrier weight ratio: terpineol 60 ~ 98%, citric acid tributyl vinegar 10 ~ 30%, ethyl cellulose 2 ~ 10 %, nitrocellulose 1~5 %, hydrogenated castor oil 0.1~5 %, lecithin 0.1~5 %; glass ceramics SiO2 ~A12O3~CaO~B203~Bi2O3 ~La2O3 Rare earth, oxide-based glass-ceramics, the weight ratio of each oxide is: SiO2 20~60%, A12O35~35 %, CaO 10~35 %, B2031~15%, La2O3 0. 3~15%, Bi2O3 10~30%. The nucleating agent is: Ti021~10%, ZrO21~10 %; rare earth oxides are one or more of cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum and cerium oxide.
一种PTC稀土厚膜电路智能电热元件的制备方法，其特征在于，它是将金属基板、稀土介质浆料、PTC厚膜电路热敏电阻浆料、电极浆料、封装浆料按工艺流程制备成PTC稀土厚膜电路电热元件，其工艺流程如下：Method for preparing PTC rare earth thick film circuit intelligent electric heating element, characterized in that it is prepared by metal substrate, rare earth medium slurry, PTC thick film circuit thermistor paste, electrode paste and package slurry according to the process flow The process of forming a PTC rare earth thick film circuit electric heating element is as follows:
A、金属基板→CAD\光绘制版→G网印刷→烘干烧结→检验包装,其中介质层厚度＞65μm，PTC厚膜电路热敏电阻膜厚度＞15μm ；A, metal substrate → CAD \ light drawing version → G network printing → drying and sintering → inspection packaging, wherein the thickness of the dielectric layer is > 65 μm, the thickness of the PTC thick film circuit thermistor film > 15 μm;
B、烧结，升、降温速率:每分钟50-70℃，峰值温度：800-950℃。B, sintering, rising and cooling rate: 50-70 ° C per minute, peak temperature: 800-950 ° C.
所述稀土介质浆料的制备工艺，它包括如下步骤： The preparation process of the rare earth medium slurry comprises the following steps:
① 制备稀土微晶玻璃粉：按重量配比将各氧化物，晶核剂，经混合均匀后熔炼，熔炼温度为：1100 ~1450 ℃。保温 90~180 分钟后，出炉水淬，得到玻璃微渣；球磨玻璃微渣，制备出粒径1~3 微米的微晶玻璃粉；1 Preparation of rare earth glass-ceramic powder: each oxide and crystal nucleating agent are mixed and smelted according to the weight ratio, and the melting temperature is: 1100 ~1450 °C. After 90-180 minutes of heat preservation, the water is quenched to obtain glass micro-slag; the glass micro-slag is ball-milled to prepare a glass-ceramic powder having a particle diameter of 1 to 3 μm;
② 配制有机溶剂载体：将各化工原料按配比混合均匀，在80 ~100 ℃ 的水中溶浴数小时；调整乙基纤维素含量，将有机载体的粘度调整在150 ~ 28OmPaS的范围内； 2 Preparation of organic solvent carrier: Mix all chemical raw materials according to the ratio, at 80 ~ 100 °C The bath in water for several hours; adjust the ethyl cellulose content, adjust the viscosity of the organic carrier in the range of 150 ~ 28OmPaS;
③ 介质浆料调制：将固相成分与有机溶剂载体的重量比按 65 : 85~ 35 ：15；经R-S01型双向旋转＋振动机械，混合、搅拌、分散一小时后，三棍轧制得到成品，粘度值为150 ~ 200PaS / RPM。3 medium slurry preparation: the weight ratio of the solid phase component to the organic solvent carrier is 65: 85~35 :15; After R-S01 bidirectional rotation + vibration machine, after mixing, stirring and dispersing for one hour, the three sticks are rolled to obtain the finished product, and the viscosity value is 150 ~ 200PaS / RPM.
所述PTC厚膜电路热敏电阻浆料的制备工艺，它包括如下步骤：The preparation process of the PTC thick film circuit thermistor paste comprises the following steps:
①微晶玻璃粉制备：按上述氧化物、晶核剂配比在三维混料机中混合均匀后，熔炉熔炼，温度为：1100 ~1450℃，保温1 ~ 3小时后，将玻璃熔液水淬，得到微渣，经球磨获得粒径1.0~3.0 微米的玻璃微粉；1 Preparation of glass-ceramic powder: After mixing the above oxide and crystal nucleating agent in a three-dimensional mixer, the furnace is smelted at a temperature of 1100. ~1450 ° C, after 1 ~ 3 hours of heat preservation, the glass melt is water quenched to obtain fine slag, and the glass micropowder having a particle diameter of 1.0 to 3.0 μm is obtained by ball milling;
②二氧化钌、氧化铜、氧化钇复合粉制备：二氧化钌、氧化铜、氧化钇重量配比为：75 ~ 59 : 15 ~ 40.5 : 10 ~ 0.5，经三维搅拌、混合均匀、球磨得到复合粉，粒径均为：0.30~1.0μm ；2 Preparation of cerium oxide, copper oxide and cerium oxide composite powder: weight ratio of cerium oxide, copper oxide and cerium oxide: 75 ~ 59 : 15 ~ 40.5 : 10 ~ 0.5, after three-dimensional stirring, mixing and uniform, ball milling to obtain composite powder, the particle size is: 0.30~1.0μm;
③有机载体制备：将上述化工原料按比例，经高效搅拌、混合均匀，在 80 ~ 100 ℃ 的水中溶解数小时，调整增稠剂含量，将有机载体溶剂的粘度调整在 180~280mPaS 的范围内即可；3 Preparation of organic carrier: The above chemical raw materials are proportioned, highly efficiently stirred and uniformly mixed, at 80 ~ 100 °C After being dissolved in water for several hours, the content of the thickener is adjusted, and the viscosity of the organic carrier solvent is adjusted within a range of 180 to 280 mPaS;
④PTC厚膜电路热敏电阻浆料综合调制：固相成分由二氧化钌、氧化铜、氧化钇复合粉和微晶玻璃粉组成,重量比为： 75~ 55 : 25 ~ 45；固相成分和有机载体重量比：65~85 : 35 ~15，将固相粉体、有机载体溶剂经R-S01型双向旋转＋振动机械，搅拌、混合均匀后，进行三辊反复轧制得到成品，粘度值为150 ~ 200PaS / RPM 。4PTC thick film circuit thermistor slurry comprehensive modulation: solid phase composition consists of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder, the weight ratio is: 75~ 55 : 25 ~ 45; solid phase composition and organic carrier weight ratio: 65~85: 35 ~15, the solid phase powder and the organic carrier solvent are subjected to two-way rotation + vibration machine of R-S01 type, stirred and mixed uniformly, and then subjected to three-roll repeated rolling to obtain a finished product, and the viscosity value is 150 ~ 200 PaS / RPM. .
所述稀土电极浆料的制备工艺，它包括如下步骤：The preparation process of the rare earth electrode slurry comprises the following steps:
①微晶玻璃粉制备：按原料重量比将各氧化物、晶核剂混合均匀后熔炼，温度为：1100 ~1450℃ ，保温1~3 小时，水淬得到玻璃微渣，球磨获得3 微米玻璃微粉；1 Preparation of glass-ceramic powder: The oxides and crystal nucleating agents are uniformly mixed according to the weight ratio of raw materials, and then smelted at a temperature of 1100 ~ 1450 °C. , heat preservation for 1-3 hours, water quenching to obtain glass micro slag, ball milling to obtain 3 micron glass micropowder;
②制备银钯钇复合粉；银钯钇复合粉，粒径为： 3μm ，在三维混料机中按重量比为；99 ~82：0.6 ~10：0.4~8 调制混合均匀； 2 Preparation of silver-palladium-ruthenium composite powder; silver-palladium-ruthenium composite powder, particle size: 3μm, in the three-dimensional mixer by weight ratio; 99 ~ 82: 0.6 ~10:0.4~8 Modulation and mixing evenly;
③有机载体制备；按原料重量比混合后在 80~100℃水中溶解数小时，调整乙基纤维素含量，粘度控制在150~280mPas 范围； 3 organic carrier preparation; mixed according to the weight ratio of raw materials Dissolve in water at 80~100 °C for several hours, adjust the content of ethyl cellulose, and control the viscosity in the range of 150~280mPas;
④制备稀土电极浆料：按比例将微晶玻璃粉、银钯钇复合粉、有机溶剂载体置于三维混料机中搅拌混合均匀后入三辊轧机反复轧制，得到稀土电极浆料，粘度值为150 ~200PaS / RPM。4 Preparation of rare earth electrode slurry: The microcrystalline glass powder, the silver palladium ruthenium composite powder and the organic solvent carrier are placed in a three-dimensional mixing machine in proportion, stirred and uniformly mixed, and then repeatedly rolled into a three-roll mill to obtain a rare earth electrode slurry, viscosity. Value is 150 ~200PaS / RPM.
有益效果Beneficial effect
本发明采用上述技术解决方案所能达到的有益效果是：The beneficial effects that the present invention can achieve by using the above technical solutions are:
1、本发明采用将金属基板、系列稀土电子浆料、系列稀土电子浆料制备在金属基板上，上述稀土电子浆料是专业为电热领域设计的，同时还公开了介质浆料、电极浆料、PTC厚膜电路热敏电阻浆料的配方,是对现有技术的进一步升级和提高,除加热温度场均匀可分级自控、热响应快、功率密度大、设计灵活、结构紧凑、节能环保、安全可靠外，还具有高温远红外功能，该智能电热元件温度适应范围广：25--400℃. 高低压（3—380V）、交直流：Ac、Dc均能启动使用，广泛适用于太阳能、风能、锂离子电池等各类新能源领域。1. The invention adopts a metal substrate, a series of rare earth electronic pastes and a series of rare earth electronic pastes prepared on a metal substrate. The above rare earth electronic paste is specially designed for the electric heating field, and also discloses a dielectric slurry and an electrode slurry. The formulation of PTC thick film circuit thermistor slurry is a further upgrade and improvement of the prior art, except that the heating temperature field is uniform and gradable, the thermal response is fast, the power density is large, the design is flexible, the structure is compact, and the energy saving and environmental protection are Safe and reliable, it also has high-temperature far-infrared function. The temperature of the intelligent electric heating element is wide: 25-400 °C. High and low voltage (3-380V), AC and DC: Ac, Dc can be used, widely used in solar energy, wind energy, lithium-ion batteries and other new energy fields.
2、本发明采用上述技术方案效果明显，尤其是各功能相配方均含有稀土元素。由于加入了稀土金属，浆料的相容性、湿润性、热性能、电性能、工艺性、适应性有显著改进提高，稀土厚膜电路电热元件由此得名，基于金属基板的稀土厚膜电路智能电热元件成功的开发、应用有开拓性的创新意义。2. The invention adopts the above technical schemes, and the effect is obvious, in particular, each functional phase formula contains rare earth elements. Due to the addition of rare earth metals, the compatibility, wettability, thermal properties, electrical properties, processability and adaptability of the slurry are significantly improved. The rare earth thick film circuit electric heating element is named after the rare earth thick film based on the metal substrate. The successful development and application of circuit intelligent electric heating elements has pioneering and innovative significance.
附图说明DRAWINGS
图1为本发明的PTC稀土厚膜电路智能电热元件结构示意图。1 is a schematic structural view of a PTC rare earth thick film circuit intelligent electric heating element according to the present invention.
附图标记说明：1、金属基板 2、PTC厚膜电路热敏电阻 3、稀土厚膜电阻电路。DESCRIPTION OF REFERENCE NUMERALS: 1. Metal substrate 2. PTC thick film circuit thermistor 3. Rare earth thick film resistor circuit.
本发明的最佳实施方式BEST MODE FOR CARRYING OUT THE INVENTION
如图1所示，本发明一种PTC稀土厚膜电路智能电热元件，它包括金属基板1及其上设置的PTC厚膜电路热敏电阻2和稀土厚膜电阻电路3，PTC厚膜电路热敏电阻是以厚膜电路的形式和稀土厚膜电阻电路叠加或处于同一平面内，来控制厚膜电路电热元件的温度，使控制精度和灵敏度得以大幅度提高；又可单独以厚膜电路形式做成可控电热元件 ;金属基板为铁素体Cr15、 1Cr17或 00Cr18Mo2系列不锈钢基板 。 As shown in FIG. 1 , the invention discloses a PTC rare earth thick film circuit intelligent electric heating element, which comprises a metal substrate 1 and a PTC thick film circuit thermistor 2 and a rare earth thick film resistor circuit 3 disposed thereon, and a PTC thick film circuit heat. The varistor is in the form of a thick film circuit and the rare earth thick film resistor circuit is superimposed or in the same plane to control the temperature of the thick film circuit electric heating element, so that the control precision and sensitivity can be greatly improved; and the thick film circuit can be separately used. Controllable electric heating element The metal substrate is a ferritic Cr15, 1Cr17 or 00Cr18Mo2 series stainless steel substrate.
PTC稀土厚膜电路智能电热元件是由金属基板、系列稀土电子浆料、系列稀土电子浆料制备在金属基板上，经烧结工艺制备而成。系列稀土电子浆料包括稀土介质浆料、稀土电极浆料，系列电子浆料均由功能相和有机载体组成。系列稀土电子浆料还包括PTC厚膜电路热敏电阻浆料，上述稀土电子浆料是专业用于电热领域的。所述系列稀土电子浆料是指系列介质浆料、PTC厚膜电路热敏电阻浆料、电极浆料、包封浆料等掺杂稀土氧化物镧、铈、钕、钷、钆、铒、钪、钇和氧化铽 等化学元素，根据不同温度、不同功率、不同用途的电子浆料对方阻、温度系数、电性能、热性能及远红外功能的要求，按实验数理模式添加不同种类、不同份额的稀土氧化物，来增添或更换配方成分组成要求中的一项或多项调配而成。PTC rare earth thick film circuit intelligent electric heating element is prepared by metal substrate, series rare earth electronic paste, series rare earth electronic paste on metal substrate and sintered process. The series rare earth electronic paste comprises a rare earth medium slurry and a rare earth electrode slurry, and the series of electronic pastes are composed of a functional phase and an organic carrier. The series rare earth electronic paste also includes a PTC thick film circuit thermistor paste, and the above rare earth electronic paste is specialized in the field of electric heating. The series of rare earth electronic pastes refers to a series of dielectric pastes, PTC thick film circuit thermistor pastes, electrode pastes, encapsulating pastes and the like doped rare earth oxides lanthanum, cerium, lanthanum, cerium, lanthanum, cerium,钪, 钇 and 铽 And other chemical elements, according to different temperature, different power, different uses of electronic paste resistance, temperature coefficient, electrical properties, thermal properties and far-infrared function requirements, according to the experimental mathematical model to add different types, different proportions of rare earth oxides, To add or replace one or more of the ingredients in the formula.
一、系列稀土电子浆料的制备方法:First, the preparation method of series rare earth electronic paste:
1、稀土介质浆料的制备:1. Preparation of rare earth medium slurry:
稀土介质浆料由固相成分与有机溶剂载体组成，其重量比为：65 : 35 ~ 85 : 15 ；固相成分为：Si02 ~ Al203~CaO~B2O3 ~ La2O3等稀土氧化物系微晶玻璃，重量配比为：Si02 30 ~ 65 ％、Al203 5 ~ 26 ％、CaO 15~38 ％、 B2O3 2 ~16 ％、La2O3 0 . 3 ~15 ％。Co2O3 0.05~ 6 ％。晶核剂为TiO2 1 ~ 10 ％、ZrO : 1 ~10 ％。溶剂载体配比为：丁基卡必醇 66 ~89 ％、柠檬酸三丁醋 5~ 15% 、乙基纤维素 0.5 ~10 ％、氢化蓖麻油 0.1 ~ 5 ％、卵磷脂 0.1~5 ％。稀土氧化物为:镧、铈、钕、钷、钆、铒、钪、钇和氧化铽。稀土氧化物可根据不同温度、不同用途的介质浆料对热性能、化学性能、机械性能及远红外功能的要求，按照试验数理模式添加不同种类、不同份额的稀土氧化物。来增添或更换微晶玻璃成分组成要求的一项或多项。 The rare earth medium slurry is composed of a solid phase component and an organic solvent carrier, and the weight ratio thereof is 65:35 ~ 85 : 15 The solid phase composition is: SiO2 - Al203~CaO~B2O3 ~ La2O3 and other rare earth oxide-based glass-ceramics, the weight ratio is: Si02 30 ~ 65 %, Al203 5 ~ 26%, CaO 15~38%, B2O3 2~16%, La2O3 0. 3 ~15%. Co2O3 0.05~ 6 %. The nucleating agent is TiO2 1 ~ 10%, ZrO: 1 ~ 10%. The solvent carrier ratio is: butyl carbitol 66 ~ 89%, citric acid tributyl vinegar 5 ~ 15%, ethyl cellulose 0.5 ~ 10%, hydrogenated castor oil 0.1 ~ 5 %, lecithin 0.1~5 %. The rare earth oxides are: antimony, bismuth, antimony, bismuth, antimony, bismuth, antimony, antimony and antimony oxide. According to the requirements of thermal, chemical, mechanical and far-infrared functions of the dielectric pastes of different temperatures and different uses, the rare earth oxides may be added with different types and different proportions of rare earth oxides according to the experimental mathematical model. To add or replace one or more of the requirements for the composition of the glass-ceramics.
稀土介质浆料的制备工艺步骤：  Preparation process of rare earth medium slurry:
① 制备稀土微晶玻璃粉：按重量配比将各氧化物，晶核剂，经混合均匀后熔炼。熔炼温度为：1 100 ~1450 ℃。保温 90 ~180 分钟后，出炉水淬，得到玻璃微渣；球磨玻璃微渣，制备出粒径3 微米的微晶玻璃粉；1 Preparation of rare earth glass-ceramic powder: Each oxide and crystal nucleating agent are uniformly mixed and smelted according to the weight ratio. Melting temperature is: 1 100 ~1450 °C. After holding for 90-180 minutes, the water is quenched to obtain glass micro-slag; the glass micro-slag is ball-milled to prepare a glass-ceramic powder with a particle size of 3 microns;
② 配制有机溶剂载体：将各化工原料按配比混合均匀：在80 ~100 ℃ 的水中溶浴数小时。调整乙基纤维素含量，将有机载体的粘度调整在150 ~ 28OmPaS的范围内； 2 Preparation of organic solvent carrier: Mix all chemical raw materials according to the ratio: 80 ~ 100 °C The bath in water is for several hours. Adjusting the ethyl cellulose content, adjusting the viscosity of the organic carrier in the range of 150 ~ 28OmPaS;
③ 介质浆料调制：将固相成分与有机溶剂载体的重量比按 65 : 85 ~ 35 ：15;经R-S01型双向旋转＋振动机械，高效混合、搅拌、分散一小时后，三棍轧制得到成品。粘度值为150 ~ 200PaS / RPM。 3 medium slurry preparation: the weight ratio of the solid phase component to the organic solvent carrier is 65: 85 ~ 35 :15; After R-S01 two-way rotation + vibration machine, after mixing, stirring and dispersing for one hour, the three sticks are rolled to obtain the finished product. The viscosity value is 150 ~ 200PaS / RPM.
2、PTC厚膜电路热敏电阻浆料的制备2. Preparation of PTC thick film circuit thermistor paste
PTC厚膜电路热敏电阻浆料，由二氧化钌、氧化铜、氧化钇复合粉和微晶玻璃粉及有机载体组成，二氧化钌、氧化铜、氧化钇与有机载体的重量比为 65 ~85 : 35 ~15 ；二氧化钌、氧化铜、氧化钇复合粉与微晶玻璃粉组成固相成分，固相成分中二氧化钌、氧化铜、氧化钇复合粉与微晶玻璃的重量比为 75 ~ 55 : 25~ 45 ；二氧化钌、氧化铜、氧化钇复合粉中的二氧化钌、氧化铜、氧化钇粉的重量比为：75 ~59：15~40.5 : 10 ~ 0.5，二氧化钌、氧化铜、氧化钇复合粉的粒径为：0.30--1.0μm ；微晶玻璃粉为：CaO~SiO2 ~ A12O3 ~ B2O3 ~ Bi2O3 ~ La2 03 等稀土氧化物系微晶玻璃；各氧化物重量比：SiO2 20 ~ 60 ％、A12O3 5 ~ 35 ％、CaO 10 ~ 350%、Bi2O31O ~ 30 ％、B203 1~ 10 ％、 La2O3 O.3 ~8 ％。晶核剂为：TiO21~8 ％、ZrO21~10 % ；有机载体各组分的重量比：松油醇 68 ~ 78 ％、柠檬酸三丁醋 2 ~ 18 ％、乙基纤维素 0 .4 ~ 9％、硝基纤维素 0 .4~ 9％、氢化蓖麻油 0 .1 ~ 6% 、卵磷脂 0 .1 ~ 6％。PTC thick film circuit thermistor paste consists of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder and organic carrier. The weight ratio of cerium oxide, copper oxide, cerium oxide and organic carrier is 65. ~85 : 35 ~15 ; the solid phase composition of cerium oxide, copper oxide, cerium oxide composite powder and glass ceramic powder, the weight ratio of cerium oxide, copper oxide, cerium oxide composite powder and glass ceramic in the solid phase composition For 75 ~ 55 : 25~ 45 ; The weight ratio of cerium oxide, copper oxide and cerium oxide powder in cerium oxide, copper oxide and cerium oxide composite powder is: 75 ~ 59: 15 ~ 40.5 : 10 ~ The particle size of 0.5, cerium oxide, copper oxide and cerium oxide composite powder is 0.30--1.0μm; the glass ceramic powder is: CaO~SiO2 ~ A12O3 ~ B2O3 ~ Bi2O3 ~ Rare earth oxide-based glass-ceramics such as La2 03; weight ratio of each oxide: SiO2 20 ~ 60 %, A12O3 5 ~ 35 %, CaO 10 ~ 350%, Bi2O31O ~ 30 %, B203 1~ 10 %, La2O3 O.3 ~ 8%. The nucleating agent is: TiO21~8 %, ZrO21~10%; the weight ratio of each component of the organic carrier: terpineol 68 ~ 78 %, 2 ~ 18 % citric acid citrate, 0.4 ~ 9% ethyl cellulose, 0.4 ~ 9% nitrocellulose, hydrogenated castor oil 0.1 to 6%, lecithin 0 .1 ~ 6%.
上述稀土氧化物为；镧、铈、钕、钷、钆、铒、钪、钇和氧化铽。稀土氧化物可根据不同功率、不同温度、不同用途的PTC厚膜电路热敏电阻浆料对方阻、温度系数、热性能、及远红外功能的要求，按照试验数理模式添加不同种类、不同份额的稀土氧化物。来增添或更换成分组成要求的一项或多项。The above rare earth oxides are lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium and cerium oxide. Rare earth oxides can be added according to different power, temperature, and different applications of PTC thick film circuit thermistor paste resistance, temperature coefficient, thermal performance, and far infrared function, according to the experimental mathematical model to add different types, different proportions Rare earth oxides. To add or replace one or more of the ingredient composition requirements.
PTC厚膜电路热敏电阻浆料的制备，包括如下工艺步骤：The preparation of the PTC thick film circuit thermistor paste includes the following process steps:
①微晶玻璃粉制备：按上述氧化物、晶核剂配比在三维混料机中混合均匀后，熔炉熔炼，温度为：1100 ~ 1450℃，保温1 ~ 3小时后，将玻璃熔液水淬，得到微渣，以蒸镏水为介质球磨4-6小时，经球磨获得粒径3-5μm 微米的玻璃微粉；1 Preparation of glass-ceramic powder: According to the above oxide and crystal nucleating agent ratio, the mixture is uniformly mixed in a three-dimensional mixer, and the furnace is smelted at a temperature of 1100 ~ After heat preservation at 1450 ° C for 1 ~ 3 hours, the glass melt is water quenched to obtain micro slag, which is ball milled for 4-6 hours with steamed water as a medium, and obtained by using ball milling to obtain a glass micropowder having a particle size of 3-5 μm micron;
②二氧化钌、氧化铜、氧化钇复合粉制备：二氧化钌、氧化铜、氧化钇重量配比为：75 ~ 59 : 15 ~ 40.5 : 10 ~ 0.5，经三维搅拌、混合均匀得到复合粉；将复合粉以乙醇为介质球磨9~ 18小时，粒径控制为：0.30--1.0μm ；2 Preparation of cerium oxide, copper oxide and cerium oxide composite powder: the weight ratio of cerium oxide, copper oxide and cerium oxide is: 75 ~ 59 : 15 ~ 40.5 : 10 ~ 0.5, the composite powder is obtained by three-dimensional stirring and mixing; the composite powder is ball milled for 9 to 18 hours with ethanol as the medium, and the particle size is controlled to be 0.30--1.0 μm;
③有机载体制备：将上述化工原料按比例，经高效搅拌、混合均匀，在 80 ~ 100 ℃ 的水中溶解数小时，三维搅拌直至乙基纤维素完全溶解。按比例加入表面活性剂，调整增稠剂含量，将有机载体溶剂的粘度调整在 180~280mPaS 的范围内即可；3 Preparation of organic carrier: The above chemical raw materials are proportioned, highly efficiently stirred and uniformly mixed, at 80 ~ 100 °C The water is dissolved for several hours and stirred in three dimensions until the ethyl cellulose is completely dissolved. The surfactant is added in proportion, the content of the thickener is adjusted, and the viscosity of the organic carrier solvent is adjusted to 180-280 mPaS. Within the scope of;
④PTC厚膜电路热敏电阻浆料综合调制：固相成分由二氧化钌、氧化铜、氧化钇复合粉和微晶玻璃粉组成，重量比为： 75~ 55 : 25 ~ 45;固相成分和有机载体重量比：65~85 : 35 ~ 15,将固相粉体、有机载体溶剂经R-S01型双向旋转＋振动机械，搅拌混合均匀，进行三辊反复轧制得到PTC厚膜电路热敏电阻浆料。粘度值为150 ~ 200PaS / RPM。4PTC thick film circuit thermistor slurry comprehensive modulation: solid phase composition consists of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder, the weight ratio is: 75~ 55 : 25 ~ 45; solid phase composition and organic carrier weight ratio: 65~85: 35 ~ 15. The solid phase powder and the organic carrier solvent are subjected to R-S01 bidirectional rotation + vibration machine, stirred and uniformly mixed, and three-roll repeated rolling is performed to obtain a PTC thick film circuit thermistor slurry. Viscosity value is 150 ~ 200PaS / RPM.
3、稀土电极浆料的制备，3. Preparation of rare earth electrode slurry,
稀土电极浆料由固相成分与有机溶剂载体组成，重量比为 70 ~ 90：30~10 ；固相成分包括银钯钇复合粉与微晶玻璃粉，银钯钇复合粉与微晶玻璃粉重量比为 99.4 ~0.6：0.6~6；银钯钇复合粉重量比为： 0.6 ~10：99~82：0.4 ~ 8；粒径为：3μm。有机溶剂载体重量比为：松油醇 60 ~ 98 ％、柠檬酸三丁醋 10~30 ％、乙基纤维素 2 ~10 ％、硝基纤维素 1~5 ％、氢化蓖麻油 0.1~5 ％、卵磷脂 0.1~5 ％。微晶玻璃为SiO2 ~A12O3~CaO~B203~Bi2O3 ~La2O3的稀土、氧化物系微晶玻璃，各氧化物的成分重量比为：SiO2 20~60 ％、A12O35~35 ％、CaO 10~35 ％、B2031~15 ％、La2O3 0. 3~15 ％、 Bi2O3 10 ~30 ％。晶核剂为：Ti021~10 ％、ZrO21~10 ％。 The rare earth electrode slurry is composed of a solid phase component and an organic solvent carrier, and the weight ratio is 70 to 90:30~10. The solid phase composition includes silver-palladium-ruthenium composite powder and glass-ceramic powder, the weight ratio of silver-palladium-iridium composite powder to glass-ceramic powder is 99.4 ~ 0.6: 0.6~6; the weight ratio of silver-palladium-ruthenium composite powder is: 0.6 ~10:99~82:0.4 ~ 8; particle size: 3μm. The weight ratio of the organic solvent carrier is: terpineol 60 ~ 98%, tributyl citrate 10~30%, ethyl cellulose 2 ~ 10 %, nitrocellulose 1~5 %, hydrogenated castor oil 0.1~5 %, lecithin 0.1~5 %. Glass-ceramics are SiO2 ~ A12O3 ~ CaO ~ B203 ~ Bi2O3 ~La2O3 rare earth, oxide-based glass-ceramics, the weight ratio of each oxide is: SiO2 20~60%, A12O35~35 %, CaO 10~35 %, B2031~15 %, La2O3 0. 3~15%, Bi2O3 10~30%. The crystal nucleating agent is: Ti021~10%, ZrO21~10%.
上述稀土氧化物为:镧、铈、钕、钷、钆、铒、钪、钇和氧化铽。稀土氧化物可根据不同温度的电极浆料对导电性能、热性能、化学性能的要求,按照试验数理模式添加不同种类、不同份额的稀土氧化物。来增添或更换成分组成要求的一项或多项。 The above rare earth oxides are: antimony, bismuth, antimony, bismuth, antimony, bismuth, antimony, antimony and antimony oxide. Rare earth oxides can be added according to the requirements of electrical conductivity, thermal properties and chemical properties of electrode pastes at different temperatures, and different types and different proportions of rare earth oxides are added according to the experimental mathematical model. To add or replace one or more of the ingredient composition requirements.
稀土电极浆料的制备，包括如下工艺步骤：The preparation of the rare earth electrode slurry includes the following process steps:
①微晶玻璃粉制备：按原料重量比将氧化物、晶核剂混合均匀后熔炼，温度为：1100 ~1450℃ ，保温1~3 小时，水淬得到玻璃微渣，球磨获得3 微米玻璃微粉；1 Preparation of glass-ceramic powder: The oxide and crystal nucleating agent are uniformly mixed according to the weight ratio of raw materials, and the temperature is: 1100 ~ 1450 °C , heat preservation for 1-3 hours, water quenching to obtain glass micro slag, ball milling to obtain 3 micron glass micropowder;
②制备银钯钇复合粉；银钯钇复合粉，粒径为： 3μm ，在三维混料机中按重量比为；99 ~82：0.6 ~10：0.4~8 调制混合均匀； 2 Preparation of silver-palladium-ruthenium composite powder; silver-palladium-ruthenium composite powder, particle size: 3μm, in the three-dimensional mixer by weight ratio; 99 ~ 82: 0.6 ~10:0.4~8 Modulation and mixing evenly;
③有机载体制备；按原料重量比混合后在 80~100℃水中溶解数小时，调整乙基纤维素含量，粘度控制在150~280mPas 范围； 3 organic carrier preparation; mixed according to the weight ratio of raw materials Dissolve in water at 80~100 °C for several hours, adjust the content of ethyl cellulose, and control the viscosity in the range of 150~280mPas;
④制备稀土电极浆料：按比例将微晶玻璃粉、银钯钇复合粉、有机溶剂载体置于三维混料机中搅拌混合均匀后入三辊轧机反复轧制，得到稀土电极浆料，粘度：150 ~200PaS / RPM。4 Preparation of rare earth electrode slurry: The microcrystalline glass powder, the silver palladium ruthenium composite powder and the organic solvent carrier are placed in a three-dimensional mixing machine in proportion, stirred and uniformly mixed, and then repeatedly rolled into a three-roll mill to obtain a rare earth electrode slurry, viscosity. :150 ~200PaS / RPM.
二、金属基板基PTC稀土厚膜电路智能电热元件的制备Second, the preparation of metal substrate based PTC rare earth thick film circuit intelligent electric heating element
将备用金属基板、稀土介质浆料、PTC厚膜电路热敏电阻浆料、电极浆料、封装浆料按工艺流程制备稀土厚膜电路电热元件。浆料放置过久，使用前需进行匀浆处理。 A rare earth thick film electric heating element is prepared according to a process flow by using a spare metal substrate, a rare earth medium slurry, a PTC thick film circuit thermistor paste, an electrode slurry, and a package slurry. The slurry is left for too long and needs to be homogenized before use.
工艺流程：Process flow:
A、金属基板→光绘制版→钢网印刷→烘干烧结→检验包装A, metal substrate → light drawing plate → steel mesh printing → drying and sintering → inspection packaging
要求介质层厚度＞65μm ，热敏厚膜电路方阻膜厚度＞15μm ；The thickness of the dielectric layer is required to be >65 μm, and the thickness of the thermal thick film circuit is >15 μm;
B、烧结工艺：升、降温速率每分钟50-70℃，峰值温度：800-950℃ 。B, sintering process: rising and cooling rate of 50-70 ° C per minute, peak temperature: 800-950 ° C.
本发明的适应范围：The scope of adaptation of the present invention:
1、调整本发明功能相成分、含量及烧结工艺，该PTC厚膜电路热敏电阻浆料、电极浆料可和多种金属基板介质浆料相容。例如：铝合金基板、铜合金基板、钛合金基板等。1. Adjusting the functional phase composition, content and sintering process of the present invention, the PTC thick film circuit thermistor paste and the electrode paste are compatible with a plurality of metal substrate dielectric pastes. For example, an aluminum alloy substrate, a copper alloy substrate, a titanium alloy substrate, or the like.
2、调整本发明功能相、稀土氧化物和粘接相成分、含量及烧结工艺，该PTC厚膜电路热敏电阻浆料、电极浆料、封装浆料可制备在氧化铝基板（Al2O3）、氮化铝（AIN）基板、碳化硅（SiC）基板、微晶玻璃基板、高分子复合陶瓷等基板上，且产生牢固的键结合效果，并具有高效远红外功能。2. Adjusting the functional phase, rare earth oxide and bonding phase composition, content and sintering process of the present invention, the PTC thick film circuit thermistor paste, electrode paste, and package slurry can be prepared on an alumina substrate (Al2O3), On a substrate such as an aluminum nitride (AIN) substrate, a silicon carbide (SiC) substrate, a glass-ceramic substrate, or a polymer composite ceramic, a strong bond-bonding effect is produced, and a high-efficiency far-infrared function is obtained.
金属基板基PTC稀土厚膜电路智能电热元件，是目前高低压、交直流均能启动、体积小，表面热负荷大，热效率高，热启动快，温度场均匀可分级自控，导热性能优良、抗热冲击能力强，具有远红外功能，易于加工，绿色、低碳环保、安全可靠，广泛适应太阳能、风能、锂离子电池等新能源要求的新型智能电加热元件系列产品。Metal substrate based PTC rare earth thick film circuit intelligent electric heating element, is currently high and low voltage, AC and DC can start, small volume, large surface thermal load, high thermal efficiency, fast hot start, uniform temperature field, self-control, excellent thermal conductivity Strong thermal shock capability, with far-infrared function, easy to process, green, low-carbon, environmentally friendly, safe and reliable, widely adapt to new energy requirements such as solar, wind, lithium-ion batteries and other new intelligent electric heating components.
以下是结合附图1对本发明的实施方式进行进一步描述，本实施例为两秒速热（达98℃）无热胆、增氧型电热水壶用稀土厚膜电路电热元件，按产品图纸技术要求选取金属基板，如上图所示。经冲压成型后进行草酸阳极化处理后备用，将调制好的系列稀土电子浆料含包封浆料、PTC厚膜电路热敏电阻浆料、稀土电极浆料、稀土介质浆料，按以下工艺和图纸要求，制备稀土厚膜电路可控电热元件：The following is a further description of the embodiments of the present invention with reference to FIG. 1. This embodiment is a rare earth thick film circuit electric heating element for a two-second heat (up to 98 ° C) non-heating and oxygen-increasing electric kettle, and is selected according to the technical requirements of the product drawings. The metal substrate is as shown in the figure above. After stamping and forming, the oxalic acid anodizing treatment is carried out, and the prepared series rare earth electronic slurry contains encapsulating slurry, PTC thick film circuit thermistor slurry, rare earth electrode slurry, rare earth medium slurry, according to the following process And drawings require the preparation of rare earth thick film circuit controllable electric heating elements:
工艺流程：Process flow:
A.金属基板→B.CAD\光绘制版→C.G网印刷→D.烘干烧结→E.检验包装A. Metal substrate→B.CAD\light drawing version→C.G network printing→D. Drying sintering→E. Inspection packaging
a.介质层厚度＞65μm b.热敏厚膜电路方阻膜厚度＞15μm a. dielectric layer thickness > 65μm b. thermal thick film circuit square film thickness > 15μm
B.烧结工艺：B. Sintering process:
a.升、降温速率每分钟50-70℃ b.峰值温度：800-950℃a. Increasing and cooling rate is 50-70 ° C per minute b. Peak temperature: 800-950 ° C
注：浆料放置过久，使用前需进行匀浆处理。Note: The slurry is left for too long and needs to be homogenized before use.
经测试，稀土厚膜电路可控电热元件达到以下设计要求。After testing, the rare earth thick film circuit controllable electric heating element meets the following design requirements.
本发明实施例的稀土厚膜电路可控电热元件性能参数：热响应速率：150℃/秒The rare earth thick film circuit controllable electric heating element performance parameter of the embodiment of the invention: thermal response rate: 150 ° C / sec
本实施例的PTC厚膜电路热敏电阻电性能： The electrical properties of the PTC thick film circuit thermistor of this embodiment:
①电性能：1 electrical performance:
厚膜热敏电阻 ------ 分辨率 ----------------------- TCR/ppm/℃ ---------------- -老化强度 ； Thick Film Thermistor ------ Resolution ----------------------- TCR/ppm/°C ---------------- - aging strength;
100±2Ω/□ ------------0.1mm ------------------------2200±300ppm×10-6/℃ ---＞10（N/mm2） ； 100±2Ω/□ ------------0.1mm ------------------------ 2200±300ppm×10-6/°C --->10(N/mm2) ;
R-T特性 --------------0℃：4800±1.5%Ω ；R-T characteristics --------------0 °C: 4800 ± 1.5% Ω;
-------------------------25℃：5180±1.5%Ω； ------------------------- 25 ° C: 5180 ± 1.5% Ω;
--------------------------200℃：6840±1.5%Ω；--------------------------200 ° C: 6840 ± 1.5% Ω;
-------------------------250℃：趋向无穷大 。-------------------------250 °C: tends to infinity.
②物理性能2 physical properties
流变特性------- 热敏电阻膜厚度 -------浆料粘度 -----------------单位用量 ；Rheological properties ------- Thermistor film thickness -------Slurry viscosity -----------------Unit dosage ;
触变宜网印 -----＞15μm ----------------168±20Pas/10RPM ---80cm2/克 。Touch-sensitive screen printing ----->15μm ----------------168±20Pas/10RPM ---80cm2 / gram.
本实施例的稀土介质浆料的性能： The performance of the rare earth medium slurry of this embodiment:
稀土介质浆料膜层厚度为：≥65μm The thickness of the rare earth dielectric slurry film layer is: ≥65μm
①物理性能：1 physical properties:
颜色（选） -----------固体含量 -------丝网数目 ------浆料粘度------- 烧结温度 ，Color (optional) -----------solid content -------number of screens ------slurry viscosity ------- Sintering temperature ,
蓝（灰、黑）色------ 77% ------------180 1------------25PaS/RPM ----870℃ 。Blue (gray, black) color ------ 77% ------------180 1------------25PaS/RPM ----870°C.
②电器性能：2 electrical performance:
泄漏电流 -------------------绝缘电阻--------------------- 击穿强度 ，Leakage current -------------------Insulation resistance --------------------- Breakdown strength
＜5mA（250VDC） ----＞50MΩ（500VDC） ---＞1800VAC 。<5mA (250VDC) ---->50MΩ (500VDC) --->1800VAC.
本实施例的稀土电极浆料性能： The performance of the rare earth electrode slurry of this embodiment:
①电性能： 1 electrical performance:
方阻 ------------分辨率------------ 抗拉强度 -------------老化强度 ，Square resistance ------------resolution ------------ tensile strength -------------Aging intensity,
＜3±2mΩ/□ ---0.1mm ----------＞16（N/mm2） -----10（N/mm2） 。<3±2mΩ/□ ---0.1mm ---------->16(N/mm2) -----10(N/mm2).
②物理性能 2 physical properties
流变特性：触变 宜网印 ；Rheological properties: thixotropic is suitable for screen printing;
电极层厚度 ：＞12μm ； Electrode layer thickness: >12μm;
浆料粘度 ：186PaS/RPM ；Slurry viscosity: 186 PaS / RPM;
单位用量 ： 88cm2/克 。Unit dosage: 88cm2 / gram.
本发明专利上述实施例和附图所示仅为本发明较佳实施例之一，并不能以此局限本发明，如厚膜电路加热元件在基片上的电路轨迹还可为同心圆状或阿基米德螺旋线状，厚膜电路加热元件的基片也可以为不同形状及不同材质的基板等，在不脱离本发明精髓的条件下，本领域技术人员所做的任何变动，都属本发明的保护范围。The above embodiments and the accompanying drawings of the present invention are only one of the preferred embodiments of the present invention, and the invention may not be limited thereto. For example, the circuit trace of the thick film circuit heating element on the substrate may be concentric or The substrate of the Kimede spiral-shaped, thick-film circuit heating element may also be a substrate of different shapes and different materials, and any changes made by those skilled in the art without departing from the essence of the invention belong to the present invention. The scope of protection of the invention.

Claims (10)

  1. 一种PTC稀土厚膜电路智能电热元件,其特征在于,它包括金属基板及其上设置的PTC厚膜电路热敏电阻和稀土厚膜电阻电路，PTC厚膜电路热敏电阻是以厚膜电路的形式和稀土厚膜电阻电路叠加或处于同一平面内，来控制厚膜电路电热元件的温度；或单独以厚膜电路形式做成可控电热元件。 A PTC rare earth thick film circuit intelligent electric heating element, characterized in that it comprises a metal substrate and a PTC thick film circuit thermistor and a rare earth thick film resistor circuit disposed thereon, and the PTC thick film circuit thermistor is a thick film circuit The form and the rare earth thick film resistor circuit are superimposed or in the same plane to control the temperature of the thick film circuit electric heating element; or the controllable electric heating element is separately formed in the form of a thick film circuit.
  2. 根据权利要求1所述的一种PTC稀土厚膜电路智能电热元件，其特征在于，所述金属基板为铁素体Cr15\1Cr17\00Cr18Mo2系列不锈钢基板。The PTC rare earth thick film circuit intelligent electric heating element according to claim 1, wherein the metal substrate is a ferrite Cr15\1Cr17\00Cr18Mo2 series stainless steel substrate.
  3. 根据权利要求1所述的一种PTC稀土厚膜电路智能电热元件，其特征在于，所述PTC厚膜电路热敏电阻由PTC厚膜电路热敏电阻浆料制成，稀土厚膜电阻电路由稀土介质浆料和稀土电极浆料制成。The PTC rare earth thick film circuit intelligent electric heating element according to claim 1, wherein the PTC thick film circuit thermistor is made of a PTC thick film circuit thermistor paste, and the rare earth thick film resistor circuit is It is made of rare earth medium slurry and rare earth electrode slurry.
  4. 根据权利要求3所述的一种PTC稀土厚膜电路智能电热元件，其特征在于，所述稀土介质浆料由固相成分与有机溶剂载体组成，其重量比为：65 : 35 ~ 85 : 15 ；固相成分为：Si02 ~ Al203~CaO~B2O3 ~ La2O3稀土氧化物系微晶玻璃，重量配比为：Si02 30 ~ 65 ％、Al203 5 ~ 26 ％、CaO 15~38 ％、 B2O3 2 ~16 ％、La2O3 0 . 3 ~15 ％。Co2O3 0 . 05~ 6 ％；晶核剂为TiO2 1 ~ 10 ％、ZrO : 1 ~10 ％；溶剂载体配比为：丁基卡必醇 66 ~89 ％、柠檬酸三丁醋 5~ 15% 、乙基纤维素 0.5 ~10 ％、氢化蓖麻油 0.1 ~ 5 ％、卵磷脂 0.1~5 ％；稀土氧化物为镧、铈、钕、钷、钆、铒、钪、钇和氧化铽中的一种或多种。 The PTC rare earth thick film circuit intelligent electric heating element according to claim 3, wherein the rare earth medium slurry is composed of a solid phase component and an organic solvent carrier, and the weight ratio thereof is 65. : 35 ~ 85 : 15 ; The solid phase composition is: Si02 ~ Al203~CaO~B2O3 ~ La2O3 rare earth oxide-based glass-ceramics, the weight ratio is: Si02 30 ~ 65 %, Al203 5 ~ 26 %, CaO 15~38 %, B2O3 2 ~ 16 %, La2O3 0 . 3 ~ 15%. Co2O3 0 . 05~ 6 %; crystal nucleating agent is TiO2 1 ~ 10%, ZrO: 1 ~ 10%; solvent carrier ratio: butyl carbitol 66 ~ 89%, citric acid tributyl vinegar 5 ~ 15%, ethyl cellulose 0.5 to 10%, hydrogenated castor oil 0.1 to 5 %, lecithin 0.1 to 5%; rare earth oxides are one or more of cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum and cerium oxide.
  5. 根据权利要求3所述的一种PTC稀土厚膜电路智能电热元件，其特征在于，所述PTC厚膜电路热敏电阻浆料，由二氧化钌、氧化铜、氧化钇复合粉和微晶玻璃粉及有机载体组成，二氧化钌、氧化铜、氧化钇与有机载体的重量比为 65 ~85 : 35 ~15；二氧化钌、氧化铜、氧化钇复合粉与微晶玻璃粉组成固相成分，固相成分中二氧化钌、氧化铜、氧化钇复合粉与微晶玻璃的重量比为 75 ~ 55 : 25~ 45 ；二氧化钌、氧化铜、氧化钇复合粉中的二氧化钌、氧化铜、氧化钇粉的重量比为：75 ~59：15~40.5 : 10 ~ 0.5，二氧化钌、氧化铜、氧化钇复合粉的粒径为：0.30--1.0μm；微晶玻璃粉为：CaO~SiO2 ~ A12O3 ~ B2O3 ~ Bi2O3 ~ La2 03 的稀土氧化物系微晶玻璃；各氧化物重量比：SiO2 20 ~ 60 ％、A12O3 5 ~ 35 ％、CaO 10 ~ 350%、Bi2O31O ~ 30 ％、B203 1~ 10 ％、 La2O3 O.3 ~8 ％；晶核剂为：TiO21~8 ％、ZrO21~10 %；有机载体各组分的重量比：松油醇 68 ~ 78 ％、柠檬酸三丁醋 2 ~ 18 ％、乙基纤维素 0 .4 ~ 9％、硝基纤维素 0 .4~ 9％、氢化蓖麻油 0 .1 ~ 6% 、卵磷脂 0 .1 ~ 6％；上述稀土氧化物为；镧、铈、钕、钷、钆、铒、钪、钇和氧化铽中的一种或几种。The PTC rare earth thick film circuit intelligent electric heating element according to claim 3, wherein the PTC thick film circuit thermistor paste comprises cerium oxide, copper oxide, cerium oxide composite powder and glass ceramics. Powder and organic carrier composition, the weight ratio of cerium oxide, copper oxide, cerium oxide and organic carrier is 65 ~ 85 : 35 ~ 15; solid phase composition of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder, the weight of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic in solid phase composition The ratio is 75 ~ 55 : 25~ 45 ; The weight ratio of cerium oxide, copper oxide and cerium oxide powder in cerium oxide, copper oxide and cerium oxide composite powder is: 75 ~ 59: 15 ~ 40.5 : 10 ~ The particle size of 0.5, cerium oxide, copper oxide and cerium oxide composite powder is 0.30--1.0μm; the glass-ceramic powder is: CaO~SiO2 ~ A12O3 ~ B2O3 ~ Bi2O3 ~ Rare earth oxide-based glass-ceramics of La2 03; weight ratio of each oxide: SiO2 20 ~ 60 %, A12O3 5 ~ 35 %, CaO 10 ~ 350%, Bi2O31O ~ 30 %, B203 1~ 10 %, La2O3 O.3 ~ 8%; nucleating agent: TiO21~8 %, ZrO21~10%; weight ratio of each component of organic carrier: terpineol 68 ~ 78 %, 2 ~ 18 % citric acid citrate, 0.4 ~ 9% ethyl cellulose, 0.4 ~ 9% nitrocellulose, hydrogenated castor oil 0.1 to 6%, lecithin 0 .1 ~ 6%; the above rare earth oxides are one or more of cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum and cerium oxide.
  6. 根据权利要求3所述的一种PTC稀土厚膜电路智能电热元件，其特征在于，所述稀土电极浆料由固相成分与有机溶剂载体组成，重量比为 70 ~ 90：30~10 ；固相成分包括银钯钇复合粉与微晶玻璃粉，银钯钇复合粉与微晶玻璃粉重量比为 99.4 ~0.6：0.6~6；银钯钇复合粉重量比为： 0.6 ~10 ：99~82：0.4 ~ 8；粒径为：3μm；有机溶剂载体重量比为：松油醇 60 ~ 98 ％、柠檬酸三丁醋 10~30 ％、乙基纤维素 2 ~10 ％、硝基纤维素 1~5 ％、氢化蓖麻油 0.1~5 ％、卵磷脂 0.1~5 ％；微晶玻璃为SiO2 ~A12O3~CaO~B203~Bi2O3 ~La2O3 的稀土、氧化物系微晶玻璃，各氧化物的成分重量比为：SiO2 20~60 ％、A12O35~35 ％、CaO 10~35 ％、B2031~15 ％、La2O3 0. 3~15 ％、 Bi2O3 10 ~30 ％。晶核剂为：Ti021~10 ％、ZrO21~10 ％；稀土氧化物为镧、铈、钕、钷、钆、铒、钪、钇和氧化铽中的一种或几种。The PTC rare earth thick film circuit intelligent electric heating element according to claim 3, wherein the rare earth electrode paste is composed of a solid phase component and an organic solvent carrier, and the weight ratio is 70 ~ 90:30~10; solid phase composition includes silver-palladium-ruthenium composite powder and glass-ceramic powder, the weight ratio of silver-palladium-iridium composite powder to glass-ceramic powder is 99.4 ~ 0.6:0.6~6; silver-palladium-ruthenium composite powder weight The ratio is: 0.6 ~ 10 : 99 ~ 82: 0.4 ~ 8; particle size: 3 μm; organic solvent carrier weight ratio: terpineol 60 ~ 98%, citric acid tributyl vinegar 10 ~ 30%, ethyl cellulose 2 ~10%, nitrocellulose 1~5 %, hydrogenated castor oil 0.1~5 %, lecithin 0.1~5 %; glass ceramics SiO2 ~A12O3~CaO~B203~Bi2O3 ~La2O3 rare earth, oxide-based glass-ceramics, the weight ratio of each oxide is: SiO2 20~60%, A12O35~35 %, CaO 10~35 %, B2031~15 %, La2O3 0. 3~15%, Bi2O3 10~30%. The nucleating agent is: Ti021~10%, ZrO21~10 %; rare earth oxides are one or more of cerium, lanthanum, cerium, lanthanum, cerium, lanthanum, cerium, lanthanum and cerium oxide.
  7. 一种PTC稀土厚膜电路智能电热元件的制备方法，其特征在于，它是将金属基板、稀土介质浆料、PTC厚膜电路热敏电阻浆料、电极浆料、封装浆料按工艺流程制备成PTC稀土厚膜电路电热元件，其工艺流程如下：Method for preparing PTC rare earth thick film circuit intelligent electric heating element, characterized in that it is prepared by metal substrate, rare earth medium slurry, PTC thick film circuit thermistor paste, electrode paste and package slurry according to the process flow The process of forming a PTC rare earth thick film circuit electric heating element is as follows:
    A、金属基板→CAD\光绘制版→G网印刷→烘干烧结→检验包装,其中介质层厚度＞65μm,PTC厚膜电路热敏电阻膜厚度＞15μm ;A, metal substrate → CAD \ light drawing version → G network printing → drying and sintering → inspection packaging, wherein the dielectric layer thickness > 65μm, PTC thick film circuit thermistor film thickness > 15μm ;
    B、烧结，升、降温速率每分钟50-70℃，峰值温度：800-950℃。B, sintering, rising and cooling rates of 50-70 ° C per minute, peak temperature: 800-950 ° C.
  8. 根据权利要求7所述的一种PTC稀土厚膜电路智能电热元件的制备方法，其特征在于，所述稀土介质浆料的制备工艺，它包括如下步骤： The method for preparing a PTC rare earth thick film circuit intelligent electric heating element according to claim 7, wherein the preparation process of the rare earth medium slurry comprises the following steps:
    ① 制备稀土微晶玻璃粉：按重量配比将各氧化物，晶核剂，经混合均匀后熔炼，熔炼温度为：1100 ~1450 ℃。保温 90~180 分钟后，出炉水淬，得到玻璃微渣；球磨玻璃微渣，制备出粒径1~3 微米的微晶玻璃粉；1 Preparation of rare earth glass-ceramic powder: Each oxide and crystal nucleating agent are mixed and smelted according to the weight ratio, and the melting temperature is: 1100 ~ 1450 °C. Insulation After 90~180 minutes, the water is quenched to obtain glass micro-slag; the glass micro-slag is ball-milled to prepare a glass-ceramic powder with a particle size of 1-3 microns;
    ② 配制有机溶剂载体：将各化工原料按配比混合均匀，在80 ~100 ℃ 的水中溶浴数小时；调整乙基纤维素含量，将有机载体的粘度调整在150 ~ 28OmPaS的范围内； 2 Preparation of organic solvent carrier: Mix all chemical raw materials according to the ratio, at 80 ~ 100 °C The bath in water for several hours; adjust the ethyl cellulose content, adjust the viscosity of the organic carrier in the range of 150 ~ 28OmPaS;
    ③ 介质浆料调制：将固相成分与有机溶剂载体的重量比按 65 : 85 ~35 ：15；经R-S01型双向旋转＋振动机械，混合、搅拌、分散一小时后，三棍轧制得到成品，粘度值为150 ~ 200PaS / RPM。3 medium slurry preparation: the weight ratio of the solid phase component to the organic solvent carrier is 65: 85 ~ 35 :15; After R-S01 bidirectional rotation + vibration machine, after mixing, stirring and dispersing for one hour, the three sticks are rolled to obtain the finished product, and the viscosity value is 150 ~ 200PaS / RPM.
  9. 根据权利要求7所述的一种PTC稀土厚膜电路智能电热元件的制备方法，其特征在于，所述PTC厚膜电路热敏电阻浆料的制备工艺，它包括如下步骤：The method for preparing a PTC rare earth thick film circuit intelligent electric heating element according to claim 7, wherein the PTC thick film circuit thermistor paste preparation process comprises the following steps:
    ①微晶玻璃粉制备：按上述氧化物、晶核剂配比在三维混料机中混合均匀后，熔炉熔炼，温度为：1100 ~ 1450℃，保温1 ~ 3小时后，将玻璃熔液水淬，得到微渣，经球磨获得粒径1.0~3.0 微米的玻璃微粉；1 Preparation of glass-ceramic powder: According to the above-mentioned oxide and crystal nucleating agent ratio, the mixture is uniformly mixed in a three-dimensional mixer, and the furnace is smelted at a temperature of 1100 ~ 1450 ° C, and the temperature is 1 ~ After 3 hours, the glass melt is water quenched to obtain fine slag, and the glass micropowder having a particle diameter of 1.0 to 3.0 μm is obtained by ball milling;
    ②二氧化钌、氧化铜、氧化钇复合粉制备：二氧化钌、氧化铜、氧化钇重量配比为：75 ~59 : 15 ~ 40.5 : 10 ~ 0.5，经三维搅拌、混合均匀、球磨得到复合粉，粒径均为：0.30--1.0μm ；2 Preparation of cerium oxide, copper oxide and cerium oxide composite powder: the weight ratio of cerium oxide, copper oxide and cerium oxide is: 75 ~ 59 : 15 ~ 40.5 : 10 ~ 0.5, after three-dimensional stirring, mixing and uniform, ball milling to obtain composite powder, the particle size is: 0.30--1.0μm;
    ③有机载体制备：将上述化工原料按比例，经高效搅拌、混合均匀，在 80 ~100 ℃ 的水中溶解数小时，调整增稠剂含量，将有机载体溶剂的粘度调整在 180~280mPaS 的范围内即可；3 Preparation of organic carrier: The above chemical raw materials are proportioned, stirred efficiently and uniformly, at 80 ~ 100 °C After being dissolved in water for several hours, the content of the thickener is adjusted, and the viscosity of the organic carrier solvent is adjusted within a range of 180 to 280 mPaS;
    ④PTC厚膜电路热敏电阻浆料综合调制：固相成分由二氧化钌、氧化铜、氧化钇复合粉和微晶玻璃粉组成，重量比为： 75~ 55 : 25 ~ 45；固相成分和有机载体重量比：65~85 : 35 ~ 15，将固相粉体、有机载体溶剂经R-S01型双向旋转＋振动机械，搅拌、混合均匀后，进行三辊反复轧制得到成品，粘度值为150 ~ 200PaS / RPM 。4PTC thick film circuit thermistor slurry comprehensive modulation: solid phase composition consists of cerium oxide, copper oxide, cerium oxide composite powder and glass-ceramic powder, the weight ratio is: 75~ 55 : 25 ~ 45; solid phase composition and organic carrier weight ratio: 65~85: 35 ~ 15. The solid phase powder and the organic carrier solvent are subjected to R-S01 bidirectional rotation + vibration machine, stirred and mixed uniformly, and then subjected to three-roll repeated rolling to obtain a finished product having a viscosity of 150 to 200 PaS / RPM. .
  10. 根据权利要求7所述的一种PTC稀土厚膜电路智能电热元件的制备方法，其特征在于，所述稀土电极浆料的制备工艺，它包括如下步骤：The method for preparing a PTC rare earth thick film circuit intelligent electric heating element according to claim 7, wherein the preparation process of the rare earth electrode slurry comprises the following steps:
    ①微晶玻璃粉制备：按原料重量比将各氧化物、晶核剂混合均匀后熔炼，温度为：1100 ~1450℃ ，保温1~3 小时，水淬得到玻璃微渣，球磨获得3 微米玻璃微粉；1 Preparation of glass-ceramic powder: Each oxide and crystal nucleating agent are uniformly mixed according to the weight ratio of raw materials, and then smelted at a temperature of 1100 ~ 1450 ° C, and the temperature is 1~3 Hours, water quenching to obtain glass micro-slag, ball milling to obtain 3 micron glass micropowder;
    ②制备银钯钇复合粉；银钯钇复合粉，粒径为： 3μm ，在三维混料机中按重量比为：99 ~82：0.6 ~10：0.4~8 调制混合均匀； 2 Preparation of silver-palladium-ruthenium composite powder; silver-palladium-ruthenium composite powder, particle size: 3μm, in the three-dimensional mixer by weight ratio: 99 ~ 82: 0.6 ~ 10: 0.4 ~ 8 Modulation and mixing evenly;
    ③有机载体制备；按原料重量比混合后在 80~100℃水中溶解数小时，调整乙基纤维素含量，粘度控制在150~280mPas 范围； 3 Preparation of organic carrier; after mixing in the weight ratio of raw materials, it is dissolved in 80~100 °C water for several hours to adjust the ethyl cellulose content, and the viscosity is controlled at 150~280mPas. Scope
    ④制备稀土电极浆料：按比例将微晶玻璃粉、银钯钇复合粉、有机溶剂载体置于三维混料机中搅拌混合均匀后入三辊轧机反复轧制，得到稀土电极浆料，粘度值为150 ~200PaS / RPM。4 Preparation of rare earth electrode slurry: The microcrystalline glass powder, the silver palladium ruthenium composite powder and the organic solvent carrier are placed in a three-dimensional mixing machine in proportion, stirred and uniformly mixed, and then repeatedly rolled into a three-roll mill to obtain a rare earth electrode slurry, viscosity. Value is 150 ~200PaS / RPM.
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