CN112869248B - Preparation method of ceramic atomizing core - Google Patents
Preparation method of ceramic atomizing core Download PDFInfo
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- CN112869248B CN112869248B CN202110042990.5A CN202110042990A CN112869248B CN 112869248 B CN112869248 B CN 112869248B CN 202110042990 A CN202110042990 A CN 202110042990A CN 112869248 B CN112869248 B CN 112869248B
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- 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
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- 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
Abstract
The invention provides a preparation method of a ceramic atomizing core, which comprises the following steps: s1, ceramic powder surface modification: mixing the ceramic powder with a surface modifier, carrying out ball milling pretreatment together, and drying to obtain the surface modified ceramic powder. S2, preparing a mixed feed: and mixing an organic glue system with the surface modified ceramic powder to obtain a mixed feed. S3, injection molding: and putting the mixed feed into a screw type injection machine, and performing injection molding to obtain a ceramic atomization core green body. S4, degreasing: and degreasing the ceramic atomization core green body by using a solvent to obtain a solvent-degreased green body. S5, sintering: and sintering the solvent degreased green body by adopting a hot pressing method to obtain the ceramic atomization core. The preparation method of the ceramic atomizing core provided by the invention can effectively improve the strength of the ceramic atomizing core, and the ceramic atomizing core has good oil absorption rate, and the preparation method is simple and efficient.
Description
Technical Field
The invention belongs to the technical field of electronic cigarettes, and particularly relates to a preparation method of a ceramic atomizing core.
Background
In the prior art, a ceramic porous atomizing core is mostly formed into a blank body by adopting a hot-press casting mode, then the blank body is embedded into an adsorbent, the temperature is increased to 900-1100 ℃ at a proper speed, a blank body forming binder is removed, so that the blank body has certain strength, and finally, the blank body with certain strength is placed into a sintering furnace to be sintered, so that a final product can be obtained. The method needs high-temperature heating during sintering, and high-temperature sintering may cause the strength of the ceramic to be lower.
With the rapid development of modern information technology, increasingly high requirements are put forward on the aspects of miniaturization, portability, multifunction, high reliability, low cost and the like of electronic products. The lower sintering temperature is a necessary condition for reducing the production cost and realizing large-scale industrial production.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a ceramic atomizing core, which can realize sintering at low temperature, can effectively improve the strength of the ceramic atomizing core, has good oil absorption rate and is simple and efficient.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a ceramic atomizing core comprises the following steps:
s1, ceramic powder surface modification: mixing the ceramic powder with a surface modifier, and carrying out ball milling pretreatment together to obtain surface modified ceramic powder; wherein the ceramic powder is natural diatomite or synthetic silicon dioxide;
s2, preparing a mixed feed: mixing an organic glue system with the surface modified ceramic powder prepared in the step S1 to obtain a mixed feed;
s3, injection molding: putting the mixed feed prepared in the step S2 into a screw type injection machine for injection molding to obtain a ceramic atomizing core green body;
s4, degreasing: removing the surface modifier and the organic colloid system in the ceramic atomizing core green body prepared in the step S3 by using a solvent, heating and drying to obtain a solvent degreased green body;
s5, sintering: and (5) sintering the solvent degreased green body prepared in the step (S4) by adopting a hot pressing method to obtain the ceramic atomization core.
The technical scheme is further improved as follows:
the granularity of the ceramic powder is 15-30 mu m.
The surface modifier in the step S1 comprises at least one of stearic acid, oleic acid, dodecahydroxystearic acid and citric acid, and the mass part of the surface modifier added is 1-5 parts per 100 parts by mass of the ceramic powder.
The organic glue system in the step S2 comprises a silicon rubber adhesive, stearic acid, polyethylene, polypropylene and resin; the silicone rubber adhesive comprises stearic acid, polyethylene, polypropylene and resin, and the mass ratio is (1-50); wherein the required organic colloid accounts for 15-30 parts by mass per 100 parts by mass of the mixed feed.
Before the step S2, an organic rubber system banburying step is also included:
heating the silicone rubber adhesive in an internal mixer to a molten state, continuously heating the silicone rubber adhesive in the molten state to 180-200 ℃, respectively adding resin, polyethylene and polypropylene, starting the internal mixer, carrying out internal mixing for 20-40min, then adding stearic acid, and further carrying out internal mixing for 3-4h.
The molding temperature in the injection molding in the step S3 is 120-160 ℃, and the molding pressure is 50-120MPa.
In the step S4, the solvent is one of kerosene, gasoline or white gasoline, the degreasing temperature is 90-120 ℃, and the degreasing time is 20-24h.
The method also comprises the following steps after the step S4:
and (3) placing the solvent degreased green body in a water bath kettle for further degreasing and cleaning, wherein the water bath temperature is 80-90 ℃, and the time is 18-24h, so as to obtain the water bath degreased green body.
And S5, placing the solvent degreased green body prepared in the step S4 in constant-temperature pressurizing equipment, and sintering by adopting a hot-pressing method to obtain the ceramic atomization core.
The sintering temperature is 160-200 ℃, the pressure is 350-500MPa, and the heat preservation and pressure maintaining time is 20-30min.
According to the technical scheme of the invention, the preparation method of the ceramic atomizing core firstly carries out surface modification on the ceramic powder to ensure that the ceramic powder is tightly combined with the surface modifier. And the organic colloid is combined with the ceramic powder, so that the organic colloid has good wettability with the ceramic powder, the interface bonding strength between the organic colloid and the ceramic powder is improved, and the strength of the atomizing core is improved. And because the organic colloid is uniformly distributed in the ceramic powder, the ceramic can have a uniform pore structure after the organic colloid is removed subsequently, so that the oil absorption rate of the ceramic atomization core is improved. In the molding step, an injection molding mode of an injection machine is adopted, and the injection machine extrudes the ceramic green body during injection molding, so that the ceramic green body has higher green body density, and the sintering strength of a final product is improved. The hot pressing method is adopted to sinter the green body, so that the sintering temperature is effectively reduced, the cost is saved, and the strength of the atomizing core is improved. The ceramic atomizing core prepared by the method disclosed by the invention not only is effectively improved in strength, but also is uniform in pores, high in oil absorption rate and good in comprehensive performance.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a ceramic 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.
Example 1: the preparation method of the ceramic atomizing core comprises the following steps:
s1, ceramic powder surface modification: the method is characterized in that natural microporous diatomite or synthetic silica is used as ceramic powder, and the particle size of the ceramic powder is 15 microns. And mixing the ceramic powder with a surface modifier, carrying out ball milling pretreatment together to form a coating layer on the surface of the ceramic powder, and drying to obtain the surface modified ceramic powder. The mass ratio of the ceramic powder to the surface modifier is 100:1, the thickness of the coating layer is 10nm.
The surface modifier is composed of at least one of stearic acid, oleic acid, dodecahydroxystearic acid and citric acid, and the mass part of the surface modifier added is 1-5 parts per 100 parts by mass of the ceramic powder.
In the step, the ceramic powder has small particle size and uniform particles, and is more favorable for being uniformly mixed with the surface modifier, so that the bonding property of the ceramic powder is better, and the strength of the ceramic is favorably improved.
S2, preparing mixed feed: firstly, banburying an organic rubber system, and then mixing the banburied organic rubber system with the surface modified ceramic powder prepared in the step S1 to obtain mixed feed, wherein the mass ratio of the mixed feed to the organic rubber system is 100:15.
the organic glue system comprises a silicon rubber adhesive (PW), stearic Acid (SA), polyethylene (PE), polypropylene (PP) and resin; the mass ratio PW to SA to PP to resin = 37.
And (3) banburying an organic rubber system, namely putting the PW into a W-shaped twin-roll internal mixer for heating, respectively adding resin, PE and PP after the PW is in a molten state and the temperature of the liquid PW reaches 200 ℃, starting the internal mixer, banburying for 30min, adding SA, continuing to banbury for 4h, then finishing banburying, and adding micro-positive pressure 100Pa during banburying.
S3, injection molding: and (3) putting the mixed feed prepared in the step (S2) into a screw type injection machine, and performing injection molding to obtain a ceramic atomizing core green compact. The molding temperature during injection molding was 120 ℃ and the molding pressure was 120MPa.
S4, degreasing: and (4) taking one of kerosene, gasoline or white electric oil as an organic solvent, completely soaking the ceramic atomizing core green body prepared in the step (S3) in the organic solvent in a constant-temperature oil bath, heating to 120 ℃, and preserving heat for 20 hours. And (3) removing the surface modifier in the ceramic atomized core green body and the component which is soluble in the organic solvent in the organic glue system by organic solvent extraction degreasing to obtain the solvent degreased green body.
And (3) placing the solvent degreased green body in a water bath kettle for further degreasing and cleaning, wherein the water bath temperature is 80 ℃, and the time is 24 hours, so as to obtain the water bath degreased green body. The water bath extraction degreasing can further remove water-soluble organic components in the ceramic atomizing core green body.
And (3) drying the water-bath degreased green body in a muffle furnace for 12h at the drying temperature of 90 ℃ at the heating speed of 4 ℃/min to finally obtain the degreased green body.
S5, sintering: and (5) placing the degreased green body prepared in the step (S4) in constant-temperature pressurizing equipment, applying high pressure and low temperature, and sintering by adopting a hot-pressing method. The low temperature is 200 ℃, the high pressure is 350MPa, and the heat preservation and pressure maintaining time is 30min, so that the ceramic atomization core is obtained.
In the embodiment, the organic glue system is used as a pore-forming agent, and the phenolic resin is used for providing bonding strength, so that the ceramic atomization core green body forms porous structure ceramic with certain strength after degreasing, the porous structure is favorable for improving the oil absorption rate of the atomization core, and the improvement of the strength is favorable for prolonging the service life of the atomization core.
Example 2, the method of making the ceramic atomizing core of this example, is substantially the same as example 1, except that:
s1, ceramic powder surface modification: the particle size of the ceramic powder is 30 microns, and the mass ratio of the ceramic powder to the surface modifier is 100:5, the thickness of the coating layer is 20nm.
S2, preparing a mixed feed: the mass ratio of the mixed feed to the organic glue system is 100:20. the mass ratio of the organic glue system PW to SA to PP to resin = 43.
And (3) banburying an organic rubber system, namely putting the PW into a W-shaped pair roller banbury mixer to heat, adding resin, PE and PP respectively after the PW is in a molten state and the temperature of the liquid PW reaches 180 ℃, starting the banbury mixer, banburying for 40min, adding SA, continuing to banbury for 3h, finishing banburying, and adding micro-positive pressure 250Pa during banburying.
S3, injection molding: the molding temperature during injection molding was 160 ℃ and the molding pressure was 50MPa.
S4, degreasing: the heating temperature in the constant temperature oil bath is 90 ℃, and the heat preservation time is 24h.
The water bath temperature is 90 ℃ and the time is 18h.
And (3) drying the water-bath degreased green body in a muffle furnace for 14h at the drying temperature of 80 ℃ at the heating speed of 3 ℃/min to finally obtain the degreased green body.
Example 3, a method of making a ceramic atomizing core of this example, substantially as in example 1, except that:
s1, ceramic powder surface modification: the particle size of the ceramic powder is 20 microns, and the mass ratio of the ceramic powder to the surface modifier is 100:2.5, the thickness of the coating layer is 15nm.
S2, preparing mixed feed: the mass ratio of the mixed feed to the organic glue system is 100:30. the mass ratio of the organic glue system PW to SA to PP to resin = 50.
And (3) banburying of an organic rubber system, namely putting the PW into a W-shaped twin-roll internal mixer for heating, respectively adding the resin, the PE and the PP after the PW is in a molten state and the temperature of the liquid PW reaches 190 ℃, starting the internal mixer, banburying for 20min, adding SA, continuing to banbury for 3.5h, then finishing banburying, and adding 150Pa under micro-positive pressure during banburying.
S3, injection molding: the molding temperature in the injection molding was 140 ℃ and the molding pressure was 80MPa.
S4, degreasing: the heating temperature in the constant temperature oil bath is 100 ℃, and the heat preservation time is 22h.
The water bath temperature was 85 ℃ and the time was 21h.
And (3) drying the water-bath degreased green body in a muffle furnace for 10h at the drying temperature of 100 ℃, wherein the heating speed is 5 ℃/min during heating, and finally obtaining the degreased green body.
Example 4, a method of making a ceramic atomizing core of this example, substantially as in example 1, except that:
s1, ceramic powder surface modification: the particle size of the ceramic powder is 25 micrometers, and the mass ratio of the ceramic powder to the surface modifier is 100: and 3, the thickness of the coating layer is 17nm.
S2, preparing mixed feed: the mass ratio of the mixed feed to the organic glue system is 100:25. the mass ratio of the organic glue system PW to SA to PP to resin = 30.
S5, sintering: the low temperature is 170 ℃, the high pressure is 500MPa, and the heat preservation and pressure maintaining time is 20min.
Example 5, a method of making a ceramic atomizing core of this example, substantially as in example 1, except that:
s5, sintering: the low temperature is 160 ℃, the high pressure is 450MPa, and the heat preservation and pressure maintaining time is 20min.
Example 6, a method of making a ceramic atomizing core of this example, substantially as in example 1, except that:
s5, sintering: the low temperature is 180 ℃, the high pressure is 400MPa, and the heat preservation and pressure maintaining time is 25min.
Comparative example: the ceramic atomizing core of the comparative example is prepared by adopting a traditional hot-press casting method, and is mainly used for comparison with the embodiment, and the specific steps are as follows:
1. and adding a surface modifier into the ceramic powder, and performing ball milling and mixing to obtain the surface modified ceramic powder.
2. And (2) adding the surface modified ceramic powder prepared in the step (1) into molten paraffin, and stirring and mixing the mixture uniformly to obtain slurry.
3. And (3) adding the slurry prepared in the step (2) into a hot-press casting forming machine, and injecting the slurry into a die at a proper pressure and temperature for casting forming to obtain a ceramic atomized core green body.
4. Demoulding, properly finishing the ceramic atomizing core green body, embedding the ceramic atomizing core green body into an adsorbent, and heating to 900-1100 ℃ at a proper speed to completely remove paraffin in the ceramic atomizing core green body.
5. And finally, placing the ceramic atomizing core green body subjected to wax removal in the step 5 into a sintering furnace, and sintering and forming at 1150 ℃ to finally obtain the ceramic atomizing core.
In order to prove that the preparation method of the invention is real and effective, the ceramic atomizing cores prepared in the above examples and comparative examples are tested and the performances of the two are compared, and the comparison result is shown in table 1:
TABLE 1
| Examples | Oil absorption rate mg/s | Compressive strength MPa |
| 1 | 6.1 | 6.3375 |
| 2 | 6.4 | 6.345 |
| 3 | 6.3 | 6.3625 |
| 4 | 6.6 | 6.4125 |
| 5 | 6.9 | 6.3825 |
| 6 | 7.2 | 6.3575 |
| 7 | 6.3 | 6.425 |
| Comparative example | 3.7 | 4.0925 |
According to the detection results, the oil absorption rate and the compressive strength of the six embodiments of the invention are much higher than those of the ceramic atomizing core prepared by the traditional hot die-casting method, so that the ceramic atomizing core prepared by the method has better comprehensive performance. The ceramic atomizing core prepared by the invention combines organic materials with inorganic materials, improves the interface bonding strength of the green body of the ceramic atomizing core, adopts an injection molding mode, greatly improves the production efficiency and the production quality stability, has higher oil absorption rate and higher strength, and greatly prolongs the service life of the atomizing core.
All possible combinations of the technical features in the above embodiments may not be described for the sake of brevity, but should be considered as being within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above examples only express the preferred embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as the limitation of the invention patent scope. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (4)
1. The preparation method of the ceramic atomizing core is characterized by comprising the following steps of:
s1, ceramic powder surface modification: mixing ceramic powder with a surface modifier, carrying out ball milling pretreatment together to form a coating layer on the surface of the ceramic powder, and drying to obtain surface modified ceramic powder; wherein the ceramic powder is natural diatomite or synthetic silicon dioxide; the granularity of the ceramic powder is 15-30 mu m; 1-5 parts of surface modifier is added into every 100 parts of the ceramic powder by mass;
s2, preparing mixed feed: mixing an organic glue system with the surface modified ceramic powder prepared in the step S1 to obtain a mixed feed; the organic adhesive system comprises a silicone rubber adhesive, stearic acid, polyethylene, polypropylene and resin; the resin is phenolic resin; the mass ratio of the silicone rubber adhesive to stearic acid to polyethylene to polypropylene to resin = 30-50;
before the step S2, an organic glue system banburying step is also included:
heating the silicone rubber adhesive in an internal mixer to a molten state, continuously heating the silicone rubber adhesive in the molten state to 180-200 ℃, respectively adding resin, polyethylene and polypropylene, starting the internal mixer, carrying out internal mixing for 20-40min, then adding stearic acid, and further carrying out internal mixing for 3-4 h;
s3, injection molding: putting the mixed feed prepared in the step S2 into a screw type injection machine, and performing injection molding to obtain a ceramic atomizing core green body; the molding temperature during the injection molding is 120-160 ℃, and the molding pressure is 50-120 MPa;
s4, degreasing: removing the surface modifier and the organic colloid system in the ceramic atomizing core green body prepared in the step S3 by using a solvent to obtain a solvent degreased green body; the degreasing temperature is 90-120 ℃, and the degreasing time is 20-24 h;
placing the solvent degreased green body in a water bath kettle for further degreasing and cleaning, wherein the water bath temperature is 80-90 ℃, and the time is 18-24 hours, so as to obtain a water bath degreased green body; placing the water-bath degreased green body in a muffle furnace for drying to obtain a degreased green body;
s5, sintering: sintering the degreased green body prepared in the step S4 by adopting a hot pressing method to obtain a ceramic atomizing core; the sintering temperature is 160-200 ℃, the pressure is 350-500MPa, and the heat preservation and pressure maintaining time is 20-30min.
2. The method of making a ceramic atomizing core of claim 1, wherein: the surface modifier in step S1 includes at least one of stearic acid, oleic acid, dodecahydroxystearic acid, and citric acid.
3. The method of making a ceramic atomizing core of claim 1, wherein: in the step S4, the solvent is one of kerosene, gasoline or white electric oil.
4. The method of making a ceramic atomizing core according to claim 1, characterized in that: and S5, placing the degreased green body obtained in the step S4 in constant-temperature pressurizing equipment, and sintering by adopting a hot-pressing method to obtain the ceramic atomizing core.
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