WO2020107910A1 - Novel ceramic heating element composition and preparation and use of heating element using same - Google Patents

Novel ceramic heating element composition and preparation and use of heating element using same Download PDF

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Publication number
WO2020107910A1
WO2020107910A1 PCT/CN2019/097568 CN2019097568W WO2020107910A1 WO 2020107910 A1 WO2020107910 A1 WO 2020107910A1 CN 2019097568 W CN2019097568 W CN 2019097568W WO 2020107910 A1 WO2020107910 A1 WO 2020107910A1
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Prior art keywords
heating element
ceramic heating
nitride
resistance
heating
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PCT/CN2019/097568
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French (fr)
Chinese (zh)
Inventor
刘华臣
邓腾飞
李丹
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湖北中烟工业有限责任公司
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Publication of WO2020107910A1 publication Critical patent/WO2020107910A1/en

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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
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A24F40/46—Shape or structure of electric heating means
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/70—Manufacture

Definitions

  • the invention relates to the field of functional ceramics, and more particularly, to a novel ceramic heating body composition for low-temperature smoke, and a method and application for preparing the heating body.
  • the ceramic heating body is an efficient heater with uniform heat distribution and excellent thermal conductivity, which can ensure that the hot surface temperature is uniform, thereby eliminating hot spots and cold spots of the equipment.
  • the ceramic heating body also has a long life, good thermal insulation performance, and mechanical Strong performance, corrosion resistance, magnetic field resistance and other advantages.
  • PTC ceramic heating element is a thermistor. It is composed of PTC ceramic heating element and aluminum tube. It has the advantages of small thermal resistance and high heat exchange efficiency. It is an automatic constant temperature and power saving electric heater.
  • MCH ceramic heating element uses alumina ceramic, which is a new type of high-efficiency, environmentally friendly and energy-saving ceramic heating element. Compared with PTC ceramic heating element, it can save 20-30% of electric energy under the same heating effect.
  • the MCH ceramic heating element uses a screen printing method to print the metal heating layer on the ceramic base layer, that is, high temperature refractory metal such as molybdenum tungsten
  • a series of special preparation processes are co-fired under a reducing atmosphere of 1400 °C to 1800 °C to obtain an efficient and energy-saving cermet heating element, which usually uses an aluminum oxide casting blank as the insulating layer
  • the prepared high-temperature metal thick film paste wiring is printed on one side of the blank, and then the upper and lower alumina ceramic substrates are laminated and sliced, and the leads are welded after high-temperature sintering in a hydrogen reduction furnace, thereby preparing MCH heating stuff.
  • Silicon carbon rod electric heating element is a kind of non-metal electric heating element which is made of silicon carbide as the main raw material, after a certain molding process, through high temperature sintering. The process of conversion of silicon carbide rods into electrical energy is essentially different from the heating of metal resistance wires. During the heating process of silicon carbon rod, its resistivity changes nonlinearly with temperature.
  • the resistivity decreases rapidly with the increase of temperature, and reaches the lowest value at 800°C. As the temperature further increases, the resistivity begins to increase, and the magnitude of the increase becomes higher and higher.
  • the maximum use temperature of silicon carbon rods cannot exceed 1450°C. If the use temperature exceeds this value, the silicon carbon rods will quickly age and the service life will be seriously affected.
  • the resistance value of the silicon carbon rod will increase slowly during use. When the resistance value increases to four times the resistance value at the beginning of use, the life of the silicon carbon rod ends.
  • the resistance of the silicon carbon rod is measured by using special electrical testing equipment to measure the high temperature resistance. It is not measured at room temperature. If a multimeter or other instrument is used for measurement, the error is very large, so the resistance value of the silicon carbon rod at a low temperature (20 °C) Uncertainty leads to uncertainty of normal temperature resistance.
  • the purpose of the present invention is to completely overcome the above-mentioned shortcomings in the prior art.
  • a product with high yield, fast heating, uniform heating A new type of ceramic heating element with low temperature resistance measurable, small error, and long service life of low-temperature use products completes the present invention.
  • the present invention provides a composition for preparing a novel ceramic heating element, wherein the composition for preparing a novel ceramic heating element comprises: a heating body material, a heating stabilizer and a binder .
  • the heating body material of the present invention includes at least one of carbide, nitride, molybdenum disilicide, etc.
  • the carbide includes titanium carbide, silicon carbide, tungsten carbide
  • the nitride includes titanium nitride, nitrogen Vanadium, zirconium nitride, tantalum nitride, manganese nitride, tungsten nitride, silicon nitride, boron nitride, copper nitride, zinc nitride, silver nitride, etc.
  • the heat stabilizer of the present invention includes graphene, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, molybdenum, ruthenium, rhodium, palladium, silver, tungsten, gold, platinum, iridium, And at least one of the foregoing metal oxides, the foregoing metal alloys, and the like.
  • the adhesives described in the present invention are common adhesives, including esters, resins, fibers, alcohols and polyols. Specific examples include at least one of carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, starch, water glass, and synthetic resin.
  • the heat generating host material accounts for 60%-99.9% of the composition, preferably 63%-98%, more preferably 65%-95%; the heat generating stabilizer accounts for 0.2%-35% of the composition , Preferably 0.5%-30%, more preferably 1%-25%; the binder accounts for 0.3%-30% of the composition, preferably 0.5%-25%, more preferably 1%-20%.
  • the novel ceramic heating component prepared by the optimized composition ratio has the advantages of good molding process, high product firing rate, high thermal conversion efficiency of the prepared product, and long product life.
  • the invention also discloses a novel ceramic heating component prepared by using the composition.
  • the novel ceramic heating component is mainly composed of a novel ceramic heating body and a heating body base.
  • the novel ceramic heating element of the present invention is mainly composed of two parts, including: the heating main body portion of the first part of the new ceramic heating element and the electrode portion of the second part of the new ceramic heating element, wherein the new type After the electrode part of the second part of the ceramic heating body is connected to the power source, the heating body part of the first part of the new ceramic heating body generates heat.
  • the temperature of the first part of the main body of the new-generation ceramic heating body for heating by current is relatively high.
  • the temperature of the heating body of the first part of the new ceramic heating body is heated to 220°C to about 500°C.
  • the temperature of the first part of the new ceramic heating body is from 250°C to about 340°C.
  • the structure of the new ceramic heating element according to the present invention includes any structural form that can be inserted into an aerosol medium.
  • the main body of the new ceramic heating element includes a heating base that generates heat by electricity, and its structure is Cylinder, elliptical cylinder, blade structure, prismatic structure, rectangular parallelepiped, etc.
  • the end of the new ceramic heating element inserted into the aerosol generating medium also includes a tip portion, which can be naturally extended from the heating substrate
  • the part can also be a separately manufactured part to solve the problem of easy insertion.
  • the heating base and the end of the novel ceramic heating body are connected together.
  • the size of the novel ceramic heating element can be selected according to the aerosol generating medium or the heating device.
  • the length of the new ceramic heating element is 5mm-60mm, preferably 8mm-45mm.
  • part of the heat of the end portion of the new ceramic heating element will generate a part of heat after passing current, which is used to heat the aerosol generating medium.
  • the length of the heating base of the new ceramic heating element is greater than the length of the end of the new ceramic heating element.
  • the novel ceramic heating body is directly used for heating, and its heating body includes at least one heating base part.
  • the heating body includes at least two heating bases, and at least one of the heating bases passes current. , For fever.
  • the gap between the heating substrates of the new ceramic heating body is filled with an insulating material or a sensor with a temperature sensing function, wherein the filling of the insulating material is preferred Ceramics, zirconia, aluminum nitride, glass, clay, boron nitride, silicon carbide, coated insulating metals or alloys, etc.
  • the new ceramic heating body is made of a material having a limited relationship between temperature and resistance, so that the new ceramic heating body can be used both for heating an aerosol-forming medium and It can be used to monitor the temperature of the heater in real time.
  • the electrode part of the second part of the new ceramic heating body is located at the other end of the new ceramic heating body.
  • the length of the new ceramic heating body is longer than the length of the electrode of the second part of the new ceramic heating body .
  • the heating body of the novel ceramic heating body is made of a composition including the following: a heating body material, a heating stabilizer and a binder.
  • the new ceramic heating element base has the function of fixing the new ceramic heating element, ensuring that the new ceramic heating element can be stably installed in the aerosol generating device.
  • the base of the new-type ceramic heating element is connected to the electrode of the new-type ceramic heating element through an electrical contact and has a power supply function.
  • the electrode of the second part of the new ceramic heating body can be used as an electrical contact with the base of the new ceramic heating body, and at the same time, the new ceramic heating body can be fixedly connected to the new ceramic heating body base Parts.
  • the base of the new ceramic heating element is made of a material with high temperature resistance and low thermal conductivity, which reduces the problems in the application of the new ceramic heating element in the product.
  • the selected material can withstand the high temperature heating of the new ceramic heating element.
  • the high temperature resistant materials include organic materials and inorganic materials, such as polyether ether ketone, high temperature resistant silica gel, polytetrafluoroethylene, ceramic materials, zirconia, aluminum nitride, silicon carbide, glass, etc.
  • the base portion of the new ceramic heating element is raised on the basis of smaller than the size of the base, and the raised portion has electrical contacts.
  • the specific size and structure are the same as the first portion of the new ceramic heating element
  • the size and structure of the heating body part are the same, or the size and structure of the convex part are different from those of the first part of the new type ceramic heating body.
  • the size of the convex part is selected according to the characteristics of the base material to ensure that the temperature of the base is not too high.
  • the present invention also provides a method for preparing the above ceramic heating element, wherein the method includes the following steps:
  • the semi-dry press method is used to form the sample into a target shape under a certain forming pressure.
  • the sample is first pressed slowly during the press forming process to discharge the air in the material;
  • the temperature is raised at a certain temperature increase rate, and heat preservation is fired in multiple temperature regions, and then sintered at 1600-2600°C to obtain a heating element.
  • the method for preparing the ceramic heating element includes the following steps:
  • the sample is made into the target shape under the molding pressure of 1KN-500KN.
  • the sample is first pressed slowly during the compression molding process to discharge the air in the material, and the pressure is maintained at the final pressure for 5s- 100s;
  • the welding time is 6h-24h
  • the welding temperature is 1200°C-1600°C.
  • the particle size of the heat generating host material and the heat generating stabilizer in the above step 1) and step 2) is 400-1200 mesh, and the preferred particle size is 500-1000 mesh.
  • the present invention also provides the use of the new ceramic heating element prepared according to the above-mentioned new ceramic heating element composition in heating non-burning cigarettes and electronic cigarettes using a solid smoking medium or a liquid smoking medium.
  • the novel ceramic heating element prepared according to the novel ceramic heating element composition of the present invention does not require a printed circuit and can be fired at one time.
  • the preparation process is simple, the heating is fast, the heating is uniform, the low temperature resistance is measurable and the stability is high, the error is small, and the finished product
  • the ceramic heating element with a high rate can effectively improve the heating efficiency and reliability and obtain a stable user experience when it is applied to heating non-burning cigarettes and electronic cigarettes using a solid smoking medium or a liquid smoking medium.
  • FIG. 3 is a view of another new type ceramic heating element of the present invention from the direction of the electrode;
  • FIG. 4 is a view of another novel ceramic heating element of the present invention from the direction of the electrode;
  • FIG. 5 is a schematic cross-sectional view of the novel ceramic heating component of the present invention.
  • FIG. 6 is a schematic cross-sectional view of a new type ceramic heating element of another structure of the present invention.
  • the present invention provides a new type of ceramic heating element, wherein the new type of ceramic heating element includes a first part and a second part, in particular the first part is a heating body part, and the second part is an electrode part.
  • the heat-generating body part of the novel ceramic heat-generating body according to the present invention is made of a composition including the following: a heat-generating body material, a heat-generating stabilizer and a binder.
  • Carbides and nitrides are some of the substances that have the characteristics of metals, such as high hardness, cutting and conductivity, such as titanium carbide, silicon carbide, tungsten carbide, titanium nitride, vanadium nitride, zirconium nitride, nitrogen Tantalum, manganese nitride, tungsten nitride, silicon nitride, boron nitride, copper nitride, zinc nitride, silver nitride, etc.
  • MoSi 2 is the highest silicon content in the Mo-Si binary alloy system
  • An intermediate phase is a Dalton-type intermetallic compound with a fixed composition.
  • the novel ceramic heating body composition of the present invention includes at least one kind of heating body material of carbide, nitride, molybdenum disilicide, etc.
  • the carbide includes titanium carbide, silicon carbide, tungsten carbide, and the nitride Including titanium nitride, vanadium nitride, zirconium nitride, tantalum nitride, manganese nitride, tungsten nitride, silicon nitride, boron nitride, copper nitride, zinc nitride, silver nitride, etc.
  • the percentage of the heating body material in the new ceramic heating body composition is 60% to 99.5%, preferably 63% to 98%, and more preferably 65% to 95%.
  • the novel ceramic heating element composition heating stabilizer of the present invention mainly includes graphene, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, molybdenum, ruthenium, rhodium, palladium, silver, tungsten , Gold, platinum, iridium, and at least one of the foregoing metal oxides, the foregoing metal alloys, etc.
  • the heat stabilizer accounts for 0.2% of the new ceramic heating element composition 35%, preferably 0.5%-30%, more preferably 1%-25%.
  • the type and amount of the binder of the novel ceramic heating element composition of the present invention are not particularly limited, and may be the type and amount of binders common in the art.
  • the binders are esters, resins, fibers, alcohols, polyols and the like. Specifically, at least one of carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, starch, water glass, synthetic resin, etc.
  • the binder accounts for 0.3% of the new ceramic heating element composition. 30%, preferably 0.5%-25%, more preferably 1%-20%.
  • the material of the electrode part of the new ceramic heating element is not particularly limited, and metals or non-metals with low conductivity that are common in the art, such as copper, zinc, nickel, chromium, gold, silver, platinum, and aluminum, can be used , Iron, cobalt, silicon, silicon carbide, and alloys of the foregoing metals.
  • welding there is no particular limitation on the "welding" process, and suitable means common in the art may be used, such as placing the fired heating body and the metal or non-metallic electrode part of low conductivity into a vacuum welding furnace for welding.
  • FIG. 1 is a schematic cross section of a novel ceramic heating element provided by the present invention.
  • the new ceramic heating element mainly includes a heating element end cap 1, a heating base 2, a heating element electrode 3, and a cavity in the heating element 4 four parts.
  • the heating element electrode 3 is connected to an external power source, and the external power source supplies power to the new ceramic heating element through the heating element electrode 3.
  • the material of the electrode portion of the new ceramic heating element is not particularly limited, and can be used in the art Common low conductivity metal or non-metal.
  • the heating element electrode 3 is composed of at least one of low conductivity metal and non-metal, such as copper, zinc, nickel, chromium, gold , Platinum, silver, aluminum, iron, cobalt, silicon, silicon carbide, and alloys of the foregoing metals, etc.
  • the electrode is made of copper, gold, silver, platinum, or the like.
  • the heating base 2 After the current passes through the current loop formed by the heating base 2 and the end cap 1 of the heating body, the heating base 2 will generate heat due to the passage of the current to achieve the purpose of heating.
  • the heat-generating body end cap 1 will also generate a part of heat after passing an electric current, which is used to heat the aerosol generating medium.
  • the heating temperature of the heating substrate 2 is from 220°C to about 500°C, preferably, the temperature of the heating substrate 2 is from 250°C to about 340°C.
  • FIG. 1 is a schematic cross section of a new type ceramic heating element.
  • the shape and structure of the new type ceramic heating element can be a cylinder, an elliptical body, a blade structure, a prismatic structure, a rectangular parallelepiped, etc.
  • the size of the ceramic heating element can be selected according to the aerosol generating medium or the heating device. In a preferred embodiment, the length of the new ceramic heating element is 5mm-60mm, preferably 8mm-45mm.
  • the length of the new ceramic heating base 2 is greater than the length of the end cap 1 of the new ceramic heating body, and the length of the new ceramic heating base 2 is greater than the length of the electrode 3 of the new ceramic heating body.
  • the novel ceramic heating base 2 is composed of at least two heating base parts, and at least one of the heating base parts passes current to generate heat.
  • Figures 2, 3 and 4 list different types of new ceramic heating elements from the direction of the electrode.
  • Figure 2 shows a cylindrical heating element.
  • the heating substrate is a two-equal distribution heating substrate.
  • the basic structure is The two-part heat distribution base 8 and the two-part heat distribution cavity 9 consist of a cylindrical heating body.
  • the heating base is a four-part heat distribution base.
  • the basic structure consists of a four-part heating base 10 and
  • the quadrant-type heating body cavity 11 is composed of a cylindrical two-part heat distributing heat matrix as shown in FIG. 4, and the basic structure is composed of a two-part heat distributing base 12 and a two-body heat distributing cavity 13.
  • the cavity 4 in the heating body is left between the novel ceramic heating substrate 2, or the cavity 4 in the heating body is filled with an insulating material, or the cavity 4 in the heating body is filled with a sensor having a temperature sensing function, in a preferred embodiment
  • the filled insulating material is at least one of ceramic, zirconia, aluminum nitride, glass, clay, boron nitride, silicon carbide, coated insulating metal or alloy.
  • the new ceramic heating base 2 is made of a material having a limited relationship between temperature and resistance, so that the new ceramic heating body can be used not only for heating an aerosol-forming medium but also for real-time monitoring of the temperature of the heating body .
  • the novel ceramic heating substrate 2 is prepared by a composition composed of a heating body material, a heating stabilizer and a binder.
  • the host material includes at least one of carbide, nitride, molybdenum disilicide, etc.
  • the carbide includes titanium carbide, silicon carbide, tungsten carbide
  • the nitride includes titanium nitride, vanadium nitride, zirconium nitride , Tantalum nitride, manganese nitride, tungsten nitride, silicon nitride, boron nitride, copper nitride, zinc nitride, silver nitride, etc.
  • Heat stabilizers include graphene, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, molybdenum, ruthenium, rhodium, palladium, silver, tungsten, gold, platinum, iridium, and the foregoing metal oxides , At least one of the aforementioned metal alloys.
  • Binders are common binders, including esters, resins, fibers, alcohols and polyols. Specific examples include at least one of carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, starch, water glass, and synthetic resin.
  • the heating body material accounts for 60%-99.5% of the new ceramic heating body composition, the heating stabilizer accounts for 0.2%-35% of the new ceramic heating body composition, and the binder The percentage of the new ceramic heating element composition is 0.3%-30%.
  • the novel ceramic heating body end cap 1 and the heating base body 2 can be made of the same material or different materials.
  • FIG. 5 is a schematic cross-sectional view of a new ceramic heating element with a new ceramic heating element base according to the present invention, which is mainly composed of a heating element end 1, a heating base 2, a heating element electrode 3, a heating body cavity 4 and a heating element base 5 It is composed of electrode lead hole 6 and other parts.
  • the heating element base is composed of heating element base 5, electrode point (heating element electrode 3 fixed point) and electrode lead hole 6, etc. It has the function of fixing new ceramic heating element to ensure The new ceramic heating element can be stably installed in the aerosol generating device.
  • the heating element base is connected to the heating element electrode through electrical contacts and has a power supply function.
  • the heating element electrode 3 can be used as an electrical contact to connect with the heating element base 5, and at the same time, it can also be a component that connects the new type ceramic heating element to the heating element base.
  • the cavity 4 of the heating body may not be filled with any substance, or the cavity 4 of the heating body is filled with an insulating material, or the cavity 4 of the heating body is filled with a sensor having a temperature sensing function.
  • the insulating material is preferably at least one of ceramics, zirconia, aluminum nitride, glass, clay, boron nitride, silicon carbide, coated insulating metal, or alloy.
  • the heating element base 5 is made of a material with high temperature resistance and low thermal conductivity, which reduces the problems of the application of the new ceramic heating element in subsequent products.
  • the selected materials can withstand the high temperature heating of the new ceramic heating element and pass through the battery. The heat transferred from the connection.
  • the high temperature resistant materials include organic materials and inorganic materials, such as polyetheretherketone, high temperature resistant silica gel, polytetrafluoroethylene, ceramic materials, zirconia, aluminum nitride, silicon carbide, glass, etc. Or, the material is the same as that of the new ceramic heating element.
  • FIG. 6 shows that the convex heating element base 7 replaces the conventional heating element base 5, and this type of base has a heating element base protrusion 14 whose size is smaller than that of the convex heating element base 7.
  • the convex heating element base 7 has electrical contacts, the specific size and structure are the same as those of the heating element electrode 3, or the convex heating element base 7 is different from the new type ceramic heating element composed of the heating base 2 in size and structure Body size and structure.
  • the height of the base 7 of the convex heating element is selected according to the characteristics of the base material to ensure that the temperature of the base is not too high, and the selected material may be the same as or different from the material of the heating element.
  • the semi-dry press method is used to form the sample into the target shape at a molding pressure of 100KN.
  • the sample is first slowly pressed during the press molding process to discharge the air in the material and maintain the pressure for 60 seconds at the final pressure;
  • Example 1 pure titanium carbide is used as the main heating material, no heating stabilizer is added, the binder and the like are in accordance with the ratio of Example 1, and the preparation method and steps are carried out as in Example 1. The same test was performed in Example 1 and compared.
  • Example 2 It can be seen from Table 2 that the average deviation rate of Example 1 is only 2.02, and the average deviation rate of the control reaches 9.27, which is 4.59 times that of Example 1, indicating that after adding a heating stabilizer to the new ceramic heating element, the product resistance The stability is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 3 for details.
  • the average limit thermal cycle test number of the control when half the resistance value is twice the initial resistance is 2018, and the average limit thermal cycle test number of Example 1 is 3021 times, which is 1.5 times, which means that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
  • the preparation process and step implementation steps of the new ceramic heating element are prepared in accordance with step 1)-step 7 in Example 1.
  • the specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 4 below:
  • Heating body material Fever stabilizer Binder Substance name Silicon carbide titanium Carboxymethyl cellulose Component ratio (%) 85 10 5
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 7 for details.
  • the preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1.
  • the specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 8 below:
  • Heating body material Fever stabilizer Binder Substance name Tungsten carbide vanadium Carboxymethyl cellulose Component ratio (%) 99.5 0.2 0.3
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic
  • the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 11 for details. It can be seen from Table 11 that in the control, the average limit thermal cycle test number after the half resistance value is twice the initial resistance is 2067, and the average limit thermal cycle test number of the sample in this implementation is 3029 times, which is in this example. 1.47 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
  • the preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1.
  • the specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 12 below:
  • Heating body material Fever stabilizer Binder Substance name Titanium nitride chromium Polyvinyl alcohol Component ratio (%) 88 7 5
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic
  • the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 15 for details. It can be seen from Table 15 that in the control, when the half resistance value is twice the initial resistance, the average limit thermal cycle test number is 1788 times, and the average limit thermal cycle test number of the sample in this implementation is 2527 times, which is in this example. 1.41 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
  • the preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1.
  • the specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 16 below:
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic
  • the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 19 for details. It can be seen from Table 19 that in the control, the average limit thermal cycle test number after the half resistance value is twice the initial resistance is 1811 times, and the average limit thermal cycle test number of the sample in this implementation is 2557 times, which is in this example. 1.41 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
  • the preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1.
  • the specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 20 below:
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic
  • the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 23 for details. From Table 23, it can be seen that the average limit thermal cycle test number of the control after half the resistance value is twice the initial resistance is 1879 times, and the average limit thermal cycle test number of the sample in this implementation is 2770 times, which is in this example. 1.47 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
  • the preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1.
  • the specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 24 below:
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 27 for details.
  • the average limit thermal cycle test number after the half resistance value is twice the initial resistance in the control is 1617 times
  • the average limit thermal cycle test number of the sample in this implementation is 2606 times, which is 1.61 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
  • step 1)-step 7) The preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1)-step 7) in Example 1, the specific heating main material, heating stabilizer and binder components and proportions are shown in Table 28 below:
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 31 for details.
  • the average limit thermal cycle test number of the control after half the resistance value is twice the initial resistance is 1544 times
  • the average limit thermal cycle test number of the sample in this implementation is 2692 times, which is 1.74 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
  • the preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1.
  • the specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 32 below:
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 35 for details.
  • the preparation process and implementation steps of the new ceramic heating element are prepared in accordance with steps 1) to 7) in Example 1.
  • the specific heating body materials, heating stabilizers and binder components and proportions are shown in Table 36 below:
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 39 for details.
  • the average limit thermal cycle test times after half the resistance value is twice the initial resistance in the control is 1765 times
  • the average limit thermal cycle test times of the sample in this implementation is 2807 times, which is 1.59 times, indicating that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
  • the preparation process and implementation steps of the new ceramic heating element are prepared in accordance with steps 1) to 7) in Example 1.
  • the specific heating body materials, heating stabilizers and binder components and proportions are shown in Table 40 below:
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1.
  • the specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 44 below:
  • the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation.
  • the experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
  • the thermal cycle test of the new type ceramic heating element the product limit thermal cycle test from room temperature to 1600 °C, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic
  • the experiment is terminated, and the number of cycles at this time is the life of the product, as shown in Table 47.
  • Table 47 it can be seen that the average limit thermal cycle test number of the control after half the resistance value is 2 times the initial resistance is 1764 times, and the average limit thermal cycle test number of the sample in this implementation is 2820 times, which is in this example. 1.60 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
  • the defective rate of products is significantly reduced, the average resistance and the average deviation of resistance between multiple batches are significantly reduced, the product heats up quickly and uniformly, and the product withstands thermal shock Significantly increased the number of times, can significantly increase the life of the new ceramic heating element.

Abstract

Disclosed are a novel ceramic heating element composition and a preparation method therefor. The novel ceramic heating element composition is mainly comprised of a heating main body material, a heating stabilizer and a binder, wherein the heating main body material is selected from at least one of a carbide, a nitride and molybdenum disilicide, and the heating stabilizer is at least one of graphene, a metal, an alloy and a metal oxide. Further provided is a novel ceramic heating component manufactured using the novel ceramic heating element composition, the assembly comprising a novel ceramic heating element and a novel ceramic heating element base (5), wherein the novel ceramic heating element is installed on the novel ceramic heating element base (5), and the novel ceramic heating element comprises a heating body and an electrode (3). The method provides the use of the novel ceramic heating component in a heat-not-burn cigarette or electronic cigarette. The prepared novel ceramic heating element has the characteristics of fast heating, stable working, a small deviation, a long product service life, a simple preparation process, a high yield, etc.

Description

一种新型陶瓷发热体的组合物及其发热体制备和应用A novel ceramic heating element composition and its preparation and application 技术领域Technical field
本发明涉及功能陶瓷领域，更具体地，涉及一种低温烟用新型陶瓷发热体组合物及其发热体制备方法和应用。The invention relates to the field of functional ceramics, and more particularly, to a novel ceramic heating body composition for low-temperature smoke, and a method and application for preparing the heating body.
背景技术Background technique
陶瓷加热体是一种高效热分布均匀且热导性极佳的加热器，可以确保热面温度均匀，从而消除设备的热点及冷点，此外陶瓷加热体还具有长寿命、保温性能好、机械性能强、耐腐蚀、抗磁场等优点。目前，陶瓷加热体主要分两种，分别是PTC陶瓷发热体和MCH陶瓷发热体。这两种产品所使用的材质是完全不同的，只是成品类似于陶瓷，所以统称为“陶瓷发热体”。PTC陶瓷发热体是热敏电阻，采用PTC陶瓷发热元件与铝管组成，有热阻小、换热效率高的优点，是一种自动恒温、省电的电加热器。MCH陶瓷发热体使用氧化铝陶瓷，是一种新型高效环保节能陶瓷发热元件，相比PTC陶瓷发热体，具有相同加热效果情况下节约20～30％电能。The ceramic heating body is an efficient heater with uniform heat distribution and excellent thermal conductivity, which can ensure that the hot surface temperature is uniform, thereby eliminating hot spots and cold spots of the equipment. In addition, the ceramic heating body also has a long life, good thermal insulation performance, and mechanical Strong performance, corrosion resistance, magnetic field resistance and other advantages. At present, there are two main types of ceramic heaters, namely PTC ceramic heaters and MCH ceramic heaters. The materials used by these two products are completely different, but the finished products are similar to ceramics, so they are collectively called "ceramic heating elements". PTC ceramic heating element is a thermistor. It is composed of PTC ceramic heating element and aluminum tube. It has the advantages of small thermal resistance and high heat exchange efficiency. It is an automatic constant temperature and power saving electric heater. MCH ceramic heating element uses alumina ceramic, which is a new type of high-efficiency, environmentally friendly and energy-saving ceramic heating element. Compared with PTC ceramic heating element, it can save 20-30% of electric energy under the same heating effect.
在目前的低温烟领域中大多采用MCH陶瓷发热体作为发热元件，具体地，MCH陶瓷发热体是用丝网印刷法将金属发热层印刷于陶瓷基层上，即以钼钨等耐高温难熔金属作为发热电路的内电极，通过一系列特殊的制备工艺在1400℃至1800℃的还原气氛下共烧得到的一种高效节能的金属陶瓷发热体，其中通常采用氧化铝流延坯体作为绝缘层和基体，将制备好的高温金属厚膜浆料布线印刷在坯体的一面上，然后将上下氧化铝陶瓷基层叠压、切片，在氢气还原炉中经高温烧结后焊接引线，从而制得MCH发热体。MCH陶瓷制作陶瓷发热体的技术工艺极其复杂，对生产涂布工艺要求高，通常需要烧成三次，不仅耗费大量人力物力，而且用生坯印刷浆料再包裹技术受到空间限制，自动化生产低，导致生产效率低下，产品次品率极高。硅碳棒电热元件，是以碳化硅为主要原材料，经过一定的成型工艺，通过高温烧结而制作而成的一种非金属电热元件。硅碳棒将电能转化为热能的过程与金属电阻丝的发热有本质的区别。硅碳棒在通电发热过程中，其电阻率随着温度的不同而呈非线性变化。在室温至800℃，随着温度的升高电阻率迅速减小，在800℃时达到最低值，随着温度进一步升高，其电阻率开始增大，并且增加的幅度愈来愈高。硅碳棒的最高使用温度不能超过1450℃，使用温度超过此值硅碳棒将快速老化，使用寿命将受到严重影响。硅碳棒在使用过程中电阻值将缓慢增大，当其电阻值增大到开始使用时阻值的四倍时，即硅碳棒寿命终结。硅碳棒的电阻测定是采用专用的电器检测设备测高温电阻的，不做常温测定，如果采用万用表等仪器 测量，误差很大，因而硅碳棒在温度较低时(20℃)电阻率数值具有不确定性，导致常温电阻的不确定性。In the current low-temperature smoke field, most of the MCH ceramic heating elements are used as heating elements. Specifically, the MCH ceramic heating element uses a screen printing method to print the metal heating layer on the ceramic base layer, that is, high temperature refractory metal such as molybdenum tungsten As the internal electrode of the heating circuit, a series of special preparation processes are co-fired under a reducing atmosphere of 1400 ℃ to 1800 ℃ to obtain an efficient and energy-saving cermet heating element, which usually uses an aluminum oxide casting blank as the insulating layer And the substrate, the prepared high-temperature metal thick film paste wiring is printed on one side of the blank, and then the upper and lower alumina ceramic substrates are laminated and sliced, and the leads are welded after high-temperature sintering in a hydrogen reduction furnace, thereby preparing MCH heating stuff. The technical process of MCH ceramics for making ceramic heating elements is extremely complicated, and the requirements for the production coating process are high. It usually needs to be fired three times, which not only consumes a lot of manpower and material resources, but also uses the green printing paste rewrapping technology is limited by space, and the automatic production is low As a result, production efficiency is low and the defective rate of products is extremely high. Silicon carbon rod electric heating element is a kind of non-metal electric heating element which is made of silicon carbide as the main raw material, after a certain molding process, through high temperature sintering. The process of conversion of silicon carbide rods into electrical energy is essentially different from the heating of metal resistance wires. During the heating process of silicon carbon rod, its resistivity changes nonlinearly with temperature. From room temperature to 800°C, the resistivity decreases rapidly with the increase of temperature, and reaches the lowest value at 800°C. As the temperature further increases, the resistivity begins to increase, and the magnitude of the increase becomes higher and higher. The maximum use temperature of silicon carbon rods cannot exceed 1450℃. If the use temperature exceeds this value, the silicon carbon rods will quickly age and the service life will be seriously affected. The resistance value of the silicon carbon rod will increase slowly during use. When the resistance value increases to four times the resistance value at the beginning of use, the life of the silicon carbon rod ends. The resistance of the silicon carbon rod is measured by using special electrical testing equipment to measure the high temperature resistance. It is not measured at room temperature. If a multimeter or other instrument is used for measurement, the error is very large, so the resistance value of the silicon carbon rod at a low temperature (20 ℃) Uncertainty leads to uncertainty of normal temperature resistance.
发明内容Summary of the invention
本发明的目的在于彻底克服上述提及的现有技术中的缺陷，按照本发明提供的一种制备新型陶瓷发热体的组合物，可以制备出一种产品成品率高、发热快、发热均匀、低温电阻可测且误差小、低温使用产品寿命长的新型陶瓷发热体，从而完成本发明。The purpose of the present invention is to completely overcome the above-mentioned shortcomings in the prior art. According to the composition for preparing a novel ceramic heating element provided by the present invention, a product with high yield, fast heating, uniform heating, A new type of ceramic heating element with low temperature resistance measurable, small error, and long service life of low-temperature use products completes the present invention.
为了实现上述目的，一方面，本发明提供了一种制备新型陶瓷发热体的组合物，其中，所述的制备新型陶瓷发热体的组合物包括：发热主体材料、发热稳定剂和粘结剂组成。In order to achieve the above object, on the one hand, the present invention provides a composition for preparing a novel ceramic heating element, wherein the composition for preparing a novel ceramic heating element comprises: a heating body material, a heating stabilizer and a binder .
本发明所述的发热主体材料包括碳化物、氮化物、二硅化钼等的至少一种，所述的碳化物包括碳化钛、碳化硅、碳化钨、所述的氮化物包括氮化钛、氮化钒、氮化锆、氮化钽、氮化锰、氮化钨、氮化硅、氮化硼、氮化铜、氮化锌、氮化银等。The heating body material of the present invention includes at least one of carbide, nitride, molybdenum disilicide, etc., the carbide includes titanium carbide, silicon carbide, tungsten carbide, and the nitride includes titanium nitride, nitrogen Vanadium, zirconium nitride, tantalum nitride, manganese nitride, tungsten nitride, silicon nitride, boron nitride, copper nitride, zinc nitride, silver nitride, etc.
本发明所述的发热稳定剂包括石墨烯、钛、钒、铬、锰、铁、钴、镍、铜、锌、钇、钼、钌、铑、钯、银、钨、金、铂、铱、及前述金属氧化物、前述金属合金等的至少一种。The heat stabilizer of the present invention includes graphene, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, molybdenum, ruthenium, rhodium, palladium, silver, tungsten, gold, platinum, iridium, And at least one of the foregoing metal oxides, the foregoing metal alloys, and the like.
本发明所述的粘结剂为常见粘结剂，包括酯类、树脂类、纤维类、醇及多元醇等。具体的如羧甲基纤维素、聚乙烯醇、乙基纤维素、淀粉、水玻璃、合成树脂等的至少一种。The adhesives described in the present invention are common adhesives, including esters, resins, fibers, alcohols and polyols. Specific examples include at least one of carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, starch, water glass, and synthetic resin.
所述的发热主体材料占组合物的百分数为60％-99.5％，优选63％-98％，更优选65％-95％；所述的发热稳定剂占组合物的百分数为0.2％-35％，优选0.5％-30％，更优选1％-25％；所述的粘结剂占组合物的百分数为0.3％-30％，优选0.5％-25％，更优选1％-20％。优选后的组合物比例制备的新型陶瓷发热组件具有成型工艺好、产品烧制成品率高，并且制备的产品热转化效率高，产品寿命长等优点。The heat generating host material accounts for 60%-99.9% of the composition, preferably 63%-98%, more preferably 65%-95%; the heat generating stabilizer accounts for 0.2%-35% of the composition , Preferably 0.5%-30%, more preferably 1%-25%; the binder accounts for 0.3%-30% of the composition, preferably 0.5%-25%, more preferably 1%-20%. The novel ceramic heating component prepared by the optimized composition ratio has the advantages of good molding process, high product firing rate, high thermal conversion efficiency of the prepared product, and long product life.
本发明还公开了利用所述的组合物制备的新型陶瓷发热组件，所述的新型陶瓷发热组件主要由新型陶瓷发热体和发热体底座组成。The invention also discloses a novel ceramic heating component prepared by using the composition. The novel ceramic heating component is mainly composed of a novel ceramic heating body and a heating body base.
本发明所述的新型陶瓷发热体主要由两部分组成，包括：所述的新型陶瓷发热体第一部分的发热主体部分和所述的新型陶瓷发热体第二部分的电极部分，其中所述的新型陶瓷发热体第二部分的电极部分与电源连通后，新型陶瓷发热体第一部分的发热主体部分进行发热。The novel ceramic heating element of the present invention is mainly composed of two parts, including: the heating main body portion of the first part of the new ceramic heating element and the electrode portion of the second part of the new ceramic heating element, wherein the new type After the electrode part of the second part of the ceramic heating body is connected to the power source, the heating body part of the first part of the new ceramic heating body generates heat.
所述的用于通过电流加热的新型陶瓷发热体第一部分发热主体部分的温度较高。在一个优选实施例中，所述的新型陶瓷发热体第一部分发热主体部分的温度加热到220℃到大约500℃，优选的，新型陶瓷发热体第一部分的温度在250℃到大约340℃。The temperature of the first part of the main body of the new-generation ceramic heating body for heating by current is relatively high. In a preferred embodiment, the temperature of the heating body of the first part of the new ceramic heating body is heated to 220°C to about 500°C. Preferably, the temperature of the first part of the new ceramic heating body is from 250°C to about 340°C.
本发明所述的新型陶瓷发热体的结构包括能够***气溶胶介质的任何结构形式，在本发明的一个优选实施方式中，所述的新型陶瓷发热体主体包括通电发热的发热基体，其结构为圆柱体、椭圆柱体、刀片式结构、棱形结构、长方体等，所述的***气溶胶产生介质的新型陶瓷发热体的端部，还包括一个尖端部，其可以由与发热基体自然延伸的部分，也可以是单 独制作的部分，解决便于***问题，所述的新型陶瓷发热体的发热基体和端部连接在一起。The structure of the new ceramic heating element according to the present invention includes any structural form that can be inserted into an aerosol medium. In a preferred embodiment of the present invention, the main body of the new ceramic heating element includes a heating base that generates heat by electricity, and its structure is Cylinder, elliptical cylinder, blade structure, prismatic structure, rectangular parallelepiped, etc. The end of the new ceramic heating element inserted into the aerosol generating medium also includes a tip portion, which can be naturally extended from the heating substrate The part can also be a separately manufactured part to solve the problem of easy insertion. The heating base and the end of the novel ceramic heating body are connected together.
所述的新型陶瓷发热体的尺寸可以根据气溶胶产生介质或者加热器具进行选择。在一个优选实施方式中，所述的新型陶瓷发热体的长度在5mm-60mm，优选8mm-45mm。The size of the novel ceramic heating element can be selected according to the aerosol generating medium or the heating device. In a preferred embodiment, the length of the new ceramic heating element is 5mm-60mm, preferably 8mm-45mm.
在本发明的一个优选实施方式中，所述的新型陶瓷发热体端部部分通过电流后也会产生部分热量，用于对气溶胶产生介质的加热。In a preferred embodiment of the present invention, part of the heat of the end portion of the new ceramic heating element will generate a part of heat after passing current, which is used to heat the aerosol generating medium.
在本发明的一个优选实施方式中，所述的新型陶瓷发热体的发热基体的长度大于新型陶瓷发热体的端部的长度。In a preferred embodiment of the present invention, the length of the heating base of the new ceramic heating element is greater than the length of the end of the new ceramic heating element.
所述的新型陶瓷发热体直接用于加热，其发热主体包括至少一个发热基体部分组成，在一个优选实施方式中，所述发热主体包括至少两个发热基体，所述发热基体的至少一个通过电流，用于发热。The novel ceramic heating body is directly used for heating, and its heating body includes at least one heating base part. In a preferred embodiment, the heating body includes at least two heating bases, and at least one of the heating bases passes current. , For fever.
在本发明的一个优选实施方式中，所述的新型陶瓷发热主体的发热基体之间留有间隙，或者用绝缘材料填充，或者用具有温度感应功能的传感器填充，其中，填充所述绝缘材料优选陶瓷、氧化锆、氮化铝、玻璃、陶土、氮化硼、碳化硅、镀层绝缘金属或合金等。In a preferred embodiment of the present invention, the gap between the heating substrates of the new ceramic heating body is filled with an insulating material or a sensor with a temperature sensing function, wherein the filling of the insulating material is preferred Ceramics, zirconia, aluminum nitride, glass, clay, boron nitride, silicon carbide, coated insulating metals or alloys, etc.
在本发明的一个优选实施方式中，所述的新型陶瓷发热主体由在温度和电阻之间具有限定关系的材料制成，使得所述的新型陶瓷发热体既能够用于加热气溶胶形成介质也能够用于实时监控发热器的温度。In a preferred embodiment of the present invention, the new ceramic heating body is made of a material having a limited relationship between temperature and resistance, so that the new ceramic heating body can be used both for heating an aerosol-forming medium and It can be used to monitor the temperature of the heater in real time.
所述的新型陶瓷发热体的第二部分的电极部分位于新型陶瓷发热主体的另一端，在一个优选实施方式中，所述的新型陶瓷发热主体的长度大于新型陶瓷发热体第二部分电极的长度。The electrode part of the second part of the new ceramic heating body is located at the other end of the new ceramic heating body. In a preferred embodiment, the length of the new ceramic heating body is longer than the length of the electrode of the second part of the new ceramic heating body .
在本发明的一个优选实施方式中，所述的新型陶瓷发热体的发热主体由包括以下的组合物制成：发热主体材料、发热稳定剂和粘结剂组成。In a preferred embodiment of the present invention, the heating body of the novel ceramic heating body is made of a composition including the following: a heating body material, a heating stabilizer and a binder.
所述的新型陶瓷发热体底座具有固定新型陶瓷发热体的功能，确保新型陶瓷发热体能够稳定的安装在气溶胶产生装置中。The new ceramic heating element base has the function of fixing the new ceramic heating element, ensuring that the new ceramic heating element can be stably installed in the aerosol generating device.
所述的新型陶瓷发热体底座通过电接点与新型陶瓷发热体电极连接并具有供电的功能。在一个优选实施方式中，所述的新型陶瓷发热体第二部分的电极既可以作为与新型陶瓷发热体底座连接的电接点，同时，亦可以将新型陶瓷发热体与新型陶瓷发热体底座固定连接的部件。The base of the new-type ceramic heating element is connected to the electrode of the new-type ceramic heating element through an electrical contact and has a power supply function. In a preferred embodiment, the electrode of the second part of the new ceramic heating body can be used as an electrical contact with the base of the new ceramic heating body, and at the same time, the new ceramic heating body can be fixedly connected to the new ceramic heating body base Parts.
所述的新型陶瓷发热体底座由耐高温、导热率低的材料制备而成，降低新型陶瓷发热体在产品中应用存在的问题，选用的材料能够耐受新型陶瓷发热体高温发热后。所述的耐高温材料包括有机材料和无机材料，例如聚醚醚酮、耐高温硅胶、聚四氟乙烯、陶瓷材料、氧化锆、氮化铝、碳化硅、玻璃等。The base of the new ceramic heating element is made of a material with high temperature resistance and low thermal conductivity, which reduces the problems in the application of the new ceramic heating element in the product. The selected material can withstand the high temperature heating of the new ceramic heating element. The high temperature resistant materials include organic materials and inorganic materials, such as polyether ether ketone, high temperature resistant silica gel, polytetrafluoroethylene, ceramic materials, zirconia, aluminum nitride, silicon carbide, glass, etc.
在本发明的一个优选实例中，所述的新型陶瓷发热体底座部分在小于底座尺寸基础上进 行凸起一部分，凸起部分带有电接点，具体的尺寸和结构上与新型陶瓷发热体第一部分发热主体部分尺寸和结构相同，或者凸起部分在尺寸和结构不同于新型陶瓷发热体第一部分发热主体部分尺寸和结构。凸起部分的尺寸，根据底座材料的特性进行选择，确保底座的温度不至于过高。In a preferred example of the present invention, the base portion of the new ceramic heating element is raised on the basis of smaller than the size of the base, and the raised portion has electrical contacts. The specific size and structure are the same as the first portion of the new ceramic heating element The size and structure of the heating body part are the same, or the size and structure of the convex part are different from those of the first part of the new type ceramic heating body. The size of the convex part is selected according to the characteristics of the base material to ensure that the temperature of the base is not too high.
另一方面，本发明还提供了一种制备上述陶瓷发热体的方法，其中，所述方法包括以下步骤：On the other hand, the present invention also provides a method for preparing the above ceramic heating element, wherein the method includes the following steps:
1)将发热主体材料、发热稳定剂按照所需比例进行配比，混合后得到混合料；1) Mix the heating body material and the heating stabilizer according to the required ratio, and then mix to obtain the mixture;
2)将混合料倒入研钵中，向混合料中加入所需比例的粘结剂作为成型剂，将料混匀，并进行造粒；2) Pour the mixture into the mortar, add the required proportion of binder to the mixture as a molding agent, mix the material, and granulate;
3)将配比好的发热体组合物置于密闭环境陈腐，以使粘结剂分布均匀，为坯体成型做准备；3) Place the heating element composition with good ratio in a closed environment and stale to make the binder evenly distributed and prepare for the molding of the green body;
4)采用半干压法成型，在一定的成型压力下将试样制成目标形状，试样压制成型过程先缓慢加压，以排出料中的空气；4) The semi-dry press method is used to form the sample into a target shape under a certain forming pressure. The sample is first pressed slowly during the press forming process to discharge the air in the material;
5)将成型好的试样置入的烘箱干燥；5) Dry the formed sample into the oven;
6)以一定的升温速率进行升温，并在多个温度区域进行保温烧制，再在1600-2600℃条件下烧结，制得发热体。6) The temperature is raised at a certain temperature increase rate, and heat preservation is fired in multiple temperature regions, and then sintered at 1600-2600°C to obtain a heating element.
7)将上述烧成的发热体与低导电率的金属或非金属电极部分放入真空焊接炉中焊接在一起。7) Put the fired heating element and the metal or non-metallic electrode part with low conductivity into a vacuum welding furnace to weld together.
在本发明的一个优选实例中，所述制备上述陶瓷发热体的制备方法包括以下步骤：In a preferred embodiment of the present invention, the method for preparing the ceramic heating element includes the following steps:
1)将发热主体材料、发热稳定剂按照所需比例进行配比，混合后得到混合料；1) Mix the heating body material and the heating stabilizer according to the required ratio, and then mix to obtain the mixture;
2)将混合料倒入研钵中，向混合料中加入所需比例的粘结剂作为成型剂，将料混匀，并进行造粒；2) Pour the mixture into the mortar, add the required proportion of binder to the mixture as a molding agent, mix the material, and granulate;
3)将配比好的发热体组合物置于密闭环境陈腐6-48小时，以使粘结剂分布均匀，为坯体成型做准备；3) Place the heating element composition with good ratio in a closed environment and stale for 6-48 hours to make the binder evenly distributed and prepare for green body molding;
4)采用半干压法成型，在1KN-500KN成型压力下将试样制成目标形状，试样压制成型过程先缓慢加压，以排出料中的空气，并在最终压力下保压5s-100s；4) Using semi-dry pressing method, the sample is made into the target shape under the molding pressure of 1KN-500KN. The sample is first pressed slowly during the compression molding process to discharge the air in the material, and the pressure is maintained at the final pressure for 5s- 100s;
5)将成型好的试样置入的90-100℃烘箱干燥6～18h；5) Place the formed samples in an oven at 90-100℃ for 6-18 hours;
6)以1-10℃/min的速度升温，在500℃、600℃、700℃、800℃、900℃、1000℃各保温20-120min，在最高烧成温度1600-2600℃保温30-300min，制得发热体。6) Heat up at a rate of 1-10°C/min, hold at 500°C, 600°C, 700°C, 800°C, 900°C, 1000°C for 20-120min each, and hold at the highest firing temperature of 1600-2600°C for 30-300min To produce a heating element.
7)将上述烧成的发热体与低导电率的金属或非金属电极部分放入真空焊接炉中焊接， 焊接时间6h-24h，焊接温度1200℃-1600℃。7) Put the fired heating element and the metal or non-metallic electrode part with low conductivity into a vacuum welding furnace for welding, the welding time is 6h-24h, and the welding temperature is 1200℃-1600℃.
上述步骤1)和步骤2)中的发热主体材料和发热稳定剂的粒度为400-1200目，优选的粒度为500-1000目。The particle size of the heat generating host material and the heat generating stabilizer in the above step 1) and step 2) is 400-1200 mesh, and the preferred particle size is 500-1000 mesh.
再一方面，本发明还提供了根据上述的新型陶瓷发热体组合物制备的新型陶瓷发热体在采用固体发烟介质或液体发烟介质的加热不燃烧卷烟和电子烟中的用途。In still another aspect, the present invention also provides the use of the new ceramic heating element prepared according to the above-mentioned new ceramic heating element composition in heating non-burning cigarettes and electronic cigarettes using a solid smoking medium or a liquid smoking medium.
根据本发明的新型陶瓷发热体组合物制备的新型陶瓷发热体不需要印刷电路，且可以一次烧成，制备工艺简单、发热快、发热均匀、低温电阻可测且稳定性高、误差小、成品率高的陶瓷发热体，在应用到采用固体发烟介质或液体发烟介质的加热不燃烧卷烟和电子烟中时，能够有效提高加热效率和可靠性、并获得稳定的用户体验。The novel ceramic heating element prepared according to the novel ceramic heating element composition of the present invention does not require a printed circuit and can be fired at one time. The preparation process is simple, the heating is fast, the heating is uniform, the low temperature resistance is measurable and the stability is high, the error is small, and the finished product The ceramic heating element with a high rate can effectively improve the heating efficiency and reliability and obtain a stable user experience when it is applied to heating non-burning cigarettes and electronic cigarettes using a solid smoking medium or a liquid smoking medium.
附图说明BRIEF DESCRIPTION
附图是用来提供对本发明的进一步理解，并且构成说明书的一部分，与下面的具体实施方式一起用于解释本发明，但并不构成对本发明的限制。在附图中：The drawings are used to provide a further understanding of the present invention, and constitute a part of the specification, together with the following specific embodiments to explain the present invention, but do not constitute a limitation of the present invention. In the drawings:
图1为本发明新型陶瓷发热体的截面示意图；1 is a schematic cross-sectional view of the new ceramic heating element of the present invention;
图2为本发明新型陶瓷发热体从电极方向的视图；2 is a view of the new ceramic heating element of the present invention from the direction of the electrode;
图3为本发明另一种新型陶瓷发热体从电极方向的视图；3 is a view of another new type ceramic heating element of the present invention from the direction of the electrode;
图4为本发明另一种新型陶瓷发热体从电极方向的视图；4 is a view of another novel ceramic heating element of the present invention from the direction of the electrode;
图5为本发明的新型陶瓷发热组件的截面示意图；5 is a schematic cross-sectional view of the novel ceramic heating component of the present invention;
[根据细则91更正 05.09.2019]　
图6为本发明另一种结构的新型陶瓷发热组件的截面示意图。[Correction according to Rule 91 05.09.2019]
6 is a schematic cross-sectional view of a new type ceramic heating element of another structure of the present invention.
图中：1-发热体端帽；2-发热基体；3-发热体电极；4-发热体内空腔；5-发热体底座；6-电极引线孔；7-凸型发热体底座；8二均分发热基体；9-二均分发热体空腔；10-四分型发热基体；11-四分型发热体空腔；12-二均分圆形发热基体；13-二均分发热体空腔；14-发热体底座凸起。In the picture: 1- heating element end cap; 2- heating element base; 3- heating element electrode; 4- heating element cavity; 5- heating element base; 6-electrode lead hole; 7- convex heating element base; 8 two Uniform heat distribution body; 9-two uniform heat distribution cavity; 10-quarter heat-generating base; 11-quarter heat-generating cavity; 12-two-equal heat-generating base; 13-two-equal heat distribution Cavity; 14- heating body base raised.
具体实施方式detailed description
以下对本发明的具体实施方式进行详细说明。应当理解的是，此处所描述的具体实施方式仅用于说明和解释本发明，并不用于限制本发明。The specific embodiments of the present invention will be described in detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention, and are not intended to limit the present invention.
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值，这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说，各个范围的端点值之间、各个范围的端点值和单独的点值之间，以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围，这些数值范围应被视为在本文中具体公开。The endpoints and any values of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, between the end points of each range, between the end points of each range and individual point values, and between individual point values can be combined with each other to obtain one or more new numerical ranges, these values The scope should be considered as specifically disclosed herein.
一方面，本发明提供了一种新型陶瓷发热体，其中，所述新型陶瓷发热体包括第一部分 和第二部分，具体的第一部分为发热主体部分，第二部分为电极部分。In one aspect, the present invention provides a new type of ceramic heating element, wherein the new type of ceramic heating element includes a first part and a second part, in particular the first part is a heating body part, and the second part is an electrode part.
本发明所述的新型陶瓷发热体的发热主体部由包括以下的组合物制成：发热主体材料、发热稳定剂和粘结剂组成。The heat-generating body part of the novel ceramic heat-generating body according to the present invention is made of a composition including the following: a heat-generating body material, a heat-generating stabilizer and a binder.
碳化物、氮化物是中的一些物质具有金属的特性，具有高硬度、切割性和导电性等特性，例如碳化钛、碳化硅、碳化钨、氮化钛、氮化钒、氮化锆、氮化钽、氮化锰、氮化钨、氮化硅、氮化硼、氮化铜、氮化锌、氮化银等，同时，MoSi 2是Mo-Si二元合金系中含硅量最高的一种中间相，是成分固定的道尔顿型金属间化合物。具有金属与陶瓷的双重特性，是一种性能优异的高温材料。很好的高温抗氧化性，抗氧化温度高达1600℃以上，与SiC相当，具有良好的电热传导性。但是这类物质在低温或常温下电阻测量误差大，不易在低温下使用，为提高低温的可以行。本发明所述的新型陶瓷发热体组合物发热主体材料包括碳化物、氮化物、二硅化钼等的至少一种，所述的碳化物包括碳化钛、碳化硅、碳化钨、所述的氮化物包括氮化钛、氮化钒、氮化锆、氮化钽、氮化锰、氮化钨、氮化硅、氮化硼、氮化铜、氮化锌、氮化银等，在本发明的一个优选实例中，所述的发热主体材料占新型陶瓷发热体组合物的百分数为60％-99.5％，优选63％-98％，更优选65％-95％。 Carbides and nitrides are some of the substances that have the characteristics of metals, such as high hardness, cutting and conductivity, such as titanium carbide, silicon carbide, tungsten carbide, titanium nitride, vanadium nitride, zirconium nitride, nitrogen Tantalum, manganese nitride, tungsten nitride, silicon nitride, boron nitride, copper nitride, zinc nitride, silver nitride, etc. At the same time, MoSi 2 is the highest silicon content in the Mo-Si binary alloy system An intermediate phase is a Dalton-type intermetallic compound with a fixed composition. With the dual characteristics of metal and ceramic, it is a high-temperature material with excellent performance. Very good high temperature oxidation resistance. The oxidation resistance temperature is as high as 1600℃ or more, which is equivalent to SiC and has good electrothermal conductivity. However, this kind of material has a large resistance measurement error at low temperature or normal temperature, and it is not easy to use it at low temperature. It is feasible to increase the low temperature. The novel ceramic heating body composition of the present invention includes at least one kind of heating body material of carbide, nitride, molybdenum disilicide, etc. The carbide includes titanium carbide, silicon carbide, tungsten carbide, and the nitride Including titanium nitride, vanadium nitride, zirconium nitride, tantalum nitride, manganese nitride, tungsten nitride, silicon nitride, boron nitride, copper nitride, zinc nitride, silver nitride, etc. In a preferred example, the percentage of the heating body material in the new ceramic heating body composition is 60% to 99.5%, preferably 63% to 98%, and more preferably 65% to 95%.
经过本发明人的反复试验研究发现，碳化物、氮化物和二硅化钼中添加发热稳定剂可以显著的提升所制备的陶瓷发热体的低温电阻可测性，并且具有稳定性高、误差小发热均匀、发热快的特点。After repeated experiments and researches by the present inventors, it has been found that the addition of heating stabilizers to carbides, nitrides and molybdenum disilicide can significantly improve the low-temperature resistance testability of the prepared ceramic heating body, and has high stability and small errors. Uniform and fast heating characteristics.
本发明所述的新型陶瓷发热体组合物发热稳定剂主要包括石墨烯、钛、钒、铬、锰、铁、钴、镍、铜、锌、钇、钼、钌、铑、钯、银、钨、金、铂、铱、及前述金属氧化物、前述金属合金等的至少一种，在本发明的一个优选实例中，所述的发热稳定剂占新型陶瓷发热体组合物的百分数为0.2％-35％，优选0.5％-30％，更优选1％-25％。The novel ceramic heating element composition heating stabilizer of the present invention mainly includes graphene, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, molybdenum, ruthenium, rhodium, palladium, silver, tungsten , Gold, platinum, iridium, and at least one of the foregoing metal oxides, the foregoing metal alloys, etc. In a preferred embodiment of the present invention, the heat stabilizer accounts for 0.2% of the new ceramic heating element composition 35%, preferably 0.5%-30%, more preferably 1%-25%.
根据本发明，对本发明的新型陶瓷发热体组合物粘结剂的种类和用量没有特别的限定，可以为本领域中常见的粘结剂种类和用量。在本发明的一个优选实施方式中，所述的粘结剂为酯类、树脂类、纤维类、醇及多元醇等。具体的如羧甲基纤维素、聚乙烯醇、乙基纤维素、淀粉、水玻璃、合成树脂等的至少一种，所述的粘结剂占新型陶瓷发热体组合物的百分数为0.3％-30％，优选0.5％-25％，更优选1％-20％。According to the present invention, the type and amount of the binder of the novel ceramic heating element composition of the present invention are not particularly limited, and may be the type and amount of binders common in the art. In a preferred embodiment of the present invention, the binders are esters, resins, fibers, alcohols, polyols and the like. Specifically, at least one of carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, starch, water glass, synthetic resin, etc. The binder accounts for 0.3% of the new ceramic heating element composition. 30%, preferably 0.5%-25%, more preferably 1%-20%.
根据本发明，对新型陶瓷发热体电极部分的材质没有特别的限制，可以采用本领域中常见的低导电率金属或非金属，例如包括铜、锌、镍、铬、金、银、铂、铝、铁、钴、硅、碳化硅、及前述金属的合金等的至少一种。According to the present invention, the material of the electrode part of the new ceramic heating element is not particularly limited, and metals or non-metals with low conductivity that are common in the art, such as copper, zinc, nickel, chromium, gold, silver, platinum, and aluminum, can be used , Iron, cobalt, silicon, silicon carbide, and alloys of the foregoing metals.
根据本发明，对“焊接”工艺没有特别的限制，可以采用本领域中常见的合适手段，例如将烧成的发热主体与低导电率的金属或非金属电极部分放入真空焊接炉中焊接。According to the present invention, there is no particular limitation on the "welding" process, and suitable means common in the art may be used, such as placing the fired heating body and the metal or non-metallic electrode part of low conductivity into a vacuum welding furnace for welding.
以下结合具体的新型陶瓷发热体结构对所属的新型陶瓷发热体的结构进行说明，但是不构成对发明的具体限定。The structure of the new ceramic heating element will be described below with reference to the specific structure of the new ceramic heating element, but it does not constitute a specific limitation on the invention.
图1所示的为本发明提供的一种新型陶瓷发热体的示意图的横截面，所述的新型陶瓷发热体主要由发热体端帽1、发热基体2、发热体电极3和发热体内空腔4等四部分组成。FIG. 1 is a schematic cross section of a novel ceramic heating element provided by the present invention. The new ceramic heating element mainly includes a heating element end cap 1, a heating base 2, a heating element electrode 3, and a cavity in the heating element 4 four parts.
所述的发热体电极3与外部电源连接，外部电源通过发热体电极3对新型陶瓷发热体进行供电，根据本发明，对新型陶瓷发热体电极部分的材质没有特别的限制，可以采用本领域中常见的低导电率金属或非金属，在一个优选实施方式中，所述的发热体电极3由低电导率金属、非金属中的至少一种组成，例如包括铜、锌、镍、铬、金、铂、银、铝、铁、钴、硅、碳化硅、及前述金属的合金等的至少一种，在一个优选实施方式中，电极采用铜、金、银、铂等制备而成。The heating element electrode 3 is connected to an external power source, and the external power source supplies power to the new ceramic heating element through the heating element electrode 3. According to the present invention, the material of the electrode portion of the new ceramic heating element is not particularly limited, and can be used in the art Common low conductivity metal or non-metal. In a preferred embodiment, the heating element electrode 3 is composed of at least one of low conductivity metal and non-metal, such as copper, zinc, nickel, chromium, gold , Platinum, silver, aluminum, iron, cobalt, silicon, silicon carbide, and alloys of the foregoing metals, etc. In a preferred embodiment, the electrode is made of copper, gold, silver, platinum, or the like.
所述的电流通过发热基体2和发热体端帽1形成的电流回路后，发热基体2由于电流的通过会发热，达到加热的目的。在本发明的一个优选实施方式中，所述的发热体端帽1通过电流后也会产生部分热量，用于对气溶胶产生介质的加热。其中，所述的发热基体2加热温度到220℃到大约500℃，优选的，发热基体2的温度在250℃到大约340℃。After the current passes through the current loop formed by the heating base 2 and the end cap 1 of the heating body, the heating base 2 will generate heat due to the passage of the current to achieve the purpose of heating. In a preferred embodiment of the present invention, the heat-generating body end cap 1 will also generate a part of heat after passing an electric current, which is used to heat the aerosol generating medium. Wherein, the heating temperature of the heating substrate 2 is from 220°C to about 500°C, preferably, the temperature of the heating substrate 2 is from 250°C to about 340°C.
图1所示的为新型陶瓷发热体的示意图的横截面，所述的新型陶瓷发热体的形状及结构可以为圆柱体、椭圆主体、刀片式结构、棱形结构、长方体等，所述的新型陶瓷发热体的尺寸可以根据气溶胶产生介质或者加热器具进行选择。在一个优选实施方式中，所述的新型陶瓷发热体的长度在5mm-60mm，优选8mm-45mm。FIG. 1 is a schematic cross section of a new type ceramic heating element. The shape and structure of the new type ceramic heating element can be a cylinder, an elliptical body, a blade structure, a prismatic structure, a rectangular parallelepiped, etc. The size of the ceramic heating element can be selected according to the aerosol generating medium or the heating device. In a preferred embodiment, the length of the new ceramic heating element is 5mm-60mm, preferably 8mm-45mm.
所述的新型陶瓷发热基体2的长度大于新型陶瓷发热体端帽1的长度，所述的新型陶瓷发热基体2的长度大于新型陶瓷发热体电极3的长度。The length of the new ceramic heating base 2 is greater than the length of the end cap 1 of the new ceramic heating body, and the length of the new ceramic heating base 2 is greater than the length of the electrode 3 of the new ceramic heating body.
所述的新型陶瓷发热基体2至少由两个发热基体部分组成，并且所述发热基体部分至少一个通过电流，用于发热。图2、图3和图4列出了不同类型的新型陶瓷发热体从电极方向的视图，图2所示的为圆柱形发热体，所述的发热基体为二均分发热基体，基本结构由二均分发热基体8和二均分发热体空腔9组成，图3所示的为圆柱形发热体，所述的发热基体为四均分发热基体，基本结构由四分型发热基体10和四分型发热体空腔11组成，图4所示的亦为圆柱形二均分发热基体，基本结构由二均分圆形发热基体12和二均分发热体空腔13组成。The novel ceramic heating base 2 is composed of at least two heating base parts, and at least one of the heating base parts passes current to generate heat. Figures 2, 3 and 4 list different types of new ceramic heating elements from the direction of the electrode. Figure 2 shows a cylindrical heating element. The heating substrate is a two-equal distribution heating substrate. The basic structure is The two-part heat distribution base 8 and the two-part heat distribution cavity 9 consist of a cylindrical heating body. The heating base is a four-part heat distribution base. The basic structure consists of a four-part heating base 10 and The quadrant-type heating body cavity 11 is composed of a cylindrical two-part heat distributing heat matrix as shown in FIG. 4, and the basic structure is composed of a two-part heat distributing base 12 and a two-body heat distributing cavity 13.
所述的新型陶瓷发热基体2之间留有发热体内空腔4，或者发热体内空腔4用绝缘材料填充，或者发热体内空腔4用具有温度感应功能的传感器填充，在一个优选实施方式中，填充的所述绝缘材料优选陶瓷、氧化锆、氮化铝、玻璃、陶土、氮化硼、碳化硅、镀层绝缘金属或合金等的至少一种。The cavity 4 in the heating body is left between the novel ceramic heating substrate 2, or the cavity 4 in the heating body is filled with an insulating material, or the cavity 4 in the heating body is filled with a sensor having a temperature sensing function, in a preferred embodiment Preferably, the filled insulating material is at least one of ceramic, zirconia, aluminum nitride, glass, clay, boron nitride, silicon carbide, coated insulating metal or alloy.
所述的新型陶瓷发热基体2由在温度和电阻之间具有限定关系的材料制成，使得所述的新型陶瓷发热体既能够用于加热气溶胶形成介质也能够用于实时监控发热体的温度。The new ceramic heating base 2 is made of a material having a limited relationship between temperature and resistance, so that the new ceramic heating body can be used not only for heating an aerosol-forming medium but also for real-time monitoring of the temperature of the heating body .
所述的新型陶瓷发热基体2通过由发热主体材料、发热稳定剂和粘结剂组成的组合物制备。主体材料包括碳化物、氮化物、二硅化钼等的至少一种，所述的碳化物包括碳化钛、碳 化硅、碳化钨、所述的氮化物包括氮化钛、氮化钒、氮化锆、氮化钽、氮化锰、氮化钨、氮化硅、氮化硼、氮化铜、氮化锌、氮化银等。发热稳定剂包括石墨烯、钛、钒、铬、锰、铁、钴、镍、铜、锌、钇、钼、钌、铑、钯、银、钨、金、铂、铱、及前述金属氧化物、前述金属合金等的至少一种。粘结剂为常见粘结剂，包括酯类、树脂类、纤维类、醇及多元醇等。具体的如羧甲基纤维素、聚乙烯醇、乙基纤维素、淀粉、水玻璃、合成树脂等的至少一种。所述的发热主体材料占新型陶瓷发热体组合物的百分数为60％-99.5％，所述的发热稳定剂占新型陶瓷发热体组合物的百分数为0.2％-35％，所述的粘结剂占新型陶瓷发热体组合物的百分数为0.3％-30％。The novel ceramic heating substrate 2 is prepared by a composition composed of a heating body material, a heating stabilizer and a binder. The host material includes at least one of carbide, nitride, molybdenum disilicide, etc., the carbide includes titanium carbide, silicon carbide, tungsten carbide, and the nitride includes titanium nitride, vanadium nitride, zirconium nitride , Tantalum nitride, manganese nitride, tungsten nitride, silicon nitride, boron nitride, copper nitride, zinc nitride, silver nitride, etc. Heat stabilizers include graphene, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, molybdenum, ruthenium, rhodium, palladium, silver, tungsten, gold, platinum, iridium, and the foregoing metal oxides , At least one of the aforementioned metal alloys. Binders are common binders, including esters, resins, fibers, alcohols and polyols. Specific examples include at least one of carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, starch, water glass, and synthetic resin. The heating body material accounts for 60%-99.5% of the new ceramic heating body composition, the heating stabilizer accounts for 0.2%-35% of the new ceramic heating body composition, and the binder The percentage of the new ceramic heating element composition is 0.3%-30%.
所述的新型陶瓷发热体端帽1与发热基体2可以由相同的材料制成，或者由不同的材料制成。The novel ceramic heating body end cap 1 and the heating base body 2 can be made of the same material or different materials.
图5所示的为本发明具有新型陶瓷发热体底座的新型陶瓷发热组件的截面示意图，主要由发热体端冒1、发热基体2、发热体电极3、发热体内空腔4、发热体底座5和电极引线孔6等几部分组成，所述的发热体底座由发热体底座5、电极点(发热体电极3固定点)和电极引线孔6等组成，具有固定新型陶瓷发热体的功能，确保新型陶瓷发热体能够稳定的安装在气溶胶产生装置中。5 is a schematic cross-sectional view of a new ceramic heating element with a new ceramic heating element base according to the present invention, which is mainly composed of a heating element end 1, a heating base 2, a heating element electrode 3, a heating body cavity 4 and a heating element base 5 It is composed of electrode lead hole 6 and other parts. The heating element base is composed of heating element base 5, electrode point (heating element electrode 3 fixed point) and electrode lead hole 6, etc. It has the function of fixing new ceramic heating element to ensure The new ceramic heating element can be stably installed in the aerosol generating device.
所述的发热体底座通过电接点与发热体电极连接并具有供电的功能。所述的发热体电极3既可以作为与发热体底座5连接的电接点，同时，亦可以将新型陶瓷发热体与发热体底座固定连接的部件。在发热体内空腔4内可以不填充任何物质，或者发热体内空腔4用绝缘材料填充，或者发热体内空腔4用具有温度感应功能的传感器填充，在一个优选实施方式中，所述的填充绝缘材料优选陶瓷、氧化锆、氮化铝、玻璃、陶土、氮化硼、碳化硅、镀层绝缘金属或合金等的至少一种。The heating element base is connected to the heating element electrode through electrical contacts and has a power supply function. The heating element electrode 3 can be used as an electrical contact to connect with the heating element base 5, and at the same time, it can also be a component that connects the new type ceramic heating element to the heating element base. The cavity 4 of the heating body may not be filled with any substance, or the cavity 4 of the heating body is filled with an insulating material, or the cavity 4 of the heating body is filled with a sensor having a temperature sensing function. In a preferred embodiment, the filling The insulating material is preferably at least one of ceramics, zirconia, aluminum nitride, glass, clay, boron nitride, silicon carbide, coated insulating metal, or alloy.
所述的发热体底座5由耐高温、导热率低的材料制备而成，降低新型陶瓷发热体在后续产品中应用存在的问题，选用的材料能够耐受新型陶瓷发热体高温发热后，通过电池连接处传导过来的热量，所述的耐高温材料包括有机材料和无机材料，例如聚醚醚酮、耐高温硅胶、聚四氟乙烯、陶瓷材料、氧化锆、氮化铝、碳化硅、玻璃等，或者材料与新型陶瓷发热体的材料相同。The heating element base 5 is made of a material with high temperature resistance and low thermal conductivity, which reduces the problems of the application of the new ceramic heating element in subsequent products. The selected materials can withstand the high temperature heating of the new ceramic heating element and pass through the battery. The heat transferred from the connection. The high temperature resistant materials include organic materials and inorganic materials, such as polyetheretherketone, high temperature resistant silica gel, polytetrafluoroethylene, ceramic materials, zirconia, aluminum nitride, silicon carbide, glass, etc. Or, the material is the same as that of the new ceramic heating element.
图6所示的为凸型发热体底座7替代常规型发热体底座5，该种底座具有一个发热体底座凸起14，所述的发热体底座凸起14在的尺寸小于凸型发热体底座7，凸型发热体底座7带有电接点，具体的尺寸和结构上与发热体电极3尺寸和结构相同，或者凸型发热体底座7在尺寸和结构不同于发热基体2组成的新型陶瓷发热体尺寸和结构。凸型发热体底座7的高度，根据底座材料的特性进行选择，确保底座的温度不至于过高，选用的材料亦可以与发热体的材料相同或者不同。FIG. 6 shows that the convex heating element base 7 replaces the conventional heating element base 5, and this type of base has a heating element base protrusion 14 whose size is smaller than that of the convex heating element base 7. The convex heating element base 7 has electrical contacts, the specific size and structure are the same as those of the heating element electrode 3, or the convex heating element base 7 is different from the new type ceramic heating element composed of the heating base 2 in size and structure Body size and structure. The height of the base 7 of the convex heating element is selected according to the characteristics of the base material to ensure that the temperature of the base is not too high, and the selected material may be the same as or different from the material of the heating element.
下面对新型陶瓷发热体中关键部分发热基体2的制备工艺及配方进行实例阐述和说明。In the following, the preparation process and formulation of the key part of the heating element 2 in the new ceramic heating element are explained and illustrated by examples.
实施例1Example 1
新型陶瓷发热体制备工艺及步骤实施步骤：New ceramic heating element preparation process and steps implementation steps:
1)将发热主体材料碳化钛按质量百分比为95％与发热稳定剂石墨烯质量百分比为2.5％进行配比，在球磨机中混合得到混合料；1) Mix the heating body material titanium carbide with a mass percentage of 95% and a heating stabilizer graphene mass percentage of 2.5%, and mix in a ball mill to obtain a mixture;
2)将混合料倒入研钵中，向混合料中加入质量百分比为2.5％的PVA作为成型粘结剂，将料混匀，并进行造粒；2) Pour the mixture into a mortar, add 2.5% by mass of PVA as a molding binder to the mixture, mix the material, and granulate;
3)将配比好的发热体组合物置于密闭环境陈腐12h，以使粘结剂PVA分布均匀，为坯体成型做准备；3) Place the heating element composition with good ratio in a sealed environment and stale for 12h to make the binder PVA evenly distributed and prepare for green body molding;
4)采用半干压法成型，在100KN成型压力下将试样制成目标形状，试样压制成型过程先缓慢加压，以排出料中的空气，并在最终压力下保压60s；4) The semi-dry press method is used to form the sample into the target shape at a molding pressure of 100KN. The sample is first slowly pressed during the press molding process to discharge the air in the material and maintain the pressure for 60 seconds at the final pressure;
5)将成型好的试样置入95～100℃的烘箱干燥12h；5) Place the formed sample in an oven at 95～100℃ for 12 hours;
6)以5℃/min的速度升温，在500℃、600℃、700℃、800℃、900℃、1000℃各保温60min，在最高烧成温度1600-2600℃保温120min，烧成发热体；6) Increase the temperature at a rate of 5°C/min, hold at 500°C, 600°C, 700°C, 800°C, 900°C, and 1000°C for 60 minutes each, and hold at the highest firing temperature of 1600-2600°C for 120 minutes, and fire the heating element;
7)将上述烧成的发热体与镍铬合金电极部分放入真空焊接炉中焊接，焊接时间8h，焊接温度1200℃-1600℃。7) Put the calcined heating element and the nickel-chromium alloy electrode part into a vacuum welding furnace for welding, welding time is 8h, welding temperature is 1200℃-1600℃.
对照实施例采用纯的碳化钛作为发热主体材料，不添加发热稳定剂，其粘合剂等按照实施例1比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与实施例1中进行相同测试，并进行比较。In the comparative example, pure titanium carbide is used as the main heating material, no heating stabilizer is added, the binder and the like are in accordance with the ratio of Example 1, and the preparation method and steps are carried out as in Example 1. The same test was performed in Example 1 and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表1所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000001
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表2所示。从表2中看以看出实施例1的平均偏差率只有2.02，对照的平均偏差率达到了9.27，是实施例1中的4.59倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 1. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000001
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (the resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 2. It can be seen from Table 2 that the average deviation rate of Example 1 is only 2.02, and the average deviation rate of the control reaches 9.27, which is 4.59 times that of Example 1, indicating that after adding a heating stabilizer to the new ceramic heating element, the product resistance The stability is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表3。 从表3中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为2018次，实施例1平均极限热循环测试次数为3021次，是实施例1中的1.5倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 3 for details. It can be seen from Table 3 that the average limit thermal cycle test number of the control when half the resistance value is twice the initial resistance is 2018, and the average limit thermal cycle test number of Example 1 is 3021 times, which is 1.5 times, which means that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表1Table 1
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8585 8686 8585 8383 8181 8484
实施例1Example 1 9494 9595 9595 9393 9292 9494
表2Table 2
Figure PCTCN2019097568-appb-000002
Figure PCTCN2019097568-appb-000002
表3table 3
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 20872087 18951895 21562156 20162016 19851985 20282028
实施例1Example 1 28762876 30833083 29572957 31213121 30673067 30213021
实施例2Example 2
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表4所示：The preparation process and step implementation steps of the new ceramic heating element are prepared in accordance with step 1)-step 7 in Example 1. The specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 4 below:
表4Table 4
名称name 发热主体材料Heating body material 发热稳定剂Fever stabilizer 粘结剂Binder
物质名称Substance name 碳化硅Silicon carbide 钛titanium 羧甲基纤维素Carboxymethyl cellulose
组分比例(％)Component ratio (%) 8585 1010 55
对照实施例采用纯的碳化硅作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表4比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例中样品进行相同测试，并进行比较。In the comparative example, pure silicon carbide is used as the main body material for heating, no heating stabilizer is added, the binder and the like are in proportion to Table 4, and the preparation method and steps are carried out as in Example 1. The heating element prepared is the same as this embodiment The samples in the example were tested the same and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表5所示。用电阻测定仪测定其低温电阻(25℃)，根据5 个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000003
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表6所示。从表6中看以看出本实例的平均偏差率只有3.00，对照的平均偏差率达到了8.43，是本实例中的2.81倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 5. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R5, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000003
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 6 for details. It can be seen from Table 6 that the average deviation rate of this example is only 3.00, and the average deviation rate of the control has reached 8.43, which is 2.81 times that of this example, indicating that the stability of the product resistance after the new ceramic heating element is added with a heating stabilizer The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表7。从表7中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1914次，本实施中样品平均极限热循环测试次数为2883次，是本实例中的1.51倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 7 for details. It can be seen from Table 7 that when the half resistance value in the control is 1914 times the average limit thermal cycle test after the initial resistance is 2 times, the average limit thermal cycle test times of the sample in this implementation is 2883 times 1.51 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表5table 5
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8787 8585 8888 8686 8484 8686
实施例2Example 2 9595 9696 9595 9393 9797 9595
表6Table 6
Figure PCTCN2019097568-appb-000004
Figure PCTCN2019097568-appb-000004
表7Table 7
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 19851985 18761876 18991899 18761876 19361936 19141914
实施例2Example 2 27662766 28522852 29782978 29252925 28932893 28832883
实施例3Example 3
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表8所示：The preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1. The specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 8 below:
表8Table 8
名称name 发热主体材料Heating body material 发热稳定剂Fever stabilizer 粘结剂Binder
物质名称Substance name 碳化钨Tungsten carbide 钒vanadium 羧甲基纤维素Carboxymethyl cellulose
组分比例(％)Component ratio (%) 99.599.5 0.20.2 0.30.3
对照实施例采用纯的碳化钨作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表8比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure tungsten carbide is used as the main heating material, no heating stabilizer is added, the binder and the like are according to the ratio in Table 8, and the preparation method and steps are carried out as in Example 1. The heating element produced is the same as this embodiment The same test was carried out in the sample and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表9所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000005
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表10所示。从表10中看以看出本实例的平均偏差率只有3.58，对照的平均偏差率达到了7.85，是本实例中的2.81倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 9. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000005
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (the resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 10. From Table 10, it can be seen that the average deviation rate of this example is only 3.58, and the average deviation rate of the control has reached 7.85, which is 2.81 times that of this example. The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表11。从表11中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为2067次，本实施中样品平均极限热循环测试次数为3029次，是本实例中的1.47倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 11 for details. It can be seen from Table 11 that in the control, the average limit thermal cycle test number after the half resistance value is twice the initial resistance is 2067, and the average limit thermal cycle test number of the sample in this implementation is 3029 times, which is in this example. 1.47 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表9Table 9
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8585 8686 8585 8888 8282 8585
实施例3Example 3 9494 9393 9595 9494 9696 9494
表10Table 10
Figure PCTCN2019097568-appb-000006
Figure PCTCN2019097568-appb-000006
表11Table 11
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 20112011 21332133 20642064 20812081 20482048 20672067
实施例3Example 3 30663066 30143014 29832983 29712971 31103110 30293029
实施例4Example 4
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表12所示：The preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1. The specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 12 below:
表12Table 12
名称name 发热主体材料Heating body material 发热稳定剂Fever stabilizer 粘结剂Binder
物质名称Substance name 氮化钛Titanium nitride 铬chromium 聚乙烯醇Polyvinyl alcohol
组分比例(％)Component ratio (%) 8888 77 55
对照实施例采用纯的氮化钛作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表12比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure titanium nitride was used as the main heating material, no heating stabilizer was added, and the binder was prepared according to the ratio in Table 12, and the preparation method and steps were carried out as in Example 1. The same test was carried out in the samples of the examples and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表13所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000007
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表14所示。从表14中看以看出本实例的平均偏差率只有3.16，对照的平均偏差率达到了11.8，是本实例中的3.73倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 13. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000007
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 14 for details. It can be seen from Table 14 that the average deviation rate of this example is only 3.16, and the average deviation rate of the control has reached 11.8, which is 3.73 times that of this example, indicating that the stability of the product resistance after the new ceramic heating element is added with a heating stabilizer The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个 批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表15。从表15中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1788次，本实施中样品平均极限热循环测试次数为2527次，是本实例中的1.41倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 15 for details. It can be seen from Table 15 that in the control, when the half resistance value is twice the initial resistance, the average limit thermal cycle test number is 1788 times, and the average limit thermal cycle test number of the sample in this implementation is 2527 times, which is in this example. 1.41 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表13Table 13
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8888 8585 8383 8484 8181 8484
实施例4Example 4 9595 9494 9393 9595 9595 9494
表14Table 14
Figure PCTCN2019097568-appb-000008
Figure PCTCN2019097568-appb-000008
表15Table 15
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 16871687 17831783 18921892 17021702 18751875 17881788
实施例4Example 4 24672467 25312531 24782478 26122612 25482548 25272527
实施例5Example 5
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表16所示：The preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1. The specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 16 below:
表16Table 16
Figure PCTCN2019097568-appb-000009
Figure PCTCN2019097568-appb-000009
对照实施例采用纯的氮化钒和氮化锆作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表16比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure vanadium nitride and zirconium nitride were used as the main heating materials, no heating stabilizer was added, and the binder was prepared according to the ratio in Table 16, and the preparation methods and steps were carried out as in Example 1. The heating element was subjected to the same test as the sample of this example and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表17所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000010
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表18所示。从表18中看以看出本实例的平均偏差率只有3.95，对照的平均偏差率达到了9.48，是本实例中的2.40倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above-mentioned preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 17. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000010
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 18. From Table 18, it can be seen that the average deviation rate of this example is only 3.95, and the average deviation rate of the control has reached 9.48, which is 2.40 times that of this example. The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表19。从表19中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1811次，本实施中样品平均极限热循环测试次数为2557次，是本实例中的1.41倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 19 for details. It can be seen from Table 19 that in the control, the average limit thermal cycle test number after the half resistance value is twice the initial resistance is 1811 times, and the average limit thermal cycle test number of the sample in this implementation is 2557 times, which is in this example. 1.41 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表17Table 17
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8585 8686 8888 8787 8585 8686
实施例5Example 5 9595 9393 9696 9696 9494 9595
表18Table 18
Figure PCTCN2019097568-appb-000011
Figure PCTCN2019097568-appb-000011
Figure PCTCN2019097568-appb-000012
Figure PCTCN2019097568-appb-000012
表19Table 19
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 17841784 18751875 17931793 18341834 17671767 18111811
实施例5Example 5 25432543 25922592 25122512 25282528 26112611 25572557
实施例6Example 6
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表20所示：The preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1. The specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 20 below:
表20Table 20
Figure PCTCN2019097568-appb-000013
Figure PCTCN2019097568-appb-000013
对照实施例采用纯的氮化钽和氮化锰作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表20比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure tantalum nitride and manganese nitride were used as the main heating materials, no heating stabilizer was added, and the binder was prepared according to the ratio in Table 20. The heating element was subjected to the same test as the sample of this example and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表21所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000014
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表22所示。从表22中看以看出本实例的平均偏差率只有2.36，对照的平均偏差率达到了6.30，是本实例中的2.67倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above-mentioned preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 21. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000014
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 22 for details. It can be seen from Table 22 that the average deviation rate of this example is only 2.36, and the average deviation rate of the control has reached 6.30, which is 2.67 times that of this example, indicating that the stability of the product resistance after the new ceramic heating element is added with a heating stabilizer The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表23。从表23中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1879次，本实施中样品平均极限热循环测试次数为2770次，是本实例中的1.47倍，说明添加了 新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 23 for details. From Table 23, it can be seen that the average limit thermal cycle test number of the control after half the resistance value is twice the initial resistance is 1879 times, and the average limit thermal cycle test number of the sample in this implementation is 2770 times, which is in this example. 1.47 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表21Table 21
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8888 8989 8484 8585 8787 8787
实施例6Example 6 9494 9595 9898 9696 9797 9696
表22Table 22
Figure PCTCN2019097568-appb-000015
Figure PCTCN2019097568-appb-000015
表23Table 23
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 18941894 17671767 19341934 18321832 19681968 18791879
实施例6Example 6 27652765 28562856 28252825 27942794 26112611 27702770
实施例7Example 7
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表24所示：The preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1. The specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 24 below:
表24Table 24
Figure PCTCN2019097568-appb-000016
Figure PCTCN2019097568-appb-000016
对照实施例采用纯的氮化钽和氮化锰作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表24比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure tantalum nitride and manganese nitride were used as the main heating materials, no heating stabilizer was added, and the binder was prepared according to the ratio in Table 24. The preparation method and steps were carried out as in Example 1. The heating element was subjected to the same test as the sample of this example and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表25所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000017
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表26所示。从表26中看以看出本实例的平均偏差率只有3.04，对照的平均偏差率达到了8.75，是本实例中的2.87倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 25. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000017
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 26. It can be seen from Table 26 that the average deviation rate of this example is only 3.04, and the average deviation rate of the control has reached 8.75, which is 2.87 times that of this example, indicating that the stability of the product resistance after the new ceramic heating element is added with a heating stabilizer The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表27。从表27中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1617次，本实施中样品平均极限热循环测试次数为2606次，是本实例中的1.61倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 27 for details. From Table 27, it can be seen that the average limit thermal cycle test number after the half resistance value is twice the initial resistance in the control is 1617 times, the average limit thermal cycle test number of the sample in this implementation is 2606 times, which is 1.61 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表25Table 25
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8282 8989 8484 8484 8686 8585
实施例7Example 7 9595 9393 9898 9797 9595 9696
表26Table 26
Figure PCTCN2019097568-appb-000018
Figure PCTCN2019097568-appb-000018
表27Table 27
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 15651565 16541654 16281628 599599 16381638 14171417
实施例7Example 7 24572457 26822682 26372637 25912591 26632663 26062606
实施例8Example 8
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表28所示：The preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1)-step 7) in Example 1, the specific heating main material, heating stabilizer and binder components and proportions are shown in Table 28 below:
表28Table 28
Figure PCTCN2019097568-appb-000019
Figure PCTCN2019097568-appb-000019
对照实施例采用纯的氮化硼和氮化铜作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表28比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure boron nitride and copper nitride were used as the main body materials for heat generation, no heat stabilizer was added, and the binder was prepared according to the ratio in Table 28. The preparation methods and steps were carried out as in Example 1. The heating element was subjected to the same test as the sample of this example and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表29所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000020
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表30所示。从表30中看以看出本实例的平均偏差率只有3.07，对照的平均偏差率达到了8.79，是本实例中的2.86倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above-mentioned preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 29. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000020
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 30. From Table 30, it can be seen that the average deviation rate of this example is only 3.07, and the average deviation rate of the control has reached 8.79, which is 2.86 times that of this example. The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表31。从表31中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1544次，本实施中样品平均极限热循环测试次数为2692次，是本实例中的1.74倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 31 for details. From Table 31, it can be seen that the average limit thermal cycle test number of the control after half the resistance value is twice the initial resistance is 1544 times, and the average limit thermal cycle test number of the sample in this implementation is 2692 times, which is 1.74 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表29Table 29
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8383 8080 7979 8484 8383 8282
实施例8Example 8 9393 9191 9494 9292 9494 9393
表30Table 30
Figure PCTCN2019097568-appb-000021
Figure PCTCN2019097568-appb-000021
表31Table 31
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 14551455 15281528 15731573 15231523 16431643 15441544
实施例8Example 8 26182618 27812781 27322732 26822682 26492649 26922692
实施例9Example 9
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表32所示：The preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1. The specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 32 below:
表32Table 32
Figure PCTCN2019097568-appb-000022
Figure PCTCN2019097568-appb-000022
对照实施例采用纯的氮化锌、氮化银和氮化硅作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表32比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure zinc nitride, silver nitride and silicon nitride are used as the main heating materials, no heating stabilizer is added, and the binder is in accordance with the ratio in Table 32. The prepared heating element was subjected to the same test as the sample of this example, and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表33所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000023
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表34所示。从表34中看以看出本实例的平均偏差率只有2.13，对照的平均偏差率达到了5.02，是本实例中的2.36倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 33. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000023
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 34. It can be seen from Table 34 that the average deviation rate of this example is only 2.13, and the average deviation rate of the control has reached 5.02, which is 2.36 times that of this example, indicating that the stability of the product resistance after the new ceramic heating element is added with a heating stabilizer The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表35。从表35中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1880次，本实施中样品平均极限热循环测试次数为2895次，是本实例中的1.54倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 35 for details. From Table 35, it can be seen that the average limit thermal cycle test number of the control after half the resistance value is twice the initial resistance is 1880 times, and the average limit thermal cycle test number of the sample in this implementation is 2895 times, which is 1.54 times, indicating that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, which can significantly increase the life of the new ceramic heating element.
表33Table 33
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8383 8585 8585 8484 8686 8585
实施例9Example 9 9494 9494 9696 9494 9595 9595
表34Table 34
Figure PCTCN2019097568-appb-000024
Figure PCTCN2019097568-appb-000024
表35Table 35
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 17821782 18911891 19451945 19151915 18671867 18801880
实施例9Example 9 28762876 29842984 30113011 29342934 26712671 28952895
实施例10Example 10
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表36所示：The preparation process and implementation steps of the new ceramic heating element are prepared in accordance with steps 1) to 7) in Example 1. The specific heating body materials, heating stabilizers and binder components and proportions are shown in Table 36 below:
表36Table 36
Figure PCTCN2019097568-appb-000025
Figure PCTCN2019097568-appb-000025
对照实施例采用纯的氮化锆和碳化硅作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表36比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure zirconium nitride and silicon carbide were used as the main heating materials, no heating stabilizer was added, and the binders were in proportions according to Table 36. The preparation methods and steps were carried out as in Example 1 The same test was carried out in the sample of this example and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表37所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000026
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表38所示。从表38中看以看出本实例的平均偏差率只有3.79，对照的平均偏差率达到了8.77，是本实例中的2.31倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above preparation method, each batch produced 100 ceramic heating elements, and the yield (Y) of each batch was measured, as shown in Table 37. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000026
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 38. It can be seen from Table 38 that the average deviation rate of this example is only 3.79, and the average deviation rate of the control has reached 8.77, which is 2.31 times that of this example, indicating that the stability of the product resistance after the new ceramic heating element is added with a heating stabilizer The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表39。从表39中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1765次，本实施中样品平均极限热循环测试次数为2807次，是本实例中的1.59倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新 型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product. See Table 39 for details. From Table 39, it can be seen that the average limit thermal cycle test times after half the resistance value is twice the initial resistance in the control is 1765 times, the average limit thermal cycle test times of the sample in this implementation is 2807 times, which is 1.59 times, indicating that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表37Table 37
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8181 8484 8282 8383 8484 8383
实施例10Example 10 9393 9696 9595 9494 9595 9595
表38Table 38
Figure PCTCN2019097568-appb-000027
Figure PCTCN2019097568-appb-000027
表39Table 39
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 18711871 17651765 17491749 16831683 17591759 17651765
实施例10Example 10 27682768 28762876 28362836 27742774 27812781 28072807
实施例11Example 11
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表40所示：The preparation process and implementation steps of the new ceramic heating element are prepared in accordance with steps 1) to 7) in Example 1. The specific heating body materials, heating stabilizers and binder components and proportions are shown in Table 40 below:
表40Table 40
Figure PCTCN2019097568-appb-000028
Figure PCTCN2019097568-appb-000028
对照实施例采用纯的氮化硅和碳化硅作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表40比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure silicon nitride and silicon carbide are used as the main body materials for heat generation, no heat stabilizer is added, the binder and the like are in the proportion of Table 40, and the preparation methods and steps are carried out as in Example 1 The same test was carried out in the sample of this example and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表41所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000029
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表42所示。从表42中看以看出本实例的平均偏差率只有3.46，对照的平均偏差率达到了8.81，是本实例中的2.55倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above preparation method, each batch produced 100 ceramic heating elements, and the yield (Y) of each batch was measured, as shown in Table 41. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000029
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 42. It can be seen from Table 42 that the average deviation rate of this example is only 3.46, and the average deviation rate of the control has reached 8.81, which is 2.55 times that of this example, indicating that the stability of the product resistance after the new ceramic heating element is added with a heating stabilizer The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表43。从表43中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1651次，本实施中样品平均极限热循环测试次数为2671次，是本实例中的1.62倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product, as shown in Table 43. From Table 43, it can be seen that the average limit thermal cycle test number of the control after half the resistance value is twice the initial resistance is 1651 times, and the average limit thermal cycle test number of the sample in this implementation is 2671 times, which is 1.62 times, indicating that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, which can significantly increase the life of the new ceramic heating element.
表41Table 41
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8080 8484 8484 8383 8282 8383
实施例11Example 11 9494 9696 9292 9494 9595 9494
表42Table 42
Figure PCTCN2019097568-appb-000030
Figure PCTCN2019097568-appb-000030
表43Table 43
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 15651565 17651765 16451645 16381638 16421642 16511651
实施例11Example 11 26732673 27392739 26442644 25852585 27132713 26712671
实施例12Example 12
新型陶瓷发热体制备工艺及步骤实施步骤按照实施例1中的步骤1)-步骤7)进行制备，具体的发热主体材料、发热稳定剂和粘结剂组分及比例如下表44所示：The preparation process and step implementation steps of the new ceramic heating element are prepared according to step 1) to step 7) in Example 1. The specific heating body materials, heating stabilizer and binder components and proportions are shown in Table 44 below:
表44Table 44
Figure PCTCN2019097568-appb-000031
Figure PCTCN2019097568-appb-000031
对照实施例采用纯的氮化硼和碳化硅作为发热主体材料，不添加发热稳定剂，其粘合剂等按照表44比例，制备的方法和步骤按照实施例1中的进行，制得的发热体与本实施例样品中进行相同测试，并进行比较。In the comparative example, pure boron nitride and silicon carbide are used as the main heating materials, no heating stabilizer is added, and the binder is in accordance with the ratio in Table 44. The preparation method and steps are carried out as in Example 1 to obtain the heating The same test was carried out in the sample of this example and compared.
按照上述制备方法制备5个批次陶瓷发热体，每个批次生产100个陶瓷发热体，然后测量每个批次的成品率(Y)，如表45所示。用电阻测定仪测定其低温电阻(25℃)，根据5个批次电阻平均值R1、R2、R3、R4和R5，计算5个批次平均电阻R和平均偏差
Figure PCTCN2019097568-appb-000032
(n为1、2、3、4或5)，并进一步计算5个批次的电阻的平均偏差率(5个批次的电阻偏差除以电阻平均值)，具体见表46所示。从表46中看以看出本实例的平均偏差率只有3.91，对照的平均偏差率达到了7.93，是本实例中的2.03倍，说明新型陶瓷发热体添加了发热稳定剂后，产品电阻的稳定性显著提高，并且电阻值显著降低，能够满足大功率发热的要求。 Five batches of ceramic heating elements were prepared according to the above-mentioned preparation method, each batch produced 100 ceramic heating elements, and then the yield (Y) of each batch was measured, as shown in Table 45. Measure the low temperature resistance (25℃) with a resistance tester, and calculate the average resistance R and average deviation of 5 batches based on the average resistance R1, R2, R3, R4 and R5 of 5 batches
Figure PCTCN2019097568-appb-000032
(n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance of 5 batches (the resistance deviation of 5 batches divided by the average value of resistance), as shown in Table 46. It can be seen from Table 46 that the average deviation rate of this example is only 3.91, and the average deviation rate of the control has reached 7.93, which is 2.03 times that of this example, indicating that the stability of the product resistance after the new ceramic heating element is added with a heating stabilizer The performance is significantly improved, and the resistance value is significantly reduced, which can meet the requirements of high-power heating.
同时，将制备的新型陶瓷发热体进行性能测试，将成品接通380v以下电源，检测发热均匀性，实验结构表明，五个批次的新型陶瓷发热体均较对照样发热快、且发热均匀。At the same time, the performance of the prepared new ceramic heating body was tested, and the finished product was connected to a power source below 380v to detect the uniformity of heat generation. The experimental structure showed that the five batches of new ceramic heating body heat faster and more uniformly than the control.
并对新型陶瓷发热体进行热循环测试，从室温到1600℃进行产品极限热循环测试，每个批次测试100个产品，以测试次数用N标识，当循环N次后，超过一半的新型陶瓷发热体低温电阻变为初始电阻2倍后，即终止实验，此时的循环次数即为产品的寿命，具体见表47。从表47中看以看出对照中当一半电阻值是初始电阻2倍后的平均极限热循环测试次数为1764次，本实施中样品平均极限热循环测试次数为2820次，是本实例中的1.60倍，说明添加了新型陶瓷发热体添加了发热稳定剂后，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。And the thermal cycle test of the new type ceramic heating element, the product limit thermal cycle test from room temperature to 1600 ℃, each batch test 100 products, with the number of tests marked with N, after N cycles, more than half of the new ceramic After the low-temperature resistance of the heating element becomes twice the initial resistance, the experiment is terminated, and the number of cycles at this time is the life of the product, as shown in Table 47. From Table 47, it can be seen that the average limit thermal cycle test number of the control after half the resistance value is 2 times the initial resistance is 1764 times, and the average limit thermal cycle test number of the sample in this implementation is 2820 times, which is in this example. 1.60 times, which shows that after adding a new ceramic heating element and adding a heating stabilizer, the number of times the product withstands thermal shock is significantly increased, and the life of the new ceramic heating element can be significantly improved.
表37Table 37
单位(％)unit(%) Y1Y1 Y2Y2 Y3Y3 Y4Y4 Y5Y5 平均YAverage Y
对照样Control 8686 8282 8585 8383 8484 8484
实施例12Example 12 9292 9494 9595 9292 9191 9393
表38Table 38
Figure PCTCN2019097568-appb-000033
Figure PCTCN2019097568-appb-000033
表39Table 39
单位(次)Unit (times) N1N1 N2N2 N3N3 N4N4 N5N5 平均NAverage N
对照样Control 17691769 18321832 17921792 17431743 16841684 17641764
实施例12Example 12 28752875 27472747 28452845 27922792 28432843 28202820
由上述实施例可知，通过本发明的陶瓷发热体，产品次品率显著降低，多个批次之间的电阻平均值及电阻平均偏差都显著降低，产品发热快并且均匀，产品耐受热冲击的次数显著提高，可以明显的提高新型陶瓷发热体的寿命。，It can be seen from the above examples that with the ceramic heating element of the present invention, the defective rate of products is significantly reduced, the average resistance and the average deviation of resistance between multiple batches are significantly reduced, the product heats up quickly and uniformly, and the product withstands thermal shock Significantly increased the number of times, can significantly increase the life of the new ceramic heating element. ,
以上详细描述了本发明的优选实施方式，但是，本发明并不限于上述实施方式中的具体细节，在本发明的技术构思范围内，可以对本发明的技术方案进行多种简单变型，这些简单变型均属于本发明的保护范围。The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical idea of the present invention, various simple modifications can be made to the technical solution of the present invention. These simple modifications All belong to the protection scope of the present invention.
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合，为了避免不必要的重复，本发明对各种可能的组合方式不再另行说明。In addition, it should be noted that the specific technical features described in the above specific embodiments can be combined in any suitable manner without contradictions. In order to avoid unnecessary repetition, the present invention The combination method will not be explained separately.
此外，本发明的各种不同的实施方式之间也可以进行任意组合，只要其不违背本发明的思想，其同样应当视为本发明所公开的内容。In addition, various combinations of various embodiments of the present invention can also be arbitrarily combined, as long as it does not violate the idea of the present invention, it should also be regarded as the content disclosed by the present invention.

Claims (10)

  1. 一种制备陶瓷发热体的组合物，主要由发热主体材料、发热稳定剂和粘结剂组成，其特征在于，所述的发热主体材料选自碳化物、氮化物和二硅化钼中的至少一种，所述的发热稳定剂为石墨烯、金属、合金、金属氧化物中的至少一种。A composition for preparing a ceramic heating element is mainly composed of a heating element material, a heating stabilizer and a binder, characterized in that the heating element material is selected from at least one of carbide, nitride and molybdenum disilicide The heat generation stabilizer is at least one of graphene, metal, alloy, and metal oxide.
  2. 根据权利要求1所述的制备陶瓷发热体的组合物，其中，所述的碳化物选自碳化钛、碳化硅、碳化钨，所述的氮化物选自氮化钛、氮化钒、氮化锆、氮化钽、氮化锰、氮化钨、氮化硅、氮化硼、氮化铜、氮化锌、氮化银。The composition for preparing a ceramic heating element according to claim 1, wherein the carbide is selected from titanium carbide, silicon carbide, and tungsten carbide, and the nitride is selected from titanium nitride, vanadium nitride, and nitride Zirconium, tantalum nitride, manganese nitride, tungsten nitride, silicon nitride, boron nitride, copper nitride, zinc nitride, silver nitride.
  3. 根据权利要求1或2所述的制备陶瓷发热体的组合物，其中，基于组合物的总质量，所述发热主体材料的含量为60％-99.5％。The composition for preparing a ceramic heating element according to claim 1 or 2, wherein the content of the heating main material is 60% to 99.5% based on the total mass of the composition.
  4. 根据权利要求1至3任一项所述的制备陶瓷发热体的组合物及其发热体制备，其中，所述的发热稳定剂选自石墨烯、钛、钒、铬、锰、铁、钴、镍、铜、锌、钇、钼、钌、铑、钯、银、钨、金、铂、铱、前述金属氧化物和前述金属合金，基于组合物的总质量，所述发热稳定剂的含量为0.2％-35％。The composition for preparing a ceramic heating element according to any one of claims 1 to 3 and the preparation thereof, wherein the heating stabilizer is selected from graphene, titanium, vanadium, chromium, manganese, iron, cobalt, Nickel, copper, zinc, yttrium, molybdenum, ruthenium, rhodium, palladium, silver, tungsten, gold, platinum, iridium, the foregoing metal oxides and the foregoing metal alloys, based on the total mass of the composition, the content of the heating stabilizer is 0.2%-35%.
  5. 根据权利要求1至4任一项所述的制备陶瓷发热体的组合物，其中，所述的粘结剂为选自羧甲基纤维素、聚乙烯醇、乙基纤维素、淀粉、水玻璃、合成树脂中的至少一种，基于组合物的总质量，所述粘结剂的含量为0.3％-30％。The composition for preparing a ceramic heating element according to any one of claims 1 to 4, wherein the binder is selected from carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, starch, water glass At least one of synthetic resins, based on the total mass of the composition, the content of the binder is 0.3%-30%.
  6. 一种用于产生气溶胶的陶瓷发热组件，所述陶瓷发热组件包括由权利要求1-5任一项所述的制备陶瓷发热体的组合物制备的陶瓷发热体和发热体底座，其特征在于，所述的陶瓷发热体安装在发热体底座上，陶瓷发热体包括发热主体和电极。A ceramic heating element for generating an aerosol, the ceramic heating element comprising a ceramic heating element and a heating element base prepared from the composition for preparing a ceramic heating element according to any one of claims 1 to 5, characterized in that The ceramic heating element is installed on the heating element base. The ceramic heating element includes a heating body and an electrode.
  7. 根据权利要求6所述的用于产生气溶胶的陶瓷发热组件，其特征在于，所述的发热体主体包括陶瓷发热基体和端帽，所述的陶瓷发热基体由至少一个发热基体部分组成，并且，至少一个发热基体部分通过电流，用于发热。The ceramic heating element for generating aerosols according to claim 6, characterized in that the heating element body includes a ceramic heating element and an end cap, and the ceramic heating element is composed of at least one heating element, and At least one heat-generating base part passes current for heat generation.
  8. 根据权利要求7所述的用于产生气溶胶的陶瓷发热组件，其特征在于所述的发热基体之间有空腔，或填充具有耐高温、绝热材料。The ceramic heating element for generating aerosol according to claim 7, characterized in that there is a cavity between the heating bases, or it is filled with a high temperature resistant and heat insulating material.
  9. 根据权利要求6所述的用于产生气溶胶的陶瓷发热组件，其特征在于所述的发热体底座能够固定和给陶瓷发热体供电，并且发热体底座具有与电源连接的电极接点。The ceramic heating element for generating aerosol according to claim 6, characterized in that the heating element base can fix and supply power to the ceramic heating element, and the heating element base has electrode contacts connected to the power source.
  10. 根据权利要求1至5任一项所述的制备陶瓷发热体的组合物和权利要求6-9任一项所述的用于产生气溶胶的陶瓷发热组件应用在固体发烟介质或液体发烟介质的加热不燃烧卷烟或电子烟中。The composition for preparing a ceramic heating element according to any one of claims 1 to 5 and the ceramic heating element for generating an aerosol according to any one of claims 6 to 9 are applied to a solid smoke medium or liquid smoke The heating of the medium does not burn cigarettes or electronic cigarettes.
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