阅读说明：本技术 金属浆料、发热电路、雾化芯及其制备方法、以及电子烟 (Metal slurry, heating circuit, atomizing core and preparation method thereof, and electronic cigarette ) 是由 李程峰 余明先 徐玉金 张霖 王伟江 刘友昌 戴高环 王超 何培与 何晓刚 姚伟 于 2021-07-19 设计创作，主要内容包括：本发明提供一种金属浆料,包括金属粉、玻璃粉和有机载体；所述金属粉、玻璃粉和有机载体的质量比为100：5-10：10-20；所述金属粉包括N i粉、Cr粉和N i Cr-(20)合金粉；其中所述N i粉和Cr粉的中位粒径均小于10μm,所述N i Cr-(20)合金粉的中位粒径范围为15-50μm；所述玻璃粉的化学式为B-Si-A l-M-2O-NO,其中M为碱金属,N为碱土金属。还提供一种由上述金属浆料制成的发热电路、包括多孔陶瓷和上述的发热电路的雾化芯、雾化芯的制备方法及电子烟。由本发明提供的金属浆料制备的发热电路与多孔陶瓷的结合强度高,且不影响多孔陶瓷本身的强度,能够满足电子烟雾化芯的装配和使用需求,使电子烟的使用寿命得到提高。(The invention provides a metal slurry, which comprises metal powder, glass powder and an organic carrier; the mass ratio of the metal powder to the glass powder to the organic carrier is 100: 5-10: 10-20 parts of; the metal powder comprises N i powder, Cr powder and Ni Cr powder 20 Alloy powder; wherein the N i powder and the Cr powder both have median particle size of less than 10 μm, and the Ni Cr powder 20 The median particle size range of the alloy powder is 15-50 mu m; the chemical formula of the glass powder is B-Si-A l-M 2 O-NO, wherein M is an alkali metal and N is an alkaline earth metal. Also provides a heating circuit made of the metal slurryThe atomizing core comprises porous ceramic and the heating circuit, the preparation method of the atomizing core and the electronic cigarette. The heating circuit prepared from the metal slurry provided by the invention has high bonding strength with the porous ceramic, does not influence the strength of the porous ceramic, can meet the assembly and use requirements of the electronic cigarette atomizing core, and prolongs the service life of the electronic cigarette.)

1. A metal paste characterized by: comprises metal powder, glass powder and an organic carrier; the mass ratio of the metal powder to the glass powder to the organic carrier is 100: 5-10: 10-20 parts of;

the metal powder comprises Ni powder, Cr powder and NiCr powder₂₀Alloy powder; wherein the Ni powder and the Cr powder both have median particle size of less than 10 μm, and the NiCr powder₂₀The median particle size range of the alloy powder is 15-50 mu m;

the chemical formula of the glass powder is B-Si-Al-M₂O-NO, wherein M is a baseThe metal and N are alkaline earth metals.

2. The metal paste according to claim 1, characterized in that: in every 100 parts by mass of the metal powder, 10-30 parts of Ni powder, 5-20 parts of Cr powder and the balance of NiCr₂₀And (3) alloy powder.

3. The metal paste according to claim 1, characterized in that: said M is K, Na, or Li; and N is Ca, Mg, Ba or Zn.

4. The metal paste according to claim 1, characterized in that: the organic carrier comprises ethyl cellulose and terpineol; wherein the mass ratio of the ethyl cellulose to the terpineol is 20-40: 60-80.

5. A heat generating circuit, characterized by: made from the metal paste of any one of claims 1-4; the thickness of the heating circuit is 50-100 μm.

6. An atomizing core, characterized in that: the atomizing device comprises porous ceramic and a heating circuit arranged on an atomizing surface of the porous ceramic; the heating circuit as set forth in claim 5, wherein the pore diameter of the porous ceramic is matched with the particle diameters of the metal powder and the glass powder, and the depth of the metal paste impregnated into the porous ceramic is 15-30 μm.

7. The atomizing core of claim 6, wherein: the porosity of the porous ceramic is 45-65%, and the pore diameter is 10-40 μm.

8. The atomizing core of claim 7, wherein: the axial direction of the middle hole of the porous ceramic is obliquely arranged with the plane of the atomization surface, and the inclination angle is 30-90 degrees.

9. A preparation method of an atomization core is characterized in that: the method comprises the following steps:

separately providing a porous ceramic and a metal slurry, wherein the porous ceramic is the porous ceramic according to any one of claims 6 to 8, and the metal slurry is the metal slurry according to any one of claims 1 to 4;

coating the metal slurry on the atomized surface of the porous ceramic to form the heating circuit;

sintering the porous ceramic coated with the metal slurry, wherein the sintering temperature is 1030 ℃ and 1150 ℃, and the sintering time is 7-12 minutes.

10. The utility model provides an electronic cigarette, including the shell, with the base of connection can be dismantled to the shell is fixed in power on the base, its characterized in that: the atomization device further comprises an atomization core arranged in the shell, the atomization core is prepared by the preparation method of claim 9, and a heating circuit of the atomization core is electrically connected with the power supply.

Technical Field

The invention belongs to the technical field of electronic cigarettes, and particularly relates to metal slurry, a heating circuit, an atomization core, a preparation method of the atomization core and an electronic cigarette.

Background

The electron cigarette is equipped with the piece that generates heat on the atomizing face of atomizing core, and present the piece that generates heat is mostly the one deck metal thick liquids of printing on porous ceramic matrix surface, through the thick film heating circuit that the stoving sintering formed, and the circular telegram back, the tobacco tar on the atomizing face is infiltrated in the heating circuit heating, makes its atomizing generate smog, supplies the user suction. Because there is no fixing part between the thick film heating circuit and the porous ceramic, the two are combined and fixed only by sintering, therefore, the combination strength between the two directly influences the service life of the electronic cigarette. The bonding strength is generally evaluated by a dry burning method (for example, under the constant power of 6.0W, the power is continuously supplied for 6min) or a cold and hot impact method (for example, under the constant power of 6.0W, the power is supplied for 3s, the power is stopped for 15s, the power is supplied for 3s again, and the power is stopped for 15s … … for 20 times in total, and the total time is 6min), when the bonding strength is not enough to support the experimental conditions, the thick film heating circuit is separated from the porous ceramic, the peeling phenomenon of the thick film heating circuit occurs, and the heating circuit is even caused to fall off from the porous ceramic matrix.

In the prior art, more glass powder is generally added into resistance paste to improve the interface bonding strength between a heating circuit and porous ceramics, but when the content of the glass powder in the paste is more, although the bonding strength between the heating circuit and a ceramic matrix is improved, the ceramic matrix is vitrified when the porous ceramic matrix is impregnated with excessive glass powder, the ceramic matrix is easily brittle and broken, and the assembly and use requirements of the electronic cigarette atomizing core are seriously influenced.

Disclosure of Invention

The invention aims to overcome the defects in the prior art and provides the metal slurry, the heating circuit, the atomizing core, the preparation method of the atomizing core and the electronic cigarette.

In order to achieve the purpose, the invention adopts the technical scheme that:

the metal slurry comprises metal powder, glass powder and an organic carrier; the mass ratio of the metal powder to the glass powder to the organic carrier is 100: 5-10: 10-20 parts of;

the metal powder comprises Ni powder, Cr powder and NiCr powder₂₀Alloy powder; wherein the Ni powder and the Cr powder both have median particle size of less than 10 μm, and the NiCr powder₂₀The median particle size range of the alloy powder is 15-50 mu m;

the chemical formula of the glass powder is B-Si-Al-M₂O-NO, wherein M is an alkali metal and N is an alkaline earth metal.

The further improvement of the technical scheme is as follows:

in every 100 parts by mass of the metal powder, 10-30 parts of Ni powder, 5-20 parts of Cr powder and the balance of NiCr₂₀And (3) alloy powder.

Said M is K, Na, or Li; and N is Ca, Mg, Ba or Zn.

The organic carrier comprises ethyl cellulose and terpineol; wherein the mass ratio of the ethyl cellulose to the terpineol is 20-40: 60-80.

The invention also provides a heating circuit which is made of the metal slurry; the thickness of the heating circuit is 50-100 μm.

The invention also provides an atomizing core, which comprises porous ceramic and a heating circuit arranged on the atomizing surface of the porous ceramic; the heating circuit is the heating circuit, the pore diameter of the porous ceramic is matched with the particle diameters of the metal powder and the glass powder, and the depth of the porous ceramic infiltrated by the metal slurry is 15-30 mu m.

Further, the porosity of the porous ceramic is 45-65%, and the pore diameter is 10-40 μm.

Furthermore, the axial direction of the middle hole of the porous ceramic is obliquely arranged with the plane of the atomization surface, and the inclination angle is 30-90 degrees.

The invention also provides a preparation method of the atomization core, which comprises the following steps:

respectively providing porous ceramic and metal slurry, wherein the porous ceramic is the porous ceramic, and the metal slurry is the metal slurry;

coating the metal slurry on the atomized surface of the porous ceramic to form the heating circuit;

sintering the porous ceramic coated with the metal slurry, wherein the sintering temperature is 1030 ℃ and 1150 ℃, and the sintering time is 7-12 minutes.

The invention also provides an electronic cigarette, which comprises a shell, a base detachably connected with the shell, a power supply fixed on the base, and an atomizing core arranged in the shell, wherein the atomizing core is prepared by the preparation method, and a heating circuit of the atomizing core is electrically connected with the power supply.

According to the technical scheme of the invention, the metal powder of the metal slurry comprises Ni powder, Cr powder and NiCr powder₂₀Alloy powder of three kinds, and NiCr₂₀The alloy powder has larger median particle size and the Ni powder and the Cr powder have smaller median particle size, so that NiCr powder has larger median particle size in the process of preparing the heating circuit₂₀Because the grain diameter of the alloy powder is larger, the pores of the porous ceramic are filled firstly, and most of the volume of the pores is occupied; ni powder and Cr powder are filled in NiCr powder due to small particle size₂₀Gaps formed between the alloy powder and the porous ceramics; the remaining pores are filled with molten glass frit. Because the metal powder is filled firstly, only a small amount of glass powder is infiltrated into the pores of the porous ceramic, and the phenomenon of vitrification of the porous ceramic caused by excessive glass powder infiltration is effectively avoided. According to the atomizing core, the pore diameter of the porous ceramic is matched with the particle diameters of the metal powder and the glass powder, so that the metal powder and the glass powder cannot penetrate too much under the condition of ensuring that the porous ceramic has enough bonding strength, the continuity of a sintered heating circuit film layer is ensured, the resistance stability of a heating circuit is ensured, and errors are reduced.

Drawings

Fig. 1 is a schematic flow chart of a method for preparing an atomizing core according to an embodiment of the present invention.

Detailed Description

To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

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. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

The embodiment provides a metal paste which comprises metal powder, glass powder and an organic carrier. The mass ratio of the metal powder to the glass powder to the organic carrier is 100: 5-10: 10-20.

The metal powder comprises Ni powder, Cr powder and NiCr powder₂₀Alloy powder; wherein the Ni powder and the Cr powder both have median particle size of less than 10 μm, and the NiCr powder₂₀The median particle size of the alloy powder is 15-50 μm. Wherein, in every 100 parts by mass of the metal powder, the Ni powder is 10-30 parts, the Cr powder is 5-20 parts, and the rest is NiCr₂₀And (3) alloy powder.

The chemical formula of the glass powder is B-Si-Al-M₂O-NO, wherein M is an alkali metal and N is an alkaline earth metal. Said M is K, Na, or Li; and N is Ca, Mg, Ba or Zn. The glass transition temperature of the glass powder is 400-800 ℃.

The organic carrier comprises ethyl cellulose and terpineol; wherein the mass ratio of the ethyl cellulose to the terpineol is 20-40: 60-80.

When the metal slurry is prepared, powder and an organic carrier are respectively prepared. When the powder is prepared, firstly, metal powder is prepared according to the mass ratio requirement, after the metal powder is uniformly mixed, a proper amount of glass powder is added into the metal powder according to the mass ratio requirement, and the metal powder and the glass powder are uniformly mixed. When preparing the organic carrier, mixing the ethyl cellulose and the terpineol uniformly according to the mass ratio requirement. And gradually adding the prepared powder into the prepared organic carrier, and stirring while adding until the metal slurry can continuously draw and flow.

The embodiment also provides a heating circuit, which is prepared from the metal slurry, and the thickness of the heating circuit is 50-100 μm. The preparation method can adopt any mode of screen printing, spraying and dipping. The heating circuit comprises a heating part in the middle and electrodes respectively connected to two ends of the heating part.

The embodiment also provides an atomizing core, which comprises porous ceramic and a heating circuit arranged on the atomizing surface of the porous ceramic; the heating circuit is the heating circuit, the pore diameter of the porous ceramic is matched with the particle diameters of the metal powder and the glass powder, and the depth of the porous ceramic infiltrated by the metal slurry is 15-30 mu m.

Wherein the porosity of the porous ceramic is 45-65%, and the pore diameter is 10-40 μm. The axial direction of the middle hole of the porous ceramic is obliquely arranged with the plane of the atomization surface, and the inclination angle is 30-90 degrees.

As shown in fig. 1, this embodiment further provides a method for preparing an atomizing core, which includes the following steps:

s1, providing a porous ceramic and metal slurry: respectively providing porous ceramic and metal slurry, wherein the porous ceramic is the porous ceramic, and the metal slurry is the metal slurry.

S1.1, preparing porous ceramic: in order to ensure that the holes of the porous ceramic are orderly arranged and ensure the inclination angle between the axial direction of the holes in the porous ceramic and the atomization surface, the porous ceramic can be prepared by adopting a template method. Taking the preparation of zirconia porous ceramic as an example, the preparation of the porous ceramic comprises the following steps:

adding 1 part of polymer into 4-6 parts of binary system organic solvent, dissolving under the condition of keeping out of the sun, and uniformly mixing to obtain a mixed solution. And adding a binder and zirconia ceramic powder into the mixed solution in sequence, uniformly mixing, carrying out ball milling for 48-72 h, putting the ball-milled mixed solution into a vacuum box, vacuumizing for 30-60 min, taking the mixed solution out of the vacuum box, putting the mixed solution into a mold with a nylon net, and carrying out phase conversion by using water or gasoline as an extractant of an organic solvent to obtain a porous ceramic green body. The phase inversion time is 100-120 min. The depth of the die is 1-2 mm, and the aperture of the nylon net is 150-250 mu m. And taking the porous ceramic green body out of the mold, putting the porous ceramic green body into a drying oven, and drying at the temperature of 50-60 ℃ for 2-5 h. Then placing the dried porous ceramic green body into a box-type furnace for sintering, wherein the sintering is divided into three stages in total, namely, the first stage, heating to 280-320 ℃, and preserving heat for 1.5-2.5 h; in the second stage, the temperature is raised to 700-750 ℃, and the temperature is kept for 1.5-2.5 h; and in the third stage, the temperature is raised to 1000-1050 ℃, and the temperature is kept for 0.5-1.5 h. After sintering, the porous ceramic with the micro-channels is obtained.

The supercritical state drying of alcohol after extraction can prevent porosity reduction caused by collapse of pores due to surface tension of liquid in the drying process.

The mass ratio of the mixed solution to the binder to the zirconia ceramic powder is as follows: 1: 0.012-0.015: 0.75 to 0.80. The polymer comprises one or two of polysulfone, polyethersulfone, cellulose acetate, or vinylidene fluoride. The organic solvent comprises one or two of N-methyl pyrrolidone, N-dimethylformamide, N-dimethylacetamide and dimethyl sulfoxide. The binder is polyvinylpyrrolidone (PVP).

In order to increase the bonding strength between the porous ceramic and the glass phase in the metal slurry, the porous ceramic preferably includes at least one component having the same composition as the glass phase, and may include, for example, silica and/or alumina.

In order to enable the micro-channels and the plane of the atomizing surface to form a certain inclination angle, the direction of the template can be set in the preparation process, and the angle between the processed atomizing surface and the micro-channels can meet the setting requirement by processing the formed porous ceramic.

S1.2, preparing metal slurry: respectively preparing powder and an organic carrier. The powder is a mixture of metal powder and glass powder, when the powder is prepared, firstly, the metal powder is prepared according to the mass ratio requirement, after the metal powder is uniformly mixed, a proper amount of glass powder is added into the metal powder according to the mass ratio requirement, and the metal powder and the glass powder are uniformly mixed. When preparing the organic carrier, mixing the ethyl cellulose and the terpineol uniformly according to the mass ratio requirement. And gradually adding the prepared powder into the prepared organic carrier, and stirring while adding until the metal slurry can continuously draw and flow.

S2, coating metal slurry: and coating the metal slurry on the atomized surface of the porous ceramic to form the heating circuit.

S3, sintering: sintering the porous ceramic coated with the metal slurry, wherein the sintering temperature is 1030 ℃ and 1150 ℃, and the sintering time is 7-12 minutes. In order to provide the heating circuit and the porous ceramic with better performance, the sintering temperature is preferably 1100-1120 ℃, and the sintering time is preferably 8-11 minutes.

The embodiment also provides an electronic cigarette, which comprises a shell, a base detachably connected with the shell, a power supply fixed on the base, and an atomizing core arranged in the shell, wherein the atomizing core is prepared by the preparation method, and a heating circuit of the atomizing core is electrically connected with the power supply.

To prove the effectiveness of the method of the present invention, the atomizing core prepared in the above example was tested by first bonding wires on the electrodes of the heating circuit and then performing a pull test using a tensile tester, and the test result was that the bonding strength between the heating circuit and the porous ceramic was higher than 0.100 kgf. When the atomization core is evaluated by adopting a dry burning method and a cold and hot impact method, the heating circuit is not blown or dropped, and the use requirement can be met.

The atomization core is detected, the thickness of the heating circuit is 50-100 μm, the infiltration depth of the metal slurry is 15-30 μm, and the bonding strength between the heating circuit and the porous ceramic is higher than 0.100 kgf. The impregnation depth is proper, so that the bonding strength between the heating circuit and the porous ceramic can be ensured, and the phenomenon that the heating circuit is short-circuited or burnt due to uneven heating caused by overlarge impregnation depth is avoided.

Example 1: in the atomizing core of the embodiment, the mass ratio of the metal powder, the glass powder and the organic carrier in the metal slurry is 100: 10: 20.

wherein, each 100 parts by mass of the metal powder comprises 20 parts of Ni powder, 15 parts of Cr powder and 65 parts of NiCr₂₀And (3) alloy powder. Wherein the Ni powder has a median particle diameter D50 of 9.8 μm, the Cr powder has a median particle diameter D50 of 9.6 μm, and NiCr₂₀The median particle diameter D50 of the alloy powder was 30 μm.

The glass powder comprises 40 parts of Si, 20 parts of Al, 10 parts of B and 30 parts of the rest components in each 100 parts by mass of the glass powder. The median particle diameter D50 of the glass frit was 20 μm. In the organic carrier, the mass ratio of ethyl cellulose to terpineol is 30: 70.

the porosity of the porous ceramic is 50%, the pore diameter is 30 μm, and the thickness of the prepared heating circuit is 50 μm.

Example 2: the metal paste of the atomizing core of this example is substantially the same as that of example 1, except that: the glass powder comprises 42 parts of Si, 19 parts of Al, 10 parts of B and 29 parts of the rest components in each 100 parts by mass of the glass powder.

Example 3: the metal paste of the atomizing core of this example is substantially the same as that of example 1, except that: the glass powder comprises 44 parts of Si, 19 parts of Al, 9 parts of B and 28 parts of the rest components per 100 parts by mass of the glass powder.

Example 4: the metal paste of the atomizing core of this example is substantially the same as that of example 1, except that: the glass powder comprises 46 parts of Si, 18 parts of Al, 9 parts of B and 27 parts of the rest components in each 100 parts by mass of the glass powder.

Example 5: the metal paste of the atomizing core of this example is substantially the same as that of example 1, except that: the glass powder comprises 48 parts of Si, 18 parts of Al, 8 parts of B and the balance of 26 parts per 100 parts by mass of the glass powder.

Example 6: the metal paste of the atomizing core of this example is substantially the same as that of example 1, except that: the glass powder comprises 50 parts of Si, 17 parts of Al, 8 parts of B and 25 parts of the rest components in each 100 parts by mass of the glass powder.

Example 7: the metal paste of the atomizing core of this example is substantially the same as that of example 1, except that: the glass powder comprises, per 100 parts by mass, 52 parts of Si, 17 parts of Al, 7 parts of B and the balance of 24 parts.

Example 8: the metal paste of the atomizing core of this example is substantially the same as that of example 1, except that: the glass frit includes, per 100 parts by mass of the glass frit, 54 parts of Si, 16 parts of Al, 7 parts of B, and 23 parts of the remaining components.

Example 9: the metal paste of the atomizing core of this example is substantially the same as that of example 1, except that: the glass powder comprises 56 parts of Si, 16 parts of Al, 6 parts of B and 22 parts of the rest components in each 100 parts by mass of the glass powder.

Example 10: in the atomizing core of the embodiment, the mass ratio of the metal powder, the glass powder and the organic carrier in the metal slurry is 100: 8: 10.

the glass powder comprises 50 parts of Si, 17 parts of Al, 8 parts of B and 25 parts of the rest components in each 100 parts by mass of the glass powder. The median particle diameter D50 of the glass frit was 50 μm. In the organic carrier, the mass ratio of ethyl cellulose to terpineol is 40: 60.

the porosity of the porous ceramic is 65%, the pore diameter is 40 μm, and the thickness of the prepared heating circuit is 50 μm.

Each 100 parts by mass of the metal powder comprises 10 parts of Ni powder, 20 parts of Cr powder and 70 parts of NiCr₂₀And (3) alloy powder. Wherein the Ni powder has a median particle diameter D50 of 6 μm, the Cr powder has a median particle diameter D50 of 9 μm, and NiCr₂₀The median particle diameter D50 of the alloy powder was 30 μm.

Example 11: the metal paste of the atomizing core of this example is substantially the same as that of example 10, except that: the metal powder comprises 20 parts of Ni powder, 15 parts of Cr powder and 65 parts of NiCr powder per 100 parts by mass of metal powder₂₀And (3) alloy powder. Wherein the Ni powder has a median particle diameter D50 of 8 μm, the Cr powder has a median particle diameter D50 of 6 μm, and NiCr₂₀The median particle diameter D50 of the alloy powder was 25 μm.

Example 12: the metal paste of the atomizing core of this example is substantially the same as that of example 10, except that: the metal powder comprises 30 parts of Ni powder, 8 parts of Cr powder and 62 parts of NiCr powder per 100 parts by mass of the metal powder₂₀And (3) alloy powder. Wherein the Ni powder has a median particle diameter D50 of 9 μm, the Cr powder has a median particle diameter D50 of 4 μm, and NiCr₂₀The median diameter D50 of the alloy powder was 50 μm.

The impregnation depth and the interfacial strength of the above examples were measured and are shown in table 1.

TABLE 1

As can be seen from the data in the above table, in the above 12 examples, the impregnation depth of the heat generating circuit was not more than 30 μm at the maximum and not less than 15 μm at the minimum, and the interface bonding strength was 0.1005 at the minimum, and the impregnation depth was appropriate, which effectively ensured the bonding strength between the heat generating circuit and the porous ceramic.

The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.

The above examples only express preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.