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CN112811925A - Humidity-sensitive porous ceramic, atomizing core and preparation method thereof - Google Patents

Humidity-sensitive porous ceramic, atomizing core and preparation method thereof Download PDF

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Publication number
CN112811925A
CN112811925A CN202110024103.1A CN202110024103A CN112811925A CN 112811925 A CN112811925 A CN 112811925A CN 202110024103 A CN202110024103 A CN 202110024103A CN 112811925 A CN112811925 A CN 112811925A
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CN
China
Prior art keywords
component
porous ceramic
parts
sensitive porous
humidity
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Pending
Application number
CN202110024103.1A
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Chinese (zh)
Inventor
林光榕
秦飞
刘卫丽
郑贤彬
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Huizhou Xinhongwei Technology Co ltd
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Huizhou Xinhongwei Technology Co ltd
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Priority to CN202110024103.1A priority Critical patent/CN112811925A/en
Publication of CN112811925A publication Critical patent/CN112811925A/en
Priority to PCT/CN2021/131626 priority patent/WO2022148146A1/en
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Abstract

The invention relates to a humidity-sensitive porous ceramic, an atomizing core and a preparation method thereof, wherein the humidity-sensitive porous ceramic is prepared from a substrate material comprising 1-20 parts of a component A, 1-10 parts of a component B, 1-20 parts of a component C, 1-30 parts of a pore-forming agent and 1-10 parts of a sintering aid, wherein the component A is SnO2、ZnO、TiO2The component B is LiZnVO4、ZnCrVO4，V2O5、Fe2O3C component is Li2O、Na2O，K2O，MgO，CaOne or more of O; the atomization core comprises a liquid guide body and a heating element, and the liquid guide body is made of humidity-sensitive porous ceramics; the preparation method comprises the following steps: weighing a component A, a component B, a component C, a pore-forming agent and a sintering aid, and placing the components in a ball milling device for mixing and ball milling; baking and drying to obtain mixed powder; thirdly, heating the paraffin until the paraffin is melted, stirring and adding the mixed powder to obtain paraffin slurry; fourthly, injecting paraffin slurry into the mold, and cooling to obtain a wax mold; placing the sample into a furnace for wax removal to obtain a wax-removed sample; sixthly, sintering the mixture in a protective atmosphere to obtain the humidity-sensitive porous ceramic.

Description

Humidity-sensitive porous ceramic, atomizing core and preparation method thereof
Technical Field
The invention belongs to the technical field of humidity-sensitive porous ceramics and atomizing cores made of humidity-sensitive porous ceramics, and particularly relates to humidity-sensitive porous ceramics, an atomizing core and a preparation method thereof.
Background
The electronic atomizer comprises a liquid storage device and an atomizing core, wherein the liquid storage device is filled with liquid to be atomized, the liquid to be atomized can be tobacco liquid or a solution containing a medicine, the atomizing core generally comprises a liquid guide element and a heating element, the liquid guide element receives, permeates and conducts the liquid to be atomized in the liquid storage device, the heating element generates heat after being electrified, and the atomizing core is used for heating, evaporating and atomizing the liquid to be atomized into aerosol or steam and vapor so that a user can conveniently suck the liquid to achieve the purpose of health medical treatment. The atomizing core is the key part of electronic atomizer, and its performance is good or bad and has directly decided electronic atomizer's atomization effect, heating efficiency and use experience.
The atomizing core in the existing market is usually composed of a liquid guide cotton and a heating resistance wire or a ceramic liquid guide and a heating resistance wire, the combination mode of the resistance wire and the ceramic liquid guide is implantable, printed, surface-mounted and the like, and different combination modes bring certain degree of promotion on heat transfer efficiency. The existing atomizing core is to use up or conduct when not smooth and easy when waiting to atomize liquid, and the temperature of atomizing core will sharply rise, leads to atomizing core to take place dry combustion method, and atomizing core is burnt easily and is lost and produce the taste of scorching, causes bad use experience for the user. The existing method for preventing the atomization core from being burnt dry is to detect the temperature and turn off the power supply to stop using when the temperature rises to a set threshold value. The temperature is detected only after the lack of the liquid to be atomized occurs, so that the method has certain hysteresis and avoids the occurrence of dry burning to a certain degree.
Disclosure of Invention
The invention aims to solve the technical problem of untimely dry burning prevention of the existing atomizing core and provides a humidity-sensitive porous ceramic, an atomizing core and a preparation method thereof.
The invention adopts the technical scheme that the moisture-sensitive porous ceramic is prepared from a substrate material, wherein the substrate material comprises a component A, a component B, a component C, a pore-forming agent and a sintering aid, and the component A is SnO2、ZnO、TiO2The component B is LiZnVO4、ZnCrVO4，V2O5、Fe2O3Is Li, the C component is Li2O、Na2O，K2One or more of O, MgO and CaO, wherein the component A comprises 1-20 parts, the component B comprises 1-10 parts, the component C comprises 1-20 parts, the pore-forming agent comprises 1-30 parts, and the sintering aid comprises 1-10 parts.
Preferably, the component A comprises 1-10 parts of component B, 1-5 parts of component C, 1-20 parts of pore-forming agent and 1-10 parts of sintering aid.
Preferably, the pore-forming agent is at least one of graphite, starch, flour, bean flour, polystyrene microspheres, polymethyl methacrylate microspheres, carbonate, ammonium salt, sucrose and fibers, and the particle size of the pore-forming agent is 1-200 microns.
Preferably, the sintering aid is at least one of boron oxide, boric acid, oleic acid, stearic acid, sodium silicate and calcium oxide.
Preferably, the base material further comprises the following components in parts by weight: 1-40 parts of nano silicon oxide.
Preferably, the nano silicon oxide is nano silicon dioxide, and the nano silicon dioxide is colloidal nano silicon dioxide or powdery nano silicon dioxide.
Preferably, the porosity of the moisture-sensitive porous ceramic is 30-70%.
The other technical solution of the invention is that the atomizing core comprises a liquid guide body for conducting liquid to be atomized and a heating element arranged on the liquid guide body, wherein the liquid guide body is made of the humidity-sensitive porous ceramic.
The invention also provides a technical scheme that the preparation method of the humidity-sensitive porous ceramic comprises the following steps:
weighing a component A, a component B, a component C, a pore-forming agent and a sintering aid according to a formula, and placing the components in a ball milling device for mixing and ball milling; the component A is SnO2、ZnO、TiO2The component B is LiZnVO4、ZnCrVO4，V2O5、Fe2O3Is Li, the C component is Li2O、Na2O，K2One or more of O, MgO and CaO;
baking and drying the mixture subjected to ball milling to obtain mixed powder;
thirdly, heating the paraffin to a melting state, adding the mixed powder while stirring, and continuously stirring for 1-8 hours after the addition is finished to obtain paraffin slurry;
fourthly, injecting the paraffin slurry into a pre-prepared mold, cooling and molding, and demolding to obtain a wax mold;
fifthly, putting the wax mold into a furnace for preheating for paraffin removal, so as to obtain a paraffin removal sample;
sixthly, placing the paraffin removal sample into a furnace and sintering in a protective atmosphere, wherein the sintering process comprises heating, heat preservation and cooling, and the humidity-sensitive porous ceramic is obtained.
Preferably, in the first step, the rotating speed of the ball milling device is set to be 150-350 rpm, the ball milling time is 1-12 h, and the diameter of the grinding material is 1-20 mm.
Preferably, in the step II, the temperature of baking and drying is 60-120 ℃, and the time of baking and drying is 2-12 h.
Preferably, in the step three, the melting point of the paraffin is 50-110 ℃, and the weight of the paraffin is 10-60% of the weight of the mixed powder.
Preferably, in the step fifthly, the temperature for removing the wax is 400-800 ℃, and the time for removing the wax is 2-12 hours.
Preferably, in the step sixteenth, the sintering temperature is 700-1200 ℃, the heating speed is 1-5 ℃/min, and the sintering heat preservation time is 2-12 hours; the sintering protective atmosphere is a reducing atmosphere, the reducing atmosphere comprises the mixture of hydrogen and gases such as argon, nitrogen, helium and the like, wherein the hydrogen accounts for 1-20% of the mixed gas.
Compared with the prior art, the invention has the beneficial effects that:
the invention utilizes the characteristic that the humidity sensitive material has different resistance values when the dryness and humidity of the liquid to be atomized are different, the humidity sensitive material is added into the ceramic matrix material to be integrated with the porous ceramic to form the humidity sensitive porous ceramic as the liquid guide of the atomizing core, the liquid guide can conduct the liquid to be atomized and has the resistance value sensitive to the humidity, and the humidity can be measured by detecting the resistance of the liquid guide, so that the humidity of the liquid to be atomized is reduced and can be rapidly detected when the liquid to be atomized is lacked in the liquid guide, thereby reducing the power or shutting down the power supply in time and preventing the atomizing core from being dried and burnt rapidly without delay.
Drawings
Fig. 1 is a schematic view of the structure of an atomizing core of the present invention.
Detailed Description
The moisture-sensitive material in the present invention refers to a functional material whose resistance value changes with the humidity of the environment, and is formed by processing materials which are easy to absorb moisture, such as magnesium oxide and chromium oxide, into an electric insulating material. It can convert the change of humidity into electric signal through resistance value. The humidity sensitive material can realize automatic indication, automatic recording, automatic control and regulation of humidity.
The invention relates to a humidity-sensitive porous ceramic, which is prepared from a substrate material, wherein the substrate material comprises a component A, a component B, a component C, a pore-forming agent and a sintering aid, and the component A is SnO2、ZnO、TiO2One or more of the components B is LiZnVO4、ZnCrVO4，V2O5、Fe2O3One or more of them, and the C component is Li2O、Na2O，K2One or more of O, MgO and CaO, wherein the component A comprises 1-20 parts, the component B comprises 1-10 parts, the component C comprises 1-20 parts, the pore-forming agent comprises 1-30 parts, and the sintering aid comprises 1-10 parts. Preferably, the component A is 1-10 parts, the component B is 1-5 parts,1-10 parts of a component C, 1-20 parts of a pore-forming agent and 1-10 parts of a sintering aid.
The pore-forming agent is at least one of graphite, starch, flour, bean flour, polystyrene microspheres, polymethyl methacrylate microspheres, carbonate, ammonium salt, sucrose and fibers, and the particle size of the pore-forming agent is 1-200 microns. The sintering aid is at least one of boron oxide, boric acid, oleic acid, stearic acid, sodium silicate and calcium oxide. The porosity of the moisture-sensitive porous ceramic is 30-70%.
In addition, the base material can also comprise the following raw material components in parts by weight: 1-40 parts of nano silicon oxide, wherein the nano silicon oxide is nano silicon dioxide, and the nano silicon dioxide is colloidal nano silicon dioxide or powdery nano silicon dioxide. After the components of the nano-silicon oxide are added, a micro-nano composite structure is formed through a curing reaction in the calcining process, the nano-silicon oxide can effectively reduce the sintering temperature during the solid phase reaction with the ceramic powder due to the ultrahigh specific surface area and the large amount of hydroxyl on the surface, and the nano-silicon oxide can ensure that the product can simultaneously keep high porosity and realize high strength. Under the conditions of high strength and stable internal structure, the moisture-sensitive porous ceramic is not easy to crack, impurities are not easy to separate out and heavy metals are not easy to precipitate in the using process, and the heavy metals can be prevented from exceeding the standard to the maximum extent.
The humidity-sensitive porous ceramic can be made into an atomizing core, the atomizing core is used for electronic atomizing equipment (not shown in the figure), the electronic atomizing equipment comprises an atomizing component and a battery component, and the battery component is used for controlling the atomizing component and supplying power to the atomizing component. The atomization assembly comprises a liquid storage device and an atomization core, liquid to be atomized is filled in the liquid storage device, and the liquid to be atomized can be tobacco juice or a solution containing medicines. The atomizing core comprises a liquid guide body used for conducting liquid to be atomized and a heating element arranged on the liquid guide body, wherein the liquid guide body is made of humidity-sensitive porous ceramic.
The preparation method of the humidity-sensitive porous ceramic comprises the following steps:
weighing a component A, a component B, a component C, a pore-forming agent and a sintering aid according to a formula, and placing the components in a ball milling device for mixing and ball milling; the group ADivided into SnO2、ZnO、TiO2The component B is LiZnVO4、ZnCrVO4，V2O5、Fe2O3Is Li, the C component is Li2O、Na2O，K2One or more of O, MgO and CaO;
baking and drying the mixture subjected to ball milling to obtain mixed powder;
thirdly, heating the paraffin to a melting state, adding the mixed powder while stirring, and continuously stirring for 1-8 hours after the addition is finished to obtain paraffin slurry;
fourthly, injecting the paraffin slurry into a pre-prepared mold, cooling and molding, and demolding to obtain a wax mold;
fifthly, putting the wax mold into a furnace for preheating for paraffin removal, so as to obtain a paraffin removal sample;
sixthly, placing the paraffin removal sample into a furnace and sintering in a protective atmosphere, wherein the sintering process comprises heating, heat preservation and cooling, and the humidity-sensitive porous ceramic is obtained.
In the step, the rotating speed of a ball milling device is set to be 150-350 rpm, the ball milling time is 1-12 h, and the diameter of the grinding material is 1-20 mm. In the step II, the temperature for baking and drying is 60-120 ℃, and the time for baking and drying is 2-12 h. In the step three, the melting point of the paraffin is 50-110 ℃, and the weight of the paraffin is 10-60% of the weight of the mixed powder. In the step, the temperature for removing the wax is 400-800 ℃, and the time for removing the wax is 2-12 hours. Sixthly, sintering at the temperature of 700-1200 ℃, heating at the speed of 1-5 ℃/min, and keeping the sintering temperature for 2-12 h; the sintering protective atmosphere is a reducing atmosphere, the reducing atmosphere comprises the mixture of hydrogen and gases such as argon, nitrogen, helium and the like, wherein the hydrogen accounts for 1-20% of the mixed gas.
The invention will be further described in detail with reference to the following examples:
example one
The humidity-sensitive porous ceramic provided by the embodiment of the invention is prepared from a substrate material, wherein the substrate material comprises a component A, a component B, a component C, a pore-forming agent and a sintering aid, and the component A comprises SnO2、ZnO、TiO2The component B comprises ZnCrVO4，V2O5The C component includes Li210 parts of component A, 5 parts of component B, 5 parts of component C, 20 parts of pore-forming agent, 150-micron graphite and 10 parts of sintering aid, namely oleic acid.
Example two
The humidity-sensitive porous ceramic provided by the embodiment of the invention is prepared from a substrate material, wherein the substrate material comprises a component A, a component B, a component C, a pore-forming agent and a sintering aid, and the component A comprises SnO2、ZnO、TiO2The component B comprises ZnCrVO4，V2O5The C component includes Li210 parts of component A, 5 parts of component B, 5 parts of component C, 20 parts of pore-forming agent, 150-micron graphite, 10 parts of sintering aid, and 20 parts of nano silicon dioxide. The nano-silica is silica sol with the particle size of 150nm, and the amount of the nano-silica in the silica sol is calculated by the solid silica in the silica sol.
EXAMPLE III
As shown in fig. 1, the atomizing core of the embodiment of the present invention includes a liquid guiding body 1, a heating element (not shown), positive and negative electrodes 2 disposed at two ends of the heating element, and a humidity detection electrode 3 connected to a humidity sensitive material, the heating element is disposed inside the liquid guiding body 1, the liquid guiding body 1 is used for guiding a liquid to be atomized, the liquid guiding body 1 is made of the humidity sensitive porous ceramic described in the previous embodiment, the liquid to be atomized flows to the liquid guiding body 1 from top to bottom, and the liquid guiding body 1 can guide and permeate the liquid to be atomized. The liquid guide body 1 comprises a humidity sensitive material, the humidity sensitive material has certain conductivity and resistance, the resistance of the humidity sensitive material changes along with the difference of humidity, a humidity detection electrode 3 is connected with the humidity sensitive material, and the humidity in the liquid guide body 1 can be detected through the humidity detection electrode 3.
The humidity of the liquid leading body 1 means relative humidity, and when the liquid leading body 1 completely absorbs, permeates, and stores the liquid to be atomized to the maximum, the humidity is 100%, and when the liquid leading body 1 does not absorb the liquid to be atomized, that is, completely dry, the humidity is 0%. The humidity sensor 13 can sense the humidity of the liquid 1 by a resistance change.
Example four
The preparation method of the humidity-sensitive porous ceramic provided by the embodiment of the invention comprises the following steps:
weighing A component and SnO according to a formula2、ZnO、TiO2The component B comprises ZnCrVO4，V2O5The C component includes Li210 parts of component A, 5 parts of component B, 5 parts of component C, 20 parts of pore-forming agent, 150-micron graphite, 10 parts of sintering aid, oleic acid, and the components are placed in a ball milling device for mixing and ball milling, wherein the rotating speed of the ball milling device is set to 300rpm, the ball milling time is 8 hours, and the diameter of the grinding material is 20 mm;
and baking and drying the mixture subjected to ball milling to obtain mixed powder, wherein the baking and drying temperature is 90 ℃, and the baking and drying time is 10 hours.
Thirdly, heating the paraffin to 65 ℃ to be in a melting state, adding the mixed powder while stirring, and continuously stirring for 8 hours after the addition is finished to obtain paraffin slurry; the melting point of the paraffin is 60 ℃, and the weight of the paraffin is 50 percent of the weight of the mixed powder;
fourthly, injecting the paraffin slurry into a pre-prepared mold, cooling and molding, and demolding to obtain a wax mold;
fifthly, putting the wax mold into a furnace for preheating for wax removal, wherein the wax removal temperature is 800 ℃, and the wax removal time is 12 hours, so that a wax removal sample is obtained;
sixthly, placing the paraffin removal sample into a furnace and sintering the paraffin removal sample in a protective atmosphere, wherein the sintering process comprises heating, heat preservation and cooling, the sintering temperature is 1000 ℃, the heating speed is 5 ℃/min, the sintering heat preservation time is 10h, the sintering protective atmosphere is a reducing atmosphere, the reducing atmosphere comprises hydrogen and argon, the hydrogen accounts for 15% of the mixed gas, and finally the humidity-sensitive porous ceramic is obtained.
The above-mentioned embodiments are only preferred embodiments of the present invention, and all equivalent changes and modifications made within the scope of the claims of the present invention should be covered by the claims of the present invention.

Claims (14)

1. The humidity-sensitive porous ceramic is characterized by being prepared from a matrix material, wherein the matrix material comprises a component A, a component B, a component C, a pore-forming agent and a sintering aid, and the component A is SnO2、ZnO、TiO2The component B is LiZnVO4、ZnCrVO4，V2O5、Fe2O3Is Li, the C component is Li2O、Na2O，K2One or more of O, MgO and CaO, wherein the component A comprises 1-20 parts, the component B comprises 1-10 parts, the component C comprises 1-20 parts, the pore-forming agent comprises 1-30 parts, and the sintering aid comprises 1-10 parts.
2. The moisture-sensitive porous ceramic according to claim 1, wherein the component A comprises 1-10 parts, the component B comprises 1-5 parts, the component C comprises 1-10 parts, the pore-forming agent comprises 1-20 parts, and the sintering aid comprises 1-10 parts.
3. The moisture-sensitive porous ceramic according to claim 1, wherein the pore-forming agent is at least one of graphite, starch, flour, bean flour, polystyrene microspheres, polymethyl methacrylate microspheres, carbonate, ammonium salt, sucrose and fibers, and the particle size of the pore-forming agent is 1-200 microns.
4. The moisture-sensitive porous ceramic according to claim 1, wherein the sintering aid is at least one of boron oxide, boric acid, oleic acid, stearic acid, sodium silicate, and calcium oxide.
5. The moisture-sensitive porous ceramic according to claim 1, wherein the matrix material further comprises the following components in parts by weight: 1-40 parts of nano silicon oxide.
6. The moisture-sensitive porous ceramic according to claim 5, wherein the nano-silica is nano-silica, and the nano-silica is colloidal nano-silica or powdered nano-silica.
7. The moisture-sensitive porous ceramic according to claim 1, wherein the porosity of the moisture-sensitive porous ceramic is 30 to 70%.
8. An atomizing core, which is characterized by comprising a liquid guide body for conducting liquid to be atomized and a heating element arranged on the liquid guide body, wherein the liquid guide body is made of the humidity-sensitive porous ceramic as claimed in any one of claims 1 to 7.
9. A preparation method of humidity-sensitive porous ceramic is characterized by comprising the following steps:
weighing a component A, a component B, a component C, a pore-forming agent and a sintering aid according to a formula, and placing the components in a ball milling device for mixing and ball milling; the component A is SnO2、ZnO、TiO2The component B is LiZnVO4、ZnCrVO4，V2O5、Fe2O3Is Li, the C component is Li2O、Na2O，K2One or more of O, MgO and CaO;
baking and drying the mixture subjected to ball milling to obtain mixed powder;
thirdly, heating the paraffin to a melting state, adding the mixed powder while stirring, and continuously stirring for 1-8 hours after the addition is finished to obtain paraffin slurry;
fourthly, injecting the paraffin slurry into a pre-prepared mold, cooling and molding, and demolding to obtain a wax mold;
fifthly, putting the wax mold into a furnace for preheating for paraffin removal, so as to obtain a paraffin removal sample;
sixthly, placing the paraffin removal sample into a furnace and sintering in a protective atmosphere, wherein the sintering process comprises heating, heat preservation and cooling, and the humidity-sensitive porous ceramic is obtained.
10. The method for preparing the moisture-sensitive porous ceramic according to claim 9, characterized in that in the step of performing, the rotating speed of a ball milling device is set to be 150-350 rpm, the ball milling time is 1-12 h, and the diameter of the grinding material is 1-20 mm.
11. The preparation method of the moisture-sensitive porous ceramic according to claim 9, wherein in the second step, the temperature of baking and drying is 60-120 ℃, and the time of baking and drying is 2-12 h.
12. The method for preparing the moisture-sensitive porous ceramic according to claim 9, wherein in the third step, the melting point of the paraffin is 50 to 110 ℃, and the weight of the paraffin is 10 to 60 percent of the weight of the mixed powder.
13. The preparation method of the moisture-sensitive porous ceramic according to claim 9, characterized in that in the step fifthly, the temperature for removing the wax is 400-800 ℃, and the time for removing the wax is 2-12 hours.
14. The method for preparing the humidity-sensitive porous ceramic according to claim 9, characterized in that in the step sixteenth, the sintering temperature is 700-1200 ℃, the temperature rising speed is 1-5 ℃/min, and the sintering heat preservation time is 2-12 h; the sintering protective atmosphere is a reducing atmosphere, the reducing atmosphere comprises the mixture of hydrogen and gases such as argon, nitrogen, helium and the like, wherein the hydrogen accounts for 1-20% of the mixed gas.
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Application publication date: 20210518