CN114133222A - Preparation method of conductive ceramic, product and application of conductive ceramic in heating atomizer - Google Patents
Preparation method of conductive ceramic, product and application of conductive ceramic in heating atomizer Download PDFInfo
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- CN114133222A CN114133222A CN202111613389.3A CN202111613389A CN114133222A CN 114133222 A CN114133222 A CN 114133222A CN 202111613389 A CN202111613389 A CN 202111613389A CN 114133222 A CN114133222 A CN 114133222A
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- conductive ceramic
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- atomizer
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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Abstract
The invention discloses a preparation method of conductive ceramic, a product and application of the conductive ceramic in a heating atomizer, belonging to the technical field of electronic cigarette atomization; mixing the conductive phase raw material and the sintering phase raw material, and then molding and sintering to obtain conductive ceramic; taking the conductive ceramic as a main body, and connecting the conductive ceramic with a lead through an electrode welding spot to obtain a heating atomizer; the conductive ceramic prepared by the invention has the advantages of high heating cycle stability, adjustable resistivity, large resistance temperature coefficient regulation range, no metal volatile component, corrosion resistance, safety, environmental protection, health and the like; compared with a metal wire and rock wool, organic cotton or ceramic heating and atomizing mode, the conductive ceramic has the characteristics of integration of heating and atomizing and simplified structure; the heating atomizer made of the conductive ceramic material has the characteristics of high heating speed, uniform heating and atomization, high mouthfeel reduction degree and long service life.
Description
Technical Field
The invention belongs to the technical field of electronic cigarette atomization, and particularly relates to a preparation method of conductive ceramic, a product and application of the conductive ceramic in a heating atomizer.
Background
At present, electronic cigarettes can be used as smoking cessation substitutes due to the characteristics of low harm, various tastes, large smoke quantity and the like, are increasingly favored by young people, are concerned by various governments in the world while being full of commercial opportunities in the market of the electronic cigarettes, and have increasingly significant safety, environmental protection and health problems. The atomizer is used as a core component of the electronic cigarette and consists of metal wires, rock wool, organic cotton or ceramic, the atomization mechanism is that after the metal wires are electrified, the metal wires generate heat and then atomize tobacco tar adsorbed by the rock wool, the organic cotton or the porous ceramic, or the metal wires and the ceramic plate are compounded and inserted into the tobacco, the heat generated by the metal wires is transferred to the ceramic plate, and then the tobacco is heated and atomized. However, in the normal heating and atomizing process, the temperature of the metal wire cannot be precisely controlled, if the temperature is too high, the tobacco tar is easy to be coked and gelatinized, the taste is not good, and excessive harmful substances are generated, and if the temperature is too low, the tobacco tar cannot be sufficiently atomized to cause lung choking, so that the smoking taste is reduced. In addition, the metal wire can produce surface oxidation, metal ash volatilize at the repeated heating in-process to arouse the health problem, the tobacco tar is to the corrosive action that the metal wire produced, also can influence user's safety and health.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of conductive ceramic, a product and application of the conductive ceramic in a heating atomizer, wherein a heating atomization component in the heating atomizer is made of the conductive ceramic, and has the advantages of uniform heating, accurate and controllable temperature, no coking and pasting, stable property, oxidation resistance, corrosion resistance, high smoke oil reduction degree and long service life compared with a metal wire.
In order to achieve the purpose, the invention provides the following technical scheme:
one of the technical schemes of the invention is as follows: a process for preparing electrically conductive ceramic includes such steps as mixing electrically conductive phase with sintered phase, shaping and sintering.
Further, the mass percentages of the conductive phase raw materials and the sintering phase raw materials are (5-65%) to (35-95%).
Further, the sintering phase raw material comprises at least one of zirconia, alumina, yttria, silica, silicon carbide or silicon nitride; the conductive phase raw material comprises at least one of titanium nitride, zirconium nitride, titanium carbonitride, titanium carbide, zirconium carbide, thallium carbide, hafnium carbide, titanium boride, zirconium boride, molybdenum silicide or tungsten carbide.
Further, the sintering is carried out in an inert atmosphere at 1500-2200 ℃ for 0.5-5 h.
The second technical scheme of the invention is as follows: a conductive ceramic prepared according to the above preparation method.
The resistivity of the conductive ceramic prepared by the method is 6.57 multiplied by 10-6～9.85×103Omega. m region, preferably less than 2.50X 10-2Omega.m; the temperature coefficient of resistance is in the range of-4000 to 4000, preferably higher than 450. When the conductive ceramic prepared by the invention is used for heating an atomizer, the heating temperature can be well controlled.
The mechanical property of the conductive ceramic prepared by the method of the invention is as follows: the breaking strength is 260-800 MP, and the preferred value is more than 370 MPa; the fracture toughness is 2.5-9 MPa.m1/2Preferably greater than 4.5MPa · m1/2(ii) a The Vickers hardness is 7.5-29.5 GPa, and the optimal value is more than 12.5 GPa.
The third technical scheme of the invention is as follows: the conductive ceramic is applied to a heating atomizer, in particular to an electronic cigarette heating atomizer.
The fourth technical scheme of the invention is as follows: an electronic cigarette heating atomizer comprises a main body and a lead, wherein the main body is the conductive ceramic; the main body and the lead are connected through an electrode pad.
The main body can be in the shape of a sheet, a ring or a cylinder, and can be secondarily designed on the sheet, the ring or the cylinder, such as slotting and punching; the shape characteristics of the body include, but are not limited to, those described above, and various shapes of the body of the atomizer product prepared using the conductive ceramic are within the scope of the present invention according to the requirements of atomization.
Furthermore, the electrode welding spot is made of alloy, the alloy is a complex of several metal simple substances, and the melting point is low; the electrode welding spots comprise a positive welding spot and a negative welding spot, and the two welding spots are positioned on the surface of the main body and are symmetrical in position; the other end of the lead is connected with a power supply unit.
Further, the power supply unit comprises a battery and a control system, the control system is used for controlling power output, and the output power of the power supply unit is 6-75W, and is further preferably 8-25W.
The positions of the welding spots of the electrodes determine the resistance and the heating uniformity of the main body, the positions of the welding spots need to have a certain symmetrical relation, not only the position relation of two ends, but also the positions of the welding spots influence the resistance value of the heater (the conductive lengths are different, and the resistance values are different), the areas of the welding spots are required to be as large as possible, the contact resistance can be effectively reduced, but the contact resistance cannot be too large, and the conductive length can be influenced if the contact resistance is too large; the main body resistance is controlled to be 0.2-20 omega, preferably 0.35-1.60 omega by controlling the position of the welding spot.
The heating temperature of the heating atomizer provided by the invention is 230-450 ℃, and preferably 260-320 ℃; the resistance is 0.2-20 omega, preferably 0.35-1.60 omega; the heating speed is 1-15 s and reaches the set temperature; the heating power is 6-75W, preferably 8-25W.
In the metal wire and ceramic mode, in the cyclic heating process, because the difference between the thermal expansion coefficients of metal and ceramic is large, the metal wire is easy to fall off from the ceramic, so that the cyclic stability is poor, and in addition, ash is generated in the cyclic heating process of metal, so that the heating stability of the metal wire can be seriously influenced; in comparison, the conductive ceramic is integrated with conduction and heating, so that the cycle stability of the conductive ceramic is obviously higher.
The fifth technical scheme of the invention is as follows: an electronic cigarette comprises the electronic cigarette heating atomizer.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses the conductive ceramics to replace the metal wire as the heating component, and the conductive ceramics replaces the metal heating wire for the first time, thereby improving the comprehensive performance of the atomizer and having obvious technical iteration advantage;
the conductive ceramic prepared by the invention has the advantages of high heating cycle stability, adjustable resistivity, large resistance temperature coefficient regulation range, no metal volatile component, corrosion resistance, safety, environmental protection, health and the like; compared with a metal wire and rock wool, organic cotton or ceramic heating and atomizing mode, the conductive ceramic has the characteristics of heating and atomizing integration and simplified structure; the heating atomizer made of the conductive ceramic material has the characteristics of high heating speed, uniform heating and atomization, high mouthfeel reduction degree and long service life.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a metallographic microstructure of the conductive ceramic prepared in example 1;
FIG. 2 is a schematic view of a heating atomizer simulating an electronic cigarette heating atomized tobacco tar; wherein, the device comprises 1-a lithium battery, 2-a control system, 3-a heating atomizer, 3-1 a conductive ceramic main body, 3-2 electrode welding spots, 3-3 leads and 4-tobacco tar;
FIG. 3 is a structural view of a heated atomizer prepared in example 1;
FIG. 4 is a structural view of a heated atomizer prepared in example 2;
FIG. 5 is a structural view of a heated atomizer prepared in example 3.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
The preparation of the electronic cigarette heating atomizer comprises the following steps:
(1) preparing conductive ceramics: uniformly mixing zirconia powder (purchased from Shandong national porcelain functional material Co., Ltd.) with partially stabilized yttria powder with the average particle size of 0.3 mu m, alumina powder with the average particle size of 0.03 mu m and titanium carbide powder with the average particle size of 0.5 mu m according to the mass ratio of 35: 40: 25, then adding 4 wt% of PVA aqueous solution as a binder according to 1.2 times of the total weight of the mixed powder, uniformly mixing by using a ball mill, then carrying out spray granulation, putting the granulated powder into a special mold, carrying out compression molding at 150MPa, drying a blank, putting the dried blank into a sintering furnace, heating to 1700 ℃ under the argon atmosphere, preserving heat for 1 hour, and naturally cooling to obtain the conductive ceramic;
the metallographic microstructure of the conductive ceramic prepared as described above is shown in fig. 1, in which the white particles are a conductive phase, the gray regions are a sintered phase, and the black regions with irregular shapes are pores or pits left by the falling particles.
(2) And (2) cutting the conductive ceramic prepared in the step (1) by warps, carrying out CNC (computer numerical control) processing, carrying out laser drilling, and carrying out grinding and polishing processing to obtain a main body component of the heating atomizer, then carrying out a brazing process, and firmly welding a copper lead and the surface of the conductive ceramic by using silver-titanium-copper alloy paste to form an electrode welding spot at an alloy position, thus obtaining the heating atomizer of the electronic cigarette.
A schematic diagram of the prepared heating atomizer for simulating the electronic cigarette to heat and atomize the tobacco tar is shown in fig. 2, wherein 1 is a lithium battery for providing electric energy for the electronic cigarette, 2 is a control system for controlling power output, and 3 is a heating atomizer comprising a conductive ceramic main body 3-1, an electrode welding point 3-2, a lead 3-3 and the tobacco tar 4; after the battery supplies power, the control system outputs stable voltage and specific current to heat the heating atomizer, so that the tobacco tar is heated and atomized.
The specific structure of the heating atomizer 3 is shown in fig. 3: the conductive ceramic main body 3-1 is in a sheet shape, the total length is 7.50mm, the width is 2.5mm, the thickness is 0.25mm, and the radius of the semi-circle at the two ends is 1.25 mm; the semi-circles at the two ends are main electrode points, the copper lead 3-3 and the surface of the conductive ceramic main body 3-1 are firmly welded by silver-titanium-copper alloy paste through a brazing process, the electrode welding points 3-2 occupy the whole semi-circle, the area is large, the contact resistance is reduced, the heating temperature at the position is favorably reduced, and the smoke oil is prevented from passing through the semi-circleHeating to coking and pasting; in the middle section of the main body, 8 orderly arranged micropores 3-4 with the size of
The micropore is favorable to increasing the area of contact of main part and tobacco tar to increase atomizing area, the micropore provides the passageway for atomizing tobacco tar in addition, is favorable to increasing the fog volume in the twinkling of an eye, improves and inhales and experiences.
Through detection: the resistivity of the conductive ceramic prepared in this example was 5.6 x 10-4Omega.m, a temperature coefficient of resistance of 750, a breaking strength of 502MPa, a fracture toughness of 5.2 MPa.m1/2The Vickers hardness is 13.6 GPa; the resistance of the heating atomizer is 0.35 omega, the heating rated temperature is 280 ℃, and the tobacco tar can be quickly and uniformly atomized within 3s under the power of 8.5W.
Example 2
The preparation of the electronic cigarette heating atomizer comprises the following steps:
(1) preparing conductive ceramics: uniformly mixing alumina powder with the average particle size of 0.3 mu m, yttrium oxide powder with the average particle size of 0.1 mu m and titanium boride powder with the average particle size of 2.5 mu m according to the mass ratio of 55: 15: 32, then adding water which is 1.5 times of the total weight of the mixed powder as a solvent, uniformly mixing by using a ball mill, then carrying out spray drying, mixing the dried powder, paraffin and high-density polyvinyl alcohol according to the mass ratio of 100: 8: 11, granulating, pouring into an injection molding machine, completing injection molding, drying a blank, putting into a sintering furnace, heating to 1650 ℃ under the argon atmosphere, preserving heat for 2 hours, and naturally cooling to obtain the conductive ceramic;
(2) carrying out CNC (computer numerical control) processing, laser grooving, grinding and polishing processing on the conductive ceramic prepared in the step (1) to obtain a heating atomizer main body component, then carrying out a brazing process, firmly welding a silver lead wire and the surface of the conductive ceramic by using silver-aluminum alloy paste, and forming an electrode welding spot at an alloy position to obtain the electronic cigarette heating atomizer, wherein the structure of the electronic cigarette heating atomizer is shown in figure 4: the conductive ceramic main body 4-1 is in a circular ring shape, and has the outer diameter of 5.00mm, the inner hole of 2.50mm and the height of 5.00 mm; the upper and lower end ring surfaces are main body electrode points, the silver lead 4-3 is firmly welded with the surface of the main body by using silver-aluminum alloy paste through a brazing process, the electrode welding points 4-2 occupy the whole ring surface, the area is large, the contact resistance is reduced, the heating temperature at the position is favorably reduced, and the tar is prevented from being coked and gelatinized due to excessive heating; at the ring side surface, 12 through grooves which are orderly arranged are designed, the length is 3.00mm, the width is 0.35mm, the through grooves are favorable for increasing the contact area of the main body and the tobacco tar, so that the atomization area is increased, in addition, the through grooves provide a channel for the atomized tobacco tar, the instantaneous fog amount is favorable for increasing, and the smoking experience is improved.
The resistivity of the conductive ceramic was found to be 7.8 x 10-2Omega.m, temperature coefficient of resistance 3482, breaking strength 285MPa, and fracture toughness 3.1 MPa.m1/2The Vickers hardness is 14.1 GPa; the resistance of the heating atomizer is 0.55 omega, the heating rated temperature is 290 ℃, and the tobacco tar can be quickly and uniformly atomized within 4.5s under the power of 10.5W.
Example 3
The preparation method of the electronic cigarette heating atomizer comprises the following steps:
(1) preparing conductive ceramics: uniformly mixing silicon carbide powder with the average particle size of 0.5 mu m, yttrium oxide powder with the average particle size of 0.1 mu m, aluminum oxide powder with the average particle size of 0.3 mu m and titanium boride powder with the average particle size of 2.5 mu m according to the mass ratio of 55: 4: 6: 27, then adding water which is 1.5 times of the total weight of the mixed powder as a solvent, uniformly mixing by using a ball mill, then carrying out spray drying, heating and mixing the dried powder and paraffin according to the mass ratio of 100: 15, pouring into a hot die casting machine to complete hot die casting molding, drying a blank, putting into a sintering furnace, heating to 2050 ℃ under the argon atmosphere, preserving heat for 2.5 hours, and naturally cooling to obtain the conductive ceramic;
(2) carrying out CNC (computer numerical control) processing, laser grooving, grinding and polishing processing on the conductive ceramic prepared in the step (1) to obtain a heating atomizer main body component, then carrying out a brazing process, firmly welding a silver-aluminum lead wire and the surface of the conductive ceramic by using titanium-aluminum alloy paste, and forming an electrode welding spot at an alloy position to obtain the electronic cigarette heating atomizer, wherein the structure of the electronic cigarette heating atomizer is shown in figure 5: the conductive ceramic main body 5-1 is cylindrical, and has an outer diameter of 8.60mm, an inner hole of 6.00mm and a height of 35.00 mm; cylindrical surfaces at the upper end and the lower end are main body electrode points, the silver-aluminum lead 5-3 is firmly welded with the surface of the main body by using titanium-aluminum alloy paste through a brazing process, the electrode welding points 5-2 occupy the whole cylindrical surface, the area is large, the contact resistance is reduced, the heating temperature at the position is favorably reduced, and the tar is prevented from being coked and gelatinized due to excessive heating; the side surface of the cylinder is provided with a plurality of through holes 5-4 which are arranged in order, the diameter of each through hole is 0.8mm, the through holes are beneficial to reducing the heating area of the cylinder, and after the tobacco is inserted into the cylinder, the heat generated by electrifying the cylinder heats the tobacco more intensively, so that the heat loss is reduced, the heating power is reduced, and the use times of the battery are prolonged.
The resistivity of the conductive ceramic prepared in this example was found to be 4.3 x 10-1Omega.m, a temperature coefficient of resistance of 2155, a breaking strength of 383MPa, and a fracture toughness of 5.3 MPa.m1/2The Vickers hardness is 26.4 GPa; the resistance of the heating atomizer is 0.50 omega, the heating rated temperature is 320 ℃, and the tobacco can be rapidly and uniformly heated and atomized within 5.6s under the power of 20.0W.
The above description is only for the preferred embodiment of the present invention, and the protection scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention, the technical solution and the inventive concept of the present invention equivalent or change within the technical scope of the present invention.
Claims (10)
1. A preparation method of conductive ceramics is characterized in that a conductive phase raw material and a sintering phase raw material are mixed, and then the mixture is formed and sintered.
2. The preparation method of claim 1, wherein the mass percentage of the conductive phase raw material to the sintering phase raw material is (5-65%): 35-95%.
3. The method of claim 1, wherein the sintering phase feedstock comprises at least one of zirconia, alumina, yttria, silica, silicon carbide, or silicon nitride; the conductive phase raw material comprises at least one of titanium nitride, zirconium nitride, titanium carbonitride, titanium carbide, zirconium carbide, thallium carbide, hafnium carbide, titanium boride, zirconium boride, molybdenum silicide or tungsten carbide.
4. The method according to claim 1, wherein the sintering is performed in an inert atmosphere at 1500 to 2200 ℃ for 0.5 to 5 hours.
5. A conductive ceramic prepared by the preparation method according to any one of claims 1 to 4.
6. Use of the conductive ceramic of claim 5 in a heated atomizer.
7. An electronic cigarette heating atomizer, which is characterized by comprising a main body and a lead wire, wherein the main body is the conductive ceramic of claim 5; the main body and the lead are connected through an electrode pad.
8. The heating atomizer of claim 7, wherein the electrode pads are made of an alloy, and comprise a positive electrode pad and a negative electrode pad, and the two pads are located on the surface of the main body and are symmetrical in position; the other end of the lead is connected with a power supply unit.
9. The electronic cigarette heating atomizer according to claim 8, wherein the power supply unit is composed of a battery and a control system, and the output power of the power supply unit is 6-75W.
10. An electronic cigarette, characterized by comprising the electronic cigarette heating atomizer of any one of claims 7 to 9.
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